Method for preparing 3,3,5-trimethyl-cyclohexanone by selectively hydrogenating isophorone
A technology of trimethylcyclohexanone and isophorone, which is applied in the field of preparation of 3,3,5-trimethylcyclohexanone, can solve problems such as unsatisfactory effect, high cost, and difficulty in product separation
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Embodiment 1
[0022] This example shows that using isophorone as a raw material, the reaction temperature is 100°C, no solvent is added, the reaction time is 4 hours, and a supported 5% Pd / activated carbon catalyst is used (5%Pd / AC catalyst, the mass fraction is 5 % of metal Pd supported on activated carbon), compared the method of hydrogenation of isophorone to 3,3,5-trimethylcyclohydrogenation without adding co-catalyst and adding co-catalyst (mass ratio of 1:1 to Pd) The effect of hexanone.
[0023] Experiment without adding co-catalyst: Take 0.67 g of isophorone and 60 mg of palladium-carbon catalyst (5%Pd / AC) in a 25 mL high-temperature and high-pressure reactor, without adding co-catalyst, and replace the reactor with hydrogen The air in it is finally filled with hydrogen with an initial pressure of 2.0 MPa. Put the reaction kettle into the heating furnace, turn on the stirring, when the temperature rises to 100°C, the stopwatch starts timing, stop stirring after 4 hours, immediately...
Embodiment 2
[0029]This example illustrates the process of using isophorone as the raw material, the mass ratio of co-catalyst and supported Pd catalyst in the reaction material is 1.33:1, the reaction temperature is 100°C, no solvent is added, and the reaction time is 4 hours.
[0030] Take 0.67 g of isophorone, 60 mg of palladium carbon catalyst (5% Pd / AC catalyst, 5% metal Pd supported on activated carbon), and 80 mg of zinc chloride in a 25 mL high-temperature and high-pressure reactor, Charge hydrogen to replace the air in the reactor, and finally charge hydrogen with an initial pressure of 2.0 MPa. Put the reaction kettle into the heating furnace, turn on the stirring, when the temperature rises to 100°C, the stopwatch starts timing, stop stirring after 4 hours, immediately take out the reaction kettle and put it in a cold water bath to terminate the reaction. After the reaction kettle was cooled, it was diluted with dichloromethane and taken out.
[0031] After the reaction product...
Embodiment 3
[0033] This embodiment illustrates that with isophorone as a raw material, the reaction temperature is 90 ° C, and dichloromethane is used as a solvent, and the reaction time is 4 hours. The mass ratio of the co-catalyst and the loaded Pd catalyst is not added in the co-catalyst or reaction mass. 1:1.1 process method.
[0034] Experiment without adding co-catalyst: 0.67 g of isophorone, 66 mg of palladium carbon catalyst (5% Pd / AC catalyst, 5% metal Pd supported on activated carbon by mass fraction) and about 5 ml of solvent dichloromethane in In the 25 mL high-temperature and high-pressure reactor, hydrogen was filled to replace the air in the reactor, and finally hydrogen with an initial pressure of 2.0 MPa was filled. Put the reaction kettle into the heating furnace, turn on the stirring, when the temperature rises to 90°C, the stopwatch starts timing, stop stirring after 4 hours, immediately take out the reaction kettle and put it in a cold water bath to terminate the reac...
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