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Preparation method of spherical silicon dioxide

A spherical silica and carbon dioxide technology, applied in the directions of silica, silica, carbonate preparations, etc., can solve the problems of inability to achieve good application effects, difficult to handle and reuse, and difficult to large-scale industrial production, etc. Achieve the effect of low production cost, large pore volume and narrow particle size distribution

Active Publication Date: 2019-07-19
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the process is simple in operation and low in cost, it will produce a large amount of Na 2 SO 4 Wastewater, difficult to treat and reuse
In addition, the controllability of the process is poor, and the product is easy to agglomerate, so it is often necessary to add surfactants to improve the dispersion of the product
Chinese patent CN104058415A discloses a method for preparing highly dispersed nano-silica. Although the dispersion of the product is improved by surfactant sodium carboxymethylcellulose and microporous dispersion, the prepared silica has a three-dimensional network structure , the specific surface area is 80-300m 2 / g, the particle size is 10-35nm, its dispersibility is not good, still can not achieve good application effect
This process can synthesize monodisperse spherical silica, but its raw material cost is high and the production process is complicated, so it is difficult to apply to large-scale industrial production

Method used

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  • Preparation method of spherical silicon dioxide
  • Preparation method of spherical silicon dioxide
  • Preparation method of spherical silicon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Spherical silica was prepared as follows:

[0036] (1) Dissolve 6 g of sodium silicate nonahydrate in 100 mL of water, and stir until dissolved at room temperature to obtain an aqueous solution of sodium silicate.

[0037] (2) The sodium silicate aqueous solution obtained in step (1) and pure carbon dioxide gas are simultaneously passed into the membrane dispersion microreactor, and the average pore diameter of the dispersion membrane is 0.5 μm; the volume flow ratio of carbon dioxide gas and sodium silicate aqueous solution is 5:1, The obtained reaction liquid is recycled and fed, and the carbonization reaction temperature is 20° C., and when the pH value of the reaction liquid is 8, the aeration is stopped.

[0038] (3) The reaction solution obtained in step (2) was put into an aging reaction kettle, and aged in a water bath at 80° C. for 10 minutes without stirring during the aging process.

[0039] (4) Centrifuge to obtain a precipitate, wash with water, then dispe...

Embodiment 2

[0042] Spherical silica was prepared as follows:

[0043] (1) Dissolve 6 g of sodium silicate nonahydrate in 300 mL of water, and stir until dissolved at room temperature to obtain an aqueous solution of sodium silicate.

[0044] (2) Pass the sodium silicate aqueous solution obtained in step (1) and pure carbon dioxide gas into the membrane dispersion microreactor simultaneously, and the average pore diameter of the dispersion membrane is 5 μm. The sodium silicate aqueous solution is fed once, the volume flow ratio of carbon dioxide gas and sodium silicate aqueous solution is 2:1, the carbonization reaction temperature is 40°C, and when the pH value of the reaction solution is 8, stop aeration.

[0045] (3) The reaction solution obtained in step (2) was put into an aging reaction kettle, and aged in a water bath at 100° C. for 6 hours without stirring during the aging process.

[0046] (4) Centrifuging and separating to obtain a precipitate, washing with water, then dispersin...

Embodiment 3

[0049] Spherical silica was prepared as follows:

[0050] (1) Dissolve 6 g of sodium silicate nonahydrate in 100 mL of water, and stir until dissolved at room temperature to obtain an aqueous solution of sodium silicate.

[0051] (2) Pass the sodium silicate aqueous solution obtained in step (1) and mixed gas (50% carbon dioxide+50% nitrogen) into the membrane dispersion microreactor simultaneously, and the average pore size of the dispersion membrane is 50 μm. The obtained reaction liquid is recycled and fed, the volume flow ratio of the mixed gas to the sodium silicate aqueous solution is 10:1, the carbonization reaction temperature is 15°C, and when the pH value of the reaction liquid is 8, the aeration is stopped.

[0052] (3) The reaction solution obtained in step (2) was put into an aging reaction kettle, and aged in a water bath at 85° C. for 10 minutes, and the stirring speed was 500 rpm during the aging process.

[0053] (4) Centrifuging and separating to obtain a prec...

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Abstract

The invention discloses a preparation method of spherical silicon dioxide, and belongs to the technical field of chemical synthesis. The method specifically comprises the following steps: introducingsodium silicate and carbon dioxide-containing gas into a micro-reactor, carrying out carbonization reaction, aging and separating to obtain a precipitate, and conducting washing and spray drying to obtain spherical silicon dioxide. The spherical silicon dioxide prepared by the preparation method is high in specific surface area, large in pore volume and good in dispersity, and has a uniform mesoporous structure; and the preparation method has the advantages that the raw materials are easy to obtain, the production cost is low, the process is stable and controllable, and continuous production is easy to realize, and has remarkable advantages in large-scale production of high-quality silicon dioxide.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of spherical silica. Background technique [0002] Silica, due to its advantages of high specific surface area, large pore volume, chemical stability, biocompatibility and low dielectric constant, is widely used in the fields of rubber, coatings, catalysts, biomedicine, photoelectricity and adsorption separation. The morphology and dispersion of silica directly affect its application effect, and spherical silica has attracted much attention because of its good dispersion. [0003] Industrial large-scale production of silica usually adopts the precipitation method, that is, water glass and sulfuric acid are used as raw materials, reacted at high temperature, and then subjected to post-treatment such as acidification and aging to obtain silica. Although the process is simple in operation and low in cost, it will produce a large amount of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18C01D7/02
CPCC01B33/18C01D7/02C01P2004/32C01P2004/61C01P2004/62C01P2006/12C01P2006/14
Inventor 骆广生韩春黎王凯
Owner TSINGHUA UNIV
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