A kind of method for preparing 1,4-cyclohexanediol by catalytic hydrogenation of p-benzoquinone
A technology for catalytic hydrogenation of cyclohexanediol, which is applied in hydrogenation preparation, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve problems such as high price of samarium iodide, difficulty in industrialization, non-green solvent and other problems, and achieve Conducive to competition, reduced post-processing steps, and low cost effects
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Embodiment example 1
[0026] Weigh 0.5g of titanium dioxide and dissolve it in 10ml of aqueous solution in a round-bottomed flask, add 0.054g of palladium nitrate dihydrate solid under continuous stirring, continue stirring for 12 hours, turn off the stirring, and remove excess aqueous solution by rotary evaporation after standing still for 12 hours. It was dried overnight, calcined at 450°C for 8 hours, and finally reduced at 300°C for 6 hours under hydrogen atmosphere to obtain a catalyst of noble metal palladium supported on titania. Take the catalyst 0.1g of titanium dioxide supported noble metal palladium prepared above, 25ml of water, and 0.5g of p-benzoquinone and add them to the reaction kettle, replace the air in the reaction kettle with hydrogen for 5 times, at a temperature of 80°C, a pressure of 0.5MPa, and a stirring speed of 900rpm, After reacting for 1 h, after cooling to room temperature, the reaction solution was taken out and analyzed by gas chromatography: the conversion rate was ...
Embodiment example 2
[0028] Weigh 0.5g of titanium dioxide and dissolve it in 10ml of aqueous solution in a round-bottomed flask, add 0.054g of palladium nitrate dihydrate solid under continuous stirring, continue stirring for 6 hours, turn off the stirring, and remove the excess aqueous solution by rotary evaporation after 12 hours of standing still , dried overnight, calcined at 550°C for 4 hours, and finally reduced at 200°C for 8 hours under a hydrogen atmosphere to obtain a catalyst of noble metal palladium supported on titania. Take 0.1g of catalyst, 25ml of water, and 0.5g of p-benzoquinone into the reaction kettle, replace the air in the reaction kettle with hydrogen for 5 times, react at a temperature of 120°C, a pressure of 0.5MPa, a stirring speed of 900rpm, and react for 2 hours. After cooling to room temperature, take out The reaction solution was analyzed by gas chromatography: the conversion rate was 95.97%, and the selectivity was 98.34%.
Embodiment example 3
[0030] Weigh 0.5g of titanium dioxide and dissolve it in 10ml of aqueous solution in a round-bottomed flask, add 0.054g of palladium nitrate dihydrate as a solid under continuous stirring, continue stirring for 12 hours, turn off the stirring, and remove the excess aqueous solution by rotary evaporation after standing still for 4 hours , dried overnight, calcined at 450°C for 8 hours, and finally reduced at 300°C for 6 hours under a hydrogen atmosphere to obtain a catalyst of noble metal palladium supported on titania. Take 0.1g of catalyst, 25ml of water, and 0.5g of p-benzoquinone into the reaction kettle, replace the air in the reaction kettle with hydrogen 5 times, react at a temperature of 100°C, a pressure of 1.5MPa, and a stirring speed of 900rpm, and react for 3h. After cooling to room temperature, take out The reaction solution was analyzed by gas chromatography: the conversion rate was 94.21%, and the selectivity was 70.22%.
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