Study On The Synthesis Process Of Ethyl Acetate By Catalytic Distillation

As an important kind of organic dissolvent and chemical raw stuff, ethyl acetate is wildly used in industries such as organic synthesis, paint, coating, medicine, aromatics and binder etc. At present, ethyl acetate is mainly produced by a traditional technology in our country, which ethyl acetate is directly synthesized by acetate acid and alcohol with concentrated sulfuric acid as catalyst. There are still some existing disadvantages though it is a mature technology: on one hand, concentrated sulfuric acid has so strong corrosion that many side reactions occurred on the equipment such as dehydrolysis , etherification, carbonization etc. It will affect product quality and feedstock yield. On the other hand, for the traditional production technology is restricted by balance, the one-way conversion of material is low.Synthesis of ethyl acetate by catalytic distillation is investigated in this paper. D072 Strong-acidic cation exchange-resin is chosen to synthesis ethyl acetate for is good catalytic properties. On the purpose of synthesis kinetics of ethyl acetate, D072 Strong-acidic cation exchange-resin is adopted. After the influence of internal and external diffusion is eliminated, some parameters can be obtained as follow: the quantity of catalyst is between 0.017～0.083g _(catalyst)·g^-1_{(acetic add)},the temperature is between 53.0℃～74.0℃,The kinetics equation of ethyl acetate system is :Meantime , the equations of kinetics are proved having good rightness and high confidence level of 98%. These provide a theoretical principle for design of catalytic distillation tower. D072 Strong-acidic cation exchange-resin is characterized using specific surface area analyzer, IR, XRD et al. preliminary study on the reasons of increase and decrease of catalytic activity for the catalyst of the catalyst are also taken into consideration.In this paper, the strong-acidic cation exchange-resin powder is developed on the basis of the original catalytic distillation technology. The mode of catalyst entering is changed. The fine catalyst particles mix with liquid phase through flowing down in the column, that is fluidizing catalytic distillation. In the system of air-water, the hydrodynamics of packing column are studied on the presence of the catalyst powder. The results show that the catalyst powder has no noticeable impact to the pressure drop and the liquid holdup of the packing column. The strong-acid cation change-resin powder mixed with acatic acid flows down in the column and recycles between the catalytic distillation column and catalyst recovery. The fluidizing catalytic distillation process is experimentally studied on the esterification of acetate acid by alcohol. The experiments are carried out in a glass column with an inner diameter of 30mm and the catalyst is strong-acidic cation exchange-resin powder. The effects of catalyst concentration, reflux ratio, feed mole ratio of acetate acid to alcohol and total feed flow on the process are experimentally investigated. Based on the analysis, the experiment results indicate that: the feasible technological conditions of ethyl acetate synthesis are inlet amount of acetate acid is 2.8mol·h^-1 in Y₂, alcohol is 1mol·h^-1 in Y₂, total amount is 3.8mol·h^-1, acid/alcohol mole ratio of 2.8:1.0 and reflux ratio of 3.0:1.0, the catalyst concentration is 0.033 g_(catalyst)·g^-1_{(acetic acid)}, The composition of tower top organic phase are ethyl acetate 90.60%, acid 0.028%, alcohol 2.90% and water 6.47%. The product of tower top rectify in the distillation tower distilled in the distillation column directly, the product of athyl acetate can be obtained, the content of ethyl acetate is up to 99%. The technological parameters obtained from experiments afford a good foundation for engineering development of synthesis of ethyl acetate by catalytic distillation.