Preparation method of mesophase carbon microspheres from coal liquefaction residues

A technology for mesophase carbon microspheres and coal liquefaction residues is applied in chemical processing of tar pitch/petroleum pitch/natural pitch, tar pitch/petroleum pitch/natural pitch, and petroleum industry, etc. Simple process, smooth ball surface effect

Inactive Publication Date: 2011-10-26
ZIBO MINING GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The technical solutions disclosed in these patents have been improved to a certain extent in improving the quality of MCMB, but none of them involves the method of preparing MCMB from coal liquefaction residue

Method used

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  • Preparation method of mesophase carbon microspheres from coal liquefaction residues
  • Preparation method of mesophase carbon microspheres from coal liquefaction residues
  • Preparation method of mesophase carbon microspheres from coal liquefaction residues

Examples

Experimental program
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Effect test

Embodiment 1

[0035] The method for preparing mesophase carbon microspheres from the coal liquefaction residue is completed in the following steps:

[0036] a. Dry the coal liquefaction residue until the moisture content is below 3%, and add one or two of toluene, xylene, and dimethyl sulfoxide to it according to the mass ratio of extraction agent: coal liquefaction residue at a ratio of 1:3 to 4. One or more than two kinds, stirring for 20min for extraction, then centrifuged at 4800-7000r / min to remove insoluble matter, and the extract phase after removal of insoluble matter was evaporated under reduced pressure for 4h at a temperature of 200-220°C and a pressure ≤0.2atm , to obtain refined pitch containing 0.5% quinoline insoluble matter, and its softening point is 92°C;

[0037] b. Add 2% of nucleation accelerator and 0.7% of chemical auxiliary agent to the refined asphalt obtained in step a. Heat to a temperature above the softening point, then stir and mix the chemical additives and n...

Embodiment 2

[0040] The method for preparing mesophase carbon microspheres from the coal liquefaction residue is completed in the following steps:

[0041] a. Dry the coal liquefaction residue until the moisture content is below 3%, and add one or two of N-methylpyrrolidone, quinoline, and pyridine in a mass ratio of extraction agent: coal liquefaction residue of 1:4-5. One or more kinds, stirring for 30-40 minutes to extract, and then separate and remove the insoluble matter at a rotating speed of 4800-7000r / min. The extract phase after removal of insoluble matter was evaporated under reduced pressure for 5 hours at a temperature of 220-240°C and a pressure of ≤0.2 atm to obtain refined pitch containing 0.1% quinoline insoluble matter, and its softening point was 101°C.

[0042] b. Adding 1.3% of chemical additives and 1% of nucleation accelerator by mass of the refined asphalt to the refined asphalt obtained in step a. Heat to a temperature above the softening point, then stir and mix t...

Embodiment 3

[0045] The method for preparing mesophase carbon microspheres from the coal liquefaction residue is completed in the following steps:

[0046] a. Dry the coal liquefaction residue until the moisture content is below 3%, and add one or both of tetrahydrofuran and dimethylacetamide to it according to the mass ratio of extractant: coal liquefaction residue at 1:5-6 (simultaneously The mass ratio of tetrahydrofuran and dimethylacetamide is 4:6 when two kinds are selected), stirred for 30-40 minutes for extraction, and then centrifuged at 4800-7000 r / min to remove insoluble matter. The extract phase after removal of insolubles was evaporated under reduced pressure for 5 hours at a temperature of 230-250°C and a pressure of ≤0.2atm to obtain refined pitch containing 0.1% quinoline insolubles, and its softening point was 92°C.

[0047] b. Adding 1.8% of chemical additives and 1.5% of nucleation accelerator to the refined asphalt obtained in step a. Heating to a temperature above the...

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Abstract

The invention discloses a preparation method of mesophase carbon microspheres from coal liquefaction residues serving as raw materials, which comprises the following steps of: firstly carrying out solvent extraction on the coal liquefaction residues, then carrying out a series of processing to obtain refined asphalt with different contents of quinoline insoluble substances, and carrying out thermal polycondensation reaction on the refined asphalt in the presence of a chemical auxiliary agent and a nucleating accelerator at the temperature of 380-450 DEG C, the pressure of 0-5 MPa and the stirring rotation speed of 40-500 r/min for 1-20 hours to obtain the mesophase microspheres. According to the invention, the chemical auxiliary agent and the nucleating accelerator can be added during theheat treatment process to improve the yield and narrow the particle size distribution of the mesophase carbon microbeads, and the mesophase carbon microspheres are prepared from the coal liquefactionresidues serving as the raw materials and have the advantages of low cost, simple preparation process, high yield (up to 35%), narrow particle size distribution, good sphericity, etc.

Description

technical field [0001] A method for preparing mesophase carbon microspheres from coal liquefaction residues relates to the field of coal deep processing, in particular to a method for preparing mesophase carbon microspheres using coal liquefaction residues. Background technique [0002] Mesocarbon microspheres (MCMB) is a new type of carbon material, which can be used to prepare lithium-ion secondary battery electrode materials, high-density and high-strength various graphite or carbon materials and other products. Mesophase carbon microspheres are developed with the discovery and research of mesophase pitch. In 1961, when Taylor was studying coal coking, he found that some optically different small spheres were produced, grown and merged in viritrinite, and finally formed a mosaic structure. In fact, these small anisotropic spheres are MCMB. By 1973, MCMB was separated from liquid-phase carbonized pitch, and spherulites were used to manufacture binder-free isotropic high-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/00C10C3/00C10C3/02C10C3/08
Inventor 王剑惠友权董凤波向柠朱晓露滕少朋张晓兰
Owner ZIBO MINING GRP
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