分子蒸馏、薄膜蒸发与精馏耦合技术用于分离苯乙酮和α-苯乙醇的研究  

Separation of Acetophenone and α-Phenylethanol by Molecular Distillation,Thin-film Evaporation Coupling Distillation Technology

作　　者：杨祖金[1,2] 张玉姣[3] 方岩雄[3] 纪红兵[4,2] 

机构地区：[1]中山大学化学工程与技术学院,广东广州510275 [2]中山大学惠州研究院,广东惠州516216 [3]广东工业大学轻工化工学院,广东广州510275 [4]中山大学化学与化学工程学院,广东广州510275

出　　处：《化学试剂》2016年第8期705-708,720,共5页Chemical Reagents

基　　金：国家自然科学基金资助项目(21376279;2127-6102;21425627);广东省热敏性精细化学品合成与分离工程研究中心项目(2015B090903061);广东省重大科技专项(2012A080103005);中央高校基本科研业务费(14lgpy28);广州市科技计划项目(2014J4100125)

摘　　要：苯乙酮是一种重要的有机化工原料,广泛地应用于食品、药品和化妆品等行业。工业上一般是以乙苯为原料、环烷酸锆为催化剂,通过空气氧化法合成苯乙酮,该反应容易生成α-苯乙醇等副产物。由于它们具有相似的物理化学性质,采用普通的蒸馏方法很难实现两种组分的分离。在前期研究的基础上,采用分子蒸馏、薄膜蒸发与精馏耦合技术对等质量混合的苯乙酮与α-苯乙醇混合物进行分离。首先对影响分离的因素如系统温度、压力和回流比对两种组分的得率和纯度的影响进行优化,分别得到轻、重两种组分。进一步对纯度高的苯乙酮混合物的分离工艺进行研究,通过优化系统温度、压力和回流比对混合物的分离进行研究。实验结果表明,经过两次分离后,苯乙酮的纯度从50%上升至99.12%,得率为80.23%。该研究为具有相近沸点的二元组分的分离提供了一定的参考。Acetophenone is an important organic chemical raw material,and widely used in the food,beverage and cosmetic industries. Commercially,it is produced from air oxidation of acetophenone by using zirconium naphthenate as a catalyst. It is a typic alsubstance for asymmetric transfer hydrogenation of ketones,with the by-product of chiral α-phenylethanol. The separation of them by regular distillation or crystallization is barely feasible due to the similar physical and chemical properties. In this work,a tripleintegration technology including molecular distillation,thin-film evaporation,and distillation was adopted to separate the mixtures of acetophenone and α-phenylethanol with quality ratio of 1∶ 1. The effects of various reaction variables e. g. temperature,pressure,and reflux ratio of the system on the separation efficiency have been investigated,and heavy-and light-fractions of the mixture were obtained,respectively. Light fractions were further separated to obtain high purity products with optimum conditions for separation of two components. The results indicated that the purity of acetophenone was increased from 50% to 99. 12% with the yield of 80. 23%. It is especially suitable for the separation of the two components with the similar boiling point.

关 键 词：苯乙酮 Α-苯乙醇 耦合技术 分离 

分 类 号：TQ65[化学工程—精细化工]