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Intumescent compound flame retardant modified epoxy resin material with high thermal stability and preparation method of intumescent compound flame retardant modified epoxy resin material

A technology of compounding flame retardants and high thermal stability, which is applied in the field of resin-based composite materials, can solve the problems of not being able to meet processing requirements, lower thermal stability, and low flame retardant efficiency, and achieve low raw material prices and excellent thermal stability , Improve the effect of flame retardant efficiency

Pending Publication Date: 2022-03-22
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the reported intumescent flame retardants often have poor compatibility with the matrix after addition, resulting in difficulty in dispersion, resulting in a sharp drop in the initial decomposition temperature of the flame-retardant modified epoxy resin material, resulting in a sharp drop in thermal stability. Reduce the phenomenon, so it can not meet the processing requirements of medium and high-grade plastics, and the flame retardant efficiency is low
It can be seen that it is still a great challenge to obtain flame-retardant modified epoxy resin materials with high thermal stability and high flame-retardant efficiency.

Method used

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  • Intumescent compound flame retardant modified epoxy resin material with high thermal stability and preparation method of intumescent compound flame retardant modified epoxy resin material
  • Intumescent compound flame retardant modified epoxy resin material with high thermal stability and preparation method of intumescent compound flame retardant modified epoxy resin material
  • Intumescent compound flame retardant modified epoxy resin material with high thermal stability and preparation method of intumescent compound flame retardant modified epoxy resin material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The preparation of embodiment 1 focused piperazine phosphates

[0040] Under nitrogen protection, first add phosphoric acid (concentration 85%) 86g in the five-necked flask; Add anhydrous piperazine 32g and 20g distilled water in the beaker, after dissolving at 45 ℃, add dropwise to five-necked flask through constant pressure dropping funnel Then, the temperature of the reaction solution was raised to 95° C., and the reaction was stopped after 2 hours of reaction. After cooling to room temperature, the reaction solution was filtered, rinsed and dried to obtain 97 g of the intermediate piperazine diphosphate. Put piperazine diphosphate into a rotary evaporator for vacuum dehydration. First, carry out nitrogen replacement, and then vacuumize to an absolute pressure of 20 mmHg. The heating rate was controlled, and the temperature was gradually raised to a dehydration temperature of 280° C. and a dehydration time of 3 hours, and finally 91.6 g of piperazine focused phospha...

Embodiment 2

[0041] The preparation of embodiment 2 focused piperazine phosphates

[0042] Under nitrogen protection, first add phosphoric acid (concentration 85%) 86g in the five-necked flask; Add anhydrous piperazine 32g and 20g distilled water in the beaker, after dissolving at 45 ℃, add dropwise to five-necked flask through constant pressure dropping funnel Then, the temperature of the reaction solution was raised to 85°C, and the reaction was stopped after 3 hours of reaction. After cooling to room temperature, the reaction solution was filtered, rinsed and dried to obtain 96.8 g of intermediate piperazine diphosphate. Put piperazine diphosphate into a rotary evaporator for vacuum dehydration. First, carry out nitrogen replacement, and then vacuumize, the absolute pressure is 60mmHg. The heating rate was controlled, and the temperature was gradually raised to a dehydration temperature of 260° C., and a dehydration time of 2 hours, to finally obtain 92.1 g of piperazine-focused phosph...

Embodiment 3

[0043] The preparation of embodiment 3 focused piperazine phosphates

[0044] Under nitrogen protection, first add phosphoric acid (concentration 85%) 86g in the five-necked flask; Add anhydrous piperazine 32g and 20g distilled water in the beaker, after dissolving at 45 ℃, add dropwise to five-necked flask through constant pressure dropping funnel Then, the temperature of the reaction solution was raised to 90°C, and the reaction was stopped after 2.5 hours of reaction. After cooling to room temperature, the reaction solution was filtered, rinsed and dried to obtain 96.6 g of the intermediate piperazine diphosphate. Put piperazine diphosphate into a rotary evaporator for vacuum dehydration. First, carry out nitrogen replacement, and then vacuumize, the absolute pressure is 40mmHg. The heating rate was controlled, and the temperature was gradually raised to a dehydration temperature of 270° C. and a dehydration time of 2.5 hours, and finally 91.8 g of focused piperazine phosp...

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Abstract

The invention provides an intumescent compound flame retardant modified epoxy resin material with high thermal stability and a preparation method of the intumescent compound flame retardant modified epoxy resin material. The preparation method comprises the following steps: blending focused piperazine phosphate, halloysite nanotubes and melamine cyanurate according to a mass ratio of (5-8): (1-2): (4-1) to prepare a P-N-Si intumescent compound flame retardant; the flame retardant is prepared from the following components in percentage by weight: 55-83.6% of epoxy resin, 4.4-20% of intumescent compound flame retardant and 12-25% of curing agent, and is added into epoxy resin for flame-retardant modification. According to the method, a novel P-N-Si intumescent compound flame retardant is formed by synthesizing a P-N flame retardant with high thermal stability at low cost and adding a small amount of Si and N flame retardants, the flame-retardant material prepared by the method has good interfacial compatibility and thermal stability and excellent flame-retardant efficiency, the flame retardance of modified epoxy resin can reach UL94 V-0 grade, and the flame-retardant property of the modified epoxy resin can reach UL94 V-0 grade. And the limit oxygen index can reach 34.3%.

Description

technical field [0001] The invention belongs to the field of resin-based composite materials, and in particular relates to a high thermal stability expansion-type composite flame retardant modified epoxy resin material and a preparation method thereof. Background technique [0002] Resin-based composite materials have the characteristics of high specific strength and specific stiffness, strong designability, good fatigue fracture resistance, corrosion resistance, good structural stability, and large-scale molding. They are widely used in aerospace, automotive, electronic appliances, and marine industries. The field has wide application. Advanced resin-based composite materials are mostly carbon fiber-reinforced thermosetting resin composite materials, mainly including epoxy resin (EP), bismaleimide resin, polyimide resin and other thermosetting resins. Among them, epoxy resin dominates the market of high-performance composite materials due to its advantages of excellent pro...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08L85/02C08K7/26C08K5/3492
CPCC08L63/00C08L2201/02C08L2201/22C08L85/02C08K7/26C08K5/34928Y02P20/10
Inventor 马静刘美哲汪宝和朱璟
Owner TIANJIN UNIV
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