A kind of silicon oxide reinforced polyimide airgel micropowder and preparation method thereof

A technology of polyimide and airgel, which is applied in the field of online polyimide airgel micropowder and its preparation, can solve the problems of high cost, poor lightness, and low strength, and achieve low cost and functional group Numerous, low-cost effects

Active Publication Date: 2022-01-04
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing polyimide aerogels cannot be used as powder fillers due to their high toughness and difficulty in making powder. In addition, the traditional polyimide aerogels are expensive, and the skeleton structure is all organic components, which is slightly poor, low intensity

Method used

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  • A kind of silicon oxide reinforced polyimide airgel micropowder and preparation method thereof
  • A kind of silicon oxide reinforced polyimide airgel micropowder and preparation method thereof
  • A kind of silicon oxide reinforced polyimide airgel micropowder and preparation method thereof

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preparation example Construction

[0026] A preparation method of linear polyimide airgel micropowder reinforced by silicon oxide, comprising the following steps:

[0027] Step (1), methyl vinyl ether-maleic anhydride copolymer, 3-aminopropyltriethoxysilane and aromatic diamine are dissolved in solvent respectively to obtain methyl vinyl ether-maleic anhydride copolymer solution, 3-aminopropyltriethoxysilane solution and aromatic diamine solution;

[0028] Step (2), the methyl vinyl ether-maleic anhydride copolymer solution, the 3-aminopropyltriethoxysilane solution and the aromatic diamine solution are stirred and mixed in a certain proportion and left to stand to form a gel, Then soak the formed gel in a dehydrating agent for chemical imidization to obtain an imidized gel;

[0029] In step (3), the imidized gel is pulverized, solvent replaced, and dried to obtain a linear polyimide airgel micropowder reinforced with silicon oxide nanoparticles.

[0030] Among them, the aromatic diamine described in step (1)...

Embodiment 1

[0039] (1) Configuration of the monomer solution: take 10g of methyl vinyl ether-maleic anhydride copolymer, 1g of 3-aminopropyltriethoxysilane, and 5g of p-phenylenediamine, and dissolve them in 100ml of N-methyl In base pyrrolidone, it is configured to have a concentration of 0.1, 0.01, 0.05g / cm 3 The solution.

[0040] (2) Synthesis of gel: Take 100, 5 and 30ml of the above solutions respectively, mix them evenly, form a gel at 0°C, then soak the gel in a mixed solution of pyridine and acetic anhydride (volume ratio 1:1) for dehydration .

[0041] (3) Preparation of polyimide airgel micropowder—grinding, solvent replacement and drying: the dehydrated gel (imidized gel) was first squeezed at 30°C for 3 hours under a pressure of 2 MPa, and then Stir at a speed of 1000 rpm for 3 hours to obtain wet gel micropowder, and then soak in 2 times the volume of methanol for solvent replacement. The methanol is replaced every 5 hours for a total of 3 replacements. The replaced gel w...

Embodiment 2

[0043] (1) Configuration of monomer solution: Take 30g of methyl vinyl ether-maleic anhydride copolymer, 5g of 3-aminopropyltriethoxysilane, and 20g of p-phenylenediamine, and dissolve them in 100ml N, N -In dimethylacetamide, configure the concentration to be 0.3, 0.05, 0.2g / cm 3 The solution.

[0044] (2) Synthesis of gel: Take 100, 5 and 30ml of the above solutions respectively, mix them evenly, form a gel at 40°C, and then soak the gel in a mixed solution of triethylamine and acetic anhydride (volume ratio 1:1) Medium dehydration.

[0045] (3) Preparation of polyimide airgel micropowder - pulverization, solvent replacement and drying: first extrude the above-mentioned dehydrated gel at 50°C and 3MPa pressure for 1 hour, and then stir at a speed of 2000 rpm After 2 hours, the wet gel micropowder was obtained, and then soaked in 2 times the volume of ethanol for solvent replacement. The ethanol was changed every 10 hours for a total of 3 times. The replaced gel was dried ...

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Abstract

The invention provides a silicon oxide reinforced polyimide airgel micropowder and a preparation method thereof, which belong to the technical field of nanoporous materials and thermal insulation. The preparation method comprises: respectively dissolving methyl vinyl ether-maleic anhydride copolymer, 3-aminopropyltriethoxysilane, and aromatic diamine in a solvent; Mix, stir evenly and react statically to form a gel, prepare micropowder gel by mechanical pulverization, then soak the gel in a dehydrating agent; finally replace the dehydrated gel with solvent, and supercritically dry to obtain silica nanoparticle reinforcement linear polyimide airgel micropowders. The polyimide airgel micropowder obtained by the present invention is brown, has an organic-inorganic double network structure, has the rigidity of silicon oxide and the toughness of polyimide, and has a low density (0.03~0.3g / cm 3 ), high specific surface area (200~600m 2 / g), high temperature resistance and other excellent characteristics.

Description

technical field [0001] The invention relates to a silicon oxide-reinforced linear polyimide airgel micropowder and a preparation method thereof, belonging to the technical field of nanoporous materials and thermal insulation. Background technique [0002] Airgel is a kind of porous nano material, which is currently the lightest solid material with the best thermal insulation performance in the world. Since silica airgel has a high specific surface area (400-1500m 2 / g), high porosity (80-99.8%), low density (0.003-0.6g / cm 3 ) and low thermal conductivity (0.013-0.038W / mk), which make it very important in the fields of high temperature resistance and heat insulation, ultra-low density, acoustic impedance coupling, gas adsorption and filtration, catalyst carrier, drug carrier, etc. So far, various types of aerogels have been prepared by chemical crosslinking, including silica aerogels (CN102424538A; CN102633269A), chitosan aerogels (CN102417606A), carbon aerogels (CN10242366...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08K3/36C08G73/10C08J9/28
CPCC08J9/28C08G73/10C08K3/36C08J2379/08C08J2205/026C08K2201/011
Inventor 马晶晶赵一搏杨汝平贾地郭超许小强
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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