Preparation method of efficient catalytic curing phenylacetylene terminated polyimide resin system

A technology of acetylene-based polyimide resin and polyimide resin, which is applied in the field of preparation of high-efficiency catalytic curing phenylacetylene-terminated polyimide resin system, and can solve the problem of high curing temperature and polyimide resin curing temperature. Advanced problems, to achieve the effect of uniform reaction, stable process and simple operation

Inactive Publication Date: 2020-08-07
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problem of high curing temperature of phenylacetylene-terminated polyimide resin, and provide a preparation method for highly efficient catalytic curing phenylacetylene-terminated polyimide resin system, the prepared phenylacetylene-terminated polyimide resin Imide resin can still maintain excellent heat resistance
[0005] The invention aims at the problem of high curing temperature of phenylacetylene-capped polyimide resin, adding a free radical catalyst to initiate crosslinking of phenylacetylene groups, and using a coordination catalyst to regulate the crosslinking structure of the polyimide resin directional

Method used

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  • Preparation method of efficient catalytic curing phenylacetylene terminated polyimide resin system
  • Preparation method of efficient catalytic curing phenylacetylene terminated polyimide resin system
  • Preparation method of efficient catalytic curing phenylacetylene terminated polyimide resin system

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Effect test

Embodiment 1

[0029] A kind of preparation method of high-efficiency catalytic curing phenylacetylene-terminated polyimide resin system, the specific steps are as follows:

[0030] A, preparation of phenylethynyl polyimide resin system

[0031] Weigh 60 parts of phenylethynyl-terminated polyimide and 40 parts of 1,4-dioxane, mix the two to obtain phenylethynyl-terminated polyimide resin solution;

[0032] B. Mixing of new high-efficiency catalyst and resin system

[0033] The new high-efficiency catalyst is composed of cumene hydroperoxide and cobalt naphthenate in a mass ratio of 20:80; mix the new catalyst and the resin system at room temperature, and use a magnetic stirrer to continuously stir for 2 hours to ensure that the two are mixed evenly. The mass ratio of resin system to cumene hydroperoxide and cobalt naphthenate is 100:4:1;

[0034] C. Establishment of Gradient Temperature Curing Process

[0035] Keep the mixed resin system and the new high-efficiency composite catalyst in a...

Embodiment 2

[0041] A kind of preparation method of high-efficiency catalytic curing phenylacetylene-terminated polyimide resin system, the specific steps are as follows:

[0042] A. Preparation of composite catalyst and phenylethynyl polyimide resin system

[0043] Weigh 70 parts of phenylethynyl-terminated polyimide and 30 parts of 1,4-dioxane, mix the two to obtain phenylethynyl-terminated polyimide resin solution;

[0044] B. Mixing of new high-efficiency catalyst and resin system

[0045] The new high-efficiency catalyst is composed of cumene hydroperoxide and cobalt naphthenate in a mass ratio of 20:80. Mix the new catalyst and the resin system at room temperature, and use a magnetic stirrer to continuously stir for 2 hours to ensure that the two are mixed evenly. The mass ratio of the resin system to cumene hydroperoxide and cobalt naphthenate is 100:3:1;

[0046] C. Establishment of Gradient Temperature Curing Process

[0047] Keep the mixed resin system and the new high-efficie...

Embodiment 3

[0050] A kind of preparation method of high-efficiency catalytic curing phenylacetylene-terminated polyimide resin system, the specific steps are as follows:

[0051] A. Preparation of composite catalyst and phenylethynyl polyimide resin system

[0052] Weigh 80 parts of phenylethynyl-terminated polyimide and 20 parts of 1,4-dioxane, mix the two to obtain phenylethynyl-terminated polyimide resin solution;

[0053] B. Mixing of new high-efficiency catalyst and resin system

[0054] The new high-efficiency catalyst is composed of cumene hydroperoxide and cobalt naphthenate in a mass ratio of 20:80. Mix the new catalyst and the resin system at room temperature, and use a magnetic stirrer to continuously stir for 2 hours to ensure that the two are mixed evenly. The mass ratio of the resin system to cumene hydroperoxide and cobalt naphthenate is 100:1:1;

[0055] C. Establishment of Gradient Temperature Curing Process

[0056] Keep the mixed resin system and the new high-efficie...

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Abstract

The invention discloses a preparation method of an efficient catalytic curing phenylacetylene terminated polyimide resin system, and belongs to the field of materials. The method is characterized by comprising the following steps: preparing a phenylacetylene terminated polyimide resin solution; adding a novel efficient catalyst into a resin system; carrying out gradient curing on a resin system added with a novel efficient compound catalyst, firstly curing at 120 DEG C for 1 hour, then performing curing at 240 DEG C for 2 hours, and finally performing curing at 300 DEG C for 3-4 hours to obtain the completely cured phenylethynyl-terminated polyimide resin. The preparation method has the advantages that the curing temperature of the phenylethynyl-terminated polyimide resin prepared by the preparation method is obviously reduced, and the highest curing temperature does not exceed 300 DEG C. The phenylethynyl-terminated polyimide resin disclosed by the invention is reliable in low-temperature curing process, and a novel efficient catalyst is adopted to catalyze a curing reaction, so that the reaction is uniform, the operation is simple, the process is stable, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of adopting resins, and in particular relates to a preparation method of a high-efficiency catalytic curing phenylacetylene-terminated polyimide resin system. Background technique [0002] Phenylacetylene-terminated polyimide is a high-performance resin developed around the 1990s. Its molecular structure contains an imide five-membered heterocyclic structure, and it consists of imide oligomers containing active phenylacetylene end groups. It is formed by curing and cross-linking, and the cured product is mainly aromatic structure. This structure endows the polyimide resin with a higher glass transition temperature, above 270°C, which can be used at high temperature for a long time, and the thermal decomposition temperature can reach above 500°C. At the same time, its mechanical properties are also excellent, with low thermal expansion coefficient and good dielectric properties. It is widely used in high-temperature f...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08G73/12C08F299/02C08J3/24C08L79/08
CPCC08G73/1003C08G73/12C08F299/022C08J3/24C08J2379/08
Inventor张春华杨锦帅钱秀松王彦直
OwnerHARBIN INST OF TECH