Method for preparing Ni12P5 by reducing nickel oxide at low temperature
A nickel oxide, phosphine technology, applied in catalyst activation/preparation, chemical instruments and methods, phosphide and other directions, can solve the problems of high preparation temperature, temperature-programmed reduction is difficult to achieve, and achieves low preparation temperature and equipment cost. Low, short production cycle effect
Inactive Publication Date: 2012-01-25
NANKAI UNIV
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Problems solved by technology
Although this method is simple and feasible, this method needs to break the P-O bond in the phosphate during the preparation process, thus requiring a higher preparation temperature (generally above 550°C)
Moreover, temperature-programmed reduction is also difficult to achieve in large-scale production.
Method used
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Embodiment 1
[0013] First, 4.28 g of sodium hypophosphite (NaH 2 PO 2 .H 2 O) was added into 18mL deionized water, and after dissolving for 10min, 1.49g of NiO was added. After continuing to stir for 2 hours, the resulting solution was put into a petri dish and dried at 80°C. Then put the dried precursor powder into the reactor, heat treatment at 250°C for 10min in a static nitrogen protection, and then wash the obtained product with water and then dry it. The obtained sample has figure 1 Characteristics.
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The invention provides a new method for preparing nickel phosphide (Ni12P5) by utilizing phosphine produced by thermal decomposition of sodium hypophosphite to reduce nickel oxide precursor. In the method, nickel nitrate is adopted as a nickel source and then roasted to obtain nickel oxide, the obtained nickel oxide is dipped into sodium hypophosphite solution to obtain the nickel oxide precursor, and simple low temperature thermal treatment of the nickel oxide precursor is carried out so as to synthesize Ni12P5. The invention has the characteristics of simple process, low Ni12P5 preparation temperature, short production period, without the complex steps of temperature programming and the like as well as just simple thermal treatment at normal pressure. Raw materials used in the method are low in price and safe, and devices used in the method are low in cost. As the hydrodesulfurization and hydrodenitrogenation activities of Ni12P5-phase catalyst are both higher than that of the traditional sulfided phase catalyst, the Ni12P5-phase catalyst can be widely used for hydrogenation treatment of oils.
Description
technical field [0001] The present invention proposes a kind of nickel phosphide (Ni 12 P 5 ) of the new method. In this method, nickel nitrate is used as the nickel source to obtain nickel oxide after roasting, and the obtained nickel oxide is impregnated with sodium hypophosphite solution to obtain a precursor, and the precursor is synthesized by simple low-temperature heat treatment. 12 P 5 . The present invention is characterized in that the technique adopted is simple, Ni 12 P 5 The preparation temperature is low, the production cycle is short, and complex steps such as temperature programming are not required, and only simple heat treatment under normal pressure is required. The raw materials used are cheap and safe, and the cost of required equipment is low. because you 12 P 5 The hydrodesulfurization and hydrodenitrogenation activities of the catalyst in the phase are higher than those of the traditional catalyst in the sulfide phase, so it can be widely used ...
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IPC IPC(8): B01J27/185B01J37/16C01B25/08
Inventor 李伟关庆鑫张明慧
Owner NANKAI UNIV
