Apparatus of manufacturing mesoporous silica and method of manufacturing mesoporous silica using the same

An apparatus and a method of manufacturing mesoporous silica are provided. The apparatus includes a mount, a reactor rotatably coupled to the mount, in which mixed solution of surfactant, water and acid is to be poured, an impeller installed to the reactor and rotating to stir the mixed solution, and a heating unit installed to cover an outer surface of the reactor thereby heating the reactor.

CROSS-REFERENCE TO RELATED APPLICATION

This U.S. non-provisional patent application claims priority under 35 U.S.C. § 119 to Korean Patent Application No. 10-2014-0192119, filed on Dec. 29, 2014, in the Korean Intellectual Property Office, the disclosure of which is hereby incorporated by reference in its entirety.

BACKGROUND

Embodiments of the inventive concepts relate to an apparatus of manufacturing mesoporous silica and a method of manufacturing mesoporous silica using the same, and more particularly relate to an apparatus of manufacturing mesoporous silica capable of manufacturing a large quantity of mesoporous silica promptly and stably and a method of manufacturing mesoporous silica using the same.

Porous material has been applied to a catalyzer or a carrier because of large interior surface area. The porous materials are classified into microporous under 2 nm, mesoporous of 2 nm though 50 nm and macroporous over 50 nm according to size of pores.

In 1992, a synthesis of MCM-41 and MCM-48 which are a series of mesoporous materials named as M41 group was introduced by researchers of Mobile Corporation, and researchers of Santa Barbara independently synthesized mesoporous material named as SBA-15 from layered material similar with the MCM-41.

These materials are mesoporous material in which meso-pores with uniform diameter from 2 nm to 10 nm are arranged regularly. These mesoporous materials have large surface area (700-1500 m/g) as well as chemical and thermal stability, and porous molecular sieve substance has regularly arranged micro pore with uniform size to separate and adsorb molecular level substance selectively and has advantage capable of controlling molecules in the pore to be widely used as a catalyst and a carrier for the catalyst.

In addition, other series of synthesizing methods for mesoporous material such as MSU, FSM can be exampled. Most mesoporous materials have particle size at micro scale, and mesoporous silica nanoparticles capable of arranging regularly and controlling particle shape have been synthesized in recent research.

A synthesizing method of Professor Victor Lin of Iowa State University is based on MCM-41 method, in which CTAB (Cetyltrimethylammonium bromide) is used as a surfactant in alkali state, Organotrimethoxysilane of ionize function group and TEOS (tetraethylorthorsilicate) are supplied followed by Sol-gel synthesis, thereby manufacturing mesoporous silica nanoparticles of nano-size.

Since this method of manufacturing mesoporous silica, however, needed stirring a mixed solution of acid and water followed by transferring to steel bomb and aging in closed system, there were problems that mass production was difficult and process time was much required.

SUMMARY

Embodiments of the inventive concept provide an apparatus of manufacturing mesoporous silica including: a mount; a reactor rotatably coupled to the mount, in which a mixed solution of surfactant, water and acid is to be poured; an impeller installed to the reactor and rotating to stir the mixed solution; and a heating unit installed to cover an outer surface of the reactor, thereby heating the reactor.

The reactor may include a cylindrical main body; a supporter coupled to a bottom surface of the main body; and a reactor cover covering a top surface of the main body.

Shafts may be respectively coupled on both sides of an upper portion of the main body, and the shafts may extend along a horizontal direction. A pair of brackets may be installed to the mount, and shafts may be inserted in the brackets, respectively.

A stopper may be formed to protrude from a bottom surface of the supporter. A coupling plate may be installed to the mount and may be coupled with the stopper to fasten the reactor to the mount.

A lifting apparatus may be installed on the mount. The lifting apparatus may apply external force to the reactor in order to rotate the reactor around the shaft.

The lifting apparatus may include: a pulley installed on the mount; a wire wound around pulley and connected to the reactor; and a rotation motor rotating the pulley.

The impeller may include: a rotation axis installed on the reactor cover; an impeller motor installed on an upper end portion of the rotation axis; and a blade installed on a lower end portion of the rotation axis.

A height adjusting apparatus may be installed on the mount. The height adjusting apparatus may be coupled to the impeller thereby moving the impeller vertically.

The height adjusting apparatus may include: a guide bar vertically installed on the mount; a slider coupled to the guide bar and movable in a vertical direction; and a connector connecting the slider and the impeller.

The heating unit may include: an inner case covering an outer surface of the main body; an outer case covering the inner case; and a heating line installed on an inner surface of the outer case.

A temperature sensor may be installed at the reactor cover and may extend into the reactor to detect temperature.

An ageing cap may be installed on the reactor cover. The ageing cap may close the reactor for ageing process of the mixed solution after removing the impeller.

A drain cap may be installed on the reactor cover. The drain cap may draw off the mesoporous silica after removing the aging cap.

An embodiment of the inventive concepts provides a method of manufacturing mesoporous silica including: pouring a mixed solution of surfactant, acid and water into a reactor after fastening the reactor on a mount; heating the reactor using a heating unit and simultaneously operating an impeller to stir the mixed solution; installing an ageing cap on a reactor cover to completely close the interior of the reactor after removing the impeller from the reactor cover; and heating the reactor by the heating unit to increase inner pressure of the reactor and to raise temperature of the mixed solution to perform the ageing of the mixed solution.

The method may further include rotating the reactor on the mount to draw off the mesoporous silica through a drain.

The method may further include adjusting height of the impeller in order to immerse a blade of the impeller in the mixed solution before the mixed solution is stirred by the impeller.

DETAILED DESCRIPTION OF THE EMBODIMENTS

The inventive concepts will now be described more fully hereinafter with reference to the accompanying drawings, in which exemplary embodiments of the inventive concepts are shown. The advantages and features of the inventive concepts and methods of achieving them will be apparent from the following exemplary embodiments that will be described in more detail with reference to the accompanying drawings. It should be noted, however, that the inventive concepts are not limited to the following exemplary embodiments, and may be implemented in various forms. Accordingly, the exemplary embodiments are provided only to disclose the inventive concepts and let those skilled in the art know the category of the inventive concepts. In the drawings, embodiments of the inventive concepts are not limited to the specific examples provided herein and are exaggerated for clarity.

FIG. 1is a perspective view illustrating an overall structure of an apparatus of manufacturing mesoporous silica according to an embodiment of the inventive concepts.FIG. 2is a lower perspective view illustrating an apparatus of manufacturing mesoporous silica according to an embodiment of the inventive concepts.FIG. 3is a perspective view illustrating a state where a reactor and a heating unit are disjointed from the apparatus ofFIG. 1.FIG. 4is a top view illustrating an apparatus of manufacturing mesoporous silica according to an embodiment of the inventive concepts.FIG. 5is a side view illustrating an apparatus of manufacturing mesoporous silica according to an embodiment of the inventive concepts.

As shown inFIGS. 1 to 5, an apparatus of manufacturing mesoporous silica according to an embodiment of inventive concepts may include a mount100, a reactor200, an impeller300and a heating unit400.

The mount100is a part for shaping entire appearance of the apparatus of manufacturing mesoporous silica. The mount100has structure of interconnecting metal frames.

A plurality of wheels is mounted on the lower part of the mount100such that an operator can move the mount to predetermined position by hands.

The reactor200may be installed to the mount100, and a mixed solution of surfactant for manufacturing mesoporous silica, water and acid may be to be poured in the reactor200.

The surfactant may be polyalkylene oxide block copolymer, for example polyethylene oxide-block-polypropylene oxide-polyethylene oxide. The surfactant may be available from Pluronic P123 of BASF Corporation. The acid act as a catalyst, for example hydrochloric acid may be available.

Further, a silica precursor and a transition metal salt may be further added to the mixed solution. A variety of silica precursors well known in this field may be available, for example TEOS (TetraEthylOrthoSilicate). At least one of titanium, vanadium, chrome, manganese, iron, cobalt, nickel, copper or zinc may be selected. Then, the transition metal salt may be nitrate, hydrochloride, acetate, sulfate, carbonate, oxide or hydroxide of these transition metals.

As shown inFIG. 3, the reactor200may include a cylindrical main body210, a supporter220coupled to the bottom surface of the main body210and a reactor cover230covering the top surface of the main body210.

The reactor200is not limited to this structure, and can be implemented in various forms. For example, the main body210and the supporter may be in one body. The reactor200may be rotatably coupled to the mount100.

Shafts211may be respectively coupled to both sides of an upper portion of the main body210to extend horizontally, a pair of brackets120where the shafts211are respectively inserted may installed on the mount100.

When the reactor200is pushed or pulled by external force, the shaft211is rotated while being inserted in the bracket120, thereby the reactor200can be rotated on the mount100.

If the reactor200is installed rotatably to the mount100, it is available that the mesoporous silica formed in the reactor200be easily drawn off by rotating the reactor after stirring process by the impeller200and ageing process under pressurizing and heating condition. This will now be described more fully hereinafter.

There are accident hazards if the reactor200is vibrated or rotated during the stirring and the ageing processes. Thus, the reactor200may be fastened on the mount100during the stirring and ageing processes.

So, a stopper221may be installed to protrude on the bottom surface of the supporter220, and a coupling plate130may be installed on the mount100. The coupling plate130is coupled with the stopper221to fasten the reactor200on the mount100.

Therefore, the operator couples the stopper221to the coupling plate130thereby the reactor200is fastened on the mount during the stirring and ageing processes, and release the stopper221from the coupling plate130thereby the reactor200can be rotated on the mount100when the mesoporous silica is drawn off from the reactor200after the stirring and ageing processes.

Since the reactor200is manufactured to have a size capable of containing the mixed solution over 20 liter, the weight is not light. And, it is difficult for the operator to rotate the reactor200directly because the reactor200is heated by a heating unit400.

Thus, a lifting apparatus500may be installed on the mount100. The lifting apparatus500may apply external force to the reactor200thereby the reactor200turns on the shaft211.

The lifting apparatus500may include, as shown inFIG. 1, a pulley520installed on the mount100, a wire wound around the pulley520and connected to the reactor200and a rotation motor530rotating the pulley520to wind the wire510.

The stopper221is removed from the coupling plate130and then the wire510is connected to the bottom portion of the reactor200, for example the supporter220or the stopper221followed by operating the rotation motor530to wind the wire510by the pulley520, thereby the reactor200may be tilted by tensile force of the wire510to pivot on the shaft211.

The impeller300may be installed at the reactor200to play a part of stirring the mixed solution.

The impeller300may include a rotation axis310installed at the reactor cover, an impeller motor320installed on the top end of the rotation axis310and a blade330installed on the bottom end of the rotation axis310.

If the impeller320starts operation to rotate the rotation axis310, the blade330located in the reactor200are rotating with the rotation axis310to stir the mixed solution uniformly.

A height adjusting apparatus600is installed on the mount100. The height adjust apparatus600is coupled to the impeller thereby moving the impeller300vertically.

If solution level in the reactor200is low such that the blade330is not immersed in the mixed solution330, the blade330runs idle in the reactor200to cause abnormal stirring process. Thus, it is necessary that the height adjusting apparatus500for vertically moving the impeller300is additionally installed on the mount100to adjust height of the impeller300according to amount of the mixed solution poured in the reactor200.

The height adjusting apparatus600may include a guide bar610installed in vertical direction on the mount100, a slider620coupled vertical movably on the guide bar610and a connector630connecting the slider620and the impeller300.

When the mixed solution is poured in the reactor insufficiently, the slider620is vertically descended along the guide bar610to have the impeller300connected with the connector630lowered such that the blade300located in the reactor200is immersed in the mixed solution. It is a matter of cause that the slider620can be ascended to move up the height of the impeller300as occasion demands.

The heating unit400is installed to cover the outer surface of the reactor200to play a role for heating the reactor200.

The stirring process by the impeller300and the ageing process performed after the stirring process may be implemented at different temperatures each other. Specifically, the stirring process by the impeller300may be performed at 30° C. to 50° C., and the ageing process may be performed at 110° C. to 130° C.

Thus, the heating unit400may heat the reactor200until temperature of the mixed solution in the reactor becomes 30° C. to 50° C., and then heat the reactor200until 110° C. to 130° C. during the ageing process.

As shown inFIG. 2, the heating unit400may include an inner case410covering an outer surface of the main body210, an outer case420covering the inner case410and a heating line430installed on an inner surface of the outer case420.

Thus, power is supplied to the heating line430, and then heat generated by the heating line430is transferred through the inner case420to the reactor200, that is to say, main body210thereby heating the mixed solution at predetermined temperature.

A temperature sensor700may be installed at the reactor cover230. The temperature sensor700may extend into the main body210to measure temperature of the mixed solution. The temperature of the mixed solution can be confirmed in real time such that the mixed solution can be maintained at even temperature during the stirring and ageing process.

FIG. 6is a perspective view illustrating structure of an aging cap and a drain cap according to an embodiment of the inventive concepts.

The ageing process may be performed heating and pressurizing condition that the reactor200is heated by the heating unit400while closing the interior of the reactor200. Thus, if the stirring process is complete, the impeller300is removed from the reactor cover230and an ageing cap800shown inFIG. 5is installed on the reactor cover230thereby closing the reactor200.

After completing the ageing process, as described above, the reactor is tilted on the mount100to draw off the mesoporous silica from the reactor200for the purpose of following process such as cleaning and drying.

In this time, after removing the ageing cap800from the reactor cover230, a drain cap shown inFIG. 6(b)which has a drain910extending into the reactor200is installed at the reactor cover230such that the mesoporous silica may draw off through the drain910.

The notation C is a controller which drives the impeller motor320, the heating unit400and the rotation motor530.

The process for manufacturing the mesoporous silica using the apparatus of manufacturing the mesoporous silica according to the embodiments of the inventive concept will be described hereinafter.

First of all, the stopper221is coupled at the coupling plate130to fasten the reactor200on the mount100followed by pouring the mixed solution of surfactant, acid and water. Transition metal salt and silica precursor may be added to the mixed solution.

While maintaining the mixed solution at 30° C. to 50° C. by heating the reactor200using the heating unit400, the impeller300is driving to stir the mixed solution.

The height of the impeller300may be adjusted according to amount of the mixed solution which is poured in the reactor200in order that the blade330of the impeller stirring the mixed solution is immersed in the mixed solution.

After removing the impeller300from the reactor cover230, the ageing cap800is installed at the reactor cover230to close completely the interior of the reactor200.

The reactor200is heated by the heating unit400to increase inner pressure of the reactor200and simultaneously raise temperature of the mixed solution until 110° C. to 130° C. such that the mixed solution is aged in heating and pressurizing condition.

After forming the mesoporous silica in the reactor200by the aging process, the ageing cap800may be removed from the reaction cover230followed by installing the drain cap900with drain910at the reactor cover230.

After removing the stopper221from the coupling plate130, the reactor is pivoted on the mount100such that the mesoporous silica draws off through the drain910.

The pivoting of the reactor200may be implemented naturally if the wire510wound around the pulley520is connected to the bottom end of the reactor200followed by rotating the pulley520to be winding the wire510.

Finally, the mesoporous silica which was drawn off is filtered and cooled at room temperature followed by cleaning with water, and then cleaned mesoporous silica is dried and calcined to manufacture the mesoporous silica with meso-pores.

According to the embodiments of the inventive concept, the stirring and ageing process is sequentially processed in the reactor, and more specifically the heating unit heats the reactor at the temperatures necessary for the stirring and ageing process sequentially. Thus, time for manufacturing process can be steeply reduced without transferring the mixed solution by processes like conventional arts.

Further, according to the embodiments of the inventive concept, the capacity of the reactor can be increased as occasion demands to manufacture the mesoporous silica in large quantities.