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Preparation method of polyimide fibers containing symmetric bispyrimidine structures

A technology of polyimide fiber and bispyrimidine, which is applied in the field of preparation of polyimide fiber with symmetrical bispyrimidine structure, can solve the problems of difficult removal of polar solvents and degradation of physical and chemical properties of materials, and achieve high performance , excellent mechanical properties, broad application prospects

Active Publication Date: 2016-06-15
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is often accompanied by many disadvantages such as the difficulty in removing the polar solvent complexed with the polymer, and the reduction of the physical and chemical properties of the material.

Method used

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  • Preparation method of polyimide fibers containing symmetric bispyrimidine structures

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Under nitrogen protection, 500gP 2 o 5 Add polyphosphoric acid with a content of 80% into a 1L reactor, heat to 150°C and stir for 1.5 hours to obtain a clear polyphosphoric acid solution.

[0028] Add successively 62.4g (0.15mol) of diamine monomer 2,2'-(1,4-phenylene)bis[5-(4-aminophenyl)]pyrimidine, 20g of anhydrous stannous chloride, 48.3g (0.15mol) of 3,3',4,4'-benzophenonetetraacid dianhydride (BTDA), and add 166g of P 2 o 5 , the mass of diamine and dianhydride accounts for 14.2% of the total mass of the reaction system, P 2 o 5 The quality accounts for 85% of the polyphosphoric acid solution quality. The temperature was raised, and the reaction system was reacted at 180° C. for 5 hours, and at 220° C. for 5 hours to obtain a liquid crystal polyimide spinning solution. The solution is yellow and transparent, with an intrinsic viscosity of 1.77dL / g (concentrated sulfuric acid as a solvent, measured at 25°C).

[0029] The liquid crystal spinning stock soluti...

Embodiment 2

[0032] Under nitrogen protection, 500gP 2 o 5 Add polyphosphoric acid with a content of 80% into a 1L reactor, heat to 150°C and stir for 1.5 hours to obtain a clear polyphosphoric acid solution.

[0033]Add successively 58.2g (0.14mol) of diamine monomer 2,2'-(1,4-phenylene)bis[5-(4-aminophenyl)]pyrimidine, 18g of anhydrous stannous chloride, 41.1g (0.14mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA), and added 269gP 2 o 5 . The quality of diamine and dianhydride accounts for 11.4% of the total mass of the reaction system, P 2 o 5 The quality accounts for 87% of the polyphosphoric acid solution quality. Then the temperature was raised, and the reaction system was reacted at 190° C. for 4 hours and 230° C. for 5 hours to obtain a liquid crystal polyimide spinning solution. The solution is yellow and transparent, with an intrinsic viscosity of 2.21dL / g (concentrated sulfuric acid is used as a solvent, measured at 25°C).

[0034] The liquid crystal spinning ...

Embodiment 3

[0037] Under nitrogen protection, 500gP 2 o 5 Add polyphosphoric acid with a content of 80% into a 1L reactor, heat to 150°C and stir for 1.5 hours to obtain a clear polyphosphoric acid solution.

[0038] Add successively 70.4g (0.17mol) of diamine monomer 2,2'-(1,4-phenylene)bis[5-(4-aminophenyl)]pyrimidine, 25g of anhydrous stannous chloride, 37.1g (0.14mol) of pyromellitic dianhydride (PMDA) and 240g of P 2 o 5 To the reaction system, the quality of diamine and dianhydride accounts for 12.7% of the total mass of the reaction system, P 2 o 5 Accounting for 86.5% of the total mass of polyphosphoric acid solution. The temperature was raised, and the reaction system was reacted at 175° C. for 5 hours, and at 220° C. for 5 hours to obtain a liquid crystal polyimide spinning solution. The solution is yellow and transparent, with an intrinsic viscosity of 2.05dL / g (concentrated sulfuric acid as a solvent, measured at 25°C).

[0039] The liquid crystal spinning stock solutio...

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Abstract

The invention relates to a preparation method of polyimide fibers containing symmetric bispyrimidine structures. The preparation method comprises steps as follows: 2,2'-(1,4-phenylene)bis(5-(4-aminophenyl)) pyrimidine and anhydrous stannous chloride are added to polyphosphoric acid, aromatic dianhydride monomers and P2O5 are sequentially added, the mixture reacts at the temperature of 170-200 DEG C for 4-6 h, then, the mixture is heated to 200-240 DEG C and reacts for 3-6 h, and a liquid crystal type polyimide spinning solution is obtained; a twin-screw extruder is adopted, and polyimide nascent fibers are obtained from the liquid crystal type polyimide spinning solution through spinning, multi-coagulation bath forming, water washing and winding; three-level hot drafting is performed on the polyimide nascent fibers under the protection of nitrogen after the polyimide nascent fibers are dried, and the polyimide fibers are obtained. The polyimide fibers prepared with the method have excellent mechanical performance and have wide application prospect, and the synthesis and processing problems that conventional phenol and phenyl polyhalide type solvents have high toxicity, aprotic solvents are difficult to remove with a two-step processing method and the like are solved.

Description

technical field [0001] The invention belongs to the field of polyimide fiber preparation, in particular to a preparation method of polyimide fiber containing symmetrical bipyrimidine structure. Background technique [0002] As a variety of high-performance fibers, polyimide fiber has high theoretical strength and modulus, and has many advantages such as high temperature resistance, solvent resistance, chemical stability, and radiation resistance. It is considered to be the polymer with the best comprehensive performance. It has been widely used in high-tech fields such as aviation, aerospace, and microelectronics. The structure of polyimide fibers is highly controllable, and polyimide fibers with different shapes and properties can be obtained by adjusting the structure and type of monomers. High-performance polyimide fibers usually have a rigid chemical structure, a high degree of order in the aggregate structure, and generally have high heat resistance, and their glass tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74D01D5/06D01D4/02D01D5/12D01D10/02D01D10/06C08G73/10
CPCC08G73/1032C08G73/106C08G73/1064C08G73/1067C08G73/1071D01D4/02D01D5/06D01D5/12D01D10/02D01D10/06D01F6/74
Inventor 张清华甘锋吴婷婷方玉婷赵昕董杰
Owner DONGHUA UNIV
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