發(fā)布時(shí)間：2018-04-04 20:33

  本文選題：烷基化反應(yīng)　切入點(diǎn)：離子液體　出處：《鄭州大學(xué)》2016年碩士論文

【摘要】：環(huán)己基苯(cyclohexylbenzene,CHB),又稱為苯基環(huán)己烷,是一種重要的化工中間體,也是一種高沸點(diǎn)溶劑。主要用來做鋰電池添加劑、制備苯酚和環(huán)己酮,也可作為合成液晶材料的原料等,具有十分廣泛的應(yīng)用。目前,環(huán)己基苯的售價(jià)為每噸12萬元左右,因此研究環(huán)己基苯的合成工藝,獲得高收率、高純度的環(huán)己基苯,具有十分可觀的經(jīng)濟(jì)價(jià)值。鹽酸三乙胺-三氯化鋁離子液體是烷基化反應(yīng)常用的催化劑之一。在氮?dú)獗Ｗo(hù)下,分別采用正交試驗(yàn)和單因素試驗(yàn)方法,產(chǎn)物使用內(nèi)標(biāo)法進(jìn)行氣相分析。以離子液體連續(xù)使用兩次得到的環(huán)己基苯的平均收率為指標(biāo),分別考察氯化鋁與鹽酸三乙胺的摩爾比、反應(yīng)溫度、反應(yīng)時(shí)間對(duì)離子液體催化性能的影響。通過一步法,經(jīng)過冰水浴和溫水浴,最終得到鹽酸三乙胺-三氯化鋁離子液體的較優(yōu)合成工藝條件。以苯和環(huán)己烯為原料,在得到的離子液體工藝條件基礎(chǔ)上,對(duì)合成環(huán)己基苯的工藝條件進(jìn)行優(yōu)化,考察了離子液體用量、反應(yīng)時(shí)間、反應(yīng)溫度、苯烯比對(duì)環(huán)己基苯收率的影響,最終得到純度大于99.5%,平均收率為88.09%的環(huán)己基苯產(chǎn)品。在環(huán)己基苯合成工藝基礎(chǔ)上,對(duì)離子液體進(jìn)行循環(huán)使用,考察了靜置時(shí)間對(duì)離子液體循環(huán)使用性能的影響,確定了離子液較佳靜置時(shí)間為2.5~3 h,離子液體可以循環(huán)使用四次并保持較高的活性。并考察了三氯化鋁量對(duì)再生離子液體性能的影響,結(jié)果表明當(dāng)加入初始量50%的三氯化鋁時(shí),離子液體可以使用三次并保持較高的活性。通過紅外光譜儀,熱重分析儀,金屬離子與EDTA絡(luò)合的方法三種分析方法研究了離子液體失活的原因,并確定有機(jī)相帶走離子液體是離子液體失活的原因之一。
[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，

本文編號(hào)：1711577