Method for producing acetovanillone and acetic acid by biomass directional catalysis
A vanilla ethyl ketone, biomass technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of complex catalyst preparation process, high substrate purity requirements, and high reactor cost, and achieve sustainable development. The effect of good performance, low equipment requirements and low reaction temperature
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Embodiment 1
[0019] Mix methanol and choline chloride according to the molar ratio of 1:1 to prepare alcohol ionic liquid, add alkali lignin at a concentration of 10% by mass, and according to the amount of alkali lignin, according to alkali lignin: copper salt: 1 , the mass ratio of 10-phenanthroline is 8:1:1 and copper acetate and 1,10-phenanthroline are added, and 0.4MPa of O is charged into the reactor. 2 , reacted at 60° C. for 3 h to obtain the product, the yield of vanillyl ethyl ketone was 46.09%, the yield of acetic acid was 40.62% (calculated based on the mass of alkali lignin), and the conversion rate of alkali lignin was 90%.
Embodiment 2
[0021] Mix methanol and choline chloride at a molar ratio of 4:1 to prepare an alcohol-based ionic liquid. According to the amount of lignin in the hydrothermally pretreated corn cob, add the hydrothermal pretreatment with a lignin concentration of 5% by mass. Corn cob (hydrothermal pretreatment method is based on the method reported in Cellulose, 24(11), 4899-4909), and the mass ratio of lignin: copper salt: 1,10-phenanthroline is 4:1:1. Copper acetate and 1,10-phenanthroline, and fill the reactor with 2MPa of O 2 , reacted at 80°C for 30 minutes to obtain the product, the yield of vanillyl ethyl ketone was 23.50%, the yield of acetic acid was 37.51% (calculated based on the quality of lignin), and the conversion rate of lignin in the hydrothermally pretreated corn cob was 65%. .
Embodiment 3
[0023] Methanol and choline chloride were mixed according to the molar ratio of 8:1 to prepare the alcohol ionic liquid, according to the amount of lignin in the untreated corn cob, the lignin concentration was 1% mass percent concentration, and the untreated corn cob was added, and Add copper acetate and 1,10-phenanthroline according to lignin: copper salt: 1,10-phenanthroline mass ratio of 1:1:1, and fill the reactor with 3MPa of O 2 , reacted at 100° C. for 1 h to obtain the product, the yield of vanillyl ethyl ketone was 27.91%, the yield of acetic acid was 21.49% (calculated based on the mass of lignin), and the conversion rate of lignin in untreated corn cob was 52%.
[0024] The foregoing examples prove that by using the alcohol ionic liquid system described above, different forms of lignin substrates are directly converted into vanillyl ethyl ketone and acetic acid, the reaction temperature is low, the time is short, and the purity of the target product is high; While ...
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