Preparation method of metal phosphide-containing medium oil type hydrocracking catalyst
A metal phosphide, hydrocracking technology, applied in physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of insufficient catalyst stability and unstable heteropolyacid properties.
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Embodiment 1
[0037] Prepare an ammonium dihydrogen phosphate solution with a weight concentration of 30%, impregnate the above-mentioned dried carrier T-1 with the prepared phosphorus-containing solution for 2 hours, dry at 120°C for 4 hours, and then use the impregnation solution containing tungsten and nickel Immerse at room temperature for 2 hours, dry at 120°C for 4 hours, and then reductively activate under hydrogen atmosphere. to 700°C, and kept at 700°C for 2 hours to prepare the catalyst C-1 of the present invention.
[0038] Through XRD analysis (under nitrogen protection condition), it can be seen that there are tungsten phosphide (WP) and nickel phosphide (Ni phosphide) in the catalyst of the present invention. 2 The characteristic diffraction peak of P) forms the phosphating state of the active metal.
Embodiment 2
[0043] Prepare an ammonium dihydrogen phosphate solution with a weight concentration of 40%, impregnate the carrier T-2 of Comparative Example 2 with the prepared phosphorus-containing solution for 2 hours, dry at 120°C for 5 hours, and then use the impregnating solution containing tungsten and nickel Immerse at room temperature for 2 hours, dry at 100°C for 6 hours, and then perform hydrogen activation in a hydrogen atmosphere. First, increase from room temperature to 350°C at a rate of 10°C / min, then increase from 350°C to 600°C at a rate of 1°C / min. °C, and kept at 600 °C for 4 hours to prepare the phosphating transition metal catalyst C-2.
Embodiment 3
[0048] Prepare a solution of ammonium dihydrogen phosphate with a concentration of 60%, impregnate the carrier T-3 of Comparative Example 3 with the prepared phosphorus-containing solution for 2 hours, dry at 110°C for 5 hours, and then use the impregnating solution containing tungsten and nickel at room temperature Immerse for 2 hours, dry at 110°C for 6 hours, and then perform activation treatment under hydrogen atmosphere, firstly increase from room temperature to 450°C at 8°C / min, then rise from 450°C to 650°C at a rate of 1°C / min , and kept at 650° C. for 4 hours to prepare the phosphating transition metal catalyst C-3.
[0049] Table 1 Physicochemical properties of catalyst supports.
[0050] Numbering T-1 T-2 T-3 Molecular sieve, wt% 12.0 7.0 4.0 Amorphous silica-alumina, wt% 25.0 53.0 30.0 Macroporous alumina, wt% 43.0 20.0 46.0 Binder, wt% 20.0 20.0 20.0 Pore volume, ml / g 0.73 0.76 0.78 Specific surface area,...
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