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Polyimide resin and preparation method thereof

A polyimide resin and the same technology, applied in the field of polyimide resin and its preparation, can solve the problems of low open-hole compressive strength, unsatisfactory service temperature upper limit of composite materials, unsatisfactory toughness, etc., and achieve low porosity , high mechanical properties, excellent heat resistance

Inactive Publication Date: 2008-06-04
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Chuang et al. (A high TgPMR polyimide composites (DMBZ-15), Journal of Advanced Materials, 33 (4), p33) of NASA in 2001 reported a kind of PMR type polyimide matrix resin (DMBZ-15), the The matrix resin has a high glass transition temperature, and the prepared resin-based composite has excellent bending strength and interlaminar shear strength at high temperature, but its open-hole compressive strength is low and the toughness is not ideal
In 2003, Chuang et al. (6F-polyimides with phenylethylenyl endcap for 315-370°C applications, High Performance Polymers, 15(4), p459.) reported the use of phenylacetylene phthalic anhydride as a capping agent to prepare PMR polyimide resin base Composite materials, composite materials have high toughness and temperature cycle impact resistance, but the upper limit of the service temperature of composite materials is not ideal

Method used

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  • Polyimide resin and preparation method thereof
  • Polyimide resin and preparation method thereof
  • Polyimide resin and preparation method thereof

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0031] 80 parts by weight of 2,3,3',4'-biphenyltetraacid dianhydride (a-BPDA) was heated under reflux in 100 parts by weight of ethanol for 1 hour to obtain an aromatic diacid diester (a-BPDE) solution. Heat reflux 42 parts by weight of end-capping agent-phenylacetylene phthalic anhydride in 66 parts by weight of ethanol for 5 hours to obtain monoacid monoester (PEPE) solution. Under the protection of nitrogen, dissolve the p-phenylenediamine (p-PDA) of 30 parts by weight in the ethanol of 40 parts by weight, add the PEPE and a-BPDE solution of above-mentioned preparation successively after stirring for half an hour; The mixture was stirred at 5° C. for 15 hours to obtain a polyimide resin matrix solution with a solid content of 42% (weight percent); its viscosity (25° C.) was 25-28 mPa.s. The resin solution has good storage stability at room temperature and 0°C, and at room temperature and 0°C, the infrared spectrum absorption peak and viscosity of the resin solution basicall...

Embodiment 2

[0034] 90 parts by weight of 2,3,3', 4'-biphenyltetraacid dianhydride (a-BPDA) was refluxed for 5 hours in 170 parts by weight of ethanol to obtain aromatic diacid diester (a-BPDE ) solution. Heat and reflux 45 parts by weight of end-capping agent-phenylacetylene phthalic anhydride in 60 parts by weight of ethanol for 1 hour to obtain monoacid monoester (PEPE) solution. Under the protection of argon, 72 parts by weight of diamine monomer p-phenylenediamine (p-PDA) and 8 parts by weight of m-phenylenediamine (m-PDA) were dissolved in 110 parts by weight of ethanol, and after stirring for half an hour The previously prepared PEPE and a-BPDE solutions were sequentially added, and the mixture was stirred at 50° C. for 2 hours to obtain a polyimide homogeneous resin solution with a solid content of 39% (weight percent). Its viscosity (25°C) is 24-27mPa.s. The resin solution has good storage stability at room temperature and 0°C, and at room temperature and 0°C, the infrared spect...

Embodiment 3

[0037] 220 parts by weight of 2,3,3',4'-biphenyltetraacid dianhydride (a-BPDA) was heated to reflux in 380 parts by weight of ethanol for 2 hours to obtain an aromatic diacid diester (a-BPDE) solution , 90 parts by weight of 3,3',4,4'-benzophenonetetraacid dianhydride (BTDA) was heated to reflux in 170 parts by weight of ethanol for 3 hours to obtain an aromatic diacid diester (BTDE) solution. Heat reflux 90 parts by weight of end-capping agent-phenylacetylene phthalic anhydride in 130 parts by weight of ethanol for 3 hours to obtain monoacid monoester (PEPE) solution. Under the protection of nitrogen, the diamine monomer p-PDA of 190 parts by weight is dissolved in 200 parts by weight of ethanol, and after stirring for half an hour, PEPE, a-BPDE and BTDE solutions prepared before are added successively, and the mixed solution is in Stirring at 25° C. for 8 hours to obtain a polyimide homogeneous resin solution with a solid content of 40% (weight percent). Its viscosity (25°C...

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Abstract

The invention discloses polyimide resin and a preparation method thereof. The polyimide resin is polymer having molecular structural formula as shown in formulation I. The resin employs aromatic dianhydride, aromatic diamine and reactivity blocking agent as raw materials and is prepared by adopting a PMR method. The process of preparing the invention is that the aromatic dianhydride, the aromatic diamine and the reactivity blocking agent are heated, refluxed and mixed so as to prepare resin solution. The polyimide resin matrix of the invention can directly compounded with enhanced body to prepare resin matrix composites, or the resin solution is die processed after heat treatment to obtain resin molded parts. The polyimide resin matrix solution of the invention is characterized by high solid content, low viscosity, good stability of storage, etc., and the resin molded parts and the resin matrix composites prepared has low porosity, excellent heat resistance, and high mechanical property, and have potential applying value in high-technology field such as spaceflight, aviation, space technology, etc. when being taken as light weight, high-temperature resistant structure components or secondary structure components.

Description

technical field [0001] The invention relates to a polyimide resin for preparing resin-based composite materials and a preparation method thereof. Background technique [0002] Resin Matrix Composite (Resin Matrix Composite), also known as Fiber Reinforced Plastics (Fiber Reinforced Plastics), is a relatively mature technology and the most widely used type of composite materials. Raw materials of resin matrix composites, including raw materials and additives of matrix phase and reinforcement phase. The matrix phase material refers to various polymers as a matrix, including thermosetting resins and thermoplastic resins, and the reinforcement phase material refers to various fibers, such as glass fibers, carbon fibers, aramid fibers, high-density polyethylene fibers, etc. [0003] Polyimide resin is a high-performance resin used as a matrix material for high-performance composite materials. In 1972, T.T.Serafini et al. (Thermally Stable Polyimide fromSolutions of Monomeric Re...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08L79/08
Inventor 杨士勇陈建升左红军范琳高群峰
Owner INST OF CHEM CHINESE ACAD OF SCI
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