催化氧化合成δ-环戊内酯的工艺研究

Study on Catalytic Oxidation Synthesis Technology of δ-Valerolactone

以环戊酮为原料,质量分数为30%过氧化氢为氧化剂,Sn/W-2-600为催化剂,环己烷为带水剂,丙酸为溶剂,负压条件下合成了δ-环戊内酯。经减压蒸馏的方式对实验产物进行提纯,并经FT IR表征分析。通过单因素和正交试验对δ-环戊内酯的合成工艺进行优化。结果表明最优条件为:环戊酮0.025mol,Sn/W-2-600用量为环戊酮质量的40%,n(过氧化氢)∶n(环戊酮)=1.5,n(丙酸)∶n(环戊酮)=13.5,反应时间4.5h,真空度为0.07 MPa,带水剂环己烷15mL。在此条件下,δ-环戊内酯的收率为72.26%。

δ-Valerolactone was synthesized from cyclopentanone using,30% aqueous hydrogen peroxide solution as oxidant,propionic acid as solvent and the composite metal oxide Sn/W-2-600 as catalyst.During the process,cyclohexane was used as water carrying agent and the whole device was under negative pressure conditions.The product was purified by vacuum distillation and then characterized and analyzed by FT IR.Through single-factor and orthogonal experiments,the synthesis technology was optimized.The optimal condtions were as follows:n(cyclopentanone)=0.025mol;the amount of catalyst was 40%;n(H2O2)∶n(cyclopentanone)=1.5;n(propionic acid)∶n(cyclopentanone)=13.5;the reaction time was4.5h,and the vacuum pressure was 0.07 MPa.Under these conditions,the yield ofδ-valerolactone could reach 72.26%.