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Amorphous state nanometer silicon dioxide micro powder and preparation method thereof

A nano-silica, amorphous technology, applied in the direction of silica, silicon oxide, nanotechnology, etc., can solve the problems of large environmental pollution, many organic waste solvents, etc., and achieve low reaction temperature, high silicon-oxygen content, The effect of less waste removal

Active Publication Date: 2015-02-18
陕西宝塔山油漆股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that compared with the precipitation method listed in its patent, the pollution is relatively small, but its filtration process, filter cake washing process, and organic solvent replacement process still produce more organic waste solvents and waste water. Handling is also a more serious problem at the same time, and the environmental pollution is still relatively large relative to the preparation method of the present invention

Method used

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  • Amorphous state nanometer silicon dioxide micro powder and preparation method thereof
  • Amorphous state nanometer silicon dioxide micro powder and preparation method thereof
  • Amorphous state nanometer silicon dioxide micro powder and preparation method thereof

Examples

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Effect test

Embodiment 1

[0031] Prepare tetramethylammonium hydroxide into a 25% aqueous solution (weight concentration), then mix according to the weight ratio of octamethylcyclotetrasiloxane: tetramethylammonium hydroxide = 100:0.1, and then rapidly heat up to 90°C , heat preservation reaction 1h; then dropwise add 30 parts of vinyltrimethoxysilane, react for 2.5h, then add 5 parts of 50% ethanol aqueous solution, then add 0.1 part of tetramethylammonium hydroxide aqueous solution, and then add 5 Part of distilled water was reacted for 1 hour to start vacuum distillation, and at the same time, the temperature was raised to 130°C, the pressure was -700mmHg, and the solution was turned into a gel after vacuum distillation for 10 minutes;

[0032] Dry the wet gel at room temperature for 1 hour to obtain dry xerogel, which can be simply ground into a fine powder; calcinate the xerogel at 350°C for 1.5 hours to obtain white amorphous nano-silica micropowder with a particle size of 70-200nm.

Embodiment 2

[0034] Tetramethylammonium hydroxide was formulated into a 25% aqueous solution (weight concentration), then mixed according to the weight ratio of decamethylcyclopentasiloxane:tetramethylammonium hydroxide=100:0.5, and then rapidly heated to 85°C, Insulation reaction for 1.5h; then 30 parts of vinyltrimethoxysilane was added dropwise, reacted for 2.5h, then 5 parts of 50% ethanol aqueous solution was added, and 0.1 part of tetramethylammonium hydroxide aqueous solution was added, and then 15 parts of Parts of distilled water reacted for 1 hour and began to distill under reduced pressure. At the same time, the temperature was raised to 130°C, the pressure was -700mmHg, and the solution was distilled under reduced pressure for 40 minutes, and the solution became a gel;

[0035] Dry the wet gel at room temperature for 1 hour to obtain dry xerogel, which can be simply ground into a fine powder; calcinate the xerogel at 350°C for 1.5 hours to obtain white amorphous nano-silica micr...

Embodiment 3

[0037]Prepare tetramethylammonium hydroxide into a 25% aqueous solution (weight concentration), then mix according to the weight ratio of dodecamethylcyclohexasiloxane: tetramethylammonium hydroxide = 100:0.8, and then rapidly heat up to 80°C , keep warm for 1 hour; then add 40 parts of vinyltrimethoxysilane dropwise, react for 2 hours, then add 6 parts of 50% ethanol aqueous solution, then add 0.5 parts of tetramethylammonium hydroxide aqueous solution, and then add 8 parts The distilled water was reacted for 1 hour to start vacuum distillation, and at the same time, the temperature was raised to 130°C, the pressure was -700mmHg, and the vacuum distillation was 30 minutes, and the solution became a gel;

[0038] Dry the wet gel at room temperature for 1 hour to obtain dry xerogel, which can be simply ground into a fine powder; calcinate the xerogel at 300°C for 2 hours to obtain white amorphous nano-silica powder with a particle size of 70 ~200nm.

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Abstract

The invention discloses an amorphous state nanometer silicon dioxide micro powder and a preparation method thereof. The preparation method comprises the following steps: a reactant of tetramethylammonium hydroxide and silane and vinyl trimethoxy silane are used as a raw material, the tetramethylammonium hydroxide is used as a temporary catalyst, a low-temperature reaction is performed for 2-5 hours in an oil bath, then a solution is converted into gel through warming, decompressing and sucking filtration, the gel is calcined at the low temperature of 300-500 DEG C to prepare silicon dioxide coacervate, an obtained power body is amorphous state globular coacervate, and the particle diameter is 70-200 nm. The preparation method disclosed by the invention has the advantages that the reaction temperature is mild, the period is short, the calcining temperature is low, at the same time, technology equipment is simple, raw materials are easy to obtain, the discharge in the production process is extremely few, and the obtained amorphous state nanometer silicon dioxide micro powder has the advantages of high purity, uniform particle size and easy dispersal.

Description

technical field [0001] The invention belongs to the preparation technology of inorganic nanometer materials, and in particular relates to a preparation method of amorphous nanopowder by cyclosilane and ethylenic silsesquisilane. Background technique [0002] Amorphous nano silica powder is a non-toxic, odorless, non-polluting inorganic non-metallic material, which plays an important role in functional fibers, new coatings and ink modification, optical materials, textile industry, sealant and rubber, etc. application. Although there are different methods to develop nano-silica, it is still one of the current research hotspots to produce high-purity, short-cycle, simple-process, and low-cost products. [0003] Regarding the preparation technology of silica powder, Chinese patent CN101746767A discloses "a method for preparing high-purity spherical nano-silicon dioxide", which uses SiO 2 Raw materials are processed at 450°C to 1000°C, ground into powder, treated with acid, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18B82Y30/00
Inventor 陈杰刘宪文张林来信
Owner 陕西宝塔山油漆股份有限公司
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