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Method for preparing mesocarbon microbeads by cyclic pyrocondensation polymerization of byproduct asphalt

A technology of mesophase carbon microspheres and thermal condensation, which is applied in the preparation/purification of carbon, etc., can solve the problems of the influence of mesophase carbon microsphere material properties, the insignificant increase in product yield, and the low use efficiency of by-product pitch. Achieve the effects of improving particle size distribution and surface morphology, reducing production costs, and facilitating operation

Inactive Publication Date: 2018-09-28
CCTEG CHINA COAL RES INST
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Problems solved by technology

[0004] The above existing technologies all have certain deficiencies, or the preparation process is complicated, the energy consumption is large, the cost is high, or the price of the added components is high, and it has a certain impact on the properties of the mesophase carbon microsphere material, or has a negative impact on the product yield. While the improvement is not obvious, the production cost is also increased, or the use efficiency of the by-product asphalt is low, and the economic loss is large

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  • Method for preparing mesocarbon microbeads by cyclic pyrocondensation polymerization of byproduct asphalt
  • Method for preparing mesocarbon microbeads by cyclic pyrocondensation polymerization of byproduct asphalt
  • Method for preparing mesocarbon microbeads by cyclic pyrocondensation polymerization of byproduct asphalt

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preparation example Construction

[0029]The invention provides a method for preparing mesophase carbon microspheres, comprising: step 1, mixing coal-based pitch, by-product pitch, and a first solvent to obtain a mixed material, wherein the by-product pitch is a thermal polycondensation reaction After separating the pitch obtained after the mesophase carbon microspheres, the first solvent is an aromatic hydrocarbon, and / or solvent oil containing aromatic hydrocarbons; step 2, heating the mixed material to the reaction temperature for thermal polycondensation reaction, Obtain the polycondensation pitch containing mesophase carbon microspheres; step 3, extract and separate the polycondensation pitch in the second solvent to obtain solid phase components and liquid phase components; step 4, extract the solid phase The components are dried to obtain the mesophase carbon microspheres; the liquid phase components are distilled to obtain by-product pitch and recover the second solvent.

[0030] The preparation method ...

Embodiment 1

[0044] Add medium-temperature asphalt with a softening point of 85°C and by-product asphalt into a stainless steel reactor in a mass ratio of 2:1, add anthracene oil to the total asphalt at a mass ratio of 1:9, self-boost after nitrogen purging, and normal temperature to 350 The average temperature rise rate of ℃ is 8°C / min. After staying at a constant temperature of 350°C for 1 hour, the temperature rises to 440°C at a rate of 2°C / min and stays at a constant temperature for 8 hours. After the reaction is completed, the solvent pyridine is added for extraction at 80°C. The volume ratio of the polycondensation pitch to the carbon-containing microspheres is 4:1, and the solid insolubles are obtained by filtering through a filter with a pore size of 5 μm, and the solid insolubles are dried at 80° C. and a vacuum of 1 KPa to obtain mesophase carbon microspheres. The mass yield (based on the raw material) is 42.2%, the D10 particle size is 1.0 μm, the D50 particle size is 19.0 μm, a...

Embodiment 2

[0046] Add medium-temperature asphalt with a softening point of 85°C and by-product asphalt into a stainless steel reactor in a mass ratio of 6:1, the mass ratio of the amount of anthracene oil added to the total asphalt is 1:14, and the pressure is stabilized at 1 MPa after nitrogen purging. The average heating rate at 320°C is 7°C / min. After staying at a constant temperature of 320°C for 1.5 hours, the temperature rises to 420°C at a rate of 1.5°C / min, and stays at a constant temperature for 8 hours. After the reaction, add washing oil and extract at 120°C. The volume ratio of the washing oil to the polycondensation pitch of the carbon-containing microspheres is 2:1, and the solid insoluble matter is obtained by filtering through a filter with a pore size of 5 μm, and the solid insoluble matter is dried at 120 ° C and a vacuum of 1 KPa to obtain the mesophase carbon microspheres. Balls, the mass yield (based on raw materials) is 44.4%, the D10 particle size is 1.7 μm, the D50...

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Abstract

The invention relates to a method for preparing mesocarbon microbeads by cyclic pyrocondensation polymerization of a byproduct asphalt. The method comprises the steps: mixing coal-based asphalt, the byproduct asphalt and a first solvent to obtain a mixed material; heating the mixed material to a reaction temperature for a pyrocondensation polymerization reaction to obtain polycondensed asphalt containing mesocarbon microbeads; extracting and separating the polycondensed asphalt in a second solvent to obtain a solid-phase component and a liquid-phase component; drying the solid-phase componentto obtain the mesocarbon microbeads; and distilling the liquid-phase component to obtain the byproduct asphalt, and recovering the second solvent. The preparation method provided by the invention is simple in process, raw materials are not needed to be pretreated, a catalyst or a nucleating agent is not needed to be additionally added, and meanwhile, the byproduct asphalt generated by pyrocondensation polymerization can be recycled to take part in the pyrocondensation polymerization reaction again, so that the yield is high, and the prepared mesocarbon microbeads are relatively narrow in particle size distribution, good in sphericity and smooth in bead surfaces.

Description

technical field [0001] The invention belongs to the field of preparation of mesophase carbon microspheres, and in particular relates to a method for preparing mesophase carbon microspheres by circulating thermal condensation polymerization of by-product pitch. Background technique [0002] Mesophase carbon microspheres were first prepared by Japanese scholars Honda and Yamada through the process of pitch thermal condensation polymerization, which immediately aroused great interest of carbon material workers and conducted in-depth research. The mesophase is a discotic nematic liquid crystal structure formed by the regular arrangement of polycyclic aromatic hydrocarbons during the carbonization process. In the early stage of the reaction, small spheres of the mesophase are gradually formed due to surface tension. As the carbonization time prolongs, the small spheres melt and grow. The unique molecular structure of mesophase carbon microspheres makes it have excellent electrica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05
CPCC01B32/05
Inventor 王光耀颜丙峰李军芳吴艳谷小会王学云陈来夫李培霖毛学锋
Owner CCTEG CHINA COAL RES INST
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