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Method for preparing controllable monodisperse spherical large-particle-size nano-silicon dioxide

A nano-silicon dioxide and silicon dioxide technology, applied in the direction of silicon dioxide, silicon oxide, etc., can solve the problems of small particle size and can not meet the size requirements of shear thickening liquid, and achieve high production efficiency and single particle size. Excellent dispersibility and easy post-processing

Active Publication Date: 2014-08-27
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the patent, nano-silica particles with good regularity of 8-15nm are prepared. The particle size provided by this patent is small, which cannot meet the particle size requirements for the preparation of shear thickening liquid.

Method used

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  • Method for preparing controllable monodisperse spherical large-particle-size nano-silicon dioxide
  • Method for preparing controllable monodisperse spherical large-particle-size nano-silicon dioxide
  • Method for preparing controllable monodisperse spherical large-particle-size nano-silicon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Disperse a certain amount of ammonia water in the ethanol solution, the molar ratio of ethanol to ammonia water is 16:1, disperse evenly with electric stirring, add tetraethyl orthosilicate in the mixed solution, control the dropping rate to 25ml / min, TEOS and h 2 O molar ratio is 1:5.

[0041] (2) At room temperature, control the stirring speed to 650r / min, react for 5h, and obtain the silica sol.

[0042] (3) Add TEOS step by step to the silica sol obtained in step (2), control 650r / min constant speed stirring, add TEOS dropwise to the constant pressure funnel, control the dropping rate to 25ml / min, and add The molar ratio of TEOS is 1:2, and it is added at one time. After the dropwise addition is completed, it is controlled to stir at a constant speed of 650r / min and react for 4h.

[0043] (4) The reactant obtained in step (3) is centrifuged, the supernatant is removed, and the centrifuge is redispersed in acetone. Repeat the dissolution and separation operati...

Embodiment 2

[0049] (1) Disperse a certain amount of ammonia water in the ethanol solution, the molar ratio of ethanol to ammonia water is 13:1, disperse evenly with electric stirring, add tetraethyl orthosilicate in the mixed solution, control the dropping rate to 20ml / min, TEOS and h 2 O molar ratio is 1:4.

[0050] (2) At room temperature, control the stirring speed to 600r / min, react for 5h, and obtain the silica sol.

[0051] (3) Add TEOS step by step to the silica sol obtained in step (2), control the stirring speed at 600r / min, add TEOS dropwise through the constant pressure funnel, control the rate of addition to be 20ml / min, and add TEOS with step (1). The molar ratio of TEOS was 1:1, and it was added in two times. After each dropwise addition, the stirring speed was controlled to 600r / min and stirred at a constant speed, and the reaction was carried out for 3h.

[0052] (4) The reactant obtained in step (3) is centrifuged, the supernatant is removed, and the centrifuge is redis...

Embodiment 3

[0057] (1) Disperse a certain amount of ammonia water in the ethanol solution, the molar ratio of ethanol to ammonia water is 11:1, electric stirring is used to disperse evenly, and ethyl orthosilicate is added to the mixed solution, and the dropping rate is controlled to be 40ml / min, TEOS and h 2 O molar ratio is 1:6.

[0058] (2) At room temperature, control the stirring speed to 700r / min, react for 6h, and obtain silica sol.

[0059] (3) Add TEOS step by step in the silica sol obtained in step (2), control the stirring speed at 700r / min, add TEOS dropwise to the constant pressure funnel, control the rate of addition to be 40ml / min, and add in the step (1) The molar ratio of TEOS is 2:1, and it is added three times. After each dropwise addition, the stirring speed is controlled to 700r / min to stir at a constant speed, and the reaction is carried out for 2h.

[0060] (4) The reactant obtained in step (3) is centrifuged, the supernatant is removed, and the centrifuge is redi...

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Abstract

The invention relates to a method for preparing controllable monodisperse spherical large-particle-size nano-silicon dioxide. According to the method, on the basis of the Stober sol-gel method, tetraethoxysilane hydrolyzes to obtain orthosilicic acid, and dehydration synthesis is carried out through the method for replenishing tetraethoxysilane intermittently to obtain silicon dioxide. The method is simple in technological process, moderate in condition, high in production efficiency and suitable for industrial production, and the post-treatment mode is easy and convenient to perform. By replenishing the reagent intermittently, the large-particle-size nano-silicon dioxide particles can be synthesized in a controllable mode. The nano-silicon dioxide particles obtained through the preparation method have the advantages of being regular in spherical shape, excellent in monodispersity and the like.

Description

Technical field: [0001] The invention relates to a method for preparing controllable monodisperse spherical large particle size nano-silica, which utilizes Controllable synthesis of spherical SiO with excellent monodispersity by sol-gel method combined with intermittent addition of reactants 2 Particles belong to the field of nanomaterial synthesis. Background technique: [0002] In recent years, nano-silica particles have been widely studied in scientific research and industrial fields. Among them, nano-silica can be used in the preparation of shear thickening fluid and in the research of soft body armor. Shear thickening fluid is generally obtained by dispersing a certain concentration of solid particles in a liquid. Shear thickening fluid generally consists of a two-phase dispersion system, one phase is composed of nanoparticles, such as silica, calcium carbonate, PMMA particles, etc., and the other phase is a carrier fluid, such as water, polyethylene glycol, etc., d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
Inventor 吴丝竹赵爽吴友平赵秀英
Owner BEIJING UNIV OF CHEM TECH
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