A study on slurrybed hydrotreating process of distillate oil:I Catalyst preparation
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摘要: 对浆态床加氢催化剂的制备方法、助剂和活性组分负载量进行了考察。研究结果表明,最佳的催化剂(SP25)制备方法为,采用一定粒度的γ-Al2O3微球作载体,浸渍四硫代钼酸铵的络合剂水溶液,120℃干燥12h,然后浸渍硝酸镍和磷酸二氢铵的水溶液,120℃干燥12h,在氮气气氛中500℃焙烧3h。SP25催化剂的主要物性为比表面积212.3m2/g,孔径11.3nm,孔容0.60mL/g,平均粒度17.3μm,骨架密度2.79g/cm3。制成的催化剂活性组分为硫化态,使用时不需进行预硫化。XRD和H2TPR表征结果表明,浸渍液中加入络合剂可以提高MoS2在载体表面的分散度。在反应温度350℃,压力6MPa,反应时间2h,催化剂加入量6%(占原料油质量)的反应条件下,催化剂对FCC柴油的脱硫率为85.1%,脱氮率为82.0%。Abstract: The catalyst for slurrybed hydrotreating of distillate oil was prepared; the preparation parameters like the loading of active components and phosphorus additive on the hydrotreating performance were investigated. The optimum catalyst (SP25) was obtained through impregnation of γ-Al2O3 particles with an aqueous solution of ammonium tetrathiomolybdate (ATTM) and certain complexing agent, drying at 120℃ for 12h, then impregnation with an aqueous solution nickel nitrate and ammonium dihydrogen phosphate, drying at 120℃ for 12h, at last calcined at 500℃ in N2 atmosphere for 3h. The as-prepared catalyst SP25 exhibited a specific surface area of 212.3m2/g, pore diameter of 11.3nm, pore volume of 0.60mL/g, particle size of 17.3μm, skeleton density of 2.79g/cm3; the active components in the asprepared catalyst were in sulfided form and presulfurization was not necessary before using. XRD and H2TPR suggested that the addition of complexing agent during impregnation could enhance the dispersion of MoS2 on γAl2O3. Under the conditions of 350℃, 6MPa, wcatal/woil = 6%, reaction time 2h, the efficiencies of hydrodesulfurization and hydrodenitrogenation for FCC diesel oil reached 85.1% and 82.0%, respectively.
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Key words:
- slurry-bed /
- hydrotreating /
- distillate oil /
- catalyst preparation /
- ammonium tetrathiomolybdate (ATTM)
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