Method for preparing phthalonitrile resin cured product by amino-terminated polyarylether curing agent containing phthalazinone biphenyl structure

A technology of phthalonitrile resin and naphthalene biphenyl, which is applied in the field of material science, can solve problems such as defects, volatile or decomposed resin, etc., and achieves wide processing window, excellent melt processing fluidity, and excellent thermal stability. sexual effect

Active Publication Date: 2021-02-19
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention aims at the problem that the traditional small molecule aromatic amine curing agent of phthalonitrile resin is easy to volatilize or decompose under high temperature curing and cause resin defects, and adopts a type of amino-terminated polyaryl ether containing phthalazinone biphenyl structure preparation of phthalonitrile resin

Method used

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  • Method for preparing phthalonitrile resin cured product by amino-terminated polyarylether curing agent containing phthalazinone biphenyl structure
  • Method for preparing phthalonitrile resin cured product by amino-terminated polyarylether curing agent containing phthalazinone biphenyl structure
  • Method for preparing phthalonitrile resin cured product by amino-terminated polyarylether curing agent containing phthalazinone biphenyl structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 1g of resorcinol-based phthalonitrile resin precursor, add 0.1g of amino-terminated polyaryl ether ketone curing agent, grind it thoroughly, and put it into a reactor with a temperature of 180°C , heat and stir until completely melted, then pour the liquid mixture into a mold, and heat in a muffle furnace at 200°C / 2 hours; 250°C / 2 hours; 300°C / 2 hours; 350°C / 2 hours; 375°C / 2 hours; program curing at 400°C / 2 hours, and then cooled to room temperature to prepare isophthalonitrile resin.

[0029] After curing, the phthalonitrile resin has a 5% thermal weight loss temperature of 553.2°C under a nitrogen atmosphere, and a carbon residue rate of 76.9% at 800°C.

[0030] Rheological analysis shows that when the temperature rises to 182.5°C, the viscosity decreases to within 50Pa·s, the lowest viscosity is 0.167Pa·s, the gel temperature is 377.1°C, and the processing temperature window is 194.6°C.

Embodiment 2

[0032] Weigh 1g of resorcinol-based phthalonitrile resin precursor, add 0.2g of amino-terminated polyaryl ether ketone curing agent, grind it thoroughly, and put it into a reactor with a temperature of 180°C , heat and stir until completely melted, then pour the liquid mixture into a mold, and heat in a muffle furnace at 200°C / 2 hours; 250°C / 2 hours; 300°C / 2 hours; 350°C / 2 hours; 375°C / 2 hours; program curing at 400°C / 2 hours, and then cooled to room temperature to prepare isophthalonitrile resin.

[0033] After curing, the phthalonitrile resin has a 5% thermal weight loss temperature of 548.8°C under a nitrogen atmosphere, and a carbon residue rate of 77.5% at 800°C.

[0034] Rheological analysis shows that when the temperature rises to 181.5°C, the viscosity decreases to within 50Pa·s, the lowest viscosity is 0.255Pa·s, the gel temperature is 279.2°C, and the processing temperature window is 97.7°C.

Embodiment 3

[0036] Weigh 1g of resorcinol-based phthalonitrile resin precursor, add 0.3g of amino-terminated naphthalene biphenyl polyaryletherketone curing agent, grind it thoroughly, and put it into a reactor with a temperature of 180°C , heat and stir until completely melted, then pour the liquid mixture into a mold, and heat in a muffle furnace at 200°C / 2 hours; 250°C / 2 hours; 300°C / 2 hours; 350°C / 2 hours; 375°C / 2 hours; program curing at 400°C / 2 hours, and then cooled to room temperature to prepare isophthalonitrile resin.

[0037] After curing, the phthalonitrile resin has a 5% thermal weight loss temperature of 542.5°C under a nitrogen atmosphere, and a carbon residue rate of 77.9% at 800°C.

[0038] Rheological analysis shows that when the temperature rises to 179.3°C, the viscosity decreases to within 50Pa·s, the minimum viscosity is 0.524Pa·s, the gel temperature is 222.8°C, and the processing temperature window is 43.5°C.

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Abstract

The invention provides a method for preparing a cured phthalonitrile resin with an amino-terminated polyaryl ether curing agent containing a phthalazinone biphenyl structure, and belongs to the field of material science and technology. The amino-terminated polyaryl ether containing phthalazinone biphenyl structure is used as the curing agent to mix with the phthalonitrile resin precursor, and the temperature is programmed to be cured. The amino-terminated polyarylether curing agent containing phthalazinone biphenyl structure that the present invention adopts has excellent thermal stability, and the cured product of resorcinol-based phthalonitrile resin prepared with it as curing agent is heated in nitrogen The maximum thermal weight loss temperature of 5% in the atmosphere can reach 553.2°C, the maximum carbon residue rate at 800°C is 78.1%, and the glass transition temperature is higher than 400°C; the lowest melt viscosity is 0.167Pa·s, showing excellent melt Processing fluidity; has a very wide processing window, the widest can reach 194.6 ℃. The cured phthalonitrile resin has excellent thermal stability and thermomechanical properties.

Description

technical field [0001] The invention belongs to the technical field of material science and relates to a method for preparing a cured phthalonitrile resin with an amino-terminated polyaryl ether curing agent containing a phthalazinone biphenyl structure. Background technique [0002] Phthalonitrile resin is a general term for a class of high-performance thermosetting resins containing phthalonitrile structure at the end of the molecular chain. It has excellent high temperature resistance, mechanical properties, high flame retardancy, low water absorption, and chemical resistance. And have unique optical and electrical properties. But the problem that phthalonitrile resin exists is that its curing process is very difficult. For example, the biphenol-type phthalonitrile monomer needs to be reacted at 280°C for nearly 100 hours before an obvious gel can be observed. [0003] The Keller research group of the US Naval Laboratory found that mixing phthalonitrile monomers with ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06
CPCC08G73/0638
Inventor 蹇锡高翁志焕王锦艳胡月张守海刘程
Owner DALIAN UNIV OF TECH
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