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A kind of preparation method of high-purity large particle size silica sol

A silica sol, large particle size technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of small silica sol particle size, difficult to control particle size, large dispersion, etc., to achieve large particle size, The effect of short synthesis cycle and fast growth of particle size

Active Publication Date: 2020-10-16
临沂市科翰硅制品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at the problems in the prior art that the silica sol has small particle size, difficult particle size control, large dispersion and poor stability, the present invention provides a preparation method of high-purity large-particle-size silica sol, which can synthesize silica sol with a smaller particle size Silica sol with large size, higher concentration and more uniform particle size distribution can meet the polishing requirements of new devices in the electronics industry

Method used

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  • A kind of preparation method of high-purity large particle size silica sol

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Embodiment 1

[0032] (1) Preparation of sol crystal grains: add 0.5% polyethylene glycol 2000 whose mass is silica sol solution to the acidic silica sol solution, adjust the pH value to 9.7, heat to 100°C, and obtain sol grains with an average particle diameter of 50nm ;

[0033] (2) Preparation of aluminum-modified silicic acid: at 60°C, add acid to activate the resin, wash the resin until the pH is 3.0, add aluminum nitrate and water glass, and the water glass has an average particle size of 9nm through ion exchange reaction, and the stability Good aluminum-modified silicic acid, wherein the addition of aluminum nitrate is 0.3% of water glass weight.

[0034] (3) Preparation of large particle size silica sol: heat the sol grains in step (1) to 100°C, add the aluminum-modified silicic acid prepared in step (2), the flow rate of the aluminum-modified silicic acid is 14mL / min , add sodium hydroxide at the same time, adjust the pH value to 9.6, synthesize while ultrafiltration, and heat reac...

Embodiment 2

[0037] (1) Preparation of sol grains: add 0.5% polyethylene glycol 6000 with a mass of silica sol solution to the acidic silica sol solution, adjust the pH value to 9.7, heat to 100°C, and obtain sol grains with an average particle size of 100nm ;

[0038] (2) Preparation of aluminum-modified silicic acid: at 60°C, add acid to activate the resin, wash the resin until the pH is 3.0, add sodium metaaluminate and water glass, and the water glass has an average particle size of 8 nm through ion exchange reaction. Aluminum-modified silicic acid with good stability, wherein the addition of sodium metaaluminate is 0.3% of water glass weight.

[0039] (3) Preparation of large particle size silica sol: heat the sol grains in step (1) to 100°C, add aluminum-modified silicic acid in step (2), the flow rate of aluminum-modified silicic acid is 12mL / min, and simultaneously Add sodium hydroxide, adjust the pH value to 9.5, synthesize while ultrafiltration, and heat reaction at 100°C for 4 ...

Embodiment 3

[0042] (1) Preparation of sol grains: Add polyethylene glycol 6000 with a mass of 1% of the mass of the silica sol solution to the acidic silica sol solution, adjust the pH value to 9.5, heat and boil, and obtain sol grains with an average particle size of 150 nm;

[0043] (2) Preparation of aluminum-modified silicic acid: at 60°C, add acid to activate the resin, wash the resin until the pH is 4.0, add sodium metaaluminate and water glass, and the water glass undergoes ion exchange reaction to obtain an average particle size of 10nm. Aluminum-modified silicic acid with good stability, wherein the addition of sodium metaaluminate is 0.5% of water glass weight;

[0044](3) Preparation of large particle size silica sol: the sol matrix of step (1) is boiled, and aluminum-modified silicic acid is added in step (2), and sodium hydroxide is added at the same time to adjust the pH value to 9.5, and the silicic acid The flow rate is 10mL / min, synthesized while ultrafiltration, and heat...

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Abstract

The invention discloses a preparation method of high-purity large-particle-size silica sol, which belongs to the technical field of silica sol preparation. The specific preparation method comprises the following steps of mixing an acidic silica sol solution with a pH value of 2-3 with polyethylene glycol 2000-10000, adjusting the pH value to 8-9.5, and heating and boiling to obtain sol crystal grains, adding acid activated resin, washing the resin until the pH value is 3.0-4.5, adding an aluminum salt modifier and water glass, and carrying out ion exchange reaction on the water glass to obtainaluminum modified silicic acid, and adding aluminum modified silicic acid into the sol crystal grains, adding an alkaline solution to adjust the pH value to 9.5-10.5, synthesizing while performing ultrafiltration, and heating to synthesize the high-purity large-particle-size silica sol. The acidic silica sol is subjected to hydroxylation reaction, so that the gel is aggregated to form a large-particle silica sol matrix, the water glass is used as a raw material, the aluminum-modified active silicic acid is prepared by adopting an ion exchange method, ultrafiltration and synthesis are carriedout simultaneously, the particle size is increased quickly, the energy consumption is low, the synthesis period is short, the production efficiency is improved, and the polishing requirements of noveldevices in electronic industry can be met.

Description

technical field [0001] The invention belongs to the technical field of silica sol preparation, and in particular relates to a preparation method of high-purity and large-diameter silica sol. Background technique [0002] Silica sol is a colloidal solution in which amorphous silica particles are dispersed in water. It is a very important inorganic material and is widely used in petroleum catalysis, precision casting, textiles, papermaking, refractory materials, coatings and electronics. According to the pH range of the solution, it can be divided into acidic silica sol and alkaline silica sol, and alkaline silica sol is a stable system. According to colloid theory, the size of silica sol particles is divided into 5-100nm. However, due to the development and progress of silica sol technology, silica sol has broken through the traditional 100nm dividing line, tending to a larger particle size and stable silica sol system. [0003] At present, the preparation methods of silica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/141
CPCC01B33/141C01P2004/32C01P2004/62C01P2006/80
Inventor 康利彬
Owner 临沂市科翰硅制品有限公司
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