CN1803757A - Ethyl acetate dehydrating extraction method - Google Patents
Ethyl acetate dehydrating extraction method Download PDFInfo
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- CN1803757A CN1803757A CN 200610033048 CN200610033048A CN1803757A CN 1803757 A CN1803757 A CN 1803757A CN 200610033048 CN200610033048 CN 200610033048 CN 200610033048 A CN200610033048 A CN 200610033048A CN 1803757 A CN1803757 A CN 1803757A
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Abstract
The disclosed dewatering purification method for ethyl acetate comprises: leading the coarse ethyl acetate with water, acetic acid and ethanol into rectifying tower at 75~78Deg to form the ternary azeotrope and rectify to obtain the oil with ethanol, water and little ethyl acetate, residual liquid with acetic acid, and ethyl acetate on tower top, tower bottom and middle of tower respectively; drawing out the oil to condense and separate phases to discharge the water and reflux some oil by ratio as 6~11:1, recovering other oil; cooling and refluxing some the ethyl acetate by ratio as 1~5:1 to leave residue as final product. This invention reduces cost and energy consumption.
Description
Technical field
The present invention relates to a kind of method of purification of organic compound, the method that particularly a kind of ethyl acetate dehydration is purified.
Background technology
Ethyl acetate is a kind of important chemical material, has a wide range of applications in spices, medicine and paint industry.Industrial production vinyl acetic monomer is to be raw material with acetate and ethanol, and the vitriol oil is that catalyzer carries out in reactor.In the process of purification vinyl acetic monomer, because product water and ethanol can form binary and ternary azeotrope with vinyl acetic monomer, also partial miscibility under the normal temperature has brought very big difficulty for the purification of vinyl acetic monomer.At present industrial mainly be utilize the azeotropic of vinyl acetic monomer-alcohol-water form with normal temperature under the difference of mutual solubility, rectifying-condensation-reflux dewatering circulates, this method mainly comprises two parts, first part is acetate, an ethanol synthesizing ethyl acetate in reactor, and second section is to go out concentration in the ethyl acetate more than 99% through three grades of rectifying separation from the mixture of the ester that generates, alcohol and water.Second section is a typical chemical separation process.In this process, the character of utilizing ethyl acetate and water section to dissolve each other allows ester phase reflux dewatering in quantizer, and water is delivered to recovery tower, progressively the water in the cat head azeotrope of sequence of constant boiling and rectification (ester of extraction, water, alcohol) is removed, and the purity of ester is improved constantly.The water content of dissolving each other because of the water content and the normal temperature lower section of azeotropic composition differs less, makes the band outlet capacity of backflow ester very poor, causes the reflux ratio of esterification column and dehydration tower very big, makes the production energy consumption of vinyl acetic monomer very high.
People such as Qiu Xueqing, Cai Jintuan research influences ester-water binary system mutual solubility by interpolation promotor and changes the liquid-liquid equilibrium of ternary component, reach the following minute water outlet of normal temperature, the purpose of purification vinyl acetic monomer, and a kind of energy-conservation separation method of industrial production vinyl acetic monomer has been proposed.This method has increased by a cover extraction plant and a promotor retrieving arrangement on the basis of above-mentioned three grades of distillation and separation methods, the feasible thick ester that comes out from esterification column is first after the promotor processed, a part of backflow esterification column, and all the other are transported to dehydration tower.
The shortcoming of above-mentioned technical process is: restricted by the ethyl acetate water amount, the existing reflux ratio of esterification column is higher, causes plant energy consumption higher, and there is unreasonable part in process design.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, the method that provides the ethyl acetate dehydration to purify by dehydration and refining deacidification that rectifying tower can be finished ethyl acetate simultaneously, is isolated highly purified ethyl acetate, significantly cuts down the consumption of energy.
The method that ethyl acetate dehydration of the present invention is purified comprises the steps:
(1) is 75 ℃～78 ℃ with temperature, contains water, acetate, the thick ethyl acetate of alcoholic acid and enter in the tower, form ethanol, water and ethyl ester ternary azeotrope from the rectifying tower middle part;
(2) obtain containing the hair oil of ethanol, water and amount of ethyl acetate after the ternary azeotrope rectifying at cat head, obtain containing the debris of acetate at the bottom of the tower, obtain ethyl acetate in the tower;
(3) debris is discharged at the bottom of tower; Hair oil is extracted out from cat head, after the condensation, carried out phase-splitting and handle, obtain water and oil phase, water is discharged, the part oil phase refluxes, and reflux ratio is 6～11: 1, and all the other oil phases reclaim;
(4) the ethyl acetate cooling that obtains of Jiang Tazhong, partial reflux, its reflux ratio is 1～5: 1, the finished product that all the other ethyl acetate make for the present invention.
Preferred version of the present invention: in the described rectifying tower, the tower internal pressure is 1.0am～1.3am, and tower top temperature is 70 ℃～78 ℃, and temperature is 80 ℃～87 ℃ in the tower, and column bottom temperature is 83 ℃～90 ℃.
The present invention carries out integrated improvement by the flow process coupling to corresponding rectifying, the complicated rectifying tower that adopts the band stage casing to extract out be coupled dehydration tower, finished product rectifying tower in the present technology, make waste water and light constituent from the cat head extraction, heavy burder is discharged the extraction from tower of ethyl ester finished product at the bottom of containing the tower of part acetic acid at the bottom of tower.The present invention is integrated with dehydration tower, the coupling of finishing column two complete equipments, more simplifies than the equipment that traditional technology is used, and has fundamentally improved separation efficiency, reduced facility investment and has reduced process cost.
The present invention compared with prior art has following advantage:
(1) the present invention is integrated with dehydration tower and finishing column coupling, has reached process intensification, and the purpose of streamlining has reduced the facility investment expense, operational cost.
(2) method of the present invention can be transformed on the basis of original device, is suitable for the Production Flow Chart transformation of existing conventional with ethanol, acid esterification synthesizing ethyl acetate.
(3) method of the present invention makes energy consumption descend 46%, and the facility investment expense reduces 25%, by producing 20000 tons of ethyl acetate per year, can save 1,200,000 yuan of process costs every year, and economic benefit is more remarkable.
Description of drawings
Fig. 1 is the schema of ethyl acetate dehydration purified method of the present invention.
Embodiment
As shown in Figure 1, thick ethyl acetate enters rectifying tower from the middle part of rectifying tower 1, after rectifying tower rectifying, rectifying tower top size oil is extracted out by reflux pump 4, phase-splitting after 3 condensations of minute flow container obtains water and oil phase, and water is discharged from minute flow container, the part of oil phase is back to rectifying tower by pipeline, and another part reclaims.The part of the waste liquid of rectifier bottoms is got back to rectifying tower after handling by azeotropic device 2, and another part reclaims.Be ethyl acetate in the rectifying Tata, its part is back to rectifying tower through reflux pump 5, and another part is a finished product.
Embodiment 1
(1) it is 75 ℃ with temperature, the thick ester of ethyl acetate of ethanol, 96.95% (weight) of water, 1.86% (weight) that contains the acetate, 1.17% (weight) of 0.012% (weight) enters the rectifying tower middle part with the flow of 3150kg/h, forms ethanol, water and ethyl ester ternary azeotrope;
(2) obtain containing the hair oil of ethanol, water and amount of ethyl acetate after the ternary azeotrope rectifying at cat head, obtain containing the debris of acetate at the bottom of the tower, obtain ethyl acetate in the tower;
(3) debris is discharged at the bottom of tower; Hair oil is extracted out from cat head, after the condensation, carried out phase-splitting and handle, obtain water and oil phase, water is discharged, the part oil phase refluxes, and reflux ratio is 6: 1, and all the other oil phases reclaim;
(4) the ethyl acetate cooling that obtains of Jiang Tazhong, partial reflux, its reflux ratio is 1: 1, the finished product that all the other ethyl acetate make for the present invention.
In the rectifying tower, the tower internal pressure is 1.0am, and tower top temperature is 70 ℃, and temperature is 80 ℃ in the tower, and column bottom temperature is 83 ℃.
It is as shown in the table to separate each component concentration of back:
Energy consumption in the above-mentioned sepn process is as shown in the table:
| Project | Load (kw) | |
| Public utility | The rectifying tower reboiler | 671.9 |
| The rectifying tower condenser duty | 400.1 | |
| Total load kw | 1082.0 | |
| Energy consumption (KJ/Kg ethyl acetate) | 1222.3 | |
| Traditional technology production energy consumption (KJ/Kg ethyl acetate) | 2300 | |
The energy consumption that the dehydration of ethyl acetate is purified drops to 1222.3KJ/Kg from 2300KJ/Kg.
Embodiment 2
(1) it is 78 ℃ with temperature, the thick ester of ethyl acetate of ethanol, 96.95% (weight) of water, 1.86% (weight) that contains the acetate, 1.17% (weight) of 0.012% (weight) enters the rectifying tower middle part with the flow of 3150kg/h, forms ethanol, water and ethyl ester ternary azeotrope;
(2) obtain containing the hair oil of ethanol, water and amount of ethyl acetate after the ternary azeotrope rectifying at cat head, obtain containing the debris of acetate at the bottom of the tower, obtain ethyl acetate in the tower;
(3) debris is discharged at the bottom of tower; Hair oil is extracted out from cat head, after the condensation, carried out phase-splitting and handle, obtain water and oil phase, water is discharged, the part oil phase refluxes, and reflux ratio is 8: 1, and all the other oil phases reclaim;
(4) the ethyl acetate cooling that obtains of Jiang Tazhong, partial reflux, its reflux ratio is 5: 1, the finished product that all the other ethyl acetate make for the present invention.
In the rectifying tower, the tower internal pressure is 1.1am, and tower top temperature is 78 ℃, and temperature is 85 ℃ in the tower, and column bottom temperature is 90 ℃.
It is as shown in the table to separate each component concentration of back:
Energy consumption in the above-mentioned sepn process is as shown in the table:
| Project | Load (kw) | |
| Public utility | The rectifying tower reboiler | 680.9 |
| The rectifying tower condenser duty | 406.1 | |
| Total load kw | 1071.0 | |
| Energy consumption (KJ/Kg ethyl acetate) | 1226.3 | |
| Traditional technology production energy consumption (KJ/Kg ethyl acetate) | 2300 | |
The energy consumption that the dehydration of ethyl acetate is purified drops to 1226.3KJ/Kg from 2300KJ/Kg.
Embodiment 3
(1) it is 76 ℃ with temperature, the thick ester of ethyl acetate of ethanol, 96.95% (weight) of water, 1.86% (weight) that contains the acetate, 1.17% (weight) of 0.012% (weight) enters the rectifying tower middle part with the flow of 3150kg/h, forms ethanol, water and ethyl ester ternary azeotrope;
(2) obtain containing the hair oil of ethanol, water and amount of ethyl acetate after the ternary azeotrope rectifying at cat head, obtain containing the debris of acetate at the bottom of the tower, obtain ethyl acetate in the tower;
(3) debris is discharged at the bottom of tower; Hair oil is extracted out from cat head, after the condensation, carried out phase-splitting and handle, obtain water and oil phase, water is discharged, the part oil phase refluxes, and reflux ratio is 11: 1, and all the other oil phases reclaim;
(4) the ethyl acetate cooling that obtains of Jiang Tazhong, partial reflux, its reflux ratio is 3: 1, the finished product that all the other ethyl acetate make for the present invention.
In the rectifying tower, the tower internal pressure is 1.3am, and tower top temperature is 75 ℃, and temperature is 87 ℃ in the tower, and column bottom temperature is 85 ℃.
It is as shown in the table to separate each component concentration of back:
Energy consumption in the above-mentioned sepn process is as shown in the table:
| Project | Load (kw) | |
| Public utility | The rectifying tower reboiler | 681.9 |
| The rectifying tower condenser duty | 405.1 | |
| Total load kw | 1087.0 | |
| Energy consumption (KJ/Kg ethyl acetate) | 1242.3 | |
| Traditional technology production energy consumption (KJ/Kg ethyl acetate) | 2300 | |
The energy consumption that the dehydration of ethyl acetate is purified drops to 1242.3KJ/Kg from 2300KJ/Kg, and energy consumption reduces by 46%.
Claims (2)
1, a kind of method of ethyl acetate dehydration purification comprises the steps:
(1) is 75 ℃～78 ℃ with temperature, contains water, acetate, the thick ethyl acetate of alcoholic acid and enter in the tower, form ethanol, water and ethyl ester ternary azeotrope from the rectifying tower middle part;
(2) obtain containing the hair oil of ethanol, water and amount of ethyl acetate after the ternary azeotrope rectifying at cat head, obtain containing the debris of acetate at the bottom of the tower, obtain ethyl acetate in the tower;
(3) debris is discharged at the bottom of tower; Hair oil is extracted out from cat head, after the condensation, carried out phase-splitting and handle, obtain water and oil phase, water is discharged, the part oil phase refluxes, and reflux ratio is 6～11: 1, and all the other oil phases reclaim;
(4) the ethyl acetate cooling that obtains of Jiang Tazhong, partial reflux, its reflux ratio is 1～5: 1, the finished product that all the other ethyl acetate make for the present invention.
2, method according to claim 1 is characterized in that in the described rectifying tower that the tower internal pressure is 1.0am～1.3am, and tower top temperature is 70 ℃～78 ℃, and temperature is 80 ℃～87 ℃ in the tower, and column bottom temperature is 83 ℃～90 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100330488A CN100357250C (en) | 2006-01-18 | 2006-01-18 | Ethyl acetate dehydrating extraction method |
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| CNB2006100330488A CN100357250C (en) | 2006-01-18 | 2006-01-18 | Ethyl acetate dehydrating extraction method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148407B (en) * | 2007-10-16 | 2010-04-14 | 南京师范大学 | Method for extracting ethyl acetate from ketoconazole production by continuous side line discharging method |
| CN106693429A (en) * | 2016-05-20 | 2017-05-24 | 百川化工(如皋)有限公司 | Treatment system and method for ethyl acetate production water |
| CN108358754A (en) * | 2018-04-03 | 2018-08-03 | 烟台国邦化工机械科技有限公司 | The process and system of a kind of separating alcohol, ethyl acetate and aqueous mixtures |
| CN109096066A (en) * | 2018-09-29 | 2018-12-28 | 天津科林泰克科技有限公司 | A kind of method and device removed and recycle butyl glycol ether in coating waste-water |
| CN112299999A (en) * | 2020-11-13 | 2021-02-02 | 南京化学试剂股份有限公司 | Refining method of high-purity ethyl acetate |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076337C (en) * | 1996-12-18 | 2001-12-19 | 中国科学院成都有机化学研究所 | Constant boiling agent for separating ethyl acetate and constant boiling distillation process |
| CN1210851A (en) * | 1997-09-08 | 1999-03-17 | 中国科学院成都有机化学研究所 | Process for purifying ethyl acetate |
| JP2001139523A (en) * | 1999-11-18 | 2001-05-22 | Daikin Ind Ltd | Method for purifying carboxylic acid esters |
| GB0410603D0 (en) * | 2004-05-12 | 2004-06-16 | Bp Chem Int Ltd | Ester synthesis |
| CN100497291C (en) * | 2004-09-14 | 2009-06-10 | 上海吴泾化工有限公司 | Esterification tower reaction separation flow process for producing ethyl acetate |
| CN1325463C (en) * | 2005-04-25 | 2007-07-11 | 上海吴泾化工有限公司 | High purity ethyl acetate purifying and refining tower and its application |
| CN1312105C (en) * | 2005-04-27 | 2007-04-25 | 上海吴泾化工有限公司 | Method for purifying and refining ethyl acetate in high purity |
-
2006
- 2006-01-18 CN CNB2006100330488A patent/CN100357250C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148407B (en) * | 2007-10-16 | 2010-04-14 | 南京师范大学 | Method for extracting ethyl acetate from ketoconazole production by continuous side line discharging method |
| CN106693429A (en) * | 2016-05-20 | 2017-05-24 | 百川化工(如皋)有限公司 | Treatment system and method for ethyl acetate production water |
| CN108358754A (en) * | 2018-04-03 | 2018-08-03 | 烟台国邦化工机械科技有限公司 | The process and system of a kind of separating alcohol, ethyl acetate and aqueous mixtures |
| CN108358754B (en) * | 2018-04-03 | 2024-02-27 | 烟台国邦化工机械科技有限公司 | Process method and system for separating ethanol, ethyl acetate and water mixture |
| CN109096066A (en) * | 2018-09-29 | 2018-12-28 | 天津科林泰克科技有限公司 | A kind of method and device removed and recycle butyl glycol ether in coating waste-water |
| CN109096066B (en) * | 2018-09-29 | 2021-07-30 | 天津科林泰克科技有限公司 | Method and device for removing and recycling ethylene glycol butyl ether in coating wastewater |
| CN112299999A (en) * | 2020-11-13 | 2021-02-02 | 南京化学试剂股份有限公司 | Refining method of high-purity ethyl acetate |
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| CN100357250C (en) | 2007-12-26 |
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