Method for preparing mesophase carbon microspheres by using emulsification-hydrogenation-thermal polymerization ternary coupling system

A mesophase carbon microsphere and thermal polymerization technology, which is applied in the preparation/purification of carbon, can solve the problems of unsatisfactory degree of graphitization and complicated process, and achieve good sphericity, uniform particle size distribution and uniform particle size Effect

Active Publication Date: 2020-12-04
NORTHWEST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the above emulsification method patents, documents, and vapor deposition method patents, mesocarbon microspheres with good sphericity and uniform particle size distribution have been prepared, but the process is complicated and the degree of graphitization is not ideal, so further improvement It is meaningful to explore a more reasonable and efficient preparation process

Method used

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  • Method for preparing mesophase carbon microspheres by using emulsification-hydrogenation-thermal polymerization ternary coupling system
  • Method for preparing mesophase carbon microspheres by using emulsification-hydrogenation-thermal polymerization ternary coupling system
  • Method for preparing mesophase carbon microspheres by using emulsification-hydrogenation-thermal polymerization ternary coupling system

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Experimental program
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Embodiment 1

[0042] The method for preparing mesophase carbon microspheres in this embodiment is specifically:

[0043] (1) According to the added amount of hydrogen donating solvent is 15.00wt%, the added amount of modified catalyst is 0.05wt%, and the added amount of emulsified solvent is 84.95wt%, and mixed to prepare emulsified-hydrogenation-thermal polymerization three-way coupling solvent system, wherein , the mass ratio of the modified catalyst is blue coke:coke:graphene:modifier=80:10:5:5.

[0044] (2) Put 2.5kg of medium and low temperature coal tar in a rectification kettle for distillation, and distill out soft asphalt with a distillate section at 330-420°C, with a softening point of 40 and an aromaticity of 0.4, according to soft asphalt: three-way coupling Solvent system = 1:3 ratio mixing, placed in a high-pressure reactor for three-stage heating reaction, that is, the first stage is dominated by emulsification and dispersion, rising from normal temperature to 220°C, constant...

Embodiment 2

[0048] The method for preparing mesophase carbon microspheres in this embodiment is specifically:

[0049] (1) According to the added amount of hydrogen-donating solvent is 12.00wt%, the added amount of modified catalyst is 0.5wt%, and the emulsified solvent is added to 100%, and mixed to prepare an emulsified-hydrogenation-thermal polymerization three-way coupled solvent system, wherein, modified The mass ratio of the active catalyst is blue carbon: coke: graphene: modifier = 75:5:15:5.

[0050] (2) Put 2.5kg of medium and low temperature coal tar in a rectification kettle for distillation, and distill out soft asphalt with a distillate section at 330-420°C, with a softening point of 40 and an aromaticity of 0.4, according to soft asphalt: three-way coupling Solvent system = 1:4 ratio mixing, placed in a high-pressure reactor for three-stage heating reaction, that is, the first stage is dominated by emulsification and dispersion, from normal temperature to 200 ° C, constant t...

Embodiment 3

[0054] The method for preparing mesophase carbon microspheres in this embodiment is specifically:

[0055] (1) According to the added amount of hydrogen-donating solvent is 10.00wt%, the added amount of modified catalyst is 0.01wt%, and the emulsified solvent is added to 100%, and mixed to prepare an emulsified-hydrogenation-thermal polymerization three-way coupled solvent system, wherein, modified The mass ratio of the active catalyst is blue carbon:coke:graphene:modifier=88.9:10:1:0.1.

[0056] (2) Put 2.5kg of medium and low temperature coal tar in a rectification kettle for distillation, and distill out soft asphalt with a distillate section at 330-420°C, with a softening point of 70 and an aromaticity of 0.5, according to soft asphalt: three-way coupling Solvent system = 1:5 ratio mixing, placed in a high-pressure reactor for three-stage heating reaction, that is, the first stage is dominated by emulsification and dispersion, rising from normal temperature to 250°C, const...

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Abstract

The invention proposes a method for preparing mesophase carbon microspheres with an emulsification-hydrogenation-thermal polymerization ternary coupling system, which belongs to the technical field of preparation of mesocarbon microspheres. The method steps are 1) using a hydrogen-donating solvent, a modified catalyst and Prepare emulsification-hydrogenation-thermal polymerization ternary coupling solvent system by emulsifying solvent; 2) Add medium and low temperature coal tar pitch with a fraction of 330°C to 420°C into the emulsification-hydrogenation-thermal polymerization ternary coupling solvent system to prepare the mesophase asphalt; 3) the mesophase pitch is extracted with an organic solvent, dried, pre-oxidized under air atmosphere, N 2 Carbonization and graphitization under atmosphere can obtain mesophase carbon microspheres. The preparation method of mesocarbon microspheres of the present invention is a brand-new one-pot emulsification system, which provides a good production environment for the growth of mesocarbon microspheres, and ensures that the prepared mesocarbon microspheres have good sphericity and smooth surface. The particle size distribution is uniform and the degree of graphitization is high.

Description

technical field [0001] The invention relates to the technical field of preparation of mesophase carbon microspheres, in particular to a method for preparing mesophase carbon microspheres by using an emulsification-hydrogenation-thermal polymerization ternary coupling system. Background technique [0002] Mesophase carbon microspheres are a nematic liquid crystal structure formed during the carbonization of polycyclic aromatic compounds (such as coal tar pitch, coal tar, petroleum pitch, naphthalene, etc.). In the initial stage of mesophase transformation, it is spherical due to the effect of surface tension. As time goes on, the mesophase spheres grow up and merge, and finally anisotropic mesophase pitch is obtained. Separating the small balls formed in the early stage of the mesophase transformation from the mother liquor by an appropriate method is the mesophase carbon microspheres. Mesocarbon microspheres have been widely used in high-performance carbon materials, cataly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/05
CPCC01B32/05
Inventor 李冬田育成郑金欣崔楼伟淡勇李稳宏黄晔高峰
Owner NORTHWEST UNIV
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