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Bismaleimide prepolymer with high solubility and good temperature resistant performance as well as preparation method and application thereof

A technology of bismaleimide and prepolymer, which is applied in the direction of adhesives, etc., can solve the problems of lowering the thermal decomposition temperature of bismaleimide resin, so as to improve spin and flexibility, reduce melt viscosity, The effect of widening the processing window

Pending Publication Date: 2018-08-14
常州杰铭新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Diamine toughening modification is the most commonly used research method, but the thermal decomposition temperature of the obtained bismaleimide resin is generally lower

Method used

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  • Bismaleimide prepolymer with high solubility and good temperature resistant performance as well as preparation method and application thereof
  • Bismaleimide prepolymer with high solubility and good temperature resistant performance as well as preparation method and application thereof
  • Bismaleimide prepolymer with high solubility and good temperature resistant performance as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]Under nitrogen protection, N,N-dimethylacetamide (DMAc, 11g) through vacuum distillation was added to a three-neck round bottom flask with mechanical stirring, and then 3,4'-diaminodiphenyl ether (3,4'-diaminodiphenyl ether (3 ,4'-ODA, 0.02mol, 4g), after it is completely dissolved, accurately weigh 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA, 0.01mol, 3.10g) and add Reaction solution, add solvent DMAc11g at the same time, add capping agent maleic anhydride (MAH, 0.02mol, 1.96g) after reacting at room temperature for 6 hours, then add a certain amount of DMAc solvent until the solid content of the solution is 20%, continue The reaction was stirred for 16 hours, then acetic anhydride (0.06mol, 6.13g) and triethylamine (0.06mol, 6.07g) were added dropwise in the generated bismaleimide acid solution, reacted at room temperature for 6 hours, and finally Wash the obtained solution with 500mL of distilled water for 3 times and 500mL of ethanol for 1 time until...

Embodiment 2

[0042] Under nitrogen protection, N,N-dimethylformamide (DMF, 18g) after vacuum distillation was added to a three-neck round bottom flask with mechanical stirring, and then 3,4'-diaminodiphenyl ether ( 3,4'-ODA, 0.03 mol, 6g), after it is completely dissolved, accurately weigh 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA, 0.02mol, 6.20g) Add the reaction solution, and add the solvent DMF18g at the same time, add the capping agent maleic anhydride (MAH, 0.02mol, 1.96g) after reacting at room temperature for 2 hours, and then add a certain amount of DMF solvent until the solid content of the solution is 20%. Continue to stir and react for 6 hours, then add acetic anhydride (0.06mol, 6.13g) and triethylamine (0.06mol, 6.07g) dropwise in the bismaleimide acid solution generated, react at room temperature for 12 hours, Finally, the obtained solution was washed with 500 mL of distilled water for 3 times until the pH value of the filtered water was approximately equal...

Embodiment 3

[0044] Under nitrogen protection, N,N-dimethylacetamide (DMAc, 11g) through vacuum distillation was added to a three-neck round bottom flask with mechanical stirring, and then 3,4'-diaminodiphenyl ether (3,4'-diaminodiphenyl ether (3 ,4'-ODA, 0.02mol, 4g), after it was completely dissolved, accurately weigh 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA, 0.005mol, 1.55g) and 2,3,3',4'-Biphenyltetracarboxylic dianhydride (a-BPDA, 0.005mol, 1.47g) was added to the reaction solution, and the solvent DMAc11g was added at the same time, and the end-capping agent maleic butene was added after reacting at room temperature for 2 hours dianhydride

[0045] (MAH, 0.02mol, 1.96g), then add a certain amount of DMAc solvent to a solution solid content of 20%, continue to stir the reaction for 24 hours, then add acetic anhydride dropwise in the bismaleimide acid solution that generates

[0046] (0.06mol, 6.13g) and triethylamine (0.04mol, 4.05g), reacted at room temperature f...

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Abstract

The invention relates to a bismaleimide prepolymer and a preparation method. The material has the following structure formula shown in the description. The preparation method comprises the following steps of under the nitrogen gas protection, 3,4'-diaminodiphenyl ether are dissolved in an organic solvent; after complete dissolution, 2,3,3',4'-biphenyl tetracarboxylic dianhydride or 2,3,3',4'-diphenyl ether tetracarboxylic acid dianhydride are added; meanwhile, the organic solvent is added so that the solid content of the solution is 5 to 50 percent; room temperature reaction is performed; an end-capping reagent of maleic anhydride is added; reaction is continuously performed; then, dewatering agents and catalysts are added drip by drip; reaction, washing, drying and crushing are performedto obtain the bismaleimide prepolymer. The prepared bismaleimide material has good comprehensive performance; before crosslinking, the high dissolution degree, low vitrification conversion temperatureand higher temperature processing window are realized; after the heating curing, good temperature resistant performance is realized. The material can be prepared into films, high-performance resin-based composite materials and high-temperature-resistant structure bonding agents and the like, the bismaleimide prepolymer can be applied to the fields of aerospace, printed circuit boards, semiconductor encapsulation and the like.

Description

technical field [0001] The invention belongs to the field of thermosetting polymer materials and the preparation thereof, in particular to a bismaleimide material with high solubility and good temperature resistance and a preparation method thereof. Background technique [0002] Bismaleimide resin is a class of compounds with a bifunctional imide structure, and is an important member of the thermosetting resin family. The prepolymer has fluidity and moldability, and has good thermo-oxidative stability after curing ( High temperature use temperature is higher than 230 ℃), flame retardancy, chemical stability and corrosion resistance and other excellent properties. Bismaleimide has been widely used in high-tech fields such as printed circuit boards in microelectronics, packaging semiconductors, and aerospace as high-temperature insulating materials, adhesives, and composite material matrix resins. [0003] However, the commonly used bismaleimide prepolymer has a rigid and sym...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/12C08L79/08C09J179/08
CPCC08G73/127C08L79/085C08L2201/08C09J179/085
Inventor 宇平王巍胡一鸣潘丽静
Owner 常州杰铭新材料科技有限公司
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