摘要
以脱氢芳樟醇水蒸气蒸馏残液为原料,反应压力为常压,反应温度为103~142℃,残液中的二聚脱氢芳樟醇和脱氢芳樟醇在浓KOH或NaOH水溶液催化作用下进行分解反应,生成6-甲基-5-庚烯-2-酮和乙炔。考察了碱浓度、温度、油碱质量比对残液分解反应的影响,提出了反应历程。以w(KOH)=50%的水溶液为催化剂,反应温度124~127℃,残液与碱液质量比15∶1,残液中的二聚脱氢芳樟醇、脱氢芳樟醇质量分数分别为60.1%、33.6%,搅拌速度100~200 r/min,反应5 h,脱氢芳樟醇水蒸气蒸馏残液分解生成6-甲基-5-庚烯-2-酮的反应收率为94.3%,反应液中的6-甲基-5-庚烯-2-酮质量分数为92.1%。
2,6,9, 13-Tetramethyl-2, 12-tetradecadien-7-yne-6,9-diol ( Ⅰ ), dimer of dehydrolinalool ( Ⅱ ), exists in the residuum formed in the stripping process of dehydrolinalool. Both Ⅰ and Ⅱ can be converted into 6-methyl-5-hepten-2-one and C2H2 in the presence of concentrated solution of KOH or NaOH at 103 - 142 ℃ under atomspheric pressure. When the reaction proceeded at 122 - 127 ℃ for 5 h with the residuum (containing 60. 1% of Ⅰ and 33.6% of Ⅱ ) and 50% KOH solution in weight ratio 15:1, the yield and purity of 6-methyl-5-hepten-2-one were 94.3% and 92. 1%, respectively. Mechanism of the reaction is discussed.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2008年第6期606-609,共4页
Fine Chemicals