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Electronic-grade ultrafine silicon dioxide and preparation method thereof

An ultra-fine silicon dioxide, electronic grade technology, applied in the direction of silicon dioxide, silicon oxide, etc., can solve the problems of not being able to be used as electronic materials, and achieve the effects of easy promotion and implementation, significant economic benefits, and high quality

Active Publication Date: 2014-07-30
FUJIAN SANMING TONGSHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method only examines the technical method for removing sodium ions, and does not consider metal ions such as aluminum, potassium, calcium, magnesium, and copper, which are more stringent in the electronics industry.
And the final product has not been tested for indicators, strictly speaking, it cannot be used as an electronic material. Therefore, we have developed a low-cost, high-quality production method for electronic-grade ultra-fine silicon dioxide

Method used

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  • Electronic-grade ultrafine silicon dioxide and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Prepare sodium silicate into 500g of sodium silicate aqueous solution of 5wt% based on silicon dioxide, weigh 100g of exchanged cation exchange resin and 50g of anion exchange resin, add the sodium silicate solution into the reaction tank, start stirring, at 30°C Add cation exchange resin 50g to carry out exchange reaction, reaction time is 50 minutes, control reaction final pH value is 2; Filter and remove resin, then add anion exchange resin 50g and carry out exchange reaction, reaction time is 50 minutes, reaction final pH value is 8; Filter the formed sol to remove the resin, add 50g of cation exchange resin for exchange reaction, the reaction time is 30 minutes, control the pH value to 5; heat up to 30°C and keep it warm until a gel is formed; wash the gel with deionized water, The conductivity of the washing water is 30 μs / cm; then, it is flash-dried at 200° C., and the dried material is pulverized by a jet mill, with an average particle size of 5.6 microns.

Embodiment 2

[0027] Prepare sodium silicate into 500g of 10wt% sodium silicate aqueous solution based on silicon dioxide, weigh 400g of exchanged cation exchange resin and 200g of anion exchange resin, add the sodium silicate solution into the reaction tank, start stirring, Next, add cation exchange resin 200g to carry out exchange reaction, reaction time is 40 minutes, control reaction final pH value is 3; filter and remove resin, then add anion exchange resin 200g and carry out exchange reaction, reaction time is 30 minutes, reaction final pH value is 9; Filter the formed sol to remove the resin, add 200g of cation exchange resin to carry out the exchange reaction, the reaction time is 30 minutes, and control the pH to 7; heat up to 50°C and keep it until the gel is formed; wash the gel with deionized water, and the conductivity of the washing water The rate is 25 μs / cm; then flash drying is carried out at 250° C., and the dried material is pulverized by a jet mill, with an average partic...

Embodiment 3

[0029] Sodium silicate was formulated into 500g of sodium silicate solution of 12wt% based on silica, weighed 360g of exchanged cation exchange resin and 180g of anion exchange resin, added the sodium silicate solution into the reaction tank, started stirring, and heated at 35°C Add cation exchange resin 180g to carry out exchange reaction, reaction time 30 minutes, control reaction final pH value is 4; Filter and remove resin, then add anion exchange resin 180g and carry out exchange reaction, reaction time 30 minutes, reaction final pH value is 10; Filter the formed sol to remove the resin, add 180g of cation exchange resin for exchange reaction, the reaction time is 30 minutes, control the pH8; heat up to 40°C and keep it until gel is formed; wash the gel with deionized water, and the conductivity of the washing water The rate is 25μs / cm. Then flash drying is carried out at 300°C, and the dried material is pulverized by a jet mill with an average particle size of 10 microns....

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Abstract

The invention provides electronic-grade ultrafine silicon dioxide and a preparation method thereof. The specific technical scheme comprises the following steps: performing exchange reaction on a sodium silicate water solution and cation exchange resin at 30-35 DEG C for 30-60 minutes to form sol, wherein the end point of the reaction is pH 2-4; filtering to remove the resin, then adding anion exchange resin, and performing exchange reaction to form sol, wherein the end point of the reaction is pH 8-10; filtering to remove the resin, adding cation resin again, and performing exchange reaction for 30-60 minutes, wherein the end point of the reaction is pH 5-8; and filtering to remove the resin, then heating to 30-50 DEG C, keeping the temperature until gelation, washing the gel with water, performing expansion drying at 200-300 DEG C, and pulverizing to prepare the electronic-grade ultrafine silicon dioxide.

Description

technical field [0001] The invention belongs to the field of preparation of electrodeless materials, and in particular relates to an electronic-grade ultrafine silicon dioxide and a preparation method thereof. Background technique [0002] Ultrafine silicon dioxide is an X-ray amorphous substance with the molecular formula mSiO 2 ·nH 2 o 2 , with hydroxyl groups distributed on the surface, widely used in textile, paint, paper, rubber, ceramics, precision casting and electronics industries. [0003] At present, the production methods of ultrafine silica include precipitation method, gel method and gas phase method. Among the three methods, due to the high metal impurities of the ultrafine silica prepared by the precipitation method and the gel method, it cannot be used in the electronics industry, and the gas phase method is expensive and acidic, which is corrosive to electronic components. nature, which limits its use. CN101475181A discloses a "preparation method of e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
Inventor 卢元方陈家茂赵晓彬
Owner FUJIAN SANMING TONGSHENG CHEM
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