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Method for synthesizing mixed ester through catalyst distillation

A catalytic distillation and mixed ester technology, which is applied in the field of catalytic distillation to synthesize mixed esters, catalytic distillation to simultaneously synthesize ethyl acetate and butyl acetate, and can solve the problem that the specifications and performance of catalyst components are difficult to process into a consistent type, catalyst amount, and filler performance It is difficult to unify with the porosity in the tower, and the advantages of catalytic distillation technology cannot be well utilized, so as to achieve the effects of reducing energy consumption, simple regeneration operation, and reduced difficulty

Inactive Publication Date: 2018-03-23
GUANGXI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] (1) In terms of catalyst components, the catalyst used is required to be a solid catalyst and is granular. It is difficult to process the specifications and performance of the catalyst components into a consistent type, and it is difficult to unify the amount of catalyst, the performance of the packing and the void ratio in the tower.
[0009] (2) The material wrapping the catalyst component is easy to corrode, the corrosion problem is difficult to solve, and the catalyst packing is difficult to replace
[0010] (3) Due to the formation of multiple azeotropes in the esterification reaction system, the reaction products cannot all enter the top or bottom of the tower, and the technical advantages of catalytic distillation cannot be well utilized

Method used

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  • Method for synthesizing mixed ester through catalyst distillation

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Embodiment 1

[0032] A kind of method of catalytic distillation synthetic mixed ester, this method is raw material with ethanol, n-butanol, acetic acid, and the mol ratio of acetic acid, ethanol, n-butanol is 2:0.8:0.5 in the raw material; With strongly acidic cation exchange resin D072 as Catalyst, the dosage of catalyst is 0.5% of the mass of acetic acid added. Using the catalytic distillation tower as the reactor, the catalytic distillation reflux reaction is carried out. The reaction temperature is 60°C; the reaction time is 60min; the reflux ratio is 0.5, and the catalyst is reused 10 times. Finally, phase separation is carried out to obtain the mixed fat of ethyl acetate and butyl acetate. After the reaction, the single-pass conversion rate of ethanol is greater than 95.2%, and the single-pass conversion rate of butanol is greater than 97.5%.

Embodiment 2

[0034] A method for synthesizing mixed esters by catalytic distillation, the method takes ethanol, n-butanol and acetic acid as raw materials, and the mol ratio of acetic acid, ethanol and n-butanol in the raw material is 2.3:0.85:0.6; with strongly acidic cation exchange resin D002 as Catalyst, the amount of catalyst is 2% of the mass of acetic acid added. Using the catalytic distillation tower as the reactor, the catalytic distillation reflux reaction is carried out. The reaction temperature is 70°C; the reaction time is 100min; the reflux ratio is 1, and the catalyst is reused 11 times. Finally, phase separation is carried out to obtain the mixed fat of ethyl acetate and butyl acetate. After the reaction, the one-pass conversion rate of ethanol is greater than 95.6%, and the one-pass conversion rate of butanol is greater than 97.4%.

Embodiment 3

[0036]A method for synthesizing mixed esters by catalytic distillation, the method takes ethanol, n-butanol, acetic acid as raw material, and the mol ratio of acetic acid, ethanol, n-butanol in the raw material is 2.7:0.9:0.7; with strongly acidic cation exchange resin D008 as Catalyst, catalyst consumption is 4% of adding acetic acid quality. Using the catalytic distillation tower as the reactor, the catalytic distillation reflux reaction is carried out. The reaction temperature is 80°C; the reaction time is 140min; the reflux ratio is 2, and the catalyst is reused 12 times. Finally, phase separation is carried out to obtain the mixed fat of ethyl acetate and butyl acetate. After the reaction, the single-pass conversion rate of ethanol is greater than 95.3%, and the single-pass conversion rate of butanol is greater than 97.6%.

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Abstract

The invention discloses a method for synthesizing mixed ester through catalyst distillation. The method comprises the following steps: by taking ethanol, n-butyl alcohol and acetic acid as raw materials, a strong acid cation exchange resin as a catalyst and a catalyst distillation tower as a reactor, performing a catalyst distillation backflow reaction, and finally performing phase separation, thereby obtaining mixed ester of ethyl acetate and butyl acetate. According to the method, the intense water carrying power of the butyl acetate is utilized, azeotrope is prepared from the butyl acetate,butanol and water, and water generated from reactions is completely carried out from a tower top. Therefore, the conversion rate of alcohol reactants and the content of the acetic acid in the catalyst distillation tower can be increased, and the influence of product water to the reaction process in the tower is also eliminated. A tower top product is generally an ester-water mixture and comprisesa very small amount of acetic acid, so that the later purification difficulty of the ethyl acetate and the butyl acetate is greatly reduced, the production procedures are simplified, the production efficiency is improved, and the energy consumption is reduced.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, in particular to a method for synthesizing mixed esters by catalytic distillation, in particular to a method for simultaneously synthesizing ethyl acetate and butyl acetate by catalytic distillation. Background technique [0002] Catalytic distillation (CD, catalytic distillation) technology is a chemical process in which heterogeneous catalytic reaction and distillation separation are coupled in the same equipment. This process strengthens both chemical reaction and distillation separation. As a heterogeneous reaction distillation process, the existing catalyst for catalytic distillation adopts solid catalyst and fills it into the tower in a certain form, which can play the double role of catalysis and packing. In the process of catalytic distillation technology, the reaction product can be separated from the reaction area in time. According to the principle of reversible reaction, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/54C07C69/14
CPCC07C67/08C07C67/54C07C69/14Y02P20/10
Inventor 廖安平李媚蓝平蓝丽红王克之覃琴谢涛
Owner GUANGXI UNIV FOR NATITIES
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