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Method for preparing particle diameter homogeneous polysilicon oxide microsphere with active group

An active and oxide technology, applied in the field of chemistry and materials, can solve the problems of poor reproducibility, non-uniform particles, difficult to apply to the production field, etc., to achieve the effect of simple operation, short production cycle and low cost

Inactive Publication Date: 2008-05-28
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Such as Robert I. Nooney, Dhanasekaran Thirunavukkarasu, Yimei Chen, Robert Josephs, and Agnes E. Ostafin "synthesis of Nanoscale Mesoporous Silica Spheres with Controlled Particle Size" ("Chem. Mater." 14 (11), 4721-4728, 2002) , however, the particles obtained by these methods are not very uniform, and the reproducibility is not good
Chinese patent CN 87106208A discloses a process method for manufacturing porous silica spheres with uniform particle size, but the surface of silica prepared by this method has not been modified by functional groups, so it is difficult to apply to specific production fields

Method used

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  • Method for preparing particle diameter homogeneous polysilicon oxide microsphere with active group
  • Method for preparing particle diameter homogeneous polysilicon oxide microsphere with active group
  • Method for preparing particle diameter homogeneous polysilicon oxide microsphere with active group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 500 moles of absolute ethanol and 2.5 liters of 30% ammonia water in proportion to the polytetrafluoroethylene liner reactor, and stir for 5 minutes at room temperature. Mix 10 moles of ethyl orthosilicate and 15 moles of n-octyltriethoxysilane at room temperature, and then slowly add them from the feeding port to the above-mentioned reactor and stir and mix at a speed of 300 rpm to make the mixture evenly mixed. The reaction is uniform. The reaction temperature is controlled at about 25°C for a constant temperature reaction for about 5 hours.

[0032] After the reaction is completed, the mixture in the kettle is filtered and washed with deionized water for 2 to 3 times. The solid particles are washed with toluene or tetrahydrofuran for 2 to 3 times. The resulting filter cake is dried in an oven at 100°C for two hours to obtain a powder. It is octyl functionalized polysilicon oxide particles. The powder is placed in a muffle furnace at a constant temperature of about 30...

Embodiment 2

[0034] Add 500 moles of absolute ethanol and 2.5 liters of 30% ammonia water in proportion to the polytetrafluoroethylene liner reactor, and stir for 5 minutes at room temperature. Mix 10 moles of ethyl orthosilicate and 2 moles of aminopropyltriethoxysilane at room temperature, and then slowly add them to the above-mentioned reaction kettle from the feeding port and stir and mix at a speed of 300 rpm to make the mixture evenly mixed. The reaction is uniform. The reaction temperature is controlled at about 25°C for a constant temperature reaction for about 5 hours.

[0035] After the reaction is completed, the mixture in the kettle is filtered and washed with deionized water 2 to 3 times, and the solid particles are washed with toluene or tetrahydrofuran 2 to 3 times. The resulting filter cake is dried in an oven at 80°C for two hours to obtain a powder. It is an aminopropyl functionalized polysilicon oxide particle. The powder is placed in a muffle furnace at a constant temperatu...

Embodiment 3

[0037] Add 250 moles of absolute ethanol and 2.5 liters of 30% ammonia water in proportion to the reaction kettle with a polytetrafluoroethylene liner, and stir for 5 minutes at room temperature. Mix 5 moles of potassium silicate, 5 moles of ethyl orthosilicate and 5 moles of vinyl triethoxy silane at room temperature, and then slowly add them from the feed port to the above-mentioned reactor at 300 revolutions per minute. Stir and mix at speed to make the reaction uniform. The reaction temperature is controlled at about 25°C for a constant temperature reaction for about 5 hours.

[0038]After the reaction is completed, the mixture in the kettle is filtered and washed with deionized water for 2 to 3 times. The solid particles are washed with toluene or tetrahydrofuran for 2 to 3 times. The resulting filter cake is dried in an oven at 80°C for two hours to obtain a powder. It is vinyl functionalized polysilicon oxide particles. The powder is placed in a muffle furnace at a constant...

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Abstract

The invention discloses a preparation method of a polysilicon oxide microsphere with active groups, which comprises the steps that (1) ethanol, catalyst and deionized water are evenly mixed and are added with four silicone monomer and three silicone monomer; the obtained solution is evenly stirred and mixed, and then mixture reacts for 3 to 20 hours at the temperature of -5 to 100 DEG C; (2). the obtained solution from step (1) is filtrated, and the obtained cake is washed by deionized water, toluene or tetrahydrofuran, then is dried to get the finished product, polysilicon oxide microsphere. The method of invention is simple in operation, low in cost and short in production period. The polysilicon oxide microsphere can be widely applied to such fields as catalyst carrier, filler of chromatographic column, substrate for fixing enzyme, insulation device, carrier for control released drug and other chemical products, adsorbent, filler, cigarette filtration material and other application on filtration and separation.

Description

Technical field [0001] The invention relates to the technical field of chemistry and materials, and in particular to a method for preparing spherical polysilicon oxide microspheres with active groups with uniform particle size. Background technique [0002] Homogeneous catalysis heterogeneity is the most practical and potential application research field in materials research. The existing method is mainly to support catalyst immobilization, which firstly requires functionalization of the carrier surface, that is, grafting organic groups onto hydroxyl-terminated silica to give the carrier new properties, such as improving the adsorption and separation of silica Aspects of performance, enhance the compatibility of oxides and organic dispersion media, improve the process performance of silica, etc. [Du Zuodong. Organosilicon Chemistry. Beijing: Higher Education Press, 1990.]. This method of grafting groups is difficult to chemically bond to the surface of some organic monomers with...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/113B01J13/00B01J20/10
Inventor 王惠钢郏建军何丽
Owner ZHEJIANG SCI-TECH UNIV
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