Preparation method of spherical silicon dioxide nano-particles

A spherical silica and nanoparticle technology, applied in chemical instruments and methods, nanotechnology, inorganic chemistry, etc., can solve the problems of high cost, inability to prepare silica with uniform sphericity and particle size, and increasing the difficulty of product separation.

Active Publication Date: 2019-03-12
TSINGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the silica precipitation is confined in the droplet, the particle size can be controlled, but it also increases the difficulty of product separation and the cost

Method used

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  • Preparation method of spherical silicon dioxide nano-particles
  • Preparation method of spherical silicon dioxide nano-particles
  • Preparation method of spherical silicon dioxide nano-particles

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0028] The invention provides a method for preparing spherical silica nanoparticles, including the following steps:

[0029] Disperse nitrogen vertically through the microporous membrane into the flowing sodium silicate solution to obtain the precursor solution;

[0030] Disperse the sulfuric acid solution vertically in the flowing precursor solution through the microporous membrane, cause a precipitation reaction to occur, and age to obtain spherical silica nanoparticles;

[0031] The initial flow rate of the sulfuric acid solution through the microporous membrane is 5-30 mL / min, and the flow rate of the sulfuric acid solution through the microporous membrane is increased once every 1 to 2 min, and the increase is 0.1-10 mL / min each time, The final flow rate is 12-40mL / min.

[0032] In the present invention, unless otherwise specified, all raw material components are commercially available components well known to those skilled in the art.

[0033] In the present invention, nitrogen i...

Example Embodiment

[0053] Example 1

[0054] Place the membrane dispersion microreactor in a 70℃ water bath;

[0055] Disperse nitrogen vertically through the microporous membrane in the membrane dispersion microreactor at a flow rate of 1000 mL / min into a sodium silicate solution with a concentration of 1 mol / L and a flow rate of 18 mL / min to obtain a precursor solution;

[0056] The 1.2mol / L sulfuric acid solution was vertically dispersed into the flowing precursor solution through the microporous membrane, and the precipitation reaction occurred. The pH value of the end of the reaction was 8.75. The initial flow rate of the sulfuric acid solution was 10mL / min. The sulfuric acid was removed every 2min. The flow rate of the solution was increased by 1 mL / min until the flow rate of the sulfuric acid solution reached 15 mL / min, and the flow rate of the sulfuric acid solution was no longer increased.

[0057] The product system obtained by the above precipitation reaction was aged for 3 hours in a stirred...

Example Embodiment

[0061] Example 2

[0062] Place the membrane dispersion microreactor in a water bath at 80°C;

[0063] Disperse nitrogen vertically through the microporous membrane in the membrane dispersion microreactor at a flow rate of 1000 mL / min into a sodium silicate solution with a concentration of 1 mol / L and a flow rate of 20 mL / min to obtain a precursor solution;

[0064] The 1.2mol / L sulfuric acid solution was vertically dispersed into the flowing precursor solution through the microporous membrane, and the precipitation reaction occurred. The pH of the reaction end point was 8.75, and the initial flow rate of the sulfuric acid solution was 12mL / min. The sulfuric acid was removed every 1 minute. The flow rate of the solution was increased by 1 mL / min until the flow rate of the sulfuric acid solution reached 15 mL / min, and the flow rate of the sulfuric acid solution was no longer increased.

[0065] The product system obtained by the above precipitation reaction was aged for 3 hours in a st...

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Abstract

The invention provides a preparation method of spherical silicon dioxide nano-particles. The preparation method comprises the following steps of vertically dispersing nitrogen into a flowing sodium silicate solution through a microporous membrane to obtain a precursor solution; and vertically dispersing a sulfuric acid solution into the flowing precursor solution through the microporous membrane,and performing precipitation reaction and ageing to obtain the spherical silicon dioxide nano-particles, wherein the initial flow rate of the sulfuric acid solution passing through the microporous membrane is 5-30 mL/min, the flow rate of the sulfuric acid solution passing through the microporous membrane is increased by one time per 1-2 min, each increase amplitude is 0.1-10 mL/min, and the finalflow rate is 12-40 mL/min. According to records of the embodiment of the invention, the particle size of the silicon dioxide nano-particles prepared by the preparation method provided by the invention is 20-80 nm, and the degree of sphericity is good.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a method for preparing spherical silica nanoparticles. Background technique [0002] Spherical silica nanoparticles are a kind of white amorphous silica powder with small particle size, good dispersion, large specific surface area, low thermal conductivity, stable chemical properties, corrosion resistance and many other superior properties, so they can be widely used In coatings, papermaking, cosmetics, medicine and other fields. [0003] At present, the commonly used methods for preparing nano-scale spherical silica mainly include the following: ① gas phase method: silicon-containing halides (such as SiCl 4 、CH 3 SiCl 3 ) at high temperature (1200-1600°C) to obtain nano-silica by gas-phase hydrolysis. The silica obtained by the above preparation method has the advantages of high purity, low surface hydroxyl content, good dispersibility, small particle size, ...

Claims

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Application Information

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IPC IPC(8): C01B33/193B82Y40/00
CPCB82Y40/00C01B33/193C01P2004/04C01P2004/32C01P2004/64C01P2006/12C01P2006/14C01P2006/16C01P2006/17
Inventor 王玉军刘羽白张帆杨璐帆骆广生王承辉聂志明
Owner TSINGHUA UNIV
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