CN110862321A - New process for combined rectification of ethyl acetate and n-butyl acetate - Google Patents

New process for combined rectification of ethyl acetate and n-butyl acetate Download PDF

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CN110862321A
CN110862321A CN201911099415.8A CN201911099415A CN110862321A CN 110862321 A CN110862321 A CN 110862321A CN 201911099415 A CN201911099415 A CN 201911099415A CN 110862321 A CN110862321 A CN 110862321A
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ethyl acetate
dehydration
equal
butyl acetate
percent
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张超
何晓芳
卢晓峰
吴清云
樊仕伟
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LINYI JINXIMENG BIOLOGICAL TECHNOLOGY Co Ltd
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LINYI JINXIMENG BIOLOGICAL TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • C07C67/52Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Abstract

The invention discloses a new process for the combined rectification of ethyl acetate and n-butyl acetate, which comprises the steps of co-producing and rectifying the ethyl acetate and the n-butyl acetate, introducing gas phase heat at the top of a dehydration tower of an n-butyl acetate device in the prior art to the bottom of the dehydration tower of the ethyl acetate device to be used as a heating source of the dehydration tower, modifying a heating system of the ethyl acetate dehydration tower, and condensing gas phase materials of the dehydration tower of the n-butyl acetate while saving steam in the ethyl acetate dehydration tower to realize the heat coupling. The invention can realize the combined rectification of the ethyl acetate and the n-butyl acetate, obtain the high-purity ethyl acetate and the high-purity n-butyl acetate, greatly save the steam consumption, fully utilize the waste heat, greatly reduce the energy consumption in the rectification process, realize the purposes of saving energy and reducing consumption, reduce the cost and improve the efficiency.

Description

New process for combined rectification of ethyl acetate and n-butyl acetate
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a new process for jointly rectifying ethyl acetate and n-butyl acetate.
Background
Ethyl acetate and n-butyl acetate are important organic solvents in chemical production, and are widely applied to industries such as paint, spice, textile and the like. In the conventional reactive distillation esterification method commonly used in domestic industry at present, in the process of producing ethyl acetate and n-butyl acetate by the esterification method, acetic acid, ethanol and n-butyl alcohol respectively react in an esterification kettle to generate ethyl acetate and n-butyl acetate, the ethyl acetate and the n-butyl acetate are primarily rectified by an esterification tower and layered by a phase separator, and then the upper semi-finished product overflows and enters a crude ester tank; one part of the water is conveyed to the top of the esterification tower for reflux, and the other part of the water is conveyed to a dehydration tower in a refining procedure for rectification, dehydration and dealcoholization so as to meet the requirements of water, alcohol, acid and other impurity contents in a finished product. Because the two devices need to feed for dehydration and dealcoholization in the refining process, the energy consumption in the dehydration process is larger. Therefore, it is very important to develop a process scheme with simple flow, high thermodynamic efficiency and low energy consumption.
Disclosure of Invention
In order to solve the problem of high energy consumption in refining and separating acetic ester in the prior art, the invention provides a new process for jointly rectifying ethyl acetate and n-butyl acetate, which introduces the gas phase heat at the top of a dehydration tower of an n-butyl acetate device in the prior art to the bottom of the dehydration tower of the ethyl acetate device to be used as a heating source of the dehydration tower, reforms a heating system of the ethyl acetate dehydration tower, and condenses the gas phase material of the dehydration tower of the n-butyl acetate while saving steam in the ethyl acetate dehydration tower. The heat coupling is realized, and the energy consumption is effectively reduced.
In order to achieve the purpose, the invention provides the following technical scheme:
a new process for rectifying ethyl acetate and n-butyl acetate comprises the following steps:
(1) conveying the n-butyl acetate crude ester generated in the n-butyl acetate esterification procedure to a dehydration tower T1102 through a dehydration preheater E1106, and after rectification dehydration and dealcoholization, forming an n-butyl acetate gas phase material on the upper part of the dehydration tower T1102;
(2) conveying the ethyl acetate crude ester generated in the ethyl acetate esterification procedure to a dehydration tower T2301 for rectification dehydration and dealcoholization, and forming a gas phase material on the upper part of the dehydration tower T2301;
(3) introducing the n-butyl acetate gas phase material formed on the upper part of the dehydrating tower T1102 in the step (1) into an ethyl acetate rectification process section condensate reboiler E1113 to exchange heat with an ethyl acetate liquid phase material in the condensate reboiler E1113, wherein the n-butyl acetate gas phase material is changed into a liquid phase after heat exchange, enters a condensate tank V1110, is conveyed to a secondary condenser E1110 of the dehydrating tower by using a condensate conveying pump P1109 to be cooled, enters a phase separator V1108 of the dehydrating tower to be layered, an upper ester layer is conveyed to the top of the dehydrating tower T1102 through a dehydrating reflux tank V1109 by using a dehydrating reflux pump P1107 to be subjected to full reflux after being layered, and lower water and alcohol are taken as wastewater for recycling; after materials at the bottom of the dehydrating tower T1102 are detected to be qualified, the materials are extracted by a finished product conveying pump P1108, cooled by a finished product first-stage condenser E1111 and a finished product second-stage condenser E1112 and then enter a finished product tank to obtain a finished n-butyl acetate product;
(4) after heat exchange is carried out between an ethyl acetate liquid phase material in a condensate reboiler E1113 in the ethyl acetate rectification process section and an n-butyl acetate gas phase material, the liquid phase ethyl acetate is changed into a gas phase, the gas phase material enters a dehydration tower T2301 and forms a gas phase material on the upper part of the dehydration tower T2301, the gas phase material is condensed and cooled by a dehydration first-stage condenser E2302, a dehydration second-stage condenser E2303, a dehydration third-stage condenser E2304 and a dehydration cooler E2305 and then enters a dehydration phase separator V2301 for layering, after layering, an upper ester layer is sent to the top of the dehydration tower T2301 by a dehydration reflux pump P2301 for full reflux, and lower water and alcohol are recovered as wastewater; and (3) detecting materials at the bottom of the dehydration tower T2301 to be qualified, extracting the materials by using a finished product extraction pump P2303, and cooling the materials by using a finished product cooler E2306 to obtain an ethyl acetate finished product.
Further, the composition of the gas phase material of n-butyl acetate formed at the upper part of the dehydrating tower T1102 in the step (1) is as follows: 40-53% of n-butyl acetate, 7-10% of water, 40-50% of n-butanol and less than or equal to 0.004% of acetic acid.
Further, the composition of the ethyl acetate gas phase material formed at the upper part of the dehydrating tower T2301 in the step (2) is as follows: 70-80% of ethyl acetate, 8-11% of water, 5-10% of ethanol, 2-6% of methyl acetate and less than or equal to 0.004% of acetic acid.
Further, the qualified state of the materials at the bottom of the dehydrating tower T1102 in the step (3) is as follows: more than or equal to 99.7 percent of butyl acetate, less than or equal to 0.01 percent of water, less than or equal to 0.05 percent of n-butyl alcohol and less than or equal to 0.004 percent of acetic acid; purity of n-butyl acetate finished product: more than or equal to 99.7 percent of butyl acetate, less than or equal to 0.01 percent of water, less than or equal to 0.05 percent of n-butyl alcohol and less than or equal to 0.004 percent of acetic acid.
Further, the qualified state of the tower bottom materials of the dehydrating tower T2301 in the step (4) is as follows: ethyl acetate is more than or equal to 99.9 percent, water is less than or equal to 0.01 percent, ethanol is less than or equal to 0.01 percent, and acetic acid is less than or equal to 0.004 percent; the purity of the ethyl acetate finished product is as follows: more than or equal to 99.9 percent of ethyl acetate, less than or equal to 0.01 percent of water, less than or equal to 0.01 percent of ethanol and less than or equal to 0.004 percent of acetic acid.
Further, the ethyl acetate liquid phase material in the condensate reboiler E1113 in the step (3) is the material at the bottom of the dehydrating tower T2301.
The invention has the beneficial effects that:
(1) the invention optimizes the traditional acetate process, combines the rectification sections of ethyl acetate and n-butyl acetate, and realizes combined rectification; and introducing the gas-phase material at the top of the n-butyl acetate dehydrating tower into a heating system of the ethyl acetate dehydrating tower, and fully utilizing the heat in the gas-phase material to realize the heat coupling of the two towers. When the material contained in the n-butyl acetate gas phase material can not meet the requirement, the dehydration reboiler supplies heat to the ethyl acetate dehydration tower, and the normal and orderly rectification is ensured.
(2) By adopting the rectification process, the combined rectification of the ethyl acetate and the n-butyl acetate can be realized, the high-purity ethyl acetate and the high-purity n-butyl acetate can be obtained, the steam consumption can be greatly saved, the waste heat is fully utilized, the energy consumption in the rectification process is greatly reduced, the purposes of saving energy and reducing consumption are realized, the cost is reduced, and the efficiency is improved.
Drawings
The above and other features, properties and advantages of the present invention will become more apparent from the following description of the embodiments with reference to the accompanying drawings in which like reference numerals denote like features throughout the several views, wherein:
FIG. 1 is a process flow diagram of the ethyl acetate rectification section in the combined rectification process of the invention.
FIG. 2 is a process flow diagram of the n-butyl acetate rectification section in the combined rectification process of the invention.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
example 1 referring to figures 1 and 2, a new process for the rectification of ethyl acetate and n-butyl acetate comprises the following steps: (1) conveying the n-butyl acetate crude ester generated in the n-butyl acetate esterification procedure to a dehydration tower T1102 through a dehydration preheater E1106, and after rectification dehydration and dealcoholization, forming an n-butyl acetate gas phase material on the upper part of the dehydration tower T1102;
(2) conveying the ethyl acetate crude ester generated in the ethyl acetate esterification procedure to a dehydration tower T2301 for rectification dehydration and dealcoholization, and forming a gas phase material on the upper part of the dehydration tower T2301;
(3) introducing the gas phase material of n-butyl acetate formed at the upper part of the dehydrating tower T1102 in the step (1) into a condensate reboiler E1113 of an ethyl acetate rectification process section to exchange heat with an ethyl acetate liquid phase material in the condensate reboiler E1113, wherein the ethyl acetate liquid phase material in the condensate reboiler E1113 is a tower bottom material of the dehydrating tower T2301; the method comprises the following steps of (1) changing a butyl acetate gas phase material into a liquid phase after heat exchange, entering a condensate tank V1110, sending the liquid phase material into a secondary condenser E1110 of a dehydration tower by using a condensate conveying pump P1109 for cooling, entering a phase separator V1108 of the dehydration tower for layering after cooling, conveying an upper ester layer to the top of the dehydration tower T1102 for full reflux by using a dehydration reflux pump P1107 through a dehydration reflux tank V1109 after layering, and recovering lower water and alcohol as wastewater; after materials at the bottom of the dehydrating tower T1102 are detected to be qualified, the materials are extracted by a finished product conveying pump P1108, cooled by a finished product first-stage condenser E1111 and a finished product second-stage condenser E1112 and then enter a finished product tank to obtain a finished n-butyl acetate product;
(4) after heat exchange is carried out between an ethyl acetate liquid phase material in a condensate reboiler E1113 in the ethyl acetate rectification process section and an n-butyl acetate gas phase material, the liquid phase ethyl acetate is changed into a gas phase, the gas phase material enters a dehydration tower T2301 and forms a gas phase material on the upper part of the dehydration tower T2301, the gas phase material is condensed and cooled by a dehydration first-stage condenser E2302, a dehydration second-stage condenser E2303, a dehydration third-stage condenser E2304 and a dehydration cooler E2305 and then enters a dehydration phase separator V2301 for layering, after layering, an upper ester layer is sent to the top of the dehydration tower T2301 by a dehydration reflux pump P2301 for full reflux, and lower water and alcohol are recovered as wastewater; and (3) detecting materials at the bottom of the dehydration tower T2301 to be qualified, extracting the materials by using a finished product extraction pump P2303, and cooling the materials by using a finished product cooler E2306 to obtain an ethyl acetate finished product.
Wherein the composition of the n-butyl acetate gas phase material formed at the upper part of the dehydrating tower T1102 in the step (1) is as follows: 40-53% of n-butyl acetate, 7-10% of water, 40-50% of n-butanol and less than or equal to 0.004% of acetic acid.
The composition of the ethyl acetate gas phase material formed at the upper part of the dehydrating tower T2301 in the step (2) is as follows: 70-80% of ethyl acetate, 8-11% of water, 5-10% of ethanol, 2-6% of methyl acetate and less than or equal to 0.004% of acetic acid.
And (3) the qualified state of the materials at the bottom of the dehydration tower T1102 tower is as follows: more than or equal to 99.7 percent of butyl acetate, less than or equal to 0.01 percent of water, less than or equal to 0.05 percent of n-butyl alcohol and less than or equal to 0.004 percent of acetic acid; purity of n-butyl acetate finished product: more than or equal to 99.7 percent of butyl acetate, less than or equal to 0.01 percent of water, less than or equal to 0.05 percent of n-butyl alcohol and less than or equal to 0.004 percent of acetic acid.
The qualified state of the tower bottom materials of the dehydration tower T2301 in the step (4) is as follows: ethyl acetate is more than or equal to 99.9 percent, water is less than or equal to 0.01 percent, ethanol is less than or equal to 0.01 percent, and acetic acid is less than or equal to 0.004 percent; the purity of the ethyl acetate finished product is as follows: more than or equal to 99.9 percent of ethyl acetate, less than or equal to 0.01 percent of water, less than or equal to 0.01 percent of ethanol and less than or equal to 0.004 percent of acetic acid.
Comparing the data of the combined rectification process of 1-6 months and the data of the single rectification process of the traditional acetate in the company, the energy consumption parameters are counted, and the comparison results are shown in table 1:
TABLE 1 comparison of energy consumption of Unit products of Combined and Individual rectification
Figure DEST_PATH_IMAGE001
As can be seen from the data in Table 1, the combined rectification of ethyl acetate and n-butyl acetate can save steam consumption by at least 8000 kg per month on average. Therefore, the combined rectification process has obvious energy-saving effect and is worthy of popularization.
It should be noted that the above-mentioned embodiments are only some of the preferred modes for implementing the invention, and not all of them. Obviously, all other embodiments obtained by persons of ordinary skill in the art based on the above-mentioned embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.

Claims (6)

1. A new process for the combined rectification of ethyl acetate and n-butyl acetate is characterized by comprising the following steps:
(1) conveying the n-butyl acetate crude ester generated in the n-butyl acetate esterification procedure to a dehydration tower T1102 through a dehydration preheater E1106, and after rectification dehydration and dealcoholization, forming an n-butyl acetate gas phase material on the upper part of the dehydration tower T1102;
(2) conveying the ethyl acetate crude ester generated in the ethyl acetate esterification procedure to a dehydration tower T2301 for rectification dehydration and dealcoholization, and forming a gas phase material on the upper part of the dehydration tower T2301;
(3) introducing the n-butyl acetate gas phase material formed on the upper part of the dehydrating tower T1102 in the step 1 into a condensate reboiler E1113 of an ethyl acetate rectification process section, exchanging heat with an ethyl acetate liquid phase material in the condensate reboiler E1113, changing the n-butyl acetate gas phase material into a liquid phase after heat exchange, entering a condensate tank V1110, sending the liquid phase material into a secondary condenser E1110 of the dehydrating tower by using a condensate conveying pump P1109 for cooling, entering a phase separator V1108 of the dehydrating tower for layering after cooling, conveying an upper ester layer to the top of the dehydrating tower T1102 for full reflux by using a dehydrating reflux pump P1107 through a dehydrating reflux tank V1109 after layering, and recovering lower water and alcohol as wastewater; after materials at the bottom of the dehydrating tower T1102 are detected to be qualified, the materials are extracted by a finished product conveying pump P1108, cooled by a finished product first-stage condenser E1111 and a finished product second-stage condenser E1112 and then enter a finished product tank to obtain a finished n-butyl acetate product;
(4) step 3, after heat exchange is carried out between an ethyl acetate liquid phase material in a condensate reboiler E1113 in the ethyl acetate rectification process section and an n-butyl acetate gas phase material, the liquid phase ethyl acetate is changed into a gas phase, the gas phase material enters a dehydration tower T2301 and forms a gas phase material at the upper part of the dehydration tower T2301, the gas phase material enters a dehydration phase separator V2301 for layering after being condensed and cooled by a dehydration primary condenser E2302, a dehydration secondary condenser E2303, a dehydration tertiary condenser E2304 and a dehydration cooler E2305, the layered product is sent to the top of the dehydration tower T2301 for full reflux by a dehydration reflux pump P2301, and the lower layer water and alcohol are recovered as wastewater; and (3) detecting materials at the bottom of the dehydration tower T2301 to be qualified, extracting the materials by using a finished product extraction pump P2303, and cooling the materials by using a finished product cooler E2306 to obtain an ethyl acetate finished product.
2. The new process for the combined rectification of ethyl acetate and n-butyl acetate as claimed in claim 1, wherein the gas phase material of n-butyl acetate formed at the upper part of the dehydrating column T1102 in the step (1) consists of: 40-53% of n-butyl acetate, 7-10% of water, 40-50% of n-butanol and less than or equal to 0.004% of acetic acid.
3. The new process for the combined rectification of ethyl acetate and n-butyl acetate according to claim 1, wherein the composition of the gas phase material of ethyl acetate formed at the upper part of the dehydration column T2301 in the step (2) is as follows: 70-80% of ethyl acetate, 8-11% of water, 5-10% of ethanol, 2-6% of methyl acetate and less than or equal to 0.004% of acetic acid.
4. The new process for the combined rectification of ethyl acetate and n-butyl acetate according to claim 1, wherein the qualified status of the materials at the bottom of the dehydration column T1102 in the step (3) is as follows: more than or equal to 99.7 percent of butyl acetate, less than or equal to 0.01 percent of water, less than or equal to 0.05 percent of n-butyl alcohol and less than or equal to 0.004 percent of acetic acid; purity of n-butyl acetate finished product: more than or equal to 99.7 percent of butyl acetate, less than or equal to 0.01 percent of water, less than or equal to 0.05 percent of n-butyl alcohol and less than or equal to 0.004 percent of acetic acid.
5. The new process for rectifying ethyl acetate and n-butyl acetate according to claim 1, wherein the qualified state of the materials at the bottom of the dehydrating tower T2301 in the step (4) is as follows: ethyl acetate is more than or equal to 99.9 percent, water is less than or equal to 0.01 percent, ethanol is less than or equal to 0.01 percent, and acetic acid is less than or equal to 0.004 percent; the purity of the ethyl acetate finished product is as follows: more than or equal to 99.9 percent of ethyl acetate, less than or equal to 0.01 percent of water, less than or equal to 0.01 percent of ethanol and less than or equal to 0.004 percent of acetic acid.
6. The new process for rectifying ethyl acetate and n-butyl acetate according to claim 1, wherein the ethyl acetate liquid phase material in the condensate reboiler E1113 in the step (3) is the bottom material of a dehydrating tower T2301.
CN201911099415.8A 2019-11-12 2019-11-12 New process for combined rectification of ethyl acetate and n-butyl acetate Pending CN110862321A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101830799A (en) * 2010-05-25 2010-09-15 张超 Single-tower rectifying method for synthetizing ethyl acetate by esterification method
CN102643195A (en) * 2012-04-20 2012-08-22 临沂市金沂蒙生物科技有限公司 Production method of n-butyl acetate
CN102675093A (en) * 2012-02-25 2012-09-19 中国石油大学(华东) Process for synthesizing n-butyl acetate
CN202688237U (en) * 2012-04-20 2013-01-23 临沂市金沂蒙生物科技有限公司 Production device for n-butyl acetate
CN103951544A (en) * 2014-05-19 2014-07-30 临沂市巅峰化工技术有限公司 Method for separating ethyl acetate and ethanol azeotrope by differential pressure rectification
CN107954866A (en) * 2017-12-13 2018-04-24 中国石油大学(华东) The method and its device of differential pressure heat coupled reaction rectifying synthesis of acetic acid isopropyl ester

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101830799A (en) * 2010-05-25 2010-09-15 张超 Single-tower rectifying method for synthetizing ethyl acetate by esterification method
CN102675093A (en) * 2012-02-25 2012-09-19 中国石油大学(华东) Process for synthesizing n-butyl acetate
CN102643195A (en) * 2012-04-20 2012-08-22 临沂市金沂蒙生物科技有限公司 Production method of n-butyl acetate
CN202688237U (en) * 2012-04-20 2013-01-23 临沂市金沂蒙生物科技有限公司 Production device for n-butyl acetate
CN103951544A (en) * 2014-05-19 2014-07-30 临沂市巅峰化工技术有限公司 Method for separating ethyl acetate and ethanol azeotrope by differential pressure rectification
CN107954866A (en) * 2017-12-13 2018-04-24 中国石油大学(华东) The method and its device of differential pressure heat coupled reaction rectifying synthesis of acetic acid isopropyl ester

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