双丙酮丙烯酰胺的合成及提取工艺的优化

OPTIMIZATION OF PARAMETERS INOLVED IN THE SYNTHESIS AND PURIFYING OF DIACETONE ACRYLAMIDE

用正交实验设计法对双丙酮丙烯酰胺合成过程的工艺条件进行了优化 ,较优条件为 :n (丙酮 )∶ n (丙烯腈 )∶ n (浓硫酸 ) =2 .4∶ 1∶ 1 .1 ,反应温度 50℃ ,反应时间 4 h。对产品的提取工艺进行了改进 :将反应液在减压蒸馏前用水萃取 ,盐析 ,碱洗 ,除去大部分杂质。碱洗所用的 1 5%氢氧化钠溶液∶有机层 (质量比 ) =2∶ 1 0。产物经减压蒸馏后无需重结晶 ,收率 54.5% ,熔点 53～ 56℃。

The orthoganal experimental method was used in optimizing the technical parameters involved in the synthesis of diacetone acrylamide (DAAM), the optimum reaction conditions were as following: n(acetone)∶n(acrylonitrile)∶n(sulfuricacid)=2.4∶1∶1, the reaction temperature 50 ℃, the reaction time 4 h. The product extraction process was improved: the reaction mixture was extracted by water, salted out, and then washed by 15% NaOH solution to remove most impurity. The mass ratio of the 15% NaOH solution to organic layer was 2∶10. The product was distilled under vacuum, then no need recrystallization, the yield of DAAM with melting point of 53～56 ℃ was 54.4%.