Method for preparing carbon fiber precursor

A carbon fiber precursor and spinning dope technology, which is applied in the fields of fiber chemical characteristics, wet spinning, stretch spinning, etc., can solve the problems of uneven performance of spinning solution, low strength of carbon fiber precursor, and unstable performance. Achieve the effect of continuous stability, good uniformity and high uniformity in the spinning process

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is that the performance of the spinning solution in the existing spinning solution delivery technology is not uniform, which is not conducive to the continuous and stable spinning process, so that the strength of the carbon fiber precursor obtained by spinning is low and the performance is unstable. problem, provide a method for preparing carbon fiber precursor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The preparation method of carbon fiber precursor includes the following steps: 1. Preparation of stock solution: distilled acrylonitrile (AN) and itaconic acid (IA) in a ratio of 97:3, solid content 20wt%, azobisisobutyronitrile ( AIBN) occupies 0.4wt% of the comonomer, added to the reactor with dimethyl sulfoxide (DMSO) as the solvent, and reacted for 20 hours at a constant temperature of 60°C under the protection of nitrogen to obtain a binary acrylonitrile copolymer. 物 Spinning solution. Then the spinning solution is decompressed to remove residual monomers and bubbles to obtain a high-performance polyacrylonitrile copolymer spinning dope. After testing, the molecular weight is 10,300.

[0016] 2. Preparation of raw silk: the spinning dope is measured by a metering pump, filtered by 5μm and 3μm, and mixed with a static mixer with a jacketed insulation with a diameter of DN20 and a length-to-diameter ratio of 15 and then extruded through a spinneret Then enter the first...

Embodiment 2

[0020] The preparation method of carbon fiber precursor includes the following steps:

[0021] 1. Stock solution preparation: the steps are in accordance with Example 1;

[0022] 2. Spinning: The spinning dope is measured by a metering pump, filtered by 5μm and 2μm, and mixed with a static mixer with a jacketed insulation with a diameter of DN30 and an aspect ratio of 25, and then extruded through the spinneret Enter the first coagulation bath, the temperature of the coagulation bath is 55℃, the concentration is 65%, the draft ratio is -20%, the second coagulation bath is 60℃, the concentration is 40%, the draft ratio is 100%, and the third The coagulation bath is 60°C, the concentration is 20%, the draft ratio is 105%, and the nascent fiber is obtained; after the nascent fiber is coagulated in 3 passes, it is drawn with hot water for 3 passes. The drawing temperature of the 3 hot water is 70°C, At 80°C and 90°C, the draw ratios are 1.2, 1.4 and 2. After 3 hot-water drafting, the...

Embodiment 3

[0026] The preparation method of carbon fiber precursor includes the following steps:

[0027] 1. Preparation of stock solution: Distilled acrylonitrile (AN) and itaconic acid (IA) in a ratio of 99:1, solid content 26wt%, azobisisobutyronitrile (AIBN) accounts for 0.6wt% of the comonomer, Using dimethyl sulfoxide (DMSO) as a solvent was added to the reactor, and under the protection of nitrogen, the reaction was carried out at a constant temperature of 60° C. for 20 hours to obtain a binary acrylonitrile copolymer spinning solution. Then the spinning solution is decompressed to remove residual monomers and bubbles to obtain a high-performance polyacrylonitrile copolymer spinning dope. After testing, the molecular weight is 94600.

[0028] 2. Spinning: Spinning: The spinning dope is measured by a metering pump, filtered by 5μm and 2μm, and mixed with a static mixer with a jacketed insulation with a diameter of DN50 and a length-to-diameter ratio of 20, and then passes through the s...

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Abstract

The invention relates to a method for preparing a carbon fiber precursor, and mainly aims at solving the problems in the prior art that the carbon fiber precursor obtaining by spinning is low in strength and unstable in property caused by poor radial uniformity of properties of a spinning solution due to different radial temperatures in the transportation process. Through the technical scheme that the method for preparing the carbon fiber precursor comprises the following steps: polymerizing a first monomer acrylonitrile, a second monomer itaconic acid through the initiation of an initiator azodiisobutyronitrile in solvent dimethyl sulfoxide to obtain the spinning solution; carrying out vacuum removal on residual gas and bubbles in the spinning solution, and then filtering and mixing to obtain a high-property polyacrylonitrile copolymer spinning solution; and carrying out solidifying, drafting, washing, oiling, compacting by drying, steam drafting and steam heat setting on the spinning solution, and then rolling to obtain the carbon fiber precursor with high strength and stable performance, the problems are relatively well solved, and the method can be applied to industrial production of carbon fibers.

Description

Technical field [0001] The invention relates to a method for preparing carbon fiber precursor. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber is a new type of material that has developed rapidly in the 1960s. It has light weight, high specific strength, high specific modulus, high temperature resistance, corrosion resistance, wear resistance, fatigue resistance, and electrical conductivity. It has excellent properties such as heat conduction, and has been widely used in military industries such as satellites, launch vehicles, tactical missiles, and spacecraft, and has become an indispensable material in the aerospace industry. Excellent carbon fiber precursors should have the characteristics of high heat resistance, less pore structure, less surface defects, dense structure, and good stretchability. [0003] In industrial production, the ability to continuously and stably produce carbon fiber with stable performance is an important issue that the majorit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/38D01F11/06D01F9/22D01D5/06D01D5/14C08F220/46C08F222/02
Inventor 史纪友李磊沈志刚屠晓萍王贺团
Owner CHINA PETROLEUM & CHEM CORP
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