Synthesis Of Ethyl And Butyl Acetate By Catalytic Distillation

Acetate is an important kind of organic dissolvent and chemical raw stuff. It is wildly used in such industries as organic synthesis, paint, coating, medicine, aromatics and binder etc. At present, acetate is mainly produced by a traditional technology in our country, in which acetate is directly synthesized by acid and alcohol with concentrated sulfuric acid as catalyst in China. Although this technology is a mature one having high reactive rate, it exists many disadvantages. One hand, concentrated sulfuric acid has so strong corrosion to equipment, even serious in producing process of high boiling point acetate system. On the other hand, there are many side reactions such as dehydrolysis, etherification, carbonization etc. which will affect product quality and feedstock yield.Synthesis of ethyl acetate and butyl acetate by catalytic distillation was investigated in this paper. A new and high efficient type catalyst, cation exchange membrane, was developed and the activation conditions were investigated. Activated catalyst was used in kinetics of synthesis of ethyl acetate and butyl acetate. The kinetics equation of ethyl acetate system was obtained asThe kinetics equation of buty acetate system was obtained asAlso, the equations of kinetics were proved having good rightness and high confidence level of 98%. These provide a theoretical principle for design of catalytic distillation tower. Intermittent reactions of ethyl acetate and butyl acetate synthesis were studied without separating products from system using activated catalyst. The feasible conditions of ethyl acetate synthesis are acid/alcohol ratio in 1:1, Cat./acid ratio in 10%, reacting in boiling and reactive time in 140min, and then the conversion rate is 63.4%. Similarly the feasible conditions of butyl acetate synthesis are acid/alcohol ratio in 1:1, Cat./acid ratio in 20%, reacting in boiling and reactive time in 140min, and the conversion rate is 59.1%.A new type of catalytic packings which are propitious to catalytic distillation technology was developed using pretreated catalyst. The catalytic packings have little resistance and are easy to assemble. Meanwhile a new catalytic distillation technology for synthesis of ethyl and butyl acetate was developed. This type of catalytic packings were fixed in a 30mm column to synthesis acetate. In this catalytic distillation column, the feasible technological conditions of ethyl acetate synthesis are inlet amount in 1mol/h, acid/alcohol mole ratio of 2.5:1 and reflux ratio of 3:1. The compose of tower top organic phase is ethyl acetate 89.21%, acid 0.057%, ethanol 5.15% and water 5.61%. The feasible technological conditions of buty acetate synthesis areinlet amount in 1.5mol/h, acid/alcohol mole ratio of 3:1 and reflux ratio of 2:1. And the compose of tower top organic phase is butyl acetate 93.81%, acid 0.05%, butyl alcohol 4.10% and water 2.01%. So far, this type of catalytic packings and esterification technology have not been found in reports. The technological parameters that were obtained from experiments afford a good foundation for engineering development of synthesis of ethyl acetate and butyl acetate by catalytic distillation.