叔丁基过氧化氢环氧化合成环氧环己烷工艺研究

合成了钼 (Ⅵ )络合物———钼 (Ⅵ )合乙酰丙酮 ,并用元素分析和红外光谱技术对其进行了表征。合成并纯化了叔丁基过氧化氢 (t BuOOH) ,以此为环氧化剂 ,以钼 (Ⅵ )合乙酰丙酮为催化剂 ,研究了反应物料配比、溶剂和催化剂用量、反应温度、时间等因素对合成过程的影响 ,提出了钼 (Ⅵ )合乙酰丙酮催化环己烯、叔丁基过氧化氢合成环氧环己烷反应的机理。采用正交实验技术 ,优化出了较佳合成工艺条件 ,即n()∶n(t BuOOH) =3 5∶1 0 ,以n(t BuOOH) =0 1mol计 ,溶剂 10mL ,钼 (Ⅵ )合乙酰丙酮 0 1g ,反应温度 80℃ ,反应时间 6 0min。以t BuOOH计 ,环氧环己烷收率 99 5 % ,质量分数 99 9% (GC分析 )

Study of Process for Synthesis of Epoxycyclohexane with t-Butyl Hydroperoxide as Oxidant

A molybdenum(Ⅵ)complex,namely molybdenum dioxobis(2,4 pentanedione) MoO 2(acac) 2] ,to be used as epoxidation catalyst was synthesized.It was characterized by elementary analysis and infrared spectrum technique. t Butyl hydroperoxide ( t BuOOH) to be used as epoxidation agent was also synthesized.Under the protection of nitrogen,process of synthesizing epoxycyclohexane by reaction of cyclohexene and t BuOOH using MoO 2(acac) 2 as catalyst was investigated.Possible mechanism of the epoxidation reaction by MoO 2(acac) 2 catalysis was described.Effects of mole ratio of cyclohexene to t BuOOH and amounts of catalyst,solvent etc.on reaction yield were studied by orthogonal experiment design.The optimum reaction conditions were obtained,that is,according to n(t BuOOH) = 0 1 mol, n ()∶ n(t BuOOH)=3 5∶1 0,volume of solvent is about 10 mL,reaction temperature is about 80 ℃,and reaction time is about 60 min.Under these conditions,the yield of epoxycyclohexane based on the amount of t BuOOH is over 99 5%,and purity of epoxycyclohexane is about 99 9% by GC analysis.