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Preparation method of soluble low-temperature rapid imidization polyimide film

A technology of imidization polyimide and polyimide film, which is applied in the field of preparation of soluble, low-temperature rapid imidization polyimide film, and can solve the problem of high imidization temperature and long time problem, achieve the effect of reducing activation energy, improving interaction and reducing energy consumption

Active Publication Date: 2022-01-25
富优特(山东)新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims to solve the technical problems of high imidization temperature and long time in the process of preparing conventional polyimide in the existing method, and provides a kind of soluble, low-temperature rapid imidization polyimide film preparation method

Method used

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  • Preparation method of soluble low-temperature rapid imidization polyimide film
  • Preparation method of soluble low-temperature rapid imidization polyimide film
  • Preparation method of soluble low-temperature rapid imidization polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 120g of diglyme at room temperature into a 250mL three-necked flask equipped with mechanical stirring, add 4.4g (0.0150mol) of p-bis(5-amino-3-pyridyloxy)benzene, stir to dissolve it, and pass N 2 , add 10g (0.0156mol) 4-phenyl-2,6-bis[4-(3,4-dicarboxycyclohexane ether) phenyl]pyridine dianhydride in 3 times within 1h, and then continue at room temperature Stir for 20 hours to obtain a polyamic acid solution, vacuum degassing for 10 minutes, apply the solution to a 50 μm thick film on a dry and clean glass plate with a film applicator, and place it in a vacuum oven at 190 ° C to the maximum vacuum degree for 90 minutes. After reaching room temperature, peel off from the glass plate to obtain the polyimide film, which is soluble in diglyme at room temperature. The reaction circuit diagram of the polyimide film of the present embodiment is shown in figure 1 .

Embodiment 2

[0035] Add 120g of N,N-dimethylacetamide into a 250mL three-necked flask equipped with mechanical stirring at room temperature, add 5.6g (0.0151mol) of 2,2'-bis(5-amino-3-pyridyloxy)bis Benzene, stirred to dissolve, through N2 , add 11g (0.0157mol) 4-phenyl-2,6-bis[3-(3,4-dicarboxycyclohexyl ester) phenyl]pyridine dianhydride in 3 times within 1h, and then continue at room temperature Stir for 24 hours to obtain a polyamic acid solution, vacuum defoam for 10 minutes, use a film applicator to coat the obtained polyamic acid solution on a dry and clean glass plate into a film with a thickness of 40 μm, and place it in a vacuum box at 180°C to evacuate to the maximum vacuum temperature insulation for 80min, after being down to room temperature, peel off from the glass plate to obtain a polyimide film, which can be dissolved in N,N-dimethylacetamide at room temperature, the reaction circuit of the polyimide film of the present embodiment picture see figure 2 .

Embodiment 3

[0037] Add 140g of N,N-dimethylacetamide to a 250mL three-necked flask equipped with mechanical stirring at room temperature, add 6.75g (0.0230mol) of 3,5-bis(3-amino-5-pyridyloxy)pyridine, Stir to dissolve, pass N 2 , add 15.31g (0.0243mol) 4-phenyl-2,6-bis[3-(3,4-dicarboxyphenyl ether) phenyl]pyridine dianhydride in 3 times within 1h, then continue to stir at room temperature The polyamic acid solution was obtained in 18 hours, vacuum degassed for 10 minutes, and the obtained polyamic acid solution was coated on a dry and clean glass plate to form a 40 μm thick film with a film applicator, and placed in a vacuum oven at 175 ° C to the maximum vacuum degree Insulated for 60min, after being lowered to room temperature, peel off from the glass plate to obtain a polyimide film, which can be dissolved in N,N-dimethylacetamide at room temperature, the reaction circuit diagram of the polyimide film of this embodiment See image 3 .

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Abstract

The invention discloses a preparation method of a soluble and low-temperature rapid imidization polyimide film, and belongs to the technical field of polyimide film preparation. The method comprises the following steps: a polar aprotic organic solvent with a boiling point lower than 200 DEG C is adopted as a solvent, and the polar aprotic organic solvent comprises one or more of diethylene glycol dimethyl ether, diethylene glycol diethyl ether, N,N-dimethyl acetamide, N,N-dimethyl formamide and dimethyl sulfoxide. According to the present invention, the polyimide film can be rapidly prepared through the imidization at the temperature of less than 200 DEG C, and the imidization process does not require the use of any catalyst, such that the important practical significance is provided for the production efficiency improving and the energy consumption reducing.

Description

technical field [0001] The invention relates to the technical field of polyimide film preparation, in particular to a preparation method of a soluble, low-temperature rapid imidization polyimide film. Background technique [0002] Polyimide is a type of polymer containing imide rings in the main chain. Aromatic polyimide is widely used in aerospace, electronic and electrical industries due to its excellent high temperature resistance, mechanical properties, corrosion resistance and other comprehensive properties. Cutting-edge technology fields such as automobile manufacturing. [0003] In recent years, polyimide films have received increasing attention in the fields of semiconductor materials, nonlinear optical materials, and electronic materials based on their good electrical insulation and adhesive properties. The main chain of traditional aromatic polyimide has rigid benzene rings and strong intermolecular forces between the main chains, resulting in a high glass transit...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08J5/18C08L79/08
CPCC08G73/1085C08G73/1007C08J5/18C08J2379/08
Inventor 王新波李开明郭逸
Owner 富优特(山东)新材料科技有限公司
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