CAJ | 학술논문

以廉价的烷基胺为原料合成了SO_3H-功能化离子液体(IL),并采用NMR、ESI-MS、TG-DTG等手段对其结构及物性进行表征.将该离子液体作为催化剂,考察反应条件对离子液体催化邻苯二酚叔丁醇(TBA)烷基化反应性能的影响,以及离子液体的重复使用性,比较了离子液体与常规酸催化剂催化该烷基化反应性能的差别.结果表明,在反应温度150℃、反应时间3 h、n(邻苯二酚):n(TBA):n(IL)为2:1:0.1的优化条件下,邻苯二酚的转化率、4-叔丁基邻苯二酚(4-TBC)的选择性分别可达41.5%和97.1%,与液体酸的催化效果接近.根据实验结果和模拟计算推测了可能的反应机理.
이렴개적완기알위원료합성료SO_3H-공능화리자액체(IL),병채용NMR、ESI-MS、TG-DTG등수단대기결구급물성진행표정.장해리자액체작위최화제,고찰반응조건대리자액체최화린분이분숙정순(TBA)완기화반응성능적영향,이급리자액체적중복사용성,비교료리자액체여상규산최화제최화해완기화반응성능적차별.결과표명,재반응온도150℃、반응시간3 h、n(린분이분):n(TBA):n(IL)위2:1:0.1적우화조건하,린분이분적전화솔、4-숙정기린분이분(4-TBC)적선택성분별가체41.5%화97.1%,여액체산적최화효과접근.근거실험결과화모의계산추측료가능적반응궤리.
SO_3H-functionalized ionic liquids (IL) were synthesized by using tri-alkylamine and 1,4-butanesultone as the sources. The structures and physical properties of ILs were characterized by NMR, ESI-MS and TG-DTG. Their catalytic performances in the alkylation of catechol with tert-butyl alcohol (TBA) were investigated. The influences of reaction temperature, reaction time, reactant ratio, the amount and the recycle times of IL on the catalytic performance of IL in the tert-butylation of catechol were studied. Meanwhile, the catalytic performance of IL was compared with that of conventional liquid acids and solid acids. The results indicated that under optimized reaction conditions of 150℃, 3 h, n(Catechol) : n(TBA) : n(IL) was 2 : 1 :0.1, the conversion of catechol and the selectivity of 4-TBC were 41.5% and 97.1% respectively. The SO_3 H-functionlized ionic liquid exhibited high catalytic activity in the alkylation of catechol with TBA, which wassimilar to liquid acid. The possible mechanism for this reaction system was discussed based on thereaction results and the simulation calculated results.