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Method of preparing amino modified nanometer silicon micropowder by ambient pressure drying

A technology of nano-silica powder and amino modification, which is applied in the treatment of dyed organosilicon compounds, fibrous fillers, etc., can solve the problems of complex treatment process, achieve simple process, low requirements, and reduce production costs

Inactive Publication Date: 2014-07-16
江苏凯达石英股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the problems existing in the prior art, the present invention proposes a method for preparing amino-modified nano-silicon micropowder by normal pressure drying, so as to overcome the complicated problem of the existing normal pressure drying pretreatment process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Preparation of SiO by silicon powder dissolution method 2 Sol: first soak the industrial-grade silicon powder in hot water at 55°C to activate it, add it to the container containing the sodium hydroxide solution catalyst three times, stir and heat, the reaction temperature is controlled at 80°C, and react until there are no more bubbles SiO can be obtained by standing still and filtering until it is produced 2 Sol;

[0016] (2) Static gel: the SiO prepared in step (1) 2 The sol was left standing for 3h to obtain SiO 2 gel;

[0017] (3) SiO 2 Amino modification of the gel: take the gel obtained in step (2) and the amino modifier 3-aminopropyltriethoxysilane (APTES) and add it to toluene, and reflux at 75°C for 15 hours; The volume ratio of gel, amino modifier and toluene is 1:5:100; filter and wash 3 times with toluene to obtain amino-modified SiO 2 gel;

[0018] (4) Drying under normal pressure: drying the gel treated in step (3) at 110° C. for 12 hours to ob...

Embodiment 2

[0020] (1) Preparation of SiO by silicon powder dissolution method 2 Sol: First, soak the industrial grade silicon powder in hot water at 60°C to activate it, add it into the container containing the potassium hydroxide solution catalyst twice, stir and heat, the reaction temperature is controlled at 85°C, and the reaction is no longer SiO can be obtained by standing still and filtering until the bubbles are generated. 2 Sol;

[0021] (2) Static gel: the SiO prepared in step (1) 2 The sol was left standing for 5h to obtain SiO 2 gel;

[0022] (3) SiO 2 Amino modification of the gel: take the gel obtained in step (2) and the amino modifier 3-aminopropyltriethoxysilane (APTES) and add it to toluene at 80°C for reflux modification for 13 hours; wherein the gel, The volume ratio of amino modifier to toluene is 1:8:90; filter and wash with toluene 4 times to obtain amino modified SiO 2 gel;

[0023] (4) Drying under normal pressure: drying the gel treated in step (3) at 115°...

Embodiment 3

[0025] (1) Preparation of SiO by silicon powder dissolution method 2 Sol: Soak industrial-grade silicon powder in hot water at 70°C to activate it, add it to the container containing sodium hydroxide solution catalyst three times, stir and heat, and control the reaction temperature at 90°C until there are no more bubbles When it is produced, let it stand still and filter to get SiO 2 Sol;

[0026] (2) Static gel: the SiO prepared in step (1) 2 The sol was left standing for 8h to obtain SiO 2 gel;

[0027] (3) SiO 2 Amino modification of the gel: take the gel obtained in step (2) and the amino modifier 3-aminopropyltriethoxysilane (APTES) and add it to toluene to modify it at 85°C for 12 hours; wherein the gel, amino The volume ratio of modifier and toluene is 1:10:80; filter and wash with toluene for 5 times to obtain amino-modified SiO 2 gel;

[0028] (4) Drying under normal pressure: drying the gel treated in step (3) at 115° C. for 8 hours to obtain amino-modified na...

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Abstract

The invention discloses a method of preparing amino modified nanometer silicon micropowder by ambient pressure drying and belongs to the technical field of preparation of novel materials. The method disclosed by the invention comprises the following steps: carrying out reaction on silicon powder as a raw material and water under the catalytic effect of an alkali to obtain a SiO2 sol; adding then standing SiO2 sol and an amino modifier into methylbenzene for backflow modification; and filtering and washing and finally drying under ambient pressure to obtain the amino modified nanometer silicon micropowder material. The method disclosed by the invention is carried out at ambient pressure and is mild reaction condition, simple in process and easy to prepare on a large scale.

Description

technical field [0001] The invention relates to a production method of nano-silicon powder, in particular to a method for preparing amino-modified nano-silicon powder by drying under normal pressure. Background technique [0002] Silica powder refers to silica powder. As an inorganic material, it has good dielectric properties, low thermal expansion coefficient, thermal conductivity, high chemical stability and unique optical properties. Silica powder is widely used in aviation, aerospace, In the chemical and electronic industries, especially in the fields of potting, encapsulating materials, molding compounds, silicone rubber, paints, and coatings in the electronics, microelectronics, and electrical industries. [0003] Traditional silica powder is made of vein quartz, powder quartz, microcrystalline hard quartz ore, etc., through mineral processing, cleaning, filtering, coarse crushing, fine crushing, grinding, pickling, alkali neutralization, ion water repeated cleaning, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/28C09C3/12
Inventor 张凤凯周兴平徐腾刘祥友张勋
Owner 江苏凯达石英股份有限公司
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