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Preparation method of viscosity-controllable polyamide acid solution

A technology of polyamic acid and solution, which is applied in the direction of spinning solution preparation, rayon manufacturing, single-component synthetic polymer rayon, etc., can solve the problems of unstable viscosity control, high molecular weight, high viscosity, etc., and achieve improvement. spinning effect

Inactive Publication Date: 2016-04-27
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] The invention relates to a method for preparing a polyamic acid spinning stock solution with controllable viscosity for preparing polyimide fibers, which mainly solves the problem of polyamic acid solution in the prior art when two-step methods are used to prepare polyimide fibers. During the preparation process, the viscosity control is unstable, the molecular weight is too high, the viscosity is too high, and the spinnability is poor

Method used

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  • Preparation method of viscosity-controllable polyamide acid solution
  • Preparation method of viscosity-controllable polyamide acid solution
  • Preparation method of viscosity-controllable polyamide acid solution

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Effect test

Embodiment 1

[0029] Proportion p-phenylenediamine and 3,3′,4,4′-biphenyltetraacid dianhydride in a total molar ratio of 1:0.99, and 10.0807g (0.1mol) of p-phenylenediamine and 203.3gN, Add N-dimethylacetamide and 22.3g of 1-methyl-2-pyrrolidone into a four-necked flask (water content 410ppm), stir at room temperature and under the protection of N2, after completely dissolving, cool in an ice-water bath to 0°C, Add 29.1080 g (0.099 mol) of 3,3′,4,4′-biphenyltetraacid dianhydride powder at 250 rpm, and continue stirring for 0.5 hour to obtain the desired polyamic acid solution with a solid content of 14.8%. The solution was tested by filtration without gel generation, the apparent viscosity of the solution was 108 Pa·s at 25°C, and the intrinsic viscosity was 1.43dL / g at 25°C.

Embodiment 2

[0031] Proportion p-phenylenediamine and 3,3′,4,4′-biphenyltetraacid dianhydride in a total molar ratio of 1:1.01, mix 10.0807g (0.1mol) of p-phenylenediamine and 275.4gN, Add N-dimethylacetamide and 82.6g 1-methyl-2-pyrrolidone into a four-neck flask (water content 410ppm), stir at room temperature and 2 Under protection, after completely dissolving, cool in an ice-water bath to 10°C, add 29.6940g (0.101mol) of 3,3′,4,4′-biphenyltetraacid dianhydride powder at a stirring speed of 250 rpm, and continue stirring After 1.5 hours, the desired polyamic acid solution with a solid content of 10% was obtained. The solution was tested by filtration without gel formation, the apparent viscosity of the solution was 90 Pa·S at 25°C, and the intrinsic viscosity was 1.19 dL / g at 25°C.

Embodiment 3

[0033] Proportion p-phenylenediamine and 3,3′,4,4′-biphenyltetraacid dianhydride in a total molar ratio of 1:1, mix 10.0807g (0.1mol) of p-phenylenediamine and 112.8gN, Add N-dimethylacetamide and 5.6g 1-methyl-2-pyrrolidone into a four-neck flask (water content 410ppm), stir at room temperature and 2 Under protection, after complete dissolution, adjust the temperature to 35°C, add 29.400g (0.1mol) 3,3′,4,4′-biphenyltetraacid dianhydride powder at a stirring speed of 250 rpm, and continue stirring for 5 hours, the desired polyamic acid solution with a solid content of 25% was obtained. No gel was produced in the solution after filtration test, the apparent viscosity of the solution was 233 Pa·S at 25°C, and the intrinsic viscosity was 1.98dL / g at 25°C.

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Abstract

The invention relates to a preparation method of a viscosity-controllable polyamide acid solution for preparation of polyimide fibers. The preparation method mainly solves the problem that in the two-step polyimide fiber preparation method, a polyamide acid solution has unstable viscosity, overtop molecular weight, overtop viscosity and poor spinnability in preparation. The preparation method comprises that diamine as a polymerization raw material, a solvent and a conditioning agent are added into a reactor and are dissolved in a protective atmosphere of gas inert to the reaction substances, tetracarboxylic dianhydride is added into the solution at a temperature of -10 to 40 DEG C, the mixture undergoes a reaction for 2-10h and the reaction product is defoamed so that a polyamide acid spinning stock solution is obtained. The preparation method well solves the above problem and can be used for polyimide fiber industrial production.

Description

technical field [0001] The invention relates to a method for preparing polyamic acid spinning solution with controllable viscosity for preparing polyimide fibers. Background technique [0002] Polyimide fiber mainly refers to high-performance fibers spun from polyamic acid or polyimide solution. Its excellent heat resistance, dielectric properties, low temperature resistance, mechanical properties, and radiation resistance make it It can be widely used in aerospace, electrical insulation, atomic energy industry, national defense construction, environmental industry, protection industry, medical and health and other fields with very harsh conditions, especially in some high-tech fields. Its superior characteristics make it one of the most promising high-tech fibers. [0003] Polyimide fibers can be prepared by a two-step method through polyamic acid or a one-step method through polyimide, so the polymerization process includes the polymerization of polyamic acid and the poly...

Claims

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Application Information

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IPC IPC(8): D01F6/94D01F1/10D01D1/02C08G73/10
Inventor 崔晶黄森彪周文乐
Owner CHINA PETROLEUM & CHEM CORP
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