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Polyimide film with high strength, high thermal stability, high transparency and low glass transition temperature and preparation method thereof

A technology of polyimide film and transition temperature, applied in the field of polymer materials, can solve the problems of unrecyclable harmful catalysts, complicated reaction steps, incomplete imidization, etc., achieve good visible light transmittance, reduce rigidity, and process The effect of cost reduction

Active Publication Date: 2021-05-25
JIANGHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional PI mostly uses aromatic diamine dianhydride monomers. This type of PI has good thermal properties, but has poor flexibility, is insoluble and infusible, has poor processability, and high processing costs.
The existing technology mostly uses chemical imidization, the reaction steps are complicated, the operation is cumbersome, and there is a problem of incomplete imidization, and some harmful catalysts cannot be recovered, which will bring certain pollution

Method used

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  • Polyimide film with high strength, high thermal stability, high transparency and low glass transition temperature and preparation method thereof
  • Polyimide film with high strength, high thermal stability, high transparency and low glass transition temperature and preparation method thereof
  • Polyimide film with high strength, high thermal stability, high transparency and low glass transition temperature and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1 A kind of preparation method of polyimide film with low glass transition temperature

[0035] 1) Clean all the glass instruments to be used in the experiment and dry them for later use. At room temperature (25°C), add 3,3′-diethyl -4,4'-diaminodiphenylmethane (0.4070g, 1.6mmol), 1,3-bis(4'-aminophenoxy)benzene (0.1170g, 0.4mmol) and 3.5443g N,N-dimethyl base acetamide, magnetic sub-stir until completely dissolved, to obtain a mixed solution;

[0036] 2) Add 3,3',4,4'-benzophenone tetracarboxylic dianhydride (0.6575g, 2.04mmol) to the mixed solution obtained in step 1), the solid content is 25% (solid content is m DEDDM+TPE-R+BTDA / m DEDDM+TPE-R+BTDA+DMAc ) was stirred and dissolved, and reacted at room temperature for 12h to obtain polyamic acid glue;

[0037] 3) Drop the polyamic acid glue liquid obtained in step 2) on a clean glass plate, apply it evenly with a spatula, and heat imidize it through programmed temperature rise. ; 10°C / min to 120°C, vacu...

Embodiment 2

[0038] Embodiment 2 A kind of preparation method of polyimide film with low glass transition temperature

[0039]1) Clean all the glass instruments to be used in the experiment and dry them for later use. At room temperature (25°C), add 3,3′-diethyl -4,4'-diaminodiphenylmethane (0.3053g, 1.2mmol), 1,3-bis(4'-aminophenoxy)benzene (0.2340g, 0.8mmol) and 3.5904g N,N-dimethyl base acetamide, magnetic sub-stir until completely dissolved, to obtain a mixed solution;

[0040] 2) Add 3,3',4,4'-benzophenone tetracarboxylic dianhydride (0.6575g, 2.04mmol) to the mixed solution obtained in step 1), the solid content is 25% (solid content is m DEDDM+TPE-R+BTDA / m DEDDM+TPE-R+BTDA+DMAc ) was stirred and dissolved, and reacted at room temperature for 12h to obtain polyamic acid glue;

[0041] 3) Drop the polyamic acid glue liquid obtained in step 2) on a clean glass plate, apply it evenly with a spatula, and heat imidize it through programmed temperature rise. ; 10°C / min to 120°C, vacuu...

Embodiment 3

[0042] Embodiment 3 A kind of preparation method of polyimide film with low glass transition temperature

[0043] 1) Clean all the glass instruments to be used in the experiment and dry them for later use. At room temperature (25°C), add 3,3′-diethyl -4,4'-diaminodiphenylmethane (0.2544g, 1mmol), 1,3-bis(4'-aminophenoxy)benzene (0.2924g, 1mmol) and 3.6129g N,N-dimethylethyl Amide, stirred with a magnet until completely dissolved to obtain a mixed solution;

[0044] 2) Add 3,3',4,4'-benzophenone tetracarboxylic dianhydride (0.6575g, 2.04mmol) to the mixed solution obtained in step 1), the solid content is 25% (solid content is m DEDDM+TPE-R+BTDA / m DEDDM+TPE-R+BTDA+DMAc ) was stirred and dissolved, and reacted at room temperature for 12h to obtain polyamic acid glue;

[0045] 3) Drop the polyamic acid glue liquid obtained in step 2) on a clean glass plate, apply it evenly with a spatula, and heat imidize it through programmed temperature rise. ; 10°C / min to 120°C, vacuum in...

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Abstract

The invention relates to the technical field of high polymer materials, in particular to a polyimide film with high strength, high thermal stability, high transparency and low glass transition temperature and a preparation method thereof. According to the preparation method, diamine 3,3'-diethyl-4,4'-diaminodiphenylmethane (DEDDM), 1,3-bis(4'-aminophenoxy)benzene (TPE-R) or 1,3-bis (3-aminophenoxy)benzene (TPE-M) and dianhydride 3,3',4,4'-benzophenone tetracarboxylic dianhydride (BTDA) are selected and subjected to thermal imidization to prepare the polyimide film; an ethyl group is introduced into the prepared polyimide film so as to destroy the planarity of a main chain; meanwhile, a methylene group is introduced to destroy a conjugated structure, so the solubility and the optical transmittance of the film are improved; and moreover, ether bonds and keto-carbonyl groups are introduced, so the polyimide film with both flexibility and thermal stability can be obtained. According to the invention, the glass transition temperature of the PI film is reduced through structural modification, the strength, flexibility and transparency of the PI film are improved the cost for preparing the PI film is low, and the preparation process of the PI film is simple.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a polyimide film with high strength, high thermal stability, high transparency and low glass transition temperature and a preparation method thereof. Background technique [0002] With the wide application of high-strength and high-thermal-stability materials in various fields, polyimide (PI) has become an increasingly important material due to its light weight, flexibility, and ultra-thin properties. Since the advent of polyimide, the world's demand for it has grown at an annual rate of almost 6.5%, ranging from photovoltaic energy, semiconductor packaging, liquid crystal displays, to military, automotive, aviation and other fields, the lightweight and small size of electronic products Chemicalization makes polyimide occupy an increasingly important position, and PI has developed into one of the most widely used heat-resistant polymer materials. [0003] Although poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08J5/18C08G73/10
CPCC08J5/18C08G73/1042C08G73/1071C08G73/1007C08J2379/08
Inventor 胡思泉王刚蔡才卢春燕王亚珍汪海平
Owner JIANGHAN UNIVERSITY
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