CN103351276A - Batch extractive distillation and separation method for ethanol-benzene azeotrope - Google Patents
Batch extractive distillation and separation method for ethanol-benzene azeotrope Download PDFInfo
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- CN103351276A CN103351276A CN2013102712932A CN201310271293A CN103351276A CN 103351276 A CN103351276 A CN 103351276A CN 2013102712932 A CN2013102712932 A CN 2013102712932A CN 201310271293 A CN201310271293 A CN 201310271293A CN 103351276 A CN103351276 A CN 103351276A
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Abstract
The invention discloses a batch extractive distillation and separation method for ethanol-benzene azeotrope, and belongs to the separation technology of ethanol-benzene azeotrope. The method adopts halogenated hydrocarbon or aromatic hydrocarbon, which contains two or more halogen substituents such as 1,2-dichloropropane, 1,2,3-trichloropropane, o dichlorobenzene, and 1,2,3-trichloro-benzenes, as the extractant. Operation condition of extractive distillation column is that the mass ratio of extractant to overhead is in the range of 0.5:1 to 10:1. Ethanol, ethanol-benzene transition section I, benzene, and benzene-benzene extractant transition section II are respectively extracted from the top of the extractive distillation column by controlling different temperature and different reflux ratio of the top of the extractive distillation column. When the composition of the extractant in the bottom of the column meets the requirement, the extractant is pumped into a high-position storage tank for recycling. The batch extractive distillation and separation method for ethanol-benzene azeotrope has the advantages that ethanol-benzene azeotropic system is broken by extractant, so high-pure ethanol and benzene products are extracted, operation of single column is simple, and equipment cost is low.
Description
Technical field
The present invention relates to the intermittent extraction, distillation and separation method of a kind of ethanol-benzene azeotropic mixture, belong to the isolation technique of ethanol-benzene azeotropic mixture.
Background technology
Extracting rectifying is a kind of special extract rectification isolation technique, the separation of applicable azeotropic system.Add continuously extraction agent by the top toward rectifying tower and reach the separation purpose with the relative volatility that changes between stock blend.The batch extracting rectified advantage that has merged batch fractionating and extracting rectifying, flexible operation can separate a plurality of components by a tower, and facility investment is little, is applicable to separating of short run azeotropic system and the system of closely boiling.The chemical structural formula of ethanol is: CH
3CH
2OH, industrial being widely used.Ethanol-the benzol mixture that in the fine chemistry industry production process, produces, owing to forming azeotrope (massfraction of ethanol is 32.4%), benzene and ethanol is difficult to separate, as not reclaiming, not only pollute the environment, and the increase production cost, the separation method of therefore developing ethanol-benzene azeotropic mixture has important meaning.About article and the patent of extracting rectifying aspect are a lot, there is not yet the data of the ethanol published-benzene azeotropic system separation of extractive distillation aspect.
Summary of the invention
The object of the present invention is to provide the intermittent extraction, distillation and separation method of a kind of ethanol-benzene azeotropic mixture.The isolated benzene of the method, alcohol product purity are high.
The present invention is realized by following technical proposals.Employing comprises extractive distillation column, heating kettle, and condenser, high-level storage groove, the extracting rectifying device that receiving tank and products pot consist of, batch extracting rectified separating alcohol-benzene azeotropic mixture is characterized in that comprising following process:
With halohydrocarbon or the arene that contains two above halogenic substituents, such as 1,2-propylene dichloride, glyceryl trichloride, orthodichlorobenzene and 1,2,3-trichlorobenzene etc. is extraction agent, and extractive distillation column operates with following condition, under normal pressure, entering the extraction agent of extractive distillation column and the mass ratio of this overhead product is 0.5:1-10:1, and the feeding temperature of extraction agent is 20-60 ℃.When extracting rectifying cat head temperature is 78-78.5 ℃, with reflux ratio 1:1-6:1 by the qualified alcohol product of overhead extraction ethanol content; When extracting rectifying cat head temperature is 78.5-82.5 ℃, by overhead extraction ethanol-benzene transition section I, and stop to add extraction agent with reflux ratio 3:1-10:1; When extracting rectifying cat head temperature is 82.5-83.4 ℃, with reflux ratio 0.5:1-6:1 by overhead extraction benzene; When extracting rectifying cat head temperature surpasses 83.4 ℃, with reflux ratio 1:1-12:1 by overhead extraction benzene-extraction agent transition section II; When the extraction agent of heating kettle forms when reaching requirement, the cooling of stopping pumps into high-level storage groove with extraction agent, heating kettle pack into new a collection of ethanol-benzol mixture and transition section I and transition section II, lower batch of batch extracting rectified separation.
The idiographic flow (see photo): ethanol-benzol mixture adds in the heating kettle 3, open the thermal source of heating kettle and the low-temperature receiver of condenser 4, until the extracting rectifying cat head reflux and tower top temperature stable after, extraction agent is introduced into extractive distillation column 2 tops from high-order storage tank 1, total reflux for some time, discharging when ethanol content reaches requirement, enter receiving tank 4, when ethanol content is lower than product requirement in the extracting rectifying cat head overhead product, the material of overhead extraction enters transition section I receiving tank 6(when ethanol content forms less than azeotropic in the extracting rectifying cat head overhead product, stop to add extraction agent), when benzene content reaches product requirement in the extracting rectifying cat head overhead product, the material of extraction enters receiving tank 7, when benzene content is lower than product requirement in the extracting rectifying cat head overhead product, the material of extraction enters transition section II receiving tank 8, when the composition of heating kettle extraction agent reaches requirement, stops.Heating kettle is high-purity extraction agent, squeezes into high-level storage groove 1 and recycles.The material of transition section I and II is put in the heating kettle 3 during next batch rectifying again.
The invention has the advantages that and use rationally effectively extraction agent destruction ethanol-benzene azeotropic system, isolate high pure benzene, alcohol product, adopt single tower operation, flexible operation, cost of equipment less investment.
Description of drawings
Fig. 1 is apparatus of the present invention and schematic flow sheet.Among the figure: 1-high-level storage groove, 2-extractive distillation column, 3-heating kettle, 4-condenser, 5-alcohol product receiving tank, 6-transition section I receiving tank, 7-benzaldehyde product receiving tank, 8-transition section II receiving tank.
Embodiment
Embodiment 1: adopt batch extraction rectification device, (wherein benzene 70% to drop into 500 L ethanol-benzene azeotropic mixture at heating kettle, ethanol 30%, be mass percent), testing selected extraction agent is 1,2, the 3-trichloropropane, open heating kettle thermal source and condenser low-temperature receiver, after the extracting rectifying cat head refluxed for some time, tower top temperature was stable, add extraction agent, the cat head place is being closed in the extractant feed position, and the control extraction agent adds speed 500 L/h, total reflux operation, when extracting rectifying cat head temperature is 78-78.5 ℃, ethanol content in the overhead product 〉=99% beginning discharging, reflux ratio is 3:1, discharging speed is 200 L/h.When extracting rectifying cat head temperature is 78.5-82.5 ℃, extraction ethanol-benzene transition section, and stop to add extraction agent, reflux ratio is 9:1, when extracting rectifying cat head temperature is 82.5-83.4 ℃, during benzene content in the overhead product 〉=99%, receive benzene, reflux ratio is 4:1, when extracting rectifying cat head temperature surpasses 83.4 ℃, reflux ratio 5:1, extraction benzene-methyl-sulphoxide transition section II, when glyceryl trichloride content in the extracting rectifying cat head overhead product 〉=99%, stop, heating kettle is high-purity glyceryl trichloride.
Embodiment 2: experimental installation and working method are with embodiment 1, and extraction agent adopts 1,2-propylene dichloride.
Claims (3)
1. the intermittent extraction, distillation and separation method of ethanol-benzene azeotropic mixture, the method adopt and comprise extractive distillation column, heating kettle, condenser, high-level storage groove, the extracting rectifying device that receiving tank and products pot consist of, batch extracting rectified separating alcohol-benzene azeotropic mixture.
2. the intermittent extraction, distillation and separation method of a kind of ethanol as claimed in claim 1-benzene azeotropic mixture, it is characterized in that containing halohydrocarbon or the arene of two above halogenic substituents, such as 1,2-propylene dichloride, 1,2,3-trichloropropane, orthodichlorobenzene and 1，2，3-trichlorobenzene etc. are extraction agent.
3. the intermittent extraction, distillation and separation method of a kind of ethanol as claimed in claim 2-benzene azeotropic mixture, it is characterized in that comprising following process: extractive distillation column operates with following condition, under normal pressure, entering the extraction agent of extractive distillation column and the mass ratio of this overhead product is 0.5:1-10:1, the feeding temperature of extraction agent is 20-60 ℃, when extracting rectifying cat head temperature is 78-78.5 ℃, with reflux ratio 1:1-6:1 by the qualified alcohol product of overhead extraction ethanol content; When extracting rectifying cat head temperature is 78.5-82.5 ℃, by overhead extraction ethanol-benzene transition section I, and stop to add extraction agent with reflux ratio 3:1-10:1; When extracting rectifying cat head temperature is 82.5-83.4 ℃, with reflux ratio 0.5:1-6:1 by overhead extraction benzene; When extracting rectifying cat head temperature surpasses 83.4 ℃, with reflux ratio 1:1-12:1 by overhead extraction benzene-extraction agent transition section II; When the extraction agent of heating kettle forms when reaching requirement, the cooling of stopping pumps into high-level storage groove with extraction agent, heating kettle pack into new a collection of ethanol-benzol mixture and transition section I and transition section II, lower batch of batch extracting rectified separation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104628522A (en) * | 2015-01-12 | 2015-05-20 | 济南大学 | Intermittent extractive distillation process for ethanol-methylbenzene azeotropic mixture |
| CN112778087A (en) * | 2021-01-14 | 2021-05-11 | 山东科技大学 | Method for separating methanol-toluene azeotrope through continuous extractive distillation |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610021B (en) * | 2015-01-12 | 2017-03-08 | 济南大学 | A kind of method of mixed solvent continuous extraction rectification separating alcohol toluene azeotropic mixture |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627536A (en) * | 2012-03-23 | 2012-08-08 | 济南大学 | Batch extractive distillation separation method of methylal-methanol azeotropic mixture |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102627536A (en) * | 2012-03-23 | 2012-08-08 | 济南大学 | Batch extractive distillation separation method of methylal-methanol azeotropic mixture |
Non-Patent Citations (1)
| Title |
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| 彭昌荣等: "乙醇－苯混合物变压精馏的模拟及优化", 《化学工程师》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104628522A (en) * | 2015-01-12 | 2015-05-20 | 济南大学 | Intermittent extractive distillation process for ethanol-methylbenzene azeotropic mixture |
| CN112778087A (en) * | 2021-01-14 | 2021-05-11 | 山东科技大学 | Method for separating methanol-toluene azeotrope through continuous extractive distillation |
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