Green Synthesis And Ihe HDS Performance Characterization Of Sulfide And Composite Catalysts

As a kind of chemical raw materials, oil plays an important role in the production of life. However, the conflicts between the increasingly stringent environmental regulations and the increasingly heavy oil component in raw oil is more and more serious, which makes the cleaner production of oil is inevitable. Hydrofining is the important technology to realize the clean production of oil. Therefore, the development of new type catalyst with high efficiency has great research significance.Compared with transition metal carbides and nitrides, sulfide catalyst cause the attention of researchers because of its resistance to sulfur poisoning. This paper completed the hydrothermal synthesis of sulfide, composite catalyst and supported catalyst. The catalysts were characterized by XRD, SEM, EDS, HDS test and so on. The research results are as follows:1. The hydrothermal synthesis of sulphide:(1) When we use molybdenum oxide as the source of molybdenum, thiourea as sulfur source, hydroxylamine hydrochloride as reducing agent, the optimum condition for hydrothermal synthesis of MoS2 are:the initia molar ratio of Mo/S=1:4 and reacting 24h at 200?. The products under optimum condition is pure nano-sized powders.(2) When we use nickel chloride as the source of nickel, sodium sulfide as sulfur source, the initial molar ratio of Ni/S=1:1, the optimum condition for hydrothermal synthesis of NiS are reacting 5h at 150?. The products under optimum condition is pure micron grade powder.(3) When we use sodium molybdate as source of molybdenum, thiourea as the source of sulfur, nickel chloride as the source of nickel, hydroxylamine hydrochloride as reductant, the optimum condition for hydrothermal synthesis of MoS2-NiS are:the initia molar ratio of Ni/(Ni+Mo)=0.1 and reacting 24h at 200?. The products under optimum condition is pure nano-sized powders. 2. The synthesis of supported catalyst:(1) With ZSM-5 as the carrier, the supported catalyst was synthesized by methods of physical mixing and integral hydrothermal.(2) When the supported catalyst was synthesized by integral hydrothermal method, the carrier does not participate in the reaction, also do not change the particle size and morphology of catalyst's activity center.(3) When the supported catalyst was prepared by physical mixing method, the amount supported on carrier can be controlled precisely. 3. The characterization of HDS performance of catalysts:(1) During the HDS process, there was no phase change happened, all of the catalysts have stable performance for itself.(2) The carrier only has poorly HDS performance, which proved transition metal compound is the active ingredient of catalyst.(3) Whether the addition of Ni2P can promote the catalytic effect of MoS2, it depends on the addition amount of N12P. The supported catalyst was prepared by physical mixing method, when Ni2P/MoS2=1:1, the HDS performance of MoS2-Ni2P/ZSM-5 is lower than MoS2-ZSM-5; While when Ni2P/MoS2=3:1, the HDS performance of MoS2-Ni2P/ZSM-5 is higher than MoS2-ZSM-5.(4) The addition of a small amount of nickel can promote the HDS performance of MoS2 in sulfide catalyst system. The composite catalyst MoS2-NiS has the best HDS performance.