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Thermoset polybenzoxazine-polyimide resin composite/mesoporous molecular sieve hybrid material and preparation method thereof

A technology of polyimide resin and polybenzoxazine, which is applied in the field of organic/inorganic hybrid materials, can solve the problems of the original performance loss of the matrix resin material, and reduce the dielectric constant of the matrix material.

Inactive Publication Date: 2011-01-05
TORAY FIBER RES INST(CHINA) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some studies have shown that introducing a small amount of mesoporous molecular sieves into polyimide or epoxy resin can effectively reduce the dielectric constant of the matrix material [Polymer48 (2007) 318-329; Composites Science and Technology (2008), 1570-1578; CN 100419011C], but at the same time it will more or less cause the loss of the original properties of the matrix resin material

Method used

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  • Thermoset polybenzoxazine-polyimide resin composite/mesoporous molecular sieve hybrid material and preparation method thereof
  • Thermoset polybenzoxazine-polyimide resin composite/mesoporous molecular sieve hybrid material and preparation method thereof
  • Thermoset polybenzoxazine-polyimide resin composite/mesoporous molecular sieve hybrid material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Disperse 0.338g of MCM-41 with a particle size of 500nm in 16ml of N,N-dimethylacetamide (DMAc), and ultrasonically disperse it for 15 hours at room temperature to obtain a mesoporous molecular sieve dispersion;

[0080] Add 2.470 g of bisphenol A-aniline benzoxazine compound (BZ) to the above liquid, and continue stirring at 27° C. for 20 hours to obtain a benzoxazine compound / mesoporous molecular sieve mixed liquid;

[0081] Under the protection of an inert gas, add 0.050g of 4,4'-diaminodiphenyl ether (ODA) into 1.3ml of DMAc, stir, and slowly add 0.080g of 3,3',4,4'- Benzophenone tetra-acid dianhydride (BTDA), after the addition is complete, react at 25°C for 16 hours under the protection of an inert gas to obtain a polyamic acid solution; add the solution to the above-mentioned benzoxazine compound / mesoporous molecular sieve and mix In the liquid, stirring was continued at 20°C for 9 hours to obtain a benzoxazine compound-polyamic acid / mesoporous molecular sieve mi...

Embodiment 2

[0084] Put the toluene solution of MCM-41 with a particle size of 500nm and γ-[(2,3)-glycidoxy]propyltrimethoxysilane in a three-necked flask, reflux for more than 24 hours, filter and wash to obtain Modified MCM-41.

[0085] Disperse 0.268g of the modified MCM-41 in 16ml of N-methylpyrrolidone (NMP) and ultrasonically disperse it for 16 hours at room temperature to obtain a mesoporous molecular sieve dispersion;

[0086] Add 2.546g of bisphenol A-aniline benzoxazine compound (BZ) into the above liquid, and continue stirring at 18°C ​​for 24 hours to obtain a benzoxazine compound / mesoporous molecular sieve mixed liquid;

[0087] Under the protection of an inert gas, add 0.050g 4,4'-diaminodiphenyl ether (ODA) into 1.3ml NMP, stir, and slowly add 0.084g 3,3',4,4'- Benzophenone tetra-acid dianhydride (BTDA); after the addition is complete, react at 20°C for 20 hours under the protection of an inert gas to obtain a polyamic acid solution; add the solution to the above-mentioned ...

Embodiment 3

[0090] The toluene solution of MCM-41 with a particle size of 150nm and methyltriethoxysilane was placed in a three-necked flask, refluxed for more than 24 hours, filtered and washed to obtain the modified MCM-41 with methyl groups on the surface.

[0091] Disperse 0.132g of the modified MCM-41 in 16ml of N,N-dimethylformamide (DMF) at room temperature for 18 hours and ultrasonically disperse it uniformly to obtain a mesoporous molecular sieve dispersion;

[0092] Add 2.508g of bisphenol A-aniline benzoxazine compound (BZ) into the above liquid, and continue stirring at 20°C for 22 hours to obtain a benzoxazine compound / mesoporous molecular sieve mixed liquid;

[0093] Under the protection of an inert gas, add 0.050g of 4,4'-diaminodiphenyl ether (ODA) into 1.3ml of DMF, stir, and slowly add 0.082g of 3,3',4,4'- Benzophenone tetra-acid dianhydride (BTDA); after the addition is complete, react at 27°C for 20 hours under the protection of an inert gas to obtain a polyamic acid s...

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Abstract

The invention belongs to the field of organic / inorganic hybrid materials, and discloses a thermoset polybenzoxazine-polyimide resin composite / mesoporous molecular sieve hybrid material, which consists of a thermoset polybenzoxazine-polyimide resin composite and a mesoporous molecular sieve, wherein the mesoporous molecular sieve mass content of the hybrid material is 0.5 to 15 percent. Through a preparation method of the invention, the polybenzoxazine-polyimide resin composite / mesoporous molecular sieve hybrid material with a good interface structure and high comprehensive performance can be obtained. Compared with resin composites, the hybrid material not only maintains the heat resistance of substrate resin materials, but also has higher room-temperature storage modulus and lower dielectric constant so as to broaden the application prospect of the polybenzoxazine-polyimide resin composite in the fields of electrical engineering, electronics, information, military, aviation, aerospace and the like.

Description

technical field [0001] The invention belongs to the field of organic / inorganic hybrid materials, in particular to a novel thermosetting polybenzoxazine-polyimide resin composition / mesoporous molecular sieve hybrid material and a preparation method thereof. Background technique [0002] Polybenzoxazine is a new type of thermosetting resin developed on the basis of traditional phenolic resins. It takes benzoxazine as an intermediate and undergoes ring-opening polymerization under the action of heating or a catalyst to form Nitrogen-containing polymers with a network structure similar to phenolic resins. Polybenzoxazine not only maintains the advantages of traditional phenolic resins such as high temperature resistance, good electrical and mechanical properties, and cheap raw materials, but also improves the shortcomings of phenolic resins, such as small molecule release during curing, strong acid catalyzed corrosion equipment In addition, it also has the characteristics of lo...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08L79/04C08K7/26C08G73/10C08G73/06
Inventor 陈桥吴祯祺吴刚
Owner TORAY FIBER RES INST(CHINA) CO LTD
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