Oxide-supported noble metal monoatomic catalyst and preparation method and application thereof
A precious metal and catalyst technology, applied in the field of oxide-supported precious metal single-atom catalysts and their preparation, can solve the problems of decreased catalyst activity, difficulty in accurately distinguishing the contribution of catalytic performance, poor stability, etc., and achieves improved utilization, good low-temperature oxidation of methane Good activity and stability
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[0039] The invention provides a method for preparing an oxide-supported noble metal single-atom catalyst, such as figure 1 As shown, the preparation method at least includes the following steps:
[0040] First, step S1 is performed, dissolving the noble metal salt and the non-noble metal salt in the alcohol solvent according to the molar volume ratio to obtain a uniform mixed solution.
[0041] As an example, the noble metal salt includes one or more combinations of chloropalladate, potassium chloropalladate, sodium chloropalladate, gold chloride, chloroauric acid, chloroplatinic acid, and potassium chloroplatinate.
[0042] As an example, the non-noble metal salt includes a combination of one or more of stannous chloride dihydrate, cerium nitrate hexahydrate, zirconium nitrate pentahydrate and manganese nitrate tetrahydrate. The high-temperature stable variable-valence oxide contained in the finally obtained catalyst includes SnO x , CeO x , ZrO x , MnO x A combination o...
Embodiment 11
[0064] Embodiment 1 No. 1 catalyst (SnO 2 ) preparation
[0065] 10mmol SnCl 2 2H 2 O was added to 90mL of ethylene glycol, ultrasonically dissolved; the solution was put into an oil bath previously heated to 125°C, stirred and refluxed for about 10 minutes, until the internal temperature of the solution rose to 120°C, quickly inject 15mL of ammonia water (5M) with a syringe, and stirred Reflux for 3 hours; wait for the solution to cool to room temperature after the reflux, and centrifuge to separate the precipitate and the solution. The precipitate is washed three times with ultrapure water and once with ethanol. After washing, it is vacuum-dried at 70°C overnight; Collect and bake in a muffle furnace at 350°C for 3h with a heating rate of 2°C / min.
[0066] figure 2 It is the SnO prepared in this example 2 In-situ X-ray diffraction patterns of the catalyst in air at different temperatures, where a-h represent 300°C, 400°C, 500°C, 600°C, 700°C, 800°C, 900°C, and 1000°C, ...
Embodiment 2
[0067] Embodiment 2 No. 2 catalyst (0.5%Pd / SnO 2 ) preparation
[0068] 5mmol SnCl 2 2H 2 O was added to 60mL of ethylene glycol and dissolved by ultrasonication; then 0.1mL of 0.36M H 2 PdCl 4 Aqueous solution, stir evenly, put it into an oil bath previously heated to 95°C, stir and reflux for about 10 minutes, until the temperature in the solution rises to 90°C, quickly inject 10mL of 5M ammonia water with a syringe, stir and reflux for 6 hours; wait for the solution to cool after the reflux is completed Centrifuge to room temperature, separate the precipitate and the solution, wash the precipitate three times with ultrapure water and once with ethanol, and dry it in vacuum at 70°C overnight after washing; grind the dried sample with a mortar, collect it, and place it in a muffle furnace at 850°C Baking for 3h, the heating rate is 5°C / min. Embodiment 2 The mass fraction of palladium feeding is 0.5% of the total catalyst.
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