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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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  • Abstract
  • Description
  • Claims
  • Application Information

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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 is high
[0004] It can be seen from the above that none of the above preparation methods can prepare silica with better sphericity and uniform particle size at a lower cost.

Method used

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

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

[0030] The sulfuric acid solution is vertically dispersed in the flowing precursor solution through a microporous membrane, a precipitation reaction occurs, and aging is performed to obtain spherical silica nanoparticles;

[0031] The initial flow rate of the sulfuric acid solution through the microporous membrane is 5-30mL / min, and every 1-2min, the flow rate of the sulfuric acid solution through the microporous membrane increases once, each time the increase range is 0.1-10mL / min, 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] The invention vertica...

Embodiment 1

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

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

[0056] The sulfuric acid solution of 1.2mol / L is vertically dispersed into the flowing precursor solution through the microporous membrane, and a precipitation reaction occurs. The flow rate of the solution increases by 1mL / min until the flow rate of the sulfuric acid solution reaches 15mL / min, and then no longer increases the flow rate of the sulfuric acid solution.

[0057] The product system obtained from the above precipitation reaction was aged in a stirred tank in a water bath at 70°C for 3 hours, centrifuged at a speed of 2000r / min for 10 minutes, and washed with water to obtain crude silica;

[0058] The crude silica was mixed with water...

Embodiment 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 1000mL / min into a sodium silicate solution with a concentration of 1mol / L and a flow rate of 20mL / min to obtain a precursor solution;

[0064] The sulfuric acid solution of 1.2mol / L is vertically dispersed into the flowing precursor solution through the microporous membrane, and a precipitation reaction occurs. The flow rate of the solution increases by 1mL / min until the flow rate of the sulfuric acid solution reaches 15mL / min, and then no longer increases the flow rate of the sulfuric acid solution.

[0065] The product system obtained from the above precipitation reaction was aged in a stirred tank in a water bath at 80°C for 3 hours, centrifuged at a speed of 2000r / min for 10 minutes, and washed with water to obtain crude silica;

[0066] The crude silica was mixed with wa...

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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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