Preparation method for polyamide acid solution

A technology of polyamic acid solution, which is applied in the field of preparation of polyamic acid solution, can solve problems such as unstable viscosity control and spinning difficulties, and achieve the effects of controlling the molecular weight and viscosity of the system and improving spinnability

Active Publication Date: 2016-06-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that when the polyimide fiber is prepared by a two-step method in the prior art, the viscosity control of the polyamic acid solut

Method used

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  • Preparation method for polyamide acid solution
  • Preparation method for polyamide acid solution
  • Preparation method for polyamide acid solution

Examples

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Embodiment 1

[0032] The p-phenylenediamine and 3,3',4,4'-bipyromellitic dianhydride are proportioned at a total molar ratio of 1:0.99, 10.0807g (0.1mol) of p-phenylenediamine and 225.6gN, Add N-dimethylacetamide into a four-necked flask (water content 410ppm), stir at room temperature and 2 Under protection, after complete dissolution, cool to 0℃ in an ice-water bath, slowly add 28.8120g (0.098mol) 3,3′,4,4′-bipyromellitic dianhydride powder, the feeding time is 20 minutes, and the stirring speed is After continuing the reaction at 200 rpm for 30 minutes, add 0.296 g (0.001 mol) of 3,3′,4,4′-bipyromellitic dianhydride powder to the above solution system and continue stirring for 0.5 hours to obtain a solid content of 14.8% of the desired polyamic acid solution. The solution was tested by filtration and no gel was produced. The apparent viscosity of the solution was 116 Pa·S at 25°C, and the intrinsic viscosity was 1.40 dL / g at 25°C.

Embodiment 2

[0034] The p-phenylenediamine and 3,3',4,4'-bipyromellitic dianhydride are proportioned at a total molar ratio of 1:1.01, and 10.0807g (0.1mol) of p-phenylenediamine and 358.0gN, Add N-dimethylformamide into a four-necked flask (water content 410ppm), stir at room temperature and 2 Under protection, after dissolving completely, cool to 10℃ in ice-water bath, slowly add 27.9300g (0.095mol) 3,3′,4,4′-bipyromellitic dianhydride powder, the feeding time is 30 minutes, and the stirring speed is After continuing the reaction for 45 minutes at 250 rpm, 1.764 g (0.006 mol) of 3,3′,4,4′-bipyromellitic dianhydride powder was added to the above solution system, and stirring was continued for 1.5 hours to obtain a solid content of 10% of the desired polyamic acid solution. The solution was tested by filtration and no gel was produced. The apparent viscosity of the solution was 80 Pa·S at 25°C, and the intrinsic viscosity was 1.15 dL / g at 25°C.

Embodiment 3

[0036] The p-phenylenediamine and 3,3',4,4'-bipyromellitic dianhydride are proportioned at a total molar ratio of 1:1, and 10.0807g (0.1mol) of p-phenylenediamine and 118.4gN, Add N-dimethylacetamide into a four-necked flask (water content 410ppm), stir at room temperature and 2 Under protection, after complete dissolution, slowly add 28.224g (0.096mol) 3,3′,4,4′-bipyromellitic dianhydride powder at 35°C, the feeding time is 60 minutes, and the stirring speed is 250 rpm. After the reaction continued for 120 minutes in minutes, 1.176g (0.004mol) of 3,3′,4,4′-bipyromellitic dianhydride powder was added to the above solution system, and stirring was continued for 5 hours to obtain a solid content of 25% The required polyamic acid solution. The solution was tested by filtration and no gel was produced. The apparent viscosity of the solution was 212 Pa·S at 25°C, and the intrinsic viscosity was 2.03dL / g at 25°C.

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Abstract

The invention relates to a preparation method for a polyamide acid solution for preparing polyimide fibers, and is used for mainly solving the problems in the prior art that when a two-step method is adopted for preparing polyimide fibers, the polyamide acid solution has unstable viscosity control and too large viscosity in the preparation process to cause spinning difficulty. The problems are relatively well solved by adopting the technical schemes that the preparation method comprises the following steps: a) proportioning diamine and tetracarboxylic dianhydride according to the total molar ratio of 1 to X; b) under the protection of an inert gas, stirring diamine at low temperature to be completely dissolved in an organic solvent; and c) slowly adding tetracarboxylic dianhydride with the Y quantity ratio to the solution with the feeding time of 20-60 minutes, after the feeding is finished, continuing to carry out a reaction for 30-120 minutes, adding tetracarboxylic dianhydride with the Z quantity ratio to the reaction system, continuing to carry out a reaction for 0.5-10 hours, and thus obtaining the polyamic acid solution which can be used for industrial production of polyimide materials.

Description

Technical field [0001] The invention relates to a preparation method of a polyamic acid solution for preparing polyimide fibers, in particular to a preparation method of a polyamic acid solution with controllable viscosity. Background technique [0002] Polyimide fiber mainly refers to the high-performance fiber spun from polyamic acid or polyimide solution. Its excellent heat resistance, dielectric properties, low temperature resistance, mechanical properties, and radiation resistance make 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-end fields. Its superior characteristics make it one of the most promising high-tech fibers. [0003] The polyimide fiber can be made by a two-step method by polyamic acid or by a one-step method by polyimide, so its polymerization process includes pol...

Claims

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Application Information

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IPC IPC(8): C08G73/10D01F6/74
Inventor 崔晶黄森彪周文乐
Owner CHINA PETROLEUM & CHEM CORP
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