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Method and device for integrated production of ethyl acetate through reactive distillation and penetration vaporization

A technology of pervaporation and ethyl acetate, which is applied in chemical instruments and methods, separation/purification of carboxylate, preparation of carboxylate, etc. It can solve complex distillation separation process, proper treatment of crude ester, large product loss, etc. problems, to achieve the effect of saving recycling units, simplifying the process and saving energy

Active Publication Date: 2018-05-22
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the disadvantages of complicated rectification and separation process and high energy consumption in the production of ethyl acetate by acetic esterification, as well as the low conversion rate of the integrated process of reactive distillation and pervaporation, large product loss and inability to process the crude ester in one step etc., the present invention provides a process for the integrated production of ethyl acetate with side line reactive distillation and pervaporation without the introduction of extractant or entrainer, the present invention provides a low energy consumption, simple process, and the process of producing ethyl acetate through reactive distillation column side line and pervaporation The membrane module removes water in time to promote the positive direction of the reaction. It is not necessary to circulate the product ethyl acetate as a water-carrying agent back to the reactive distillation column to increase the circulation stream and energy consumption, while ensuring that the molar fraction of the ethyl acetate product reaches 99.0 %above

Method used

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  • Method and device for integrated production of ethyl acetate through reactive distillation and penetration vaporization
  • Method and device for integrated production of ethyl acetate through reactive distillation and penetration vaporization
  • Method and device for integrated production of ethyl acetate through reactive distillation and penetration vaporization

Examples

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Embodiment 1

[0053] process such as figure 1 As shown, ethanol and acetic acid are fed in a molar ratio of 1:1, and the feed flow rate is 20 kmol / h. The whole tower of the reactive distillation column has 26 trays in total, including the top condenser and the reboiler of the tower still (the trays are numbered from top to bottom, the condenser is the first tray, and the reboiler is the last tray, Same below), divided into 14 trays in the upper rectifying section and 12 trays in the lower reaction section. Acetic acid is fed from the 15th tray, ethanol is fed from the reboiler of the tower still, and the liquid phase is not extracted from the tower still. The reaction section is filled with sulfonic acid ion exchange resin Amberlyst 15. Assuming that 70% of the liquid holding volume on each tray is catalyst, the mass of catalyst loaded on each tray is about 38.47kg. The operating pressure of the reactive distillation column is 101.325kPa, the reflux ratio is 4, the heat load of the tower ...

Embodiment 2

[0057] process such as figure 1 As shown, ethanol and acetic acid are fed in a molar ratio of 1:1, and the feed flow rate is 20 kmol / h. The reactive distillation column has 23 trays in total, including a top condenser and a still reboiler, which are divided into 13 trays in the upper rectification section and 10 trays in the lower reaction section. Acetic acid is fed from the 14th tray, ethanol is fed from the reboiler of the tower still, and the liquid phase is not extracted from the tower still. The reaction section is filled with solid acid catalyst PMB-II. Assuming that 70% of the liquid holding volume on each tray is catalyst, the mass of catalyst loaded on each tray is 35.9kg. The operating pressure of the reactive distillation column is 120kPa, the reflux ratio is 4.5, the heat load of the tower reboiler is 1428.46kW, the temperature of the tower top is 75.6°C, and the temperature of the tower bottom is 99.9°C. The liquid phase is extracted from the second tray, and t...

Embodiment 3

[0061] process such as figure 1As shown, ethanol and acetic acid are fed in a molar ratio of 1:1, and the feed flow rate is 20 kmol / h. The reactive distillation column has 20 trays in total, including a top condenser and a still reboiler, and is divided into 10 trays in the upper rectification section and 10 trays in the lower reaction section. Acetic acid is fed from the 11th tray, ethanol is fed from the reboiler of the tower still, and the liquid phase is not extracted from the tower still. The reaction section is filled with acidic ion exchange resin catalyst Purolite CT179, assuming that 70% of the liquid holding volume on each tray is catalyst, the mass of catalyst loaded on each tray is 19.6kg. The operating pressure of the reactive distillation column is 140kPa, the reflux ratio is 5, the heat load of the tower reboiler is 1669.10kW, the temperature at the top of the tower is 84.2°C, and the temperature at the bottom is 104.9°C. The liquid phase is extracted from the...

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Abstract

The invention provides a method for integrated production of ethyl acetate through reactive distillation and penetration vaporization. The whole tower of a reactive distillation tower is divided intoa distillation section and a reactive distillation section; acetic acid is fed from the top of the reactive distillation section; ethyl alcohol is fed from a tower kettle bottom reboiler; no extract is obtained at the tower kettle; a stream of liquid phase mainly containing water is extracted from the lateral line of the distillation section, and is moved out of the system. Tower top extracts enter a penetration vaporization membrane assembly; water permeates to pass through the membrane; remained ethyl acetate is the product. One part of water generated by esterification reaction is extractedfrom the lateral line; one part of the water is discharged out from the membrane assembly; the water is timely discharged out of the system in the two modes; the proceeding of the esterification reaction is promoted. Compared with a traditional process, the process has the advantages that the flow process is simple; the number of equipment is small; the energy consumption is low; entrainers or extracting agents are not introduced.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a new production process of ethyl acetate, in particular to a method and a device for producing ethyl acetate by using acetic acid and ethanol as raw materials through a new process integrating rectification with side line reaction and pervaporation. Background technique [0002] The process of preparing ethyl acetate by acetic acid esterification is to send a certain proportion of acetic acid and ethanol into the esterification reactor, use sulfuric acid or solid acid as a catalyst, carry out esterification reaction in the esterification reactor, and then separate to obtain ethyl acetate ester products. The outlet of the reactor generally obtains a crude ester product composed of ethyl acetate, ethanol and water, and there is a complex azeotropic phenomenon in this ternary system. It is necessary to adopt special distillation methods such as azeotropic distillation, extractive di...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/48C07C69/14
CPCC07C67/08C07C67/48C07C69/14Y02P20/10
Inventor 汤吉海乔旭金浩张竹修陆佳伟孔倩费兆阳崔咪芬陈献刘清
Owner NANJING UNIV OF TECH