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Preparation method of high-compression-resistance fire-resistant composite epoxy foam

A fire-resistant, composite ring technology, applied in the field of epoxy foam, can solve the problems of reducing the cell size, strengthening the cell wall, reducing the activity of benzyl hydroxyl, etc., to increase the initial decomposition temperature, improve flame resistance, and shorten the gel the effect of time

Active Publication Date: 2022-07-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the above problems, the present invention is based on the principle that the activity of benzyl hydroxyl group is controllable, and the structure of epoxy novolac resin is modified, and the boron-oxygen bond is introduced into the molecular structure of the resin, which effectively improves the decomposition temperature and carbon residue rate of the resin. It provides a foaming matrix for the preparation of refractory foam materials, and reduces the activity of benzyl hydroxyl groups in the resin synthesis process by using weakly alkaline ammonia water as a catalyst and stepwise heating method, which solves the problem caused by the high activity of benzyl hydroxyl groups in the resin synthesis process. The problem of the loss of epoxy groups and the remaining boric acid; by adding a dual-functional blowing agent with synergistic curing effect in the foaming process, the mismatch between the resin gel and the decomposition of the blowing agent is solved; through The modification of graphene oxide grafted by boron phenolic epoxy resin obtained a multifunctional graphene oxide reinforced particle, which was used as a modifier of epoxy foam, which effectively reduced the cell size, strengthened the cell wall, and promoted During the flame combustion process, a stable and strong graphitized carbon layer is formed on the surface of the foam, and the thermal resistance effect and thermal infrared absorption effect of graphene oxide particles are used to reduce the thermal conductivity. Composite epoxy foam material with high compressive strength, excellent heat insulation performance, and strong shape retention ability in flames, which solves the problem that current epoxy foam materials cannot have both high compressive performance and flame resistance due to insufficient heat resistance of the foamed resin matrix performance problem

Method used

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  • Preparation method of high-compression-resistance fire-resistant composite epoxy foam

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Experimental program
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Effect test

Embodiment 1

[0022] The organic solvent selects n-butanol for use, the mol ratio of bisphenol A diglycidyl ether and formaldehyde is 1:1.2, the mass ratio of ammonia water and bisphenol A diglycidyl ether is 1:50; the mass ratio of boric acid and bisphenol A diglycidyl ether is 1:50; The molar ratio is 1:5; N,N-dimethylformamide is selected as the organic dispersant, sodium hydroxide is selected as the basic catalyst, diethyltoluene diamine is selected as the amine curing agent, and nonylphenol polyoxygen is selected as the surfactant. Vinyl ether and carboxyl-terminated nitrile rubber are selected as the toughening agent. The specific operation steps are as follows:

[0023] (1) the synthesis process of boron novolac epoxy resin: 1) addition reaction: bisphenol A diglycidyl ether and formaldehyde are dissolved in n-butanol, mechanically stirred for 10min, then add the catalyst ammonia water that concentration is 28wt%, heat up The reaction was carried out at 80 °C for 2.5 h; after the rea...

Embodiment 2

[0047] The organic solvent is selected from toluene, the mol ratio of bisphenol A diglycidyl ether and formaldehyde is 1:1.0, the mass ratio of ammonia water and bisphenol A diglycidyl ether is 1:20; the mol ratio of boric acid and bisphenol A diglycidyl ether is 1:20. It is 1:2; n-butanol is selected as organic dispersant, potassium hydroxide is selected as basic catalyst, m-xylylenediamine is selected as amine curing agent, octylphenol polyoxyethylene ether is selected as surfactant, and carboxyl terminal is selected as toughening agent Nitrile rubber, the specific operation steps are as follows:

[0048] (1) Synthesis process of boron novolac epoxy resin: 1) Addition reaction: bisphenol A diglycidyl ether and formaldehyde are dissolved in toluene, mechanically stirred for 5min, then add the catalyst ammonia water with a concentration of 28wt%, be warming up to 90 ℃ reaction for 2h; after the reaction is completed, the temperature is cooled to 50 ℃, and the solution is disti...

Embodiment 3

[0057] The organic solvent selects xylene, the mol ratio of bisphenol A diglycidyl ether and formaldehyde is 1:1.5, the mass ratio of ammonia water and bisphenol A diglycidyl ether is 1:100; the mol of boric acid and bisphenol A diglycidyl ether is 1:100; The ratio is 1:10; the organic dispersant is selected from toluene, the basic catalyst is selected from barium hydroxide, the amine curing agent is selected from diaminodiphenylmethane, the surfactant is selected from sorbitan ester, and the toughening agent is selected from epoxy nitrile rubber , the specific operation steps are as follows:

[0058] (1) Synthesis process of boron novolac epoxy resin: 1) Addition reaction: dissolving bisphenol A diglycidyl ether and formaldehyde in xylene, mechanically stirring for 10min, then adding catalyst ammonia water with a concentration of 28wt%, warming up to Reaction at 85°C for 3h; after the reaction was completed, the temperature was cooled to 55°C, and the solution was distilled u...

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Abstract

The invention relates to the technical field of preparation of epoxy foam materials, and mainly relates to a preparation method of high-pressure-resistant fire-resistant composite epoxy foam. On the basis of the controllable benzyl hydroxyl activity principle, the benzyl hydroxyl activity in the boron novolac epoxy resin synthesis process is reduced by taking ammonia water as a catalyst and adopting a stepped heating method, so that the problems of epoxy value reduction and boric acid residue caused by over-high benzyl hydroxyl activity in resin synthesis are solved; the boron-containing high-temperature-resistant foaming resin matrix is successfully prepared; a bifunctional foaming agent with a synergistic curing effect is added in the foaming process, so that the problem that resin gel and foaming agent decomposition are not matched is solved; boron novolac epoxy resin grafted and modified graphene oxide is added into epoxy foam, so that the size of a foam hole is reduced, the wall of the foam hole is enhanced, the surface of the epoxy foam is promoted to form a stable graphitized carbon layer in flame, the heat conductivity is reduced, and finally the epoxy foam material integrating compression resistance, heat insulation and flame resistance functions is prepared.

Description

technical field [0001] The invention relates to the technical field of epoxy foam, and mainly relates to a preparation method of a high-pressure and fire-resistant composite epoxy foam. Background technique [0002] With the rapid development of aerospace, rail transit, automobile and other industries, the problem of massive energy consumption has become increasingly severe, and the use of lightweight and high-strength materials is an important way to reduce energy consumption. Compared with metal materials, foam materials made from polymers have received extensive attention in the industry due to their high specific strength, low density, low thermal conductivity and low cost. However, due to the heat resistance of the polymer foam matrix. Poor, polymer foam materials cannot maintain excellent compressive performance in flames. How to improve the flame resistance performance of polymer foam materials while maintaining high mechanical strength is a scientific problem that ne...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/04C08K3/04C08J9/10C08J9/00C08G59/14
CPCC08J9/105C08J9/0066C08G59/1405C08J2363/04C08J2203/04C08K3/042Y02P20/10
Inventor 贾晓龙吉早明黎何丰还献华郭天乐朱家宝杨小平
Owner BEIJING UNIV OF CHEM TECH
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