摘要:从合成的观点来看,烯烃的氧化是很重要的。本课题苯乙烯催化氧化合成环氧苯乙烷,它是重要的医药和香料中间体,可用做环氧树脂稀释剂、增香剂、稳定剂,广泛应用于苯乙醇、左旋眯唑等的制备。因此,研究苯乙烯催化氧化反应来制备环氧苯乙烷有重要意义。近年来,随着国内外环氧苯乙烷需求量的逐渐增加,开发环境友好的环氧苯乙烷的合成工艺是十分必要的。本课题以苯乙烯为原料,采用双氧水为绿色氧化剂,硫酸锰为催化剂,尿素为助剂,这样所形成的催化氧化体系不仅反应条件温和,而且原料的转化率高,环氧苯乙烷及其同分异构体苯乙醛的选择性也比较高。本课题通过二因素四水平的正交实验以及选择性单因素曲线,得出反应的最优条件为:n ( 苯乙烯) : n(H2O2) =1:2.0 ,n ( 苯乙烯) : n(尿素) =1:2.5,反应温度为10~20℃,反应时间为10小时,进气相色谱分析,测得转化率接近100%,选择性为95%。9470
关键词: 绿色氧化;苯乙烯;催化氧化;双氧水;环氧苯乙烷
Synthesis of styrene oxide
Abstract: From the synthetic point of view, the oxidation of alkenes is very important. This topic through the catalytic oxidation of styrene to prepare styrene oxide, which is an important intermediate of medicines and spices, available to synthesize Epoxy resin diluents, flavor agent, stabilizing agent, widely used in the preparation of Phenyl ethyl alcohol and Sigma L-blind. Therefore, the study of catalytic oxidation of styrene to prepare styrene oxide is very important. In recent years, it is a very necessary process to develop environmentally friendly synthesis of styrene oxide with increasing demand at home and abroad. The study used the styrene as the raw material, hydrogen peroxide as the green oxidant, the manganese sulfate as the catalyst, urea as the additive, in order to form by catalytic oxidation system. The system is not only a mild and steady reaction conditions with lower temperature, but the conversion of styrene is also high, almost up to 100 %, and the system has a positive effect on the selectivity of styrene oxide and its isomer phenyl acetaldehyde. This study was based on the four levels of the two factors of orthogonal experiments, as well as single-factor selective curve, the best reaction conditions obtained as follows: styrene / H2O2=1/2.0, styrene / urea=1/2.5,the reaction temperature is 10~20 ℃ (reflux temperature), the reaction time is 10 hours. After at least 5 hours’ reaction, then detected by the gas chromatography (GC), and measured the conversion rate approximate to 100% and its selectivity up to 95%.
Keywords: Green oxidation; styrene; catalytic oxidation; hydrogen peroxide; styrene oxide
目 录
1 绪论 6
1.1 合成香料的国、内外概况 6
1.2 绿色环保 7
1.2.1 绿色氧化 7
1.2.2 原子经济性 9
1.3苯乙烯简介及其市场概况 12
1.4环氧苯乙烷简介及研究现状 12
1.4.1环氧苯乙烷简介 12
1.4.2环氧苯乙烷的研究现状 13
1.5 工艺设计特点 15
1.6 本课题研究的目的意义 16
2 实验内容 17
2.1环氧苯乙烷的合成 17
2.1.1环氧苯乙烷合成路线的选择 17
2.1.2反应原理 17
2.2使用的材料试剂、仪器设备 18
2.2.1主要化学原料与试剂 18
2.2.2仪器设备 18
2.3实验操作 19
2.4 产品分析 20
3 实验结果与讨论 20
3.1 苯乙烯在不同条件下发生氧化反应的转化率 20
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