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Spherical silicon dioxide granule preparation method

A technology of spherical silica and silica, applied in the direction of silica, silica, chemical instruments and methods, etc., can solve problems such as difficult to obtain products and harsh experimental conditions, achieve uniform particle size, shorten polymerization time, Effect of Particle Size Homogenization

Active Publication Date: 2007-06-06
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the defect that it is difficult to obtain uniform products with a particle size of more than 2 microns in the preparation of spherical silica particles in the prior art, and the experimental conditions are relatively harsh, thereby providing a functional pore size, particle size and surface base. Preparation method of spherical silica particles with adjustable group and mild conditions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 10ml of tetraethoxysilane (TEOS) after vacuum distillation was dissolved in 20ml of acetone, and 0.75ml of deionized water (0.47) and 0.3ml of 37% (wt) concentrated hydrochloric acid (mol (HCl) / mol(TEOS)=0.068; mol(H2O) / mol(TEOS)=1.17), the formed mixed solution was stirred for 10 min and then heated to 60°C. Stir gently to keep the system slightly boiling for about 1 hour to evaporate the acetone. The temperature of the system was raised to 80°C and kept for 3 hours, and the alkoxysilane was polymerized under the catalysis of hydrochloric acid. The liquid was placed at 140°C and 20mmHg vacuum, and the TEOS monomer and oligomer were evaporated. After the system is down to normal temperature, it is dissolved in acetone to obtain 10ml of solution, and the solution is placed in a membrane emulsification device for emulsification. The external phase is 50ml of 10v% acetone aqueous solution, the average pore diameter of the emulsified membrane is 800nm, and the gas operating...

Embodiment 2

[0023] Dissolve 20 ml of tetraethoxysilane (TEOS) after vacuum distillation in 30 ml of acetone, add 1.5 ml of deionized water and 0.6 ml of 37% (wt) concentrated hydrochloric acid (mol (HCl) / mol (TEOS) under stirring =0.068; mol(H 2 (0) / mol(TEOS)=1.17), the formed mixed solution was stirred for 10 min and then heated to 60° C., and stirred gently to ensure that the system boiled slightly for about 1 hour to distill off the acetone. The temperature of the system was raised to 90°C and kept for 4 hours to polymerize the alkoxysilane under the catalysis of hydrochloric acid, and the liquid was placed at 140°C under a vacuum of 10 mmHg to evaporate TEOS monomers and oligomers. After the system is lowered to normal temperature, it is dissolved in acetone dispersed with 1.5g of polystyrene microspheres with a particle size of 300nm to obtain a 20ml solution, which is placed in a membrane emulsification device for emulsification, and the external phase is 100ml of 20v% acetone aqueo...

Embodiment 3

[0025]Dissolve 40ml of tetraethoxysilane (TEOS) distilled under reduced pressure and 10ml of methyltriethoxysilane (MTES) distilled under reduced pressure in 100ml of acetone, add 4ml of deionized water and 1.5ml of 37 The concentrated hydrochloric acid of % (wt) (mol (HCl) / mol (TEOS+MTES)=0.066, mol (H 2 (0) / mol(TEOS+MTES)=1.2), the formed mixed solution was stirred for 10 min and then heated to 60° C., and stirred gently to ensure that the system boiled slightly for about 1 hour to evaporate the acetone. The temperature of the system was raised to 100° C. and kept for 4 hours, and the alkoxysilane was polymerized under the catalysis of hydrochloric acid. The liquid was placed at 150° C. and a vacuum of 10 mmHg, and monomers and oligomers were evaporated. After the system is lowered to normal temperature, it is dissolved in acetone dispersed with 2.8g of polystyrene microspheres with a particle size of 150nm to obtain a 40ml solution, which is placed in a membrane emulsificat...

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Abstract

The invention discloses a making method of spherical silica particle, which comprises the following steps: dissolving the alkoxy silane in the acetone; adding the deionized water and concentrated alcaine to polymerize at 80-100 deg.c; dissolving the decompressing distilling mucago in the dispersed acetone or alcohol solution with single grain size polystyrene microball; proceeding emulsification in the film emulsification device; adding ammonia, organic amine, hydramine or amine glycol to filter, age and clean the silica microball; igniting the microball at 500-700 deg.c for 3-5 hours; adding surface group modifier in the aggregation step. The invention simplifies the experimental condition to produce different grain sizes of polystyrene microball in the broad scale, which doesn't lead in any metal salt ion to satisfy higher demand occasion of metal ion impurity.

Description

technical field [0001] The invention relates to a preparation method of spherical silica particles, in particular to a preparation method of spherical silica microspheres with adjustable functional aperture, particle diameter and surface groups. Background technique [0002] Silica microspheres with adjustable functional pore size and particle size have been highly valued by researchers because of their wide application prospects in drug controlled release, industrial catalysis and high performance liquid chromatography packing. At present, there are many relatively mature preparation methods of silica microspheres: 1) spray drying method, 2) stacking microsphere method, and 3) Sol-Gel method. In the spray drying method, the particle size of the obtained microspheres is directly affected by the atomization effect of the nozzle, and it is difficult to achieve uniformity. Generally, its products need further particle size classification. The stacked silicon sphere method als...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/16C01B33/145C01B33/146
Inventor 刘海弟陈运法杜尚丰曾冬冬
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI