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A kind of phthalonitrile resin prepolymer and preparation method thereof

A technology of phthalonitrile resin and phthalonitrile, applied in the field of preparation of phthalonitrile resin prepolymer

Active Publication Date: 2022-06-24
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • A kind of phthalonitrile resin prepolymer and preparation method thereof
  • A kind of phthalonitrile resin prepolymer and preparation method thereof
  • A kind of phthalonitrile resin prepolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Prepolymerization of phthalonitrile resin:

[0025] In the four-necked flask, add 10g (22.83mmol) of biphenyl-type phthalonitrile resin monomer, 2g (9.79mmol) of 1,7-bishydroxymethyl-m-carborane, and then add 20g of N-methylpyrrolidone , heated to 180 ° C, mechanically stirred for 4 hours, after the reaction was completed, the solution was poured into deionized water, stirred for 30 minutes, and filtered under reduced pressure to obtain the precipitated precipitate. The precipitate was dried in an oven at 100 °C for 20 h to obtain a biphenyl-type phthalonitrile resin prepolymer. The prepolymer has good properties in ethyl acetate, acetone, tetrahydrofuran, 1,4-dioxane, N,N-dimethylformamide, N,N-dimethylacetamide and N-methylpyrrolidone. good solubility.

[0026] Prepolymer curing:

[0027] Weigh the synthesized biphenyl phthalonitrile resin prepolymer in a ceramic crucible, and solidify it in a muffle furnace according to the following step heating program (heating ...

Embodiment 2

[0031] Prepolymerization of phthalonitrile resin:

[0032] In the four-necked flask, add 15g (31.25mmol) of bisphenol A type phthalonitrile resin monomer, 1.5g (7.34mmol) of 1,7-bishydroxymethyl-m-carborane, then add 25g of N,N - Dimethylformamide, heated to 150°C, mechanically stirred for 2 hours, poured the solution into deionized water after the reaction, stirred for 60 minutes, and filtered under reduced pressure to obtain the precipitated precipitate. The precipitate was dried in an oven at 100 °C for 20 h to obtain a biphenyl-type phthalonitrile resin prepolymer. The prepolymer has good properties in ethyl acetate, acetone, tetrahydrofuran, 1,4-dioxane, N,N-dimethylformamide, N,N-dimethylacetamide and N-methylpyrrolidone. good solubility.

[0033] Prepolymer curing:

[0034] Weigh the synthesized bisphenol A phthalonitrile resin prepolymer in a ceramic crucible, and solidify it in a muffle furnace according to the following step heating program (the heating rate is 5 ...

Embodiment 3

[0037] Prepolymerization of phthalonitrile resin:

[0038] In the four-necked flask, add 30g (68.49mmol) of biphenyl-type phthalonitrile resin monomer, 8g (39.16mmol) of 1,7-bishydroxymethyl-m-carborane, then add 40g of N,N-dicarbonyl Methylacetamide was heated to 165°C and mechanically stirred for 6 hours. After the reaction, the solution was poured into deionized water, stirred for 10 minutes, and filtered under reduced pressure to obtain the precipitated precipitate. The precipitate was dried in an oven at 100 °C for 5 h to obtain a biphenyl-type phthalonitrile resin prepolymer. The prepolymer has excellent properties in ethyl acetate, acetone, tetrahydrofuran, 1,4-dioxane, N,N-dimethylformamide, N,N-dimethylacetamide and N-methylpyrrolidone. good solubility.

[0039] Prepolymer curing:

[0040] Weigh the synthesized biphenyl phthalonitrile resin prepolymer in a ceramic crucible, and solidify it in a muffle furnace according to the following step heating program (the heati...

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Abstract

The invention discloses a high temperature resistant phthalonitrile resin prepolymer and a preparation method thereof. Its technical feature is: 100 parts (mass fraction) of phthalonitrile resin and 1-100 parts of 1,7-bismethylol-m-carborane are dissolved in an organic solvent, and the pre-treatment is carried out at 100-250°C. Polymerization reaction 1 ~ 8h. After the prepolymerization, the reaction solution was cooled to room temperature, poured into water, and the precipitate was obtained by suction filtration, and the precipitate was dried to obtain a phthalonitrile resin prepolymer. The phthalonitrile resin prepolymer prepared by the present invention has excellent thermal oxidation resistance, mechanical properties and dielectric properties, has good solubility in common organic solvents, reduces curing temperature, and is used in aerospace, national defense , communications and other fields have broad application prospects.

Description

technical field [0001] The invention relates to the preparation of a phthalonitrile resin prepolymer, namely 1,7-bismethylol-m-carborane catalyzed prepolymerized phthalonitrile resin and a preparation method thereof. Background technique [0002] As an important high temperature resistant matrix material, phthalonitrile resin has a wide range of applications in many important fields such as aerospace and national defense. It is characterized by containing cyano groups in the molecule, which can react to form a variety of nitrogen-containing aromatic rings under the action of the curing agent. This kind of material has excellent thermal oxidation resistance, dielectric properties and mechanical properties. [0003] The phthalonitrile resin was successfully developed by the Keller team of the US Naval Laboratory. The resin system has a high decomposition temperature after curing, and the decomposition temperature in air and nitrogen is almost the same, showing good thermal oxi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06
CPCC08G73/0672
Inventor 周权贾宇翔王茂源侯锐钢
Owner EAST CHINA UNIV OF SCI & TECH
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