Fluorine-containing polyimide basal body resin and preparation method thereof

A fluorine-containing polyimide matrix, polyimide matrix technology, applied in the field of polyimide resin and its preparation, can solve the need to improve melt processing performance, poor impact toughness of composite materials, easy to produce microcracks, etc. problems, to achieve the effect of improving long-term thermal oxidation stability, good molding processability, and low porosity

Inactive Publication Date: 2007-10-24
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, PMR-15 and KH-304 polyimide matrix resins also have some shortcomings, which to a certain extent have affected the progress of their practical application.
These disadvantages mainly include: 1) One of the main monomers (4,4-diaminodiphenylmethane) used to prepare the matrix resin has potential carcinogenicity; 2) When preparing large and complex parts, melt processing performance requires 3) The impact toughness of the composite material prepared by it is poor and needs to be further improved; 4) The composite material parts are prone to microcracks during service at high temperature, etc.

Method used

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  • Fluorine-containing polyimide basal body resin and preparation method thereof
  • Fluorine-containing polyimide basal body resin and preparation method thereof
  • Fluorine-containing polyimide basal body resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 80 parts of 3,3',4,4'-benzophenonetetraacid dianhydride (BTDA) was heated to reflux in 100 parts of ethanol for 3 hours to obtain the corresponding aromatic diacid diester solution (BTDE). Heat 35 parts of end-capping agent NA acid anhydride in 55 parts of ethanol to reflux for 3 hours to obtain the corresponding monoacid monoester solution (NE). Dissolve 80 parts of organic diamine monomer (6FAPB) in 60 parts of ethanol, and after stirring for half an hour, add the above-prepared NE and BTDE solutions sequentially; the mixture is stirred at 50°C for 5 hours to obtain 47% solid content Polyimide matrix resin solution; its absolute viscosity (25°C) is 20-35mPa.s.

[0029] The viscous liquid obtained after the resin solution is rotary evaporated at 60-80° C. to remove most of the solvent is heated and dried (50-220° C.) to obtain resin molding powder. Put 50g of molding powder into the mold, heat it in a press preheated to 250°C, pressurize at 270-300°C to 1-10MPa, conti...

Embodiment 2

[0031] 121 parts of 3,3',4,4'-diphenyl ether tetra-acid dianhydride (ODPA) were heated to reflux in 200 parts of ethanol for 1 hour to obtain the corresponding aromatic diacid diester solution (ODPE). Heat 40 parts of the end-capping agent NA acid anhydride in 55 parts of ethanol to reflux for 5 hours to obtain the corresponding monoacid monoester solution (NE). Dissolve 185 parts of diamine monomer 6FBAB in 160 parts of ethanol, stir for half an hour, then add the previously prepared NE and BTDE solutions in turn, and stir the mixture at 5°C for 15 hours to obtain polyamide with a solid content of 45%. imine homogeneous resin solution. Its absolute viscosity (25°C) is 15-35mPa.s.

[0032] The viscous liquid obtained after the resin solution is rotary evaporated at 60-80° C. to remove most of the solvent is heated and dried (50-220° C.) to obtain resin molding powder. Put 50g of molding powder into the mold, heat the mold in a press preheated to 250°C, pressurize 1-10MPa at ...

Embodiment 3

[0034] 400 parts of 3,3',4,4'-benzophenone tetra-acid dianhydride (BTDA) were heated to reflux in 620 parts of ethanol for 3 hours to obtain the corresponding aromatic diacid diester solution (BTDE). Heat 52 parts of end-capping agent NA acid anhydride in 64 parts of ethanol to reflux for 2 hours to obtain the corresponding monoacid monoester solution (NE). Dissolve 356 parts of diamine monomer 6FAPB in 400 parts of ethanol, stir for half an hour, then add the NE and BTDE solutions prepared above in turn, and stir the mixture at 20°C for 10 hours to obtain a polyamide with a solid content of 43%. imine homogeneous resin solution. Its absolute viscosity (25°C) is 15-35mPa.s.

[0035]Composite the matrix resin solution with carbon fiber on a winding machine to prepare prepregs. After most of the solvents are volatilized, laminate them according to the requirements. Stages of prepreg (tape or cloth). Put the prepreg in stage B into a press preheated to 260°C, apply a pressure ...

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Abstract

The invention discloses a fluorine polyimide base resin and making method, which is characterized by the following: adopting aromatic dianhydride, substituted organic fluorine diamine and reacted terminated agent as raw material to produce thermostable product as formula I through PMR method; leading fluorine group in the main chain molecular structure of resin; improving the manufacturing property and long-time oxidizing stability; possessing potential applying value in the high and new technological domain.

Description

technical field [0001] The invention relates to a polyimide resin and a preparation method thereof, in particular to a fluorine-containing polyimide matrix resin and a preparation method thereof. Background technique [0002] In 1972, T.T.Serafini et al. (Thermally StablePolyimide from Solutions of Monomeric Reactants, J.Appl.Polym.Sci., 1972, 16:905; U.S.Patent 3,745,149) of the NASA Lewis Research Center in the United States reported the in-situ polymerization of monomer reactants (In situ Polymerization of Monomer Reactants) method prepared high temperature resistant (316 ℃) carbon fiber reinforced polyimide resin-based composite material matrix resin (PMR-15). During the same period, the Institute of Chemistry, Chinese Academy of Sciences successfully developed a PMR polyimide matrix resin (KH-304). Different from PMR-15, KH-304 matrix resin uses non-toxic and harmless low-boiling anhydrous ethanol instead of anhydrous methanol as the main solvent in the resin preparati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
Inventor 杨士勇陈建升杨海霞范琳左红军
Owner INST OF CHEM CHINESE ACAD OF SCI
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