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A kind of high-performance mesophase carbon microspheres and preparation method thereof

A technology of mesophase carbon microspheres and mesophase pitch, which is applied in the preparation/purification of carbon, chemical instruments and methods, carbon compounds, etc., to achieve the effects of high yield, uniform particle size distribution, and accelerated formation and growth

Active Publication Date: 2022-07-29
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 was used as the feed of the process, and the n-heptane insolubles were separated through n-heptane extraction, and 200 g of the extracted oil after the solvent was evaporated to dryness was mixed with 6 g of molybdenum hexacarbonyl, and the mixed solution was placed in the autoclave. , under nitrogen protection, the temperature was raised to 300 °C for 3 h of shallow catalytic reaction, and the potential mesophase pitch precursor with components >450 °C was separated under reduced pressure; 170 g of mesophase pitch precursor, 20 g of n-heptane insoluble matter and four 10g of hydronaphthalene was fully mixed, and the mixture was placed in an autoclave. Under 3Mpa nitrogen pressure, the temperature was raised to 400°C for 4h heterogeneous nucleation reaction to obtain a parent phase pitch rich in mesophase pellets, which was naturally cooled to room temperature , adding the parent phase pitch rich in mesophase pellets to the washing...

Embodiment 2

[0028] The medium and low temperature coal tar is used as the feed of this process, and the n-heptane insolubles are separated through n-heptane extraction, 200g of the extracted oil after evaporating the solvent and 10.5g of carbonyl iron are mixed, and the mixed solution is taken and placed in the autoclave. , under nitrogen protection, the temperature was raised to 340 °C for 3 h of shallow catalytic reaction, and the potential mesophase pitch precursor with components > 450 °C was separated under reduced pressure; 150 g of mesophase pitch precursor, 30 g of n-heptane insoluble matter and four 10 g of hydronaphthalene was fully mixed, and the mixture was placed in an autoclave. Under the nitrogen pressure of 3 Mpa, the temperature was raised to 440 °C for 4 h of heterogeneous nucleation to obtain a parent phase pitch rich in mesophase spheres, which was naturally cooled to room temperature. , adding the parent phase pitch rich in mesophase pellets to the washing oil, adding ...

Embodiment 3

[0030]The high-temperature coal tar is used as the feed of the process, and the n-heptane insolubles are separated through n-heptane extraction, and 200 g of the extracted oil after the solvent is evaporated to dryness and 15 g of platinum naphthenate are mixed, and the mixed solution is placed in the autoclave. , under nitrogen protection, the temperature was raised to 320 °C for 3 h of liquid-phase induced polycondensation reaction, and the potential mesophase pitch precursor with components >450 °C was separated under reduced pressure; 170 g of mesophase pitch precursor, 20 g of n-heptane insoluble matter and 10g of tetrahydronaphthalene was fully mixed, and the mixture was placed in an autoclave. Under 3Mpa nitrogen pressure, the temperature was raised to 420°C for 4h heterogeneous nucleation reaction to obtain a parent phase pitch rich in mesophase pellets, which was naturally cooled to At room temperature, the parent phase pitch rich in mesophase pellets was added to the ...

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Abstract

The invention relates to a high-performance mesophase carbon microsphere and a preparation method thereof. Heavy oil is used as a raw material, insoluble matter is extracted and separated by n-heptane, and deasphalted oil is doped with 3wt% to 10wt% of organic metal complexes 5wt%-15wt% of n-heptane insolubles and 1wt%-10wt% of free radicals were added to the potential mesophase pitch precursor with components >450℃ extracted under reduced pressure Auxiliary, through the heterogeneous nucleation reaction, the parent phase pitch rich in mesophase pellets is obtained, and the mesophase pellets are enriched by thermal centrifugation / hot filtration, and then the mesophase carbon microspheres are obtained after solvent extraction, washing and drying. The raw material used in the invention has low selection conditions and low price; the process and equipment are simple and easy to operate; the prepared mesophase carbon microspheres have high yield, controllable particle size and uniform distribution, and also realizes metal intercalation, and the lamellar structure is obtained. Optimization and improvement; product performance is superior and widely used.

Description

technical field [0001] The invention relates to a high-performance mesocarbon microsphere and a preparation method thereof. Taking heavy oil as a raw material, the high-performance mesocarbon microsphere is prepared by a combined process of shallow catalysis and synergistic polycondensation, and belongs to the preparation of novel carbon materials. field. Background technique [0002] Mesophase pitch is an aggregate of aromatic hydrocarbons with optical anisotropy. Due to its excellent performance, mesophase pitch has the characteristics of liquid crystal, both liquid form and optical anisotropy, and its preparation cost is low. , high oxidation activity, high carbon purity, it has been widely used in carbon fiber, foam carbon, needle coke, lithium ion secondary batteries and other fields. [0003] Mesophase pitch carbon microbeads are liquid-phase carbonaceous microbeads formed under the action of surface tension according to certain orientation and arrangement of polycycl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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)