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A kind of preparation method of silicon oxide/phenolic binary composite airgel

A binary composite and silicon oxide technology, which is applied in the field of composite airgel and its preparation, silicon oxide/phenolic binary airgel and its preparation, can solve the problem of destroying the formation of phenolic airgel network structure, increasing the viscosity of the mixed system, Poor alkaline matching and other problems, to achieve the effect of increasing room temperature stability, excellent heat resistance performance, and improving mechanical properties

Active Publication Date: 2022-05-03
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are many problems in this method in practical application. The curing of phenolic resin is generally carried out under alkaline conditions, and the acidic characteristics of acidic silica sol and the alkalinity matching of the curing system of phenolic sol are poor, resulting in extremely poor Easy to gel quickly, making the viscosity of the mixed system increase
This mismatch not only brings great inconvenience to the actual glue injection process, but also makes it difficult to realize the practical application of industrial processes; at the same time, the rapid gelation of the silicon system will destroy the formation of the phenolic airgel network structure, directly affecting the compounding process. Properties of airgel materials

Method used

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  • A kind of preparation method of silicon oxide/phenolic binary composite airgel
  • A kind of preparation method of silicon oxide/phenolic binary composite airgel
  • A kind of preparation method of silicon oxide/phenolic binary composite airgel

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Experimental program
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Effect test

Embodiment 1

[0029] (1) Synthesis of alkaline alcohol solvent-type silica sol: Weigh 1mol of tetraethyl orthosilicate and place it in a three-necked flask, add 416g of ethanol solvent to the system, and stir the system evenly to obtain a mixed solution A; weigh 4mol of Deionized water, add concentrated ammonia water to it, and configure it as 200mmol / L ammonia solution B; add solution B dropwise to solution A at 40°C, and continue the reaction for 12 hours after the dropwise addition is completed to obtain 10% ethanol base Reactive silica sol.

[0030] (2) Configure the composite sol of silicon oxide and phenolic formaldehyde: Weigh 120g of boron phenolic resin, add it to 100g of ethanol alkaline silica sol, then add 68.9g of ethanol solvent, stir the mixed sol evenly, and then add curing agent black Rotropine 24g (20% of phenolic sol mass), continue to stir 2h, obtain the composite sol (the solute mass ratio is 12:1 in phenolic sol and silica sol) of clear solid content 45%;

[0031] (3)...

Embodiment 2

[0034] (1) Synthesis of alkaline alcohol solvent-type silica sol: Weigh 1mol of tetraethyl orthosilicate and place it in a three-necked flask, add 416g of ethanol solvent to the system, and stir the system evenly to obtain a mixed solution A; weigh 1mol of orthosilicate Deionized water, add concentrated ammonia water to it, and configure 10mmol / L ammonia solution B; add solution B dropwise to solution A at 90°C, and continue the reaction for 6 hours after the dropwise addition is completed to obtain 10% ethanol alkaline Silica sol.

[0035] (2) Configure the composite sol of silicon oxide and phenolic sol: weigh 90g of molybdenum phenolic resin, add it to 900g of ethanol alkaline silica sol, then add 210g of ethanol solvent, stir the mixed sol evenly, and then add curing agent urethane Tropin 13.5g (15% of phenolic sol mass), continue to stir 12h, obtain the composite sol of clear solid content 15% (the solute mass ratio is 1:1 in phenolic sol and silica sol);

[0036] (3) Tr...

Embodiment 3

[0039](1) Synthesis of alkaline alcohol solvent-type silica sol: Weigh 1mol of tetraethyl orthosilicate and place it in a three-necked flask, add 416g of ethanol solvent to the system, and stir the system evenly to obtain a mixed solution A; weigh 2mol of Deionized water, add concentrated ammonia water to it, and configure it as 50mmol / L ammonia solution B; add solution B dropwise to solution A at 70°C, and continue to react for 9 hours after the dropwise addition is completed to obtain 10% ethanol alkaline Silica sol.

[0040] (2) Composite sol of silicon oxide and phenolic formaldehyde: Weigh 100g of novolac resin, add it to 200g of the above ethanol silica sol, and then add 100g of ethanol solvent, stir the mixed sol evenly, and then add curing agent Uroto Product 10g (10% of phenolic sol mass), continue to stir 3h, obtain the composite sol (the solute mass ratio is 5:1 in phenolic sol and silica sol) of clear solid content 30%;

[0041] (3) Transfer the prepared composite...

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Abstract

The invention discloses a preparation method of silicon oxide / phenolic binary composite airgel. The purpose is to overcome the deficiencies of the existing technology, enhance the acid-base matching between silica sol and phenolic sol, and make alkaline alcohol-solvent-type silica sol by self-made. , and mix it with the phenolic resin sol system, adopt high-temperature sol-gel reaction, and obtain the silica / phenolic binary composite airgel material under normal pressure drying conditions. This method uses alkaline silica sol as the silicon source. Compared with the traditional acidic silica sol, it can better match the alkalinity of the phenolic curing system, which increases the room temperature stability of the composite sol and makes the application of the actual industrial process At the same time, this matching property effectively promotes the formation of the hybrid airgel interpenetrating network structure.

Description

technical field [0001] The invention relates to a composite airgel with an organic-inorganic double network structure and a preparation method thereof, in particular to a silicon oxide / phenolic binary airgel and a preparation method thereof, which can be used in the technical field of light heat protection. Background technique [0002] Phenolic materials, as ablation-resistant materials, are widely used in aerospace and various cutting-edge fields of national defense. In recent years, phenolic aerogels have attracted more and more attention from researchers because of their low price, light weight, high mechanical strength, and low thermal conductivity. As the aerodynamic and thermal environment of various high-speed aircraft is getting worse and worse, ordinary organic phenolic aerogels have obvious deficiencies in high temperature ablation resistance, heat insulation and oxidation resistance, which greatly limits the application of materials, improving and Improving the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L61/14C08L61/06C08K3/36C08J9/28
CPCC08J9/28C08J2361/14C08J2361/06C08K3/36C08J2205/026
Inventor 孔德隆刘韬刘圆圆徐春晓郭慧李健李文静杨洁颖
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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