Novel mould-pressing polyimide foamed plastic and preparation method thereof

A technology of molding polyimide and foam plastics, which is applied in the field of polyimide foam materials, can solve the problems of foam performance degradation, etc., and achieve the effects of uniform foaming, simple process, and convenience for mass production and popularization and application

Inactive Publication Date: 2013-04-03
QINGDAO ADVANCED MARINE MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method overcomes the deficiency of by-products in the process of preparing diacid diesters from the esterification of aromatic dianhydrides, but the introduction of siloxane reduces the performance of the foam

Method used

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  • Novel mould-pressing polyimide foamed plastic and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 1000ml three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, put 129 grams (0.4mol) of 3,3 , ,4,4 , Benzophenone tetracarboxylic dianhydride (BTDA), 140 grams of anhydrous methanol and 80 grams of tetrahydrofuran were refluxed at 65° C. to form a clear solution, and cooled to room temperature. Add 79.5 g (0.4 mol) 4,4 ， Diaminodiphenylmethane (MDA) and 0.2 grams of isoquinoline catalyst, continue to reflux reaction until clear and transparent, add 0.1% organic fluorine surfactant to prepare a foamable polyimide precursor solution, and put this solution in Vacuum dry in a rotary evaporator at 70°C to remove methanol and tetrahydrofuran. Cool to room temperature to obtain a loose solid-phase polyimide precursor, which is ground into powder to obtain a precursor powder.

Embodiment 2

[0028] In a 1000mL three-neck flask equipped with a stirrer, thermometer, constant temperature water bath and reflux condenser, put 129 grams (0.4mol) of 3,3 , ,4,4 , Benzophenone tetracarboxylic dianhydride (BTDA), 160 grams of anhydrous methanol and 20 grams of distilled water were refluxed at 65°C to obtain a clear solution, and cooled to room temperature. Add 65 g (0.32 mol) 4,4 ， Diaminodiphenylmethane (MDA) reacts until the solid particles disappear, add 9 grams (0.08mol) of diaminopyridine and 0.5 grams of isoquinoline catalyst, continue the reflux reaction until the solution is clear and transparent, add 0.1% organic fluorine surfactant A foamable polyimide precursor solution was obtained, and the solution was vacuum-dried in a rotary evaporator at 70° C. to remove methanol. Cool to room temperature to obtain a loose solid-phase polyimide precursor, which is ground into powder to obtain a precursor powder.

Embodiment 3

[0030] In a 50L stainless steel reaction kettle equipped with a stirrer, a thermometer and a reflux condenser, 1560 grams of 3,3 , ,4,4 , Benzophenone tetracarboxylic dianhydride (BTDA), 2500ml of anhydrous methanol and 1000ml of tetrahydrofuran were refluxed at 75°C to obtain a clear solution, and cooled to room temperature. Add 960g 4,4 ， Diaminodiphenylmethane (MDA) and 15 grams of isoquinoline catalyst were reacted until the solid particles disappeared, and the reflux reaction was continued until the solution was clear and transparent, and 0.1% organic fluorine surfactant was added to prepare a foamable polyimide precursor Solution, the solution was vacuum-dried in batches at 70°C in a rotary evaporator to remove methanol and tetrahydrofuran. Cool to room temperature to obtain a loose solid-phase polyimide precursor, grind it into a polyimide precursor powder with a fineness of 43-35 μ with an ultrafine pulverizer,

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Abstract

The invention discloses a novel mould-pressing polyimide foamed plastic and a preparation method thereof. The foamed plastic comprises the following chemical components based on 100 mass parts of aromatic dianhydride: 100 parts of aromatic dianhydride, 60-70 parts of solvent, 60-65 parts of aromatic diamine, 100-130 parts of fatty alcohol, 1-5 parts of a foam stabilizing agent, 0.5-1 part of a catalyst and 20-30 parts of a foaming agent. The preparation method comprises the following steps of: (1) esterifying the aromatic dianhydride and the fatty alcohol to prepare diacid diester; (2) reacting the diacid diester with the aromatic dianhydride to prepare a precursor solution; (3) preparing a surfactant and a catalyst removal solvent by the precursor solution, drying and grinding into powder; (4) preparing a melt by taking the water as a foaming agent; (5) by a microwave foaming process, preparing a thermoplastic polyimide foam body; and (6) cutting the foam body and carrying out mould-pressing to prepare polyimide foam boards differing in density. The novel mould-pressing polyimide foamed plastic disclosed by the invention is simple in preparation process, dense and uniform in foam bubbles, low in preparation cost and easy in industrial production.

Description

technical field [0001] The invention relates to a novel molded polyimide foam plastic and a preparation method thereof, belonging to the field of polyimide foam materials. Background technique [0002] DuPont of the United States first applied for the polyimide foam patent USP3249561 in 1966. This patent is to add an acid that can generate gas to the polyamic acid solution to generate carbon monoxide or carbon dioxide as a blowing agent to prepare polyimide foam material. , the process technology is backward and has not been used. [0003] US Patent No. 5,077,318 filed by U.S. Ethyl Corporation in 1991 discloses a method for preparing flexible low-density polyimide foams according to required density. With benzophenone tetracarboxylic dianhydride (BTDA) and diaminodiphenylmethane (MDA) as main agent, silanol surfactant, water is as blowing agent, prepare polyimide precursor solution, spray drying Grind into powder. The preparation of flexible polyimide foam by powder foam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J9/04C08L79/08
Inventor 刘连河张树华莫立新王志鹏魏浩
Owner QINGDAO ADVANCED MARINE MATERIAL TECH
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