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A kind of preparation method of mesophase pitch and mesophase carbon microspheres

A technology for mesophase carbon microspheres and mesophase pitch, which is applied in the preparation/purification of carbon, the processing of tar pitch/petroleum pitch/natural pitch, and the processing of tar pitch/petroleum pitch/natural pitch by selective extraction, etc. The problems of low yield and uneven particle size distribution of mesophase pitch and mesophase carbon microspheres can achieve the effect of high raw material processing depth, narrow size distribution and good sphericity

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 existing method only undergoes a thermal polycondensation reaction or a direct catalytic polycondensation process, and the yield of the obtained mesophase pitch and mesophase carbon microspheres is low and the particle size distribution is uneven

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The medium and low temperature coal tar heavy oil fraction was extracted and separated by n-heptane solvent to obtain n-heptane insoluble matter, and 300 g of the solvent was extracted after the oil was evaporated to dryness. In the autoclave, at the reaction temperature of 330°C, N 2 Under atmospheric protection, the reaction time was 5h for shallow catalysis, and the polycondensation heavy product with components > 450 °C was pulled out through the decompression device; 10 mg of n-heptane insoluble matter and 6 g of free radical auxiliary tetralin were added to the polycondensation heavy product to fully After mixing, take 200 g of it and add it to the autoclave, and react at a reaction temperature of 420 °C, a reaction pressure of 4 MPa, and a reaction time of 8 h. After the synergistic polycondensation of the two, the content of the wide-area mesophase pitch is 94.7%, and the softening point is 246 °C; After the mesophase pitch is cooled to room temperature, pulveri...

Embodiment 2

[0025]The high-temperature coal tar heavy oil fraction was extracted and separated by n-heptane solvent to obtain n-heptane insoluble matter. After the solvent was extracted from the oil and evaporated to dryness, 300 g of the oil was taken, and 6 g of carbonyl iron was doped into it. After fully mixing, it was added to the high-pressure reaction In the kettle, at the reaction temperature of 350°C, N 2 Under the atmosphere protection, the reaction time was 6 h for shallow catalysis, and the polycondensation heavy product with components > 450 °C was pulled out through the decompression device; 10 mg of n-heptane insoluble matter and 2 g of the free radical auxiliary decalin were added to the polycondensation heavy product to fully After mixing, take 200g and add it to the autoclave, at a reaction temperature of 450°C, N 2 The reaction time was 8h under the protection of atmosphere. After the two synergistic polycondensation, the content of wide-area mesophase pitch was 97.7% a...

Embodiment 3

[0027] The vacuum residue oil is extracted and separated by n-heptane solvent to obtain n-heptane insoluble matter. After the solvent is extracted and the solvent is evaporated to dryness, 300 g of the oil is taken, 21 g of cobalt naphthenate is doped into it, and the mixture is fully mixed and added to the autoclave. , at a reaction temperature of 330 °C, N 2 Carry out shallow catalysis under the condition of reaction time of 5h under atmosphere protection, and pull out the polycondensation heavy product with components > 450 ℃ through the decompression device; add 20 mg of n-heptane insoluble matter and 10 g of free radical auxiliary dihydrophenanthrene to the polycondensation heavy product , after fully mixing, take 200 g of it and add it to the high-pressure reaction kettle, and react at a reaction temperature of 440 ° C, a reaction pressure of 3 MPa, and a reaction time of 10 h. After the synergistic polycondensation of the two, the content of the wide-area mesophase pitch...

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Abstract

The invention relates to a preparation method of mesophase pitch and mesophase carbon microspheres. Heavy oil is used as a raw material, insoluble matter is separated by n-heptane extraction, and 3wt% to 10wt% of organic metal is doped in deasphalted oil. The complex was subjected to shallow catalysis, and the subsequent carbon microsphere structure was modified by metal intercalation; the catalytic product was decompressed and the polycondensation heavy product of the component >450 °C was extracted, and 10 ~ 200ug / g of n-heptane was added to insoluble. A wide-area mesophase asphalt is obtained by the synergistic polycondensation of the two and 1wt% to 10wt% of a free radical additive, which is crushed and sieved, and the mesophase asphalt particles of different sieving meshes are added to the high boiling point dispersion medium to emulsify into spheres. After washing and drying, mesophase carbon microspheres were obtained. The present invention has the advantages of using cheap and easy-to-obtain heavy oil as raw material, and preparing mesocarbon microspheres by a shallow catalytic-co-polycondensation-emulsification ternary combination process, and has the advantages of high yield, uniform particle size distribution and adjustable particle size. Controllable advantages, in addition, metal intercalation is also achieved, and the lamellar structure is optimized and improved.

Description

technical field [0001] The invention relates to a preparation method of mesophase pitch and mesophase carbon microspheres, in particular, using heavy oil as a raw material, and preparing the mesophase pitch and mesophase carbon microspheres through a combination process of shallow catalysis, synergistic polycondensation and emulsification, It belongs to the field of advanced new carbon material preparation. Background technique [0002] The crude oil in the world is becoming heavier, and the production of heavy oil is increasing day by day. The output of crude oil processed, including vacuum residue, atmospheric residue, catalytic cracking slurry, coal tar, ethylene tar, etc., has also increased year by year. The production of high value-added carbon materials provides an effective way of utilizing heavy oil. . [0003] Mesophase pitch is a liquid crystal phase compound containing a considerable amount of mesophase formed by a series of reactions such as bond breaking, deo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10C3/08C10C3/02C01B32/05
CPCC10C3/08C10C3/026C01B32/05
Inventor 刘东龚鑫李志浩崔俊杰赵燕
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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