PDF全文下载：2011050446
吴现印， 吕志果*， 张伟伟（青岛科技大学 化工学院，山东 青岛 266042）
摘要： 研究了乙醛酸和异丁醛（IBD）在胺类催化剂作用下羟醛缩合及其缩合产物在纳米铜基催化剂上一步加氢脱水环化制备α-羟基-β, β-二甲基-γ-丁内酯的绿色合成新工艺。结果表明：在物料配比n(乙醛酸) ∶n(异丁醛) ∶n(三乙胺)为1∶1∶1.2，缩合温度60 ℃、反应时间2 h的条件下羟醛缩合，IBD的转化率大于95%；将缩合产物采用负载于硅胶上的纳米铜基催化剂在120 ℃、n(H2)∶n(IBD)＝80∶1，氢气压力8.0 MPa 、液空速0.6～1.0 h-1的条件下连续固定床加氢、环化脱水，减压蒸馏（真空度0.096 MPa），收集110 ~120 ℃馏分，DL-泛内酯的收率大于90%，产品纯度达到99.65%。
关键词： DL-泛内酯； 催化加氢； 乙醛酸； 铜基催化剂
中图分类号： TQ 463.26文献标志码： A
New Technology for Green Synthesis
of α-Hydroxy-β,β-dimethyl-γ-butyrolactone
WU Xian-yin, L Zhi-guo, ZHANG Wei-wei
(College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China)
Abstract: The new synthesis process of DL-pantolactone was researched, which employed glyoxalic acid and iso-butyraldehyde (IBD) as raw materials. The process included aldol condensation，catalytic hydrogenation of aldol condensate and dehydration-cyclization under nano copper-based catalyst in the fixed bed reactor. The results showed that the conservation of IBD was more than 95% under the following conditions in aldol condensation: reaction temperature 60 ℃, n (glyoxalic acid) ∶ n (IBD) ∶n (TEA) = 1∶1∶1.2 and reaction time 2 h. Under the conditions of reaction temperature 120 ℃, n (H2) ∶ n (IBD) = 80∶1, H2 pressure 8.0 MPa, liquid airspeed 0.6 ~ 1.0 h -1, and vacuum distillation (the vacuity was 0.096 MPa), the yield of DL-pantolactone was 90%, meanwhile the purity of the product reached 99.65%.
Key words: DL-pantolactone; catalytic hydrogenation; glyoxylic acid; copper-based catalyst
收稿日期：2011-01-15
作者简介： 吴现印（1984—），男，硕士研究生.*通信联系人.
