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Method for preparing polyimide using water as dispersion medium and method for recovering water

A technology of polyimide and polyimide membrane, which is applied in the field of recycling water used as a dispersion medium, can solve problems such as environmental pollution, increase in preparation cost, and residual solvents, and achieve reduction of environmental pollution, reduction of preparation cost, and reaction The effect of low temperature

Active Publication Date: 2017-02-22
IND ACADEMIC CORP FOUND YONSEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022] In the present invention, in order to solve the problems of environmental pollution, production cost increase, residual solvent, etc. produced by using organic solvents in the existing polyimide preparation method, a new method of using water as a dispersion medium is proposed. preparation method

Method used

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  • Method for preparing polyimide using water as dispersion medium and method for recovering water
  • Method for preparing polyimide using water as dispersion medium and method for recovering water
  • Method for preparing polyimide using water as dispersion medium and method for recovering water

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preparation example Construction

[0037] More specifically, the present invention relates to a method for preparing polyimide. The method for preparing the above-mentioned polyimide includes: step a), dispersing the dianhydride compound and the diamine compound in water; and step b), dissolving the above-mentioned dispersion After placing in a pressure vessel and sealing it, the dianhydride compound and the diamine compound are reacted at a temperature of 5° C. to 400° C. under pressure.

[0038] The present invention relates to a preparation method of polyimide, the preparation method of the above polyimide also includes: step a), dispersing the dianhydride compound and the diamine compound in water; step b), putting the above dispersion liquid into a pressure vessel And after sealing, the dianhydride compound and the diamine compound are reacted at a temperature of 5° C. to 400° C. and under pressure; and step c), after step b) is completed, by discharging from the pressure vessel in step b ) to cool and con...

Embodiment 1-1

[0074] Example 1-1: Preparation of wholly aromatic polyimide

[0075] 22.6 g of pyromellitic dianhydride and 21.13 g of 4,4'-diaminodiphenyl ether were dispersed in 200 mL of distilled water. After transferring the above reaction solution to a 500mL pressure vessel with a stirrer, a nitrogen injection device and a temperature regulator attached, the air in the pressure vessel was replaced with nitrogen gas, and the temperature was adjusted to 135°C, and then under a pressure of 60bar, The polyimide was synthesized by stirring for 3 hours. After the above reaction was completed, water vapor was discharged from the pressure vessel and passed through a transfer pipe and a cooler in order to cool and condense the water vapor, thereby recovering about 180 mL of distilled water. The recovered distilled water was subjected to nuclear magnetic resonance (NMR), and it was finally confirmed that no impurities were present. In the infrared absorption spectrum of the synthesized polymer...

Embodiment 1-2

[0076] Embodiment 1-2. Preparation of fully aromatic polyimide

[0077] Disperse 11.106 g of 4,4'-(hexafluoroisopropylidene)bisaniline and 8.005 g of 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl in 200 mL of distilled water middle. After transferring the above reaction solution to a 500mL pressure vessel with a stirrer, a nitrogen injection device and a temperature regulator attached, the air in the pressure vessel was replaced with nitrogen gas, and the temperature was adjusted to 135°C, and then under a pressure of 60bar, The polyimide was synthesized by stirring for 3 hours. After the above reaction was completed, water vapor was discharged from the pressure vessel and passed through a transfer pipe and a cooler in order to cool and condense the water vapor, thereby recovering about 180 mL of distilled water. NMR was performed on the recovered distilled water, and it was finally confirmed that no impurities were present. In the infrared absorption spectrum of the synth...

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Abstract

The present invention relates to a method for preparing a polyimide using water as a dispersion medium for reaction and, more particularly, to a method for preparing a polyimide by dispersing a dianhydride compound and a diamine compound in water and reacting the compounds in a pressurized state within a sealed pressure vessel under temperature conditions of 5 degrees or above. The present invention also provides a method for recovering water by discharging vapor generated during the preparation of the polyamide and cooling and condensing the vapor. By using water as a dispersion medium, the method according the present invention does not generate organic-based waste fluid and is thus environmentally-friendly, reduces production costs, minimizes residual solvents after drying and thus does not have a problem that physical properties are degraded due to the residual solvents, and is advantageous in that the reaction temperature is lower, reaction steps are reduced, and the reaction time is shortened compared to conventional methods. Since water can be recovered after the reaction is completed, the method also allows recycling of water and is thus economical and very environmentally-friendly. In addition, the polyimide prepared by the method according to the present invention has the advantage of increasing thermal stability and molecular weight compared to polyimides prepared by conventional synthesis methods.

Description

technical field [0001] The present invention relates to the preparation method of polyimide, relate to the preparation method of the polyimide that uses water as dispersing medium in more detail and the method for reclaiming the water that is used as dispersing medium, by using water as dispersing medium, come The organic waste liquid is produced, which is environmentally friendly, the preparation cost is low, and the residual solvent can be minimized after drying. Background technique [0002] With the development of high technology, high heat-resistant polymer materials are used as necessary raw materials for the miniaturization, high performance and high reliability of products, such as films, molded products, fibers, coatings, adhesives and composite materials. Forms of materials, etc., are used in a wide range of industrial fields such as aerospace, aviation, electrical / electronics, automobiles, and precision instruments. Among them, films mainly developed as electroni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J3/00C08J5/18C08L79/08
CPCC08G73/10C08J3/00C08J5/18C08L79/08
Inventor 郑灿文刘焕哲李雄熙
Owner IND ACADEMIC CORP FOUND YONSEI UNIV
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