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High-performance mesocarbon microbead and preparation method thereof

A mesophase carbon microsphere, high-performance technology, applied in carbon preparation/purification, chemical instruments and methods, carbon compounds, etc., to achieve the effects of slowing growth and fusion, inhibiting fusion, and increasing reactivity

Active Publication Date: 2021-04-13
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production process of the existing method needs to be optimized, and the uniformity and yield of carbon microspheres need to be greatly improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The medium and low temperature coal tar is used as the feed material of this process, and the n-heptane insoluble matter is separated by n-heptane extraction, and 200g of the extracted oil after the solvent is evaporated is mixed with 6g of molybdenum hexacarbonyl, and the mixed solution is placed in a high-pressure reactor , under the protection of nitrogen, the temperature was raised to 300°C for 3h shallow catalytic reaction, and the potential mesophase pitch precursor of the >450°C component was separated under reduced pressure; 170g of the mesophase pitch precursor, 20g of n-heptane insolubles and four Mix 10g of hydronaphthalene fully, take the mixed solution and put it in a high-pressure reactor, under 3Mpa nitrogen pressure, raise the temperature to 400°C for 4 hours for heterogeneous nucleation reaction, obtain the parent phase pitch rich in mesophase spheres, and cool down to room temperature naturally , adding the parent phase pitch rich in mesophase beads to ...

Embodiment 2

[0028] Medium and low temperature coal tar is used as the feed material of this process, and the n-heptane insoluble matter is separated by n-heptane extraction, 200g of the extracted oil after the solvent is evaporated is mixed with 10.5g of carbonyl iron, and the mixed solution is placed in a high-pressure reactor , under the protection of nitrogen, the temperature was raised to 340°C for 3h shallow catalytic reaction, and the potential mesophase pitch precursor of the >450°C component was separated under reduced pressure; 150g of the mesophase pitch precursor, 30g of n-heptane insolubles and four Mix 10g of hydronaphthalene fully, take the mixed solution and put it in a high-pressure reactor, under 3Mpa nitrogen pressure, raise the temperature to 440°C for 4h heterogeneous nucleation reaction, obtain the parent phase pitch rich in mesophase spheres, and naturally cool down to room temperature , adding the parent phase pitch rich in mesophase beads to the washing oil, adding ...

Embodiment 3

[0030]Use high-temperature coal tar as the feed material of this process, extract and separate n-heptane insoluble matter through n-heptane extraction, take 200g of the extracted oil after evaporating the solvent and mix with 15g of molybdenum naphthenate, and take the mixed solution and place it in a high-pressure reactor , under the protection of nitrogen, the temperature was raised to 320°C for 3h liquid-phase induced polycondensation reaction, and the potential mesophase pitch precursor of the >450°C component was separated under reduced pressure; 170g of the mesophase pitch precursor, 20g of n-heptane insolubles and 10g of tetrahydronaphthalene is fully mixed, the mixed solution is placed in a high-pressure reactor, and under 3Mpa nitrogen pressure, the temperature is raised to 420°C for 4h heterogeneous nucleation reaction, and the parent phase pitch rich in mesophase pellets is obtained, and the temperature is naturally cooled to At room temperature, add the parent phase...

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PUM

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Abstract

The invention relates to high-performance mesocarbon microbeads and a preparation method thereof.The preparation method includes the steps that heavy oil serves as a raw material, insoluble substances are separated out through n-heptane extraction, 3 wt%-10 wt% of organic metal complexes are doped in deasphalted oil for shallow catalysis, and metal intercalation modification is achieved; pulling out potential mesophase pitch precursor >450 DEG C under reduced pressure; adding 5wt%-15wt% of n-heptane insoluble substances and 1wt%-10wt% of free radical auxiliaries into the potential mesophase pitch precursor, carrying out heterogeneous nucleation reaction to obtain parent-phase pitch rich in mesophase spheres, carrying out thermal centrifugation / thermal filtration to enrich the mesophase spheres, and carrying out solvent extraction, washing and drying to obtain the mesocarbon microbeads. The used raw materials are low in selection condition and low in price; the process and equipment are simple and convenient to operate; the prepared mesocarbon microbeads are high in yield, controllable in particle size and uniform in distribution, metal intercalation is achieved, and the lamellar structure is optimized and improved; the product has excellent performance and wide application.

Description

technical field [0001] The invention relates to a high-performance mesophase carbon microsphere and a preparation method thereof. Using heavy oil as a raw material, the high-performance mesophase carbon microsphere is prepared through a combined process of shallow catalysis-cooperative polycondensation, which belongs to the preparation of new carbon materials. field. Background technique [0002] Mesophase pitch is an aggregate of aromatic hydrocarbons with optical anisotropy. Due to its excellent performance and liquid crystal characteristics, mesophase pitch has both liquid form and optical anisotropy characteristics, and its preparation cost is low. , high oxidation activity, and high carbon purity, it has been widely used in many fields such as carbon fiber, foam carbon, needle coke, and lithium-ion secondary batteries. [0003] Mesophase pitch carbon microspheres are liquid-phase carbonaceous microspheres formed by condensed-ring aromatic hydrocarbon macromolecules in ...

Claims

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Application Information

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IPC IPC(8): C01B32/05C01B32/205
CPCC01B32/05C01B32/205
Inventor 刘东龚鑫赵燕崔俊杰
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)