摘要
研究了固体超强酸催化合成乙酸橙花酯和乙酸香叶酯 ,寻找能替代浓硫酸的新型高效催化剂 ,并对不同催化剂、催化剂用量、反应时间、不同带水剂及带水剂用量等因素对体系的影响作了较详细的探讨。结果发现 ,催化剂的催化效果由强到弱的顺序为 :Fe2 O3 SO4 2 ->ZrO2 SO4 2 ->磷钨酸 >磷钼酸 >对甲苯磺酸 >浓硫酸 ;带水剂能明显提高酯化收率 ,在苯、甲苯、二甲苯 3种带水剂中 ,以甲苯最好 ;优化的反应条件为 :乙酸 7.8g (0 .130 0mol) ,橙花醇香叶醇 15 4g(0 10 0 0mol) ,催化剂Fe2 O3 SO4 2 -0 5g (0 0 0 19mol) ,带水剂甲苯 2 0mL ,反应温度为回流温度 ,反应时间 4h ,酯化收率可达 95 44 %
Solid superacid was used as catalyst for the preparation of neryl acetate and geranyl acetate by esterification. The descending order of activity ratings of catalysts was: Fe2O3-SO42- > ZrO2-SO42- > phosphotungstic acid > phosphomolybdic acid > p-CH3(C6H4)SO3H > H2SO4. Suitable conditions were investigated, such as kind and amount of catalyst, reaction time and kind and amount of water-carrying reagent. Use of water-carrying reagent could enhance the esterification rate. Toluene was the best water-carrying reagent among benzene, toluene and xylene. The yield of esterification achieved 95.4% with acetic acid 7.8 g (1.3000 mol), nerol and geraniol 15.4 g (0.1000 mol), Fe2O3-SO42- 0.5 g (0.0019 mol) and toluene 20 mL reacting at reflux temperature for 4 h.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2001年第11期641-644,共4页
Fine Chemicals
