Preparation method of silica supported nickel phosphide catalyst
A technology of silica and nickel catalysts, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc.
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Embodiment 1
[0016] Weigh 29.7g Ni(NO 3 ) 2 ·6H 2 O was dissolved in water to make a 100ml solution; another 18.9g NaSiO 3 9H 2 O and 11.7 g Na 2 CO 3 Dissolve in water to make 100ml solution. Add the above two solutions dropwise to 200ml of distilled water at the same time under stirring to form a green precipitate. After washing the precipitate with distilled water, add 200ml of n-butanol, evaporate to dryness in a water bath, and then dry it in a 393K oven to obtain Nickel catalyst supported on silicon.
Embodiment 2
[0018] Weigh 5 g of the silica-supported nickel catalyst of Example 1 and fill it into a reactor, raise the temperature to 673K, feed hydrogen at a flow rate of 100ml / min, reduce the temperature for 2h, then cool down to 543K, and feed 4 wt% triphenyl The n-heptane solution of base phosphine was phosphated for 12h, and the flow rate of n-heptane solution was 15ml / h. 2 Passivate with 1% nitrogen for 12 hours, and the flow rate of nitrogen is 20ml / min, to obtain a passivated silicon dioxide-supported nickel phosphide catalyst. The specific surface area of the prepared catalyst (named NP1) is 123m 2 / g, XRD spectrum is shown in accompanying drawing.
Embodiment 3
[0020] Weigh 5 g of the silica-supported nickel catalyst of Example 1 and fill it into a reactor, raise the temperature to 673K, feed hydrogen at a hydrogen flow rate of 100ml / min, reduce the temperature for 2h, then cool down to 443K, and feed 4wt% triphenyl The n-heptane solution of base phosphine was phosphated for 12h, and the flow rate of n-heptane solution was 15ml / h. 2 Passivate with 1% nitrogen for 12 hours, and the flow rate of nitrogen is 20ml / min, to obtain a passivated silicon dioxide-supported nickel phosphide catalyst. The specific surface area of the prepared catalyst (named NP2) is 197m 2 / g, XRD spectrum is shown in accompanying drawing.
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