盐酸三乙胺离子液体催化苯和环己烯合成环己基苯

发布时间：2018-04-04 20:33

  本文选题：烷基化反应　切入点：离子液体　出处：《郑州大学》2016年硕士论文

【摘要】：环己基苯(cyclohexylbenzene,CHB),又称为苯基环己烷,是一种重要的化工中间体,也是一种高沸点溶剂。主要用来做锂电池添加剂、制备苯酚和环己酮,也可作为合成液晶材料的原料等,具有十分广泛的应用。目前,环己基苯的售价为每吨12万元左右,因此研究环己基苯的合成工艺,获得高收率、高纯度的环己基苯,具有十分可观的经济价值。盐酸三乙胺-三氯化铝离子液体是烷基化反应常用的催化剂之一。在氮气保护下,分别采用正交试验和单因素试验方法,产物使用内标法进行气相分析。以离子液体连续使用两次得到的环己基苯的平均收率为指标,分别考察氯化铝与盐酸三乙胺的摩尔比、反应温度、反应时间对离子液体催化性能的影响。通过一步法,经过冰水浴和温水浴,最终得到盐酸三乙胺-三氯化铝离子液体的较优合成工艺条件。以苯和环己烯为原料,在得到的离子液体工艺条件基础上,对合成环己基苯的工艺条件进行优化,考察了离子液体用量、反应时间、反应温度、苯烯比对环己基苯收率的影响,最终得到纯度大于99.5%,平均收率为88.09%的环己基苯产品。在环己基苯合成工艺基础上,对离子液体进行循环使用,考察了静置时间对离子液体循环使用性能的影响,确定了离子液较佳静置时间为2.5~3 h,离子液体可以循环使用四次并保持较高的活性。并考察了三氯化铝量对再生离子液体性能的影响,结果表明当加入初始量50%的三氯化铝时,离子液体可以使用三次并保持较高的活性。通过红外光谱仪,热重分析仪,金属离子与EDTA络合的方法三种分析方法研究了离子液体失活的原因,并确定有机相带走离子液体是离子液体失活的原因之一。
[Abstract]:Cyclohexylbenzeneurane, also known as phenylcyclohexane, is an important chemical intermediate and a high boiling point solvent.It is mainly used as additive for lithium battery to prepare phenol and cyclohexanone, and can also be used as raw material for synthesizing liquid crystal.At present, the price of cyclohexylbenzene is about 120000 yuan per ton, so it is of great economic value to study the synthetic process of cyclohexylbenzene to obtain high yield and high purity cyclohexylbenzene.Triethylamine hydrochloride-aluminum chloride ionic liquid is one of the commonly used catalysts for alkylation.Under the protection of nitrogen, orthogonal test and single factor test were used, and the products were analyzed by internal standard method.The effects of molar ratio of aluminum chloride and triethylamine hydrochloride, reaction temperature and reaction time on the catalytic performance of ionic liquid were investigated with the average yield of cyclohexylbenzene obtained by continuous use of ionic liquid as the index.The optimum synthetic conditions of triethylamine hydrochloride and aluminum chloride ionic liquid were obtained by one step method through ice bath and warm water bath.The synthesis of cyclohexylbenzene was optimized by using benzene and cyclohexene as raw materials. The effects of the amount of ionic liquid, reaction time, reaction temperature and the ratio of benzene to alkene on the yield of cyclohexylbenzene were investigated.The purity of cyclohexylbenzene was higher than 99.5, and the average yield was 88.09%.Based on the synthesis process of cyclohexylbenzene, ionic liquids were reused and the influence of statics time on the recycling performance of ionic liquids was investigated.It was determined that the optimal time of the ionic liquid was 2.5 鈩，

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