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A kind of preparation technology of mesophase pitch and pitch-based carbon fiber

A technology of pitch-based carbon fiber and mesophase pitch, applied in the processing of tar pitch/petroleum pitch/natural pitch, processing tar pitch/petroleum pitch/natural pitch with selective extraction, fiber chemical characteristics, etc., can solve the problem of unrealized inferior heavy oil High value-added utilization and other issues, to achieve the effect of low cost of raw materials and production process, reduce production cost, and promote development

Active Publication Date: 2022-07-29
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this patent uses a small amount of aromatic oil as an auxiliary agent to modify lignin, and does not realize the high value-added utilization of inferior heavy oil

Method used

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  • A kind of preparation technology of mesophase pitch and pitch-based carbon fiber
  • A kind of preparation technology of mesophase pitch and pitch-based carbon fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1: Pretreatment to obtain aromatic-rich oil

[0031] Under the condition of absolute pressure of 5KPa, 3000g of catalytic oil slurry is subjected to precision fractionation under reduced pressure to obtain a heavy distillation segment with a temperature of more than 300°C, and the mixed components (mixing volume ratio of 1-5) of the extractant furfural are 0.5-1m 3 The flow rate of / h was transferred to the ultrasonic thermal filtration coupled extraction system, the power of the ultrasonic generator was adjusted to 600-900W, the temperature of the mixed material was 60-90°C, and a ceramic membrane with a pore size of 20-200nm was used as the filter medium. Settling and separation of the agent oil, take the extracted oil and introduce it into the gel permeation chromatographic column;

[0032] Add a glass wool pad to the bottom of the gel column, add polystyrene gel, and add a glass wool pad to the top. Wet the gel column with 50ml of tetrahydrofuran, mix 100ml ...

Embodiment 2

[0035] The pretreatment of vacuum distillate oil is the same as in Example 1, to obtain rich aromatic oil, 200 g of rich aromatic oil and 20 g of lignin are mixed uniformly and then added to the reaction kettle, then 10 g of tetralin is added, the lid of the kettle is covered, and the reaction kettle is kept airtight. Sex is good. Use high-purity nitrogen to replace the air in the reactor three times, and finally fill the reactor with high-purity nitrogen to 4MPa; (2) turn on the heating switch, adjust the speed to 500r / min, control the reaction temperature to 410°C, the reaction pressure to 4MPa, and the reaction time After 6h, the pressure was reduced to normal pressure, and then the reaction kettle was taken out, put into cold water for rapid cooling, and when cooled to room temperature, the reaction kettle was opened to obtain mesophase pitch. The obtained mesophase pitch has a large watershed structure with an anisotropic phase and continuous phase, the H / C ratio is 0.60,...

Embodiment 3

[0037] The pretreatment of ethylene tar is the same as in Example 1, to obtain aromatic-rich oil, mix 200 g of aromatic-rich oil with 20 g of chitosan and add it to the reaction kettle, then add 5 g of tetrahydroquinoline, cover the kettle lid, and keep the reaction kettle airtight Sex is good. Use high-purity nitrogen to replace the air in the reactor three times, and finally fill the reactor with high-purity nitrogen to 6MPa; (2) turn on the heating switch, adjust the speed to 500r / min, control the reaction temperature to 420°C, the reaction pressure to 6MPa, and the reaction time After 8 hours, the pressure was reduced to normal pressure, and then the reaction kettle was taken out, put into cold water for rapid cooling, and when cooled to room temperature, the reaction kettle was opened to obtain mesophase pitch. The obtained mesophase pitch has a large watershed structure with anisotropic phase and continuous phase, H / C ratio of 0.65, carbon residue value of 82, mesophase ...

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Abstract

The invention provides a preparation process of mesophase pitch and pitch-based carbon fiber. A >40% aromatic-rich oil is doped with 5wt%-30wt% biomass and mixed uniformly as a raw material, then the raw material is placed in an autoclave, and the co-carbonization reaction is carried out under the protection of an inert gas and a co-carbonizing agent. The addition amount is 0.1-5wt%, the reaction temperature is 300-450°C, the reaction pressure is 0.1-10MPa, and the reaction time is 4-10h, and finally a mesophase pitch with good fluidity and a mesophase content of 50-100% and a softening point of 240-280°C is obtained. The obtained mesophase pitch is sequentially subjected to melt spinning, pre-oxidation, and carbonization / graphitization to obtain mesophase pitch-based carbon fibers. The method of the invention is the co-carbonization reaction of rich aromatic hydrocarbon oil and biomass, uses biomass to prepare mesophase pitch, expands the source of raw materials, solves the problem of low utilization rate of biomass resources, and saves resources.

Description

technical field [0001] The invention relates to a preparation process of mesophase pitch and pitch-based carbon fiber, belonging to the technical field of petroleum deep processing and the field of advanced new carbon material preparation Background technique [0002] Mesophase pitch generally has high purity and aromaticity, and its unique oriented and arranged aromatic macromolecular sheet structure makes it have excellent physical and chemical properties (such as optical anisotropy, thermal stability and spinnability, etc.). Due to the regularly oriented macromolecular lamellar structure inside the mesophase pitch, it is easy to graphitize when treated at high temperature, which is a typical easily graphitized carbon; at the same time, it has optical anisotropy, thermal stability, oxidation activity, spinnability and carbonization. It has the advantages of high yield and can be used as the precursor of many carbon materials; and because of its abundant and cheap raw mater...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10C3/00C10C3/08D01F9/145
CPCC10C3/00C10C3/08D01F9/145
Inventor 刘东娄斌李骏项在金龚鑫温福山师楠殷长龙杨修洁陈坤王昊喆丑维超刘晓尹晓霜周广雪郭永冯敬高
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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