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Preparation method of polyimide profiled fiber

A special-shaped fiber and polyimide technology, which is applied in fiber processing, fiber chemical characteristics, dry spinning, etc., can solve problems such as cost increase, lack of description of fiber irregularity, and fiber performance degradation, and achieve high production efficiency. Good thermal dimensional stability and convenient solvent volatilization

Inactive Publication Date: 2011-12-14
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polyimide profiled fiber has a more obvious effect on efficiently blocking or filtering high temperature, acid dust and other substances. US Patent US4801502 uses a one-step method to directly spin polyimide solution into profiled fiber, but in order to solve the solubility of the polymer , using ketone anhydride and diisocyanate as monomers, not only the cost is greatly increased, the performance of the fiber is reduced, but also the description of controlling the degree of fiber shape is lacking

Method used

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  • Preparation method of polyimide profiled fiber
  • Preparation method of polyimide profiled fiber
  • Preparation method of polyimide profiled fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Put 10kg (49.938mol) of 4,4-diaminodiphenyl ether and 83kg of N,N-dimethylformamide into the polymerization kettle, stir at room temperature until it is completely dissolved, and pass the refrigerant to reduce the temperature of the solution to -5℃ , Then add 10.893kg (49.938mol) of pyromellitic anhydride and continue to pass the refrigerant. After 24h, a polyamic acid solution with a concentration of 20wt% is obtained. After the solution is degassed, spinning can be carried out. The cross-section of the spinning solution passing through the capillary is elliptical trilobal (center distance a is 0.03mm, leaf width b is 0.2mm, leaf length c is 0.12mm) ( figure 1 The spinneret of) enters the hot-air spinning tunnel, the spinning tunnel is 10m long, the hot-air temperature is 205°C, the winding speed is 100m / min, and the thin stream solidifies into fibers to obtain the nascent fiber with irregular cross-section. The nascent fiber enters a heating box for cyclization at a te...

Embodiment 2

[0039] Put 2.5kg (23.122kmol) of p-phenylenediamine, 2.5kg (23.122kmol) of m-phenylenediamine and 86.3kg of N,N-dimethylacetamide and N-methylpyrrolidone mixture into the polymerizer and stir To completely dissolve, let the temperature of the solution drop to -5°C through refrigerant, then add 16.566kg (46.244mol) of 3,3',4,4'-benzophenone sulfone tetracarboxylic dianhydride, continue to stir through the refrigerant, after 24h A polyamic acid solution with a concentration of 18 wt% is obtained, and spinning can be performed after the solution is defoamed. The cross section of the spinning solution passing through the capillary is elliptical four-leaf (center distance a is 0.05mm, leaf width b is 0.2mm, leaf length c is 0.12mm) (such as Figure 5 The spinneret of) enters the hot-air spinning tunnel, the spinning tunnel is 10m long, the hot-air temperature is 270℃, the winding speed is 400m / min, and the thin stream solidifies into fibers to obtain the irregular cross-sectional spu...

Embodiment 3

[0041] Put 4kg (19.976mol) of 4,4-diaminodiphenyl ether, 3.960kg (19.976mol) of 4,4-diaminodiphenylmethane and 83.4kg N,N-dimethylformamide into the polymerizer, Stir at room temperature until it is completely dissolved, pass the refrigerant to reduce the temperature of the solution to -5°C, then add 12.873kg (39.952mol) of 3,3,4,4-benzophenonetetracarboxylic dianhydride, 28h to obtain a concentration of 30wt% Polyamic acid solution. Spinning can be performed after the solution is defoamed. The cross section of the spinning solution passing through the capillary is elliptical five-lobed (center distance a is 0.08mm, leaf width b is 0.2mm, leaf length c is 0.12mm) (e.g. Image 6 The spinneret of) enters the hot-air spinning tunnel, the spinning tunnel is 12m long, the hot-air temperature is 210°C, the winding speed is 800m / min, and the thin stream solidifies into fibers to obtain nascent fibers with irregular cross-sections. The nascent fiber enters the hot box to complete the ...

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Abstract

The invention relates to a preparation method of polyimide profiled fibers. The method comprises the following steps of: (1) preparing a polyamic acid solution; (2) forming by dry spinning; and (3) performing cyclization on the as-spun fibers. The dry spinning process is adopted to prepare polyimide profiled fibers, which has high production efficiency, simple procedures and strong operability, makes solvent volatilization more convenient and can achieve the effect of controlling the degree of profile of polyimide fibers. The prepared polyimide profiled fibers have good mechanical properties and high specific surface areas, maintain good dimensional stability at a high temperature, and can be widely applied to reinforcing fibers of composite materials, protective clothing against high-level radiation and other severe conditions, filtering materials used in high temperature mining conditions and so on.

Description

Technical field [0001] The invention belongs to the field of preparation of polyimide fibers, and particularly relates to a preparation method of polyimide shaped fibers. Background technique [0002] As a high-tech fiber, polyimide fiber material has good chemical stability, excellent thermomechanical properties and outstanding radiation resistance, and has become a hot spot for industrial development. Considering that polyimide is difficult to melt, polyimide fibers can only be prepared by dry or wet methods (dry and wet methods) in general. The research on the wet spinning process of polyimide fiber has been carried out for many years. It can be divided into two routes: one-step method and two-step method. The two-step route refers to the use of polyamic acid as the spinning solution for wet spinning, and the polyimide fiber is obtained after cyclizing the prepared polyamic acid fiber. Its representative patents are Japanese Patent Publication JP3287315 , JP4018115. One-ste...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74D01F6/78D01D5/04D01D5/253C08G73/10
Inventor 张清华徐圆许千赵陈嘉夏清明陈大俊
Owner DONGHUA UNIV
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