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A kind of method for preparing polyimide molding powder by solid phase polymerization

A technology of polyimide and solid phase polymerization, which is applied in the field of polyimide molding powder prepared by solid phase polymerization, can solve the problems of long polyimide synthesis process, low production efficiency, difficult solvent recovery and treatment, etc., and achieve Excellent mechanical properties, improved production efficiency, and no three wastes

Active Publication Date: 2022-02-18
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to provide a method for preparing polyimide molding powder by solid phase polymerization, which solves the problems of long polyimide synthesis process, difficult solvent recovery and low production efficiency, etc.

Method used

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  • A kind of method for preparing polyimide molding powder by solid phase polymerization
  • A kind of method for preparing polyimide molding powder by solid phase polymerization
  • A kind of method for preparing polyimide molding powder by solid phase polymerization

Examples

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Embodiment 1

[0051] After biphenyl dianhydride, diphenyl ether dianhydride, diaminodiphenyl ether, and maleic anhydride geraniol ester are pulverized separately, the main ingredients of biphenyl dianhydride, diphenyl ether dianhydride and diaminodiphenyl ether are calculated according to the molar ratio 8:2:10, the mass ratio of the total main ingredients to geraniol maleic anhydride is 100:0.5, and the ratio is mixed with a high-speed mixer before use. Raise the temperature of the twin-screw extruder with a screw diameter of 26mm, the temperature of the feeding section is 50°C and the constant temperature of the cooling water is turned on, the first section is 180°C, the second section is 250°C, the third section is 330°C, and the fourth section to the first section Section 8 is 370°C. The screw aspect ratio is 42:1. There is an air extraction hole in the first section and the second section, and the vacuum degree is maintained at -0.06MPa. Feed the uniformly mixed material continuously...

Embodiment 2

[0054] After the biphenol diether dianhydride, diaminodiphenyl ether, and maleic anhydride linalool ester are pulverized respectively, the main ingredients of biphenyldiphenol diether dianhydride and diaminodiphenyl ether are in a molar ratio of 1:1, The mass ratio of the sum of the main ingredients to linalool maleic anhydride is 100:0.1. After being pulverized separately, it is mixed with a high-speed mixer and set aside. The temperature of the twin-screw extruder with a screw diameter of 20mm is raised, the temperature of the feeding section is 70°C and the constant temperature of the cooling water is turned on, the first section is 160°C, the second section is 230°C, the third section is 270°C, and the fourth section to The tenth stage is 340°C. The screw aspect ratio is 50:1. Set the feed rate to 19.8 g / min and the screw speed to 60 rpm. There is an air extraction hole on the 2nd section and the 3rd section respectively, and the vacuum degree is maintained at -0.07MPa. ...

Embodiment 3

[0057] After bisphenol A diether dianhydride, p-phenylenediamine, and citraconic anhydride nerol ester are pulverized respectively, the main ingredients of bisphenol A diether dianhydride and p-phenylenediamine are according to the molar ratio of 1:1, the sum of the main ingredients and The mass ratio of citraconic anhydride nerol ester is 100:4.7, after being pulverized respectively, mixed with a high-speed mixer for later use. Raise the temperature of the single-screw extruder with a diameter of 35mm. The temperature of the feeding section is 90°C and the constant temperature of the cooling water is turned on. The first section is 170°C, the second section is 250°C, the third section is 270°C, and the fourth section to the first section The 10th section is 330°C. The screw aspect ratio is 56:1. Set the feed rate to 60g / min and the screw speed to 100rpm. Install air extraction holes on the 2nd and 3rd paragraphs, and keep the vacuum at -0.055MPa. Feed the uniformly mixed m...

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Abstract

The invention provides a method for preparing polyimide molding powder by solid-phase polymerization, comprising the following steps: separately making aromatic dibasic amines, aromatic dibasic acid anhydrides and toughening plasticizer butenedioic anhydride esters After being pulverized, they are mixed evenly in a high-speed mixer; the mixed materials are continuously fed in a continuously rotating screw conveying device, and react to form polyimide; the generated polyimide passes through the rotation, extrusion and The temperature is controlled to form polyimide particles and then pulverized to obtain polyimide molding powder. The method does not use organic solvents and belongs to a green production route, and the prepared polyimide sheet has high strength, impact resistance, and mechanical properties better than polyimide prepared by a solvent method.

Description

technical field [0001] The invention belongs to the technical field of polyimide synthesis, and in particular relates to a method for preparing polyimide molding powder by solid phase polymerization. Background technique [0002] Polyimide is a class of high-performance special heat-resistant materials that can be used under extreme conditions of high temperature. Due to its extremely high temperature, most polyimide products are formed by molding, and even need to be sintered after initial molding to form the final shape, such as the classic polyimide resin VESPLE. Sintered molding (US3179631). [0003] There are many ways to synthesize polyimide molding powder or molding particles. US3179631 discloses a polyimide polycondensation method using an aprotic polar solvent: dianhydride and diamine in N,N-dimethylacetamide , N,N-dimethylformamide or N-methylpyrrolidone polycondensation at low temperature to obtain a polyamic acid solution, and then add acetic anhydride and a te...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08G73/10C08K5/101
CPCC08G73/1007C08G73/1067C08G73/1071C08K5/101
Inventor 陈海波张鑫仇伟石耀东杨开业徐延伟原博郑福群刘彪
Owner WANHUA CHEM GRP CO LTD