Crosslinking type aromatic polyimide material and preparation method thereof

A technology of aromatic polyimide and polyimide, which is applied in the field of cross-linked aromatic polyimide materials and its preparation, can solve problems such as material defects and affecting material performance, so as to reduce defects and improve Mechanical properties, the effect of simple synthesis method

Inactive Publication Date: 2017-08-08
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the reaction of oligomer active groups in the process of crosslinking, most of the small molecules will be generated. If they cannot be eliminated in time, defects will often occur in the material and affect the performance of the material. Polyimide materials without small molecules are imminent
[0005]

Method used

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  • Crosslinking type aromatic polyimide material and preparation method thereof
  • Crosslinking type aromatic polyimide material and preparation method thereof
  • Crosslinking type aromatic polyimide material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Synthesis of polyamic acid: According to the molar ratio of 3,3'-dimethylbenzidinediamine: benzophenone dianhydride (BTDA)=1:1, 3,3'-dimethylbenzidine Phenylenediamine was added to the dried three-necked flask, and a metered amount of organic solvent N,N-dimethylacetamide (DMAc) was added. Stir under nitrogen to make it fully dissolved, then slowly add BTDA under mechanical stirring, so that the solid content of the solution is 15%. Then control the reaction temperature at 0-30° C. and react for 3 hours to obtain a viscous polyamic acid solution with an intrinsic viscosity of 1.9 dL / g.

[0046] (2) Preparation of polyimide fiber: put the polyamic acid prepared in the first step into the spinneret and defoam, adopt the method of wet hair spinning to prepare polyamic acid fiber, and the coagulation bath used is mass Concentration 6% DMAc aqueous solution. Then, the prepared polyamic acid fiber can be prepared into polyimide fiber by passing through a drying furnace ...

Embodiment 2

[0053] (1) Preparation of polyamic acid: According to the molar ratio of 3,3'-dimethylbenzidinediamine: benzophenone dianhydride (BTDA)=1:1, 3,3'-dimethylbenzidine Phenylenediamine was added to the dried three-necked flask, and a metered amount of organic solvent N,N-dimethylacetamide (DMAc) was added. Stir under nitrogen to make it fully dissolved, then slowly add BTDA under mechanical stirring, so that the solid content of the solution is 10%. Then control the reaction temperature at 0-30° C. and react for 5 hours to obtain a viscous polyamic acid solution with an intrinsic viscosity of 1.8 dL / g.

[0054] (2) Film making and imidization: the polyamic acid solution is evenly spread on the glass plate with a coating rod with a groove of 1 mm, and placed in the air to dry naturally to evaporate the solvent. Then put the dried film into a temperature-programmed muffle furnace for imidization. The imidization temperature is 350° C. for 2 hours.

[0055] (3) Cross-linking proces...

Embodiment 3

[0060] (1) Preparation of polyamic acid: According to the molar ratio of 3,3'-dimethylbenzidine diamine: benzophenone dianhydride (BTDA): biphenyl dianhydride (BPDA) = 2:1:1, Add 3,3'-dimethylbenzidinediamine into the dried three-necked flask, and add a metered amount of organic solvent N,N-dimethylacetamide (DMAc). Stir under nitrogen to make it fully dissolved, then slowly add BTDA and BPDA that are uniformly mixed under mechanical stirring, so that the solid content of the solution is 8%. Control the reaction temperature at 0-30° C. and react for 3 hours to obtain a viscous ternary copolymerization polyamic acid solution with an intrinsic viscosity of 1.7 dL / g.

[0061] (2) Film making and imidization: the polyamic acid solution is evenly spread on the glass plate with a coating rod with a groove of 1 mm, and placed in the air to evaporate the solvent. Then put the dried film into a temperature-programmed muffle furnace for imidization. The imidization temperature is 350° ...

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Abstract

The invention relates to a crosslinking type aromatic polyimide material containing methyl and having a main chain containing carbonyl and a preparation method thereof, which belongs to the technical field of synthesis of high molecular materials. A preparation process comprises the following steps: introducing a structure similar to diphenylketone and methyl into a polyimide molecular chain; synthesizing cross-linkable polyimide which contains the methyl and has the main chain containing the carbonyl and carrying out cross-linking treatment; specifically, taking a dianhydride monomer and a diamine monomer with the equal molar ratio as raw materials and synthesizing polyamic acid; carrying out spinning (or film preparation), imidization and cross-linking processes; finally, obtaining the crosslinking type aromatic polyimide material. The crosslinking type aromatic polyimide material prepared by the preparation method has high molecular weight and good mechanical properties and has excellent heat stability and mechanical properties, good solubility, good film-forming property and good spinnability, relatively low water absorption rate and special optical properties; a final shape of the product can be fiber and also can be thin film and the product has a wide application field.

Description

technical field [0001] The invention belongs to the technical field of polymer materials and their synthesis, and in particular relates to a cross-linked aromatic polyimide material containing methyl groups and carbonyl groups on the main chain and a preparation method thereof. Background technique [0002] Polyimide (PI) is a class of thermosetting or thermoplastic polymers characterized by imide rings. It has light weight, high specific strength and specific modulus, corrosion resistance, solvent resistance, heat stability, outstanding It is widely used in key materials in various fields such as aviation, aerospace, microelectronics, separation membranes and lasers. [0003] However, with the development of science and technology, higher and more stringent requirements are put forward for materials, and the existing polyimide can no longer meet the requirements. Compared with thermoplastic polyimide, cross-linked polyimide has higher temperature resistance and processing ...

Claims

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Application Information

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IPC IPC(8): C08G73/06D01F6/74D06M10/00C08L79/08C08J3/28C08J3/24
CPCC08G73/1067C08J3/24C08J3/28C08J2379/08C08L79/08C08L2203/16D01F6/74D06M10/001
Inventor 牛鸿庆袁东明张梦颖武德珍
Owner BEIJING UNIV OF CHEM TECH
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