CN103351276B - 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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- CN103351276B CN103351276B CN201310271293.2A CN201310271293A CN103351276B CN 103351276 B CN103351276 B CN 103351276B CN 201310271293 A CN201310271293 A CN 201310271293A CN 103351276 B CN103351276 B CN 103351276B
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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 a kind of intermittent extraction, distillation and separation method 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.By the top toward rectifying tower, add continuously extraction agent to reach separated object with the relative volatility changing between stock blend.The batch extracting rectified advantage that has merged batch fractionating and extracting rectifying, flexible operation, can separated a plurality of components by a tower, and facility investment is little, is applicable to the separated 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 producing in fine chemistry industry production process, because benzene and ethanol form azeotrope (massfraction of ethanol is 32.4%), be difficult to separated, if do not reclaimed, not only pollute the environment, and 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 ethanol-benzene azeotropic system separation of extractive distillation aspect of publishing.
Summary of the invention
The object of the present invention is to provide a kind of intermittent extraction, distillation and separation method 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 form, batch extracting rectified separating alcohol-benzene azeotropic mixture, is characterized in that comprising following process:
To contain halohydrocarbon or the arene of two above halogenic substituents, 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 tower top 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 tower top temperature is 78.5-82.5 ℃, with reflux ratio 3:1-10:1, by overhead extraction ethanol-benzene transition section I, and stop adding extraction agent; When extracting rectifying tower top temperature is 82.5-83.4 ℃, with reflux ratio 0.5:1-6:1 by overhead extraction benzene; When extracting rectifying tower top temperature surpasses 83.4 ℃, with reflux ratio 1:1-12:1 by overhead extraction benzene-extraction agent transition section II; When the extraction agent composition of heating kettle reaches requirement, stop cooling, extraction agent is pumped into high-level storage groove, heating kettle packs new a collection of ethanol-benzol mixture and transition section I and transition section II into, lower batch of batch extracting rectified separation.
Idiographic flow (see photo): ethanol-benzol mixture adds in heating kettle 3, open the thermal source of heating kettle and the low-temperature receiver of condenser 4, until extracting rectifying tower top 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 in extracting rectifying tower top overhead product, ethanol content is lower than product requirement, when the material of overhead extraction enters transition section I receiving tank 6(ethanol content in extracting rectifying tower top overhead product and is less than azeotropic and forms, stop adding extraction agent), when in extracting rectifying tower top overhead product, benzene content reaches product requirement, the material of extraction enters receiving tank 7, when in extracting rectifying tower top overhead product, benzene content is lower than product requirement, the material of extraction enters transition section II receiving tank 8, when the composition of heating kettle extraction agent reaches requirement, stop.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 heating kettle 3 during next batch rectifying again.
The invention has the advantages that and use rationally effectively extraction agent to destroy ethanol-benzene azeotropic system, isolate high pure benzene, alcohol product, adopt single tower operation, flexible operation, cost of equipment less investment.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention and schematic flow sheet.In 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% at heating kettle, to drop into 500 L ethanol-benzene azeotropic mixtures, ethanol 30%, be mass percent), testing selected extraction agent is 1, 2, 3-trichloropropane, open heating kettle thermal source and condenser low-temperature receiver, until extracting rectifying tower top, reflux after for some time, tower top temperature is stable, add extraction agent, tower top place is being closed in extractant feed position, control extraction agent and add speed 500 L/h, total reflux operation, when extracting rectifying tower top temperature is 78-78.5 ℃, in overhead product, ethanol content >=99% starts discharging, reflux ratio is 3:1, discharging speed is 200 L/h.When extracting rectifying tower top temperature is 78.5-82.5 ℃, extraction ethanol-benzene transition section, and stop adding extraction agent, reflux ratio is 9:1, when extracting rectifying tower top temperature is 82.5-83.4 ℃, in overhead product during benzene content >=99%, receive benzene, reflux ratio is 4:1, when extracting rectifying tower top temperature surpasses 83.4 ℃, reflux ratio 5:1, extraction benzene-methyl-sulphoxide transition section II, in extracting rectifying tower top overhead product during glyceryl trichloride content >=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 (1)
1. an intermittent extraction, distillation and separation method for ethanol-benzene azeotropic mixture, the method adopts and comprises extractive distillation column, heating kettle, condenser, high-level storage groove, the extracting rectifying device that receiving tank and products pot form, batch extracting rectified separating alcohol-benzene azeotropic mixture; It is characterized in that with 1,2-propylene dichloride, glyceryl trichloride, orthodichlorobenzene or 1，2，3-trichlorobenzene for extraction agent; Comprise 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 tower top 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 tower top temperature is 78.5-82.5 ℃, with reflux ratio 3:1-10:1, by overhead extraction ethanol-benzene transition section I, and stop adding extraction agent; When extracting rectifying tower top temperature is 82.5-83.4 ℃, with reflux ratio 0.5:1-6:1 by overhead extraction benzene; When extracting rectifying tower top temperature surpasses 83.4 ℃, with reflux ratio 1:1-12:1 by overhead extraction benzene-extraction agent transition section II; When the extraction agent composition of heating kettle reaches requirement, stop cooling, extraction agent is pumped into high-level storage groove, heating kettle packs new a collection of ethanol-benzol mixture and transition section I and transition section II into, lower batch of batch extracting rectified separation.
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| CN104610021A (en) * | 2015-01-12 | 2015-05-13 | 济南大学 | Method for continuous extractive distillation and separation of ethanol-toluene azeotrope with mixed solvent |
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| 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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| 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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| 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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| 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》.2006,(第10期),第15－17页. * |
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| CN104610021A (en) * | 2015-01-12 | 2015-05-13 | 济南大学 | Method for continuous extractive distillation and separation of ethanol-toluene azeotrope with mixed solvent |
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