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Modified polyimide film and modified polyimide precursor composite film waste material recovery processing method

A polyimide precursor and polyimide film technology, applied in the chemical industry, can solve the problems of unspecified separation of inorganic nano-fillers, difficulty in recycling and processing, etc., and achieve the effects of shortening time, improving purity, and increasing reaction rate

Inactive Publication Date: 2015-08-19
WUXI SHUNXUAN NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the introduction of various nano-inorganic fillers, it also brings difficulties to recycling
How to separate this part of inorganic nano fillers is not pointed out in the prior art

Method used

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  • Modified polyimide film and modified polyimide precursor composite film waste material recovery processing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Preparation of glass fiber (GF) suspension

[0032] Using 12.5g of nano-sized glass fiber (GF), add 2000ml of aprotic solvent N,N-dimethylacetamide (DMAc), under the condition of 20kHz ultrasonic dispersion, fully stir for 60min to make a stable suspension.

[0033] (2) Preparation of modified polyamic acid composite solution

[0034] Add the suspension obtained above into the polyamic acid polymerization reactor, control the temperature at 10-60°C, add 239.3g of 4,4'-diaminodiphenyl ether, and carry out mechanical stirring. After it is completely dissolved, the temperature Between 50 and 60°C, add 260.7 g of pyromellitic dianhydride in batches while stirring to prepare a polyamic acid composite solution with uniform viscosity and stability.

[0035] (3) Preparation of modified polyimide film and its polyimide precursor composition film

[0036] Put the polyamic acid composite solution obtained above to form a liquid film on a clean steel plate, put it in an oven,...

Embodiment 2

[0042] Replace the glass fiber (GF) in Example 1 with silica, the yield of 4,4'-diaminodiphenyl ether is 63.7g, the product purity is 99.9%, and the melting point is 191-192°C. The yield of the pyromellitic dianhydride product was 69.0 g. The product has a purity of 99.5% and a melting point of 284-285°C. Except above changes, other operation steps and product quality are consistent with embodiment 1.

Embodiment 3

[0044] Change glass fiber (GF) into alumina (Al 2 o 3 ), the yield of 4,4'-diaminodiphenyl ether was 63.5g. The purity of the product is 99.9%, and the melting point is 191-192°C. The yield of the pyromellitic dianhydride product was 68.5 g. The product has a purity of 99.5% and a melting point of 284-285°C. Except above changes, other operation steps and product quality are consistent with embodiment 1.

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Abstract

The invention discloses a modified polyimide film and modified polyimide precursor composite film waste material recovery processing method. The method is characterized by comprising the following steps: crushing a modified polyimide precursor composite film waste material into modified polyimide film waste material fragments with length smaller than 5mm, placing the fragments into stronger ammonia water, hydrolyzing the fragments, and centrifuging or filtering the reaction solution after the reaction is ended; acidifying the separated filter liquid by utilizing hydrochloric acid, and precipitating coarse benzene tetracarboxylic acid; washing separated insoluble substances by utilizing hydrochloric acid or sulfuric acid, carrying out the secondary centrifuging or filtering, and obtaining a coarse 4,4minute-diaminodiphenyl ether aqueous solution; neutralizing the obtained 4,4minute-diaminodiphenyl ether aqueous solution by utilizing ammonia water until the pH value is equal to 8 to 10, and precipitating 4,4minute-diaminodiphenyl ether. By adopting the method, the reaction rate is increased, the time is shortened, inorganic filler in the modified polyimide film waste material can be effectively removed, and the purity of a hydrolysis product can be further improved.

Description

Technical field: [0001] The invention belongs to the technical field of chemical industry, and relates to a recycling processing technology of polyimide film waste, in particular to a recycling processing technology of polyimide film modified by nanometer inorganic filler and polyimide precursor composition film waste. Background technique [0002] Polyimide refers to a class of polymers containing imide rings (-CO-NH-CO-) on the main chain, among which polymers containing imide structures are the most important. As a special engineering material, polyimide has been widely used in aviation, aerospace, microelectronics, nanometer, liquid crystal, separation membrane, laser and other fields. In the 1960s, all countries were researching, developing and utilizing polyimide. Polyimide is listed as one of the most promising engineering plastics in the 21st century. Because of its outstanding characteristics in performance and synthesis, polyimide, whether as a structural materia...

Claims

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Application Information

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IPC IPC(8): C08J11/16C08L79/08
CPCY02W30/62
Inventor 吕亮宋艳江刘顺祯
Owner WUXI SHUNXUAN NEW MATERIALS
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