High-dispersion palladium catalyst used for anthraquinone hydrogenation and preparation method of same
A palladium catalyst, high dispersion technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc. and other problems, to achieve good service life and regeneration cycle, improve surface properties, and reduce the effect of load
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Embodiment 1
[0037] Weigh 0.1g of dibutyltin mesylate, dissolve it in 100mL of deionized water, add 100g of Φ2-3mm spherical δ-Al 2 o 3 , after stirring evenly, put it into the microwave apparatus immediately, microwave heating for 10min, power 400W, temperature 60°C; after cooling to room temperature, filter the residual liquid, and dry the sample in vacuum at 40°C for 24h. Dissolve 0.45g palladium chloride in 100mL deionized water, put the above-mentioned δ-Al after organotin grafting 2 o 3 Carrier, crystallized at 70°C for 6h after soaking for 1h, poured off the residual liquid, washed with deionized water until neutral, dried at 100°C for 2h, calcined at 600°C for 4h, and then reduced with hydrogen at 1MPa and 50°C After 3h, a catalyst with a palladium content of 0.27wt% was obtained.
[0038] The dispersion degree of palladium in the catalyst was measured to be 53% by pulse chromatography hydrogen oxygen titration.
[0039] Catalyst performance was evaluated using a miniature fixe...
Embodiment 2
[0042] Weigh 0.1g of dibutyltin benzene sulfonate, dissolve it in 100mL of ethanol, add 100g of Φ2-3mm spherical δ-Al 2 o 3 , after stirring evenly, put it into the microwave instrument immediately, the microwave power is 800W, the reaction temperature is 150°C, and the microwave is heated for 10min. After cooling to room temperature, the residual liquid was filtered off, and the sample was vacuum-dried at 40°C for 24h. Dissolve 0.15g palladium chloride in 100mL deionized water, put the above-mentioned δ-Al after organotin grafting 2 o 3 Carrier, after soaking for 2 hours, crystallized at 60°C for 8 hours, poured off the residual liquid, washed with deionized water until neutral, dried at 120°C for 2 hours, calcined at 800°C for 2 hours, and then used at a pressure of 5MPa and 60°C Hydrogen reduction for 3 hours obtained a catalyst sample with a palladium content of 0.15%. The degree of dispersion of palladium was measured to be 65%.
[0043] With the detection condition ...
Embodiment 3
[0045] Weigh 0.15g dibutyltin p-toluenesulfonate, dissolve it in 100mL deionized water, add 100g Φ2-3mm spherical δ-Al 2 o 3 , after stirring evenly, put it into the microwave apparatus immediately, the microwave power is 600W, the reaction temperature is 120°C, and the microwave is heated for 15min. After cooling to room temperature, the residual liquid was filtered off, and the sample was vacuum-dried at 40°C for 24h. Dissolve 0.15g palladium chloride in 100mL deionized water, put the above-mentioned δ-Al after organotin grafting 2 o 3 Carrier, after soaking for 3 hours, crystallized at 60°C for 10h, poured off the residue, washed with deionized water until neutral, dried at 120°C for 2h, calcined at 600°C for 4h, and then used under pressure of 3MPa and 60°C Hydrogen reduction for 3 hours obtained a catalyst sample with a palladium content of 0.15%. The degree of dispersion of palladium was measured to be 61%.
[0046] With the detection condition of embodiment 1, reco...
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