A kind of preparation method of spherical silica

A spherical silica and carbon dioxide technology, applied in the direction of silica, silicon oxide, carbonate preparations, etc., can solve problems such as failure to achieve good application effects, difficulty in large-scale industrial production, difficulty in processing and reuse, etc. Achieve the effects of low production cost, narrow particle size distribution and large pore volume

Active Publication Date: 2021-08-27
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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  • A kind of preparation method of spherical silica
  • A kind of preparation method of spherical silica
  • A kind of preparation method of spherical silica

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 to dissolve at room temperature to obtain an aqueous sodium silicate solution.

[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 dispersed membrane is 0.5 μm; the volume flow ratio of carbon dioxide gas to the sodium silicate aqueous solution is 5:1, The obtained reaction solution was recycled and fed, and the carbonization reaction temperature was 20° C. When the pH value of the reaction solution was 8, ventilation was stopped.

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

[0039] (4) The precipitate is obtained by centrifugation, washed with water, an...

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 to dissolve at room temperature to obtain an aqueous sodium silicate solution.

[0044] (2) The sodium silicate aqueous solution obtained in step (1) and pure carbon dioxide gas are simultaneously introduced into the membrane dispersion microreactor, and the average pore diameter of the dispersion membrane is 5 μm. The sodium silicate aqueous solution is fed in a single feeding, the volume flow ratio of carbon dioxide gas to the 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, the ventilation is stopped.

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

[0046] (4) Centrifugation and separation to obtain a precipitate, w...

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 to dissolve at room temperature to obtain an aqueous sodium silicate solution.

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

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

[0053] (4) Centrifugation and separation...

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Abstract

The invention discloses a preparation method of spherical silica belonging to the technical field of chemical synthesis. Specifically, sodium silicate and carbon dioxide-containing gas are introduced into the microreactor to carry out carbonization reaction, aging, separation and extraction of precipitates, washing, and spray drying to obtain spherical silica. The spherical silica prepared by the invention has high specific surface area, large pore volume, good dispersibility and uniform mesoporous structure; the preparation method has the advantages of easy availability of raw materials, low production cost, stable and controllable process, and easy realization of continuous production. Advantages, significant advantages in large-scale production of high-quality silica.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a preparation method of spherical silica. Background technique [0002] Silica is widely used in rubber, coatings, catalysts, biomedicine, optoelectronics and adsorption separation due to its advantages of high specific surface area, large pore volume, chemical stability, biocompatibility and low dielectric constant. The morphology and dispersibility of silica directly affect its application effect, and spherical silica has attracted much attention due to its good dispersibility. [0003] Industrial large-scale production of silica usually adopts the precipitation method, that is, using water glass and sulfuric acid as raw materials, reacting at high temperature, and then post-processing such as acidification and aging to obtain silica. Although this process is simple to operate and low cost, it will produce a large amount of Na 2 SO 4 Wastewater, difficult to treat...

Claims

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Application Information

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Patent Type & Authority Patents(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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