Ionic liquid catalytic deoxygenation method in a lignin derivative hydrodeoxygenation process
An ionic liquid, hydrodeoxygenation technology, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as restricting applications, and achieve the advantages of overcoming high pressure problems, easy separation, and avoiding side reactions. Effect
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Embodiment 1
[0026] Ionic liquid synthesis: equimolar amounts of alkanolamine (5mol) and trifluoromethanesulfonic acid (5mol) were added to a round bottom flask and a constant pressure titration funnel, respectively, and 500 mL of methanol was added to the round bottom flask as a reaction solvent. Under the condition of ice water temperature, trifluoromethanesulfonic acid was slowly added dropwise to the methanol solution of alcoholamine. After the dropwise addition was completed, the reaction system was warmed up to room temperature (25°C) and reacted for 24 hours to remove methanol to obtain the target ion liquid.
[0027] The ionic liquids used in the following cases were all synthesized by the above method.
[0028] 1mmol phenol, 0.1g Rh / C (water content 55-60%) catalyst, 2g N-methyldiethanolamine trifluoromethanesulfonate ([BHEM][OTf]) ionic liquid, 1mmol n-dodecane and Magnets are added to a stainless steel autoclave with a Teflon liner and tightly sealed. Then use high-purity hydr...
Embodiment 2
[0030] 1mmol cyclohexanol, 0.1g Pt / C (water content≤80%) catalyst, 2g N-methyldiethanolamine trifluoromethanesulfonate [BHEM][OTf] ionic liquid, 1mmol n-dodecane and magnetic Pour into a stainless steel autoclave lined with polytetrafluoroethylene, and seal it tightly. Then use high-purity hydrogen to pump and vent the reactor three times to blow out the air in the reactor, and inject 4MPa hydrogen into the reactor after the last ventilation. Put the reaction kettle into the high-pressure reaction furnace, wait until the temperature is heated to the set temperature of 120°C, turn on the magnetic stirring and set the magnetic stirring speed to 550 rpm, and start timing. After reacting for 2 hours, the reaction kettle was put into ice water for cooling. After complete cooling, slowly release the remaining high-pressure hydrogen in the reactor, and blow the hydrogen in the reactor with nitrogen, then open the reactor, and extract the reaction product with 8ml of methyl tert-buty...
Embodiment 3
[0032]1mmol phenol, 0.1g Rh / C (water content 55-60%) catalyst, 2g N,N-dimethylethanolamine trifluoromethanesulfonate ([2-HTEAF][OTf]) ionic liquid, 0.1910g Add n-dodecane and magnetons into a stainless steel autoclave with a polytetrafluoroethylene liner, and tighten the seal. Then use high-purity hydrogen to pump and vent the reactor three times to blow out the air in the reactor, and inject 4MPa hydrogen into the reactor after the last ventilation. Put the reaction kettle into the high-pressure reaction furnace, wait until the temperature is heated to the set temperature of 120°C, turn on the magnetic stirring and set the magnetic stirring speed to 550 rpm, and start timing. After reacting for 10 hours, the reaction kettle was put into ice water for cooling. After complete cooling, slowly release the remaining high-pressure hydrogen in the reactor, and blow the hydrogen in the reactor with nitrogen, then open the reactor, and extract the reaction product with 8ml of methyl ...
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