应用化学
應用化學
응용화학
CHINESE JOURNAL OF APPLIED CHEMISTRY
2009年
10期
1169-1173
,共5页
罗智伟%顾辉子%周莉%严新焕
囉智偉%顧輝子%週莉%嚴新煥
라지위%고휘자%주리%엄신환
N-烷基化反应%原位液相加氢%氮烷基胺化合物
N-烷基化反應%原位液相加氫%氮烷基胺化閤物
N-완기화반응%원위액상가경%담완기알화합물
liquid-phase catalytic N-alkylation%in-situ liquid-phase hydrogenation%N-alkylated amine
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.
攷察瞭180 ℃下不同的胺與各類醇在Ni-Sn/Al_2O_3催化作用下的氮烷基化反應. 研究錶明,烷基化反應具有普遍的適用性,多數胺與甲醇、乙醇、正丁醇反應,具有較高的氮烷基化總產率. 一些胺與醇反應產率可達99%以上. 該催化劑還具有很高的穩定性,可保持活性達480 h以上. 對反應前後的催化劑進行瞭XRD和TEM錶徵,結閤錶徵結果對催化劑前期活性增加及後期活性下降給齣瞭初步分析.
고찰료180 ℃하불동적알여각류순재Ni-Sn/Al_2O_3최화작용하적담완기화반응. 연구표명,완기화반응구유보편적괄용성,다수알여갑순、을순、정정순반응,구유교고적담완기화총산솔. 일사알여순반응산솔가체99%이상. 해최화제환구유흔고적은정성,가보지활성체480 h이상. 대반응전후적최화제진행료XRD화TEM표정,결합표정결과대최화제전기활성증가급후기활성하강급출료초보분석.
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.