Method for modifying epoxy resin through phosphorus/nitrogen/silicon synergistic flame retardance

An epoxy resin and synergistic flame-retardant technology, applied in the field of flame-retardant materials, can solve the problems of reducing the mechanical properties and poor compatibility of flame-retardant products, and achieve the effects of improving heat release rate, easy control, and improving dispersion

Active Publication Date: 2021-01-12
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of practical application and production, MPP still has certain defects, such as: poor compatibility with the matrix; reducing the mechanical properties of flame-retardant products, etc.

Method used

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  • Method for modifying epoxy resin through phosphorus/nitrogen/silicon synergistic flame retardance
  • Method for modifying epoxy resin through phosphorus/nitrogen/silicon synergistic flame retardance
  • Method for modifying epoxy resin through phosphorus/nitrogen/silicon synergistic flame retardance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Melamine polyphosphate MPP and siloxane halogen-free cyclotriphosphazene APESP were baked in a vacuum oven at 80°C for 6 hours; 4.38g of APESP was dissolved in 150ml of absolute ethanol. Mix; add 39.42g of dried MPP to the APESP solution, place the three-neck flask in an oil bath, and stir for 30 minutes while raising the temperature to 80°C; then use a rotary evaporator to evaporate the ethanol at 60°C, The obtained remaining solid was put into a vacuum oven and baked at 80°C for 8 hours. When the mass became constant, it was taken out and ground into powder, and stored in a desiccator to obtain an APESP modified melamine polyphosphate flame retardant; Weigh 292g of dried bisphenol A epoxy resin prepolymer E-44 epoxy resin in a three-necked flask, and place it in an oil bath at 140°C for preheating; 20g of modified melamine polyphosphate flame retardant Add the curing agent into the three-necked flask, stir at 140°C for 30 minutes, and stir thoroughly with a mechanical...

Embodiment 2

[0033] Melamine polyphosphate MPP and siloxane halogen-free cyclotriphosphazene APESP were baked in a vacuum oven at 80°C for 6 hours; 4.38g of APESP was dissolved in 150ml of absolute ethanol, and placed in a three-necked flask at room temperature Mix well; add 17.52g of dried MPP to the APESP solution, place the three-necked flask in an oil bath, and stir for 30 minutes while raising the temperature to 80°C; then use a rotary evaporator to evaporate the ethanol to dryness at 60°C , put the remaining solid obtained in a vacuum oven at 80°C and bake for 8 hours. When the mass becomes constant, take it out and grind it into powder, and store it in a desiccator to obtain APESP modified melamine polyphosphate flame retardant ; Weigh 292g of dried bisphenol A epoxy resin prepolymer E-44 epoxy resin in a three-necked flask and place it in an oil bath at 140°C for preheating; 20g of modified melamine polyphosphate resistance Put the fuel into the three-necked flask, stir at 140°C fo...

Embodiment 3

[0035] Melamine polyphosphate MPP and siloxane halogen-free cyclotriphosphazene APESP were baked in a vacuum oven at 80°C for 6 hours; 4.38g of APESP was dissolved in 150ml of absolute ethanol, and placed in a three-necked flask at room temperature Mix well; add 17.52g of dried MPP to the APESP solution, place the three-necked flask in an oil bath, and stir for 30 minutes while raising the temperature to 60°C; then use a rotary evaporator to evaporate the ethanol to dryness at 60°C , put the remaining solid obtained in a vacuum oven at 80°C and bake for 8 hours. When the mass becomes constant, take it out and grind it into powder, and store it in a desiccator to obtain APESP modified melamine polyphosphate flame retardant ; Weigh 292g of dried bisphenol A epoxy resin prepolymer E-44 epoxy resin in a three-necked flask and place it in an oil bath at 100°C for preheating; 20g of modified melamine polyphosphate resistance Put the fuel into the three-necked flask, stir for 30 minu...

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Abstract

The invention relates to a method for modifying epoxy resin through phosphorus / nitrogen / silicon synergistic flame retardance based on an organic-inorganic hybridization technology, and belongs to thetechnical field of flame-retardant materials. According to the method, a cyclic phosphazene derivative grafted with a silicon functional group is used as a surface modifier; melamine polyphosphate isadded into an APESP solution system, stirring, heating, and drying are conducted to coat the surfaces of the MPP particles with APESP, thereby obtaining a novel modified melamine polyphosphate flame retardant based on the organic-inorganic hybridization technology. The siloxane halogen-free cyclotriphosphazene modified melamine polyphosphate flame retardant prepared by the invention is applied toa flame-retardant epoxy resin system; and the novel flame retardant integrating three flame-retardant elements of silicon, phosphorus and nitrogen based on the organic-inorganic hybridization technology is applied to an epoxy resin system, and the oxygen index, the vertical combustion level and the heat release rate of the obtained flame-retardant modified epoxy resin are remarkably improved.

Description

technical field [0001] The invention relates to a method for phosphorus / nitrogen / silicon synergistic flame-retardant modified epoxy resin based on organic-inorganic hybrid technology, and belongs to the technical field of flame-retardant materials. Background technique [0002] Epoxy resin (EP), as a thermosetting polymer material with a large amount of use, has excellent thermal stability, chemical stability, mechanical properties, processing properties, electrical properties, etc., and is widely used in electronic components, aerospace materials, coatings, etc. The field has wide application. However, the flame retardancy of epoxy resin is poor, and the limiting oxygen index (LOI) is only 19.8%. Therefore, flame retardant modification is generally required to meet the wider use requirements of epoxy resin in various fields. [0003] At present, the phosphorus nitrogen flame retardants used in epoxy resin mainly include: red phosphorus, polyphosphate (APP), melamine polyph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08K9/10C08K5/3492C08K5/5399C08G59/50
CPCC08G59/5033C08G59/504C08K5/34928C08K5/5399C08K9/10C08L2201/02C08L63/00
Inventor 李定华刘霖靖史亚丽杨荣杰
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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