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Polyimide film and preparation method thereof

A polyimide film and polyamic acid technology, which is applied in the field of organic materials, can solve the problems of reducing the thermal expansion coefficient of the film and failing to meet the requirements of near-zero thermal expansion, and achieve the effects of reducing the thermal expansion coefficient, convenient operation, and easy industrial production

Active Publication Date: 2021-03-16
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned existing technologies are based on structural design, which reduces the thermal expansion coefficient of the film to a certain extent, but does not meet the requirement for near-zero thermal expansion.

Method used

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  • Polyimide film and preparation method thereof
  • Polyimide film and preparation method thereof
  • Polyimide film and preparation method thereof

Examples

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preparation example Construction

[0047] The invention provides a kind of preparation method of polyimide film, comprises the following steps:

[0048] a) polymerizing aromatic dianhydride monomers and diamine monomers in a solvent to form a polyamic acid precursor solution;

[0049] b) performing casting, curing and heat imidization on the polyamic acid precursor solution to form a polyimide film;

[0050] The diamine monomer is a diamine shown in formula II-a, or a mixture of a diamine shown in formula II-a and other diamine monomers;

[0051] The diamine represented by the formula II-a is selected from one or more of the compounds represented by the formula II-a1 ~ formula II-a3:

[0052]

[0053] In the present invention, the polyimide is prepared by reacting the pyridazine-containing diamine monomer represented by the specific formula II-a with the aromatic dianhydride monomer, which can effectively reduce the thermal expansion coefficient of the polyimide film and achieve near-zero thermal expansion ...

preparation example 1

[0110] The preparation of 3,6-bis(4-aminophenyl) pyridazine shown in formula II-a3 of raw material preparation example 1

[0111] Under the protection of nitrogen, 4-aminophenylboronic acid pinacol ester (0.046mol, 10.08g), 3,6-dibromopyridazine (0.021mol, 5.00g), tetrakis (triphenylphosphine) palladium (0.001mol , 1.15g), anhydrous potassium carbonate (0.15mol, 20.73g), 20mL toluene and 20mL deionized water were successively added to a 50mL three-necked flask, and then the reaction was stirred and refluxed at 130°C, monitored by TLC until 3,6-dibromo Pyridazine completely disappeared, the reaction was stopped, cooled to room temperature, a large amount of solids were precipitated and filtered, and then washed with deionized water, toluene and methanol for several times, and dried in vacuum to obtain the crude product; after purification, the yellow crystal 4.79 g, namely 3,6-bis(4-aminophenyl)pyridazine, the yield is 87%.

[0112] 1 H NMR (400MHz, DMSO-d 6 ) δ 7.94 (s, 2H)...

preparation example 2

[0115] The preparation of 3,6-bis(2-aminophenyl) pyridazine shown in the example 2 of raw material preparation Ⅱ-a1

[0116] According to the preparation process of raw material preparation example 1, the difference is that the 4-aminophenylboronic acid pinacol ester in step (1) is replaced by 2-aminophenylboronic acid pinacol ester.

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Abstract

The invention provides a polyimide film and a preparation method thereof. Polyimide is prepared by reacting a diamine monomer containing a pyridazine structure as shown in a specific formula II-a withan aromatic dianhydride monomer so that the coefficient of thermal expansion of the polyimide film can be effectively reduced, the requirement of near-zero thermal expansion is met, and meanwhile, the film can be ensured to have excellent mechanical properties. Besides, the preparation method is simple in process, convenient to operate and easy for industrial production, and can be better appliedto high-precision instruments, micro-size electronic industry and other fields sensitive to size requirements.

Description

technical field [0001] The invention relates to the field of organic materials, in particular to a polyimide film and a preparation method thereof. Background technique [0002] In flexible circuits, optical devices, energy batteries, and sensor devices, multiple materials are generally used in combination, and there is a problem of device performance failure caused by different thermal expansion coefficients. In particular, high-precision optical instruments, micro-sized electronic devices, and explosive protection components have extremely strict requirements on the dimensional stability of the materials used. It is expected that the materials will exhibit near-zero thermal expansion characteristics, that is, the coefficient of thermal expansion (CTE) is between -2 and 2ppm / K. However, most polymer materials show relatively large thermal expansion, for example, the thermal expansion coefficient of polyethylene is about 200ppm / K. [0003] Polyimide is a class of high-per...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08J5/18C08L79/08
CPCC08G73/1007C08G73/1085C08J5/18C08J2379/08
Inventor 邱雪鹏鲍峰董志鑫戚福玲代学民蔡艳春姚海波
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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