High temperature solvent pretreatment method for improving yield of sodium rich coal direct liquefaction oil
A technology for directly liquefying coal and high-temperature solvents, which is applied in the treatment of hydrocarbon oil, the preparation of liquid hydrocarbon mixtures, and the petroleum industry. Application and other issues to achieve the effect of overcoming adverse effects, optimizing hydrogen distribution, and promoting transformation
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Embodiment 1
[0029]The raw coal is crushed, the crushed particle size is less than 150μm, and the crushed crushed coal and mixed solvent (tetralin, naphthalene, 0.10mol / L ferrous sulfate solution) are put into the tube bomb reaction at a mass ratio of 1:1 In the device, ultrasonic shock treatment was performed for 15 minutes. Then, the temperature of the reactor was raised to 220° C. at a heating rate of 80° C. / min, and the pretreatment residence time was 30 minutes. The treated mixed slurry was separated by centrifugal precipitation, and the recovered solvent was continued to be used in subsequent liquefaction experiments. The separated treated coal was vacuum-dried at 40°C for 6 hours and then sealed and stored. The direct liquefaction experiment was carried out under the conditions of 420°C and 3MPa hydrogen pressure. Compared with the crushed coal, the yield of liquefied oil increased by 10.5% and the conversion rate increased by 15.6% after solvothermal treatment.
Embodiment 2
[0031] The raw coal is crushed, the crushed particle size is less than 150μm, and the coal and the mixed solvent (dihydrophenanthrene, naphthalene, 0.12mol / L ferrous sulfate solution) are put into the high-pressure reactor with a mass ratio of 2:1, and ultrasonic vibration treatment 15min. Then, the reactor was heated to 230° C. at a heating rate of 100° C. / min, and the residence time was 30 minutes. The treated mixed slurry was separated by centrifugal precipitation, and the solvent was recovered and continued to be used in subsequent liquefaction experiments. The separated treated coal was vacuum-dried at 50°C for 8 hours and then sealed and stored. The direct liquefaction experiment of coal was carried out under the conditions of 440°C and 3MPa hydrogen pressure. Compared with the crushed coal, the yield of liquefied oil increased by 12.6% and the conversion rate increased by 16.3% after solvothermal treatment.
Embodiment 3
[0033] The raw coal is crushed, the crushed particle size is less than 100μm, and the crushed coal and the mixed solvent (dihydrophenanthrene, 1-methylnaphthalene, 0.15mol / L ferrous sulfate solution) are put into the high-pressure reactor at a mass ratio of 1.5:1 Within 20 minutes, ultrasonic shock treatment. Then, the reactor was heated to 230°C at a heating rate of 100°C / min, and the pretreatment residence time was 40min. The treated mixed slurry was separated by centrifugal precipitation, and the recovered solvent was continued to be used in subsequent liquefaction experiments. The separated treated coal was vacuum-dried at 50°C for 6 hours and then sealed and stored. The direct liquefaction experiment of coal was carried out under the conditions of 440°C and 2MPa hydrogen pressure. Compared with the crushed coal, the yield of liquefied oil increased by 11.3% and the conversion rate increased by 15.5% after solvothermal treatment.
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