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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 low strength of carbon fiber precursor, uneven performance of spinning solution, and unstable performance. Achieve good uniformity, continuous and stable spinning process, and high uniformity

Active Publication Date: 2017-05-10
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, comprises the following steps: 1, stock solution preparation: with distilled acrylonitrile (AN), itaconic acid (IA) in proportion 97:3, solid content 20wt%, azobisisobutyronitrile ( AIBN) accounted for 0.4wt% of the comonomer, added to the reactor with dimethyl sulfoxide (DMSO) as the solvent, and reacted at a constant temperature of 60°C for 20 hours under the protection of nitrogen to obtain a binary acrylonitrile copolymer spinning solution. Then the spinning solution is decompressed to remove residual monomers and air bubbles to obtain a high-performance polyacrylonitrile copolymer spinning stock solution. After testing, the molecular weight is 10300.

[0016] 2. Raw silk preparation: The spinning stock solution is metered by a metering pump, filtered at 5 μm and 3 μm, mixed through a SK static mixer with a diameter of DN20 and an aspect ratio of 15, and then extruded through a spinneret Then enter the first coagul...

Embodiment 2

[0019] The preparation method of carbon fiber precursor, comprises the following steps:

[0020] 1. Stock solution preparation: the steps are according to Example 1;

[0021] 2. Spinning: After the spinning stock solution is metered by a metering pump, filtered at 5 μm and 2 μm, and mixed by a SK static mixer with a diameter of DN30 and an aspect ratio of 25, it is extruded through a spinneret Enter the first coagulation bath, the temperature of the coagulation bath is 55°C, the concentration is 65%, the draft ratio is -20%, the second coagulation bath is 60°C, the concentration is 40%, the draft ratio is 100%, the third pass The coagulation bath is 60°C, the concentration is 20%, and the drafting ratio is 105% to obtain the as-spun fiber; after the as-spun fiber is solidified in 3 passes, it is drawn in 3 passes of hot water, and the drawing temperatures of the 3 passes of hot water are respectively 70°C, At 80°C and 90°C, the draw ratios are 1.2, 1.4, and 2. After 3 passes...

Embodiment 3

[0024] The preparation method of carbon fiber precursor, comprises the following steps:

[0025] 1. Preparation of stock solution: Distilled acrylonitrile (AN) and itaconic acid (IA) in proportion of 99:1, solid content of 26wt%, azobisisobutyronitrile (AIBN) accounts for 0.6wt% of comonomers, Add dimethyl sulfoxide (DMSO) as a solvent into the reactor, and react at a constant temperature of 60° C. for 20 hours under the protection of nitrogen to obtain a binary acrylonitrile copolymer spinning solution. Then the spinning solution is decompressed to remove residual monomers and air bubbles to obtain a high-performance polyacrylonitrile copolymer spinning stock solution. After testing, the molecular weight is 94600.

[0026] 2. Spinning: Spinning: The spinning stock solution is metered by a metering pump, filtered at 5 μm and 2 μm, and mixed by a SL-type static mixer with a jacket heat preservation with a diameter of DN50 and an aspect ratio of 20, and then passed through a sp...

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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 precursors. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber is a new type of material developed rapidly in the 1960s, because of its light weight, high specific strength, high specific modulus, high temperature resistance, corrosion resistance, wear resistance, fatigue resistance, electrical conductivity , thermal conductivity and other excellent properties, are widely used in satellites, launch vehicles, tactical missiles, spacecraft and other military industries, and have 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, continuous and stable production of carbon fibers with stable performance is an important issue for the majority of scientific re...

Claims

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Application Information

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Patent Type & Authority Patents(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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