Preparation method of spinnable mesophase pitch

A technology for mesophase pitch and petroleum pitch, which is applied in the field of preparation of spinnable mesophase pitch, can solve the problems of cumbersome operation process, harsh equipment conditions, high hydrogenation reaction pressure, etc., and achieves the effect of good equipment adaptability

Active Publication Date: 2020-02-11
SHAANXI TIANCE NEW MATERIAL TECH
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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 cumb

Method used

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  • 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 comprises the following steps: crushing high-softening-point petroleum pitch, carrying out hot extraction, and performing filtration to obtain purified petroleum pitch; mixing the purified petroleum pitch with octahydrophenanthrene or a hydrogen supply reagent containing octahydrophenanthrene, and carrying out a thermal polycondensation reaction; and reducing the pressure after the thermal polycondensation reaction is finished, and performing purging at 370-420 DEG C while stirring to obtain the mesophase pitch. The purified high-softening-point pitch and the hydrogen supply reagent octahydrophenanthrene are directly mixed to serve as a mesophase pitch raw material for thermal polycondensation, hydrogenation treatment and polymerization reaction are integrated, the hydrogen supply reagent does not need to be removed, so the technological process is simplified; and normal-pressure purging is carried out after thermal polycondensation, sothat the phenomenon that the melting of an intermediate phase is disturbed due to too fast escape of light components, caused by adopting a vacuum treatment mode, is avoided, the softening point of the system is also prevented from being increased too fast, and the light components with activity can be continuously retained in the reaction system to participate in polycondensation, thereby the product yield is increased.

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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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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