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Preparation method of alcohol solvent type high-purity silica sol

A technology of alcohol solvent and silica sol, which is applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of long reaction time (tens of hours or even days, cumbersome preparation process, high cost, etc.) and improve quality transfer Efficiency, simple process and easy operation

Inactive Publication Date: 2011-07-13
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above patents have disadvantages such as cumbersome preparation process, high cost, and low product purity; while the traditional Stober method, although silica sol with high purity can be prepared, generally has long reaction time (tens of hours or even days) and one-step preparation of solid Disadvantages of low content (generally less than 1%)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 512g of methanol, 8g of concentrated ammonia water, and 280g of deionized water were made into solution A, which was added to a two-stage reactor as a base material, 210g of methyl orthosilicate and 90g of methanol solution were made into solution B, and the reaction temperature was controlled at 0°C. The stirring speed was controlled at 400 rpm, and then solution B was added to the two-stage reactor at a feed rate of 4ml / min to react with solution A. After the addition was complete, the reaction was continued for 12 hours under stirring.

Embodiment 2

[0027] 340g of methanol, 0.2g of aniline, and 56g of deionized water were made into solution A, which was added to a two-stage reactor as a bottom material, and 340g of methyl orthosilicate and 60g of methanol solution were mixed to make solution B, and the reaction temperature was controlled at 25°C , the stirring speed was controlled at 800 rev / min, and then the solution B was added dropwise to the two-stage reactor at a speed of 20ml / min to react with the solution A. After the addition was completed, the reaction was carried out under stirring conditions for 18h.

Embodiment 3

[0029] 210g of methanol, 1.5g of ethylenediamine, and 60g of deionized water were made into solution A, which was added to a two-stage reactor as a bottom material, and 240g of methyl orthosilicate and 200g of methanol solution were made into solution B, and the reaction temperature was controlled at 45°C, the stirring speed was controlled at 1200 rpm, and then solution B was added to the two-stage reactor at a speed of 40ml / min to react with solution A, and the reaction was carried out under stirring conditions for 24 hours after the addition was completed.

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Abstract

The invention relates to the technical field of nano material preparation, aiming at providing a preparation method of alcohol solvent type high-purity silica sol. The method comprises the following steps: mixing an alcohol solvent, water and a catalyst and then adding the mixture as a base material to a two-stage reactor; and mixing the alcohol solvent and tetramethoxysilane and then adding the mixture in the base material at the feeding speed of 4-40 ml / min under the condition of stirring so as to react for 12-24 hours at the reaction temperature of 0-45 DEG C, thus the solvent type high-purity silica sol is obtained, wherein the solid content of the prepared silica sol is 7-10%, and the average size of the silicon dioxide particle in the silica sol is 8-20 nm. The preparation method is simple in process and is easy to operate, the reaction is controllable, and the distribution of silica sol particles is narrow; the purity of the silica sol is high, the solid content for once preparation is relative high; and aftertetramethoxysilane or tetraethyl orthosilicate is rectified, high-purity silica sol without mental ions can be prepared, and the prepared product is mainly used in the aspect of paints.

Description

technical field [0001] The invention relates to a preparation method of alcohol solvent-type high-purity silica sol, and belongs to the technical field of nanometer material preparation. Background technique [0002] Silica sol is a colloidal solution formed by the uniform diffusion of silica colloidal particles in water, also known as silicic acid solution, and its colloidal particle size is generally 1-100nm. Because the surface of silica particles in silica sol contains a large number of hydroxyl groups, it has greater reactivity, and can be miscible with organic polymers after surface modification, so it is widely used in coatings, precision casting, papermaking, textiles, and petrochemicals. , electronics and other industries. At present, the vast majority of domestic commercialized silica sols are water-based silica sols, which are not as good as solvent-based silica sols in some coating applications. However, the cost of domestic solvent-based silica sols is relative...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/145
Inventor 杨辉阙永生吴春春
Owner ZHEJIANG UNIV
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