负载型磷化钼（镍）和钼镍硫原子簇合物催化剂的制备、表征和深度加氢脱硫反应性能研究
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摘要
由于更加严格的环境法规的要求,开发新型深度加氢脱硫(HDS)催化剂是催化领域挑战性的课题。本文采用程序升温还原的方法,制备了纯相和负载型的过渡金属磷化钼、磷化镍和磷化镍钼催化剂,并对这些催化剂进行了详细的表征。以CO 为探针分子,用原位红外光谱研究了还原态磷化物催化剂的表面活性位及在硫化条件下的表面活性位的变化。反应结果表明,SiO_2负载的磷化物的DBT HDS 反应活性顺序是:Ni_2P/SiO_2 > Ni-Mo-P/SiO_2 >MoP/SiO2。磷化镍钼催化剂的HDS 活性随着Ni 含量的升高而提高。这不同于金属硫化物、氮化物和碳化物,因为在磷化的Ni 和Mo 原子之间没有观察到明显的协同作用。磷化镍钼催化剂的活性主要是磷化镍的贡献。CO 探针的红外光谱表明,在HDS 反应过程中,磷化物催化剂的体相结构可基本保持,但催化剂表面被部分硫化,形成了MoP_xS_y或NiP_xS_y活性相。这种表面被部分硫化的磷化物催化剂,在温和的条件下,可以重新活化恢复到新鲜态的状态。对于磷化物催化剂,DBT HDS 反应主要经历碳-硫键断裂的直接脱硫(DDS)反应途径,反应主要产物是联苯。本研究表明:磷化物,特别是磷化镍,是具有潜在应用前景的新型深度加氢脱硫催化剂。
另外,论文工作中还制备了纯相和负载型的过渡金属碳化钼。HDS 反应结果表明,碳化钼催化剂中加入P、Co 和Ni 之后,可以提高催化剂的HDS活性。制备了三核和四核具有簇芯为[Mo_3S_4(H_2O)_9]~(4+)和[Mo_3NiS_4 (H_2O)_(10)]~(4+)的过渡金属钼(镍)硫原子簇合物。金属原子簇合物为前驱体制备的Al2O3 负载的催化剂与传统的NiMoS/Al_2O_3催化剂相比,前者具有更小的金属粒子大小和更高的金属分散程度,且比相应的传统方法制备的硫化物催化剂具有更高的HDS 活性。
Interest in the development of novel catalysts for hydrodesulfurization hasbeen spurred by the need to meet stringent environmental regulations that haverecently been enacted throughout the world. Bulk and supported binary andternary phosphides, molybdenum phosphide, nickel phosphide and nickelmolybdenum phosphide have been prepared by temperature-programmedreduction method and characterized by X-ray diffraction (XRD), BET surface area,CO chemisorption, transmission electron microscopy (TEM) and (31)~P MAS NMRand in-situ infrared spectroscopy (IR). The hydrodesulfurization (HDS) activitiesof dibenzothiophene (DBT) were compared for these phosphide catalysts. In orderto gain insight into the nature of the phosphide catalysts under HDS conditions,the surface sites of reduced and sulfided phosphide catalysts were studied by IRspectroscopy using CO as the probe molecule.
The activities of the phosphides follow the order Ni_2P/SiO_2 > Ni-Mo-P/SiO_2> MoP/SiO_2. The HDS activities of phosphide catalysts don’t decline with thetime on stream for at least 20 h. Nickel phosphide has the highest HDS activityamong these phosphide catalysts. The Ni sites in the Ni-Mo-P/SiO_2 catalysts playa major role in the conversion of DBT, and the activity of the catalysts increaseswith increasing Ni content. This is different from sulfides, nitrides, and carbides,as no synergetic effect is observed between the phosphided Ni and Mo atoms. Italso suggests that Ni species more easily expose at the surface of the NiMoP
particles. The suface of a working Ni2P/SiO2 catalyst may be a nickelphosphosulfide (i.e., NiPxSy) phase. This unique surface composition of NiPxSy isassumed to be responsible for the excellent HDS activity of the Ni2P/SiO2 catalyst.The IR results indicate that the surface of these phosphide catalysts is partiallysulfided while the structure of the phosphides is retained under HDS reactionconditions. The sulfided phosphide surface can be fully regenerated to a freshphosphide catalyst under mild conditions. For molybdenum phosphide, nickelphosphide, and nickel molybdenum phosphide catalysts, the transformation ofDBT takes place mainly through direct desulfurization yielding biphenyl. Thiswork demonstrates that the nickel phosphide is potentially a promising catalyst forhydrodesulfurization processing. Bulk and supported transition metal molybdenum carbide were prepared.HDS reaction test results indicate that the addition of P, Co and Ni can increasethe HDS activities of β-Mo2C catalyst. The activities of β-Mo2C catalystgradually decrease with the reaction time on stream, this is different from MoPcatalyst. Molybdenum sulfur clusters with [Mo3S4(H2O)9]4+ and [Mo3NiS4 (H2O)10]4+cores were prepared. The catalyst prepared by the Mo3S4 cluster precursor hassmaller metal particle size, better metal dispersion on the support, and higher HDSactivities than the commercial NiMo sulfide catalyst prepared by traditionalmethod.
另外,论文工作中还制备了纯相和负载型的过渡金属碳化钼。HDS 反应结果表明,碳化钼催化剂中加入P、Co 和Ni 之后,可以提高催化剂的HDS活性。制备了三核和四核具有簇芯为[Mo_3S_4(H_2O)_9]~(4+)和[Mo_3NiS_4 (H_2O)_(10)]~(4+)的过渡金属钼(镍)硫原子簇合物。金属原子簇合物为前驱体制备的Al2O3 负载的催化剂与传统的NiMoS/Al_2O_3催化剂相比,前者具有更小的金属粒子大小和更高的金属分散程度,且比相应的传统方法制备的硫化物催化剂具有更高的HDS 活性。
Interest in the development of novel catalysts for hydrodesulfurization hasbeen spurred by the need to meet stringent environmental regulations that haverecently been enacted throughout the world. Bulk and supported binary andternary phosphides, molybdenum phosphide, nickel phosphide and nickelmolybdenum phosphide have been prepared by temperature-programmedreduction method and characterized by X-ray diffraction (XRD), BET surface area,CO chemisorption, transmission electron microscopy (TEM) and (31)~P MAS NMRand in-situ infrared spectroscopy (IR). The hydrodesulfurization (HDS) activitiesof dibenzothiophene (DBT) were compared for these phosphide catalysts. In orderto gain insight into the nature of the phosphide catalysts under HDS conditions,the surface sites of reduced and sulfided phosphide catalysts were studied by IRspectroscopy using CO as the probe molecule.
The activities of the phosphides follow the order Ni_2P/SiO_2 > Ni-Mo-P/SiO_2> MoP/SiO_2. The HDS activities of phosphide catalysts don’t decline with thetime on stream for at least 20 h. Nickel phosphide has the highest HDS activityamong these phosphide catalysts. The Ni sites in the Ni-Mo-P/SiO_2 catalysts playa major role in the conversion of DBT, and the activity of the catalysts increaseswith increasing Ni content. This is different from sulfides, nitrides, and carbides,as no synergetic effect is observed between the phosphided Ni and Mo atoms. Italso suggests that Ni species more easily expose at the surface of the NiMoP
particles. The suface of a working Ni2P/SiO2 catalyst may be a nickelphosphosulfide (i.e., NiPxSy) phase. This unique surface composition of NiPxSy isassumed to be responsible for the excellent HDS activity of the Ni2P/SiO2 catalyst.The IR results indicate that the surface of these phosphide catalysts is partiallysulfided while the structure of the phosphides is retained under HDS reactionconditions. The sulfided phosphide surface can be fully regenerated to a freshphosphide catalyst under mild conditions. For molybdenum phosphide, nickelphosphide, and nickel molybdenum phosphide catalysts, the transformation ofDBT takes place mainly through direct desulfurization yielding biphenyl. Thiswork demonstrates that the nickel phosphide is potentially a promising catalyst forhydrodesulfurization processing. Bulk and supported transition metal molybdenum carbide were prepared.HDS reaction test results indicate that the addition of P, Co and Ni can increasethe HDS activities of β-Mo2C catalyst. The activities of β-Mo2C catalystgradually decrease with the reaction time on stream, this is different from MoPcatalyst. Molybdenum sulfur clusters with [Mo3S4(H2O)9]4+ and [Mo3NiS4 (H2O)10]4+cores were prepared. The catalyst prepared by the Mo3S4 cluster precursor hassmaller metal particle size, better metal dispersion on the support, and higher HDSactivities than the commercial NiMo sulfide catalyst prepared by traditionalmethod.
引文
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