Preparation method of supported nickel phosphide for catalyzing selective hydrogenation of furfural to prepare furfuryl alcohol
A selective and furfuryl alcohol production technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of unsatisfactory performance of non-precious metal catalysts and expensive price of precious metal catalysts, and achieve low price and mild conditions , synthesize simple effects
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Embodiment 1
[0012] Add 60mg of graphite oxide to 30mL of ethylene glycol, and ultrasonically treat to obtain a stable and dispersed graphene oxide mixture; then add 120mg of nickel chloride hexahydrate and 107mg of sodium dihydrogen hypophosphite, stir well and place in an oil bath reflux device React at 150° C. for 1 hour. After the end, the obtained supported nickel phosphide is fully washed with water and ethanol, and dried in vacuum at 60° C. for 3 hours.
[0013] Put 10mg of supported nickel phosphide, 0.1mL of furfural and 10mL of deionized water into a stainless steel autoclave, replace the autoclave with helium and hydrogen successively, and then react at 0.3MPa hydrogen pressure at 70°C for 0.5h. After the reaction, the solid particles were separated by centrifugation, the liquid mixture was extracted and separated by dichloroethane, and the product was analyzed by gas chromatography.
Embodiment 2
[0015] Add 60mg of graphite oxide to 30mL of ethylene glycol, and ultrasonically treat to obtain a stable and dispersed graphene oxide mixture; then add 240mg of nickel chloride hexahydrate and 321mg of sodium dihydrogen hypophosphite, stir well and place in an oil bath reflux device React at 170° C. for 2 hours. After the completion of the reaction, the obtained supported nickel phosphide is fully washed with water and ethanol, and dried in vacuum at 60° C. for 3 hours.
[0016] Put 20 mg of supported nickel phosphide, 0.5 mL of furfural and 10 mL of deionized water into a stainless steel autoclave, replace the autoclave with helium and hydrogen successively, and react at 0.5 MPa hydrogen pressure at 70 °C for 1 h. After the reaction, the solid particles were separated by centrifugation, the liquid mixture was extracted and separated by dichloroethane, and the product was analyzed by gas chromatography.
Embodiment 3
[0018] Add 60mg of graphite oxide to 30mL of ethylene glycol, and ultrasonically treat to obtain a stable and dispersed graphene oxide mixture; then add 360mg of nickel chloride hexahydrate and 482mg of sodium dihydrogen hypophosphite, stir well and place in an oil bath reflux device React at 170° C. for 2 hours. After the completion of the reaction, the obtained supported nickel phosphide is fully washed with water and ethanol, and dried in vacuum at 60° C. for 3 hours.
[0019] Put 20 mg of supported nickel phosphide, 0.5 mL of furfural and 10 mL of deionized water into a stainless steel autoclave, replace the autoclave with helium and hydrogen successively, and then react at 1 MPa hydrogen pressure at 70 °C for 1 h. After the reaction, the solid particles were separated by centrifugation, the liquid mixture was extracted and separated by dichloroethane, and the product was analyzed by gas chromatography.
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