Phthalonitrile resin prepolymer and preparation method thereof

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

Active Publication Date: 2021-06-22
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Phthalonitrile resin prepolymer and preparation method thereof
  • Phthalonitrile resin prepolymer and preparation method thereof
  • Phthalonitrile resin prepolymer and preparation method thereof

Examples

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Effect test

Embodiment 1

[0024] Phthalonitrile resin prepolymerization:

[0025] Add biphenyl type phthalonitrile resin monomer 10g (22.83mmol), 1,7-bismethylol-m-carborane 2g (9.79mmol) to the four-necked flask, and then add 20g N-methylpyrrolidone , heated to 180° C., and mechanically stirred for 4 hours. After the reaction, the solution was poured into deionized water, stirred for 30 minutes, and filtered under reduced pressure to obtain precipitates. The precipitate was dried in an oven at 100° C. for 20 hours to obtain a biphenyl phthalonitrile resin prepolymer. The prepolymer has very 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 into a ceramic crucible, and solidify in a muffle furnace according to the following stepwise temperature rise program (heating rate is 5°C / min): 240°C / 2h+...

Embodiment 2

[0031] Phthalonitrile resin prepolymerization:

[0032] Add bisphenol A type phthalonitrile resin monomer 15g (31.25mmol), 1,7-bismethylol-m-carborane 1.5g (7.34mmol) to the four-necked flask, and then add 25g N,N -Dimethylformamide, heated to 150° C., mechanically stirred for 2 h, after the reaction was completed, the solution was poured into deionized water, stirred for 60 min, and filtered under reduced pressure to obtain the precipitate. The precipitate was dried in an oven at 100° C. for 20 hours to obtain a biphenyl phthalonitrile resin prepolymer. The prepolymer has very 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 into a ceramic crucible, and cure it in a muffle furnace according to the following stepwise temperature rise program (heating rate is 5°C / m...

Embodiment 3

[0037] Phthalonitrile resin prepolymerization:

[0038] Add biphenyl type phthalonitrile resin monomer 30g (68.49mmol), 1,7-bismethylol-m-carborane 8g (39.16mmol) into the four-necked flask, then add 40g N,N-di 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 precipitates. The precipitate was dried in an oven at 100° C. for 5 hours to obtain a biphenyl phthalonitrile resin prepolymer. The prepolymer has very good 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 into a ceramic crucible, and solidify in a muffle furnace according to the following stepwise temperature rise program (heating rate is 5°C / min): 240°C / 2h+...

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Abstract

The invention discloses a high-temperature-resistant phthalonitrile resin prepolymer and a preparation method thereof. The preparation method is technically characterized by comprising the following steps: dissolving 100 parts by mass of phthalonitrile resin and 1-100 parts by mass of 1, 7-bis (hydroxymethyl)-m-carborane in an organic solvent, and carrying out a prepolymerization reaction at 100-250 DEG C for 1-8 hours; and after the pre-polymerization is finished, cooling the reaction liquid to room temperature, pouring the reaction liquid into water, carrying out suction filtration to obtain a precipitated precipitate, and drying the precipitate to obtain the phthalonitrile resin prepolymer. The prepared phthalonitrile resin prepolymer has excellent thermal oxidation resistance, mechanical properties and dielectric properties, has good solubility in common organic solvents, reduces the curing temperature, and has wide application prospects in the fields of aerospace, national defense, communication and the like.

Description

technical field [0001] The invention relates to the preparation of a phthalonitrile resin prepolymer, that is, 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 been widely used in many important fields such as aerospace and national defense. Its characteristic is that the molecule contains cyano group, which can react under the action of curing agent to form a variety of nitrogen-containing aromatic rings. This kind of material has excellent thermal oxidation resistance, dielectric properties and mechanical properties. [0003] 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 oxidation resistance. ...

Claims

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Application Information

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Patent Type & Authority Applications(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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