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Method for preparing mesophase pitches or mesophase microspheres through coal and oil co-liquified residues

A technology of mesocarbon microspheres and co-liquefaction residue, which is applied in the field of preparation of mesophase pitch or mesocarbon microspheres, can solve the problem of unsatisfactory orientation of mesophase, failure to fully reflect the utilization of heavy oil, and poor sphericity of spheres and other problems, to achieve the effect of good spinnability, uniform size and low softening point

Active Publication Date: 2015-11-11
TAIYUAN UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both of these two methods need to add chemical additives or polycondensation solvents and nucleation accelerators to the bituminous substances in the coal liquefaction residue. solvents, these methods do not fully reflect the utilization of heavy oil
[0005] In the prior art, mesophase pitch is mainly prepared by using components such as asphaltene, pre-asphaltenes or asphaltenes in the liquefaction residue. The orientation of the generated mesophase is not very ideal, and the obtained mesophase generally has a wide-area structure, and the softening point Slightly high, the rheological properties after melting are not very good, and the spinnability is not good
When using heavy oil to prepare mesophase, the obtained mesophase is generally mesophase carbon microspheres and mosaic structure, the spheres do not melt and grow into a streamlined structure, and the sphericity of the spheres is not very good

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036]Mix Yanzhou coal and Shijiazhuang catalytic cracking oil slurry evenly with a mass ratio of 0.5, and put 13.5Kg of the mixture into a 50L reactor produced by SK, Germany (the reactor adopts a magnetic stirrer with adjustable speed, and the speed is 100-220rpm) Afterwards, nitrogen gas was introduced, and the nitrogen pressure was adjusted to 3 MPa, heated to 400 °C at a heating rate of 1.15 °C / min and kept for 180 min. After stopping the heating, reduce the pressure and exhaust, and directly discharge the gas in the kettle into a self-made 40L distillation kettle to collect the condensed liquid. After the gas is exhausted, the liquid and solid materials are directly discharged from the lower part of the autoclave into the distillation kettle for distillation under reduced pressure. The vacuum distillation adopts heat conduction oil for indirect heating, and the temperature of the heat conduction oil in the distillation kettle is controlled to be ≤300°C. After the distil...

Embodiment 2

[0041] Fully mix 50g of kerosene co-liquefaction residue with 250g of tetrahydrofuran in Example 1, then add it into a Soxhlet extractor, heat to 145°C, perform positive extraction for 3 hours to obtain a mixture of extract and raffinate, and then The mixture is subjected to vacuum filtration to obtain an extract mixture S1, and the tetrahydrofuran in the extract mixture S1 is evaporated and recovered by a rotary evaporator, and the residue after solvent recovery is THF soluble matter. Thoroughly mix the THF soluble matter with 232g of n-hexane, then add it into the Soxhlet extractor, heat it to 150°C, carry out normal extraction for 2 hours to obtain a mixture of extract and raffinate, and then vacuumize the mixture Filtration to obtain raffinate asphaltene and extract mixture S2. Put the raffinate asphaltene in a fume hood for 10 hours, then put it into a vacuum drying oven, set the vacuum degree to 0.08MPa, heat to 105°C, and dry for 25 hours to obtain asphaltenes, in which...

Embodiment 3

[0045] Fully mix 51g of kerosene co-liquefaction residue with 300g of tetrahydrofuran in Example 1, then add it into a Soxhlet extractor, heat to 140°C, perform positive extraction for 2 hours to obtain a mixture of extract and raffinate, and then The mixture is subjected to vacuum filtration to obtain an extract mixture S1, and the tetrahydrofuran in the extract mixture S1 is evaporated and recovered by a rotary evaporator, and the residue after solvent recovery is THF soluble matter. Thoroughly mix THF solubles with 190g of n-hexane, then add it into a Soxhlet extractor, heat to 145°C, and carry out normal extraction for 3 hours to obtain a mixture of extract and raffinate, and then vacuumize the mixture Filtration to obtain raffinate asphaltene and extract mixture S2. Put the raffinate asphaltene in a fume hood for 11 hours, then put it into a vacuum drying oven, set the vacuum degree to 0.085MPa, heat to 115°C, and dry for 23 hours to obtain asphaltenes, in which quinoline...

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Abstract

The invention provides a method for preparing mesophase pitches or mesophase microspheres through coal and oil co-liquified residues. The coal and oil co-liquified residues and a first-level extracting solvent are subjected to positive extraction, first-level extract liquor and first-level raffinate are obtained, remaining substances obtained after the first-level extracting liquid solvent is recycled are a mixture of asphaltene and heavy oil, the mixture of the asphaltene and the heavy oil and a second-level extracting solvent are subjected to position extraction, and second-level extract liquor and second-level raffinate are obtained; the second-level raffinate is processed, and asphaltene is obtained; heavy oil is obtained after the second-level extracting liquid solvent is recycled; the asphaltene and the heavy oil are mixed according to a certain proportion and evenly placed in a reactor to be subjected to co-carbonization thermal polycondensation, and thermal polycondensation products containing the mesophase pitches or thermal polycondensation products containing the mesophase microspheres are generated; the thermal polycondensation products containing the mesophase microspheres are washed through quinoline, filtered and dried, and the mesophase microspheres are obtained. The method has the advantages of being simple in technology and low in production cost.

Description

technical field [0001] The invention belongs to a method for preparing mesophase pitch or mesocarbon microspheres, in particular to a method for preparing mesophase pitch or mesocarbon microspheres with kerosene co-liquefaction residue. Background technique [0002] Co-liquefaction of kerosene is the most promising way to convert coal and vacuum or atmospheric cracking residue or other heavy oil (including catalytic cracking oil slurry, oil sand pitch, coal tar, etc.) into clean liquid fuels in the petroleum industry. route. The kerosene co-liquefaction technology is developed on the basis of the direct coal liquefaction technology. It can improve or even eliminate the defects of the direct coal liquefaction technology. The advantages of low consumption, low investment and high conversion rate. Co-liquefaction of kerosene produces a considerable amount of heavy products (ie, liquefaction residue) while obtaining light oil products and a small amount of gas. At present, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 高峰郭艳玲李允梅冉娜妮申文忠杨建丽
Owner TAIYUAN UNIV OF TECH
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