CN103351276B - Batch extractive distillation and separation method for ethanol-benzene azeotrope - Google Patents

Batch extractive distillation and separation method for ethanol-benzene azeotrope Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
benzene
ethanol
extractive distillation
extraction
extraction agent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201310271293.2A
Other languages
Chinese (zh)
Other versions
CN103351276A (en
Inventor
姜占坤
袁美龙
孙国新
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Jinan
Original Assignee
University of Jinan
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Jinan filed Critical University of Jinan
Priority to CN201310271293.2A priority Critical patent/CN103351276B/en
Publication of CN103351276A publication Critical patent/CN103351276A/en
Application granted granted Critical
Publication of CN103351276B publication Critical patent/CN103351276B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

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

The intermittent extraction, distillation and separation method of ethanol-benzene azeotropic mixture
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.
CN201310271293.2A 2013-07-01 2013-07-01 Batch extractive distillation and separation method for ethanol-benzene azeotrope Expired - Fee Related CN103351276B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310271293.2A CN103351276B (en) 2013-07-01 2013-07-01 Batch extractive distillation and separation method for ethanol-benzene azeotrope

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310271293.2A CN103351276B (en) 2013-07-01 2013-07-01 Batch extractive distillation and separation method for ethanol-benzene azeotrope

Publications (2)

Publication Number Publication Date
CN103351276A CN103351276A (en) 2013-10-16
CN103351276B true CN103351276B (en) 2014-10-15

Family

ID=49307714

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310271293.2A Expired - Fee Related CN103351276B (en) 2013-07-01 2013-07-01 Batch extractive distillation and separation method for ethanol-benzene azeotrope

Country Status (1)

Country Link
CN (1) CN103351276B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Families Citing this family (2)

* Cited by examiner, † Cited by third party
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

Citations (1)

* Cited by examiner, † Cited by third party
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

Patent Citations (1)

* Cited by examiner, † Cited by third party
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
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. *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Also Published As

Publication number Publication date
CN103351276A (en) 2013-10-16

Similar Documents

Publication Publication Date Title
CN102627536B (en) Batch extractive distillation separation method of methylal-methanol azeotropic mixture
CN103288581A (en) Batch extractive distillation separation method of benzene-propyl alcohol azeotropic mixture
CN109206291A (en) A kind of separation method of chloromethanes-dimethyl ether
CN106674292B (en) A kind of purification processing method of Sucralose water crystallization mother liquor
CN103351276B (en) Batch extractive distillation and separation method for ethanol-benzene azeotrope
CN102584525A (en) Intermittent extractive distillation separation method of methanol-methyl propionate azeotropic mixtures
CN105175280A (en) Acetonitrile-tert-butanol azeotropic mixture continuous extraction rectification separation method
CN103304373A (en) Batch extraction-rectification-separation method of dichloromethane-methanol azeotropic mixture
CN106699511B (en) Method for recycling organic/inorganic matters in glycerol chlorination distillate
CN102527072B (en) Batch extraction distillation separation method for propyl alcohol-propyl formate azeotropic mixture
CN107915640B (en) Extractive distillation separation method of dimethyl carbonate and methanol
CN101182277B (en) Method for extracting biphenyl from medium wash oil
CN101830830B (en) Method for separating acetonitrile-toluene by extractive distillation through dividing wall rectifying tower
CN106478339B (en) Method for separating cyclopentane and 2, 2-dimethylbutane
CN106008186A (en) Method for separating acetone, isopropanol and water mixed solution
CN103319309A (en) Interrupted extraction, rectification and separation method of methanol-nitromethane azeotrope
CN104876788A (en) Benzene-propyl alcohol azeotrope continuous extractive distillation technology based on choline chloride/urea low co-melting solvent
CN104447636A (en) Method and device for separating ethanol-tetrahydrofuran by extractive distillation by using dividing tower
CN105175260A (en) DL-sec-butyl acetate-isobutanol azeotropic mixture continuous extraction rectification separation method
CN105037071A (en) Method for continuous extraction distillation separation of methylbenzene-propylene glycol monomethyl ether azeotropic mixture
CN104829426A (en) Continuous isopropyl ether-isopropyl alcohol azeotrope extraction and rectification technology based on choline chloride/urea low-co-melting solvent
CN104370694A (en) Separation method of isobutanol-ethyl isobutyrate azeotrope by batch extraction rectification
CN204111623U (en) A kind of process unit of purifying for by product diisopropyl ether in Virahol production
CN111202999B (en) Rectification device and method for extracting high-purity mesitylene product from oil generated by isomerization reaction of trimethylbenzene
CN112679352B (en) Refining method and system for mixed material flow containing dimethyl carbonate

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20141015

Termination date: 20150701

EXPY Termination of patent right or utility model