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A kind of preparation method of spinnable mesophase pitch

A technology for mesophase pitch and petroleum pitch is applied in the field of preparation of spinnable mesophase pitch, which can solve the problems of low final product yield, harsh equipment conditions, high hydrogenation reaction pressure, etc., and achieves improved spinnability, Guaranteed purification effect and system viscosity reduction effect

Active Publication Date: 2021-03-09
SHAANXI TIANCE NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The purpose of the present invention is to provide a preparation method of spinnable mesophase pitch, which solves the problems of cumbersome operation process, high pressure of hydrogenation reaction, harsh equipment conditions and low yield of final product in the prior art.

Method used

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  • A kind of preparation method of spinnable mesophase pitch
  • A kind of preparation method of spinnable mesophase pitch

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preparation example Construction

[0039] The preparation method of the spinnable mesophase pitch of the present invention is prepared by purging the petroleum pitch with high aromaticity and high softening point as raw material, reacting with the high-boiling-point hydrogen-donating agent octahydrophenanthrene under lower pressure, and purging at normal pressure Spinnable mesophase pitch. Specifically include the following steps:

[0040] (1) After pulverizing the high-quality petroleum asphalt with a softening point of 110-150°C, use toluene as a solvent for thermal extraction, the extraction temperature is 110°C, and the mass ratio of the toluene solvent to the processed high-quality petroleum asphalt is ( 4~8):1, preferably 6:1. After the extraction is completed, the extract is filtered while it is hot, and the filtrate is distilled under reduced pressure to recover the solvent, and the obtained asphalt is purified petroleum asphalt.

[0041] The petroleum pitch with a softening point of 110-150°C should ...

Embodiment 1

[0049] Crush petroleum asphalt with a softening point of 120°C and an aromaticity of 86%, heat extraction with toluene with 6 times the mass of petroleum asphalt at 110°C, filter the extract with a sand core funnel after extraction, and distill the filtrate under reduced pressure to obtain Purify petroleum asphalt. The yield of purified petroleum asphalt is about 93%.

[0050] Put the purified petroleum asphalt into the high-pressure reaction kettle, add 10% pure octahydrophenanthrene of purified petroleum asphalt, and use high-purity nitrogen to replace the air after locking the kettle, and pressurize 0.4MPa, gradually raise the temperature to 400°C for 8 hours, and the stirring speed It is 300rpm, and the maximum pressure of the control system in the process does not exceed 1.8MPa.

[0051] The pressure of the system was released to close to normal pressure within 30 minutes, that is less than 0.1MPa, the stirring rate was adjusted to 250rpm, the system temperature was lowe...

Embodiment 2

[0056] Crush petroleum asphalt with a softening point of 120°C and an aromaticity of 86%, heat extraction with toluene with 8 times the mass of petroleum asphalt at 110°C, filter the extract with a sand core funnel after extraction, and distill the filtrate under reduced pressure to obtain Purify petroleum asphalt. The yield of purified petroleum asphalt is about 96%.

[0057] Put the purified petroleum asphalt into the autoclave, add 5% pure octahydrophenanthrene of purified petroleum asphalt, lock the kettle, use argon to replace the air, and pressurize 0.5MPa, gradually raise the temperature to 420°C for 6 hours, and the stirring rate is 300rpm, the maximum pressure of the control system in the process does not exceed 1.5MPa.

[0058] The system pressure was released to close to normal pressure within 30 minutes, the stirring rate was adjusted to 250 rpm, the system temperature was lowered to 410°C, and nitrogen purge was started at a flow rate of 8 L / (kg·min) for 4 hours....

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Abstract

A preparation method of spinnable mesophase pitch, which comprises pulverizing petroleum pitch with high softening point, performing thermal extraction and filtering to obtain purified petroleum pitch; mixing purified petroleum pitch with octahydrophenanthrene or a hydrogen-donating reagent containing octahydrophenanthrene , carry out thermal polycondensation reaction; after the thermal polycondensation reaction is completed, the pressure is reduced, under stirring, and purging is carried out at 370-420° C. to obtain mesophase pitch. In the present invention, the purified high softening point asphalt is directly mixed with the hydrogen-donating agent octahydrophenanthrene as the raw material of the mesophase pitch, and thermal condensation polymerization is carried out to combine the hydrogenation treatment and the polymerization reaction into one, and the removal of the hydrogen-donating agent is not required. , which simplifies the process flow; normal pressure purge is carried out after thermal polycondensation, avoiding the excessive escape of light components caused by vacuum treatment and disturbing the fusion of the mesophase, and also avoiding the rapid increase of the softening point of the system, and making it possible to still Active light components continue to remain in the reaction system to participate in polycondensation, thereby increasing product yield.

Description

technical field [0001] The invention belongs to the technical field of new materials and relates to a preparation method of spinnable mesophase pitch. Background technique [0002] Mesophase pitch is a nematic thermotropic liquid crystal substance formed by the accumulation of large planar polycyclic aromatic hydrocarbon molecules, which exhibits birefringence characteristics. It is prepared by catalyzing polycondensation under the action of a catalyst. Mesophase pitch is the precursor for preparing high-performance carbon materials such as mesophase pitch-based carbon fibers, mesophase carbon microspheres, needle coke, and mesophase foam carbon. The special structure of the mesophase endows these materials with excellent heat resistance and high thermal conductivity , good chemical stability and high electrical conductivity and other characteristics, it has broad application prospects in aerospace, precision electronics, machinery, energy and many other fields. [0003] C...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10C3/08C10C3/02
CPCC10C3/026C10C3/08
Inventor 赵宗严江汛张鸿翔孙海成马杰张亚兵
Owner SHAANXI TIANCE NEW MATERIAL TECH
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