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Soluble polyimide resin powder with low thermal expansion coefficient, and preparation method thereof

A low thermal expansion coefficient, polyimide resin technology, applied in the direction of coating, etc., can solve the problems of insufficient processability, insufficient rigidity of soluble polyimide, etc., to improve solvent solubility, increase spacing, reduce The effect of force

Inactive Publication Date: 2020-04-17
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved in the present invention is to provide a low thermal expansion coefficient polyimide resin powder for the problems of insufficient processability and insufficient rigidity of soluble and meltable polyimides existing in the existing low thermal expansion coefficient polyimide resin and its preparation method

Method used

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  • Soluble polyimide resin powder with low thermal expansion coefficient, and preparation method thereof
  • Soluble polyimide resin powder with low thermal expansion coefficient, and preparation method thereof
  • Soluble polyimide resin powder with low thermal expansion coefficient, and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] The specific preparation method is:

[0049] 1) Steps for preparing a low thermal expansion coefficient soluble polyamic acid resin solution:

[0050] The first step: Take 27.293 parts of TFDB and 250 parts of aprotic polar solvent N,N-dimethylformamide in a three-necked flask with an electric stirrer, stir until completely dissolved, add 12.394 parts of PMDA monomer, Stirring and reacting for 2h to obtain a block polyamic acid resin solution for subsequent use; wherein, in the system, TFDB is excessive relative to the PMDA monomer, and the number of repeating structural units in the obtained block polyamic acid resin solution is 2;

[0051] Step 2: Add 39.81 parts of 3,4-ODA and 600 parts of aprotic polar solvent N,N-dimethylformamide to the obtained block polyamic acid resin solution, stir until the monomers are completely dissolved, and then add 70.503 1 part of ODPA monomer (added in 3 times), stirred and reacted for 4h to obtain a soluble polyamic acid resin solut...

Embodiment 2

[0056] The specific preparation method is:

[0057] 1) Steps for preparing a low thermal expansion coefficient soluble polyamic acid resin solution:

[0058] The first step: Take 59.901 parts of TFDB and 250 parts of aprotic polar solvent DMAc in a three-necked flask with an electric stirrer, stir until completely dissolved, add 34.0 parts of PMDA monomer, and stir for 2 hours to obtain a block polymer Amic acid resin solution, standby; Wherein, in the system, TFDB is excessive relative to PMDA monomer, and the number of repeating structural units in the gained block polyamic acid resin solution is 5;

[0059] The second step: add 24.963 parts of 3,4-ODA and 550 parts of aprotic polar solvent DMAc to the obtained block polyamic acid resin solution, stir until the monomer is completely dissolved, then add 81.135 parts of BPADA monomer (in 3 times Add), stir and react for 4 hours to obtain a soluble polyamic acid resin solution with a low thermal expansion coefficient, the visc...

Embodiment 3

[0064] The specific preparation method is:

[0065] 1) Steps for preparing a low thermal expansion coefficient soluble polyamic acid resin solution:

[0066] Step 1: Take 13.702 parts of TFDB and 250 parts of aprotic polar solvent NMP in a three-necked flask with an electric stirrer, stir until completely dissolved, add 8.711 parts of PMDA monomer, and stir for 2 hours to obtain a block polyamide Acid resin solution, standby; Wherein, in the system, TFDB is excessive relative to PMDA monomer, and the number of repeating structural units in the gained block polyamic acid resin solution is 12;

[0067]The second step: add 48.538 parts of 3,4-ODA and 600 parts of aprotic polar solvent NMP to the obtained block polyamic acid resin solution, stir until the monomer is completely dissolved, then add 79.049 parts of BTDA monomer (in 3 times Add), stir and react for 4 hours to obtain a soluble polyamic acid resin solution with a low thermal expansion coefficient, the viscosity is 12,0...

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Abstract

The invention discloses a soluble polyimide resin powder with a low thermal expansion coefficient, and a preparation method thereof. The preparation method of the soluble polyimide resin powder with the low thermal expansion coefficient comprises the following steps: firstly, reacting 4,4'-diamino-2,2'-bis(trifluoromethyl)biphenyl with a dianhydride monomer with a limited structure in an aprotic polar solvent so as to obtain a block polyamide acid resin solution; then adding a diamine monomer with a limited structure and the aprotic polar solvent to the block polyamide acid resin solution, andthen adding the dianhydride monomer with the limited structure in batches, and performing a reaction to obtain a soluble polyamide acid resin solution with a low thermal expansion coefficient; and finally, imidizing the obtained solution to obtain the soluble polyimide resin powder with low thermal expansion coefficient. The polyimide resin powder disclosed by the invention can be dissolved in polar solvents such as DMAc, NMP, methylbenzene and cyclohexanone, has the low thermal expansion coefficient which is close to that of a metal copper foil, and has a valuable application prospect in electronic components.

Description

technical field [0001] The invention relates to polyimide materials, in particular to a low thermal expansion coefficient soluble polyimide resin powder and a preparation method thereof. Background technique [0002] Polyimide (PI) is widely used in the electronic and electrical industry because of its excellent high temperature resistance, mechanical properties, and chemical resistance. However, due to its inherent insoluble and infusible properties, it is difficult to process and form. The scope of application is limited. So far, there have been many literature reports that the processing temperature of polyimide can be reduced to 370°C by introducing flexible segments, twisted segments, and aliphatic segments into the molecular structure of polyimide, although It can be processed, but the conditions are still very harsh. When processing block shaped products, the size of the product is prone to be different from the size of the standard part, and there are bubbles inside...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C09D179/08
CPCC08G73/1039C08G73/1042C08G73/1071C09D179/08
Inventor 姬亚宁白小庆冯婷婷青双桂蒋耿杰
Owner GUILIN ELECTRICAL EQUIP SCI RES INST
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