Preparation method for polyimide film with low water absorption

A technology of polyimide film and low water absorption, which is applied in the field of insulating materials, can solve the problems of high film production cost, low water absorption rate, high cost, etc., achieve excellent comprehensive performance, reduce water absorption performance, and reduce the effect of water absorption performance

Active Publication Date: 2017-06-23
株洲时代华鑫新材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the water absorption rate of the polyimide film obtained by this method is significantly reduced, the introduction of fluorine-containing diamine reduces the inherent solvent resistance and other properties of the polyimide film, and the industrial production of fluorine-containing monomers is too difficult, making the industrial production of the film difficult. cost too high
[0005] Patent CN105601923A discloses a fluorine-containing soft-hard block polyimide film and its preparation method and application. Electric constant and low water absorption, but this type of polyimide film also belongs to fluorine-containing polyimide film. In addition to high cost and poor solvent resistance, this method makes the molecular chain structure and film performance It is difficult to control, the production process is complicated, and it is difficult to realize industrial produ

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0032] Example 1:

[0033] A preparation method of the low water absorption polyimide film of the present invention includes the following steps:

[0034] (1) Water bath and N at 20℃ 2 Dissolve 4g4,4'-diaminodiphenyl ether (0.02mol) and 12.3g2,2'-bis[4-(4-aminophenoxyphenyl)]propane (0.03mol) under the protection of In a three-necked flask with 120g N-methylpyrrolidone solvent, add 6.5g 3,3',4,4'-benzophenone tetracarboxylic dianhydride (0.02mol) and 5.5g pyromellitic dianhydride (0.025mol) , Stir for 3h to generate flexible polyamic acid resin terminated with amino groups, namely flexible polyamic acid resin solution A;

[0035] (2) Ice bath and N at 0℃ 2 Under the protection of, dissolve 5.5g of p-phenylenediamine (0.05mol) in another three-necked flask containing 70g of N-methylpyrrolidone solvent, add 12g of pyromellitic dianhydride (0.055mol), stir for 3h to produce Anhydride group-terminated rigid polyamic acid resin, namely rigid polyamic acid resin solution B;

[0036] (3) I...

Example Embodiment

[0038] Example 2:

[0039] A preparation method of the low water absorption polyimide film of the present invention includes the following steps:

[0040] (1) Water bath and N at 20℃ 2 Under the protection of, dissolve 10g of 4,4'-diaminodiphenyl ether (0.05mol) in a three-necked flask containing 92g of N-methylpyrrolidone solvent, and then add 9.7g of 3,3',4,4'-diphenyl Ketonetetracarboxylic dianhydride (0.03mol) and 3.3g pyromellitic dianhydride (0.015mol) were stirred for 3h to generate a flexible polyamic acid resin terminated with an amino group, that is, flexible polyamic acid resin solution A;

[0041] (2) Ice bath and N at 0℃ 2 Under the protection of, dissolve 5.5g of p-phenylenediamine (0.05mol) in another three-necked flask containing 70g of N-methylpyrrolidone solvent, add 12g of pyromellitic dianhydride (0.055mol), stir for 3h to produce Anhydride group-terminated rigid polyamic acid resin, namely rigid polyamic acid resin solution B;

[0042] (3) Ice bath and N at 10℃ 2...

Example Embodiment

[0044] Example 3:

[0045] A preparation method of the low water absorption polyimide film of the present invention includes the following steps:

[0046] (1) Water bath and N at 20℃ 2 Dissolve 4g4,4'-diaminodiphenyl ether (0.02mol) and 12.3g2,2'-bis[4-(4-aminophenoxyphenyl)]propane (0.03mol) under the protection of In a three-necked flask containing 104.5g of N-methylpyrrolidone solvent, add 9.7g of 3,3',4,4'-benzophenonetetracarboxylic dianhydride (0.03mol) and 3.3g of pyromellitic dianhydride (0.015 mol), stirring for 3h, to generate a flexible polyamic acid resin terminated with an amine group, that is, flexible polyamic acid resin solution A;

[0047] (2) Ice bath and N at 0℃ 2 Under the protection of, dissolve 4.8g m-phenylenediamine (0.045mol) in another three-necked flask filled with 70g N-methylpyrrolidone solvent, then add 11g pyromellitic dianhydride (0.05mol) and stir for 3h to produce Anhydride group-terminated rigid polyamic acid resin, namely rigid polyamic acid resi...

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PUM

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Abstract

The invention discloses a preparation method for a polyimide film with low water absorption. The preparation method comprises the following steps: under the protection of N2, mixing a diamine monomer A and a dianhydride monomer A in a polar solvent to obtain a flexible polyamide acid resin solution A; under the protection of N2, mixing a diamine monomer B and a dianhydride monomer B in the polar solvent to obtain a rigid polyamide acid resin solution B; under the protection of N2, co-mixing the flexible polyamide acid resin solution A with the rigid polyamide acid resin solution B, stirring, stopping reaction when viscosity of a to-be-reacted matter reaches 2000-3500 poises; and finally, adding an accelerant and a dehydrator to uniformly mix, salivating to form a film, and performing imidization treatment to obtain the polyimide film with the low water absorption. The polyimide film obtained by the preparation method provided by the invention has a water absorption rate lower than 1.2% which is far lower than a water absorption rate (2.3%-2.4%) of conventional polyimide; and meanwhile, excellent comprehensive performance such as mechanical and electrical performance is kept.

Description

technical field [0001] The invention belongs to the field of insulating materials for electric appliances, and in particular relates to a preparation method of a polyimide film with low water absorption. Background technique [0002] Polyimide (PI) film is a key insulating material for electrical appliances, and is widely used in printed circuit boards, power transmission and distribution equipment, wind power generation equipment, frequency conversion motors, high-speed traction motors and high-voltage transformers. [0003] Due to the special molecular structure of PI material, it contains a large number of polar groups, which is easy to absorb water. The water absorption rate of traditional polyimide film is as high as 2.3% to 2.4%, which leads to the explosion and separation of printed circuit boards during the production process. Layer and other quality defects seriously affect the performance and yield of printed circuit boards. In addition, the PI film absorbs water ...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L79/08C08G73/10
CPCC08G73/1071C08J5/18C08J2379/08
Inventor 刘杰廖波江乾王倩高纪明张步峰姜其斌
Owner 株洲时代华鑫新材料技术有限公司
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