A kind of carbon-supported palladium-based alloy catalyst, its preparation method and application of catalytic preparation of styrene
A base alloy and catalyst technology, applied in the field of selective hydrogenation catalysts, can solve the problems of complex catalyst synthesis method, toxic additives, poor effect, etc., and achieve the effects of uniform size, high dispersion and high sulfur content
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[0040] The invention provides a method for preparing a carbon-supported palladium-based alloy catalyst, comprising: S1) mixing a sulfur-doped mesoporous carbon material, a palladium salt and a first transition metal salt in a first solvent, and removing the first solvent to obtain The mixture; S2) calcining the mixture in a reducing atmosphere to obtain a carbon-supported palladium-based alloy catalyst.
[0041] Wherein, the present invention has no special limitation on the sources of all raw materials, which can be commercially available or self-made.
[0042] The content of sulfur element in the sulfur-doped mesoporous carbon material is preferably greater than or equal to 14wt%; the specific surface area of the sulfur-doped mesoporous carbon material is preferably greater than or equal to 1200m 2 / g. In the present invention, the sulfur-doped mesoporous carbon material is preferably prepared according to the following steps: A1) mixing sulfur-containing small organic mol...
Embodiment 1
[0061] 1.1 Mix 0.5g 2,2'-bithiophene, 0.5g SiO 2 Airgel and 0.25g Co(NO 3 ) 2 ·6H 2 O was dispersed in tetrahydrofuran solvent, fully stirred, the solvent was removed by rotary evaporation, and a uniform powder was obtained by grinding.
[0062] 1.2 Transfer the uniform powder obtained in 1.1 to a quartz boat, raise the temperature to 800°C at a heating rate of 5°C / min under the protection of nitrogen, keep it for 2 hours, then cool down to room temperature at a rate of 5°C / min, and maintain normal pressure in the tube furnace. Get carbon nanomaterial-1.
[0063] 1.3 Transfer the carbon nanomaterial-1 obtained in 1.2 to an Erlenmeyer flask, add 40 mL of 2M NaOH solution, stir for 48 hours, perform the first alkali etching, then fully centrifuge the solution, pour off the supernatant, and remove the The solid precipitate was transferred to the Erlenmeyer flask again, and then 40 mL of 2M NaOH solution was added, stirred for 24 hours, and the second alkali etching was perfor...
Embodiment 2
[0067] Mix the 50.0 mg sulfur-doped mesoporous carbon material obtained in Example 1 above with a palladium chloride solution containing 8.5 mg Pd, and then add a ferric chloride hexahydrate solution containing 1.5 mg Fe so that the atomic ratio of Pd to Fe is 3 :1, and finally add water to dilute to keep the total volume of the mixed solution at 40ml. The mixed solution obtained above was sonicated for 1 hour, and then stirred at room temperature for 12 hours, so that the precursor and the carbon carrier were fully mixed; Medium reduction, the heating rate is 5°C / min, the temperature is raised to 400°C, and the temperature is kept for 2h. Then cool down to room temperature naturally, and the carbon-supported palladium-based alloy material (Pd 3 Fe / meso_S-C).
[0068] Utilize scanning transmission electron microscope to analyze the carbon-supported palladium-based alloy material obtained in embodiment 2, obtain its HAADF-STEM electron micrograph, as figure 2 shown.
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