| Petroleum played an important role in various industries as fossil fuel oil, beingrefined it can be used as fuel and chemical materials. There appear many byproductssuch as sulfur-containing aromatic hydrocarbons in the refining process. Forenvironmental protection, countries will limit the sulfur content of the oil, sohydrodesulfurization process is becoming more and more important. In variouscatalytic hydrogenation reactions, transition metal phosphide exhibited excellentcatalytic activity, high stability and sulfur anti-toxic. It has became new hydrotreatingcatalyst.In this paper, we synthesized Ni2P using nontoxic red phosphorus as rawmaterials by solvothermal method. Parameters such as molar ratio, reactiontemperature and holding time were important for the preparation. Their effects on thefinal product were discussed. Characterization methods such as XRD, EDS TEM andIR were applied for morphology and composition analysis of the products. Majorconclusions are as follows:(1)Solvothermal synthesis of nano nickel phosphideNi2P nano powders were prepared by solvothermal synthesis. The particle sizeof the product ranged from10to50nm, factors such as molar ratio, reaction time andreaction temperature were studied. Experimental results were as follows:Optimum ratio of the reactants is P/Ni=4/1. Under this condition, we canobtain well crystallized and pure nano powder Ni2P. When the ratio was increased(P/Ni>4/1), there appeared red phosphorus in the product. When the ratio was decreased(P/Ni <4/1), the product was mainly Ni12P5.Ideal synthesis temperature of nano Ni2P is180℃. When the temperature raisedfrom160℃to180℃, the purity of the product grow higher, and the crystallization isenhanced. However, when the temperature raised to200℃, the product becomes Ni12P5.The ideal reaction time is5h. Under this condition the product is pure Ni2P, andhas a high crystallization. With reaction time was extended to10h, the crystallizationof the product was slightly increased. However, when the reaction time was extendedto15h, the product changed into Ni12P5mainly.(2)Research on nano-nickel phosphide solvothermal synthesis mechanismFor the sake of better understanding of the reaction mechanism of Ni2P synthesis,a serious of experiments were carried out. Conclusions were drawn as follows:Ethanolamine is a reductive solvent. In such a solvent environmental, nickelchloride was reduced into Ni. Then red phosphorus reacted with Ni, there producedNi12P5was produced in the middle of the process, Ni12P5reacted with red phosphorussequently. As a result Ni2P was produced finally.(3)Iron-nickel phosphides solvothermal synthesisAccording to conclusions mentioned above, we try to synthesized (Fe,Ni)2P. Thefinal product were characterized by XRDã€TEM and EDS. Experimental resultsshowed that the final products were well crystallized, particle sizes ranging from20to50nm. With the nickel content increasing, the crystallization of the product wasincreased. |
