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Preparation process 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

Active Publication Date: 2021-05-18
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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  • Preparation process of mesophase pitch and pitch-based carbon fiber
  • Preparation process 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 was subjected to vacuum precision fractionation to obtain a heavy distillation section greater than 300°C, and the mixed component of the extractant furfural (mixing volume ratio 1-5) was mixed with 0.5-1m 3 The flow rate per hour is sent to the ultrasonic thermal filtration coupling extraction system, the power of the ultrasonic generator is adjusted to 600-900W, the temperature of the mixed material is 60-90°C, a ceramic membrane with a pore size of 20-200nm is used as the filter medium, and then the filtrate is Static sedimentation and solvent oil separation, take the extracted oil and introduce it into the gel permeation chromatographic column;

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

Embodiment 2

[0035] The pretreatment of vacuum distillate oil is the same as in Example 1 to obtain aromatic-rich oil. After mixing 200g of aromatic-rich oil and 20g of lignin evenly, add it to the reactor, then add 10g of tetralin, cover the lid of the kettle, and keep the reactor airtight. sex is good. Use high-purity nitrogen to replace the air in the reactor for 3 times, and finally fill the reactor with high-purity nitrogen to 4MPa; (2) Turn on the heating switch, adjust the speed to 500r / min, and control the reaction temperature to 410°C, reaction pressure to 4MPa, and reaction time After 6 hours, reduce the pressure to normal pressure, take out the reaction kettle, put it into cold water for rapid cooling, and open the reaction kettle when it is cooled to room temperature to obtain mesophase pitch. The obtained mesophase pitch has a large basin structure in which the anisotropic phase is the continuous phase, the H / C ratio is 0.60, the carbon residue value is 83, the mesophase conte...

Embodiment 3

[0037] The pretreatment of ethylene tar is the same as in Example 1 to obtain rich aromatics oil, mix 200g rich aromatics oil with 20g chitosan and add to the reaction kettle, then add 5g tetrahydroquinoline, cover the still lid, and keep the reaction kettle airtight sex is good. Use high-purity nitrogen to replace the air in the reactor for 3 times, and finally fill the reactor with high-purity nitrogen to 6MPa; (2) Turn on the heating switch, adjust the speed to 500r / min, and control the reaction temperature to 420°C, reaction pressure to 6MPa, and reaction time After 8 hours, reduce the pressure to normal pressure, take out the reaction kettle, put it into cold water for rapid cooling, and open the reaction kettle when it is cooled to room temperature to obtain mesophase pitch. The obtained mesophase pitch has a large basin structure in which the anisotropic phase is the continuous phase, the H / C ratio is 0.65, the carbon residue value is 82, the mesophase content is 90%, a...

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Abstract

The invention provides a preparation process of mesophase pitch and pitch-based carbon fibers. The preparation process comprises the following steps: firstly, selecting aromatic hydrocarbon-rich oil with an aromatic carbon rate CA being greater than 40% and doping 5wt%-30wt% of biomass into the aromatic hydrocarbon-rich oil, uniformly mixing to obtain a raw material, putting the raw material into a high-pressure kettle, and carrying out co-carbonization reaction under the protection of inert gas and a co-carbonization agent at the addition amount of 0.1-5wt%, wherein the reaction temperature of 300-450 DEG C, the reaction pressure of 0.1-10MPa and the reaction time of 4-10 hours, and finally obtaining mesophase pitch with good fluidity, the mesophase content being 50-100% and the softening point being 240-280 DEG C. The obtained mesophase pitch is sequentially subjected to melt spinning, pre-oxidation and carbonization / graphitization, and the mesophase pitch-based carbon fiber is prepared. According to the method, the aromatic hydrocarbon-rich oil and the biomass are subjected to co-carbonization reaction, the biomass is used for preparing the mesophase pitch, the raw material source is expanded, the problem that the utilization rate of biomass resources is not high is solved, and the resources are saved.

Description

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

Claims

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Application Information

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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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