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Polybenzoxazine airgel thermal insulation material and preparation method thereof

A technology of polybenzoxazine and benzoxazine is applied in the field of thermal insulation materials to achieve the effects of small pore size, low thermal conductivity and low moisture absorption rate

Active Publication Date: 2020-10-09
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems existing in the existing polymer airgel heat insulation materials, the present invention provides a polybenzoxazine airgel heat insulation material and a preparation method thereof

Method used

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  • Polybenzoxazine airgel thermal insulation material and preparation method thereof
  • Polybenzoxazine airgel thermal insulation material and preparation method thereof
  • Polybenzoxazine airgel thermal insulation material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] In the first step, the BO-1 benzoxazine monomer shown in formula I is dissolved in a DMF solvent, stirred until completely dissolved, and a clear and transparent benzoxazine monomer solution with a concentration of 0.05 g / ml is obtained;

[0035] In the second step, hydrochloric acid is added as a catalyst to the benzoxazine monomer solution obtained in the first step, the reaction temperature is 10°C, and the reaction is stirred for 20 minutes to obtain polybenzoxazine sol, wherein hydrochloric acid and monomer The molar ratio is 1:1;

[0036] In the third step, the polybenzoxazine sol obtained in the second step is poured into a container, sealed and left to stand, and polybenzoxazine gel is obtained after 25 hours, and the obtained polybenzoxazine gel is dissolved in DMF solvent After medium aging for 36 hours, the solvent was replaced three times with anhydrous acetone, once every 12 hours, to obtain the polybenzoxazine gel after solvent replacement;

[0037] In th...

Embodiment 2

[0041] In the first step, the BO-2 benzoxazine monomer represented by formula II is dissolved in NMP solvent, stirred until completely dissolved, and a clear and transparent benzoxazine monomer solution with a concentration of 0.20 g / ml is obtained;

[0042] In the second step, oxalic acid is added as a catalyst to the benzoxazine monomer solution obtained in the first step, the reaction temperature is 20°C, and the reaction is stirred for 10 minutes to obtain polybenzoxazine sol, in which oxalic acid and monomer are added The molar ratio is 2:1;

[0043] In the third step, pour the sol obtained in the second step into a container, seal it and let it stand, and obtain a polybenzoxazine gel after 10 hours, and age the obtained polybenzoxazine gel in NMP solvent for 36 hours , using absolute ethanol to perform solvent replacement three times, replacing once every 12 hours, to obtain a polybenzoxazine gel after solvent replacement;

[0044] In the fourth step, the solvent-substi...

Embodiment 3

[0048] In the first step, the BO-3 benzoxazine monomer represented by formula III is dissolved in DMSO solvent, stirred until completely dissolved, and a clear and transparent benzoxazine monomer solution with a concentration of 0.30 g / ml is obtained;

[0049] In the second step, nitric acid is added as a catalyst to the benzoxazine monomer solution obtained in the first step, the reaction temperature is 50°C, and the reaction is stirred for 30 minutes to obtain polybenzoxazine sol, wherein nitric acid and monomer are added The molar ratio is 1.5:1;

[0050] In the third step, the sol obtained in the second step is poured into a container, sealed and left to stand, and polybenzoxazine gel is obtained after 4 hours, and the obtained polybenzoxazine gel is aged in DMSO solvent for 24 hours , using anhydrous acetone to perform solvent replacement three times, replacing once every 8 hours, to obtain a polybenzoxazine gel after solvent replacement;

[0051] In the fourth step, the...

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Abstract

The invention discloses a polybenzoxazine aerogel heat thermal insulation material and a preparation method thereof. The polybenzoxazine aerogel heat thermal insulation material is characterized in that a bisphenol A benzoxazine monomer is used as a base raw material, polybenzoxazine is obtained by adopting acid-catalysed ring opening polymerization, and the polybenzoxazine comprises three structures corresponding to a structural formula 1. According to the preparation method, a sol-gel method is adopted; acid catalysis ring opening polymerization is carried out at the normal temperature to obtain gel with a three-dimensional network structure; then the gel is subjected to aging, solvent replacement, CO2 supercritical drying and programmed warming and heat preservation processing to obtainthe polybenzoxazine aerogel heat thermal insulation material. The material disclosed by the invention has excellent performance of low moisture absorption, high intensity, flame retardance, low density, low thermal conductivity and the like; the preparation method is simple in process; prices of raw materials are low; low-temperature ring opening polymerization avoids a high-temperature reaction;the polybenzoxazine aerogel heat thermal insulation material and the preparation method thereof have low requirements for the environment, are short in time consumption in the overall process flow and are suitable for industrial production.

Description

technical field [0001] The invention specifically relates to a polybenzoxazine airgel heat insulation material and a preparation method thereof, belonging to the field of heat insulation materials. Background technique [0002] With the progress of society, the continuous development of industry, the demand for energy continues to increase, the contradiction between energy and demand is becoming more and more acute, and the energy crisis has become a global problem. The research and production of thermal insulation materials, especially high-performance thermal insulation materials, can greatly reduce the energy consumption of industrial, construction and civil living equipment, thereby alleviating the contradiction between energy supply and demand, and reducing environmental pollution and greenhouse effect. [0003] As a new type of high-efficiency thermal insulation material, airgel thermal insulation material is one of the research hotspots of high-performance thermal ins...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/02C08G14/06C08J9/28
CPCC08G14/06C08G73/02C08J9/28C08J2201/0484C08J2361/34C08J2379/02
Inventor 冯坚肖芸芸姜勇刚冯军宗杜东轩
Owner NAT UNIV OF DEFENSE TECH
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