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Preparation method of high modulus asphalt-based carbon fiber

A technology of pitch-based carbon fiber and high modulus, which is applied in the processing of tar pitch/petroleum pitch/natural pitch, fiber chemical characteristics, melting processing of tar pitch/petroleum pitch/natural pitch, etc., and can solve the difficulty of reaction degree and polymerization degree Control, catalyst, additives are difficult to separate, and affect the performance of pitch-based carbon fibers, etc., to achieve the effects of inhibiting excessive condensation reactions, improving composition structure distribution, and good spinnability

Active Publication Date: 2017-03-29
CHINA UNIV OF PETROLEUM (EAST CHINA) +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high polymerization temperature of the cross-linking synthesis method, the reaction is violent, and the degree of reaction and polymerization is not easy to control, so there are few studies on the cross-linking synthesis method at this stage.
[0008] The existing mesophase pitch preparation method produces mesophase pitch products, which generally have a high softening point, and the preparation process is complicated, and the catalyst and additives are difficult to separate, which will affect the performance of subsequent pitch-based carbon fiber products, and are not suitable for use as raw materials for high modulus carbon fibers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Put 200g of catalytic oil slurry into a stainless steel autoclave, replace the air with nitrogen purge 3 times, hydrogen purge 3 times to increase the pressure to 12MPa, heat up to 100°C at 2°C / min, start stirring, and continue to heat up to 420°C for 3 hours , to obtain the hydrogenation product; (2) Build a vacuum distillation device as required, and all the interface parts of the grinding instruments must be coated with vacuum sealant. After the instrument is installed, check the airtightness of the device. After confirming that the device is airtight, add the hydrogenation product into the round bottom flask, not exceeding half of the flask, add 3 to 4 zeolites, connect the vacuum system, turn on the vacuum pump, and the pressure reaches After 0.9mmHg and stabilized, start heating, and keep the heating rate at 4°C / min. Check the atmospheric and decompression temperature comparison table to find out that the vacuum distillation temperature corresponding to the nor...

Embodiment 2

[0028] (1) Put 200g of catalytic oil slurry into a stainless steel autoclave, replace the air with nitrogen purge 3 times, hydrogen purge 3 times to increase the pressure to 14MPa, heat up to 100°C at 2.5°C / min, start stirring; continue to heat up to 430°C for 2.5 h, to obtain the hydrogenation product; (2) Build a vacuum distillation device as required, and all the interface parts of the grinding instruments must be coated with vacuum sealant. After the instrument is installed, check the airtightness of the device. After confirming that the device is airtight, add the hydrogenation product into the round bottom flask, not exceeding half of the flask, add 3 to 4 zeolites, connect the vacuum system, turn on the vacuum pump, and the pressure reaches 1.0mmHg and stabilized, start heating, keep the heating rate at 4°C / min, consult the atmospheric and decompression temperature comparison table, find out that the vacuum distillation temperature corresponding to the normal temperature...

Embodiment 3

[0030] (1) Put 200g of catalytic oil slurry into a stainless steel autoclave, replace the air with nitrogen purge 3 times, hydrogen purge 3 times to increase the pressure to 16MPa, heat up to 100°C at 3°C / min, start stirring, and continue to heat up to 440°C for 2 hours , to obtain the hydrogenation product; (2) Build a vacuum distillation device as required, and all the interface parts of the grinding instruments must be coated with vacuum sealant. After the instrument is installed, check the airtightness of the device. After confirming that the device is airtight, add the hydrogenation product into the round bottom flask, not exceeding half of the flask, add 3 to 4 zeolites, connect the vacuum system, turn on the vacuum pump, and the pressure reaches 1.0mmHg and stabilized, start heating, keep the heating rate at 4°C / min, consult the atmospheric and decompression temperature comparison table, find out that the vacuum distillation temperature corresponding to the normal temper...

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Abstract

The invention relates to a preparation method of a high modulus asphalt-based carbon fiber. The preparation method comprises (1) carrying out high-pressure hydrogenation pretreatment on catalytic slurry oil under hydrogen pressure of 12-18Mpa at a reaction temperature of 420-450 DEG C for 1-3h to obtain a hydrogenation product, (2) carrying out vacuum distillation to separate a fraction at a temperature of greater than or equal to 400 DEG C and carrying out a polycondensation reaction process in an inert gas or nitrogen atmosphere at a reaction temperature of 460-500 DEG C for 6-8h to obtain a primary polycondensation product, (3) feeding nitrogen into the primary polycondensation product at a nitrogen flowing rate of 5-8L / (s. kg) under normal pressure and carrying out a reaction process at a reaction temperature of 450-500 DEG C for 4-6h to obtain high quality mesophase pitch and (4) carrying out melt spinning on the mesophase pitch and carrying out pre-oxidation, carbonization and graphitization to obtain the high modulus carbon fibers.

Description

technical field [0001] The invention relates to a method for preparing carbon fiber, specifically a method for preparing high-modulus pitch-based carbon fiber by melt spinning using catalytic oil slurry as a raw material, after high-pressure hydrogenation pretreatment and two-step polycondensation and graded carbonization to obtain mesophase products The method belongs to the technical field of advanced new carbon material preparation. Background technique [0002] Since the early 1980s, advanced new carbon materials have developed rapidly and are widely used in many fields such as defense industry, aerospace, cutting-edge technology, and daily life, and have a special and irreplaceable position in the entire material science. High modulus carbon fiber has attracted much attention because of its excellent performance. [0003] High modulus pitch-based carbon fiber is a kind of military-civilian dual-use industrial material with unique properties. It has been widely used in ...

Claims

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Application Information

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IPC IPC(8): D01F9/145C10G67/02C10C3/00C10C3/10C10C3/02
CPCC10C3/00C10C3/02C10C3/10C10G67/02D01F9/145
Inventor 刘东陈艳锋杨远兮吴中华郭爱军殷长龙陈坤夏薇吴萍萍张亚东李敏陈清泰叶家顺马文茜宋贤妮王浩丁若男黄恪
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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