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Flame-retardant epoxy resin composition, preparation method and application thereof

A technology of epoxy resin and composition, which is applied in the field of flame retardant epoxy resin composition and its preparation, can solve the problems of inability to achieve environmentally friendly flame retardant, the existence of environmental hazards, and the impact on the flexibility of epoxy resin, etc., to achieve Efficient and environmentally friendly flame retardant effect, avoiding precipitation or hydrolysis, and avoiding the effect of small molecule precipitation

Pending Publication Date: 2021-03-12
GUANGDONG GUANGSHAN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the existing field of flame retardant epoxy resins, the flame retardant efficiency of epoxy resins containing inorganic additive flame retardants such as aluminum hydroxide hydrate and magnesium hydroxide hydrate is low, and adding a large amount of inorganic flame retardants will not only affect the environment The flexibility of the epoxy resin itself makes the resin hard and brittle, and it will reduce the acid and alkali resistance of the epoxy resin
Although the flame-retardant epoxy resin containing bromine and other halogens has excellent flame-retardant performance, it will produce dioxin and other difficult-to-degrade products when burned, causing serious environmental pollution and endangering human health.
Although epoxy resins containing nitrogen / phosphorus flame retardants avoid the pollution caused by combustion products such as dioxins, there are still environmental hazards. Nitrogen / phosphorus flame retardants have Migration, precipitation, and most additive flame retardants are easy to hydrolyze and other reasons, their molecules or decomposition products or water-soluble substances will enter the environment, pollute the environment, and cannot be truly environmentally friendly flame retardant

Method used

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  • Flame-retardant epoxy resin composition, preparation method and application thereof
  • Flame-retardant epoxy resin composition, preparation method and application thereof
  • Flame-retardant epoxy resin composition, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0094] A flame retardant curing agent, the structure is as follows:

[0095]

[0096] The preparation method is as follows:

[0097] Add 1mol of 2,3-dihydroxystyrene, 1mol of DOPO and 50mL of glacial acetic acid into the reaction kettle, heat to 50°C under stirring, then add 1mmol of Pb catalyst solution of glacial acetic acid dropwise into the reaction system, and react for 16h; Separation and purification to obtain the target product.

[0098] 1 H NMR (CDCl 3 ,400MHz,TMS):δ9.35-9.51(d,2H,-OH),7.21-7.94(m,8H,H of benzene ring),6.41-6.65(m,3H,H of benzene ring),2.71- 2.84(m,1H,-CH-),1.47-1.61(t,3H,-CH 3 ).

preparation example 2

[0100] A flame retardant curing agent, the structure is as follows:

[0101]

[0102] The preparation method is as follows:

[0103] Add 1mol of dimethyl phosphite, 1mol of trans-3,5-dihydroxystilbene and 50mL of glacial acetic acid into the reactor, and heat to 55°C under stirring; Glacial acetic acid solution was added dropwise to the reaction system, and reacted for 15 hours; the product was separated to obtain the target product.

[0104] 1 H NMR (CDCl 3 , 400MHz, TMS): δ9.31-9.52 (s, 2H, -OH), 7.15-7.28 (m, 5H, H of the benzene ring), 6.17-6.31 (m, 3H, H of the benzene ring), 3.68- 3.81(d,6H,-CH 3 ),3.13-3.24(m,1H,-CH-),2.98-3.07(m,2H,-CH 2 -).

preparation example 3

[0106] A flame retardant curing agent, the structure is as follows:

[0107]

[0108] The preparation method is as follows:

[0109] Add 1 mol of dimethyl phosphite and 1 mol of 2,5-dihydroxybenzaldehyde into the reaction kettle, control the temperature in an ice bath at 0-3°C, add 1 mol of triethylamine dropwise under stirring, then gradually raise the temperature to 50°C, continue After reacting for 2h, the target product was obtained by distillation under reduced pressure.

[0110] 1 H NMR (CDCl 3 , 400MHz, TMS): δ9.31-9.57 (d, 2H, -OH), 6.69-6.93 (m, 3H, H of the benzene ring), 6.58-6.64 (m, 1H, -OH), 4.78-4.86 ( d,6H,-CH-),3.46-3.62(d,6H,-CH 3 ).

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Abstract

The invention provides a flame-retardant epoxy resin composition, a preparation method and application thereof. The flame-retardant epoxy resin composition is prepared from epoxy resin, a flame-retardant curing agent and a curing accelerator, wherein the flame-retardant curing agent has a structure shown in a formula I and contains phenolic hydroxyl and phosphorus-containing flame-retardant groups. According to the invention, phenolic hydroxyl in the flame-retardant curing agent and epoxy resin are subjected to a curing reaction, the curing efficiency is high, flame-retardant groups finally exist in the flame-retardant epoxy resin composition in the form of molecular fragments, the phenomenon that small molecules are separated out is avoided, the phenomenon that some additive flame retardants are easily dissolved in water to be separated out or hydrolyzed is also avoided, and high-efficiency environment-friendly flame retardance is truly realized; and the flame-retardant epoxy resin composition provided by the invention has excellent flame-retardant performance and mechanical performance, a copper-clad plate prepared from the flame-retardant epoxy resin composition has high flame-retardant performance and dielectric performance, the preparation process is simple, the raw materials are easy to obtain, and the flame-retardant epoxy resin composition has a wide industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a flame-retardant epoxy resin composition and a preparation method and application thereof. Background technique [0002] Epoxy resin is a very important thermosetting resin, which has excellent bonding performance, electrical insulation, wear resistance, chemical stability and mechanical properties, and has low shrinkage rate and is easy to process and shape. It is widely used in instruments, aviation Epoxy resin is one of the most commonly used polymer matrices in the fields of aerospace, adhesives, and electrical and electronic insulation materials, especially in the processing and manufacturing of copper-clad laminates, the basic materials of the electronics industry. However, the limiting oxygen index (LOI) of epoxy resin is low, it is easy to burn, and its flame retardant performance is not good. It is easy to catch fire under high temperature or stati...

Claims

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Application Information

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IPC IPC(8): C08G59/62C08L63/00C08K3/36
CPCC08G59/621C08K3/36C08L63/00
Inventor 潘庆崇
Owner GUANGDONG GUANGSHAN NEW MATERIALS CO LTD
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