CN105439858A - Purification method for ethyl acetate - Google Patents
Purification method for ethyl acetate Download PDFInfo
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- CN105439858A CN105439858A CN201510601855.4A CN201510601855A CN105439858A CN 105439858 A CN105439858 A CN 105439858A CN 201510601855 A CN201510601855 A CN 201510601855A CN 105439858 A CN105439858 A CN 105439858A
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- ethyl acetate
- tower
- ethanol
- goes out
- water
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a purification method for ethyl acetate. The purification method comprises the following steps of: (1) at least using an extraction column A, an ethyl acetate distillation column B, an extractant recovery column C and and a 95% ethanol recovery column D; (2) discharging an ethyl acetate solution layer from the top of the extraction column, and an extractant layer from at the bottom of the extraction column; (3) discharging an ethyl acetate layer from at the top of the ethyl acetate distillation column B, and the mixture of the extractant, a small amount of ethanol and water from the bottom of the ethyl acetate distillation column B; (4) discharging an extractant layer from the bottom of the the extractant recovery column C, and the mixture of acetic acid, water and ethyl acetate coming out from the top portion of the extractant recovery column C; and further discharging a ternary azeotrope of ethyl acetate, water and ethanol from the top of the 95% ethanol recovery column, 95% ethanol from the middle lower part of the the 95% ethanol recovery column, and water from the bottom of the 95% ethanol recovery column. The purification method disclosed by the present invention is high in purification and separation efficiency of the ethyl acetate and good in separation effect.
Description
Technical field
The present invention relates to chemical field, particularly a kind of purification process of ethyl acetate.
Background technology
Ethyl acetate is a kind of important industrial chemicals, has a wide range of applications in spices, medicine and paint industry.In the commercial run of production ethyl acetate, as production methods such as ethanol and acetic acid direct esterification, Catalytic oxidation of ethanol method or catalysis denitrogenations, all relate to water, alcohol is separated with ethyl acetate, separation method of the prior art is all generally utilize ethyl acetate itself to form this feature of ternary azeotrope with water and ethanol, in phase splitter, two-phase is divided into after the cooling of ternary azeotrope steam, light is ester phase mutually, is rich in ethyl acetate, another containing a small amount of second alcohol and water.Heavy phase and aqueous phase, be rich in water, secondly containing ethanol and ethyl acetate, delivers to ethyl acetate recovery tower and go to reclaim acetic acid wherein and ethyl acetate.Light mutually in part backflow, another part is to rectifying tower, and tower top steams that acetic acid second is intoxicated, the ternary azeotrope of second alcohol and water, and tower reactor leaves product ethyl acetate, but to obtain 99% ethyl acetate generally will through three grades of rectifying.The advantage of the method utilizes product ethyl acetate itself as nonvariant boiling reagent, its shortcoming is that the ester phase water content in normal temperature and pressure quantizer is more, poor as its band outlet capacity of phegma, larger reflux ratio (R=4) need be kept, go to produce the intoxicated ester phase amount of acetic acid second not quite so be sent to dehydration tower, make output limited.In addition, the ester phase water content delivered in esterification column and dehydration tower is high, so energy consumption is larger.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of purification process of ethyl acetate, this method reduces operation energy consumption, and the ethyl acetate purity obtained is high.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of purification process of ethyl acetate, is characterized in that: (1) at least comprises extraction tower A, ethyl acetate rectifying tower B, extraction agent recovery tower C and 95% ethanol recovery tower D; (2) the extraction tower tower top described in goes out ethyl acetate solution layer, and bottom goes out to extract oxidant layer; (3) the ethyl acetate rectifying tower B top described in goes out pure ethyl acetate layer, and bottom goes out the mixture of extraction agent, a small amount of second alcohol and water; (4) the extraction agent recovery tower C described in, bottom goes out to extract oxidant layer.Top goes out acetic acid, the mixture of water and ethyl acetate; In a preferred embodiment of the present invention, also comprise, described extraction agent enters extraction tower from top, and described ethyl acetate-ethanol and the extract of water enter extraction tower from bottom.
In a preferred embodiment of the present invention, the extract layer of described step (3) part is recyclable and extract with merging for the extract layer in step (1);
In a preferred embodiment of the present invention, also comprise the recovery tower of 95% ethanol described in (5), its top goes out ethyl acetate, the ternary azeotrope of water and ethanol, and middle and lower part goes out 95% ethanol, bottom water outlet.
In a preferred embodiment of the present invention, described extraction agent is Isosorbide-5-Nitrae butyleneglycol and glycerol.
In a preferred embodiment of the present invention, described ethyl acetate tower internal pressure controls at 400-900kpa.
In a preferred embodiment of the present invention, the vacuum degree control in described extraction agent recovery tower is at 1-6*10
4pa.
The invention has the beneficial effects as follows: the energy consumption that present invention reduces reaction, the purity of reaction is high, adopts extraction agent to extract, simultaneously can extraction agent reusable edible, has saved cost, has had significant economy and practicality.
Figure of description
Fig. 1 is the schema of ethyl acetate purification process provided by the invention.
Embodiment
The specific embodiment of the present invention is described in detail as follows with reference to accompanying drawing, but for illustrative purposes only instead of restriction the present invention.
The purification process of ethyl acetate provided by the invention refers to accompanying drawing 1, comprises extraction tower A, ethyl acetate rectifying tower B, extraction agent recovery tower C and 95% ethanol recovery tower D; Described extraction agent 1 enters extraction tower A from top, and the extract 2 of described ethyl acetate-ethanol and water enters extraction tower A from bottom; Described extraction tower A tower top goes out ethyl acetate solution layer 3, and bottom goes out to extract oxidant layer 4; Described ethyl acetate rectifying tower B top goes out pure ethyl acetate layer 5, and bottom goes out the mixture 6 of extraction agent, a small amount of second alcohol and water; Described extraction agent recovery tower C, bottom goes out to extract oxidant layer 7.Top goes out acetic acid, the mixture 8 of water and ethyl acetate.
In addition, invention further provides extract layer 7 recyclable and extract with merging for the extraction 4 in extraction tower A; The recovery tower D of 95% described ethanol, its top goes out ethyl acetate, the ternary azeotrope 9 of water and ethanol, and middle and lower part goes out 95% ethanol 10, bottom water outlet 11.Described extraction agent is BDO and glycerol.Described ethyl acetate tower internal pressure controls at 400-900kpa; Vacuum degree control in described extraction agent recovery tower is at 1-6*10
4pa.
The analytical procedure of each logistics all adopts gas Hunan chromatography quantitative
The thick ester that the charging of embodiment 1. extraction tower A and direct esterification obtain forms close, ethyl acetate about 88%, ethanol 6%, water 6% (weight percentage, as follows).The extraction agent recycled is that BDO adds from tower top, and thick vinegar adds at the bottom of tower, sampling analysis after operate continuously is stable.Products obtained therefrom ethyl acetate purity on average reaches 99.0%.
According to example 2, but the apple added to get agent be glycerol, ethyl acetate purity reaches 98.5%.
Claims (8)
1. a purification process for ethyl acetate, is characterized in that: (1) by extraction tower A, ethyl acetate rectifying tower B, extraction agent recovery tower C and 95% ethanol recovery tower D; (2) the extraction tower tower top described in goes out ethyl acetate solution layer, and bottom goes out to extract oxidant layer;
(3) the ethyl acetate rectifying tower B top described in goes out pure ethyl acetate layer, and bottom goes out the mixture of extraction agent, a small amount of second alcohol and water;
(4) the extraction agent recovery tower C described in, bottom goes out to extract oxidant layer.
2. top goes out acetic acid, the mixture of water and ethyl acetate.
3. the purification process of ethyl acetate according to claim 1, is characterized in that, also comprises, and described extraction agent enters extraction tower from top, and described ethyl acetate-ethanol and the extract of water enter extraction tower from bottom.
4. according to wanting the purification process of ethyl acetate according to claim 1, it is characterized in that, the extract layer of described step (3) part is recyclable and extract with merging for the extract layer in step (1).
5. the purification process of ethyl acetate according to claim 1, is characterized in that, also comprise the recovery tower of 95% ethanol described in (5), its top goes out ethyl acetate, the ternary azeotrope of water and ethanol, and middle and lower part goes out 95% ethanol, bottom water outlet.
6. the purification process of ethyl acetate according to claim 1, is characterized in that, described extraction agent is BDO and glycerol.
7. the purification process of ethyl acetate according to claim 1, is characterized in that, described ethyl acetate tower internal pressure controls at 400-900kpa.
8. the purification process of ethyl acetate according to claim 1, is characterized in that, the vacuum degree control in described extraction agent recovery tower is at 1-6*10
4pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510601855.4A CN105439858A (en) | 2015-09-21 | 2015-09-21 | Purification method for ethyl acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510601855.4A CN105439858A (en) | 2015-09-21 | 2015-09-21 | Purification method for ethyl acetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105439858A true CN105439858A (en) | 2016-03-30 |
Family
ID=55550562
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510601855.4A Pending CN105439858A (en) | 2015-09-21 | 2015-09-21 | Purification method for ethyl acetate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105439858A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06336455A (en) * | 1993-05-28 | 1994-12-06 | Showa Denko Kk | Purification of ethyl acetate |
| 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 |
| CN104177257A (en) * | 2014-08-06 | 2014-12-03 | 太仓市金锚化工有限公司 | Purification method of ethyl acetate |
-
2015
- 2015-09-21 CN CN201510601855.4A patent/CN105439858A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06336455A (en) * | 1993-05-28 | 1994-12-06 | Showa Denko Kk | Purification of ethyl acetate |
| 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 |
| CN104177257A (en) * | 2014-08-06 | 2014-12-03 | 太仓市金锚化工有限公司 | Purification method of ethyl acetate |
Non-Patent Citations (1)
| Title |
|---|
| 雷良恒: "加盐萃取-恒沸精馏联合过程研究III.乙酸乙酯提浓新工艺", 《石油化工》 * |
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Application publication date: 20160330 |
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