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Method for preparing aerogel by supercritical drying method and device for supercritical drying

A technology of supercritical drying and airgel, which is applied in the direction of dry gas arrangement, aerosol preparation, chemical instruments and methods, etc., can solve the problem that the uniformity of pore structure distribution is not enough, the structural strength of airgel, the drying efficiency and separation efficiency, and the inability to Directly obtain airgel and other issues to achieve the effect of enhanced supercritical chemical reaction structure, high separation efficiency and fluid recovery efficiency, and high pore structure strength

Active Publication Date: 2018-10-12
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN102491326A discloses a device for supercritical fluid drying and a method for preparing airgel materials. The device disclosed in this patent and the use of the device for supercritical drying to prepare aerogels can realize aerosol production in different production scales and different production methods. The preparation of gel materials, but the use of the device in this patent for supercritical drying still has the problems of insufficient uniformity of the pore structure distribution of the airgel, and the structural strength, drying efficiency and separation efficiency of the airgel need to be further improved
In addition, neither the system disclosed in CN1139390A nor the device and method disclosed in CN102491326A can directly obtain functional aerogels such as hydrophobicity

Method used

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  • Method for preparing aerogel by supercritical drying method and device for supercritical drying
  • Method for preparing aerogel by supercritical drying method and device for supercritical drying

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] Embodiment 1: the preparation of airgel material

[0085] Add ethanol solution (40% by volume) of tetraethyl orthosilicate to the preparation container, then add water, add ammonia water (1mol / L) and ammonium fluoride aqueous solution (0.1mol / L) dropwise while stirring, and start gelation reaction. Wherein, the molar ratio of substances is tetraethyl orthosilicate: water: ammonia water: ammonium fluoride = 100:400:1:1, after mixing evenly, continue stirring for 5 minutes to obtain a sol.

[0086] At room temperature, the gel continued to age for 1 day, after which the mold was removed, the wet gel was taken out, and solvent replacement was performed in absolute ethanol. Change the ethanol every 48 hours until the water content in the ethanol is lower than 1% as measured by a Karl Fischer moisture titrator.

[0087] Put the wet gel that has completed the solvent replacement into the drying kettle, and adopt the method as in the present invention figure 1 The device st...

Embodiment 2

[0090] Embodiment 2: Preparation of glass wool reinforced airgel composite

[0091] Embodiment 2 is substantially the same as embodiment 1, and the difference is: the impregnated bulk density is 0.1g / cm with the obtained sol 3 glass wool felt. Put the glass wool felt into the mold cavity first, then slowly add the above solution into the mold cavity to make the glass wool felt absorb the sol. After the glass wool felt is soaked in the sol, close the mold. After gelling at room temperature, a glass wool felt-reinforced silica wet gel is obtained.

[0092] At room temperature, the wet gel was further aged for 1 day, and then the mold was removed, and the wet gel was taken out, and put into absolute ethanol for solvent replacement. Change the ethanol every 48 hours until the water content in the ethanol is lower than 1% as measured by a Karl Fischer moisture titrator.

[0093] The glass wool felt-reinforced silica wet gel that has undergone solvent replacement is dried with s...

Embodiment 3

[0098] Example 3: Preparation of Basalt Wool Reinforced Airgel Composite

[0099] Spread the cut basalt wool into the corresponding mold cavity and close the mold. Inject 0.2MPa helium into the mold and ensure that the airtightness is intact.

[0100] Add ethanol solution (40% by volume) of tetraethyl orthosilicate to the preparation container, then add water, add ammonia water (1mol / L) and ammonium fluoride aqueous solution (0.1mol / L) dropwise while stirring, and start gelation reaction. Wherein, the molar ratio of substances is tetraethyl orthosilicate: water: ammonia water: ammonium fluoride = 100:400:1:1, after mixing evenly, continue stirring for 5 minutes to obtain a sol.

[0101] Connect the pressure injection device, put the prepared sol into the pressure tank, turn on the helium source and slowly increase it to 0.2MPa, then slowly open the injection valve and keep the glue outlet valve closed, and start pressure injection. The device is disassembled, and the presse...

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Abstract

The invention relates to a method for preparing aerogel by a supercritical drying method and a device for supercritical drying. The method comprises: placing wet gel containing a solvent in a drying kettle, making a supercritical drying fluid carry a functional modifier, uniformly dispersing the fluid by a homogenizer to supercritically drying the wet gel, and discharging the fluid so that the aerogel is obtained. The device comprises a circulating fluid storage tank for storing a supercritical drying fluid, a chemical reagent storage tank for storing a functional modifier, a pressure pump feeding the fluid into the chemical reagent storage tank, at least one drying kettle with a fluid inlet, at least one separation kettle, a recovery tank, a compression pump and a condenser, and the aboveparts are orderly communicated through a fluid communication method. The condenser is communicated with the circulating fluid storage tank. The homogenizer is arranged at the fluid inlet of the drying kettle. The method and device have high drying efficiency, can ensure uniform distribution of aerogel pore structures and can directly produce functional aerogel.

Description

technical field [0001] The invention relates to the technical field of functional airgel preparation, in particular to a method for preparing airgel by a supercritical drying method and a device for supercritical drying. Background technique [0002] Airgel is one of the solids with the smallest density in the world. It is a lightweight, porous condensed solid material composed of nano colloidal particles or polymer molecules. Its particle size is between 1 and 100nm. category. Airgel has a unique open continuous porous random structure and three-dimensional network, and has the characteristics of extremely low density, high specific surface area, high porosity and temperature resistance and heat insulation. Aerogels show unique properties in mechanics, acoustics, thermals, optics, etc., and have great application prospects in aerospace, military, communications, medical, building materials, electronics, metallurgy, and many other fields. [0003] In recent years, research...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/00F26B21/14
CPCB01J13/0095F26B21/14
Inventor 王子宁周玉贵邹军锋李文静刘斌赵英民
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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