Method for recovery processing of modified polyimide film wastes

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

Inactive Publication Date: 2015-09-30
WUXI SHUNXUAN NEW MATERIALS +1
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Due to the introduction of various nano-inorganic fillers, it also brings difficulties to rec

Method used

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  • Method for recovery processing of modified polyimide film wastes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Preparation of glass fiber (GF) suspension

[0030] 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.

[0031] (2) Preparation of modified polyamic acid composite solution

[0032] 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.

[0033] (3) Preparation of modified polyimide film

[0034] Put the polyamic acid composite solution obtained above to form a liquid film on a clean steel plate, put it in an oven, control the temperature at 150-200°C, and ta...

Embodiment 2

[0040] Replace the glass fiber (GF) in Example 1 with silica, the yield of 4,4'-diaminodiphenyl ether is 64.5g, the product purity is 99.9%, and the melting point is 191-192°C. The yield of the pyromellitic dianhydride product is 69.3g, the product purity is 99.5%, and the melting point is 284-285°C. Except above changes, other operation steps and product quality are consistent with embodiment 1.

Embodiment 3

[0042] Change glass fiber (GF) into alumina (Al 2 o 3 ), the yield of 4,4'-diaminodiphenyl ether was 64.1g. The purity of the product is 99.9%, and the melting point is 191-192°C. The yield of the pyromellitic dianhydride product was 68.9 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 method for recovery processing of modified polyimide film wastes. The method comprises the following steps: crushing the modified polyimide film wastes into modified polyimide film waste scraps with the length of less than 5mm, hydrolyzing the scraps in concentrated ammonia water, and performing centrifuging or filtration after reaction; acidifying a separated filtrate by using hydrochloric acid, and separating out crude pyromellitic acid; washing separated undissolved substances by using hydrochloric acid or sulfuric acid, and then performing secondary centrifuging or filtration to obtain a crude 4,4'-diaminodiphenyl ether aqueous solution; and neutralizing the obtained crude 4,4'-diaminodiphenyl ether aqueous solution by using ammonia water until the pH value is equal to 8-10, and then separating out 4,4'-diaminodiphenyl ether. By adopting the method disclosed by the invention, the reaction rate is increased, the time is shortened, and meanwhile, inorganic fillers in the modified polyimide film wastes can be effectively removed to further improve the purity of a hydrolysis product.

Description

Technical field: [0001] The invention belongs to the technical field of chemical industry and relates to a recycling process of polyimide film waste, in particular to a recycling process of polyimide film waste modified by nano inorganic fillers. 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 material or as a functional material, has been fully recognized for its huge appl...

Claims

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Application Information

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IPC IPC(8): C07C217/90C07C213/00C07C63/313C07C51/06
Inventor 吕亮宋艳江刘顺祯
Owner WUXI SHUNXUAN NEW MATERIALS
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