Preparation method of load type transit metallic phosphide catalyst
A transition metal, phosphide technology, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of low activity, low catalyst specific surface area, etc., achieve good repeatability, low cost, The effect of large specific surface area
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[0019] A preparation method of a supported transition metal phosphide catalyst, comprising the steps of:
[0020] Step 1. Dissolve soluble transition metal salts and ammonium phosphate salts such as diammonium hydrogen phosphate or ammonium dihydrogen phosphate in water according to the target phosphide atomic ratio, and prepare a uniform solution;
[0021] Step 2: Warm up the ethanol aqueous solution with a volume percentage of 60% to 80% to 70 to 90°C, add soluble aluminum salts such as aluminum chloride, aluminum nitrate or aluminum acetate according to the loading capacity of 10% to 30%, and hydrolyze for 0.5 to 1 hour. Then add the solution prepared in step 1, and mix uniformly to obtain a mixed solution; wherein, the loading is the amount of phosphide in Al 2 o 3 percentage of mass;
[0022] Step 3, under the condition of ice-water bath, add propylene oxide dropwise to the mixed solution in step 2, and seal and let it stand for 30-40 minutes at 30-50°C to form a gel; w...
Embodiment 1
[0027] Preparation of MoP / γ-Al with a Loading Amount of 15% by Sol-Gel Method-Temperature Programmed Reduction Method 2 o 3 catalyst. The specific method is: according to the atomic ratio of MoP (molybdenum: phosphorus = 1:1), weigh 1.25g of ammonium molybdate and 0.94g of diammonium hydrogen phosphate, mix and dissolve in 15ml of deionized water until the solution is clear, and obtain an aqueous solution of molybdenum phosphate. Measure 24ml of deionized water and 56ml of ethanol, mix and heat to 80°C, add 0.1mol aluminum chloride hexahydrate, reflux for 1 hour, add the ammonium molybdate and diamine hydrogen phosphate deionized aqueous solution prepared above, and continue to reflux for 2 hours. Then, under an ice-water bath, 56 ml of propylene oxide was added dropwise to the above solution, and mixed uniformly. The solution was sealed and placed in a 30°C oven until gel appeared. Aged at 40°C for 1 day, dried at 120°C for 12h, and calcined at 500°C for 5h to prepare the ...
Embodiment 2
[0035] Preparation of MoP / γ-Al with a Loading Amount of 10% by Sol-Gel Method-Temperature Programmed Reduction Method 2 o 3 catalyst. The specific method is: according to the atomic ratio of MoP (molybdenum: phosphorus = 1:1), weigh 0.79g ammonium molybdate and 0.59g diammonium hydrogen phosphate, mix and dissolve in 15ml deionized water until the solution is clear, and obtain a molybdenum phosphorus aqueous solution. Subsequent operations are the same as in Example 1, and the prepared loading capacity is 10% MoP / γ-Al 2 o3 The specific surface area of the catalyst is 389.34m 2 / g.
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