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A kind of halogen-free high-efficiency flame retardant, flame retardant epoxy resin and preparation method thereof

A technology of epoxy resin and solid epoxy resin, applied in the field of composite materials, can solve the problems of harsh reaction conditions of flame retardant epoxy resin, too high flame retardant addition, poor heat resistance of flame retardant epoxy resin, etc. Achieve excellent transparency, good plasticity, good flame retardant effect

Active Publication Date: 2022-08-05
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The addition method is generally modified by directly adding a halogen-free powder flame retardant to the epoxy resin structure. The flame retardant and the epoxy resin are physically mixed, which will increase the flame retardancy of the epoxy resin to a greater extent. The viscosity of the epoxy resin reduces the process performance of the resin, the amount of flame retardant added should not be too high, and the improvement of flame retardant performance is limited
The modified polymerization method is to carry out modified polymerization of epoxy resin and reactive phosphorus-containing compounds. The reaction conditions for the preparation of flame-retardant epoxy resins by this method are harsh, the processing is difficult, and the phosphorus-containing substances are generally at the modified addition end. Non-main chain, resulting in poor heat resistance of flame retardant epoxy resin

Method used

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  • A kind of halogen-free high-efficiency flame retardant, flame retardant epoxy resin and preparation method thereof
  • A kind of halogen-free high-efficiency flame retardant, flame retardant epoxy resin and preparation method thereof
  • A kind of halogen-free high-efficiency flame retardant, flame retardant epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of flame retardant:

[0035] In the reactor with gas outlet, add 372g of dimethyl methylphosphonate, add 6g of catalyst sodium carbonate simultaneously, turn on stirring, start to heat up, when the temperature reaches 120 ° C, start to drip tris(2) phosphoric acid into the reactor -Chloroethyl) ester 285g, along with the dropwise addition, there will be a reaction gas methyl chloride to generate, the reaction gas enters the refrigeration compression unit after being condensed by the reactor gas outlet through the condenser to recover, and the dripping is completed, and continue to be slowly warmed up to 160 ℃ Continue the reaction and wait until there is basically no gas discharged, indicating that the reaction is basically complete, and a halogen-free high-efficiency flame retardant is obtained.

[0036] Epoxy Formulation:

[0037]

[0038] The preparation process is as follows:

[0039] In the first step, a certain amount of low-viscosity epoxy resin,...

Embodiment 2

[0044] Preparation of flame retardant:

[0045] In the reactor with gas outlet, add 372g of dimethyl methylphosphonate, add 6g of catalyst sodium hydroxide simultaneously, turn on stirring, start to heat up, when the temperature reaches 120 ° C, start to drip tris(phosphoric acid) into the reactor. 2-Chloroethyl) ester 300g, along with the dropwise addition, there will be reaction gas methyl chloride to generate, and the reaction gas enters the refrigeration compression unit after being condensed by the reactor gas outlet through the condenser and reclaims, and the dripping is completed, and the temperature is continued to be slowly raised to 160 ℃. The reaction is continued at ℃, and when there is basically no gas discharged, it indicates that the reaction is basically complete, and a halogen-free high-efficiency flame retardant is obtained.

[0046] Epoxy Formulation:

[0047]

[0048] The preparation process is as follows:

[0049] In the first step, a certain amount o...

Embodiment 3

[0054] Preparation of flame retardant:

[0055] In the reactor with gas outlet, add 372g of dimethyl methylphosphonate, add 6g of catalyst sodium ethoxide simultaneously, turn on stirring, start to heat up, when the temperature reaches 120 ° C, start to drip tris(2) phosphoric acid into the reactor -Chloroethyl) ester 300g, along with the dropwise addition, there will be reaction gas methyl chloride to generate, and the reaction gas enters the refrigeration compression unit after being condensed by the reactor gas outlet through the condenser to recover, and the dripping is completed, and continue to be slowly warmed up to 160 ℃ Continue the reaction and wait until there is basically no gas discharged, indicating that the reaction is basically complete, and a halogen-free high-efficiency flame retardant is obtained.

[0056] Epoxy Formulation:

[0057]

[0058] The preparation process is as follows:

[0059] In the first step, a certain amount of low-viscosity epoxy resin, ...

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Abstract

The invention provides a halogen-free high-efficiency flame retardant, a flame retardant epoxy resin and a preparation method thereof. The structural formula of the halogen-free high-efficiency flame retardant is: the halogen-free high-efficiency flame retardant is synthesized by the following method: adding dimethyl methylphosphonate, tris(2-chloroethyl) phosphate and a catalyst into a reaction device, The temperature is raised to 100-180°C, and the reaction is carried out for 2-10 hours under stirring conditions. When no gas is generated in the reaction system, the reaction is completed and the product is obtained; the flame-retardant epoxy resin using the halogen-free high-efficiency flame retardant includes low-viscosity epoxy resin Resins, solid epoxy resins, halogen-free high-efficiency flame retardants, toughening agents, curing agents and accelerators. The halogen-free high-efficiency flame retardant prepared by the invention has high phosphorus content and large molecular weight, and the flame retardant epoxy resin has good flame retardant effect and is not easy to separate out.

Description

technical field [0001] The invention relates to a preparation method of a halogen-free high-efficiency flame retardant, and also relates to a flame-retardant epoxy resin using the halogen-free high-efficiency flame retardant and a preparation method thereof, belonging to the technical field of composite materials. Background technique [0002] Epoxy resin is generally a kind of resin whose end group is epoxy group, which is obtained by reacting phenolic compound with epichlorohydrin. With the development of the electrical and electronic industry, epoxy resin has been widely used in electronic circuit substrates and electrical insulating boards because of its good heat resistance, dimensional stability, modulus and rigidity, as well as excellent adhesion to metals. [0003] Due to fire protection requirements, electronic circuit substrates and electrical insulation boards have strict flame retardant requirements. The epoxy resin has the possibility of burning under high temp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5333C08L63/00C08L75/04C07F9/40
CPCC08K5/5333C08L63/00C08L75/04C07F9/4006C07F9/4075C08L2201/02C08L2201/22C08L2205/03C08L2205/025C08L2201/10
Inventor 董大为欧秋仁陈哲明周子群李阳
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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