Phase-transfer catalyst for control of oxidizing reaction and oxidizing reaction procedure
A phase transfer catalyst and a technology to control phase transfer, applied in the direction of metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, chemical/physical process, etc., can solve difficult separation and recovery problems, achieve reaction The effect of mild conditions
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example 1
[0032] Below by example the present invention is given further description. Epoxidation of Example 1 Cyclohexene
[0033] 40mmol cyclohexene was dissolved in 40mL mixed mesitylene, 20mmol of 15% hydrogen peroxide aqueous solution (w / w) was added, 0.2mmol of catalyst [(C 2 h 5 ) 3 NCH 2 Ph] 2 HAsMo 2 o 10 . At 65°C, after reacting for 1 hour, the conversion rate of cyclohexene was 49.0%, and the selectivity of epoxycyclohexane was 95.2%. At this time, the catalyst was precipitated from the reaction system, and the catalyst was recovered after centrifugation and dried in vacuum. Unreacted raw material cyclohexene and product epoxycyclohexane in the organic layer were distilled off. Add the recovered epoxidation catalyst, cyclohexene and hydrogen peroxide to the obtained distillation bottom liquid, and perform the same circular reaction as above, and the reaction results are shown in the table below.
[0034] The recovered catalyst can be recycled for the above reaction...
example 2
[0054] The epoxidation of example 2 cyclohexene
[0055] Dissolve 20mmol of 2-menaphthoquinone in a mixed solvent of 15mL dimethyl phthalate and 15mL diisobutylmethanol, add 2% of 5% Pd / C (W / W) catalyst, 6atm hydrogen, 45°C The reaction was carried out for 6 hours to hydrogenate 2-menaphthoquinone up to 50%. The hydrogenation was stopped, and the Pd / C catalyst was removed by filtration. Then in the filtrate, add cyclohexene 30mmol, catalyst [--C 5 h 5 NC 4 h 9 ] 7 PV 4 o 16 0.09mmol at 1atm O 2 At 65° C. for 2 hours, the catalyst has been precipitated from the reaction system, the conversion rate of cyclohexene is 33.0%, and the selectivity of epoxycyclohexane is 98.3%. The catalyst was recovered by suction filtration, and the obtained catalyst was naturally dried in air at room temperature. Unreacted starting material cyclohexene and product cyclohexene oxide are distilled off. Add 2% Pd / C (W / W) catalyst to the resulting distillation bottom liquid, add the recover...
example 3
[0069] Epoxidation of Example 3 Propylene
[0070] 20mmol 2-tert-butylanthraquinone was dissolved in a mixed solvent composed of 15ml mesitylene and 15ml tributyl phosphate, under the catalyst of 0.125g 5% Pd / C, 45℃, 6atm H 2 Under hydrogenation reaction, when 10mmol 2-tert-butyl anthrahydroquinone is generated, the reaction is terminated. Remove Pd / C by filtration, and pass O to the mother liquor 2 Complete oxidation produces hydrogen peroxide and 2-tert-butylanthraquinone. The oxidizing solution was transferred into an autoclave with a glass liner, and 0.09 mmol[_-C was added 5 h 5 NC 12 h 25 ] 3 [PW 4 o 16 ] and charged with 60mmol propylene, and reacted for 4 hours at 50°C. The conversion of propylene to 2-tert-butylanthrahydroquinone was 90%, and the selectivity to propylene oxide was 95%. The catalyst separated out after the reaction is recovered by centrifugation and used for the next reaction. The unreacted propylene, propylene oxide and water in the reactio...
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