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Method for improving polyimide-based carbon fiber microstructure

A polyimide-based carbon fiber, polyimide fiber technology, applied in the field of carbon fiber, can solve the problems of increased production cost, increased production time, fiber defects, etc., and achieves low cost, reduced adverse effects, and high carbon content. Effect

Active Publication Date: 2016-01-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

During the pre-oxidation process, due to the entry of oxygen atoms and the escape of non-carbon atoms, holes will be generated, resulting in defects inside the fiber
The existence of the pre-oxidation process of PAN-based carbon fibers increases the production time and production cost. Therefore, it is imperative to seek new carbon fiber precursor materials that do not require pre-oxidation treatment.

Method used

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  • Method for improving polyimide-based carbon fiber microstructure
  • Method for improving polyimide-based carbon fiber microstructure
  • Method for improving polyimide-based carbon fiber microstructure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A: BPDA and ODA were mechanically stirred in DMAc at low temperature for a certain period of time to obtain a BPDA / ODA polyamic acid solution.

[0035]B: The polyamic acid fiber is prepared by wet spinning process, and the temperature of the polyamic acid fiber is raised gradually, and the thermal imidization treatment is carried out to obtain the polyimide fiber;

[0036] C: Fix the raw silk in a vacuum tube furnace, set a gradient temperature rise program, heat from room temperature to 1500°C at a heating rate of 10°C / min and keep it at this temperature for 70 minutes, and pass through nitrogen protection, and the flow rate is 300-400ml / min, carry out carbonization treatment, and cool naturally after the end to obtain polyimide-based carbon fibers.

Embodiment 2

[0038] A: BPDA, ODA and p-PDA are mechanically stirred in DMAc at low temperature for a certain period of time to obtain BPDA / ODA / p-PDA30% (the percentage represents the mole percentage of p-PDA monomer in diamine) Copolymerized polyamic acid solution.

[0039] B: The polyamic acid fiber is prepared by wet spinning process, and the temperature of the polyamic acid fiber is raised gradually, and the thermal imidization treatment is carried out to obtain the polyimide fiber;

[0040] C: Fix the raw silk in a vacuum tube furnace, set a gradient temperature rise program, heat from room temperature to 1500°C at a heating rate of 10°C / min and keep it at this temperature for 70 minutes, and pass through nitrogen protection, and the flow rate is 300-400ml / min, carry out carbonization treatment, and cool naturally after the end to obtain polyimide-based carbon fibers.

Embodiment 3

[0042] A: BPDA, ODA and p-PDA were mechanically stirred in DMAc at low temperature for a certain period of time to prepare a 50% BPDA / ODA / p-PDA copolymerized polyamic acid solution.

[0043] B: The polyamic acid fiber is prepared by wet spinning process, and the temperature of the polyamic acid fiber is raised gradually, and the thermal imidization treatment is carried out to obtain the polyimide fiber;

[0044] C: Fix the raw silk in a vacuum tube furnace, set a gradient temperature rise program, heat from room temperature to 1500°C at a heating rate of 10°C / min and keep it at this temperature for 70 minutes, and pass through nitrogen protection, and the flow rate is 300-400ml / min, carry out carbonization treatment, and cool naturally after the end to obtain polyimide-based carbon fibers.

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Abstract

The invention discloses a method for improving a polyimide-based carbon fiber microstructure and belongs to the technical field of carbon fibers. The method comprises that BPDA, p-PDA and ODA monomers are synthesized into polyamic acid solutions with different molecular chain plane regularities, through a wet spinning technology and gradient heating heat amidation, polyimide fibers are prepared from the polyamic acid solutions, the polyimide fibers are fixed into a vacuum tube furnace and are heated for carbonization to a temperature of 1500 DEG C in a N2 protective atmosphere, and then the carbonization product is naturally cooled so that the polyimide-based carbon fibers are obtained. The polyimide fiber chemical structure has high plane regularity. The polyimide-based carbon fiber has a perfect microstructure. The invention provides the method for improving a polyimide-based carbon fiber structure. The prepared polyimide-based carbon fiber retains polyimide base fiber morphology characteristics, and has good compactness, less defects, high carbon content and conductive characteristics.

Description

technical field [0001] The invention relates to carbon fiber and a manufacturing method thereof, belonging to the technical field of carbon fiber. In particular, it relates to a polyimide-based carbon fiber with a perfect microstructure prepared by using polyimide fibers with different planar regularities as precursors. Background technique [0002] Carbon fiber refers to the fiber material in which the mass fraction of carbon element accounts for more than 90% in the chemical composition. The preparation of carbon fiber is a complex process, including the selection of precursors and fiber formation, pre-oxidation, carbonization and other links. At present, carbon fiber can usually be polyacrylonitrile fiber (PAN fiber), pitch fiber, viscose fiber or wood It is made by oxidation, low-temperature carbonization, and high-temperature carbonization of plain fibers. Among them, the carbon fiber made from PAN fiber has developed rapidly because the production process is simpler ...

Claims

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Application Information

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IPC IPC(8): D01F9/24D01F6/74D01D1/02D01D5/06C08G73/10
Inventor 武德珍曹丽牛鸿庆张梦颖何敏
Owner BEIJING UNIV OF CHEM TECH
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