Method for producing ethyl acetate with coupled reaction distillation and permeation steam generation

A technology of pervaporation and reactive distillation, which is applied in the field of coupling reactive distillation and pervaporation to produce ethyl acetate, can solve the problems of poor reflux water carrying capacity, limited production capacity, large gas-liquid phase load, etc. The effect of reducing the volume and reducing the reflux ratio

Active Publication Date: 2009-04-08
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] The alkyd esterification method used by domestic ethyl acetate manufacturers is generally a continuous method, that is, the production device consists of an esterification tower, a dehydration tower, a refining tower and a recovery tower. The process is characterized by the esterification reaction being carried out in the esterification tank. The separation process mainly adopts the azeotropic distillation process for dehydration and dealcoholization. Due to the characteristics of the ethyl acetate-water-ethanol ternary azeotropic system, the water content in the reflux of the organic phase at the top of the esterification tower is relatively high, so the ability of the reflux to carry water is poor , usually the reflux ratio of the esterification tower is around 3 to 5; the same reason causes the water content in the crude ester entering the dehydration tower to be relatively high.

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  • Method for producing ethyl acetate with coupled reaction distillation and permeation steam generation

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Effect test

Embodiment 1

[0020] Reactive distillation tower, the height of the reaction section is 50cm, the height of the rectification section and the stripping section is 40cm, and it is equipped with stainless steel θ ring packing and CT-450 solid acid catalyst. The raw materials acetic acid and ethanol are fed from the upper and lower parts of the tower respectively, and the feed flow rates are 0.8kg / h and 0.5kg / h respectively. The temperature at the bottom of the tower is controlled at 110°C, the temperature at the top of the tower is controlled at 70°C, the flow rate of the distillate at the top of the tower is 0.5kg / , and the reflux ratio in the tower is 1.5. The phase separator is equipped with an insulating layer, and the temperature is controlled at 60°C. After the top material is separated by a phase separator, the composition of the upper organic phase obtained is: water 7.5% (wt%); ethanol 0.5% (wt%); ethyl acetate 92% (wt%).

[0021] The pervaporation water-permeable membrane I is comp...

Embodiment 2

[0024] Reactive distillation tower, the height of the reaction section is 55cm, the height of the rectification section and the stripping section is 40cm, and Raschig ring packing is installed inside, and the catalyst is strong acidic cation exchange resin. Acetic acid and ethanol are fed from the upper and lower parts of the tower respectively, and the feed flow rates are 1.0kg / h and 0.5kg / h respectively. The temperature at the bottom of the tower is controlled at 110°C, the temperature at the top of the tower is controlled at 70°C, the flow rate of the output at the top of the tower is 0.5kg / h, and the reflux ratio in the tower is 2. The temperature of the phase separator is controlled at 50°C. After the top material is separated by a phase separator, the composition of the obtained upper organic phase is: water 5.3% (wt%), ethyl acetate 94.7% (wt%).

[0025] The pervaporation permeable membrane module II uses polyvinyl alcohol permeable membrane with polyacrylonitrile as t...

Embodiment 3

[0028] Reactive distillation tower, the height of the reaction section is 50cm, the height of the rectification section and the stripping section is 40cm, and the stainless steel θ ring packing is installed inside, and the catalyst is a solid acid catalyst. Acetic acid and ethanol are fed from the upper and lower parts of the tower respectively, and the feed rates are 0.8kg / h and 0.5kg / h respectively. The temperature at the bottom of the tower is controlled at 110°C, the temperature at the top of the tower is controlled at 70°C, the output rate of the top product is 0.5kg / h, and the reflux ratio in the tower is 1.5. The temperature of the phase separator is controlled at 60°C. After the top material is separated by a phase separator, the composition of the upper organic phase obtained is: water 7.5% (wt%); ethanol 0.5% (wt%); ethyl acetate 92% (wt%).

[0029] The pervaporation water-permeable membrane module I is composed of a ceramic support body and a chitosan organic layer...

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Abstract

The invention relates to a method for producing ethyl acetate by reaction rectification and pervaporation coupling. The method is as follows: raw materials, namely acetic acid and ethanol are catalyzed in a reaction rectification tower and rectified, an organic phase is separated out from the distillate at the top of the tower and passes through a pervaporation permeable film component, wherein the contained water and ethanol selectively permeate the film and then enrich on the permeable side of the film to be removed; the ethyl acetate is obtained from the non-permeable side of the film; and part of the ethyl acetate as dehydrating agent is returned to the reaction rectification tower while the rest as a product is extracted; at the same time, part of liquor extracted from the tower bottom of the reaction rectification tower is introduced into another pervaporation permeable film component, the contained moisture is enriched on the permeable side of the film to be separated and removed, the ethyl acetate is obtained from the non-permeable side of the film, and the ethyl acetate is circularly returned to an acetic acid feeding hole of the reaction rectification tower. Compared with the prior art, the method can reduce reflux ratio greatly, has the advantages of simple technical route, energy saving, environmental protection and compact device, and reduces equipment investment and production cost for the ethyl acetate remarkably.

Description

technical field [0001] The invention relates to a process for producing ethyl acetate coupled with reactive distillation and pervaporation. Background technique [0002] Ethyl acetate is an important fine chemical raw material, widely used in paints, coatings, artificial leather, nitrocellulose, adhesives, medicine and other fields. In recent years, the application of ethyl acetate at home and abroad has grown rapidly. With the further improvement of environmental protection requirements for domestic coatings and adhesive products, ethyl acetate has been widely used as a non-toxic solvent. It has been gradually used in my country's coating industry. Environmentally friendly coatings, therefore, will further drive the market growth of ethyl acetate. [0003] The alkyd esterification method used by domestic ethyl acetate manufacturers is generally a continuous method, that is, the production device consists of an esterification tower, a dehydration tower, a refining tower and ...

Claims

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Application Information

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IPC IPC(8): C07C69/14C07C67/08
CPCY02P20/10
Inventor 金万勤夏珊珊朱月馨徐南平
Owner NANJING UNIV OF TECH
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