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Preparation of phosphorus-containing bismaleimide and application thereof in flame-retardant epoxy resin

A kind of bismaleimide, maleimide technology, applied in the application of flame retardant epoxy resin, the preparation field of phosphorus-containing bismaleimide, can solve the flame retardant performance of epoxy resin, mechanical It is difficult to balance the performance and heat resistance, so as to achieve the effect of significant flame retardant effect, mild reaction conditions and improved flame retardant performance.

Active Publication Date: 2019-04-05
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides a synthesis method of a novel phosphorous-containing bismaleimide and its application in a flame-retardant epoxy resin. This type of compound can be cross-linked with an epoxy resin under the action of an amine curing agent to form an interpenetrating polymer network. The maleimide group of the structure, especially compared with the prior art, has the advantages of simple preparation process, mildness, and low energy consumption, and has the advantages of low addition and high-efficiency flame-retardant epoxy resin, and the addition amount is controlled at 4 The epoxy resin can pass the V-0 level of vertical combustion, and the limiting oxygen index can reach more than 30%, which solves the contradiction between the flame retardancy, mechanical properties and heat resistance of epoxy resin that is difficult to balance

Method used

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  • Preparation of phosphorus-containing bismaleimide and application thereof in flame-retardant epoxy resin
  • Preparation of phosphorus-containing bismaleimide and application thereof in flame-retardant epoxy resin
  • Preparation of phosphorus-containing bismaleimide and application thereof in flame-retardant epoxy resin

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Embodiment 1

[0028] The preparation method of described phosphorus-containing bismaleimide:

[0029] (1) In a 250mL reaction vessel equipped with stirring, add 7.65g of N-(4-hydroxyphenyl)maleimide and 50mL of tetrahydrofuran under ice-cooling, and dissolve them by magnetic stirring; after completely dissolving, add triethyl Amine 5.3g, continue stirring until uniformly mixed. Then, at 5-7° C., 4.5 g of a mixed solution of phenyl dichlorophosphate and tetrahydrofuran was added dropwise into the above-mentioned reaction vessel, and the system gradually produced white precipitates.

[0030] (2) After the solution was added dropwise, the system was reacted at room temperature for 10 h, the white precipitate triethylamine hydrochloride was filtered and then distilled under reduced pressure, purified and dried with ethyl acetate and petroleum ether to obtain a light yellow solid product, the yield was was 91.7%.

Embodiment 2

[0032] The preparation method of described phosphorus-containing bismaleimide:

[0033] (1) In a 250mL reaction vessel equipped with stirring, add 7.65g of N-(4-hydroxyphenyl)maleimide and 50mL of tetrahydrofuran under ice-cooling, and dissolve them by magnetic stirring; after completely dissolving, add triethyl Amine 4.89g, continue stirring until uniformly mixed. Then, at 5-7° C., 4.5 g of a mixed solution of phenyl dichlorophosphate and tetrahydrofuran was added dropwise into the above-mentioned reaction vessel, and the system gradually produced white precipitates.

[0034] (2) After the solution was added dropwise, the system was reacted at room temperature for 12 hours, the white precipitate triethylamine hydrochloride was filtered and then distilled under reduced pressure, purified and dried with ethyl acetate and petroleum ether to obtain a light yellow solid product, the yield was 92.5%.

Embodiment 3

[0041] The preparation method of described phosphorus-containing bismaleimide:

[0042] (1) In a 250mL reaction vessel equipped with stirring, add 7.65g of N-(4-hydroxyphenyl)maleimide and 50mL of tetrahydrofuran under ice-cooling, and dissolve them by magnetic stirring; after completely dissolving, add triethyl Amine 5.35g, continue to stir until evenly mixed. Then, at 5-7° C., 4.5 g of a mixed solution of phenyl dichlorophosphate and tetrahydrofuran was added dropwise into the above-mentioned reaction vessel, and the system gradually produced white precipitates.

[0043] (2) After the solution was added dropwise, the system was reacted at room temperature for 8 hours, the white precipitate triethylamine hydrochloride was filtered and then distilled under reduced pressure, purified and dried with ethyl acetate and petroleum ether to obtain a light yellow solid product, the yield was 95.3%.

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Abstract

The invention belongs to the field of flame retardants for epoxy resin, and particularly relates to preparation of phosphorus-containing bismaleimide and application thereof in flame-retardant epoxy resin. The preparation method comprises the following steps: dissolving reactant N-(4-hydroxyphenyl) maleimide in tetrahydrofuran in a container with a nitrogen protecting device under ice bath, aftertotally dissolving, adding triethylamine and dispersing uniformly, and slowly dropwise adding a mixed solution of phenyl dichlorophosphate and tetrahydrofuran; after dropwise adding is finished, stirring at the room temperature, reacting for 8-12 h, carrying out suction filtering and rotary evaporation, successively washing obtained faint yellow sticky solid with ethyl acetate, ethanol and deionized water and then purifying and drying, further refining with an ethyl acetate and petroleum ether mixed solvent to obtain the phosphorus-containing bismaleimide as a target product. The prepared phosphorus-containing bismaleimide and epoxy resin can form an interpenetration polymer network structure under the effect of an amines curing agent, a flame-retardant effect is remarkable, and purposes of low addition and efficient flame retardancy can be achieved.

Description

technical field [0001] The invention belongs to the field of flame retardants for epoxy resins, in particular to the preparation of phosphorus-containing bismaleimide and its application in flame-retardant epoxy resins. Background technique [0002] Epoxy resin (EP) has high tensile strength and modulus, good chemical resistance and corrosion resistance, excellent dimensional stability and electrical properties, and is widely used in many fields such as processing and manufacturing, electronics and aerospace . However, the flammability of epoxy resin greatly limits its application and remains a fire safety hazard during use. Therefore, the design and development of high-efficiency flame-retardant epoxy resin systems has become an urgent problem in this field. Among them, phosphorus-based flame retardants have been widely studied in flame-retardant epoxy resins due to their outstanding flame-retardant effect and low environmental pollution. [0003] However, at present, ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/572C08L63/00C08K5/523C08K5/5313
CPCC08K5/523C08K5/5313C08L2201/02C08L63/00
Inventor 赵贵哲赵斌刘艳婷刘朋委刘亚青
Owner ZHONGBEI UNIV
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