Method for producing resin microparticle aqueous dispersion, and resin microparticle aqueous dispersion and resin microparticles obtained by the same

The object of the present invention is to provide a method for producing a resin microparticle aqueous dispersion, which can produce monodisperse resin microparticles, does not cause clogging by a product, does not require a high pressure, and has a high productivity. Thus, provided is a method for producing a resin microparticle aqueous dispersion, wherein a fluid having at least one kind of resin dissolved in a solvent with which a resin is soluble and compatible and a fluid of an aqueous solvent join together in a thin film fluid formed between processing surfaces arranged opposite so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, whereby resin microparticles are obtained in the thin film fluid by way of separation/emulsification.

TECHNICAL FIELD

The present invention relates to a method for producing resin microparticle aqueous dispersion, and resin microparticle aqueous dispersion and resin microparticles obtained by this method.

BACKGROUND ART

In recent years, in the fields of paint, ink, adhesive, and the like, conversion in the composition is taking place from an organic solvent type to an aqueous type in view of such aspects as resource saving, environmental hygiene, pollution-free, and less danger. As the examples of vehicles used in an aqueous paint composition, there may be mentioned such resins as alkyd resin, acrylic resin, polyester resin, polyurethane resin, and epoxy resin. As the examples of transparent resins usable in optical applications such as an organic glass and a plastic lens, there may be mentioned such resins as methacrylic resin, polycarbonate resin, styrene resin, and epoxy resin. An aqueous emulsion formed by dispersing resin microparticles into water can be used in various uses, e.g., for resin particles in cosmetics and toners in electrophotograph, because of the spherical shape of the resin particle.

Among them, polyester resins represented by polyethylene terephthalate are excellent in such as mechanical, thermal, and electrical properties, and thus they are widely used in such articles as films, sheets, and bottles for various applications, whereby their demands are expanding. To produce such resin microparticles, as described in Patent Document 1, a method in which a solution containing dissolved resin in an organic solvent is preliminarily mixed with water and then the obtained mixture is emulsified with a mechanical energy in a batch-wise manner, is known. As described in Patent Document 2, a method for producing polyester resin microparticle aqueous dispersion, wherein a swelling material swollen in an organic solvent having a boiling temperature of below 100° C. with which the polyester resin can be swollen but is insoluble is mixed with an aqueous solvent containing a basic compound thereby neutralizing a part or all of the carboxyl group in the polyester resin by the basic compound while dispersing the swelling material into the aqueous solvent in the state of microparticles, and then the organic solvent is removed, is known. Further, as described in Patent Document 3 and Patent Document 4, a method to produce resin microparticles, wherein a molten resin is preliminarily mixed in an aqueous solvent and then a mechanical shear force is applied to the mixture thus obtained, is known.

However, with the methods as mentioned above, it has been difficult to obtain monodisperse and uniform particle diameter and particle size distribution, and in addition, raw materials usable for them have been limited. Furthermore, when an organic solvent is used, there is an absolute necessity of a step of solvent-removal after the step of emulsification/dispersion of the resin, which may be highly probable to result in complicated process and prolonged time for production. When resin microparticles are obtained by applying mechanical shear force to the molten resin, especially when the resin is molten and emulsified/dispersed in an aqueous solvent, treatment under normal pressure is difficult, whereby treatment under high temperature and high pressure becomes an absolute necessity. Naturally, this leads to a high danger, and in addition, specification of the equipment is for high temperature and high pressure, thereby tending to heavy equipment whose operation is difficult. Further, when the resin is molten under high temperature and high pressure, especially in the process in which the molten resin is preliminarily mixed in an aqueous solvent and then emulsified/dispersed, hydrolysis of the resin often occurs often because of long residence time in water at high temperature and application of mechanical shear force. All of these problems are caused by nonuniformity of the agitation in the reactor. That is, uniform distribution of concentration and temperature in the reactor is difficult to be established, and thus a complicated process, a prolonged residence time at high temperature and high pressure, excessive mechanical energy, a heavy equipment and hydrolysis accompanied by them, and so the like, would be resulted as mentioned above. Such problems may be solved by conducting the foregoing emulsification/dispersion in a microreaction field whereby temperature, concentration, and mixing state are strictly controlled, thereby enabling to accomplish uniformity of particle size and unification of reaction product effectively and efficiently.

Described in Patent Document 5, production methods of kinds of microparticles using various microreactors and micromixers are informed. There are many advantages in microreactors and systems thereof, but as the micro flow path diameter is decreased, a pressure loss is inversely proportional to the biquadrate of the flow path. That is, such high feeding pressure is necessary that a pump making possible to feed a fluid cannot be available. In the case of a reaction accompanied by separation, there is a problem that a microwave flow path is blocked by clogging of a flow path with a product or bubbles the reaction generates. Further, it is also a problem that since the reaction fundamentally depends on speed of molecular diffusion, a microscopic space is not effective or applicable to every reaction, and actual attempts of the reaction are required by trial and error, then good results are selected. Scaling up has been coped with a method of increasing the number of microreactors, that is a numbering-up system, but the number of microreactors which can be comprised is limited to several dozen, thus inherently aiming exclusively at products of high value. The increase in the number of devices leads to an increase in the absolute number of failure causes, and when the problem of clogging or the like actually occurs, it can be very difficult to detect a problem site such as a failure site.

In view of the above-mentioned, the present invention attempts to obtain resin microparticles in a thin film fluid formed between processing surfaces arranged opposite so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, and has an object to provide a method for producing a resin microparticle aqueous dispersion, which can produce resin microparticles having monodispersity depending on its purpose owing to high uniformity of temperature in the thin film fluid and of the agitation in the reactor, and does not cause clogging with a product by self-dischargeability, and does not require a high pressure, and has a high productivity. An object further is to provide a method for producing a resin microparticle aqueous dispersion, which can produce uniform resin particles with a low energy and can remove a solvent more conveniently than by conventional methods. An object further is to provide a method for producing a resin microparticle aqueous dispersion, which enables to conduct the emulsification/dispersion treatment continuously in a short time, and because of its small holding quantity the equipment can be downsized thereby securing easy handling and high safety even when the molten resin is emulsified/dispersed at a high temperature. An object further is to provide a method for producing resin microparticle aqueous dispersion, which can produce an intended particle size distribution without the preliminary mixing, with a reduced risk of hydrolysis by a short treatment time, and with low energy.

DISCLOSURE OF INVENTION

An aspect of the present invention provides a method for producing a resin microparticle aqueous dispersion, wherein:

at least two fluids are used, wherein

at least one kind of the fluids is a fluid having at least one kind of resin dissolved in a solvent with which a resin is soluble and compatible,

at least one kind of fluid other than said fluids is a liquid of an aqueous solvent, and

the respective fluids join together in a thin film fluid formed between two processing surfaces arranged opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, whereby resin microparticles are obtained in the thin film fluid by way of separation.

An aspect of the present invention provides a method for producing a resin microparticle aqueous dispersion, wherein:

at least two fluids are used, wherein

at least one kind of the fluids is a fluid having at least one kind of resin dissolved in a solvent with which a resin is soluble and compatible,

at least one kind of fluid other than said fluids is a liquid of an aqueous solvent, and

the respective fluids join together in a thin film fluid formed between two processing surfaces arranged opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, whereby resin microparticles are obtained in the thin film fluid by way of emulsification.

An aspect of the invention provides a method for producing a resin microparticle aqueous dispersion, wherein:

at least two fluids are used, wherein

at least one kind of the fluids is a fluid containing at least one kind of resin that is heated and molten,

at least one kind of fluid other than said fluids is a liquid of an aqueous solvent, and

the respective fluids join together in a thin film fluid formed between two processing surfaces arranged opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, whereby resin microparticles are obtained in the thin film fluid by way of emulsification/dispersion.

An aspect of the invention provides the method for producing resin microparticle aqueous dispersion, wherein a step of preliminary mixing of resin in an aqueous solvent in the method, before the fluid is introduced between the processing surfaces, can be omitted.

Here, the foregoing term “preliminary mixing” refers to a preliminary mixing of a resin and an aqueous solvent in such a manner that coarse resin particles become the sate of dispersion though the composition is completely the same as the resin microparticle aqueous dispersion obtained by the production method according to the present invention.

An aspect of the invention provides the method for producing a resin microparticle aqueous dispersion, wherein the production method comprises:

a fluid pressure imparting mechanism for imparting predetermined pressure to a fluid to be processed,

at least two processing members of a first processing member and a second processing member, the second processing member being capable of approaching to and separating from the first processing member, and

a rotation drive mechanism for rotating the first processing member and the second processing member relative to each other,

wherein each of the processing members is provided with at least two processing surfaces of a first processing surface and a second processing surface disposed in a position they are faced with each other,

wherein each of the processing surfaces constitutes part of a sealed flow path through which the fluid under the predetermined pressure is passed,

wherein two or more fluids to be processed, at least one of which contains a reactant, are uniformly mixed and positively reacted between the processing surfaces,

wherein, of the first and second processing members, at least the second processing member is provided with a pressure-receiving surface, and at least part of the pressure-receiving surface is comprised of the second processing surface,

wherein the pressure-receiving surface receives pressure applied to the fluid by the fluid pressure imparting mechanism thereby generating a force to move in the direction of separating the second processing surface from the first processing surface,

wherein the fluid under the predetermined pressure is passed between the first and second processing surfaces being capable of approaching to and separating from each other and rotating relative to each other, whereby the processed fluid forms a fluid film of predetermined thickness while passing between both the processing surfaces; and further comprises:

another introduction path independent of the flow path through which the fluid to be processed under the predetermined pressure is passed, and

at least one opening leading to the separate introduction path and being arranged in at least either the first processing surface or the second processing surface,

wherein at least one processed fluid sent from the introduction path is introduced into between the processing surfaces, whereby said thin film liquid is formed, wherein the resin contained in at least any one of the aforementioned processed fluids and a fluid other than said processed fluids are mixed under uniform stirring in the fluid film to obtain resin microparticles.

An aspect of the invention provides the method for producing a resin microparticle aqueous dispersion, wherein the space between the processing surfaces is cooled or heated thereby obtaining desired resin particles.

An aspect of the invention provides the method for producing a resin microparticle aqueous dispersion, wherein the separation or emulsification/dispersion is conducted in a container capable of securing a depressurized or vacuum state, to form a depressurized or vacuum state of the secondary side at which the fluid after processing is discharged thereby being capable of removing a solvent in the fluid or a gas generated by way of joining of each of the fluid in the thin film fluid and a gas contained in the fluid.

An aspect of the invention provides the method for producing a resin microparticle aqueous dispersion, wherein the separation or emulsification/dispersion is conducted in a container capable of adjusting a temperature, to heat the inside of the container thereby improving efficiency of the treatments of removing the solvent and the gas.

An aspect of the invention provides the method for producing a resin microparticle aqueous dispersion, wherein the separation or emulsification/dispersion is conducted in a container capable of adjusting a temperature, to cool the processed fluid immediately after the fluid is discharged.

An aspect of the invention provides the method for producing a resin microparticle aqueous dispersion, wherein the resin is at least one kind of resin selected from styrene resin, olefin resin, acrylic resin, halogen-containing resin, vinyl ester resin or derivatives thereof, polyester resin, polyamide resin, polyurethane resin, poly(thio)ether resin, polycarbonate resin, polysulfone resin, polyimide resin, cellulose ester resin, and epoxy resin.

An aspect of the invention provides the method for producing a resin microparticle aqueous dispersion, wherein the resin contains a colorant.

An aspect of the invention provides the method for producing a resin microparticle aqueous dispersion, wherein at least one kind of the fluids contains a dispersant like water-soluble resin such as surfactants, polyvinyl alcohol, polyethylene glycol, polyethylene oxide, polyvinyl pyrrolidone, water-soluble acrylic resin, water-soluble styrene resin and cellulose ether resin, and oligosaccharide.

An aspect of the invention provides the method for producing a resin microparticle aqueous dispersion, wherein at least one kind of the fluids contains a colorant, an electrification regulator, a releast agent, an external additive, a magnetic carrier, and electrically conductive powders.

An aspect of the invention provides the method for producing a resin microparticle aqueous dispersion, wherein at least one kind of the fluids contain silver nanoparticles.

An aspect of the invention provides the method for producing a resin microparticle aqueous dispersion, wherein the volume-average particle size of the obtained resin microparticles is 1 nm to 10000 nm.

An aspect of the invention provides a resin microparticle aqueous dispersion obtained by the production method.

An aspect of the invention provides resin microparticles obtained by the production method.

The present invention produces resin microparticles in a thin film fluid formed between processing surfaces arranged to be opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, wherein resin particles having an average particle size smaller than that of resin microparticles obtained by a usual reaction method can be obtained. The present invention is a preferable method for producing resin microparticles, wherein resin microparticles can be obtained continuously and efficiently while coping with production with high production efficiency. Depending on a necessary amount of production, the apparatus can grow in size by using general scale-up concept. Further, resin particles can be obtained uniformly with low energy. In addition, when the separation or emulsification/dispersion treatment and the solvent removal treatment are conducted almost simultaneously, the fluid containing the resin microparticles that are emulsified/dispersed between the processing surfaces is discharged in the state of mist from the processing surfaces thereby increasing surface area of the fluid, resulting in a high efficiency of the solvent removal. Accordingly, the separation or emulsification/dispersion treatment and the solvent removal treatment can be conducted in a substantially single step in a more convenient manner than conventional methods. Further, the separation or emulsification/dispersion treatment can be conducted continuously in a short time, and because of its small holding quantity the equipment can be downsized thereby securing easy handling and high safety even when the molten resin is separated or emulsified/dispersed at a high temperature. In addition, a risk of hydrolysis can be reduced due to a short treating time, and an intended particle size distribution can be obtained with low energy.

BEST MODE FOR CARRYING OUT THE INVENTION

The present invention relates to a method for producing resin microparticles by separation as described in Patent Document 5, or a method for producing resin microparticles by emulsification in a fluid as described in Patent Document 1, and is characterized in that the fluid is formed into a thin film fluid between two processing surfaces arranged so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, and resin microparticles are separated or emulsified/dispersed in the thin film fluid.

More specifically, at least two kinds of fluids are used, at least one kind of which contains at least one kind of resin, and at least one kind of a fluid other than the above fluid is an aqueous solvent, and each of said fluids join together in a thin film fluid formed between the processing surfaces thereby obtaining resin microparticles by separation or emulsification/dispersion in the thin film fluid.

An apparatus of the same principle as described in JP-A 2004-49957 filed by the present applicant, for example, can be used in the method of uniform stirring and mixing in a thin film fluid formed between processing surfaces arranged to be opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other.

Hereinafter, the fluid processing apparatus suitable for carrying out this method is described.

As shown inFIG. 1(A), this apparatus includes opposing first and second processing members10and20, at least one of which rotates to the other. The opposing surfaces of both the processing members10and20serve as processing surfaces1and2to process a fluid to be processed therebetween. The first processing member10includes a first processing surface1, and the second processing member20includes a second processing surface2.

Both the processing surfaces1and2are connected to a flow path of the fluid to constitute a part of the flow path of the fluid.

Specifically, this apparatus constitutes flow paths of at least two fluids to be processed and joins the flow paths together.

That is, this apparatus is connected to a flow path of a first fluid to form a part of the flow path of the first fluid and simultaneously forms a part of a flow path of a second fluid other than the first fluid. This apparatus joins both the flow paths together thereby mixing and reacting both the fluids between the processing surfaces1and2. In the embodiment shown inFIG. 1(A), each of the flow paths is hermetically closed and made liquid-tight (when the processed fluid is a liquid) or air-tight (when the processed fluid is a gas).

Specifically, this apparatus as shown inFIG. 1(A)includes the first processing member10, the second processing member20, a first holder11for holding the first processing member10, a second holder21for holding the second processing member20, a surface-approaching pressure imparting mechanism4, a rotation drive member, a first introduction part d1, a second introduction part d2, a fluid pressure imparting mechanism p1, a second fluid supply part p2, and a case3.

Illustration of the rotation drive member is omitted.

At least one of the first processing member10and the second processing member20is able to approach to and separate from each other, and the processing surfaces1and2are able to approach to and separate from each other.

In this embodiment, the second processing member20approaches to and separates from the first processing member10. On the contrary, the first processing member10may approach to and separate from the second processing member20, or both the processing members10and20may approach to and separate from each other.

The second processing member20is disposed over the first processing member10, and the lower surface of the second processing member20serves as the second processing surface2, and the upper surface of the first processing member10serves as the first processing surface1.

As shown inFIG. 1(A), the first processing member10and the second processing member20in this embodiment are circular bodies, that is, rings. Hereinafter, the first processing member10is referred to as a first ring10, and the second processing member20as a second ring20.

Both the rings10and20in this embodiment are metallic members having, at one end, a mirror-polished surface, respectively, and their mirror-polished surfaces are referred to as the first processing surface1and the second processing surface2, respectively. That is, the upper surface of the first ring10is mirror-polished as the first processing surface1, and the lower surface of the second ring20is mirror-polished as the second processing surface2.

At least one of the holders can rotate relative to the other holder by the rotation drive member. InFIG. 1(A), numerical50indicates a rotary shaft of the rotation drive member. The rotation drive member may use an electric motor. By the rotation drive member, the processing surface of one ring can rotate relative to the processing surface of the other ring.

In this embodiment, the first holder11receives drive power on the rotary shaft50from the rotation drive member and rotates relative to the second holder21, whereby the first ring10integrated with the first holder11rotates relative to the second ring20. Inside the first ring10, the rotary shaft50is disposed in the first holder11so as to be concentric, in a plane, with the center of the circular first ring10.

The first ring10rotates centering on the shaft center of the ring10. The shaft center (not shown) is a virtual line referring to the central line of the ring10.

In this embodiment as described above, the first holder11holds the first ring10such that the first processing surface1of the first ring10is directed upward, and the second holder21holds the second ring20such that the second processing surface2of the second ring20is directed downward.

Specifically, the first and second holders11and21include a ring-accepting concave part, respectively. In this embodiment, the first ring10is fitted in the ring-accepting part of the first holder11, and the first ring10is fixed in the ring-accepting part so as not to rise from, and set in, the ring-accepting part of the first holder11.

That is, the first processing surface1is exposed from the first holder11and faces the second holder21.

Examples of the material for the first ring10include metal, ceramics, sintered metal, abrasion-resistant steel, metal subjected to hardening treatment, and rigid materials subjected to lining, coating or plating. The first processing member10is preferably formed of a lightweight material for rotation. A material for the second ring20may be the same as that for the first ring10.

The ring-accepting part41arranged in the second holder21accepts the processing surface2of the second ring20such that the processing member can rise and set.

The ring-accepting part41of the second holder21is a concave portion for mainly accepting that side of the second ring20opposite to the processing surface2, and this concave portion is a groove which has been formed into a circle when viewed in a plane.

The ring-accepting part41is formed to be larger in size than the second ring20so as to accept the second ring20with sufficient clearance between itself and the second ring20.

By this clearance, the second ring20in the ring-accepting part41can be displaced not only in the axial direction of the circular ring-accepting part41but also in a direction perpendicular to the axial direction. In other words, the second ring20can, by this clearance, be displaced relative to the ring-accepting part41to make the central line of the ring20unparallel to the axial direction of the ring-accepting part41.

Hereinafter, that portion of the second holder21which is surrounded by the second ring20is referred to as a central portion22.

In other words, the second ring20is displaceably accepted within the ring-accepting part41not only in the thrust direction of the ring-accepting part41, that is, in the direction in which the ring20rises from and sets in the part41, but also in the decentering direction of the ring20from the center of the ring-accepting part41. Further, the second ring20is accepted in the ring-accepting part41such that the ring20can be displaced (i.e. run-out) to vary the width between itself upon rising or setting and the ring-accepting part41, at each position in the circumferential direction of the ring20.

The second ring20, while maintaining the degree of its move in the above three directions, that is, the axial direction, decentering direction and run-out direction of the second ring20relative to the ring-accepting part41, is held on the second holder21so as not to follow the rotation of the first ring10. For this purpose, suitable unevenness (not shown) for regulating rotation in the circumferential direction of the ring-accepting part41may be arranged both in the ring-accepting part41and in the second ring20. However, the unevenness should not deteriorate displacement in the degree of its move in the three directions.

The surface-approaching pressure imparting mechanism4supplies the processing members with force exerted in the direction of approaching the first processing surface1and the second processing surface2each other. In this embodiment, the surface-approaching pressure imparting mechanism4is disposed in the second holder21and biases the second ring20toward the first ring10.

The surface-approaching pressure imparting mechanism4uniformly biases each position in the circumferential direction of the second ring20, that is, each position of the processing surface2, toward the first ring10. A specific structure of the surface-approaching pressure imparting mechanism4will be described later.

As shown inFIG. 1(A), the case3is arranged outside the outer circumferential surfaces of both the rings10and20, and accepts a product formed between the processing surfaces1and2and discharged to the outside of both the rings10and20. As shown inFIG. 1(A), the case3is a liquid-tight container for accepting the first holder11and the second holder21. However, the second holder21may be that which as a part of the case, is integrally formed with the case3.

As described above, the second holder21whether formed as a part of the case3or formed separately from the case3is not movable so as to influence the distance between both the rings10and20, that is, the distance between the processing surfaces1and2. In other words, the second holder21does not influence the distance between the processing surfaces1and2.

The case3is provided with an outlet32for discharging a product to the outside of the case3.

The first introduction part d1supplies a first fluid to be processed to the space between the processing surfaces1and2.

The fluid pressure imparting mechanism p1is connected directly or indirectly to the first introduction part d1to impart fluid pressure to the first fluid. A compressor or a pump can be used in the fluid pressure imparting mechanism p1.

In this embodiment, the first introduction part d1is a fluid path arranged inside the central part22of the second holder21, and one end of the first introduction part d1is open at the central position of a circle, when viewed in a plane, of the second ring20on the second holder21. The other end of the first introduction part d1is connected to the fluid pressure imparting mechanism p1outside the second holder21, that is, outside the case3.

The second introduction part d2supplies a second fluid to be reacted with the first fluid to the space between the processing surfaces1and2. In this embodiment, the second introduction part is a fluid passage arranged inside the second ring20, and one end of the second introduction part is open at the side of the second processing surface2, and a second fluid-feeding part p2is connected to the other end.

A compressor or a pump can be used in the second fluid-feeding part p2.

The first processed fluid pressurized with the fluid pressure imparting mechanism p1is introduced from the first introduction part d1to the space between the rings10and20and will pass through the space between the first processing surface1and the second processing surface2to the outside of the rings10and20.

At this time, the second ring20receiving the supply pressure of the first fluid stands against the bias of the surface-approaching pressure imparting mechanism4, thereby receding from the first ring10and making a minute space between the processing surfaces. The space between both the processing surfaces1and2by approach and separation of the surfaces1and2will be described in detail later.

A second fluid is supplied from the second introduction part d2to the space between the processing surfaces1and2, flows into the first fluid, and is subjected to a reaction promoted by rotation of the processing surface. Then, a reaction product formed by the reaction of both the fluids is discharged from the space between the processing surfaces1and2to the outside of the rings10and20. The reaction product discharged to the outside of the rings10and20is discharged finally through the outlet of the case to the outside of the case.

The mixing and reaction of the processed fluid are effected between the first processing surface1and the second processing surface2by rotation, relative to the second processing member20, of the first processing member10with the drive member.

Between the first and second processing surfaces1and2, a region downstream from an opening m2of the second introduction part d2serves as a reaction chamber where the first and second processed fluids are reacted with each other. Specifically, as shown inFIG. 11(C)illustrating a bottom face of the second ring20, a region H shown by oblique lines, outside the second opening m2of the second introduction part in the radial direction r1of the second ring20, serves as the processing chamber, that is, the reaction chamber. Accordingly, this reaction chamber is located downstream from the openings m1and m2of the first introduction part d1and the second introduction part d2between the processing surfaces1and2.

The first fluid introduced from the first opening m1through a space inside the ring into the space between the processing surfaces1and2, and the second fluid introduced from the second opening m2into the space between the processing surfaces1and2, are mixed with each other in the region H serving as the reaction chamber, and both the processed fluids are reacted with each other. The fluid will, upon receiving supply pressure from the fluid pressure imparting mechanism p1, move through the minute space between the processing surfaces1and2to the outside of the rings, but because of rotation of the first ring10, the fluid mixed in the reaction region H does not move linearly from the inside to the outside of the rings in the radial direction, but moves from the inside to the outside of the ring spirally around the rotary shaft of the ring when the processing surfaces are viewed in a plane. In the region H where the fluids are thus mixed and reacted, the fluids can move spirally from inside to outside to secure a zone necessary for sufficient reaction in the minute space between the processing surfaces1and2, thereby promoting their uniform reaction.

The product formed by the reaction becomes a uniform reaction product in the minute space between the first processing surface1and the second processing surface2and appears as microparticles particularly in the case of crystallization or separation.

By the balance among at least the supply pressure applied by the fluid pressure imparting mechanism p1, the bias of the surface-approaching pressure imparting mechanism4, and the centrifugal force resulting from rotation of the ring, the distance between the processing surfaces1and2can be balanced to attain a preferable minute space, and further the processed fluid receiving the supply pressure applied by the fluid pressure imparting mechanism p1and the centrifugal force by rotation of the ring moves spirally in the minute space between the processing surfaces1and2, so that their reaction is promoted.

The reaction is forcedly effected by the supply pressure applied by the fluid pressure imparting mechanism p1and the rotation of the ring. That is, the reaction occurs under forced uniform mixing between the processing surfaces1and2arranged opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other.

Accordingly, the crystallization and separation of the product formed by the reaction can be regulated by relatively easily controllable methods such as regulation of supply pressure applied by the fluid pressure imparting mechanism p1and regulation of the rotating speed of the ring, that is, the number of revolutions of the ring.

As described above, this processing apparatus is excellent in that the space between the processing surfaces1and2, which can exert influence on the size of a product, and the distance in which the processed fluid moves in the reaction region H, which can exert influence on production of a uniform product, can be regulated by the supply pressure and the centrifugal force.

The reaction processing gives not only deposit of the product but also liquids.

The rotary shaft50is not limited to the vertically arranged one and may be arranged in the horizontal direction or arranged at a slant. This is because during processing, the reaction occurs in such a minute space between the processing surfaces1and2that the influence of gravity can be substantially eliminated.

InFIG. 1(A), the first introduction part d1extends vertically and coincides with the shaft center of the second ring20in the second holder21. However, the first introduction part d1is not limited to the one having a center coinciding with the shaft center of the second ring20and may be arranged in other positions in the central portion22of the second holder21as long as the first fluid can be supplied into the space surrounded by the rings10and20, and the first introduction part d1may extend obliquely as well as vertically.

A more preferable embodiment of the apparatus is shown inFIG. 12(A). As shown in this figure, the second processing member20has the second processing surface2and a pressure-receiving surface23which is positioned inside, and situated next to, the second processing surface2. Hereinafter, the pressure-receiving surface23is also referred to as a separation-regulating surface23. As shown in the figure, the separation-regulating surface23is an inclined surface.

As described above, the ring-accepting part41is formed in the bottom (i.e. a lower part) of the second holder21, and the second processing member20is accepted in the ring-accepting part41. The second processing member20is held by the second holder21so as not to be rotated with a baffle (not shown). The second processing surface2is exposed from the second holder21.

In this embodiment, a material to be processed is introduced inside the first processing member10and the second processing member20between the processing surfaces1and2, and the processed material is discharged to the outside of the first processing member10and the second processing member20.

The surface-approaching pressure imparting mechanism4presses by pressure the second processing surface2against the first processing surface1to make them contacted with or close to each other, and generates a thin film fluid of predetermined thickness by the balance between the surface-approaching pressure and the force, e.g. fluid pressure, of separating the processing surfaces1and2from each other. In other words, the distance between the processing surfaces1and2is kept in a predetermined minute space by the balance between the forces.

Specifically, the surface-approaching pressure imparting mechanism4in this embodiment is comprised of the ring-accepting part41, a spring-accepting part42arranged in the depth of the ring-accepting part41, that is, in the deepest part of the ring-accepting part41, a spring43, and an air introduction part44.

However, the surface-approaching pressure imparting mechanism4may be the one including at least one member selected from the ring-accepting part41, the spring-accepting part42, the spring43, and the air introduction part44.

The ring-accepting part41has the second processing member20fit into it with play to enable the second processing member20to be displaced vertically deeply or shallowly, that is, vertically in the ring-accepting part41.

One end of the spring43is abutted against the depth of the spring-accepting part42, and the other end of the spring43is abutted against the front (i.e., the upper part) of the second processing member20in the ring-accepting part41. InFIG. 1, only one spring43is shown, but a plurality of springs43are preferably used to press various parts of the second processing member20. This is because as the number of springs43increases, pressing pressure can be given more uniformly to the second processing member20. Accordingly, several to a few dozen springs43comprising a multi-spring type preferably attach to the second holder21.

In this embodiment, air can be introduced through the air introduction part44into the ring-accepting part41. By such introduction of air, air pressure together with pressure by the spring43can be given as pressing pressure from the space, as a pressurizing chamber, between the ring-accepting part41and the second processing member20to the second processing member20. Accordingly, adjusting the pressure of air introduced through the air introduction part44can regulate the surface-approaching pressure of the second processing surface2toward the first processing surface1during operation. A mechanism of generating pressing pressure with another fluid pressure such as oil pressure can be utilized in place of the air introduction part44utilizing air pressure.

The surface-approaching pressure imparting mechanism4not only supplies and regulates a part of the pressing pressure, that is, the surface-approaching pressure, but also serves as a displacement regulating mechanism and a buffer mechanism.

Specifically, the surface-approaching pressure imparting mechanism4as a displacement regulating mechanism can maintain initial pressing pressure by regulating air pressure against the change in the axial direction caused by elongation or abrasion at the start of or in the operation. As described above, the surface-approaching pressure imparting mechanism4uses a floating mechanism of maintaining the second processing member20so as to be displaced, thereby also functioning as a buffer mechanism for micro-vibration or rotation alignment.

Now, the state of the thus constituted processing apparatus during use is described with reference toFIG. 1(A).

At the outset, a first fluid to be processed is pressurized with the fluid pressure imparting mechanism p1and introduced through the first introduction part d1into the internal space of the sealed case. On the other hand, the first processing member10is rotated with the rotation of the rotary shaft50by the rotation drive member. The first processing surface1and the second processing surface2are thereby rotated relatively with a minute space kept therebetween.

The first processed fluid is formed into a thin film fluid between the processing surfaces1and2with a minute space kept therebetween, and a second fluid to be processed which is introduced through the second introduction part d2flows into the thin film fluid between the processing surfaces1and2to comprise a part of the thin film fluid. By this, the first and second processed fluids are mixed with each other, and a uniform reaction of both of the fluids being reacted with each other is promoted to form a reaction product. When the reaction is accompanied by separation, relatively uniform and fine particles can be formed. Even when the reaction is not accompanied by separation, a uniform reaction can be realized. The separated reaction product may be further finely pulverized by shearing between the first processing surface1and the second processing surface2with the rotation of the first processing surface1. The first processing surface1and the second processing surface2are regulated to form a minute space of 1 μm to 1 mm, particularly 1 μM to 10 μm, thereby realizing a uniform reaction and enabling production of superfine particles of several nm in diameter.

The product is discharged from the processing surfaces1and2through an outlet32of the case3to the outside of the case. The discharged product is atomized in a vacuum or depressurized atmosphere with a well-known decompression device and converted into liquid in the atmosphere to collide with each other, then what trickled down in the liquid is able to be collected as degassed liquid.

In this embodiment, the processing apparatus is provided with a case3, but may be carried out without a case. For example, a decompression tank for degassing, that is, a vacuum tank, is arranged, and the processing apparatus may be arranged in this tank. In this case, the outlet mentioned above is naturally not arranged in the processing apparatus.

As described above, the first processing surface1and the second processing surface2can be regulated to form a minute space in the order of μm which cannot be formed by arranging mechanical clearance. Now, this mechanism is described.

The first processing surface1and the second processing surface2are capable of approaching to and separating from each other, and simultaneously rotate relative to each other. In this example, the first processing surface1rotates, and the second processing surface2slides in the axial direction thereby approaching to and separating from the first processing surface.

In this example, therefore, the position of the second processing surface2in the axial direction is arranged accurately in the order of μm by the balance between forces, that is, the balance between the surface-approaching pressure and the separating pressure, thereby establishing a minute space between the processing surfaces1and2.

As shown inFIG. 12(A), the surface-approaching pressure includes the pressure by air pressure (positive pressure) from the air introduction part44by the surface-approaching pressure imparting mechanism4, the pressing pressure with the spring43, and the like.

The embodiments shown inFIG. 12toFIG. 15andFIG. 17are shown by omitting the second introduction part d2to simplify the drawings. In this respect, these drawings may be assumed to show sections at a position not provided with the second introduction part d2. In the figures, U and S show upward and downward directions respectively.

On the other hand, the separating force include the fluid pressure acting on the pressure-receiving surface at the separating side, that is, on the second processing surface2and the separation regulating surface23, the centrifugal force resulting from rotation of the first processing member10, and the negative pressure when negative pressure is applied to the air introduction part44.

When the apparatus is washed, the negative pressure applied to the air introduction part44can be increased to significantly separate the processing surfaces1and2from each other, thereby facilitating washing.

By the balance among these forces, the second processing surface2while being remote by a predetermined minute space from the first processing surface1is stabilized, thereby realizing establishment with accuracy in the order of μm.

The separating force is described in more detail.

With respect to fluid pressure, the second processing member20in a closed flow path receives feeding pressure of a processed fluid, that is, fluid pressure, from the fluid pressure imparting mechanism p1. In this case, the surfaces opposite to the first processing surface in the flow path, that is, the second processing surface2and the separation regulating surface23, act as pressure-receiving surfaces at the separating side, and the fluid pressure is applied to the pressure-receiving surfaces to generate a separating force due to the fluid pressure.

With respect to centrifugal force, the first processing member10is rotated at high speed, centrifugal force is applied to the fluid, and a part of this centrifugal force acts as separating force in the direction in which the processing surfaces1and2are separated from each other.

When negative pressure is applied from the air introduction part44to the second processing member20, the negative pressure acts as separating force.

In the foregoing description of the present invention, the force of separating the first and second processing surfaces1and2from each other has been described as a separating force, and the above-mentioned force is not excluded from the separating force.

By forming a balanced state of the separating force and the surface-approaching pressure applied by the surface-approaching pressure imparting mechanism4via the fluid between the processing surfaces1and2in the closed flow path of the fluid, a uniform reaction is realized between the processing surfaces1and2, and simultaneously a thin film fluid suitable for crystallization and separation of microscopic reaction products is formed as described above. In this manner, this apparatus can maintain a minute space between the processing surfaces1and2by the forced thin film fluid, the minute space of is not achievable with a conventional mechanical apparatus, and microparticles can be formed highly accurately as the reaction product.

In other words, the thickness of the thin film fluid between the processing surfaces1and2is regulated as desired by regulating the separating force and surface-approaching pressure, thereby realizing a necessary uniform reaction to form and process microscopic products. Accordingly, when the thickness of the thin film fluid is to be decreased, the surface-approaching pressure or separating force may be regulated such that the surface-approaching pressure is made relatively higher than the separating force. When the thickness of the thin film fluid is to be increased, the separating force or surface-approaching pressure may be regulated such that the separating force is made relatively higher than the surface-approaching pressure.

When the surface-approaching pressure is increased, air pressure, that is, positive pressure is applied from the air introduction part44by the surface-approaching pressure imparting mechanism4, or the spring43is changed to the one having higher pressing pressure, or the number of springs may be increased.

When the separating force is to be increased, the feeding pressure of the fluid pressure imparting mechanism p1is increased, or the area of the second processing surface2or the separation regulating surface23is increased, or in addition, the rotation of the first processing member10is regulated to increase centrifugal force or reduce pressure from the air introduction part44. Alternatively, negative pressure may be applied. The spring43shown is a pressing spring that generates pressing pressure in an extending direction, but may be a pulling spring that generates a force in a compressing direction to constitute a part or the whole of the surface-approaching pressure imparting mechanism4.

When the separating force is to be decreased, the feeding pressure of the fluid pressure imparting mechanism p1is reduced, or the area of the second processing surface2or the separation regulating surface23is reduced, or in addition, the rotation of the first processing member10is regulated to decrease centrifugal force or increase pressure from the air introduction part44. Alternatively, negative pressure may be reduced.

Further, properties of a processed fluid, such as viscosity, can be added as a factor for increasing or decreasing the surface-approaching pressure and separating force, and regulation of such properties of a processed fluid can be performed as regulation of the above factor.

In the separating force, the fluid pressure exerted on the pressure-receiving surface at the separating side, that is, the second processing surface2and the separation regulating surface23is understood as a force constituting an opening force in mechanical seal.

In the mechanical seal, the second processing member20corresponds to a compression ring, and when fluid pressure is applied to the second processing member20, the force of separating the second processing member20from the first processing member10is regarded as opening force.

More specifically, when the pressure-receiving surfaces at a separating side, that is, the second processing surface2and the separation regulating surface23only are arranged in the second processing member20as shown in the first embodiment, all feeding pressure constitutes the opening force. When a pressure-receiving surface is also arranged at the backside of the second processing member20, specifically in the case ofFIG. 12(B)andFIG. 17described later, the difference between the feeding pressure acting as a separating force and the feeding pressure acting as surface-approaching pressure is the opening force.

Now, other embodiments of the second processing member20are described with reference toFIG. 12(B).

As shown inFIG. 12(B), an approach regulating surface24facing upward, that is, at the other side of the second processing surface2, is disposed at the inner periphery of the second processing member20exposed from the ring-accepting part41.

That is, the surface-approaching pressure imparting mechanism4in this embodiment is comprised of a ring-accepting part41, an air introduction part44, and the approach regulating surface24. However, the surface-approaching pressure imparting mechanism4may be one including at least one member selected from the ring-accepting part41, the spring-accepting part42, the spring43, the air introduction part44, and the approach regulating surface24.

The approach regulating surface24receives predetermined pressure applied to a processed fluid to generate a force of approaching the second processing surface2to the first processing surface1, thereby functioning in feeding surface-approaching pressure as a part of the surface-approaching pressure imparting mechanism4. On the other hand, the second processing surface2and the separation regulating surface23receive predetermined pressure applied to a processed fluid to generate a force of separating the second processing surface2from the first processing surface1, thereby functioning in feeding a part of the separating force.

The approach regulating surface24, the second processing surface2and the separation regulating surface23are pressure-receiving surfaces receiving feeding pressure of the processed fluid, and depending on its direction, exhibits different actions, that is, generation of the surface-approaching pressure and generation of a separating force.

The ratio (area ratio A1/A2) of a projected area A1of the approach regulating surface24projected on a virtual plane perpendicular to the direction of approaching and separating the processing surfaces, that is, in the direction of rising and setting of the second ring20, to a total area A2of the projected area of the second processing surface2and the separating side pressure-receiving area23of the second processing member20projected on the virtual plane is called balance ratio K which is important for regulation of the opening force.

Both the top of the approach regulating surface24and the top of the separating side pressure-receiving surface23are defined by the inner periphery25of the circular second regulating part20, that is, by top line L1. Accordingly, the balance ratio is regulated for deciding the place where base line L2of the approach regulating surface24is to be placed.

That is, in this embodiment, when the feeding pressure of the processed fluid is utilized as opening force, the total projected area of the second processing surface2and the separation regulating surface23is made larger than the projected area of the approach regulating surface24, thereby generating an opening force in accordance with the area ratio.

The opening force can be regulated by the pressure of the processed fluid, that is, the fluid pressure, by changing the balance line, that is, by changing the area A1of the approach regulating surface24.

Sliding surface actual surface pressure P, that is, the fluid pressure out of the surface-approaching pressure, is calculated according to the following equation:
P=P1×(K−k)+Ps
wherein P1represents the pressure of a processed fluid, that is, fluid pressure; K represents the balance ratio; k represents an opening force coefficient; and Ps represents a spring and back pressure.

By regulating this balance line to regulate the sliding surface actual surface pressure P, the space between the processing surfaces1and2is formed as a desired minute space, thereby forming a film of the fluid to make the product minute and effecting uniform reaction processing.

Usually, as the thickness of a thin film fluid between the processing surfaces1and2is decreased, the product can be made finer. On the other hand, as the thickness of the thin film fluid is increased, processing becomes rough and the throughput per unit time is increased. By regulating the sliding surface actual surface pressure P on the sliding surface, the space between the processing surfaces1and2can be regulated to realize the desired uniform reaction and to obtain the minute product. Hereinafter, the sliding surface actual surface pressure P is referred to as surface pressure P.

From this relation, it is concluded that when the product is to be made coarse, the balance ratio may be decreased, the surface pressure P may be decreased, the space may be increased and the thickness of the film may be increased. On the other hand, when the product is to be made finer, the balance ratio may be increased, the surface pressure P may be increased, the space may be decreased and the thickness of the film may be decreased.

As a part of the surface-approaching pressure imparting mechanism4, the approach regulating surface24is formed, and at the position of the balance line, the surface-approaching pressure may be regulated, that is, the space between the processing surfaces may be regulated.

As described above, the space is regulated in consideration of the pressing pressure of the spring43and the air pressure of the air introduction part44. Regulation of the fluid pressure, that is, the feeding pressure of the processed fluid, and regulation of the rotation of the first processing member10for regulating centrifugal force, that is, the rotation of the first holder11, are also important factors to regulate the space.

As described above, this apparatus is constituted such that for the second processing member20and the first processing member10that rotates relative to the second processing member20, a predetermined thin film fluid is formed between the processing surfaces by pressure balance among the feeding pressure of the processed fluid, the rotation centrifugal force, and the surface-approaching pressure. At least one of the rings is formed in a floating structure by which alignment such as run-out is absorbed to eliminate the risk of abrasion and the like.

The embodiment shown inFIG. 1(A)also applies to the embodiment inFIG. 12(B)except that the regulating surface is arranged.

The embodiment shown inFIG. 12(B)can be carried out without arranging the pressure-receiving surface23on the separating side, as shown inFIG. 17.

When the approach regulating surface24is arranged as shown in the embodiment shown inFIG. 12(B)andFIG. 17, the area A1of the approach regulating surface24is made larger than the area A2, whereby all of the predetermined pressure exerted on the processed fluid functions as surface-approaching pressure, without generating an opening force. This arrangement is also possible, and in this case, both the processing surfaces1and2can be balanced by increasing other separating force.

With the area ratio described above, the force acting in the direction of separating the second processing surface2from the first processing surface1is fixed as the resultant force exerted by the fluid.

In this embodiment, as described above, the number of springs43is preferably larger in order to impart uniform stress on the sliding surface, that is, the processing surface. However, the spring43may be a single coil-type spring as shown inFIG. 13. As shown in the figure, this spring is a single coil spring having a center concentric with the circular second processing member20.

The space between the second processing member20and the second holder21is sealed air-tightly with methods well known in the art.

As shown inFIG. 14, the second holder21is provided with a temperature regulation jacket46capable of regulating the temperature of the second processing member20by cooling or heating. Numerical3inFIG. 14is the above-mentioned case, and the case3is also provided with a jacket35for the same purpose of temperature regulation.

The temperature regulation jacket46for the second holder21is a water-circulating space formed at a side of the ring-accepting part41and communicates with paths47and48leading to the outside of the second holder21. One of the paths47and48introduces a cooling or heating medium into the temperature regulation jacket46, and the other discharges the medium.

The temperature regulation jacket35for the case3is a path for passing heating water or cooling water, which is arranged between the outer periphery of the case3and a covering part34for covering the outer periphery of the case3.

In this embodiment, the second holder21and the case3are provided with the temperature regulation jacket, but the first holder11can also be provided with such a jacket.

As a part of the surface-approaching pressure imparting mechanism4, a cylinder mechanism7shown inFIG. 15may be arranged besides the members described above.

The cylinder mechanism7includes a cylinder space70arranged in the second holder21, a communicating part71that communicates the cylinder space70with the ring-accepting part41, a piston72that is accepted in the cylinder space70and connected via the communication part71to the second processing member20, a first nozzle73that communicates to the upper part of the cylinder space70, a second nozzle74that communicates to a lower part of the cylinder space70, and a pressing body75such as spring between the upper part of the cylinder space70and the piston72.

The piston72can slide vertically in the cylinder space70, and the second processing member20can slide vertically with sliding of the piston72, to change the gap between the first processing surface1and the second processing surface2.

Although not shown in the figure, specifically, a pressure source such as a compressor is connected to the first nozzle73, and air pressure, that is, positive pressure is applied from the first nozzle73to the upper part of the piston72in the cylinder space70, thereby sliding the piston72downward, to narrow the gap between the first and second processing surfaces1and2. Although not shown in the figure, a pressure source such as a compressor is connected to the second nozzle74, and air pressure, that is, positive pressure is applied from the second nozzle74to the lower part of the piston72in the cylinder space70, thereby sliding the piston72upward, to allow the second processing member20to widen the gap between the first and second processing surfaces1and2, that is, to enable it to move in the direction of opening the gap. In this manner, the surface-approaching pressure can be regulated by air pressure with the nozzles73and74.

Even if there is a space between the upper part of the second processing member20in the ring-accepting part41and the uppermost part of the ring-accepting part41, the piston72is arranged so as to abut against the uppermost part70aof the cylinder space70, whereby the uppermost part70aof the cylinder space70defines the upper limit of the width of the gap between the processing surfaces1and2. That is, the piston and the uppermost part70aof the cylinder space70function as a separation preventing part for preventing the separation of the processing surfaces1and2from each other, in other words, function in regulating the maximum opening of the gap between both the processing surfaces1and2.

Even if the processing surfaces1and2do not abut on each other, the piston72is arranged so as to abut against a lowermost part70bof the cylinder space70, whereby the lowermost part70bof the cylinder space70defines the lower limit of the width of the gap between the processing surfaces1and2. That is, the piston72and the lowermost part70bof the cylinder space70function as an approach preventing part for preventing the approaching of the processing surfaces1and2each other, in other words, function in regulating the minimum opening of the gap between both the processing surfaces1and2.

In this manner, the maximum and minimum openings of the gap are regulated, while a distance z1between the piston72and the uppermost part70aof the cylinder space70, in other words, a distance z2between the piston72and the lowermost part70bof the cylinder space70, is regulated with air pressure by the nozzles73and74.

The nozzles73and74may be connected to a different pressure source respectively, and further may be connected to a single pressure source alternatively or switched the connections to the sources.

The pressure source may be a source applying positive or negative pressure. When a negative pressure source such as a vacuum is connected to the nozzles73and74, the action described above goes to the contrary.

In place of the other surface-approaching pressure imparting mechanism4or as a part of the surface-approaching pressure imparting mechanism4, such cylinder mechanism7is provided to set the pressure of the pressure source connected to the nozzle73and74, and the distances z1and z2according to the viscosity and properties of the fluid to be processed in a fashion to bring the thickness value of thin film fluid of the fluid to a desired level under a shear force to realize a uniform reaction for forming fine particles. Particularly, such cylinder mechanism7can be used to increase the reliability of cleaning and sterilization by forcing the sliding part open and close during cleaning and steam sterilization.

As shown inFIG. 16(A)toFIG. 16(C), the first processing surface1of the first processing member10may be provided with groove-like depressions13. . .13extending in the radial direction, that is, in the direction from the center to the outside of the first processing member10. In this case, as shown inFIG. 16(A), the depressions13. . .13can be curved or spirally elongated on the first processing surface1, and as shown inFIG. 16(B), the individual depressions13may be bent at a right angle, or as shown inFIG. 16(C), the depressions13. . .13may extend straight radially.

As shown inFIG. 16(D), the depressions13inFIG. 16(A)toFIG. 16(C)preferably deepen gradually in the direction toward the center of the first processing surface1. The groove-like depressions13may continue in sequence or intermittence.

Formation of such depression13may correspond to the increase of delivery of the processed fluid or to the decrease of calorific value, while having effects of cavitation control and fluid bearing.

In the embodiments shown inFIG. 16, the depressions13are formed on the first processing surface1, but may be formed on the second processing surface2or may be formed on both the first and second processing surfaces1and2.

When the depressions13or tapered sections are not provided on the processing surface or are arranged unevenly on a part of the processing surface, the influence exerted by the surface roughness of the processing surfaces1and2on the processed fluid is greater than that by the above depressions13. In this case, the surface roughness should be reduced, that is, the surface should be fine-textured, as the particle size of the processed fluid are to be decreased. Particularly, regarding the surface roughness of the processing surface, the mirror surface, that is, a surface subjected to mirror polishing is advantageous in realizing uniform reaction for the purpose of uniform reaction, and in realizing crystallization and separation of fine monodisperse reaction products for the purpose of obtaining microparticles.

In the embodiments shown inFIG. 13toFIG. 17, structures other than those particularly shown are the same as in the embodiments shown inFIG. 1(A)orFIG. 11(C).

In the embodiments described above, the case is closed. Alternatively, the first processing member10and the second processing member20may be closed inside but may be open outside. That is, the flow path is sealed until the processed fluid has passed through the space between the first processing surface1and the second processing surface2, to allow the processed fluid to receive the feeding pressure, but after the passing, the flow path may be opened so that the processed fluid after processing does not receive feeding pressure.

The fluid pressure imparting mechanism p1preferably uses a compressor as a pressure device described above, but if predetermined pressure can always be applied to the processed fluid, another means may be used. For example, the own weight of the processed fluid can be used to apply certain pressure constantly to the processed fluid.

In summary, the processing apparatus in each embodiment described above is characterized in that predetermined pressure is applied to a fluid to be processed, at least two processing surfaces, that is, a first processing surface1and a second processing surface2capable of approaching to and separating from each other are connected to a sealed flow path through which the processed fluid receiving the predetermined pressure flows, a surface-approaching pressure of approaching the processing surfaces1and2each other is applied to rotate the first processing surface1and the second processing surface2relative to each other, thereby allowing a thin film fluid used for seal in mechanical seal to be generated out of the processed fluid, and the thin film fluid is leaked out consciously (without using the thin film fluid as seal) from between the first processing surface1and the second processing surface2, contrary to mechanical seal, whereby reaction processing is realized between the processed fluid formed into a film between the surfaces1and2, and the product is recovered.

By this epoch-making method, the space between the processing surfaces1and2can be regulated in the range of 1 μm to 1 mm, particularly 1 μm to 10 μm.

In the embodiment described above, a flow path for a sealed fluid is constituted in the apparatus, and the processed fluid is pressurized with the fluid pressure imparting mechanism p1arranged at the side of the introduction part (for the first processing fluid) in the processing apparatus.

Alternatively, the flow path for the processed fluid may be opened without pressurization with the fluid pressure imparting mechanism p1.

One embodiment of the processing apparatus is shown inFIG. 18toFIG. 20. The processing apparatus illustrated in this embodiment is an apparatus including a degassing mechanism, that is, a mechanism of removing a liquid from the processed product thereby finally securing objective solids (crystals) only.

FIG. 18(A)is a schematic vertical sectional view of the processing apparatus, andFIG. 18(B)is its partially cut enlarged sectional view.FIG. 19is a plane view of the first processing member101arranged in the processing apparatus inFIG. 18.FIG. 20is a partially cut schematic vertical sectional view showing an important part of the first and second processing members101and102in the processing apparatus.

As described above, the apparatus shown inFIG. 18toFIG. 20is the one into which a fluid as the object of processing, that is, a processed fluid, or a fluid carrying the object of processing, is to be introduced at atmospheric pressure.

InFIG. 18(B)andFIG. 20, the second introduction part d2is omitted for simplicity of the drawing (these drawings can be regarded as showing a section at the position where the second introduction part d2is not arranged).

As shown inFIG. 18(A), this processing apparatus includes a reaction apparatus G and a decompression pump Q. This reaction apparatus G includes a first processing member101as a rotating member, a first holder111for holding the processing member101, a second processing member102that is a member fixed to the case, a second holder121having the second processing member102fixed thereto, a bias mechanism103, a dynamical pressure generating mechanism104(FIG.19(A)), a drive part which rotates the first processing member101with the first holder111, a housing106, a first introduction part d1which supplies (introduces) a first processed fluid, and a discharge part108that discharges the fluid to the decompression pump Q. The drive part is not shown.

The first processing member101and the second processing member102are cylindrical bodies that are hollow in the center. The processing members101and102are members wherein the bottoms of the processing members101and102in a cylindrical form are processing surfaces110and120respectively.

The processing surfaces110and120have a mirror-polished flat part. In this embodiment, the processing surface120of the second processing member102is a flat surface subjected as a whole to mirror polishing. The processing surface110of the first processing member101is a flat surface as a whole like the second processing member102, but has a plurality of grooves112. . .112in the flat surface as shown inFIG. 19(A). The grooves112. . .112while centering on the first processing member101in a cylindrical form extend radially toward the outer periphery of the cylinder.

The processing surfaces110and120of the first and second processing members101and102are mirror-polished such that the surface roughness Ra comes to be in the range of 0.01 μm to 1.0 μm. By this mirror polishing, Ra is regulated preferably in the range of 0.03 μm to 0.3 μm.

The material for the processing members101and102is one which is rigid and capable of mirror polishing. The rigidity of the processing members101and102is preferably at least 1500 or more in terms of Vickers hardness. A material having a low linear expansion coefficient or high thermal conductance is preferably used. This is because when the difference in coefficient of expansion between a part which generates heat upon processing and other parts is high, distortion is generated and securement of suitable clearance is influenced.

As the material for the processing members101and102, it is preferable to use particularly SIC, that is, silicon carbide, SIC having a Vickers hardness of 2000 to 2500, SIC having a Vickers hardness of 3000 to 4000 coated thereon with DLC (diamond-like carbon), WC, that is, tungsten carbide having a Vickers hardness of 1800, WC coated thereon with DLC, and boron ceramics represented by ZrB2, BTC and B4C having a Vickers hardness of 4000 to 5000.

The housing106shown inFIG. 18, the bottom of which is not shown though, is a cylinder with a bottom, and the upper part thereof is covered with the second holder121. The second holder121has the second processing member102fixed to the lower surface thereof, and the introduction part d1is arranged in the upper part thereof. The introduction part d1is provided with a hopper170for introducing a fluid or a processed material from the outside.

Although not shown in the figure, the drive part includes a power source such as a motor and a shaft50that rotates by receiving power from the power source.

As shown inFIG. 18(A), the shaft50is arranged in the housing106and extends vertically. Then, the first holder111is arranged on the top of the shaft50. The first holder111is to hold the first processing member101and is arranged on the shaft50as described above, thereby allowing the processing surface110of the first processing member101to correspond to the processing surface120of the second processing member102.

The first holder111is a cylindrical body, and the first processing member101is fixed on the center of the upper surface. The first processing member101is fixed so as to be integrated with the first holder111, and does not change its position relative to the first holder111.

On the other hand, a receiving depression124for receiving the second processing member102is formed on the center of the upper surface of the second holder121.

The receiving depression124has a circular cross-section. The second processing member102is accepted in the cylindrical receiving depression124so as to be concentric with the receiving depression124.

The structure of the receiving depression124is similar to that in the embodiment as shown inFIG. 1(A)(the first processing member101corresponds to the first ring10, the first holder111to the first holder11, the second processing member102to the second ring20, and the second holder121to the second holder21).

Then, the second holder121is provided with the bias mechanism103. The bias mechanism103preferably uses an elastic body such as spring. The bias mechanism103corresponds to the surface-approaching pressure imparting mechanism4inFIG. 1(A)and has the same structure. That is, the bias mechanism103presses that side (bottom) of the second processing member102which is opposite to the processing surface120and biases each position of the second processing member102uniformly downward to the first processing member101.

On the other hand, the inner diameter of the receiving depression124is made larger than the outer diameter of the second processing member102, so that when arranged concentrically as described above, a gap t1is arranged between outer periphery102bof the second processing member102and inner periphery of the receiving depression124, as shown inFIG. 18(B).

Similarly, a gap t2is arranged between inner periphery102aof the second processing member102and outer periphery of the central part22of the receiving depression124, as shown inFIG. 18(B).

The gaps t1and t2are those for absorbing vibration and eccentric behavior and are set to be in a size to secure operational dimensions or more and to enable sealing. For example, when the diameter of the first processing member101is 100 mm to 400 mm, the gaps t1and t2are preferably 0.05 mm to 0.3 mm, respectively.

The first holder111is fixed integrally with the shaft50and rotated with the shaft50. The second processing member102is not rotated relative to the second holder121by a baffle (not shown). However, for securing 0.1 micron to 10 micron clearance necessary for processing, that is, the minute gap t between the processing surfaces110and120as shown inFIG. 20(B), a gap t3is arranged between the bottom of the receiving depression124, that is, the top part, and the surface facing a top part124aof the second processing member102, that is, the upper part. The gap t3is established in consideration of the clearance and the vibration and elongation of the shaft150.

As described above, by the provision of the gaps t1to t3, the second processing member102can move not only in the direction z1of approaching to and separating from the first processing member101, but also relative to the center and inclination, that is, the direction z2of the processing surface120.

That is, in this embodiment, the bias mechanism103and the gaps t1to t3constitute a floating mechanism, and by this floating mechanism, the center and inclination of at least the second processing member102are made variable in the small range of several μm to several mm. The run-out and expansion of the rotary shaft and the surface vibration and vibration of the first processing member101are absorbed.

The groove112on the processing surface110of the first processing member101is described in more detail. The rear end of the groove112reaches the inner periphery101aof the first processing member101, and its top is elongated toward the outside y of the first processing member101, that is, toward the outer periphery. As shown inFIG. 19(A), the sectional area of the groove112is gradually decreased in the direction from the center x of the circular first processing member101to the outside y of the first processing member101, that is, toward the outer periphery.

The distance w1of the left and right sides112aand112bof the groove112is decreased in the direction from the center x of the first processing member101to the outside y of the first processing member101, that is, toward the outer periphery. As shown inFIG. 19(B), the depth w2of the groove112is decreased in the direction from the center x of the first processing member101to the outside y of the first processing member101, that is, toward the outer periphery. That is, the bottom112cof the groove112is decreased in depth in the direction from the center x of the first processing member101to the outside y of the first processing member101, that is, toward the outer periphery.

As described above, the groove112is gradually decreased both in width and depth toward the outside y, that is, toward the outer periphery, and its sectional area is gradually decreased toward the outside y. Then, the top of the groove112, that is, the y side, is a dead end. That is, the top of the groove112, that is, the y side does not reach the outer periphery101bof the first processing member101, and an outer flat surface113is interposed between the top of the groove112and the outer periphery101b. The outer flat surface113is a part of the processing surface110.

In the embodiment shown inFIG. 19, the left and right sides112aand112band the bottom112cof the groove112constitute a flow path limiting part. This flow path limiting part, the flat part around the groove112of the first processing member101, and the flat part of the second processing member102constitute the dynamical pressure generating mechanism104.

However, only one of the width and depth of the groove112may be constituted as described above to decrease the sectional area.

While the first processing member101rotates, the dynamical pressure generating mechanism104generates a force in the direction of separating the processing members101and102from each other to secure a desired minute space between the processing members101and102by a fluid passing through the space between the processing members101and102. By generation of such dynamical pressure, a 0.1 μm to 10 μm minute space can be generated between the processing surfaces110and120. A minute space like that can be regulated and selected depending on the object of processing, but is preferably 1 μm to 6 μm, more preferably 1 μm to 2 μm. This apparatus can realize a uniform reaction and form microparticles by the minute space, which are not achieved in the prior art.

The grooves112. . .112may extend straight from the center x to the outside y. In this embodiment, however, as shown inFIG. 19(A), the grooves112are curved to extend such that with respect to a rotation direction r of the first processing member101, the center x of the groove112is positioned in front of the outside y of the groove112.

In this manner, the grooves112. . .112are curved to extend so that the separation force by the dynamical pressure generating mechanism104can be effectively generated.

Then, the working of this apparatus is described.

A first processed fluid R which has been introduced from a hopper170and has passed through the first introduction part d1, passes through the hollow part of the circular second processing member102, and the first processed fluid R that has received the centrifugal force resulting from rotation of the first processing member101enters the space between the processing members101and102, and uniform reaction and generation of microparticles are effected and processed between the processing surface110of the rotating first processing member101and the processing surface120of the second processing member102, then exits from the processing members101and102and is then discharged from the discharge part108to the side of the decompression pump Q. Hereinafter, the first processed fluid R is referred to simply as a fluid R, if necessary.

In the foregoing description, the fluid R that has entered the hollow part of the circular second processing member102first enters the groove112of the rotating first processing member101as shown inFIG. 20(A). On the other hand, the processing surfaces110and120that are mirror-polished flat parts are kept airtight even by passing a gas such as air or nitrogen. Accordingly, even if the centrifugal force by rotation is received, the fluid cannot enter through the groove112into the space between the processing surfaces110and120that are pushed against each other by the bias mechanism103. However, the fluid R gradually runs against both the sides112aand112band the bottom112cof the groove112formed as a flow path limiting part to generate dynamical pressure acting in the direction of separating the processing surfaces110and120from each other. As shown inFIG. 20(B), the fluid R can thereby exude from the groove112to the flat surface, to secure a minute gap t, that is, clearance, between the processing surfaces110and120. Then, a uniform reaction and generation of microparticles are effected and processed between the mirror-polished flat surfaces. The groove112has been curved so that the centrifugal force is applied more accurately to the fluid to make generation of dynamical pressure more effectively.

In this manner, the processing apparatus can secure a minute and uniform gap, that is, clearance, between the mirror surfaces, that is, the processing surfaces110and120, by the balance between the dynamical pressure and the bias force by the bias mechanism103. By the structure described above, the minute gap can be as superfine as 1 μm or less.

By utilizing the floating mechanism, the automatic regulation of alignment between the processing surfaces110and120becomes possible, and the clearance in each position between the processing surfaces110and120can be prevented from varying against physical deformation of each part by rotation or generated heat, and the minute gap in each position can be maintained.

In the embodiment described above, the floating mechanism is a mechanism arranged for the second holder121only. Alternatively, the floating mechanism can be arranged in the first holder111instead of, or together with, the second holder121.

Other embodiments of the groove112are shown inFIG. 21toFIG. 23.

As shown inFIG. 21(A)andFIG. 21(B), the groove112can be provided at the top with a flat wall surface112das a part of the flow path limiting part. In this embodiment, a step112eis arranged between the first wall surface112dand the inner periphery101ain the bottom112c, and the step112ealso constitutes a part of the flow path limiting part.

As shown inFIG. 22(A)andFIG. 22(B), the groove112includes a plurality of branches112f. . .112f, and each branch112fnarrows its width there by being provided with a flow path limiting part.

With respect to the embodiments as well, structures other than those particularly shown are similar to those of embodiments as shown inFIG. 1(A),FIG. 11(C), andFIG. 18toFIG. 20.

In the embodiments described above, at least either the width or depth of the groove112is gradually decreased in size in the direction from inside to outside the first processing member101, thereby constituting a flow path limiting part. Alternatively, as shown inFIG. 23(A)orFIG. 23(B), the groove112can be provided with a termination surface112fwithout changing the width and depth of the groove112, and the termination surface112fof the groove112can serve as a flow path limiting part. As shown the embodiments inFIG. 19,FIG. 21andFIG. 22, the width and depth of the groove112can be changed as described above thereby slanting the bottom and both sides of the groove112, so that the slanted surfaces serves as a pressure-receiving part toward the fluid to generate dynamical pressure. In the embodiment shown inFIG. 23(A)andFIG. 23(B), on the other hand, the termination surface of the groove112serves as a pressure-receiving part toward the fluid to generate dynamical pressure.

In the embodiment shown inFIG. 23(A)andFIG. 23(B), at least one of the width and depth of the groove112may also be gradually decreased in size.

The structure of the groove112is not limited to the one shown inFIG. 19andFIG. 21toFIG. 23and can be provided with a flow path limiting part having other shapes.

For example, in the embodiments shown inFIG. 19andFIG. 21toFIG. 23, the groove112does not penetrate to the outer side of the first processing member101. That is, there is an outer flat surface113between the outer periphery of the first processing member101and the groove112. However, the structure of the groove112is not limited to such embodiment, and the groove112may reach the outer periphery of the first processing member101as long as the dynamical pressure can be generated.

For example, in the case of the first processing member101shown inFIG. 23(B), as shown in the dotted line, a part having a smaller sectional area than other sites of the groove112can be formed on the outer flat surface113.

The groove112may be formed so as to be gradually decreased in size in the direction from inside to outside as described above, and the part (terminal) of the groove112that had reached the outer periphery of the first processing member101may have the minimum sectional area (not shown). However, the groove112preferably does not penetrate to the outer periphery of the first processing member101as shown inFIG. 19andFIG. 21toFIG. 23, in order to effectively generate dynamical pressure.

This processing apparatus is a processing apparatus wherein a rotating member having a flat processing surface and a fixed member having a flat processing surface are opposite to each other so as to be concentric with each other, and while the rotating member is rotated, a material to be reacted is fed through an opening of the fixed member and subjected to a reaction between the opposite flat processing surfaces of both members, wherein the rotating member is provided with a pressurizing mechanism by which pressure is generated to maintain clearance without mechanically regulating clearance and enables 1 μm to 6 μm microscopic clearance not attainable by mechanical regulation of clearance, thereby significantly improving an ability to pulverize formed particles and an ability to uniformize the reaction.

That is, this processing apparatus have a rotating member and a fixed member each having a flat processing surface in the outer periphery thereof and has a sealing mechanism in a plane on the flat processing surface, thereby providing a high speed rotation processing apparatus generating hydrostatic force, hydrodynamic force, or aerostatic-aerodynamic force. The force generates a minute space between the sealed surfaces, and provides a reaction processing apparatus with a function of non-contact and mechanically safe and high-level pulvelization and uniformizing of reactions. One factor for forming this minute space is due to the rotation speed of the rotating member, and the other factor is due to a pressure difference between the introduction side and discharge side of a processed material (fluid). When a pressure imparting mechanism is arranged in the introduction side, when a pressure imparting mechanism is not arranged in the introduction side, that is, when the processed material (fluid) is introduced at atmospheric pressure, there is no pressure difference, and thus the sealed surfaces should be separated by only the rotation speed of the rotating member. This is known as hydrodynamic or aerodynamic force.

FIG. 18(A)shows the apparatus wherein a decompression pump Q is connected to the discharge part of the reaction apparatus G, but as described above, the reaction apparatus G may be arranged in a decompression tank T without arranging the housing106and the decomposition pump Q, as shown inFIG. 24(A).

In this case, the tank T is decompressed in a vacuum or in an almost vacuum, whereby the processed product formed in the reaction apparatus G is sprayed in a mist form in the tank T, and the processed material colliding with, and running down along, the inner wall of the tank T can be recovered, or a gas (vapor) separated from the processed material and filled in an upper part of the tank T, unlike the processed material running down along the wall, can be recovered to obtain the objective product after processing.

When the decompression pump Q is used, an airtight tank T is connected via the decompression pump Q to the processing apparatus G, whereby the processed material after processing can be formed into mist to separate and extract the objective product.

As shown inFIG. 24(C), the decompression pump Q is connected directly to the Tank T, and the decompression pump Q and a discharge part for fluid R, different from the decompression pump Q, are connected to the tank T, whereby the objective product can be separated. In this case, a gasified portion is sucked by the decompression pump Q, while the fluid R (liquid portion) is discharged from the discharge part separately from the gasified portion.

In the embodiments described above, the first and second processed fluids are introduced via the second holders21and121and the second rings20and102respectively and mixed and reacted with each other.

Now, other embodiments with respect to introduction of fluids to be processed into the apparatus are described.

As shown inFIG. 1(B), the processing apparatus shown inFIG. 1(A)is provided with a third introduction part d3to introduce a third fluid to be processed into the space between the processing surfaces1and2, and the third fluid is mixed and reacted with the first processed fluid as well as the second processed fluid.

By the third introduction part d3, the third fluid to be mixed with the first processed fluid is fed to the space between the processing surfaces1and2. In this embodiment, the third introduction part d3is a fluid flow path arranged in the second ring20and is open at one end to the second processing surface2and has a third fluid feed part p3connected to the other end.

In the third fluid feed part p3, a compressor or another pump can be used.

The opening of the third introduction part d3in the second processing surface2is positioned outside, and more far from, the rotation center of the first processing surface1than the opening of the second introduction part d2. That is, in the second processing surface2, the opening of the third introduction part d3is located downstream from the opening of the second introduction part d2. A gap is arranged between the opening of the third introduction d3and the opening of the second introduction part d2in the radial direction of the second ring20.

With respect to structures other than the third introduction d3, the apparatus shown inFIG. 1(B)is similar to that in the embodiment as inFIG. 1(A). InFIG. 1(B)and further inFIG. 1(C),FIG. 1(D)andFIG. 2toFIG. 11described later, the case3is omitted to simplify the drawings. InFIG. 9(B),FIG. 9(C),FIG. 10,FIG. 11(A)andFIG. 11(B), a part of the case3is shown.

As shown inFIG. 1(C), the processing apparatus shown inFIG. 1(B)is provided with a fourth introduction part d4to introduce a fourth fluid to be processed into the space between the processing surfaces1and2, and the fourth fluid is mixed and reacted with the first processed fluid as well as the second and third processed fluids.

By the fourth introduction part d4, the fourth fluid to be mixed with the first processed fluid is fed to the space between the processing surfaces1and2. In this embodiment, the fourth introduction part d4is a fluid flow path arranged in the second ring20, is open at one end to the second processing surface2, and has a fourth fluid feed part p4connected to the other end.

In the fourth fluid feed part p4, a compressor or another pump can be used.

The opening of the fourth introduction part d4in the second processing surface2is positioned outside, and more far from, the rotation center of the first processing surface1than the opening of the third introduction part d3. That is, in the second processing surface2, the opening of the fourth introduction part d4is located downstream from the opening of the third introduction part d3.

With respect to structures other than the fourth introduction part d4, the apparatus shown inFIG. 1(C)is similar to that in the embodiment as inFIG. 1(B).

Five or more introduction parts further including a fifth introduction part, a sixth introduction part and the like can be arranged to mix and react five or more fluids to be processed with one another (not shown).

As shown inFIG. 1(D), the first introduction part d1arranged in the second holder21in the apparatus inFIG. 1(A)can, similar to the second introduction part d2, be arranged in the second processing surface2in place of the second holder21. In this case, the opening of the first introduction part d1is located at the upstream side from the second introduction part d2, that is, it is positioned nearer to the rotation center than the second introduction part d2in the second processing surface2.

In the apparatus shown inFIG. 1(D), the opening of the second introduction part d2and the opening of the third introduction part d3both are arranged in the second processing surface2of the second ring20. However, arrangement of the opening of the introduction part is not limited to such arrangement relative to the processing surface. Particularly as shown inFIG. 2(A), the opening of the second introduction part d2can be arranged in a position adjacent to the second processing surface2in the inner periphery of the second ring20. In the apparatus shown inFIG. 2(A), the opening of the third introduction part d3is arranged in the second processing surface2similarly to the apparatus shown inFIG. 1(B), but the opening of the second introduction part d2can be arranged inside the second processing surface2and adjacent to the second processing surface2, whereby the second processed fluid can be immediately introduced onto the processing surfaces.

In this manner, the opening of the first introduction part d1is arranged in the second holder21, and the opening of the second introduction part d2is arranged inside the second processing surface2and adjacent to the second processing surface2(in this case, arrangement of the third introduction part d3is not essential), so that particularly in reaction of a plurality of fluids, the fluid introduced from the first introduction part d1and the fluid introduced from the second introduction part d2are introduced, without being reacted with each other, into the space between the processing surfaces1and2, and then both the fluids can be reacted first between the processing surfaces1and2. Accordingly, the structure described above is suitable for obtaining a particularly reactive fluid.

The term “adjacent” is not limited to the arrangement where the opening of the second introduction part d2is contacted with the inner side of the second ring20as shown inFIG. 2(A). The distance between the second ring20and the opening of the second introduction part d2may be such a degree that a plurality of fluids are not completely mixed and reacted with one another prior to introduction into the space between the processing surfaces1and2. For example, the opening of the second introduction part d2may be arranged in a position near the second ring20of the second holder21. Alternatively, the opening of the second introduction part d2may be arranged on the side of the first ring10or the first holder11.

In the apparatus shown inFIG. 1(B), a gap is arranged between the opening of the third introduction part d3and the opening of the second introduction part d2in the radial direction of the second ring20, but as shown inFIG. 2(B), the second and third fluids can be introduced into the space between the processing surfaces1and2, without providing such gap, thereby immediately joining both the fluids together. The apparatus shown inFIG. 2(B)can be selected depending on the object of processing.

In the apparatus shown inFIG. 1(D), a gap is also arranged between the opening of the first introduction part d1and the opening of the second introduction part d2in the radial direction of the second ring20, but the first and second fluids can be introduced into the space between the processing surfaces1and2, without providing such gap, thereby immediately joining both the fluids together. Such arrangement of the opening can be selected depending on the object of processing.

In the embodiment shown inFIG. 1(B)andFIG. 1(C), the opening of the third introduction part d3is arranged in the second processing surface2downstream from the opening of the second introduction part d2, in other words, outside the opening of the second introduction part d2in the radial direction of the second ring20. Alternatively, as shown inFIG. 2(C)andFIG. 3(A), the opening of the third introduction part d3and the opening of the second introduction part d2can be arranged in the second processing surface2in positions different in a circumferential direction r0of the second ring20. InFIG. 3, numeral m1is the opening (first opening) of the first introduction part d1, numeral m2is the opening (second opening) of the second introduction part d2, numeral m3is the opening (third opening) of the third introduction part d3, and numeral r1is the radical direction of the ring.

When the first introduction part d1is arranged in the second ring20, as shown inFIG. 2(D), the opening of the first introduction part d1and the opening of the second introduction part d2can be arranged in the second processing surface2in positions different in the circumferential direction of the second ring20.

In the apparatus shown inFIG. 2(C), the openings of two introduction parts are arranged in the second processing surface2of the second ring20in positions different in the circumferential direction r0, but as shown inFIG. 3(B), the openings of three introduction parts can be arranged in positions different in the circumferential direction r0of the ring, or as shown inFIG. 3(C), the openings of four introduction parts can be arranged in positions different in the circumferential direction r0of the ring. InFIG. 3(B)andFIG. 3(C), numeral m4is the opening of the fourth introduction part, and inFIG. 3(C), numeral m5is the opening of the fifth introduction part. Five or more openings of introduction parts may be arranged in positions different in the circumferential direction r0of the ring (not shown).

In the apparatuses shown inFIG. 2(B),FIG. 2(D)and inFIG. 3(A)toFIG. 3(C), the second to fifth introduction parts can introduce different fluids, that is, the second, third, fourth and fifth fluids. On the other hand, the second to fifth openings m2to m5can introduce the same fluid, that is, the second fluid into the space between the processing surfaces. In this case, the second to fifth introduction parts are connected to the inside of the ring and can be connected to one fluid feed part, that is, the second fluid feed part p2(not shown).

A plurality of openings of introduction parts arranged in positions different in the circumferential direction r0of the ring can be combined with a plurality of openings of introduction parts arranged in positions different in the radial direction r1of the ring.

For example, as shown inFIG. 3(D), the openings m2to m9of eight introduction parts are arranged in the second processing surface2, wherein four openings m2to m5of them are arranged in positions different in the circumferential direction r0of the ring and identical in the radial direction r1of the ring, and the other four openings m6to m9are arranged in positions different in the circumferential direction r0of the ring and identical in the radial direction r1of the ring. Then, the other openings m6to m9are arranged outside the radial direction r1of the four openings m2to m5. The outside openings and inside openings may be arranged in positions identical in the circumferential direction r0of the ring, but in consideration of rotation of the ring, may be arranged in positions different in the circumferential direction r0of the ring as shown inFIG. 3(D). In this case too, the openings are not limited to arrangement and number shown inFIG. 3(D).

For example, as shown inFIG. 3(E), the outside opening in the radial direction can be arranged in the apex of a polygon, that is, in the apex of a rectangle in this case, and the inside opening in the radial direction can be positioned on one side of the rectangle. As a matter of course, other arrangements can also be used.

When the openings other than the first opening m1feed the second fluid into the space between the processing surfaces, each of the openings may be arranged as continuous openings in the circumferential direction r0as shown inFIG. 3(F), instead of being arranged discretely in the circumferential direction r0of the processing surface.

As shown inFIG. 4(A), depending on the object of processing, the second introduction part d2arranged in the second ring20in the apparatus shown inFIG. 1(A)can be, similar to the first introduction part d1, arranged in the central portion22of the second holder21. In this case, the opening of the second introduction part d2is positioned with a gap outside the opening of the first introduction part d1positioned in the center of the second ring20. As shown inFIG. 4(B), in the apparatus shown inFIG. 4(A), the third introduction part d3can be arranged in the second ring20. As shown inFIG. 4(C), in the apparatus shown inFIG. 4(A), the first and second fluids can be introduced into the space inside the second ring20without arranging a gap between the opening of the first introduction part d1and the opening of the second introduction part d2, so that both the fluids can immediately join together. As shown inFIG. 4(D), depending on the object of processing, in the apparatus shown inFIG. 4(A), the third introduction part d3can be, similar to the second introduction part d2, arranged in the second holder21. Four or more introduction parts may be arranged in the second holder21(not shown).

As shown inFIG. 5(A), depending on the object of processing, in the apparatus shown inFIG. 4(D), the fourth introduction part d4can be arranged in the second ring20, so that the fourth fluid may be introduced into the space between the processing surfaces1and2.

As shown inFIG. 5(B), in the apparatus shown inFIG. 1(A), the second introduction part d2can be arranged in the first ring10, and the opening of the second introduction part d2can be arranged in the first processing surface1.

As shown inFIG. 5(C), in the apparatus shown inFIG. 5(B), the third introduction part d3can be arranged in the first ring10, and the opening of the third introduction part d3and the opening of the second introduction part d2can be arranged in the first processing surface1in positions different in the circumferential direction of the first ring10.

As shown inFIG. 5(D), in the apparatus shown inFIG. 5(B), the first introduction part d1can be arranged in the second ring20instead of arranging the first introduction part d1in the second holder21, and the opening of the first introduction part d1can be arranged in the second processing surface2. In this case, the openings of the first and second introduction parts d1and d2are arranged in positions identical in the radial direction of the ring.

As shown inFIG. 6(A), in the apparatus shown inFIG. 1(A), the third introduction part d3can be arranged in the first ring10, and the opening of the third introduction part d3can be arranged in the first processing surface1. In this case, both the openings of the second and third introduction parts d2and d3are arranged in positions identical in the radial direction of the ring. However, both the openings may be arranged in positions different in the radial direction of the ring.

In the apparatus shown inFIG. 5(C), the openings of the second and third introduction parts d2and d3are arranged in positions identical in the radial direction of the first ring10and simultaneously arranged in positions different in the circumferential direction (that is, rotation direction) of the first ring10, but in this apparatus, as shown inFIG. 6(B), both the openings of the second and third introduction parts d2and d3can be arranged in positions different in the radical direction of the first ring10. In this case, as shown inFIG. 6(B), a gap can be arranged between both the openings of the second and third introduction parts d2and d3in the radial direction of the first ring10, or without arranging the gap, the second and third fluids may immediately join together (not shown).

As shown inFIG. 6(C), the first introduction part d1together with the second introduction part d2can be arranged in the first ring10instead of arranging the first introduction part d1in the second holder21. In this case, in the first processing surface1, the opening of the first introduction part d1is arranged upstream (inside the radial direction of the first ring10) from the opening of the second introduction part d2. A gap is arranged between the opening of the first introduction part d1and the opening of the second introduction part d2in the radial direction of the first ring10. Alternatively, such gap may not be arranged (not shown).

As shown inFIG. 6(D), both the openings of the first introduction part d1and the second introduction part d2can be arranged in positions different in the circumferential direction of the first ring10in the first processing surface1in the apparatus shown inFIG. 6(C).

In the embodiment shown inFIG. 6(C)andFIG. 6(D), three or more introduction parts may be arranged in the first ring10, and in the second processing surface2, so the respective openings may be arranged in positions different in the circumferential direction or in positions different in the radial direction of the ring (not shown). For example, the arrangement of openings in the second processing surface2, shown inFIG. 3(B)toFIG. 3(F), can also be used in the first processing surface1.

As shown inFIG. 7(A), in the apparatus shown inFIG. 1(A), the second introduction part d2can be arranged in the first holder11instead of arranging the part d2in the second ring20. In this case, the opening of the second introduction part d2is arranged preferably in the center of the central shaft of rotation of the first ring10, in the site surrounded with the first ring10on the upper surface of the first holder11.

As shown inFIG. 7(B), in the embodiment shown inFIG. 7(A), the third introduction part d3can be arranged in the second ring20, and the opening of the third introduction part d3can be arranged in the second processing surface2.

As shown inFIG. 7(C), the first introduction part d1can be arranged in the first holder11instead of arranging the part d1in the second holder21. In this case, the opening of the first introduction part d1is arranged preferably in the central shaft of rotation of the first ring10, in the site surrounded with the first ring10on the upper surface of the first holder11. In this case, as shown in the figure, the second introduction part d2can be arranged in the first ring10, and its opening can be arranged in the first processing surface1. In this case, the second introduction part d2can be arranged in the second ring20, and its opening can be arranged in the second processing surface2(not shown).

As shown inFIG. 7(D), the second introduction part d2shown inFIG. 7(C)together with the first introduction part d1can be arranged in the first holder11. In this case, the opening of the second introduction part d2is arranged in the site surrounded with the first ring10on the upper surface of the first holder11. In this case, the second introduction part d2arranged in the second ring20may serve as the third introduction part d3inFIG. 7(C).

In the embodiments shown inFIG. 1toFIG. 7, the first holder11and the first ring10are rotated relative to the second holder21and the second ring20, respectively. As shown inFIG. 8(A), in the apparatus shown inFIG. 1(A), the second holder21may be provided with a rotary shaft51rotating with the turning force from the rotation drive member, to rotate the second holder21in a direction opposite to the first holder11. The rotation drive member may be arranged separately from the one for rotating the rotary shaft50of the first holder11or may receive power from the drive part for rotating the rotary shaft50of the first holder11by a power transmission means such as a gear. In this case, the second holder21is formed separately from the case, and shall, like the first holder11, be rotatably accepted in the case.

As shown inFIG. 8(B), in the apparatus shown inFIG. 8(A), the second introduction part d2can be, similarly in the apparatus inFIG. 7(B), arranged in the first holder11in place of the second ring20.

In the apparatus shown inFIG. 8(B), the second introduction part d2can be arranged in the second holder21in place of the first holder11(not shown). In this case, the second introduction part d2is the same as one in the apparatus inFIG. 4(A). As shown inFIG. 8(C), in the apparatus shown inFIG. 8(B), the third introduction part d3can be arranged in the second ring20, and the opening of the third introduction part d3can be arranged in the second processing surface2.

As shown inFIG. 8(D), the second holder21only can be rotated without rotating the first holder11. Even in the apparatuses shown inFIG. 1(B)toFIG. 7, the second holder21together with the first holder11, or the second holder21alone, can be rotated (not shown).

As shown inFIG. 9(A), the second processing member20is a ring, while the first processing member10is not a ring and can be a rotating member provided directly with a rotary shaft50similar to that of the first holder11in other embodiments. In this case, the upper surface of the first processing member10serves as the first processing surface1, and the processing surface is an evenly flat surface which is not circular (that is, hollow-free). In the apparatus shown inFIG. 9(A), similarly in the apparatus inFIG. 1(A), the second introduction part d2is arranged in the second ring20, and its opening is arranged in the second processing surface2.

As shown inFIG. 9(B), in the apparatus shown inFIG. 9(A), the second holder21provided with the second ring20is independent of the case3, and a surface-approaching pressure imparting mechanism4such as an elastic body for approaching to and separating from the first processing member10can be provided between the case3and the second holder21. In this case, as shown inFIG. 9(C), the second processing member20is not a ring, but is a member corresponding to the second holder21, and the lower surface of the member can serve as the second processing surface2. As shown inFIG. 10(A), in the apparatus shown inFIG. 9(C), the first processing member10is not a ring either, and in other embodiments similarly in the apparatus shown inFIG. 9(A)andFIG. 9(B), the site corresponding to the first holder11can serve as the first processing member10, and its upper surface can serve as the first processing surface1.

In the embodiments described above, at least the first fluid is supplied from the first processing member10and the second processing member20, that is, from the central part of the first ring10and the second ring20, and after processing (mixing and reaction) of the other fluids, the processed fluid is discharged to the outside in the radial direction. Alternatively, as shown inFIG. 10(B), the first fluid can be supplied in the direction from the outside to the inside of the first ring10and second ring20. In this case, the outside of the first holder11and the second holder21is sealed with the case3, the first introduction part d1is arranged directly in the case3, and the opening of the introduction part is arranged in a site inside the case and corresponding to the abutting position of the rings10and20, as shown in the figure. In the apparatus inFIG. 1(A), a discharge part36is arranged in the position in which the first introduction part d1is arranged, that is, in the central position of the ring1of the first holder11. The opening of the second introduction part d2is arranged in the opposite side of the opening of the case behind the central shaft of rotation of the holder. However, the opening of the second introduction part d2may be, similar to the opening of the first introduction part d1, arranged in a site inside the case and corresponding to the abutting position of the rings10and20. As described above, the embodiment is not limited to the one where the opening of the second introduction part d2is formed to the opposite side of the opening of the first introduction part d1.

In this case, the outside of the diameter of both rings10and20is on the upstream side, and the inside of both the rings10and20is on the downstream side.

As such, as shown inFIG. 16(E), when the processed fluid moves from outside to inside, the first processing surface1of the first processing member10may also be provided with groove-like depressions13. . .13extending in the direction from outside to inside of the first processing member10. When the groove-like depressions13. . .13are formed, the balance ratio K described above is preferably set as 100% or more of unbalance type. As a result, dynamical pressure is generated in the groove-like depressions13. . .13upon rotating, the first and second processing surfaces1and2can rotate in a surely non-contact state, so that the risk of abrasion and the like due to contact can be eliminated. In the embodiment shown inFIG. 16(E), the separating force due to the pressure of the processed fluid is generated in an inner end13aof the depressions13.

As shown inFIG. 10(C), in the apparatus shown inFIG. 10(B), the second introduction part d2, which is arranged in the side of the case3, can be arranged in the first ring10in space of the mentioned position, and its opening can be arranged in the first processing surface1. In this case, as shown inFIG. 10(D), the first processing member10is not formed as a ring. Similarly in the apparatuses shown inFIG. 9(A),FIG. 9(B), andFIG. 10(A), in other embodiments, the site corresponding to the first holder11is the first processing member10, its upper surface being the first processing surface1, the second introduction part d2being arranged in the first processing member10, and its opening may be arranged in the first processing surface1.

As shown inFIG. 11(A), in the apparatus shown inFIG. 10(D), the second processing member20is not formed as a ring, and in other embodiments, the member corresponding to the second holder21serves as the second processing member20, and its lower surface serves as the second processing surface2. Then, the second processing member20is a member independent of the case3, and the same surface-approaching pressure imparting mechanism4as one in the apparatuses shown inFIG. 9(B),FIG. 9(C), andFIG. 10(A)can be arranged between the case3and the second processing member20.

As shown inFIG. 11(B), the second introduction part d2in the apparatus shown inFIG. 11(A)serves as the third introduction part d3, and separately the second introduction part d2can be arranged. In this case, the opening of the second introduction part d2is arranged downstream from the opening of the third introduction part d3in the second processing surface2.

In the apparatuses shown inFIG. 4and the apparatuses shown inFIG. 5(A),FIG. 7(A),FIG. 7(B),FIG. 7(D),FIG. 8(B)andFIG. 8(C), other fluids to be processed flow into the first fluid before reaching the processing surfaces1and2, and these apparatuses are not suitable for the fluid which is rapidly crystallized or separated. However, these apparatuses can be used for the fluid having a low reaction speed.

The processing apparatus suitable for carrying out the method according to the present invention is summarized as follows.

As described above, the processing apparatus comprises a fluid pressure imparting mechanism that imparts predetermined pressure to a fluid to be processed, at least two processing members, that is, a first processing member10arranged in a sealed fluid flow path through which the fluid at the predetermined pressure flows and a second processing member20capable of approaching to and separating from the first processing member10, at least two processing surfaces of a first processing surface1and a second processing surface2arranged in a position in which they are faced with each other in the processing members10and20, and a rotation drive mechanism that relatively rotates the first processing member10and the second processing member20, wherein at least two fluids to be processed are mixed and reacted between the processing surfaces1and2. Of the first processing member10and the second processing member20, at least the second processing member20has a pressure-receiving surface, at least a part of the pressure-receiving surface is comprised of the second processing surface2, and the pressure-receiving surface receives pressure applied by the fluid pressure imparting mechanism to at least one of the fluids to generate a force to move in the direction of separating the second processing surface2from the first processing surface1. In this apparatus, the fluid that has received said pressure passes through the space between the first processing surface1and the second processing surface2capable of approaching to and separating from each other, thereby generating a desired reaction between the processed fluids with the fluids being passed between the processing surfaces1and2and forming a thin film fluid of predetermined thickness.

In this processing apparatus, at least one of the first processing surface1and the second processing surface2is preferably provided with a buffer mechanism for regulation of micro-vibration and alignment.

In this processing apparatus, one of or both the first processing surface1and the second processing surface2is preferably provided with a displacement regulating mechanism capable of regulating the displacement in the axial direction caused by abrasion or the like thereby maintaining the thickness of a thin film fluid between the processing surfaces1and2.

In this processing apparatus, a pressure device such as a compressor for applying predetermined feeding pressure to a fluid can be used as the fluid pressure imparting mechanism.

As the pressure device, a device capable of regulating an increase and decrease in feeding pressure is used. This is because the pressure device should be able to keep established pressure constant and should be able to regulate an increase and decrease in feeding pressure as a parameter to regulate the distance between the processing surfaces.

The processing apparatus can be provided with a separation preventing part for defining the maximum distance between the first processing surface1and the second processing surface2and preventing the processing surfaces1and2from separating from each other by the maximum distance or more.

The processing apparatus can be provided with an approach preventing part for defining the minimum distance between the first processing surface1and the second processing surface2and preventing the processing surfaces1and2from approaching to each other by the minimum distance or less.

The processing apparatus can be one wherein both the first processing surface1and the second processing surface2are rotated in opposite directions.

The processing apparatus can be provided with a temperature-regulating jacket for regulating the temperature of either or both of the first processing surface1and the second processing surface2.

The processing apparatus is preferably one wherein at least a part of either or both of the first processing surface1and the second processing surface2is mirror-polished.

The processing apparatus can be one wherein one of or both the first processing surface1and the second processing surface2is provided with depressions.

The processing apparatus preferably includes, as a means for feeding one fluid to be reacted with another fluid, a separate introduction path independent of a path for another fluid, at least one of the first processing surface and the second processing surface is provided with an opening leading to the separate introduction path, and another fluid sent through the separate introduction path is introduced into the one fluid.

The processing apparatus for carrying out the present invention comprises a fluid pressure imparting mechanism that imparts predetermined pressure to a fluid to be processed, at least two processing surfaces of a first processing surface1and a second processing surface2capable of approaching to and separating from each other which are connected to a sealed fluid flow path through which the fluid at the predetermined pressure is passed, a surface-approaching pressure imparting mechanism that imparts surface-approaching pressure to the space between the processing surfaces1and2, and a rotation drive mechanism that relatively rotates the first processing surface1and the second processing surface2, wherein at least two fluids to be processed are reacted between the processing surfaces1and2, at least one fluid pressurized with the fluid pressure imparting mechanism is passed through the space between the first processing surface1and the second processing surface2rotating to each other and supplied with surface-approaching pressure, and another fluid is passed, so that the fluid pressurized with the fluid pressure imparting mechanism, while being passed between the processing surfaces and forming a thin film fluid of predetermined thickness, is mixed with another fluid, whereby a desired reaction is caused between the fluids.

The surface-approaching pressure imparting mechanism can constitute a buffer mechanism of regulating micro-vibration and alignment and a displacement regulation mechanism in the apparatus described above.

The processing apparatus for carrying out the present invention comprises a first introduction part that introduces, into the apparatus, at least one of two fluids to be reacted, a fluid pressure imparting mechanism p that is connected to the first introduction part and imparts pressure to a fluid to be processed, a second introduction part that introduces at least the other fluid of the two fluids to be reacted, at least two processing members, that is, a first processing member10arranged in a sealed fluid flow path through which the other fluid is passed and a second processing member20capable of relatively approaching to and separating from the first processing member10, at least two processing surfaces, that is, a first processing surface1and a second processing surface2arranged so as to be opposite to each other in the processing members10and20, a holder21that accepts the second processing member20so as to expose the second processing surface2, a rotation drive mechanism that relatively rotates the first processing member10and the second processing member20, and a surface-approaching pressure imparting mechanism4that presses the second processing member20against the first processing surface1such that the second processing surface2is contacted against or made close to the first processing surface1, wherein the fluids to be processed are reacted between the processing surfaces1and2, the holder21is provided with an opening of the first introduction part and is not movable so as to influence the space between the processing surfaces1and2, at least one of the first processing member10and the second introduction part20is provided with an opening of the second introduction part, the second processing member20is circular, the second processing surface2slides along the holder21and approaches to and separates from the first processing surface1, the second processing member20includes a pressure-receiving surface, the pressure-receiving surface receives pressure applied by the fluid pressure imparting mechanism p1to the fluid to generate a force to move in the direction of separating the second processing surface2from the first processing surface1, at least a part of the pressure-receiving surface is comprised of the second processing surface2, one of the fluids to which pressure was applied is passed through the space between the first processing surface1and the second processing surface2rotating to each other and capable of approaching to and separating from each other, and the other fluid is supplied to the space between the processing surfaces1and2, whereby both the fluids form a thin film fluid of predetermined thickness and pass through the space between both the processing surfaces1and2, the passing fluids are mixed thereby promoting a desired reaction between the processed fluids, and the minimum distance for generating the thin film fluid of predetermined thickness is kept between the processing surfaces1and2by the balance between the surface-approaching pressure by the surface-approaching pressure imparting mechanism4and the force of separating the processing surfaces1and2from each other by the fluid pressure imparted by the fluid pressure imparting mechanism p1.

In this processing apparatus, the second introduction part can be, similarly being connected to the first introduction part, arranged to be connected to a separate fluid pressure imparting mechanism and to be pressurized. The fluid introduced from the second introduction part is not pressurized by the separate fluid pressure imparting mechanism, but is sucked and supplied into the space between the processing surfaces1and2by negative pressure generated in the second introduction part by the fluid pressure of the fluid introduced into the first introduction part. Alternatively, the other fluid flows downward by its weight in the second introduction part and can be supplied into the space between the processing surfaces1and2.

As described above, the apparatus is not limited to the one wherein the opening of the first introduction part as an inlet for feeding the other fluid to be processed into the apparatus is arranged in the second holder, and the opening of the first introduction part may be arranged in the first holder. The opening of the first introduction part may be formed with at least one of the processing surfaces. However, when the fluid to be previously introduced into the space between the processing surfaces1and2should, depending on the reaction, be supplied from the first introduction part, the opening of the second introduction part as an inlet for feeding the other fluid into the apparatus should be arranged downstream from the opening of the first introduction part in any of the processing surfaces.

As the processing apparatus for carrying out the present invention, the following apparatus can be used.

This processing apparatus comprises a plurality of introduction parts that separately introduce two or more fluids to be reacted, a fluid pressure imparting mechanism p that imparts pressure to at least one of the two or more fluids, at least two processing members, that is, a first processing member10arranged in a sealed fluid flow path through which the processed fluid is passed and a second processing member20capable of approaching to and separating from the first processing member10, at least two processing surfaces1and2, that is, a first processing surface1and a second processing surface2arranged in a position in which they are faced with each other in the processing members10and20, and a rotation drive mechanism that relatively rotates the first processing member10and the second processing member20, wherein the fluids are reacted between the processing surfaces1and2, at least the second processing member20of the first processing member10and the second processing member20includes a pressure-receiving surface, at least a part of the pressure-receiving surface is comprised of the second processing surface2, the pressure-receiving surface receives pressure applied by the fluid pressure imparting mechanism to the fluid to generate a force to move in the direction of separating the second processing surface2from the first processing surface1, the second processing member20includes an approach regulating surface24that is directed to the opposite side of the second processing surface2, the approach regulating surface24receives predetermined pressure applied to the fluid to generate a force to move in the direction of approaching the second processing surface2to the first processing surface1, a force to move in the direction of separating the second processing surface2from the first processing surface1as a resultant force of total pressure received from the fluid is determined by the area ratio of the projected area of the approach regulating surface24in the approaching and separating direction to the projected area of the pressure-receiving surface in the approaching and separating direction, the fluid to which pressure was applied is passed through the space between the first processing surface1and the second processing surface2that rotate relative to each other and capable of approaching to and separating from each other, the other fluid to be reacted with the one fluid is mixed in the space between the processing surfaces, and the mixed fluid forms a thin film fluid of predetermined thickness and simultaneously passes through the space between the processing surfaces1and2, thereby giving a desired reaction product while passing through the space between the processing surfaces.

The processing method according to the present invention is summarized as follows. The processing method comprises applying predetermined pressure to a first fluid, connecting at least two processing surfaces, that is, a first processing surface1and a second processing surface2, which are capable of approaching to and separating from each other, to a sealed fluid flow path through which the fluid that has received the predetermined pressure is passed, applying a surface-approaching pressure of approaching the first processing surface1and the second processing surface2each other, rotating the first processing surface1and the second processing surface2relative to each other, and introducing the fluid into the space between the processing surfaces1and2, wherein the second fluid to be reacted with the first fluid is introduced through a separate flow path into the space between the processing surfaces1and2thereby reacting both the fluids, the predetermined pressure applied to at least the first fluid functions as a separating force for separating the processing surfaces1and2from each other, and the separating force and the surface-approaching pressure are balanced via the fluid between the processing surfaces1and2, whereby the distance between the processing surfaces1and2is kept in a predetermined minute space, the fluid is passed as a thin film fluid of predetermined thickness through the space between the processing surfaces1and2, and when both the fluids are uniformly reacted with each other while passing and accompanied by separation, a desired reaction product is crystallized or separated.

Hereinafter, other embodiments of the present invention are described in detail.FIG. 25is a schematic sectional view of a reaction apparatus wherein reactants are reacted between processing surfaces, at least one of which rotates relative to the other, and which are capable of approaching to and separating from each other.FIG. 26(A)is a schematic plane view of the first processing surface in the apparatus shown inFIG. 25, andFIG. 26(B)is an enlarged view of an important part of the processing surface in the apparatus shown inFIG. 25.FIG. 27(A)is a sectional view of the second introduction path, andFIG. 27(B)is an enlarged view of an important part for explaining the second introduction path.

InFIG. 25, arrows U and S show upward and downward directions respectively.

InFIG. 26(A)andFIG. 27(B), arrow R shows the direction of rotation.

InFIG. 27(B), arrow C shows the direction of centrifugal force (radial direction).

This apparatus uses at least two fluids as a fluid to be processed that is described above, at least one of which contains at least one kind of reactant, and the fluids join together in the space between the processing surfaces arranged to be opposite so as to able to approach to and separate from each other, at least one of which rotates relative to the other, thereby forming a thin film fluid, and the reactants are reacted in the thin film fluid.

As shown inFIG. 25, this apparatus includes a first holder11, a second holder21arranged over the first holder11, a fluid pressure imparting mechanism P and a surface-approaching pressure imparting mechanism. The surface-approaching pressure imparting mechanism is comprised of a spring43and an air introduction part44.

The first holder11is provided with a first processing member10and a rotary shaft50. The first processing member10is a circular body called a mating ring and provided with a mirror-polished first processing surface1. The rotary shaft50is fixed to the center of the first holder11with a fixing device81such as a bolt and is connected at its rear end to a rotation drive device82(rotation drive mechanism) such as a motor, and the drive power of the rotation drive device82is transmitted to the first holder1thereby rotating the first holder11. The first processing member10is integrated with the first holder11and rotated.

A receiving part capable of receiving the first processing member10is arranged on the upper part of the first holder11, wherein the first processing member10has been fixed to the first holder11by insertion to the receiving part. The first processing member10has been fixed with a rotation-preventing pin83so as not to be rotated relative to the first holder11. However, a method such as fitting by burning may be used for fixing in place of the rotation-preventing pin83in order to prevent rotation.

The first processing surface1is exposed from the first holder11and faced with the second holder21. The material for the first processing surface includes ceramics, sintered metal, abrasion-resistant steel, other hardened metals, and rigid materials subjected to lining, coating or plating.

The second holder21is provided with a second processing member20, a first introduction part d1for introducing a fluid from the inside of the processing member, a spring43as a surface-approaching pressure imparting mechanism, and an air introduction part44.

The second processing member20is a circular member called a compression ring and includes a second processing surface2subjected to mirror polishing and a pressure-receiving surface23(referred to hereinafter as separation regulating surface23) which is located inside the second processing surface2and adjacent to the second processing surface2. As shown in the figure, the separation regulating surface23is an inclined surface. The method of the mirror polishing to which the second processing surface2was subjected is the same as that to the first processing surface1. The material for the second processing member20may be the same as one for the first processing member10. The separation regulating surface23is adjacent to the inner periphery25of the circular second processing member20.

A ring-accepting part41is formed in the bottom (lower part) of the second holder21, and the second processing member20together with an O-ring is accepted in the ring-accepting part41. The second processing member20is accepted with a rotation preventive84so as not to be rotated relative to the second holder21. The second processing surface2is exposed from the second holder21. In this state, the second processing surface2is faced with the first processing surface1of the first processing member10.

The ring-accepting part41arranged in the second holder21is a depression for mainly accepting that side of the second ring20which is opposite to the processing surface2and is a groove formed in a circular form when viewed in a plane.

The ring-accepting part41is formed in a larger size than the second ring20and accepts the second ring20with sufficient clearance between itself and the second ring20.

By this clearance, the second processing member20is accepted in the ring-accepting part41such that it can be displaced not only in the axial direction of the accepting part41but also in a direction perpendicular to the axial direction. The second processing member20is accepted in the ring-accepting part41such that the central line (axial direction) of the second processing member20can be displaced so as not to be parallel to the axial direction of the ring-accepting part41.

The spring43is arranged as a processing member-biasing part in at least the ring-accepting part41of the second holder21. The spring43biases the second processing member20toward the first processing member10. As another bias method, air pressure such as one in the air introduction part44or another pressurization means for applying fluid pressure may be used to bias the second processing member20held by the second holder21in the direction of approaching the second processing member20to the first processing member10.

The surface-approaching pressure imparting mechanism such as the spring43or the air introduction part44biases each position (each position in the processing surface) in the circumferential direction of the second processing member20evenly toward the first processing member10. The first introduction part d1is arranged on the center of the second holder21, and the fluid which is pressure-fed from the first introduction part d1to the outer periphery of the processing member is first introduced into the space surrounded with the second processing member20held by the second holder21, the first processing member10, and the first holder11that holds the first processing member10. Then, the feeding pressure (supply pressure) of the fluid by the fluid pressure imparting mechanism P is applied to the pressure-receiving surface23arranged in the second processing member20, in the direction of separating the second processing member20from the first processing member10against the bias of the biasing part.

For simplifying the description of other components, only the pressure-receiving surface23is described, and as shown inFIG. 29(A)andFIG. 29(B), properly speaking, together with the pressure-receiving surface23, apart23X not provided with the pressure-receiving surface23, out of the projected area in the axial direction relative to the second processing member20in a grooved depression13described later, serves as a pressure-receiving surface and receives the feeding pressure (supply pressure) of the fluid by the fluid pressure imparting mechanism P.

The apparatus may not be provided with the pressure-receiving surface23. In this case, as shown inFIG. 26(A), the effect (micro-pump effect) of introduction of the fluid to be processed into the space between the processing surfaces formed by rotation of the first processing surface1provided with the grooved depression13formed to function the surface-approaching pressure imparting mechanism may be used. The micro-pump effect is an effect by which the fluid in the depression advances with speed toward the end in the circumferential direction by rotation of the first processing surface1and then the fluid sent to the end of the depression13further receives pressure in the direction of inner periphery of the depression13thereby finally receiving pressure in the direction of separating the processing surface and simultaneously introducing the fluid into the space between the processing surfaces. Even if the first processing surface1is not rotated, the pressure applied to the fluid in the depression13arranged in the first processing surface1finally acts on the second processing surface2to be separated as a pressure-receiving surface.

For the depression13arranged on the processing surface, its total area in the horizontal direction relative to the processing surface, and the depth, number, and shape of depressions, can be established depending on the physical properties of a fluid containing reactants and reaction products.

The pressure-receiving surface23and the depression13may be arranged in the same apparatus.

The depression13is a depression having a depth of 1 μm to 50 μm, preferably 3 μm to 20 μm, which is arranged on the processing surface, the total area thereof in the horizontal direction is 5% to 50%, preferably 15% to 25%, based on the whole of the processing surface, the number of depressions is 3 to 50, preferably 8 to 24, and the depression extends in a curved or spiral form on the processing surface or bends at a right angle. By having depth changing continuously, fluids with high to low viscosity, even containing solids, can be introduced into the space between the processing surfaces stably by the micro-pump effect. The depressions arranged on the processing surface may be connected to one another or separated from one another in the side of introduction, that is, inside the processing surface.

As described above, the pressure-receiving surface23is inclined. This inclined surface (pressure-receiving surface23) is formed such that the distance in the axial direction between the upstream end in the direction of flow of the fluid and the processing surface of the processing member provided with the depression13is longer than the distance between the downstream end and the aforesaid processing surface. The downstream end of this inclined surface in the direction of flow of the fluid is arranged preferably on the projected area in the axial direction of the depression13.

Specifically, as shown inFIG. 28(A), a downstream end60of the inclined surface (pressure-receiving surface23) is arranged on the projected area in the axial direction of the depression13. The angle θ1of the inclined surface to the second processing surface2is preferably in the range of 0.1° to 85°, more preferably in the range of 10° to 55°, still more preferably in the range of 15° to 45°. The angle θ1can vary depending on properties of the product before processing. The downstream end60of the inclined surface is arranged in the region extending from the position apart downstream by 0.01 mm from an upstream end13-bto the position apart upstream by 0.5 mm from a downstream end13-cin the depression13arranged in the first processing surface1. The downstream end60of the inclined surface is arranged more preferably in the region extending from the position apart downstream by 0.05 mm from the upstream end13-bto the position apart upstream by 1.0 mm from the downstream end13-c. Like the angle of the inclined surface, the position of the downstream end60can vary depending on properties of a material to be processed. As shown inFIG. 28(B), the inclined surface (pressure-receiving surface23) can be a curved surface. The material to be processed can thereby be introduced more uniformly.

The depressions13may be connected to one another or separated from one another as described above. When the depressions13are separated, the upstream end at the innermost peripheral side of the first processing surface1is13-b, and the upstream end at the outermost peripheral side of the first processing surface1is13-c.

In the foregoing description, the depression13was formed on the first processing surface1and the pressure-receiving surface23was formed on the second processing surface2. On the contrary, the depression13may be formed on the second processing surface2, and the pressure-receiving surface23may be formed on the first processing surface1.

Alternatively, the depression13is formed both on the first processing surface1and the second processing surface2, and the depression13and the pressure-receiving surface23are alternately arranged in the circumferential direction of each of the respective processing surfaces1and2, whereby the depression13formed on the first processing surface1and the pressure-receiving surface23formed on the second processing surface2are faced with each other and simultaneously the pressure-receiving surface23formed on the first processing surface1and the depression13formed on the second processing surface2are faced with each other.

A groove different from the depression13can be formed on the processing surface. Specifically, as shown inFIG. 16(F)andFIG. 16(G), a radially extending novel depression14instead of the depression13can be formed outward in the radial direction (FIG. 16(F)) or inward in the radial direction (FIG. 16(G)). This is advantageous for prolongation of retention time between the processing surfaces or for processing a highly viscous fluid.

The groove different from the depression13is not particularly limited with respect to the shape, area, number of depressions, and depth. The groove can be formed depending on the object.

The second introduction part d2independent of the fluid flow path introduced into the processing surface and provided with the opening d20leading to the space between the processing surfaces is formed on the second processing member20.

Specifically, as shown inFIG. 27(A), the direction of introduction of the second introduction part d2from the opening d20of the second processing surface2is inclined at a predetermined elevation angle (θ1) relative to the second processing surface2. The elevation angle (θ1) is arranged at more than 0° and less than 90°, and when the reaction speed is high, the angle (θ1) is preferably arranged at 1° to 45°.

As shown inFIG. 27(B), the direction of introduction of the second processing surface2from the opening d20has directionality in a plane along the second processing surface2. The direction of introduction of the second fluid is in the direction in which a component on the processing surface is made apart in the radial direction and in the direction in which the component is forwarded in the rotation direction of the fluid between the rotating processing surfaces. In other words, a predetermined angle (θ2) exists facing the rotation direction R from a reference line g in the outward direction and in the radial direction passing through the opening d20.

The elevation angle (θ1) is arranged at more than 0° and less than 90°, and when the reaction speed is high, the angle (θ1) is preferably arranged at 1° to 45°.

The angle (θ2) is also arranged at more than 0° and less than 90° at which the fluid is discharged from the opening d20in the shaded region inFIG. 27(B). When the reaction speed is high, the angle (η2) may be small, and when the reaction speed is low, the angle (η2) is preferably arranged larger. This angle can vary depending on various conditions such as the type of fluid, the reaction speed, viscosity, and the rotation speed of the processing surface.

The bore diameter of the opening d20is preferably 0.2 Rat to 3000 μm, more preferably 10 μm to 1000 μm. Even if the bore diameter of the opening d20is relatively large, the diameter of the second introduction part d2shall be 0.2 μm to 3000 μm, more preferably 10 μm to 1000 μm, and when the diameter of the opening d20does not substantially influence the flow of a fluid, the diameter of the second introduction part d2may be established in this range. Depending on whether the fluid is intended to be transferred straight or dispersed, the shape of the opening d20is preferably changed and can be changed depending on various conditions such as the type of fluid, reaction speed, viscosity, and rotation speed of the processing surface.

The opening d20in the separate flow path may be arranged at a position nearer to the outer diameter than a position where the direction of flow upon introduction by the micro-pump effect from the depression arranged in the first processing surface1is converted into the direction of flow of a spiral laminar flow formed between the processing surfaces. That is, inFIG. 26(B), the distance n from the outermost side in the radial direction of the processing surface of the depression arranged in the first processing surface1to the outside in the radial direction is preferably 0.5 mm or more. When a plurality of openings are arranged for the same fluid, the openings are arranged preferably concentrically. When a plurality of openings are arranged for different fluids, the openings are arranged preferably concentrically in positions different in radius. This is effective for the reactions such as cases (1) A+B→C and (2) C+D→E should occur in due order, but other case, i.e., A+B+C→F should not occur, or for circumventing a problem that an intended reaction does not occur due to insufficient contact among reactants.

The processing members are dipped in a fluid, and a fluid obtained by reaction between the processing surfaces can be directly introduced into a liquid outside the processing members or into a gas other than air.

Further, ultrasonic energy can be applied to the material just after being discharged from the space between the processing surfaces or from the processing surface.

Then, the case where temperature regulating mechanisms J1and J2are arranged in at least one of the first processing member10and the second processing member20for generating a temperature difference between the first processing surface1and the second processing surface2is described.

The temperature regulating mechanism is not particularly limited. A cooling part is arranged in the processing members10and20when cooling is intended. Specifically, a piping for passing ice water and various cooling media or a cooling element such as a Peltier device capable of electric or chemical cooling is attached to the processing members10and20.

When heating is intended, a heating part is arranged in the processing members10and20. Specifically, steam as a temperature regulating medium, a piping for passing various hot media, and a heating element such as an electric heater capable of electric or chemical heating is attached to the processing members10and20.

An accepting part for a new temperature regulating medium capable of directly contacting with the processing members may be arranged in the ring-accepting part. The temperature of the processing surfaces can be regulated by heat conduction of the processing members. Alternatively, a cooling or heating element may be embedded in the processing members10and20and electrified, or a path for passing a cooling medium may be embedded, and a temperature regulating medium (cooling medium) is passed through the path, whereby the temperature of the processing surfaces can be regulated from the inside. By way of example, the temperature regulating mechanisms J1and J2which are pipes (jackets) arranged inside the processing members10and20are shown inFIG. 25.

By utilizing the temperature regulating mechanisms J1and J2, the temperature of one of the processing surfaces is made higher than that of the other, to generate a temperature difference between the processing surfaces. For example, the first processing member10is heated to 60° C. by any of the methods, and the second processing member20is set at 15° C. by any of the methods. In this case, the temperature of the fluid introduced between the processing surfaces is changed from 60° C. to 15° C. in the direction from the first processing surface1to the second processing surface2. That is, the fluid between the processing surfaces has a temperature gradient. The fluid between the processing surfaces initiates convection due to the temperature gradient, and a flow in a direction perpendicular to the processing surface is generated. The “flow in a direction perpendicular to the processing surface” refers to a flow in which components flowing in a direction perpendicular to at least the processing surface are contained in flowing components.

Even when the first processing surface1or the second processing surface2rotates, the flow in a direction perpendicular to the processing surface is continued, and thus the flow in a direction perpendicular to the processing surface can be added to a spiral laminar flow between the processing surfaces caused by rotation of the processing surfaces. The temperature difference between the processing surfaces is 1° C. to 400° C., preferably 5° C. to 100° C.

The rotary shaft50in this apparatus is not limited to a vertically arranged shaft. For example, the rotary shaft may be arranged at a slant. This is because the influence of gravity can be substantially eliminated by a thin fluid film formed between the processing surfaces1and2during processing. As shown inFIG. 25, the first introduction part d1coincides with the shaft center of the second ring20in the second holder21and extends vertically. However, the first introduction part d1is not limited to the one coinciding with the shaft center of the second ring20, and as far as it can supply the first fluid to the space surrounded with the rings10and20, the part d1may be arranged at a position outside the shaft center in the central part22of the second holder21and may extend obliquely as well as vertically. Regardless of the angle at which the part d1is arranged, a flow perpendicular to the processing surface can be generated by the temperature gradient between the processing surfaces.

When the temperature gradient of the fluid between the processing surfaces is low, heat conduction merely occurs in the fluid, but when the temperature gradient exceeds a certain border value, a phenomenon called Benard convection is generated in the fluid. This phenomenon is governed by Rayleigh number Ra, a dimensionless number, defined by the following equation:
Ra=L3·g·β·ΔT/(α·ν)
wherein L is the distance between processing surfaces; g is gravitational acceleration; β is coefficient of volumetric thermal expansion of fluid; ν is dynamic viscosity of fluid; α is heat diffusivity of fluid; and ΔT is temperature difference between processing surfaces. The critical Rayleigh number at which Benard convection is initiated to occur, although varying depending on the properties of a boundary phase between the processing surface and the fluid, is regarded as about 1700. At a value higher than this value, Benard convection occurs. Under the condition where the Rayleigh number Ra is a large value of about 1010or more, the fluid becomes a turbulent flow. That is, the temperature difference ΔT between the processing surfaces or the distance L between the processing surfaces in this apparatus are regulated such that the Rayleigh number Ra becomes 1700 or more, whereby a flow perpendicular to the processing surface can be generated between the processing surfaces, and the reaction procedures described above can be carried out.

However, the Benard convection hardly occurs when the distance between the processing surfaces is about 1 μm to 10 μm. Strictly, when the Rayleigh number is applied to a fluid between the processing surfaces having a distance of 10 μm or less therebetween to examine the conditions under which Benard convection is generated, the temperature difference should be several thousands of degrees or more in the case of water, which is practically difficult. Benard convection is one related to density difference in temperature gradient of a fluid, that is, to gravity. When the distance between the processing surfaces is 10 μm or less, there is high possibility of minute gravity field, and in such a place, buoyancy convection is suppressed. That is, it is the case where the distance between the processing surfaces is 10 μm or more that Benard convection actually occurs.

When the distance between the processing surfaces is about 1 μm to 10 μm, convection is generated not due to density difference but due to surface tension difference of a fluid resulting from temperature gradient. Such convection is Marangoni convection. This phenomenon is governed by Marangoni number Ma, a dimensionless number, defined by the following equation:
Ma=σΔT·L/(ρ·ν·α)
wherein L is the distance between processing surfaces; ν is dynamic viscosity of fluid; α is heat diffusivity of fluid; ΔT is temperature difference between processing surfaces; ρ is density of fluid; and σ is temperature coefficient of surface tension (temperature gradient of surface tension). The critical Marangoni number at which Marangoni convection is initiated to occur is about 80, and under the conditions where the Marangoni number is higher than this value, Marangoni convection occurs. That is, the temperature difference ΔT between the processing surfaces or the distance L between the processing surfaces in this apparatus is regulated such that the Marangoni number Ma becomes 80 or more, whereby a flow perpendicular to the processing surface can be generated between the processing surfaces even if the distance therebetween is as small as 10 μm or less, and the reaction procedures described above can be carried out.

For calculation of Rayleigh number, the following equations were used.

Ra=L3·β·gv·α⁢Δ⁢⁢T⁢⁢Δ⁢⁢T=(T1-T0)⁢⁢α=kρ·Cp[Equation⁢⁢1]
L is the distance (m) between processing surfaces; β is coefficient of volumetric thermal expansion (1/K); g is gravitational acceleration (m/s2); ν is dynamic viscosity (m2/s); α is heat diffusivity (m2/s); ΔT is temperature difference (K) between processing surfaces; pis density (kg/m3); Cp is isobaric specific heat (J/kg·K); k is heat conductivity (W/m·K); T1is temperature (K) at high temperature side in processing surface; and T0is temperature (K) at low temperature side in processing surface.

When the Rayleigh number at which Benard convection is initiated to occur is the critical Rayleigh number RaC, the temperature difference ΔTC1is determined as follows:

For calculation of Marangoni number, the following equations were used.

Ma=σt·Lρ·v·α⁢Δ⁢⁢T⁢⁢Δ⁢⁢T=(T1-T0)⁢⁢α=kρ·Cp[Equation⁢⁢3]
L is the distance (m) between processing surfaces; ν is dynamic viscosity (m2/s); α is heat diffusivity (m2/s); ΔT is temperature difference (K) between processing surfaces; ρ is density (kg/m3); Cp is isobaric specific heat (J/kg·K); k is heat conductivity (W/m·K); σtis surface tension temperature coefficient (N/m·k); T1is temperature (K) of a high-temperature surface out of processing surface; and T0is temperature (K) of a low-temperature surface out of processing surface.

When the Marangoni number at which Marangoni convection is initiated to occur is the critical Marangoni number MaC, the temperature difference ΔTC2is determined as follows:

The materials for the processing surface arranged to be opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, are not particularly limited, and the processing surfaces1and2can be prepared from ceramics, sintered metals, abrasion-resistant steels, other metals subjected to hardening treatment, or rigid materials subjected to lining, coating or plating. In the present invention, the distance between the processing surfaces1and2arranged to be opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, is 0.1 μm to 100 μm, particularly preferably 1 μm to 10 μm.

Hereinafter, production of resin microparticles according to the present invention is described.

Resin microparticles are formed by forced uniform mixing between the processing surfaces1and2arranged to be opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, in the apparatus shown inFIG. 1(A).

First, a fluid containing at least one kind of aqueous solvent is introduced as a first fluid through one flow path, that is, the first introduction part d1into the space between the processing surfaces1and2arranged to be opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, thereby forming a thin film fluid out of the first fluid between the processing surfaces.

Then, a fluid wherein at least one kind of resin is dissolved, preferably dispersed in a molecular state, in a solvent solubilizing, and compatible with, the resin is introduced as a second fluid directly through another flow path, that is, the second introduction part d2into the thin film fluid out of the first fluid produced between the processing surfaces1and2.

As described above, a thin film fluid is formed between the processing surfaces1and2, the distance of which is regulated by the pressure balance between the supply pressure of the fluid and the pressure exerted between the rotating processing surfaces. Then, the first fluid and the second fluid are allowed to flow together in this thin film fluid to form a thin film fluid. The first fluid and the second fluid are allowed to flow together and mixed to form resin microparticles by separation or emulsification. Usually, a surfactant is added to the first or second fluid to give a resin microparticle liquid dispersion having resin microparticles dispersed in a water phase. The processing in the present invention may or may not be accompanied by resin phase transition.

The “emulsification” includes a step of preparing resin emulsion particles by joining the first and second fluids together in a thin film fluid between the processing surfaces and then emulsifying a resin dissolved (dispersed in a molecular state) in the thin film fluid. When the prepared resin emulsion particles are resin microparticles themselves, or when the resin emulsion particles are removed by removing the solvent from the fluid containing the resin emulsion particles, water dispersion of the resin microparticles, and resin microparticles, can also be obtained from the resin emulsion particles.

To effect the preparation of the resin microparticles between the processing surfaces1and2, the second fluid may be introduced through the first introduction part d1and the first fluid through the second introduction part d2, as opposed to the above description. That is, the expression “first” or “second” for each fluid has a meaning for merely discriminating an nthfluid among a plurality of fluids present, and third or more fluids can also be present.

The particle size, or monodispersity of the obtained resin microparticles can be regulated by changing the number of revolutions of the processing surfaces1and2, the distance between the processing surfaces1and2and the flow rate and temperature of the thin film fluid, and the concentration of materials. As described above, monodisperse resin microparticles having a smaller volume-average particle size that those obtained by the previous reaction methods can be obtained. Further, resin microparticles can be continuously and efficiently obtained with high production efficiency to cope with large-scale production. Depending on a necessary amount of production, the processing apparatus of the present invention can grow in size by using general scale-up concept. The resin microparticles can be obtained uniformly with low energy.

The solvent in which the resin is dissolved and dispersed in a molecular state is not particularly limited as long as it shows solubility and compatibility for the resin. As specific solvent, toluene, ethyl acetate, butyl acetate, methyl ethyl ketone, and methyl isobutyl ketone can be used singly or as a mixture of two or more thereof.

The aqueous solvent used in the present invention may be water alone or a mixture of water and a miscible solvent. The miscible solvent includes alcohols (methanol, isopropanol, ethylene glycol, and the like).

In place of the fluid in which a resin is dissolved or dispersed in a molecular state in the solvent with which the resin is soluble and compatible, a fluid containing at least one kind of molten resin may be used. That is, the molten resin can be emulsified and dispersed in a thin film fluid and then solidified. The fact that a resin is molten means that, for example, a crystalline resin when heated to a temperature higher than the melting point shows properties as liquid fluid. When a resin such as an amorphous resin is molten, the resin upon heating to a temperature which is generally higher than the glass transition point begins to decrease the viscosity thus showing behavior as fluid. On this occasion, the resin may be molten by itself or in a solvent with which the resin is not soluble or compatible. The solidification of the resin has an opposite meaning to melting. The molten resin can thereby be heated and molten just before emulsification/dispersion treatment and then cooled after the treatment, so that the treatment can be effected in a short time, the heat history (=the sum total of (temperature×time)) on resin can be substantially decreased, and thus the risk of resin hydrolysis can be reduced. Accordingly, the temperature of the emulsification/dispersion treatment can be made higher than in conventional production methods. Therefore, the resin viscosity can be further reduced in emulsion/dispersion treatment, and as a result, the objective particle size distribution can be obtained with low energy. When the molten resin is separated or emulsified/dispersed at high temperatures, the quantity possessed is so small that the apparatus can be reduced in size, is easily handled and is highly safe.

The step of preliminarily mixing the resin in an aqueous solvent, which has been essential for gradually pulverizing resin particles in the existing techniques, can be omitted according to the method for producing the resin microparticle liquid dispersion of the present invention. That is, before the fluid is introduced between the processing surfaces1and2, the present invention does not need the preliminarily mixing step of previously mixing the resin in an aqueous solvent such that the resin is dispersed in the state of coarse particles in the aqueous solvent, and each fluid can be introduced as such into the apparatus. Accordingly, there are advantages that the process can be simplified, the reduction in yield due to a complex process can be prevented, the heat history of resin generated during preliminary mixing can be omitted, and the risk of resin hydrolysis can be reduced. Prior to introduction of the fluid into the space between the processing surfaces1and2, mixing of the resin in a part of the aqueous solvent in the first or second fluid does not correspond to “preliminary mixing”. This is because this treatment is a treatment for supplying the resin with behavior as fluid and does not correspond to treatment for gradually pulverizing resin particles as in the prior art.

However, the production method of the present invention does not completely exclude the preliminarily mixing step. Accordingly, the same preliminarily mixing step as conventional may be arranged.

The processing surfaces can be cooled or heated thereby obtaining desired resin microparticles. Particularly, when a difference in temperature is set between the first processing surface1and the second processing surface2, there is an advantage that since convection can be generated in a thin film fluid, the forced uniform mixing between the processing surfaces1and2can further be promoted.

In addition, the space between the processing surfaces may be irradiated with ultraviolet ray (UV), depending on the object.

The separation or emulsification/dispersion processing is conducted in a container capable of securing a depressurized or vacuum state, and a secondary side at which the fluid (resin microparticle liquid dispersion) after processing is discharged is depressurized or made vacuous, thereby being able to remove a gas generated when the fluids join together in the thin film fluid and a gas contained in the fluid, or to remove the solvent of the fluid. By doing so, the resin microparticle-containing fluid between the processing surfaces is discharged in an atomized state from the processing surfaces, even when processing of removal of the solvent is conducted simultaneously with the separation or emulsification/dispersion processing, so that the surface area of the fluid is increased, and the efficiency of removal of the solvent is extremely high. Accordingly, separation or emulsification/dispersion processing and removal of the solvent can be effected in substantially one step more easily than conventional.

The separation or emulsification/dispersion processing can be conducted in a container capable of temperature regulation to cool e.g. the fluid (resin microparticle liquid dispersion) just after being discharged, thereby solidifying the molten resin. By doing so, the resin microparticles obtained by the separation or emulsification/dispersion processing can be rapidly cooled to a stable temperature range for the microparticles, that is, to a temperature lower than the melting point or lower than the glass transition point. Alternatively, the container may be heated to improve the efficiency of solvent removal and gas removal.

As the resin, any resins can be used. Examples of such resins include vinyl polymerizing thermoplastic resins (styrene resin, olefin resin, acrylic resin, halogen-containing resin, vinyl ester resin or derivatives thereof), condensed thermoplastic resins (polyester resin, polyamide resin, polyurethane resin, poly(thio)ether resin, polycarbonate resin, polysulfone resin, polyimide resin, and the like), natural product-derived resins (cellulose ester resin and the like), and epoxy resin. These resins may be singly or as a mixture of two or more thereof. The resin may be crystalline or amorphous.

The styrene resin includes homopolymers or copolymers (polystyrene, styrene-vinyl toluene copolymer, styrene-α-methyl styrene copolymer, and the like) of styrene monomers (styrene, α-methylstyrene, vinyltoluene, and the like), styrene monomer/copolymerizable monomer copolymers (styrene-acrylonitrile copolymer (AS resin), (meth)acrylate-ester-styrene copolymer (MS resin and the like), styrene-maleic anhydride copolymer, block copolymers such as styrene-butadiene block copolymer, graft polymers (impact-resistant polystyrene (HIPS, or rubber graft polystyrene resin)) produced by graft polymerization of at least styrene monomers in the presence of a rubber component, acrylonitrile-butadiene-styrene copolymer (ABS resin), graft copolymers (AXS resins such as AES resin, AAS resin and ACS resin) wherein rubber components such as ethylene propylene rubber E, acryl rubber A, chlorinated polyethylene C, and vinyl acetate polymer are used in place of butadiene rubber B of the ABS resin, and graft copolymers (methyl methacrylate-butadiene rubber-styrene copolymer (MBS resin) and the like) wherein (meth)acrylate monomers (methyl methacrylate and the like) are used in place of acrylonitrile of the ABS resin.

The olefin resin includes homopolymers or copolymers of α-C2-6 olefins, for example homopolymers or copolymers of olefins, such as polyethylene, polypropylene, ethylene-propylene copolymer, and poly(methylpentene-1), and copolymers of olefin and copolymerizable monomers (ethylene-vinyl acetate copolymer, ethylene-(meth)acrylic acid copolymer, ethylene-(meth)acrylate-ester copolymer, and the like).

The halogen-containing resin includes, for example, polyvinyl chloride resin, vinyl chloride-vinyl acetate copolymer, vinylidene chloride resin, and fluorine resin. The vinyl ester resin or its water-insoluble derivatives include, for example, homopolymers or copolymers of carboxylic acid vinyl ester (polyvinyl acetate, ethylene-vinyl acetate copolymer, and the like), their saponification products (vinyl alcohol resins such as polyvinyl alcohol with a saponification degree of 50% or less and ethylene-vinyl alcohol copolymer), and derivatives (for example, polyvinyl acetal resins such as polyvinyl formal and polyvinyl butyral) from saponification products (vinyl alcohol resins).

The polycarbonate resins include bisphenol-based aromatic polycarbonates such as bisphenol A-type polycarbonate resins, and aliphatic polycarbonates such as diethylene glycol bisallyl carbonate.

The polysulfone resins can be exemplified by polysulfone resin, polyether sulfone resin, polyaryl sulfone resin, and the like. The polyimide resins can be exemplified by polyether imide resin, polyamide imide resin, polybenzimidazole resin, and the like.

The cellulose derivatives include cellulose esters (for example, cellulose acetates (acetate cellulose) such as cellulose diacetate and cellulose triacetate, acyl celluloses such as cellulose propionate, cellulose butyrate, cellulose acetate propionate and cellulose acetate butyrate, inorganic acid esters of cellulose, and the like), and cellulose carbamates (cellulose phenyl carbamate, and the like). If necessary, for example, alkyl celluloses such as ethyl cellulose, isopropyl cellulose and butyl cellulose, aralkyl celluloses such as benzyl cellulose, and cyanoethyl cellulose may be used as water-insoluble cellulose ethers.

The epoxy resins include a ring opening polymerization product of polyepoxide (19), a polyaddition product between polyepoxide (19) and an active hydrogen group-containing compound (D) {water, polyol [the diol (11) and trivalent or more polyol (12)], dicarboxylic acid (13), trivalent or more polycarboxylic acid (14), polyamine (16), polythiol (17) and the like}, and a cured product between polyepoxide (19) and an acid anhydride of dicarboxylic acid (13) or trivalent or more polycarboxylic acid (14).

These resins may be colorant-containing kneaded resins.

At least one of the fluids may contain a dispersant. The dispersant is not particularly limited. The dispersant in an aqueous solvent includes water-soluble resins such as polyvinyl alcohol, polyethylene glycol, polyethylene oxide, polyvinyl pyrrolidone, water-soluble acrylic resin, water-soluble styrene resin and cellulose ether resin, and water-soluble saccharide compositions that contain oligosaccharide. In other solvents, known surfactants can be used and a dispersion stabilizer selected from a cationic surfactant, an anionic surfactant, a nonionic surfactant, and the like can be used. These surfactants may be used as a mixture of two or more thereof.

The nonionic surfactants include polyethylene oxide, polypropylene oxide, a combination of polypropylene oxide and polyethylene oxide, an ester between polyethylene glycol and higher fatty acid, alkyl phenol polyethylene oxide, an ester between higher fatty acid and polyethylene glycol, an ester between higher fatty acid and polypropylene oxide, sorbitan ester, and the like.

When a water dispersion of polyester resin into which carboxyl groups were introduced is prepared, a part or the whole of polar groups such as carboxyl groups on the surface of the dispersion may be contained in the fluid to stabilize the fluid by neutralization with the dispersion.

The basic substance that can be used in the neutralization includes, for example, amine compounds represented by ammonia and triethylamine and inorganic bases represented by sodium hydroxide, potassium hydroxide and lithium hydroxide.

When the resulting resin is used in an electrophotographic toner, a fluid containing at least one member selected from the above-mentioned colorant, an electrification regulator, a release agent, an external additive, a magnetic carrier, and electrically conductive powders may be used in the fluid in the method for producing the resin microparticles.

The electrification regulator used may be known one. Examples of the electrification regulator include nigrosine dyes, triphenylmethane dyes, chrome-containing metal complex dyes, molybdate chelate pigments, rhodamine dyes, alkoxy amines, quaternary ammonium salts (including fluorine-modified quaternary ammonium salts), alkyl amides, phosphorus element or compound, tungsten element or compound, fluorine activators, metal salicylate and metal salts of salicylic acid derivatives.

Other polymer microparticles include, for example, those obtained by soap-free emulsion polymerization, suspension polymerization and dispersion polymerization: for example, polystyrene, methacrylate esters and acrylate ester copolymers, polycondensation products such as silicone, benzoguanamine and nylon, and polymer particles of thermosetting resin. Such fluidizers may be surface-treated to increase hydrophobicity and can prevent deterioration in flow characteristics and electrification characteristics even under high humidity. Preferable examples of surface treatment agents include silane coupling agents, silylating agents, silane coupling agents having an alkyl fluoride group, organic titanate coupling agents, aluminum coupling agents, silicone oil and modified silicone oil.

As for magnetic carriers, conventionally known ones such as iron powder, ferrite powder, magnetite powder and magnetic resin carriers can be used. And, as for the covering materials, included are amino resins: for example, urea-formaldehyde resin, melamine resin, benzoguanamine resin, urea resin and polyamide resin.

The electrically conductive powder that can be used includes metal powder, carbon black, titanium oxide, tin oxide and zinc oxide.

As the fluid in the method for producing the resin microparticles, a fluid containing silver nanoparticles can be used. Silver microparticle-containing resin microparticles having silver nanoparticles dispersed uniformly in a resin structure can be prepared to confer an antibacterial effect on resin products.

In this manner, a dispersion (suspension) of resin microparticles having a volume-average particle size of 1 nm to 10000 nm, preferably 10 nm to 800 nm, more preferably 40 nm to 500 nm can be prepared.

As described above, the processing apparatus can be provided with a third introduction part d3in addition to the first introduction part d1and the second introduction part d2. In this case, a resin solution, a surfactant solution, and a colorant for example can be introduced separately through the respective introduction parts into the processing apparatus. By doing so, the concentration and pressure of each solution can be separately controlled, and the reaction of forming resin microparticles can be regulated more accurately. When the processing apparatus is provided with four or more introduction parts, the foregoing applies and fluids to be introduced into the processing apparatus can be subdivided in this manner.

EXAMPLE

Hereinafter, the present invention is described in detail with reference to Examples, but the present invention is not limited to Examples.

A resin solution or resin liquid dispersion is allowed to flow into an aqueous solvent in a thin film fluid between the processing surfaces1and2arranged to be opposite to each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, in use of a uniformly stirring and mixing reaction apparatus shown inFIG. 1(A), thereby uniformly mixing them in the thin film fluid.

In following Examples, the term “from the center” means “through the first introduction part d1” in the processing apparatus shown inFIG. 1(A), the first fluid refers to the first processed fluid, and the second fluid refers to the second processed fluid introduced “through the second introduction part d2” in the processing apparatus shown inFIG. 1(A). The term “part” refers to “parts by weight”.

Particle size distribution was measured with a particle size distribution measuring instrument utilizing a laser Doppler method (trade name: Microtrac UPA150, manufactured by Nikkiso Co., Ltd.), and volume-average particle size was used.

A glass flask equipped with a stirrer, a distillation column, a thermometer and a nitrogen inlet was charged with 8 moles of neopentyl glycol, 4 moles of ethylene glycol and 8 moles of terephthalic acid. The flask was heated in a nitrogen stream to 180° C. in a mantle heater, a polymerization initiator (titanium tetrabutoxide) in an amount of 0.14% based on the total amount of the acid and alcohol components charged was added, and the mixture was reacted by heating under stirring. The progress of the reaction was monitored by measuring the acid value, and when a predetermined acid value was reached, the reaction was finished to give a polyester resin having a weight-average molecular weight of 650, a Tg of 56° C., a Tm of 103° C. and an acid value of 3.2.

While an aqueous solvent (1% dodecyl sodium sulfate aqueous solution) was sent as a first fluid from the center at a supply pressure/back pressure of 0.20 MPa/0.01 MPa and at a revolution number of 500 rpm, 5% polyester resin ethyl acetate solution using the above polyester resin was introduced at a rate of 10 ml/min. as a second fluid into the space between the processing surfaces1and2such that the first and second fluids were mixed and discharged at a rate of 30 ml/min. A polyester resin microparticle dispersion having a volume-average particle size of 45.2 nm was obtained.

Examples 2 to 4

In Examples 2 to 4, the same polyester resin ethyl acetate solution and aqueous solvent as in Example 1 were used, and the number of revolutions, supply pressure and the flow rate of the discharge were changed, whereby polyester resin microparticle dispersions were obtained.

While an aqueous solvent (1% dodecyl sodium sulfate/0.5% polyvinyl alcohol aqueous solution) was sent as a first fluid from the center at a supply pressure/back pressure of 0.60 MPa/0.45 MPa and at a revolution number of 500 rpm, a softened polyester resin liquid dispersion prepared by mixing 210 g of polyester resin (weight average molecular weight 16,000, softening temperature=105° C.) in 490 g of ion-exchange water (this “mixing” does not correspond to conventional “preliminary mixing”) and then heating the resulting polyester resin liquid dispersion to 150° C. just before introduction to soften the resin (30% softened polyester resin liquid dispersion) was introduced as a second fluid at 10 ml/min. into the space between the processing surfaces1and2. A polyester resin microparticle dispersion having a volume-average particle size of 63.1 nm was obtained.

Examples 6 to 8

In Examples 6 to 8, polyester resin microparticle dispersions were obtained using the same softened polyester resin in ion-exchange water (softened polyester resin liquid dispersion) and the same aqueous solvent as in Example 5 by changing the number of revolutions, the supply pressure, and the flow rate of the discharge.

While an aqueous solvent (0.7% sodium diisooctyl sulfosuccinate (trade name: AOT, Wako Pure Chemical Industries, Ltd.)/99.3% deionized water) was sent as a first fluid from the center at a supply pressure/back pressure of 0.15 MPa/0.01 MPa and at a revolution number of 1000 rpm, 0.4% polystyrene (PS) (trade name: Polystyrene, manufactured by Sigma-Aldrich Co.)/99.6% tetrahydrofuran (THF) (also called “PS solution”) was introduced as a second fluid at 10 ml/min. into the space between the processing surfaces1and2, and the mixture was mixed and emulsified such that the amount of the discharge became 20 g/min., to give a polyester resin microparticle dispersion having a volume-average particle size of 58.3 nm.

Examples 10 to 12

In Examples 10 to 12, polyester resin microparticle dispersions were obtained using the same PS solution and the same aqueous solvent as in Example 9 by changing the number of revolutions, the supply pressure, and the flow rate of the discharge.

Comparative Example

Using the same polyester resin ethyl acetate solution and the same aqueous solvent as in Example 1, the polyester resin ethyl acetate solution was suspended in the aqueous solvent with CLEARMIX (manufactured by M Technique Co., Ltd.) to prepare a polyester resin microparticle dispersion. At this time, the number of revolutions with CLEARMIX was 20000 rpm, and stirring was conducted for 30 minutes. A polyester resin microparticle dispersion having a volume-average particle size of 105.4 nm was obtained.

The results are shown in Table 1.

The amount of energy necessary for obtaining the resin microparticles in Examples was not higher than 1/10 relative to that in Comparative Example, although the volume-average particle size was made smaller in Examples. From this result, it was found that the production method in Examples is superior in energy efficiency.