Ethyl acetate synthesis method utilizing membrane separation dehydration

A technology of ethyl acetate and synthesis method, which is applied in the direction of semi-permeable membrane separation, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of poor water-carrying ability and high energy consumption of reflux ester, and achieve reduction of reflux flow and energy consumption. The effect of low consumption, guaranteed yield and product purity

Pending Publication Date: 2018-05-04
肇庆市稳固化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the water content (about 9wt.%) in the ethyl acetate-water-ethanol ternary azeotrope differs less from the partially miscible water content (about 5-6wt%) at normal temperature, the water-carrying ability of the reflux ester is relatively poor. The reflux of the esterification tower is relatively large, usually between 3-5, and the raw ethanol itself is 95% ethanol or other ethanol with a relatively large water content, and the water brought into the kettle is more, requiring more crude oil. ester reflux; moreover, the water content in the crude oil entering the refining tower is relatively high. In order to ensure that the product extracted from the tower still does not contain water and ethanol, the reflux of the crude ester at the top of the tower is also relatively high. In addition, in order to reduce the consumption of ethanol , the organic phase separated from the mixture containing ethyl acetate, ethanol and water withdrawn from the top of the refining tower returns to the still of the esterification tower to continue to participate in the reaction, resulting in a part of water circulating in the esterification tower and the refining tower, and the energy consumption is relatively high high

Method used

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  • Ethyl acetate synthesis method utilizing membrane separation dehydration

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Experimental program
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Effect test

Embodiment 2

[0032] Crude ethanol with a water content of 15%, the feed rate is controlled at 600L / h, heated and vaporized by the raw material evaporator 2, the temperature of the hot steam is controlled at 120°C, and the steam enters the raw material pervaporation water-permeable membrane module 3, and the pressure of the feed liquid is controlled to 0.3MPa. The side pressure is 1000Pa, the dehydrated ethanol separated by the membrane has a water content of 0.33%, and enters the dehydrated ester alcohol tank 4, while the water permeated through the raw material pervaporation water-permeable membrane module 3 is collected and discharged by vacuum condensation in the condenser 6, and the water content is 99.51%.

[0033] The dehydrated ethanol in the dehydrated ester alcohol tank 4 and the acetic acid in the acetic acid tank 5 are fed into the esterification tank 10 after being reboiled continuously through the esterification reboiler 11 at a flow rate of 550 L / h and 540 L / h respectively, and...

Embodiment 3

[0038] The water content is 8% crude ethanol, the feed rate is controlled to 800L / h, and the raw material evaporator 2 is heated to evaporate and vaporize, the temperature of the hot steam is controlled to be 110°C, and it enters the raw material pervaporation water-permeable membrane module 3, and the measured pressure of the feed liquid is controlled to 0.17MPa. The side pressure is 1000Pa, the water content of dehydrated ethanol after membrane separation is 0.22%, and enters the dehydrated ester alcohol tank 4, and the water permeated by the raw material pervaporation water-permeable membrane module 3 is collected and discharged by vacuum condensation in the condenser 6, and the water content is 99.30%.

[0039] The dehydrated ethanol in the dehydration ester alcohol tank 4 and the acetic acid in the acetic acid tank 5 are fed into the esterification kettle 10 after being reboiled continuously through the esterification reboiler 11 at a flow rate of 700L / h and 695L / h respecti...

Embodiment 4

[0044] Crude ethanol with a water content of 5%, the feed rate is controlled at 900L / h, heated and evaporated by the raw material evaporator 2, the temperature of the hot steam is controlled at 105°C, and the steam enters the raw material pervaporation water-permeable membrane module 3, the pressure of the feed liquid is controlled to 0.13MPa, and the permeable The side pressure is 1000Pa, and the dehydrated ethanol has a water content of 0.17% after membrane separation, and enters the dehydrated ester alcohol tank 4, while the water permeated through the raw material pervaporation water-permeable membrane module 3 is collected and discharged by vacuum condensation in the condenser 6, with a water content of 99.32%.

[0045] The dehydrated ethanol in the dehydration ester alcohol tank 4 and the acetic acid in the acetic acid tank 5 are fed into the esterification tank 10 after being reboiled continuously through the esterification reboiler 11 at a flow rate of 800 L / h and 795 L / ...

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Abstract

The invention discloses an ethyl acetate synthesis method utilizing membrane separation dehydration. Ethyl alcohol and acetic acid are reboiled and then enter an esterification kettle so as to carry out esterification reaction in the presence of a catalyst; a reaction product enters an esterification tower so as to be separated; a gas phase is distilled off from a tower top, condensed and layeredthrough a layering tank so as to extract ethyl acetate; the ethyl alcohol is vaporized by evaporation, then enters a raw material pervaporation permeable membrane assembly so as to be dehydrated, andis then fed into the esterification tower so as to be reacted with the acetic acid; crude ethyl acetate is vaporized by evaporation, then enters an esterification pervaporation permeable membrane assembly, and is then divided into two parts; one part reflows to the esterification tower so as to be used as a water-carrying agent, and the other part enters a refining tower so as to be refined, so that purified ethyl acetate is obtained. According to the ethyl acetate synthesis method utilizing membrane separation dehydration provided by the invention, a pervaporation membrane method is adopted for removing moisture of the raw material ethyl alcohol and a coarse ester on the top of the esterification tower without the limitation of azeotropy, no third component is introduced, the yield and the product purity are ensured, a craft process is simple, the continuous operation is realized, and the energy consumption is low.

Description

technical field [0001] The invention relates to a synthesis method of ethyl acetate, in particular to a synthesis method of ethyl acetate utilizing membrane separation and dehydration. Background technique [0002] Ethyl acetate is an important organic chemical raw material, which can be used to manufacture acetamide, acetoacetate, etc., and as an industrial solvent, it can be used in paint coatings, adhesives, ethyl cellulose, artificial leather, linoleum colorants, artificial fibers As a binder, it is used in the production of printing ink and artificial pearls; as an extractant, it is used in the production of medicines, organic acids and other products and is used in flavors and fragrances, medicines, advanced inks, collodion, nitrocellulose, Widely used in industries such as dyes. [0003] Esterification synthesis is the traditional production method of ethyl acetate. Under the catalysis of concentrated sulfuric acid, ethanol and acetic acid react in the esterification...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/48C07C67/54C07C69/14B01D61/36
CPCB01D61/362B01D61/366C07C67/08C07C67/48C07C67/54C07C69/14
Inventor 黄家龙
Owner 肇庆市稳固化工有限公司
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