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
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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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