High-solid-content high-purity silica sol and preparation method thereof

A silica sol, high solid content technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of low solid content of silica sol, long concentration cycle, high cost, etc., and achieve low cost and short concentration cycle , the effect of high production efficiency

Active Publication Date: 2017-12-08
河北硅研电子材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the problems of long concentration cycle, high cost, low solid content and low purity of the prepared silica sol in the prior art, the present invention provides a high-solid high-purity silica sol and a preparation method thereof

Method used

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Examples

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preparation example Construction

[0030] In one embodiment, the preparation method at least includes the following steps:

[0031] (1) Take 45-50% ultrapure water, add part of low-molecular alcohol and pH regulator, heat up and stir to obtain solution A, wherein the molar ratio of low-molecular alcohol and pH regulator is 6-30: 0.01-0.1;

[0032] (2) Mix the remaining low-molecular-weight alcohol with part of the silicate, heat and stir to obtain solution B, wherein the molar ratio of the low-molecular-weight alcohol to the silicate is 1-10:5-15;

[0033] (3) Add solution B to solution A, keep warm and react to obtain solution C; distill and rehydrate the obtained solution C with perhydrogenated cation exchange resin, then carry out temperature rise reaction to obtain solution D, wherein the amount of water used for rehydration treatment 50%-60% of the remaining ultrapure water;

[0034] (4) Take 50%-60% of the remaining silicate, heat it up, add it to solution D, keep warm to react, and get solution E; use ...

Embodiment 1

[0045] A high-solid high-purity silica sol, comprising the following raw material components in molar numbers:

[0046] n-butanol 51 mol;

[0047] Organic amine 0.1 mol;

[0048] Methyl silicate 28 mol;

[0049] Deionized water 120mol.

[0050] The preparation method comprises the following steps:

[0051] (1) Take 45% ultrapure water, add 50mol n-butanol and 0.1mol organic amine, heat up to 40°C, and stir at 200r / min for 20min to obtain solution A;

[0052] (2) Mix 1mol n-butanol and 6mol methyl silicate, heat up to 40°C, stir at 200r / min for 20min to obtain solution B;

[0053] (3) Add solution B to solution A, react at 40°C for 4 hours to obtain solution C; distill and replenish 33 mol of solution C with perhydrogenated cation exchange resin, raise the temperature to 40°C, and react for 1 hour to obtain solution D;

[0054](4) Take 11 mol of methyl silicate, raise the temperature to 40°C, add it to solution D, react at 40°C for 4 hours, and obtain solution E; distill a...

Embodiment 2

[0057] A high-solid high-purity silica sol, comprising the following raw material components in molar numbers:

[0058] Isopropanol 62 mol;

[0059] Ammonia 0.2 mol;

[0060] Ethyl silicate 34 mol;

[0061] Deionized water 120mol.

[0062] The preparation method comprises the following steps:

[0063] (1) Take 50% ultrapure water, add 60mol isopropanol and 0.2mol pH regulator, heat up to 80°C, stir at 100r / min for 10min, and obtain solution A;

[0064] (2) Mix 2mol of isopropanol and 10mol of ethyl silicate, heat up to 80°C, stir at 100r / min for 10min, and obtain solution B;

[0065] (3) Add solution B to solution A, react at 80°C for 0.5h to obtain solution C; distill the obtained solution C with a perhydrogenated cation exchange resin, add 30 mol of water, and raise the temperature to 80°C to obtain solution D;

[0066] (4) Take 12mol of ethyl silicate, raise the temperature to 80°C, add it to solution D, react at 80°C for 0.5h, and obtain solution E; distill and add 30...

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Abstract

The invention relates to the technical field of synthesis of inorganic nanomaterials and particularly discloses high-solid-content high-purity silica sol and a preparation method thereof. The high-solid-content high-purity silica sol is prepared from the raw material ingredients by mole number: 31mol to 160mol of low-molecular-weight alcohol, 0.05mol to 0.5mol of pH regulator, 25mol to 95mol of silicate and 120mol to 250mol of deionized water. The high-solid-content high-purity silica sol provided by the invention is high in purity, high in primary solids, short in concentration cycle, low in cost and high in production efficiency.

Description

technical field [0001] The invention relates to the technical field of synthesis of inorganic nanomaterials, in particular to a high-solid high-purity silica sol and a preparation method thereof. Background technique [0002] Silica sol is a dispersion of nano-sized silica particles in water or a solvent. At present, in the industry, the silica sol with a mass fraction greater than 30% and a colloidal particle size greater than 20nm is called a large particle size and high concentration silica sol. Colloidal particles with large particle size and high concentration of silica sol have a large specific surface area (surface multi-mesoporous structure), super adsorption capacity, strong stability and bonding performance, and can form a strong film in chemical mechanical polishing , not prone to cracking. The larger the particle size of the silica sol, the greater the friction coefficient when the silica sol is attached to the solid surface, thereby improving the wear resistan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/145
CPCC01B33/145C01P2006/80
Inventor 朱斌仵靖
Owner 河北硅研电子材料有限公司
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