A kind of atmospheric pressure preparation method of silica airgel

A silicon dioxide and aerogel technology, applied in the direction of silicon dioxide, silicon oxide, etc., can solve the problems of lengthy solvent replacement treatment, poor performance parameters of aerogel products, etc., and is conducive to industrial production, reducing costs, shortening The effect of the process flow

Active Publication Date: 2019-03-22
GUANGDONG UNIV OF TECH
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Problems solved by technology

Atmospheric pressure drying has higher requirements on the process, and requires lengthy solvent replacement treatment to reduce the capillary pressure acting on the silica airgel nanostructure or increase its skeleton strength to resist these forces, resulting in the conventional technology provided by the prior art. The performance parameters of airgel products prepared by pressure drying technology are poor

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  • A kind of atmospheric pressure preparation method of silica airgel
  • A kind of atmospheric pressure preparation method of silica airgel
  • A kind of atmospheric pressure preparation method of silica airgel

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preparation example Construction

[0028] The invention provides a normal-pressure preparation method of silica airgel, comprising:

[0029] modifying the aged silica wet gel by using a metal salt compound to obtain the modified wet gel, and the metal salt compound can coordinate with a hydroxyl group;

[0030] performing solvent replacement on the modified wet gel to obtain a modified gel;

[0031] The modified gel is dried under normal pressure to obtain a silica airgel.

[0032] The invention uses metal salt compounds to modify the aged silicon dioxide wet gel to obtain the modified wet gel. In the present invention, the aged silica wet gel is preferably modified in a metal salt compound solution to obtain the modified wet gel. In the present invention, the modification temperature is preferably 20°C-30°C, more preferably 22°C-28°C, most preferably 24°C-26°C. In the present invention, the modification time is preferably 20 hours to 30 hours, more preferably 22 hours to 28 hours, most preferably 24 hours t...

Embodiment 1

[0062] Add 42mL of alcohol (ETOH), 26.8mL of tetraethyl orthosilicate (TEOS) and 6.9mL of N-N dimethylformamide (DMF) into a 250mL two-necked flask, place it in an oil bath at 60°C, and adjust the rotation speed to 500 rpm / min, oil bath magnetic stirring 10min, to obtain the mixture;

[0063] Add H to the mixture 2 O 6.4mL and concentrated hydrochloric acid continued to be magnetically stirred in an oil bath at 60°C for 1h, and the pH value was adjusted to 3 to obtain an intermediate product;

[0064] Move the intermediate product into a 250mL beaker, drop concentrated ammonia water, adjust the pH value to 9, adjust the rotation speed to 100 rpm, and let it stand to obtain a silica wet gel;

[0065] The ETOH, TEOS, H 2 The molar ratio of O and DMF is 1:6:3:0.75.

[0066] The silica wet gel is placed in the mother liquor for aging twice, each time for 24 hours, and a new mother liquor needs to be replaced after each completion to obtain the aged silica wet gel;

[0067] Ad...

Embodiment 2

[0073]Add 42mL of alcohol (ETOH), 26.8mL of tetraethyl orthosilicate (TEOS) and 6.9mL of N-N dimethylformamide (DMF) into a 250mL two-necked flask, place it in an oil bath at 60°C, and adjust the rotation speed to 700 rpm / min, oil bath magnetic stirring 30min, obtain mixture;

[0074] Add H to the mixture 2 O 6.4mL and concentrated hydrochloric acid continued to stir magnetically in an oil bath at 60°C for 2h, and adjusted the pH value to 3 to obtain an intermediate product;

[0075] Move the intermediate product into a 250mL beaker, drop concentrated ammonia water, adjust the pH value to 7, adjust the rotation speed to 100 rpm, and let it stand to obtain a silica wet gel;

[0076] Described TEOS, ETOH, H The molar ratio of O and DMF is 1:6:3:0.75

[0077] The silica wet gel is placed in the mother liquor for aging twice, each time for 24 hours, and a new mother liquor needs to be replaced after each completion to obtain the aged silica wet gel;

[0078] Add 0.9987g of cal...

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Abstract

The invention provides a normal-pressure preparation method for silicon dioxide aerogel.The normal-pressure preparation method includes the steps that a metal salt type compound is adopted for modifying aged silicon dioxide wet gel to obtain modified wet gel, and the metal salt type compound can be coordinated with a hydroxide radical; the modified wet gel is subjected to solvent displacement to obtain modified gel; the modified gel is dried at normal pressure to obtain silicon dioxide aerogel.On the basis of a normal-pressure preparation method for aerogel in the prior art, the normal-pressure preparation method for silicon dioxide aerogel is improved, and the metal salt type compound is adopted for modifying the aged aerogel to obtain the silicon dioxide aerogel product with good performance parameters.In addition, the normal-pressure preparation method for silicon dioxide aerogel can shorten technological processes and lower the cost and facilitates industrialized production.

Description

technical field [0001] The invention relates to the technical field of silica airgel, in particular to a normal-pressure preparation method of silica airgel. Background technique [0002] The process of preparing silica airgel in the prior art includes two parts: sol-gel synthesis and post-treatment. The sol-gel synthesis method is roughly the same. Generally, the silicon source is hydrolyzed under certain conditions, and water or alcohol polycondensation is followed by Synthetic wet gel. The post-treatment process includes aging and drying. The purpose of aging is mainly to enhance the mechanical properties of the fragile solid skeleton formed in the sol-gel process. Most of the existing processes soak the wet gel in the mother liquor for aging. The drying process is generally divided into supercritical drying and atmospheric drying. Supercritical drying is to place the aged wet gel in an autoclave, and heat the autoclave until the pressure and temperature in it reach the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2006/12
Inventor 阳香华杜其轩郭宇阳谭嘉燊刘硕艺
Owner GUANGDONG UNIV OF TECH
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