Institute for Technical Chemistry and Environmental Chemistry (ITUC), Friedrich Schiller University Jena, Jena, Germany.
ChemSusChem. 2011 Nov 18;4(11):1654-61. doi: 10.1002/cssc.201100154. Epub 2011 Aug 8.
The microwave-assisted hydrogenation of citral (3,7-dimethylocta-2,6-dienal) to citronellal with molecular hydrogen as the reducing agent was investigated. Several polar and non-polar solvents were screened and imidazolium-based ionic liquids were applied as modifiers for the palladium-containing porous glass catalysts (Pd/TP). The best results were obtained with N-ethyl-N'-methylimidazolium dicyanamide, N-ethyl-N'-methylimidazolium acetate, or N-ethyl-N'-methylimidazolium trifluoroacetate, which were used to prepare supported catalysts with an ionic liquid layer (SCILL) on Pd/TP by wet-impregnation. The influence of pressure and temperature when using these ionic liquid-containing catalysts, as well as their long-term stabilities, were examined. Working with microwave-assisted heating, high yields of citronellal were achieved under mild conditions within short reaction times. Catalyst characterization was carried out by means of BET measurements, X-ray photoelectron spectroscopy (XPS) and thermo-gravimetric analyses. The influences of the ionic liquid layer were derived from experiments carried out before and after the reactions.
研究了以分子氢为还原剂,用微波辅助氢化为柠檬醛(3,7-二甲基辛-2,6-二烯醛)制备香茅醛。筛选了几种极性和非极性溶剂,并将咪唑鎓基离子液体用作含钯多孔玻璃催化剂(Pd/TP)的改性剂。用N-乙基-N'-甲基咪唑二氰胺、N-乙基-N'-甲基咪唑乙酸盐或 N-乙基-N'-甲基咪唑三氟乙酸盐得到了最佳结果,它们通过湿浸渍法用于在 Pd/TP 上制备具有离子液体层(SCILL)的负载型催化剂。考察了使用这些含离子液体的催化剂时压力和温度的影响以及它们的长期稳定性。在微波辅助加热下,在温和的条件下,在短的反应时间内,以高收率获得了香茅醛。通过 BET 测量、X 射线光电子能谱(XPS)和热重分析对催化剂进行了表征。从反应前后进行的实验中得出了离子液体层的影响。