A kind of preparation method that is used for phenol hydrogenation to prepare cyclohexanone catalyst
A cyclohexanone and catalyst technology, applied in the field of catalyst preparation, can solve the problems of affecting catalyst activity, surface palladium falling off, surface palladium content reduction, etc., and achieve the effect of improving catalytic hydrogenation activity, small ash content, and preventing direct reduction
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Embodiment 1
[0028] Activated carbon pretreatment:
[0029] Weigh 100g of 4-8 mesh activated carbon, add 500mL of hydrochloric acid solution with a concentration of 0.1N, wash at 100°C for 4h, filter, and wash with water until neutral; add 200mL of triphenylphosphine solution with a concentration of 0.01N, mix well, and let stand at room temperature for 6h. Filter, wash and dry for later use.
[0030] Preparation of Palladium Carbon Catalyst:
[0031] Weigh 10g of pretreated activated carbon, ultrasonically spray and absorb a mixed solution containing 3mL of 20g / L palladium chloride and 2mL of hydrogen peroxide, add 20mL of water after standing for 1h, adjust pH=8 with sodium carbonate, add 10mL of NaHCO 3 , precipitated at 30°C for 24h, added 3mL of formaldehyde, reduced at 30°C for 8h, filtered, washed, and dried to obtain the palladium-carbon catalyst of this example.
[0032] The palladium-carbon catalyst obtained in this example has the following properties: the content of metal pal...
Embodiment 2
[0034] Weigh 100g of 4-8 mesh activated carbon, add 500mL of 0.5N hydrochloric acid solution, wash at 100°C for 4h, filter, and wash with water until neutral; add 200mL of 0.02N triphenylphosphorus solution, mix well, and let stand at room temperature for 5h. Filter, wash and dry for later use.
[0035] Preparation of Palladium Carbon Catalyst:
[0036] Weigh 10g of pretreated activated carbon, ultrasonically spray and absorb a mixed solution containing 2mL30g / L palladium chloride, 1.5mL hydrogen peroxide and 0.3mL sodium hypochlorite, add 20mL water after standing for 4 hours, adjust the pH=9 with sodium carbonate, add 10mLNaHCO 3 , Precipitate at 50°C for 24h, raise the temperature to 60°C, add 8mL formaldehyde for reduction for 6h, filter, wash, and dry to obtain the palladium-carbon catalyst of this example.
[0037] The palladium-carbon catalyst obtained in this example has the following properties: the content of metal palladium in the catalyst is 0.49%, and the cataly...
Embodiment 3
[0039] Activated carbon pretreatment:
[0040] Weigh 100g of 4-8 mesh activated carbon, add 500mL of 1N hydrochloric acid solution, wash at 80°C for 3h, filter, and wash with water until neutral; add 200mL of 0.1N tricyclohexylphosphine solution, mix well, let stand at room temperature for 5h, filter , washed and dried for later use.
[0041] Preparation of Palladium Carbon Catalyst:
[0042] Weigh 10g of pretreated activated carbon, ultrasonically spray and absorb a mixed solution containing 1.5mL 40g / L palladium chloride, 1.5mL hydrogen peroxide and 0.2mL sodium hypochlorite, add 20mL water after standing for 4 hours, adjust pH=9 with sodium carbonate, add 10mLNaHCO 3 , Precipitate at 50°C for 24h, raise the temperature to 60°C, add 8mlL formaldehyde for reduction for 6h, filter, wash, and dry to obtain the palladium-carbon catalyst of this example.
[0043] The palladium-carbon catalyst obtained in this example has the following properties: the content of metal palladium...
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