Hollow microsphere composite modified thermosetting polyimide material and preparation method thereof

A technology of polyimide and hollow microspheres, which is applied in the field of hollow microsphere composite modified thermosetting polyimide materials and its preparation, can solve the problems of difficult melting, difficult dissolution and low use temperature, and achieve outstanding performance, Special structure, reduce tangle effect

Inactive Publication Date: 2020-06-19
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Thermoplastic polyimide has good toughness, but it is difficult to dissolve and melt, and the use temperature of the product is relatively low

Method used

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  • Hollow microsphere composite modified thermosetting polyimide material and preparation method thereof
  • Hollow microsphere composite modified thermosetting polyimide material and preparation method thereof
  • Hollow microsphere composite modified thermosetting polyimide material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] First use a beaker to make a solution of 3-aminopropyltriethoxysilane (KH550) coupling agent with a mass fraction of 2% hollow microspheres and absolute ethanol (100mL absolute ethanol per 0.3g KH550), and then add the particle size Hollow microspheres of about 20um were fully impregnated and stirred for 5 hours, and finally filtered with suction, fully dried in a vacuum oven at 100°C to constant weight, and then sieved for later use. Use monomers 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA), 3,4'-diaminodiphenyl ether (3,4'-ODA) and phenylacetylene phthalic anhydride (PEPA) ) to synthesize and prepare a thermosetting polyimide prepolymer (N4) with a degree of polymerization of 4, and then add the prepared active hollow microspheres to the prepolymer N4 at a mass fraction of 3%, and use a torque rheometer in Melt and mix at a high temperature of 270° C. for 20 minutes and then take out to finally obtain a hollow microsphere / thermosetting polyimide compo...

Embodiment 2

[0038] First use the monomer 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA), 3,4'-diaminodiphenyl ether (3,4'-ODA) and phenylacetylene phthalic anhydride ( PEPA) synthetically prepares the thermosetting polyimide prepolymer (N4) that the degree of polymerization is 4, and then the hollow microspheres with a particle size of about 20um after sieving and drying are treated with a coupling agent with a mass of 3%. Fractions were added to the prepolymer N4, and the torque rheometer was used to carry out melt mixing at a high temperature of 270°C for 20 minutes and then taken out to finally obtain hollow microspheres / thermosetting polyimide composite materials.

Embodiment 3

[0040] First use a beaker to make a solution of 3-aminopropyltriethoxysilane (KH550) coupling agent with a mass fraction of 2% hollow microspheres and absolute ethanol (100mL absolute ethanol per 0.3g KH550), and then add the particle size Hollow microspheres with a diameter of about 100 nm were fully impregnated and stirred for 5 hours, and finally filtered with suction, fully dried in a vacuum oven at 100°C to constant weight, and then sieved before use. Use monomers 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA), 3,4'-diaminodiphenyl ether (3,4'-ODA) and phenylacetylene phthalic anhydride (PEPA) ) to synthesize and prepare a thermosetting polyimide prepolymer (N4) with a degree of polymerization of 4, and then add the prepared active hollow microspheres to the prepolymer N4 at a mass fraction of 3%, and use a torque rheometer in Melt and mix at a high temperature of 270° C. for 20 minutes and then take out to finally obtain a hollow microsphere / thermosetting ...

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Abstract

The invention relates to a hollow microsphere composite modified thermosetting polyimide material and a preparation method thereof. The material is prepared by the following steps: carrying out mechanical blending on the hollow microsphere and a thermosetting polyimide prepolymer according to the mass fraction ratio of (1 to 20 percent) to (99 to 80 percent) and uniformly mixing all parts to obtain a hollow microsphere / thermosetting polyimide prepolymer mixture; carrying out melting and crosslinking treatment on the mixture under high-temperature condition to prepare products such as high temperature resisting parts, adhesives and advanced composite materials. The invention aims at reducing the expensive cost of existing blocked thermosetting polyimide and further improving the comprehensive performance of the material at the same time, in particular to the melting processability of the thermosetting polyimide prepolymer and temperature resistance of cured resin. The hollow microsphere / thermosetting polyimide prepolymer obtained by modifying provided by the invention has the advantages that the cost is reduced; in addition, the melt viscosity can be greatly reduced and the meltingprocessing capacity is enhanced; the temperature resistance of the cured resin is also effectively improved.

Description

technical field [0001] The invention belongs to the field of polymer composite materials and preparation thereof, in particular to hollow microsphere composite modified thermosetting polyimide materials and a preparation method thereof. Background technique [0002] Polyimide is a kind of high-performance polymer containing imide characteristic groups on the main chain of the molecule. According to the difference between the main chain structure and the processing technology, it is divided into two categories: thermoplastic and thermosetting polyimide. Thermoplastic polyimide has good toughness, but it is difficult to dissolve and melt, and the service temperature of the product is relatively low. Thermosetting polyimide materials are obtained by introducing active reactive groups into the main chain or side chains. Before crosslinking, they are low molecular weight prepolymers with good solubility and melt processability, which can Films, adhesives and composite materials ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08K9/06C08K7/24
CPCC08K7/24C08K9/06C08K2201/003C08L79/08
Inventor 宇平王巍刘燕刚薛敏钊胡一鸣张燕黎潘丽静
Owner SHANGHAI JIAOTONG UNIV
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