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US Patent # 7,306,752. Method for preparing resin particles, resin particles and apparatus for preparing resin particles - Patents.com
United States Patent 7,306,752
Nakatani December 11, 2007
Method for preparing resin particles, resin particles and apparatus for preparing resin particles
The present provides a method for preparing resin fine particles of a homogeneous particle size used in the fields of chemistry, medicine, electronic material or the like, resin fine particles, and a production apparatus for resin fine particles.The present invention provides a method for preparing a resin fine particle, which comprises discharging a liquid comprising a polymerizable monomer as a dispersion phase into a continuous phase; splitting the liquid comprising the polymerizable monomer by applying mechanical vibration to form a liquid droplet; and polymerizing the liquid droplet in a state without splitting or integrating the liquid droplet, said method comprising recognizing a state of said liquid being split into a liquid droplet, and a condition of said discharging and/or said mechanical vibration of the liquid being determined by feedback from a result of the recognition.
Inventors: Nakatani; Yasuhiro (Mishima-gun, JP)
Appl. No.: 10/481,604
PCT No.: PCT/JP02/06208
371(c)(1),(2),(4) Date: May 07, 2004
PCT Pub. No.: WO03/000741
Jun 22, 2001 [JP] 2001-189989
Jun 22, 2001 [JP] 2001-189990
Current U.S. Class: 264/9 ; 264/40.1; 425/140; 425/6
Current International Class: B29B 9/10 (20060101)
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1. A method for preparing a resin fine particle, which comprises discharging a liquid comprising a polymerizable monomer as a dispersion phase into a continuous phase; splitting the liquid comprising the polymerizable monomer by applying mechanical vibration to form a liquid droplet; and polymerizing the liquid droplet in a state without splitting or integrating the liquid droplet, said method comprising recognizing a moment of a liquid droplet formation from a liquid column of said polymerizable monomer with a camera capable of photographing by a high shutter speed sufficient for catching the high speed liquid droplet formation state by a stationary state, or with combining the camera and a stroboscopic illumination, and a condition of said discharging and/or said mechanical vibration of the liquid being determined by feedback from a result of the recognition.
2. A method for preparing a resin fine particle, which comprises discharging a liquid comprising a polymerizable monomer as a dispersion phase into a continuous phase; splitting the liquid comprising the polymerizable monomer by applying mechanical vibration to form a liquid droplet; and polymerizing the liquid droplet in a state without splitting or integrating the liquid droplet, said method comprising measuring size of said formed liquid droplet with a method of taking in the image of the liquid droplets formed in the dispersion phase in a computer for measurement, and a condition of said discharging and/or said mechanical vibration of the liquid being determined by feedback from a result of the measurement, wherein the feedback can be controlled by sending a control signal from the computer or via a sequencer to the unit for applying the mechanical vibration or the unit for adjusting the discharge of the polymerizable monomer.
3. An apparatus, which is for carrying out the method for preparing a resin fine particle according to claim 2, which comprises a dispersion container; a jetting opening, opened in the dispersion container, for discharging a liquid comprising a polymerizable monomer into a liquid dispersion medium; a means for applying mechanical vibration to the liquid comprising the polymerizable monomer jetted into the liquid dispersion medium; and a photography unit for photographing a formed liquid droplet, wherein the photography unit is a CCD camera comprising a high speed shutter sufficient for catching the high speed liquid droplet formation in a stationary state, and a display capable of enlarging and displaying the minute liquid droplets in a visibly recognizable size.
4. An apparatus, which is for carrying out the method for preparing a resin fine particle according to claim 2, which comprises a dispersion container; a jetting opening, opened in the dispersion container, for discharging a liquid comprising a polymerizable monomer into a liquid dispersion medium; a means for applying mechanical vibration to the liquid comprising the polymerizable monomer jetted into the liquid dispersion medium; and a measuring means for measuring size of a formed liquid droplet, wherein the measuring means for size of the liquid droplets is to take in the image obtained by photographing the state of the liquid droplet formation by the photography unit into a computer, and measure size of the liquid droplets by an image processing unit, wherein the photography unit is a CCD camera comprising a high speed shutter or a stroboscopic illumination sufficient for catching the high speed liquid droplet formation in a stationary state, and a display capable of enlarging and displaying the minute liquid droplets in a visibly recognizable size.
5. An apparatus, which is for carrying out the method for preparing a resin fine particle according to claim 2, which comprises a dispersion container; a jetting opening, opened in the dispersion container, for discharging a liquid comprising a polymerizable monomer into liquid dispersion medium; a means for applying mechanical vibration to the liquid comprising the polymerizable monomer jetted into the liquid dispersion medium; a measuring means for measuring size of a formed liquid droplet, wherein the measuring means for size of the liquid droplets is to take in the image obtained by photographing the state of the liquid droplet formation by photography unit into a computer, and measure size of the liquid droplets by an image processing unit, wherein the photography unit is a CCD camera comprising a high speed shutter or stroboscopic illumination sufficient for catching the high speed liquid droplet formation in a stationary state, and a display capable of enlarging and displaying the minute liquid droplets in a visibly recognizable size and, a means for adjusting a discharging condition and/or a mechanical vibration condition of a liquid comprising a polymerizable monomer based on a measurement result of size of a liquid droplet by sending a control signal from the computer or via a sequencer to the unit for applying the mechanical vibration or the unit for adjusting the discharge of the polymerizable monomer.
The present invention relates to a method for preparing resin fine particles of a homogeneous particle size used in the fields of chemistry, medicine, electronic material or the like, resin fine particles and a production apparatus for resin fine particles.
Conventionally, as a method for producing resin fine particles, a suspension polymerization method is known. This method is a method for placing a water based medium with a dispersion stabilizer dissolved in a reaction vessel with an agitator, introducing a polymerizable monomer with a polymerization initiator dissolved while agitating, and heating, thereby obtaining resin fine particles. However, the particle size distribution of the resin fine particles obtained by the method is wide, so that a sorting operation such as classification is necessary for the application requiring the homogeneity of the particle size of a column filling material, a spacer, a toner, a material for a foamed product, or the like, and thus it is extremely complicated.
An object of the present invention is to provide a method for preparing resin fine particles of a homogeneous particle size used in the fields of chemistry, medicine, electronic material or the like, resin fine particles, and a production apparatus for resin fine particles.
According to one aspect of the present invention, provided is a resin fine particle produced by the method for preparing a resin fine particle according to the present invention, which has an average particle size of 10 to 3,000 .mu.m, and 80% or more of which falls within a range of .+-.10% of the average particle size.
FIG. 1 is a schematic diagram showing a case where liquid droplets are normally formed from a liquid column of a polymerizable monomer.
As the dispersion phase, a liquid comprising polymerizable monomer is used. Examples of the polymerizable monomer, in the case of an oil in water phase system, include a monovinyl aromatic compound such as styrene, vinyl naphthalene and alkyl substituted styrene; halo substituted styrene such as bromo styrene and chloro styrene; polyvinyl aromatic compound such as divinyl benzene, divinyl toluene, divinyl xylene, divinyl naphthalene, trivinyl benzene, divinyl diphenyl ether and divinyl diphenyl sulfone; halo olefin or vinyl halide of vinyl chloride or the like; ester of .alpha.-.beta.-ethylenically unsaturated carboxylic acid such as ester of acrylic acid or methacrylic acid; methyl methacrylate, ethyl acrylate, vinyl acetate and the like. In particular, in the case of use for the electronic material field, divinyl benzene as crosslinkable polymerizable monomer capable of obtaining the heat resistance and one produced by mixing divinyl benzene and polyfunctional acrylate are preferable. These polymerizable monomers may be used alone or in a combination of two or more kinds.
According to the method for preparing resin fine particles of the present invention, resin fine particles having a very homogeneous particle size can be obtained. According to one aspect of the present invention, provided is a resin fine particle produced by the method for preparing a resin fine particle according to the present invention, which has an average particle size of 10 to 3,000 .mu.m, and 80% or more of which falls within a range of .+-.10% of the average particle size.
Herein, the preferable lower limit of the particle size of the resin fine particles of the present invention is set at 10 .mu.m, and the upper limit is set at 3,000 .mu.m because the resin fine particles having such a particle size can hardly be produced by the suspension polymerization, so that the method for preparing resin fine particles of the present invention can be particularly effective in this range. When the resin fine particles fallen within the range of .+-.10% of the average particle size are less than 80%, the resin fine particles has an inhomogeneous particle size so that a classification step may be needed.
Although the dispersion container is not particularly limited, in consideration of photographing the liquid droplet formation state by a CCD camera or the like, and reaction after forming the liquid droplets, a transparent one durable to the heat of about 100.degree. C. is preferable. Examples of the dispersion container include a glass round or cylindrical separable flask container and the like.
Hereinafter, the present invention will be described in more detail with reference to examples, however, the present invention is not limited to these examples.
First, a production apparatus for resin fine particles as shown in FIG. 3 was produced.
By heating and agitating with an agitator and a cooling pipe installed in dispersion container 3 after jetting a predetermined amount of monomer M, Monomer M was polymerized so as to obtain resin fine particles. The average particle size of the obtained resin fine particles was 602 .mu.m, with 92% of the resin fine particles included in a range of .+-.10% of the average particle size.
A production apparatus for resin fine particles as shown in FIG. 4 was produced.
The average particle size of the obtained resin fine particles was 599 .mu.m, with 89% of the resin fine particles included in a range of .+-.10% of the average particle size.
In the same manner as in Example 1 except that the apparatus shown in FIG. 4 was used, resin fine particles were produced. That is, liquid droplets were produced by shaking liquid dispersion medium D with liquid polymerizable monomer M discharged. Size of the produced liquid droplets were measured by measuring unit S, and the result of the calculation process of the measured value was fed back to pump controller C1, so that adjustment was made for homogenizing size of the liquid droplets by the automatic operation. By heating and agitating with an agitator and a cooling pipe installed in dispersion container 3 after jetting a predetermined amount of monomer M, monomer M was polymerized so as to obtain resin fine particles.
The average particle size of the obtained resin fine particles was 601 .mu.m, with 95% of the resin fine particles included in a range of .+-.10% of the average particle size.
In the same manner as in Example 1 except that the CCD camera and the CRT monitor were not used, and the discharging condition and the frequency condition were not adjusted, resin fine particles were obtained.
The average particle size of the obtained resin fine particles was 688 .mu.m, with only 78% of the resin fine particles included in a range of .+-.10% of the average particle size.
A resin fine particle production apparatus same as the apparatus used in Example 1 except that three jetting openings 2 each having a 0.3 mm inner diameter were opened side by side in liquid dispersion medium D, was produced.
The average particle size of the resin fine particles obtained by polymerizing monomer M without adjustment for homogenizing size of the liquid droplets by a manual operation was 610 .mu.m, with only 65% of the resin fine particles included in a range of .+-.10% of the average particle size.
According to the present invention, it is possible to provide a method for preparing resin fine particles of a homogeneous particle size used in the fields of chemistry, medicine, electronic material or the like, resin fine particles and a production apparatus for resin fine particles.
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