脱氢芳樟醇催化合成柠檬醛  

Catalytic Synthesis of Citral from Dehydrolinalool

作　　者：曹正芳[1] 浦伟光[1] 赵平[2] 

机构地区：[1]华东理工大学化工学院,上海200237 [2]华东理工大学化学与分子工程学院,上海200237

出　　处：《石油化工》2008年第4期364-367,共4页Petrochemical Technology

摘　　要：以钛酸正丁酯为主催化剂、氯化亚铜为助催化剂,氮气保护下,在酸性溶液中,对脱氢芳樟醇催化反应制取柠檬醛的过程进行了探索和研究;考察了助催化剂类型和用量、总催化剂用量、反应温度、反应时间、酸的类型及加入量等因素对脱氢芳樟醇转化率和柠檬醛收率的影响。实验结果表明,最佳的反应条件为:以氯化亚铜为助催化剂,对甲基苯甲酸为酸性溶液,m(钛酸正丁酯):m(氯化亚铜)=7:1,m(钛酸正丁酯+氯化亚铜):m(对甲基苯甲酸):m(脱氢芳樟醇)=4:9:100,反应时间90min,反应温度130℃。在此条件下,脱氢芳樟醇的转化率为97.2%,柠檬醛的收率为89.1%。该工艺反应条件温和、反应时间短、操作简便、单耗低、合成的柠檬醛收率高。Citral was synthesized from dehydrolinalool through internal rearrangement with butyl titanate as main catalyst and cuprous chloride as cocatalyst in 4-methylbenzoic acid solution and atmosphere of nitrogen. Product citral was characterized by gas chromatograph-mass spectrometer and its purity was measured by gas chromatograph. Effects of cocatalyst type and dosage, total catalyst dosage, reaction time, reaction temperature, acid type and dosage on conversion of dehydrolinalool and yield to citral were investigated. Optimized conditions are： m （butyl titanate ） ： m （cuprous chloride） 7 ： 1, m （butyl titanate ＋ cuprous chloride ） ： m （4-methylbenzoic acid） ： m （dehydrolinalool） 4：9： 100, reaction time 90 min and reaction temperature 130 ℃. Under optimized condition, conversion of dehydrolinalool is 97.2% and yield to citral is 89.1%. The process features mild conditions, short reaction time and facile operation.

关 键 词：脱氢芳樟醇 柠檬醛 钛酸正丁酯 氯化亚铜 对甲基苯甲酸 合成 催化剂 

分 类 号：TQ032.4[化学工程]