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Flame-retardant epoxy resin as well as preparation method and application thereof

A technology of epoxy resin and resin, which is applied in the field of flame retardant epoxy resin and its preparation, can solve the problems of low flame retardant efficiency, agglomeration of flame retardant particles, and decreased stability of flame retardant effect, and achieve high flame retardant performance, The effect of high physical and mechanical properties and good thermal stability

Pending Publication Date: 2021-10-01
CRRC QINGDAO SIFANG CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] CN108727782A used an additive flame retardant with a core-shell structure, which easily caused the particles of the flame retardant to agglomerate during use, resulting in stress concentration points and reducing the mechanical properties of epoxy resin; and because it was difficult to control the uniform particle size and particle size Dispersion, the stability of its flame retardant effect will also decrease to a certain extent
The flame retardant disclosed in CN106700416A is a blend of various inorganic substances, which is convenient to use, but the flame retardant efficiency is low, and a large dose of flame retardant must be added to have a flame retardant effect; in this method, the inorganic flame retardant The quality of the epoxy resin is twice that of the epoxy resin, such a high addition amount will have a negative impact on the industrial production cost and the overall performance of the resin

Method used

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  • Flame-retardant epoxy resin as well as preparation method and application thereof

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Effect test

Embodiment 1

[0064] This embodiment provides a preparation method of flame retardant epoxy resin, the steps are as follows:

[0065] (1) Synthesis of phosphorus-containing flame retardant curing agent DOPO-MAH:

[0066] 200ml of xylene was placed in a three-necked flask as a solvent, and 60g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) was dissolved in it, and then divided into batches within 30min Add 27.2g of maleic acid (MA), react at a temperature of 125°C for 6h, then cool down to 80°C, add 150ml of tetrahydrofuran into the system, react for 2h, then filter with suction, wash with THF for 3 times, and then filter with suction , to obtain DOPO-maleic acid (DOPO-MA).

[0067] Pour the obtained DOPO-MA and 82ml of acetic anhydride into a three-necked flask, then react in a constant temperature water bath at 130°C for 4.5h, filter with suction, wash twice with acetic anhydride, and filter with suction again to obtain DOPO-maleic acid Anhydride (DOPO-MAH) phosphorus-conta...

Embodiment 2

[0079] This embodiment provides a preparation method of flame retardant epoxy resin, the steps are as follows:

[0080] (1) Synthesis of phosphorus-containing flame retardant curing agent:

[0081] 250ml of xylene was placed in a three-necked flask as a solvent, and 80g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) was dissolved in it, and then added in batches within 40min 35.4g maleic acid (MA), the two reacted at 130°C for 6.5h, then cooled to 85°C, added 200ml tetrahydrofuran into the system, reacted for 2.5h, filtered with suction, washed twice with tetrahydrofuran, and pumped again Filter to obtain DOPO-maleic acid (DOPO-MA).

[0082] Pour the obtained DOPO-MA and 110ml of acetic anhydride into a three-necked flask, then react in a constant temperature water bath at 130°C for 5 hours, filter with suction, wash with acetic anhydride twice, and filter with suction again to obtain DOPO-maleic anhydride (DOPO-MAH) Phosphorous curing agent.

[0083] (2) Synt...

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Abstract

The invention relates to the technical field of epoxy resin for fiber composite materials, in particular to flame-retardant epoxy resin as well as a preparation method and an application thereof. According to the preparation method of the flame-retardant epoxy resin provided by the invention, epoxy silicate resin is taken as a matrix, and the epoxy resin is subjected to flame-retardant modification according to a P-N-Si synergistic flame-retardant principle under the action of an anhydride curing agent, a phosphorus-containing flame-retardant curing agent and a synergistic flame retardant. The DOPO-MAH is selected as a flame-retardant curing agent, so that poison gas generated by combustion of a halogen flame retardant is avoided, and the problem that an additive flame retardant is poor in dispersity and compatibility is solved; meanwhile, an imidazole curing accelerator is selected, so that the curing temperature can be reduced, and the effect of a synergistic flame retardant can be achieved. According to the invention, DOPO and silicon-oxygen bonds are introduced into a resin system through chemical bonds, and the modified silicon element can cooperate with nitrogen and phosphorus elements, so that the flame retardant property of the epoxy resin is improved, and the mechanical property of the epoxy resin can also be improved.

Description

technical field [0001] The invention relates to the technical field of epoxy resin for fiber composite materials, in particular to a flame-retardant epoxy resin and its preparation method and application. Background technique [0002] Carbon fiber reinforced resin matrix composites (CFRP) have the characteristics of light weight, high strength, high temperature resistance, corrosion resistance, fatigue resistance, low expansion coefficient and good comprehensive performance, and are the most important structural composite materials. The specific strength of CFRP is 4.8 to 7.2 times that of steel, the specific modulus is 3.1 to 4.2 times that of steel, and the fatigue strength is about 2.5 times that of steel and 3.3 times that of aluminum, which is unmatched by other fiber reinforced composite materials. Carbon fiber composite materials are used as structural materials and high temperature and ablation resistant materials, and have been widely used in advanced equipment, def...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/14C08G59/42C08G59/68C08J5/04C08L63/02
CPCC08G59/1438C08G59/145C08G59/1477C08G59/686C08G59/4238C08G59/423C08G59/4215C08J5/04C08J2363/02
Inventor 刘鹏清王建军许启彬丁叁叁徐建军
Owner CRRC QINGDAO SIFANG CO LTD
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