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A kind of preparation method of pitch-based carbon fiber

A technology of pitch-based carbon fiber and mesophase pitch, which is applied in the fields of fiber chemical characteristics, textiles and papermaking, etc. It can solve the problems of high requirements for reaction equipment, complicated preparation process, and difficult operation, and achieve low equipment requirements, clean environment, and easy operation. simple effect

Active Publication Date: 2018-09-11
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing mesophase pitch preparation methods generally have the following problems: first, the composition and structure of the raw materials are strictly required, and many raw materials from abundant sources do not meet the requirements of the reactor and experimental conditions; second, the preparation process is complicated and the operation is difficult. High requirements on reaction equipment and high preparation cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Put 180g 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 13MPa, heat up to 100°C at 2°C / min, start stirring, heat up to 425°C for 3 hours, 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 of 400°C under...

Embodiment 2

[0025](1) Put 180g 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 3°C / min, start stirring, heat up to 430°C for 3 hours, 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 normal temperature of 40...

Embodiment 3

[0027] (1) Put 180g of catalytic oil slurry into a stainless steel autoclave, replace the air with nitrogen purge 3 times, hydrogen purge 3 times to raise the pressure to 16MPa, heat up to 100°C at 2°C / min, start stirring, heat up to 440°C for 2 hours, 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 normal temperature of 400°...

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Abstract

The invention relates to a preparation method of pitch-based carbon fiber, comprising the following steps: (1) using catalytic oil slurry as raw material; (2) high-pressure hydrogenation pretreatment, hydrogen pressure 12-18MPa, reaction temperature 420-450°C, reaction 1 ~3h to get the pretreated product; (3) Vacuum distillation to obtain ≥400°C fraction, add co-carbonization components (deasphalted oil of naphthenic vacuum residue or 450~550°C in naphthenic vacuum fraction) ℃ fraction or 450~550℃ fraction of catalytic cracking oil slurry hydrogenation reduction product, the co-carbonization component accounts for 10%~45% of the mass of the hydrogenation product ≥ 400℃ fraction), and the co-carbonization high-compression polymerization reaction is carried out, and the reaction condition is inert gas Or nitrogen atmosphere, reaction pressure 1~6MPa, reaction temperature 460~500°C, reaction 6~8h; (4) Unload to normal pressure, carry out negative compression polymerization reaction at 6~10L / (s·kg) nitrogen flow rate, reaction The temperature is 450-500° C., and the reaction is 4-6 hours to obtain high-quality spinnable mesophase pitch; (5) mesophase pitch is melt-spun to obtain pitch-based carbon fibers.

Description

technical field [0001] The invention relates to a preparation method of pitch-based carbon fiber, specifically a kind of method for preparing spinnable mesophase pitch by using catalytic oil slurry as raw material for high-pressure hydrogenation and then adding a co-carbonization agent for high-pressure and negative-pressure two-step polycondensation to obtain spinnable mesophase pitch. The method for the pitch-based carbon fiber belongs to the technical field of advanced new carbon material preparation. Background technique [0002] Carbon Fiber (CF for short) is a new fiber material with high strength and high modulus with a carbon content of more than 95%. It is formed by stacking organic fibers such as flake graphite microcrystals along the axial direction of the fiber. And the microcrystalline graphite material obtained by graphitization treatment. Carbon fiber has many excellent properties, such as light weight, high strength, high modulus and corrosion resistance, hi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/145
CPCD01F9/145
Inventor 刘东李志恒陈艳锋杨远兮张亚东李敏陈清泰叶家顺马文茜宋贤妮王浩丁若男龚鑫蒋瑞雪
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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