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Preparation method of silicon dioxide aerogel composite material

A composite material and silicon dioxide technology, applied in chemical instruments and methods, colloid chemistry, colloid chemistry, etc., can solve the problems of high aerogel content, large consumption of organic solvents, and low aerogel content of composite materials, and achieve The effect of thorough modification, saving input and improving the utilization rate of solvent

Active Publication Date: 2021-11-05
INST OF ADVANCED TECH UNIV OF SCI & TECH OF CHINA
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Problems solved by technology

[0004] The main purpose of the present invention is to propose a preparation method of silica airgel composite material, aiming at solving the complicated solvent exchange of silica gel in the prior art when carrying out surface modification to silica gel, which requires consumption A large amount of organic solvents, the problem of high airgel content on the surface of the composite material and low airgel content inside the composite material

Method used

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  • Preparation method of silicon dioxide aerogel composite material
  • Preparation method of silicon dioxide aerogel composite material
  • Preparation method of silicon dioxide aerogel composite material

Examples

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preparation example Construction

[0053] combine figure 1 Shown, in one embodiment, the preparation method of described silica airgel composite material comprises the following steps:

[0054] S10, providing a gel composite material;

[0055] This step mainly prepares gel composite materials, which can be purchased or prepared by yourself. When preparing by yourself, specifically, before step S10, it also includes:

[0056] S101, mixing and stirring the silicon source and water to form a silicon source aqueous solution, adding an acidic aqueous solution to the silicon source aqueous solution for acidification to obtain a silicon sol solution;

[0057] Specifically, the silicon source includes that the solute is one or more of tetraethyl orthosilicate, tetramethyl orthosilicate, methyltrimethoxysilane, dimethyldimethoxysilane, and silicon tetrachloride. The aqueous solution of the species, the time of the acidification treatment is 5-60min, the temperature of the acidification treatment is 10-70°C, the silico...

Embodiment 1

[0092] (1) First dilute the sodium silicate aqueous solution with water, take 0.6L of sodium silicate aqueous solution and 3L of water, mix well and stir evenly, and obtain the dilution solution of the silicon source. Slowly introduce the diluent of the silicon source into 216mL of 8.5mol / L hydrochloric acid solution for acidification treatment, the time of the acidification treatment is 5min, and the temperature of the acidification treatment is 70°C to obtain a sol solution;

[0093] (2) Add 2.5M ammonia solution to the silica sol solution, mix and stir to adjust the pH of the sol to 4.6, and introduce it into the fiber composite material. After the sol solution is fully impregnated, when the fiber composite material is solidified, microwave The gel composite material was obtained by irradiation treatment, the irradiation power per 400mL of silica sol solution was 0.6KW, and the treatment time was 125s;

[0094] (3) Put the gel composite material into a reactor to stand for ...

Embodiment 2

[0099] (1) First dilute the sodium silicate aqueous solution with water, take 1.34L of silicon source and 2.95L of water, mix well and stir evenly to obtain the dilution of silicon source. Slowly introduce the diluent of the silicon source into 650 mL of 4.8M hydrochloric acid solution for acidification treatment, the time of the acidification treatment is 60 minutes, and the temperature of the acidification treatment is 10°C to obtain a sol solution;

[0100] (2) Adjust the pH of the sol to 5.0 with a diluted sodium silicate aqueous solution, wherein the volume ratio of the silicon source to water is 0.2-8:1, stir evenly, and introduce it into the fiber composite material, and wait until the sol solution is fully impregnated Finally, when the fiber composite material is solidified, the gel composite material is obtained by microwave irradiation treatment, the irradiation power of each 400mL silica sol solution is 0.4KW, and the microwave irradiation treatment time is 45s.

[...

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Abstract

The invention discloses a preparation method of a silicon dioxide aerogel composite material. The preparation method comprises the following steps: S10, providing a gel composite material; s20, putting the gel composite material into a reaction kettle for standing and aging; s30, introducing an acid solution and a silsesquioxane solution into a reaction kettle,pumping the solution at the bottom of the reaction kettle out, and injecting the solution from the top of the reaction kettle to form circulation so as to obtain a modified wet gel composite material ; and s40, performing drying treatment on the wet gel composite material to obtain the hydrophobic hybrid silicon dioxide aerogel composite material. Due to the fact that the circulation process is conducted continuously, an active modifier is generated continuously, the active modifier makes full contact with the gel composite material from top to bottom, and the modification process is conducted fully, so that the gel compositematerial can be fully and efficiently modified. In addition, a large number of active modifiers generated in the modification process can be subjected to self condensation reaction when meeting water to generate silsesquioxane, and the generated silsesquioxane can participate in the next circular reaction process.

Description

technical field [0001] The invention relates to the technical field of preparation of thermal insulation materials, in particular to a preparation method of a silica airgel composite material. Background technique [0002] In the process of preparing silica airgel by atmospheric drying method, the most critical is to realize low-cost and high-efficiency hydrophobic modification of hydrogel composite materials, and then dry under normal pressure conditions to modify the surface hydrophobicity. The quality directly determines the quality of the obtained silica airgel. [0003] In the prior art, the sol-gel method is usually used to prepare silica gel, and the surface of the silica gel is modified by using trimethylchlorosilane with strong activity as a surface modifier, and finally dried under normal pressure to obtain silica gas. Gel powder. Then, the prepared airgel powder is mixed with the fiber mat by vacuum infiltration method to obtain the silica airgel composite felt ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B30/02B01J13/00
CPCC04B30/02B01J13/0091C04B2201/32C04B14/064C04B14/38C04B16/06
Inventor 张和平潘月磊程旭东龚伦伦
Owner INST OF ADVANCED TECH UNIV OF SCI & TECH OF CHINA
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