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Preparation method of petroleum asphalt based carbon fiber

A petroleum pitch and carbon fiber technology, applied in the field of advanced new carbon material preparation, can solve the problems of high manufacturing cost, low yield of mesophase, complicated technology, etc., and achieve the effect of reducing production cost, high solubility and large volume

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

AI Technical Summary

Problems solved by technology

[0006] Although carbon fiber is widely used due to its superior performance, its high manufacturing cost, low mesophase yield, and overly complex technology restrict the development of the carbon fiber industry.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (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 13MPa, heat up to 100°C at 2°C / min, start stirring, heat up to 420°C for 3 hours, Obtain the hydrogenation product; (2) Install the vacuum distillation device as required, and all the interface parts of the grinding mouth instrument 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, maintain 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 o...

Embodiment 2

[0027] (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, heat up to 430°C for 2 hours, Obtain the hydrogenation product; (2) Install the vacuum distillation device as required, and all the interface parts of the grinding mouth instrument 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 is stable, 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 400°C under this pres...

Embodiment 3

[0029] (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 heat up to 440°C for 1.5h , to obtain the hydrogenation product; (2) Install the 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 the 1.0mmHg is stable, start heating, and keep the heating rate at 4°C / min. Check the atmospheric and decompression temperature comparison table to find out that under this pressure, the vacuum distillation temperature corresponding t...

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Abstract

The invention relates to a preparation method of petroleum asphalt based carbon fiber. The preparation method comprises the following steps: (1) adopting catalytic slurry oil as a raw material; (2) performing high-pressure hydrogenation pretreatment and reacting for 1-3h to obtain a hydrogenation product, wherein the hydrogen pressure is 12-18MPa, and the reaction temperature is 420-450 DEG C; (3) performing reduced-pressure distillation to obtain a fraction at 400-550 DEG C, adding a catalyst (1:1 Lewis acid functionalized ionic liquid / BF3 composite catalyst, the Lewis acid functionalized ionic liquid is aluminum chlorate ionic liquid ([BMIM]Cl / AlCl3) or zinc chloride ionic liquid (ZnCl2 / PPh3C6H13Br) or ferric chloride ionic liquid ([BMIM]Cl / FeCl3)), and reacting for 1-8h in an inert gas or nitrogen atmosphere, wherein the reaction pressure is 1-8MPa, and the reaction temperature is 280-360 DEG C; and performing catalytic condensation to obtain mesophase asphalt; and (4) melting and spinning the mesophase asphalt to obtain petroleum asphalt based carbon fiber.

Description

technical field [0001] The invention relates to a method for preparing petroleum pitch-based carbon fibers, specifically a method for preparing petroleum pitch-based carbon fibers by melt spinning after the mesophase pitch is obtained by using catalytic oil slurry as a raw material through high-pressure hydrogenation pretreatment and catalytic polycondensation , belonging to the technical field of advanced new carbon material preparation. Background technique [0002] Research on petroleum pitch-based carbon fibers began in the 1950s, and Japan realized industrialization in the late 1960s. In 1970, United Carbide successfully prepared pitch-based carbon fiber using petroleum pitch as raw material, and it was put into industrialization in 1982. At the end of the 20th century, the production capacity of pitch-based carbon fiber in the world reached 500 tons per year. Since then, countries have stepped up research on the application of pitch-based carbon fibers, improved prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/155B01J31/26B01J31/30
CPCD01F9/155B01J27/12B01J31/0284B01J31/0288B01J31/26B01J31/30B01J35/19
Inventor 刘东于冉陈艳锋杨远兮张亚东李敏陈清泰娄斌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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