Preparation method of phenol hydrogenation catalyst
A hydrogenation catalyst, phenol technology, applied in the field of catalysis, can solve the problems of high temperature and high pressure, products accompanied by by-products, unfriendly to the environment, etc.
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Embodiment 1
[0033] (1) Preparation of ZIF-67
[0034] First prepare 50 mL of 0.8 mol / L 2-methylimidazole methanol solution and 50 mL of 0.1 mol / L cobalt nitrate hexahydrate methanol solution. First put the 2-methylimidazole solution in a 250mL Erlenmeyer flask, add 0.25g of dicyandiamide under stirring, and then add 50mL of cobalt nitrate hexahydrate methanol solution, mix and stir for 24 hours. After standing still, the product was centrifuged and washed twice with methanol, and finally the final sample was baked in an oven at 80°C for 6h.
[0035] (2) Preparation of CN carrier
[0036] Take 0.5 g of the prepared ZIF-67 in a tube furnace, the calcination atmosphere is argon, the calcination temperature is 600° C., and the calcination time is 5 h. The temperature was raised from room temperature to the target temperature at a rate of 1°C / min. Calcined samples are denoted as Co-CN D . Prepared Co-CN D The sample was pickled in 30% nitric acid solution for 3 hours at 60°C under contin...
Embodiment 2
[0042] (1) Preparation of ZIF-67
[0043] First prepare 50mL of 0.4mol / L methanol solution of 2-methylimidazole and 50mL of 0.05mol / L methanol solution of cobalt nitrate hexahydrate. First put the 2-methylimidazole solution in a 250mL Erlenmeyer flask, add 0.5g of dicyandiamide under stirring, add 50mL of methanolic cobalt nitrate hexahydrate solution after stirring evenly, mix and stir and let it stand for 12 hours. After standing still, the product was centrifuged and washed 7 times with methanol, and finally the final sample was baked in an oven at 50°C for 24h.
[0044] (2) Preparation of CN carrier
[0045] Take 0.5 g of the prepared ZIF-67 in a tube furnace, the calcination atmosphere is nitrogen, the calcination temperature is 700° C., and the calcination time is 4 hours. The temperature was raised from room temperature to the target temperature at a rate of 0.8°C / min. Calcined samples are denoted as Co-CN D . Prepared Co-CN D The sample was pickled in 35% nitric ...
Embodiment 3
[0050] (1) Preparation of ZIF-67
[0051] First prepare 50mL of 0.1mol / L methanol solution of 2-methylimidazole and 50mL of 0.02mol / L methanol solution of cobalt nitrate hexahydrate. First put the 2-methylimidazole solution in a 250mL Erlenmeyer flask, add 0.4g of dicyandiamide under stirring, add 50mL of methanolic cobalt nitrate hexahydrate solution after stirring evenly, mix and stir and let it stand for 12 hours. After standing still, the product was centrifuged and washed 4 times with methanol, and finally the final sample was dried in an oven at 100°C for 10 h.
[0052] (2) Preparation of CN carrier
[0053] Take 0.5 g of the prepared ZIF-67 in a tube furnace, the calcination atmosphere is helium, the calcination temperature is 800° C., and the calcination time is 8 h. The temperature was raised from room temperature to the target temperature at a rate of 3°C / min. Calcined samples are denoted as Co-CN D . Prepared Co-CN D The sample was pickled in 40% nitric acid s...
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