考察了180 ℃下不同的胺与各类醇在Ni-Sn/Al_2O_3催化作用下的氮烷基化反应. 研究表明,烷基化反应具有普遍的适用性,多数胺与甲醇、乙醇、正丁醇反应,具有较高的氮烷基化总产率. 一些胺与醇反应产率可达99%以上. 该催化剂还具有很高的稳定性,可保持活性达480 h以上. 对反应前后的催化剂进行了XRD和TEM表征,结合表征结果对催化剂前期活性增加及后期活性下降给出了初步分析.
A clean and efficient method has been developed for N-alkylation of amines catalyzed by Ni-Sn/Al_2O_3 with alcohol as the alkylation agent and solvent as well as hydrogen-donor. For all the reactions, the temperature was 180 ℃, the pressure was 1.5 MPa, and the flow rate was 1.0 mL/min. The structure of the catalyst was confirmed by X-ray diffraction(XRD) and transmission electron microscopy(TEM). The yields of N-alkylation amines were measured by gas chromatography(GC) while their structures were confirmed by gas chromatography-mass spectrometry(GC-MS). The results show that this catalyst has a great conjoint effect for all the reactions in in-situ hydrogenation for N-alkylation, including dehydrogenation of alcohol and hydrogenation of imine intermediates. The total yields of all the N-alkylation products were quite high, and some even greater than 99%. The catalyst had a long life of more than 480 h.
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