Preparation method of polyacrylonitrile-based carbon fiber precursor

A polyacrylonitrile-based carbon fiber, polyacrylonitrile spinning technology, applied in the direction of fiber chemical characteristics, single-component synthetic polymer rayon, textiles and papermaking, etc., can solve the problems affecting spinning stability, fiber interference, dry and wet Solve problems such as process overflow and improve the performance and quality stability of raw silk

Active Publication Date: 2014-10-08
GUANGZHOU KINGFA CARBON FIBER NEW MATERIALS DEV +1
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  • Application Information

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Problems solved by technology

[0005] Patent JP55-097199 proposes a method of changing the atmosphere in the dry section of the dry-wet process. The problem with this method is that the air flow will interfere with the fibers in the dry section. For spinning solutions with low viscosity, it will affect the stability of spinning nature, and also does not solve the problem of roaming
[0006] To sum up, the existing polyacrylonitrile-based carbon fiber precursor production process has the following disadvantages: 1. The spinning produced by the dry-wet method has a dense surface structure, which reduces the spinning performance; 2. The dry-wet process will occur Parallel phenomenon; 3. There is a problem of overflow in the dry-wet process that introduces the atmosphere in the dry section
4. The dry and wet process cannot form the groove surface like the raw silk of the wet process

Method used

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  • Preparation method of polyacrylonitrile-based carbon fiber precursor
  • Preparation method of polyacrylonitrile-based carbon fiber precursor
  • Preparation method of polyacrylonitrile-based carbon fiber precursor

Examples

Experimental program
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Effect test

Embodiment 1

[0031] This embodiment adopts 3-stage gradient coagulation, and the first-stage coagulation bath is as image 3 As shown, wherein the non-coagulating bath is simethicone oil with a viscosity of 10 cP.s, the coagulating bath is a 65% DMSO (dimethyl sulfoxide) aqueous solution, and the temperature is 45° C. The spinning dope is a DMSO solution of an acrylonitrile-itaconic acid binary copolymer, and the molar ratio of itaconic acid units to acrylonitrile units in the copolymer is 0.45:100. Use a transparent cylinder to isolate the non-coagulation bath from the coagulation bath (the components of the non-coagulation bath and the coagulation bath are immiscible with each other, the mutual solubility is very small, and their influence can be almost ignored, so there is no need to physically separate the two in the up and down direction open), cylinder length 50cm. The hole diameter of the spinneret is 0.1mm. After the wire drawing is successful, slowly add simethicone oil into the ...

Embodiment 2

[0038] In this embodiment, n-heptane is used as the non-coagulation bath, and the rest of the parts not mentioned are the same as in Embodiment 1.

[0039] After carbonization, the linear density is 0.066, the bulk density is 1.801, the tensile strength is 6.4GPa, the modulus is 265GPa, and the elongation at break is 2.3%.

[0040] The following is to compare the wet spinning process with the combined coagulation molding process of the present invention:

[0041] The hole diameter of the spinneret is 0.055mm, the three-stage gradient coagulation, the first-stage coagulation bath draft is 0.97, and the spinning speed is 150m / min. All the other unmentioned parts are the same as in Embodiment 1.

[0042] The SEM characterization of the obtained precursor surface is as follows: Figure 6a and Figure 6b shown. After carbonization, the linear density is 0.063, the bulk density is 1.786, the tensile strength is 4.9GPa, the modulus is 268GPa, and the elongation at break is 2.0%. ...

Embodiment 3

[0045] The spinning stock solution is a DMSO solution of acrylonitrile-itaconic acid-methyl acrylate terpolymer, the molar ratio of itaconic acid unit to acrylonitrile unit in the copolymer is 0.45:100, and the molar ratio of methyl acrylate unit to acrylonitrile unit The ratio is 0.55:100. Others are the same as embodiment one.

[0046] The linear density of the obtained precursor after carbonization is 0.066, the bulk density is 1.805, the tensile strength is 5.5GPa, the modulus is 275GPa, and the elongation at break is 2.1%.

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Abstract

The invention relates to a preparation method of a polyacrylonitrile-based carbon fiber precursor; after filament-out of a polyacrylonitrile spinning solution, the polyacrylonitrile spinning solution enters into a stage of non solidification bath, and then enters into a composite solidification molding process of a solidification bath. The preparation method specifically includes the following steps: after solidification molding of the polyacrylonitrile spinning solution by the composite solidification molding process, successive drafting, water washing, oiling, drying, steam drafting or boiling water drafting, heat setting, drying, and filament collection. The preparation method can overcome the shortcomings of a traditional wet and dry process and wet process, and is conducive to the control of raw filament cortex structure. By use of the process, a spinning speed more than 300m / min can be achieved, the obtained raw filament has a surface groove structure similar with that of a wet-method raw filament, is soft in hand feeling and good in splitting property, and the carbonized strength is higher than 5.8GPa. The preparation method belongs to the technical field of preparation methods of the polyacrylonitrile-based carbon fiber precursor.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of polyacrylonitrile-based carbon fiber precursors, and in particular relates to a method for preparing high-performance carbon fiber precursors by using a non-coagulation bath and a coagulation bath combined coagulation molding process. Background technique [0002] At present, polyacrylonitrile (PAN)-based carbon fiber precursors mainly adopt two processes: wet process and dry-wet process. Because in the dry-wet process, the spinning dope flows out of the spinneret holes and passes through an air layer before entering the coagulation bath, the Burroughs effect of the dope trickle can be alleviated or even eliminated. In the wet process, the solidification process will occur from the surface to the inside when the fine stream of the stock solution flows out of the spinneret hole during the extrusion expansion stage. The higher the tension is, the more obvious it is, and the tension o...

Claims

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Application Information

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IPC IPC(8): D01F6/38D01F6/18D01F9/22
Inventor 辛伟黄险波马雷蔡华伦陈大华
Owner GUANGZHOU KINGFA CARBON FIBER NEW MATERIALS DEV
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