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Preparation method of coal tar-based mesocarbon microbead

A technology of mesophase carbon microspheres and coal tar, which is applied in the direction of carbon preparation/purification, etc., can solve the problems of affecting the performance of carbon materials, increasing catalyst removal steps, complex processes, etc., and achieves low cost, wide application, and high process efficiency simple effect

Inactive Publication Date: 2012-09-05
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can significantly improve the yield of carbon microspheres, due to the addition of 0.1-20% catalyst in the raw material equipment, it is necessary to increase the removal steps of the catalyst, the process is complicated, and the presence of trace catalysts in the carbon microspheres is harmful to The performance of carbon materials prepared by subsequent processing will affect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The fraction before 280°C is cut off by atmospheric distillation of coal tar to obtain straight-run soft asphalt with a softening point of 37°C. Mix the mixed solvent of straight-run soft asphalt with heavy aromatic oil and gasoline at a mass ratio of 1:0.8, and the mass ratio of heavy aromatic oil and gasoline in the mixed solvent is 1:0.6, at 120°C at a speed of 300 rpm After stirring for 30 minutes, stand still for 1.5 hours, separate the extract phase, and distill off the solvent to obtain refined soft asphalt with a mass content of quinoline insolubles of 0.08%, and its mass percent yield is 74.2%. The obtained coal tar refined soft pitch was added to the reactor, under the protection of nitrogen, the temperature was raised to 420°C at a rate of 3°C / min, and the polymerization reaction was carried out at a stirring rate of 200 rpm for 4 hours to obtain mesophase pitch. After the mesophase pitch is cooled, it is extracted with pyridine until it is colorless. The amo...

Embodiment 2

[0038] Atmospheric pressure distillation of coal tar cuts off the fraction before 280°C to obtain straight-run soft asphalt with a softening point of 32°C. Mix straight-run soft asphalt with the mixed solvent of washing oil and kerosene in a mass ratio of 1:0.6, the mass ratio of washing oil and kerosene in the mixed solvent is 1:0.8, stir at 130°C at a speed of 500 rpm for 45 Minutes later, stand still for 3 hours, separate the extract phase, and evaporate the solvent to obtain refined soft asphalt with a mass content of quinoline insolubles of 0.09%, and its mass percent yield is 68.3%. The obtained coal tar refined soft pitch was added to the reactor, under the protection of nitrogen, the temperature was raised to 450°C at a rate of 2°C / min, and the polymerization reaction was carried out at a stirring rate of 100 rpm for 6 hours to obtain a mesophase pitch. After the mesophase pitch is cooled, it is extracted with quinoline until it is colorless. The amount of pyridine is ...

Embodiment 3

[0040] The fraction before 280°C is cut off by atmospheric distillation of coal tar to obtain straight-run soft asphalt with a softening point of 38°C. Mix straight-run soft asphalt with a mixed solvent of anthracene oil and paraffin oil in a mass ratio of 1:1.0, and the mass ratio of anthracene oil and paraffin oil in the mixed solvent is 1:1.0, at 150°C at a speed of 100 rpm After stirring for 60 minutes, stand still for 1 hour, separate the extract phase, and distill off the solvent to obtain refined soft asphalt with a mass content of quinoline insolubles of 0.02%, and its mass percent yield is 54.6%. The obtained coal tar refined soft pitch was added to the reactor, under the protection of nitrogen, the temperature was raised to 380°C at a rate of 1°C / min, and the polymerization reaction was carried out at a stirring rate of 400 rpm for 7 hours to obtain a mesophase pitch. After the mesophase pitch is cooled, it is extracted to colorless with benzene and acetone with a vo...

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Abstract

The invention discloses a preparation method of a coal tar-based mesocarbon microbead, comprising a process flow of pretreatment of raw materials, pyrocondensation polymerization reaction, separation and drying. The preparation method specifically comprises the following steps of: extracting, separating and removing primary quinoline insolubles of coal tar, as the raw materials, by using a mixed solvent to obtain coal tar refined soft pitch; then polymerizing the coal tar refined soft pitch for 1-8 hours at 350-450 DEG C under the rotating speed of 100-500 r / min and under the protection of inert gases by using anthracene oil or silicone oil as a reaction system viscosity regulator to obtain carbon microbead-containing mesophase pitches; and extracting by using a solvent, and drying to obtain the mesocarbon microbead. The particle diameter of the coal tar-based mesocarbon microbead prepared by using the method is 1-150 mu m, and the mass percent can reach 20-50%. The preparation method of the coal tar-based mesocarbon microbead has the characteristics of high product yield, controllable particle diameter, good sphericity, simple and convenient process, rich raw material sources, low cost and the like.

Description

technical field [0001] The invention belongs to the field of carbon materials, in particular to a method for preparing coal tar-based mesophase carbon microspheres. Background technique [0002] Mesophase carbon microspheres (MCMB) is a new type of carbon material. Due to its unique layered structure and excellent physical and chemical properties, it is widely used in high-density C / C composites, high specific surface activated carbon and lithium-ion secondary battery anode materials. , high-performance liquid chromatography packing, catalyst carrier and other aspects have been well applied. [0003] At present, the preparation methods of mesophase carbon microspheres mainly include thermal polycondensation method, emulsification method and suspension method. The thermal polycondensation method is to first polymerize the polycyclic aromatic hydrocarbon raw material by heat treatment to produce mesophase pitch containing carbon microspheres, and then use appropriate separati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B32/05
Inventor 赖仕全赵雪飞岳莉高丽娟周迪
Owner UNIV OF SCI & TECH LIAONING
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