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Mesoporous silica particles and production process thereof

a technology of mesoporous silica and production process, which is applied in the direction of silicon oxides, silicon compounds, coatings, etc., can solve the problems of reduced material value, difficult to use it as catalyst support or separation agent, and uniform mesopore size, etc., and achieves high yield and efficient production

Inactive Publication Date: 2005-02-03
TOKUYAMA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0011] It is an object of the present invention to provide a process capable of obtaining mesoporous silica particles having a particle diameter in a submicron order at a high yield without causing the marked collapse of mesopores and of producing them efficiently by using an ordinary pulverizer.
[0012] It is another object of the present invention to provide mesoporous silica particles having a particle diameter in a submicron order, a satisfactory mesopore volume and uniformity in mesopore diameter.

Problems solved by technology

However when mesoporous silica is pulverized into fine particles, mesopores that are the greatest feature of mesoporous silica collapse, resulting in a greatly reduced value as a material.
Since mesoporous silica produced by the above process contains the cationic resin for the prevention of the collapse of its mesoporous structure, its application is limited and there is a problem with uniformity in mesopore size due to a wide mesopore distribution.
Therefore, it is difficult to use it as a catalyst support or separating agent which is used for a specific-sized substance.

Method used

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  • Mesoporous silica particles and production process thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0116] A block copolymer of ethylene glycol and propylene glycol (Pluronic-P123 of BASF Co., Ltd.) was dissolved in ion exchange water to prepare a 20 wt % surfactant solution. 150 g of the surfactant solution, 44 g of 25 wt % sulfuric acid and 73 g of ion exchange water were mixed together to prepare a transparent solution. 133 g of sodium silicate (containing 15 wt % of SiO2 and 5.1 wt % of Na2O) was added dropwise to this solution under stirring to obtain a cloudy reaction mixture. The pH of the reaction mixture was 2.7.

[0117] The reaction mixture was maintained at 30° C. for 1 hour under stirring, heated at 95° C. and maintained at that temperature for 12 hours to produce mesoporous silica particles having the surfactant existent in mesopores.

[0118] Thereafter, a polyethylene pot was filled with 390 g of the above reaction mixture and 1,520 g of zirconia balls having a diameter of 2 mm and sealed up without a dead volume in the pot to wet pulverize the mixture with a pot mill....

example 2

[0135] A block copolymer of ethylene glycol and propylene glycol (Pluronic-F127 of BASF Co., Ltd.) was dissolved in ion exchange water to prepare a 10 wt % surfactant solution. 210 g of the surfactant solution, 59 g of 25 wt % sulfuric acid and 291 g of ion exchange water were mixed together to prepare a transparent solution. 140 g of sodium silicate (containing 15 wt % of SiO2 and 5.1 wt % of Na2O) was added dropwise to this solution under stirring to obtain a cloudy reaction mixture. The pH of the reaction mixture was 1.0.

[0136] The reaction mixture was maintained at 30° C. for 10 hours under stirring, heated at 80° C. and maintained at that temperature for 12 hours to produce mesoporous silica particles having the surfactant existent in mesopores.

[0137] Thereafter, part of the solution was removed from the above reaction mixture by decantation, and the content of the mesoporous silica particles in the reaction mixture was adjusted to 5 wt %.

[0138] A polyethylene pot was filled...

example 3

[0155] A block copolymer of ethylene glycol and propylene glycol (Pluronic-P123 of BASF Co., Ltd.) was dissolved in ion exchange water to prepare a 20 wt % surfactant solution. 100 g of the surfactant solution, 44 g of 25 wt % sulfuric acid and 123 g of ion exchange water were mixed together to prepare a transparent solution. 133 g of sodium silicate (containing 15 wt % of SiO2 and 5.1 wt % of Na2O) was added dropwise to this solution under stirring to obtain a cloudy reaction mixture. The pH of the reaction mixture was 2.7.

[0156] The reaction mixture was maintained at 30° C. for 10 hours under stirring to produce mesoporous silica particles having the surfactant existent in mesopores.

[0157] Thereafter, a polyethylene pot was filled with 390 g of the above reaction mixture and 1,520 g of zirconia balls having a diameter of 2 mm and sealed up without a dead volume in the pot to wet pulverize the mixture with a pot mill. The amount of the surfactant existent in the mesopores was 100...

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Abstract

A process for wet pulverizing mesoporous silica particles while a surfactant exists in mesopores, and mesoporous silica particles having an average particle diameter of 1 μm or less, wherein the volume of mesopores having a diameter of 2 to 50 nm is 0.7 mL / g or more and the geometric standard deviation of a mesopore distribution is 2.0 or less. In the above process, mesoporous silica particles having a particle diameter in a submicron order can be obtained at a high yield without causing the marked collapse of mesopores and can be produced efficiently by using an ordinary pulverizer and safely by using an aqueous medium. The mesoporous silica particles having an average particle diameter of 1 μm or less are useful as an ink absorbent for ink jet recording paper, low-dielectric film, catalyst support, separating agent, adsorbent and medical carrier for medicines.

Description

FIELD OF THE INVENTION [0001] The present invention relates to mesoporous silica and a production process thereof. More specifically, it relates to mesoporous silica particles having a particle diameter in a submicron order and useful as a catalyst support, separating agent, adsorbent, low-dielectric film or ink absorbent for ink jet recording paper and to a process for producing the above particles efficiently at a high yield. DESCRIPTION OF THE PRIOR ART [0002] Mesoporous silica is a new material having pores with a diameter of 2 to 50 nm (to be referred to as “mesopores” hereinafter) and expected to be used in various fields such as catalyst support and separating agents. Like other inorganic materials, it is preferably in the form of fine particles in most cases when it is actually used. [0003] For example, when it is used as thin film like an ink absorbent for ink jet recording paper or low-dielectric thin film, to obtain a flat homogeneous film, mesoporous silica must be parti...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B41M5/52C01B33/18C01B33/12C01B33/193
CPCB41M5/5218C01B33/193C01B33/18C01B33/12
Inventor FUKUDA, KENTAROFUKUNAGA, KENJIYAMASHITA, HIROYA
Owner TOKUYAMA CORP
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