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Method for preparing mesocarbon microbeads by copolycondensation

A technology of mesophase carbon microspheres and copolycondensation, which is applied in the preparation/purification of carbon, can solve problems such as difficulty in uniform dispersion, and achieve the effect of narrow particle size distribution and good sphericity

Inactive Publication Date: 2012-06-13
ZIBO MINING GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On an industrial scale, the addition of a large number of nucleation promoters involves uniform dispersion, especially if the nucleation promoter is in the nanoscale size, it will be difficult to achieve uniform dispersion.

Method used

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  • Method for preparing mesocarbon microbeads by copolycondensation
  • Method for preparing mesocarbon microbeads by copolycondensation
  • Method for preparing mesocarbon microbeads by copolycondensation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Blend 200 g of medium-temperature coal tar pitch with a QI content of 3% in quinoline insolubles and 300 g of coal liquefaction residue-based pitch without QI and add it to a 1L reactor, then add 1% (5 g) of nano-coke powder accounting for the total weight of the blend , stirred at 300°C for 20min at high speed under the protection of nitrogen, then raised the temperature to 420°C, and heat-treated for 8.5h under the pressure of 1.5MPa and stirring at 300 rpm to obtain the mother liquor pitch containing MCMB. The washing oil is used for high-temperature centrifugation, and then the tetrahydrofuran solvent is used for several times of centrifugal washing, followed by filtering and drying to obtain the MCMB product. The yield is 28% based on raw pitch.

Embodiment 2

[0027] Blend 300 g of medium-temperature coal tar pitch with a quinoline-insoluble QI content of 3% and 200 g of coal liquefaction residue-based pitch without QI into a 1L reactor, stir at 300°C for 20 minutes under nitrogen protection, and then heat up to 420°C. Under the pressure of 1 MPa and stirring at 300 rpm, heat treatment for 8 hours to obtain the mother liquor pitch containing MCMB. The medium oil is used for high-temperature centrifugation, and then tetrahydrofuran is used for several times of centrifugal washing, followed by filtering and drying to obtain the MCMB product. The yield is 20% based on raw pitch.

Embodiment 3

[0029] Blend 400g of medium-temperature coal tar pitch with 3% quinoline-insoluble QI content and 100g of coal liquefaction residue-based pitch without QI into a 1L reactor, add 0.5% carbon black, and stir at 300°C for 20min under nitrogen protection , and then raised the temperature to 420°C, under the pressure of 0.5MPa and stirring at 300 rpm, heat treatment for 8.5h to obtain the mother liquor pitch containing MCMB. The washing oil is used for high-temperature centrifugation, followed by several times of centrifugal washing with pyridine, followed by filtration and drying to obtain the MCMB product. The yield is 30% based on raw pitch.

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Abstract

The invention provides a method for preparing mesocarbon microbeads by copolycondensation, which belongs to the technical field of deep processing of coal and is characterized by comprising the following process procedures of: mixing coal tar pitch with coal liquefaction residue pitch in proportion, further heating the mixture at 300-350 DEG C till a low velocity state is obtained, reacting at 390-450 DEG C under a pressure of 0.2-2MPa for 5-12h after stirring uniformly to generate pitch containing the mesocarbon microbeads, subsequently washing with light fraction of coal tar and an organic solvent to obtain the mesocarbon microbeads. According to the invention, the coal tar pitch and the coal liquefaction residue pitch are used as raw materials in copolycondensation reaction; the problems that a large quantity of nucleation promoter needs to be added in preparation of MCMB (mesocarbon microbeads) by using the coal liquefaction residue as the raw material, especially in industrial scale, and the addition of the large quantity of nucleation promoter results in homodisperse are solved; furthermore, no compatilizer needs to be added. The prepared MCMB is narrower in particle size distribution, the yield can reach 30% and the product has good sphericity.

Description

technical field [0001] A method for preparing mesophase carbon microspheres (MCMB) by co-condensation, which belongs to the technical field of coal deep processing, and specifically relates to a coal liquefaction residue-based pitch that does not contain quinoline insolubles and coal tar pitch that contains quinoline insolubles. The method for preparing MCMB by blending and co-polycondensation. Background technique [0002] Mesocarbon microspheres (MCMB) is a new type of carbon material. Due to its unique molecular level parallel stacking structure and spherical characteristics, it has become a lithium-ion secondary battery electrode material, high-density isotropic carbon graphite block material, It is the preferred material for the preparation of ultra-high specific surface area spherical activated carbon and filling materials for high performance liquid chromatography. At the same time, recent studies have shown that MCMB also has potential applications in the preparatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B32/05
Inventor 王剑唐超朱晓露董凤波马长友滕少朋张晓兰
Owner ZIBO MINING GRP
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