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Method for preparing polyimide fibers

A polyimide fiber and polyamic acid spinning technology, which is applied in fiber treatment, fiber chemical characteristics, wet spinning, etc., can solve the problem of affecting the storage and performance of polyamic acid fiber and the low performance of polyimide fiber , unfavorable continuous production and other issues, to achieve the effect of high imidization degree and high orientation degree, simple synthesis method, and conducive to large-scale production

Active Publication Date: 2011-08-31
JIANGSU XIANNUO NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage is that the performance of the polyamic acid fiber obtained in the first step will decrease with the prolongation of storage time, and after the polyamic acid fiber is wound up, a small amount of solvent and coagulation liquid remaining in the fiber are difficult to volatilize, which will also affect the polyamic acid fiber. The storage and performance of the amic acid fiber, so the performance of the obtained polyimide fiber is not high; at the same time, this method is carried out step by step, which is not conducive to continuous production

Method used

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  • Method for preparing polyimide fibers
  • Method for preparing polyimide fibers
  • Method for preparing polyimide fibers

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Synthesis of polyamic acid solution: according to the molar ratio of PMDA: ODA = 1.05: 1, the ODA monomer is first placed in a three-necked flask, and a metered amount of solvent dimethylformamide (DMF) is added, and stirred under nitrogen protection. ODA was completely dissolved, then PMDA was added in batches and stirred to make the solid content 10%, and then stirred at 50° C. for 5 hours to obtain a viscous polyamic acid solution.

[0032] Preparation of polyimide fiber: filter the polyamic acid solution and move it into the storage tank (1), vacuum degassing, and then spinning by wet process. The polyamic acid solution is pumped out by the metering pump (2) and sprayed out through the spinneret (3), and the obtained polyamic acid fiber is drawn by the godet roller (4) and enters the coagulation bath (5) for solidification, and then passes through the godet roller After traction, it enters the cleaning bath (6) for washing. Both the coagulation bath and the cleaning...

Embodiment 2

[0034] Synthesis of polyamic acid solution: according to the molar ratio of PMDA:ODA=0.95:1, the ODA monomer is first placed in a three-necked flask, and the metered solvent dimethylacetamide (DMAc) is added, stirred under nitrogen protection to make ODA was completely dissolved, then PMDA was added in batches and stirred to make the solid content 20%, and stirred at 0°C for 2 hours to obtain a viscous polyamic acid solution.

[0035] Preparation of polyimide fiber: filter the polyamic acid solution and move it into the storage tank (1), vacuum degassing, and then spinning by wet process. The polyamic acid solution is pumped out by the metering pump (2) and sprayed out through the spinneret (3), and the obtained polyimide fiber is drawn by the godet roller (4) and enters the coagulation bath (5) for solidification, and the coagulation bath consists of The mixed solution of water and ethanol is dried by the hot plate (8), and then enters into four furnace sections composed of t...

Embodiment 3

[0037] Synthesis of polyamic acid solution: according to the molar ratio of PMDA: ODA = 1.05: 1, the ODA monomer is placed in a three-necked flask first, and the metered solvent dimethylacetamide (DMAc) is added, and stirred under nitrogen protection. ODA was completely dissolved, then PMDA was added in batches and stirred to make the solid content 25%, stirred at 0°C for 2 hours, and then stirred at 40°C for 10 hours to obtain a viscous polyamic acid solution.

[0038]Preparation of polyimide fiber: filter the polyamic acid solution and move it into the storage tank (1), vacuum degassing, and then spinning by wet process. The polyamic acid solution is pumped out by the metering pump (2) and sprayed out through the spinneret (3), and the obtained polyimide fiber is drawn by the godet roller (4) and enters the coagulation bath (5) for solidification, and then passes through the wire guide After being pulled by the roller, it enters the cleaning bath (6) for washing. The coagula...

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Abstract

The invention discloses a method for preparing polyimide fibers, and belongs to the technical field of the polyimide fibers. The method is characterized in that: polyamide acidic solution is subjected to spinning by adopting a wet spinning or dry wet spinning process, and fibers are subjected to processes of coagulating and drying or processes of washing, drying, heat treatment cyclizing and stretching continuously and are rolled finally to form the polyimide fibers. The method comprises the following specific steps of: reacting diamine with dianhydride in solvent under the protection of nitrogen to obtain polyamide acidic spinning solution; filtering the spinning solution, pouring the filtered spinning solution into a storage tank for defoaming, spinning according to the wet spinning or dry wet spinning process, pumping the spinning solution by a metering pump, and spraying from a spinneret plate; dragging by a silk guide roller, coagulating in coagulating bath, drying directly by a hot roller or a hot plate or drying by the hot roller or the hot plate after washing, and performing heat cyclizing and stretching by three sections or more than three sections of furnace sections; and finally, rolling silk. In the method, the integral process is continuous, smooth, compact and short in time, high imidization degree and degree of orientation are realized, and the high-performance fibers are obtained.

Description

technical field [0001] The invention belongs to the technical field of polyimide fibers, and in particular relates to a method for continuously preparing high-performance polyimide fibers in one step from a polyamic acid solution. Background technique [0002] As a variety of high-performance fibers, polyimide fibers have many excellent properties such as high strength and high modulus, high temperature resistance, low temperature resistance, radiation resistance, flame retardancy, and chemical corrosion resistance, and also have good biocompatibility and dielectric properties. performance. It is expected to be widely used in the fields of atomic energy industry, space environment, rescue needs, aerospace, national defense construction, new construction, high-speed transportation, marine development, sports equipment, new energy, environmental industry and protective equipment. [0003] There are currently two methods for preparing polyimide fibers. One is a one-step techn...

Claims

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Application Information

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IPC IPC(8): D01D5/00D01D5/06D01D1/10D01D10/02D01D10/06D01F6/74
CPCD01F6/74D02J1/222
Inventor 武德珍牛鸿庆齐胜利韩恩林闫晓娜赵昕吴战鹏
Owner JIANGSU XIANNUO NEW MATERIAL TECH
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