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Polyimide fiber and preparation method thereof

A polyimide fiber, polyimide technology, which is applied in the chemical characteristics of fibers, spinning solution preparation, dry spinning, etc., can solve the problems of easy sticking of filaments, large solvent residues, and high solvent toxicity. , to achieve the effect of accelerating the cyclization rate, shortening the reaction time, and avoiding side reactions

Inactive Publication Date: 2009-09-09
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One is to synthesize polyimide solution first, and then directly spin it into polyimide fiber. The disadvantage is that it needs to use phenolic solvent, which is highly toxic and has a large amount of residue in the fiber.
In the above technology, because the polyamic acid is easy to decompose, and it is difficult to solidify during solidification and spinning, the residual amount of solvent is large, and the filaments are easy to stick to the roller; at the same time, some side reactions and hydrolysis are easy to occur in the imide process. , therefore, the fiber strength is limited to some extent

Method used

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  • Polyimide fiber and preparation method thereof
  • Polyimide fiber and preparation method thereof
  • Polyimide fiber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A kind of partially cyclized polyamic acid fiber is prepared, and the steps are as follows:

[0023] (1) Synthesis of ternary copolymerization polyamic acid solution

[0024] Under nitrogen protection, in a three-necked flask, diamine (a mixture of p-phenylenediamine and 4,4'-diaminodiphenyl ether in a molar ratio of 2:8) was added to N,N'-dimethylacetamide (total solid content is 10%) in the solvent, stir quickly to make it dissolve, control the reaction temperature at 0 ° C, after the diamine is completely dissolved, add pyromellitic anhydride to the flask every half hour, and add it in four times, The molar ratio of pyromellitic anhydride to diamine is 1:1.02, and the wall of the bottle is washed several times with an appropriate amount of acetamide, and after 3 to 4 hours of copolymerization reaction, a light yellow viscous ternary copolymerized polyamic acid (PAA) is obtained solution.

[0025] (2) Preparation of partially cyclized polyamic acid

[0026] Accordi...

Embodiment 2

[0043] According to embodiment 1 technical scheme step (1) synthesis ternary copolymerization polyamic acid solution.

[0044]The solution of acetic anhydride, triethylamine and acetamide is mixed, wherein, the molar ratio of triethylamine and acetic anhydride is 1: 1, and acetamide 3ml, is prepared into partial cyclizing agent, press acetic anhydride: diamine molar ratio is 0.7:1, add part of the cyclizing agent and diamine to the polyamic acid solution, and react for 2 to 4 hours to obtain a golden yellow partially cyclized polyamic acid prepolymer.

[0045] Partially cyclized polyamic acid fibers are made by dry-wet spinning according to the technical solution step (3) of Example 1.

[0046] The obtained partially cyclized polyamic acid (PAA) fibers were loosely wound and subjected to microwave treatment under vacuum conditions for 3, 6, 10 and 15 minutes, respectively, and prepared polyimide by dehydration and cyclization treatment. fiber.

[0047] The polyimide fiber pr...

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Abstract

The invention discloses a polyimide fiber and a preparation method thereof. Synthesizing polyamide acid with a ternary polymerization method destroys the regularity and the symmetry property of molecular chains, so that the crystallization tendency of the molecular chains is reduced and the spinning property of PAA solution is improved; and partial cyclization treatment limits the degradation of polyamide acid, and spinning serum is easy to solidify and form when entering into coagulation bath. The microwave method is adopted to treat polyamide acid fiber, the cyclization rate is accelerated, and the reaction time is shortened; and simultaneously, no any side reaction is aroused under the microwave radiation. The prepared polyimide nascent fiber has high strength and good thermal resistance.

Description

technical field [0001] The invention relates to a synthetic fiber and a preparation method thereof, in particular to a polyimide fiber and a preparation method thereof, belonging to the technical field of polymer materials. Background technique [0002] Polyimide (PI) fiber has been a variety of high-performance fibers for decades. It is a class of polymer materials containing imide rings in the main chain of the molecule. It has excellent mechanical and dielectric properties. , insulation, radiation resistance, corrosion resistance, high and low temperature resistance, etc., are high-performance fibers. Due to its outstanding characteristics in performance and preparation, whether it is used as a structural material or a functional material, its huge application prospects have been recognized by people. In particular, the radiation resistance and electrical insulation properties are better than other high-performance fibers, so it can be widely used in fire protection, ele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74C08G73/10D01D1/02D01D5/04D01D5/06
Inventor 戴礼兴陈亮
Owner SUZHOU UNIV
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