Method for preparing polyimide in supercritical carbon dioxide

A technology of carbon dioxide and polyimide, applied in the production of bulk chemicals, etc., can solve problems such as high pollution, difficult solvent treatment, unstable quality of melt polymerization products, etc., and achieve the effect of pure products and simple and practical methods

Active Publication Date: 2012-11-07
HANGZHOU SURMOUNT SCI & TECH +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The object of the present invention is to provide a kind of new method for preparing polyimide, namely the method for synthesizing polyimide in supercritical carbon dioxide, this method will solve the high problem that organic solvent causes as dispersion medium in the prior art Pollution, difficult problems of solvent treatment, solve the problem of low reaction concentration in the prior art using water as the medium and the problem of unstable quality of melt polymerization products

Method used

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  • Method for preparing polyimide in supercritical carbon dioxide

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Effect test

Embodiment 1

[0018] Add 200g 4,4'-diaminodiphenyl ether, 215g pyromellitic dianhydride, 4.14g phthalic anhydride and 22g pyridine in the autoclave under the protection of nitrogen, then close the reaction vessel, vacuumize and ventilate Add carbon dioxide, heat the temperature to 50°C, supplement the pressure of the reactor, when the temperature reaches 60°C, control the pressure of the reactor to 20MPa, turn on the electromagnetic stirring, after 3 hours of reaction, raise the temperature to 200°C, control the pressure of the reactor to 50MPa, continue React for 4 hours, end the reaction, slowly open the release valve, control the release time to 2 hours, to remove a small amount of by-product-water, then open the reaction kettle, and treat the product in a vacuum oven at 300°C for 3 hours to obtain an orange-yellow product. The rate is 94%.

Embodiment 2

[0020] Add 210g 4,4'-bis(3-aminophenoxybenzene) propane, 105g pyromellitic dianhydride, 2.32g phthalic anhydride and 12g triethylamine in autoclave under nitrogen protection, and then Close the reaction vessel, evacuate, inject carbon dioxide, heat the temperature to 50°C, and supplement the pressure of the reactor. When the temperature reaches 50°C, control the pressure of the reactor to 20MPa, turn on the electromagnetic stirring, and after 1 hour of reaction, raise the temperature to 180°C. Control the pressure of the reactor to 50MPa, continue the reaction for 8 hours, end the reaction, slowly open the vent valve, and control the venting time for 2 hours to remove a small amount of by-product-water, then open the reactor, and treat the product in a vacuum oven at 260°C After 3h, a light yellow product was obtained with a yield of 92%.

Embodiment 3

[0022]Add 98g 4,4'-diaminodiphenyl ether, 165g 4,4'-oxydiphthalic anhydride, 1.92g aniline and 12g triethylamine to the autoclave under nitrogen protection, then seal the reaction vessel, Vacuumize, feed carbon dioxide, heat the temperature to 50°C, supplement the pressure of the reactor, when the temperature reaches 60°C, control the pressure of the reactor to 20MPa, turn on the electromagnetic stirring, after 2 hours of reaction, raise the temperature to 200°C, control the pressure of the reactor to 50MPa, continue to react for 6h, end the reaction, slowly open the vent valve, control the vent time to 2 hours to remove a small amount of by-product-water, then open the reaction kettle, and treat the product in a vacuum oven at 280°C for 3h to obtain a yellow Product, the yield is 91%.

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Abstract

The invention relates to a method for preparing polyimide by performing polymerization reaction in supercritical carbon dioxide, belongs to the technical field of synthesis of polyimide polymer, and solves the technical problems that an organic solvent is needed and subsequent treatment difficulty is high in the synthesis reaction process of the polyimide in the prior art. According to the method, the polyimide is synthesized by taking acid anhydride or aniline as a blocking agent and the supercritical carbon dioxide as a medium. The method comprises the following steps of: adding dianhydride, a diamine monomer, a catalyst and the blocking agent into a reaction kettle at one time or in batches, introducing carbon dioxide, and gradually raising temperature and pressure to ensure that a system is in a supercritical state; and polymerizing at certain temperature and pressure to obtain a polyimide product with a good shape and high performance. The organic solvent is not used, the product is pure, subsequent treatment is not needed, the reaction medium is non-toxic and pollution-free, and the method is an economic, practical and environment-friendly process method for synthesizing and preparing the polyimide.

Description

technical field [0001] The invention belongs to the fields of chemical industry and polymer materials, and relates to a method for preparing polyimide in supercritical carbon dioxide. Background technique [0002] Polyimide (PI) refers to a class of polymers containing imide rings on the main chain. [0003] [0004] Polyimide is a high temperature-resistant polymer material that can withstand high temperatures of 500°C for a short time and can be used for a long time below 300°C. As a cutting-edge material with outstanding performance, it is widely used in electromechanical, electronic and electrical, instrumentation, petrochemical, measurement and other fields with its excellent electrical insulation, wear resistance, high temperature radiation resistance and physical and mechanical properties, and has become a global rocket One of the indispensable materials in cutting-edge technology fields such as aerospace, aerospace, etc. However, its output and consumption are re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
CPCY02P20/54
Inventor 黄健邵志平丁洪董胜倪林碧查道鑫
Owner HANGZHOU SURMOUNT SCI & TECH
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