CN104370694A - Separation method of isobutanol-ethyl isobutyrate azeotrope by batch extraction rectification - Google Patents

Separation method of isobutanol-ethyl isobutyrate azeotrope by batch extraction rectification Download PDF

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Publication number
CN104370694A
CN104370694A CN201410619922.0A CN201410619922A CN104370694A CN 104370694 A CN104370694 A CN 104370694A CN 201410619922 A CN201410619922 A CN 201410619922A CN 104370694 A CN104370694 A CN 104370694A
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CN
China
Prior art keywords
ethyl isobutyrate
isobutanol
extractants
isopropylcarbinol
tower
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CN201410619922.0A
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Chinese (zh)
Inventor
姜占坤
刘顺江
孙国新
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University of Jinan
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University of Jinan
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Priority to CN201410619922.0A priority Critical patent/CN104370694A/en
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/40—Extractive distillation
    • 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
    • C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a separation method of an isobutanol-ethyl isobutyrate azeotrope by batch extraction rectification, which comprises the following steps: ethylene glycol and an ionic liquid 1-ethyl-3-methylimidazolyl acetate are used as extractants; under normal pressure or reduced pressure, the mass ratio of the extractants entering an extraction rectification tower to the overhead is (1.8-5):1; the charging temperature of the extractants is 20-40 DEG C, and a qualified transition section I of ethyl isobutyrate, ethyl isobutyrate and isobutanol and a transition section II of isobutanol, isobutanol and ethylene glycol are sequentially produced from the tower top; and when the components of the extractants at the tower bottom satisfy the requirements, the tower is shut down for cooling, and the extractants are pumped into a higher-position storage tank for use of the next batch of material. The extraction rectification device used by the method comprises an extraction rectification tower, a heating kettle, a condenser, a higher-position storage tank, a receiving tank, a product tank and a vacuum pump.

Description

The separation method that a kind of isopropylcarbinol-ethyl isobutyrate azeotrope is batch extracting rectified
Technical field
The present invention relates to the separation method that a kind of isopropylcarbinol-ethyl isobutyrate azeotrope is batch extracting rectified, belong to the special extract rectification isolation technique of isopropylcarbinol-ethyl isobutyrate azeotrope.
Background technology
Extracting rectifying belongs to the one of special distillation isolation technique, is applicable to the azeotropic system that separation conventional distillation is difficult to be separated.It makes the relative volatility of two or more component in former azeotropic mixture increase by adding extraction agent (solvent), thus reaches the object of separation.Gap extracting rectifying has merged the advantage of batch fractionating and extracting rectifying, and operation of equipment is flexible, and can be realized the separation of multiple component by a tower, facility investment is less, is applicable to the azeotropic system of short run or the separation of system of closely boiling.
Ionic liquid is compared with salt with conventional solvent, there is steam force down, not volatile, larger equilibrium temperature scope and higher chemical stability, have larger adjustability of structure, is suitable as separation solvent, there is medium and catalysis dual-use function, for many inorganic good with organic substance solvability, ionic liquid has larger electrochemical window, electroconductibility, thermostability and oxidation-resistance as ionogen, and ionic liquid has the functional performance of liquid and solid concurrently in a word.[Emim] [OAc] in the present invention is 1-ethyl-3-methylimidazole acetate.Chinese patent CN101028986, the method for extracting rectifying and separating benzene, selected extraction agent is the simple organic solvent such as alcohols, and stability exists certain defect.If add ionic liquid in a solvent, separating effect can be more desirable.
Isopropylcarbinol chemical molecular formula C 4h 10o, is water white liquid under normal temperature, is typically used as the raw material of senior solvent or organic synthesis.Because isopropylcarbinol and ethyl isobutyrate form azeotrope, azeotropic consists of the isopropylcarbinol of massfraction 52% and the ethyl isobutyrate of 48%.Owing to there is azeotropic, common separation method is difficult to reach, and if do not reclaimed, not only pollutes the environment, and causes waste, and the separation method therefore developing isopropylcarbinol-ethyl isobutyrate azeotropic mixture has important meaning.About the article of extracting rectifying aspect and patent a lot, but there is not yet the data of the isopropylcarbinol-ethyl isobutyrate azeotropic system separation of extractive distillation aspect published.
Summary of the invention
The object of the invention is the batch extracting rectified method developing a kind of isopropylcarbinol-ethyl isobutyrate azeotrope, and the product purity of the isopropylcarbinol that the method obtains and ethyl isobutyrate is high, and equipment is simple, and separating energy consumption is lower.
The technical solution used in the present invention is as follows
Employing comprises extractive distillation column, heating kettle, condenser, the batch extraction rectification device that high-level storage groove, receiving tank, products pot and vacuum pump are formed, and batch extracting rectified separation isopropylcarbinol-ethyl isobutyrate azeotropic mixture, its feature is as follows
The present invention adopts ethylene glycol to be extraction agent with the mixed solution of [Emim] [OAc], wherein [Emim] [OAc] massfraction is 10% ~ 15%, extractive distillation column operates under the following conditions, under normal or reduced pressure, the mass ratio of the extraction agent and this column overhead overhead product that enter extractive distillation column is 1.8 ~ 5:1, and the feeding temperature of extraction agent is 20 ~ 40 DEG C.When the temperature of tower top reaches 109 ~ 110 DEG C, with reflux ratio 8 ~ 12:1 by the qualified ethyl isobutyrate of overhead extraction; Reach 107 ~ 109 DEG C when extracting rectifying column overhead temperatures declines, with the transition section I of reflux ratio 8 ~ 12:1 by overhead extraction ethyl isobutyrate and isopropylcarbinol, and stopping adds extraction agent; When extracting rectifying column overhead temperatures drops to 107 DEG C, with reflux ratio 2.2 ~ 7:1 extraction isopropylcarbinol; When extracting rectifying column overhead temperatures is more than 107 DEG C, with the transition section II of reflux ratio 2.5 ~ 4:1 extraction isopropylcarbinol and ethylene glycol; When extracting rectifying column overhead temperatures is higher than 150 DEG C, adopt rectification under vacuum operation, working pressure is 0.01MPa ~ 0.08MPa.; When the component of tower reactor extraction agent reaches requirement, cooling of stopping, pumps into high-order storage tank by extraction agent, uses to get batch materials ready.
Idiographic flow is shown in accompanying drawing: isopropylcarbinol-ethyl isobutyrate mixture adds in heating kettle 3, open the thermal source of heating kettle and the low-temperature receiver of condenser 4, band extractive distillation column trim the top of column and tower top temperature reach stable after, extraction agent is introduced into extractive distillation column 2 top from high-order storage tank 1, total reflux for some time, the discharging when ethyl isobutyrate content reaches requirement, enter receiving tank 4, when in extractive distillation column overhead product, isopropylcarbinol content is lower than product requirement, the material that tower top just goes out enters transition section I receiving tank 6(when the content of isopropylcarbinol in extractive distillation column overhead streams effluent is less than azeotropic composition, stop adding extraction agent), when in extractive distillation column overhead product, ethyl isobutyrate content reaches requirement, the material of extraction enters receiving tank 7, when in extractive distillation column overhead product, ethyl isobutyrate 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 when next batch rectifying.
The invention has the advantages that the extraction agent using separating effect desirable is to destroy the azeotropic system of isopropylcarbinol-ethyl isobutyrate, separation obtains highly purified isopropylcarbinol and ethyl isobutyrate product, and process energy consumption is low, and single tower is flexibly simple to operate, equipment investment is little, and cost is low.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention and schematic flow sheet.
Embodiment
Embodiment 1
Adopt batch extraction rectification device, 500L isopropylcarbinol-ethyl isobutyrate mixture (wherein isopropylcarbinol 52% is dropped at heating kettle, ethyl isobutyrate 48%, be massfraction), extraction agent selected by experiment is 90wt% ethylene glycol and 10wt% [Emim] [OAc], open heating kettle thermal source and condenser low-temperature receiver, after rectifying column top return for some time to be extracted, treat that tower top temperature is stablized, add extraction agent, tower top place is being closed in extractant feed position, control extraction agent and add speed 550L/h, total reflux operation, when extracting rectifying column overhead temperatures is 109 ~ 110 DEG C, in overhead product, ethyl isobutyrate content >=99% starts discharging, reflux ratio is 9:1, discharging speed is 200L/h.When extracting rectifying tower top temperature drops to 107 ~ 109 DEG C, the transition section of extraction isopropylcarbinol-ethyl isobutyrate, and stop adding extraction agent, reflux ratio is 10:1, when extracting rectifying column overhead temperatures temperature drops to 107 DEG C, during content >=99% of overhead product isopropylcarbinol, receive ethyl isobutyrate, reflux ratio is 5:1, when extracting rectifying column overhead temperatures is more than 110 DEG C, reflux ratio 3:1, extraction isopropylcarbinol-ethylene glycol transition section II, when extractive distillation column overhead product ethylene glycol content >=99%, stops, cooling, tower reactor is high-purity extraction agent.
Embodiment 2
Adopt batch fractionating extraction plant, 500L isopropylcarbinol-ethyl isobutyrate mixture (wherein isopropylcarbinol 50% is dropped at heating kettle, ethyl isobutyrate 50%, be massfraction), extraction agent is 85wt% ethylene glycol and 15wt% [Emim] [OAc], open heating kettle thermal source and condenser low-temperature receiver, after rectifying column top return for some time to be extracted, treat that tower top temperature is stablized, add extraction agent, tower top place is being closed in feed solution position, control extraction agent and add speed 800L/h, total reflux operation, when extracting rectifying column overhead temperatures is 109 ~ 110 DEG C, in overhead product, ethyl isobutyrate content >=99% starts discharging, reflux ratio 12:1, discharging speed is 300L/h, when extracting rectifying tower top temperature drops to 107 ~ 109 DEG C, the transition section of extraction isopropylcarbinol-ethyl isobutyrate, and stop adding extraction agent, reflux ratio 10:1, when extracting rectifying column overhead temperatures drops to 107 DEG C, isopropylcarbinol content >=99% in overhead product, receive isopropylcarbinol, reflux ratio 3:1, when extracting rectifying column overhead temperatures is more than 110 DEG C, reflux ratio 3:1, the transition section II of extraction isopropylcarbinol-ethylene glycol, when heating kettle temperature is more than 170 DEG C, stop, naturally cooling, when still temperature to be heated drops to 50 DEG C, open heating kettle, decompression operation, vacuum tightness is 0.07MPa, after trim the top of column, total reflux operation 30 minutes, with reflux ratio 3:1 discharging, when in extractive distillation column overhead product during ethylene glycol content >=99%, stop, heating kettle is the ionic liquid of high-purity ethylene glycol and [Emim] [OAc].

Claims (1)

1. the separation method that isopropylcarbinol-ethyl isobutyrate azeotrope is batch extracting rectified, it is characterized in that with ethylene glycol and massfraction being that the mixed solution of the ionic liquid of 10% ~ 15% is for extraction agent, wherein ionic liquid is [Emim] [OAc], operational condition is normal pressure or decompression, and the mass ratio of the extraction agent and overhead product that enter extractive distillation column is 1.8 ~ 5:1; The feeding temperature of extraction agent controls at 20 ~ 40 DEG C, and the temperature of tower top controls at 107 ~ 150 DEG C, and control of reflux ratio is at 2.2 ~ 12:1, and when extracting rectifying column overhead temperatures is higher than 150 DEG C, adopt rectification under vacuum operation, vacuum tightness is 0.01MPa ~ 0.08MPa.
CN201410619922.0A 2014-11-07 2014-11-07 Separation method of isobutanol-ethyl isobutyrate azeotrope by batch extraction rectification Pending CN104370694A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105061145A (en) * 2015-07-17 2015-11-18 济南大学 Batch distillation process for separating isopropanol-methyl isobutyrate azeotrope through mixed extraction agent
CN105541552A (en) * 2016-01-17 2016-05-04 济南大学 Glycol dimethyl ether-isopropanol azeotropic mixture extracting distillation method
CN105646146A (en) * 2016-01-17 2016-06-08 济南大学 Propyl alcohol-triethylamine azeotropic mixture extraction and rectification method

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CN103274931A (en) * 2013-06-05 2013-09-04 中国石油大学(华东) Solvent for separating carboxylic acid mixtures by extraction and rectification
CN103435445A (en) * 2013-08-20 2013-12-11 天津科林泰克科技有限公司 Method for separating mixture of ethanol alcohol and water
CN103467286A (en) * 2013-08-20 2013-12-25 天津科林泰克科技有限公司 Method for separating ethyl acetate-ethyl alcohol compound
CN103613485A (en) * 2013-12-09 2014-03-05 北京化工大学 Method for extracting, distilling and separating alcohol-water solution through ethylene glycol and ionic liquid

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Publication number Priority date Publication date Assignee Title
CN103274931A (en) * 2013-06-05 2013-09-04 中国石油大学(华东) Solvent for separating carboxylic acid mixtures by extraction and rectification
CN103435445A (en) * 2013-08-20 2013-12-11 天津科林泰克科技有限公司 Method for separating mixture of ethanol alcohol and water
CN103467286A (en) * 2013-08-20 2013-12-25 天津科林泰克科技有限公司 Method for separating ethyl acetate-ethyl alcohol compound
CN103613485A (en) * 2013-12-09 2014-03-05 北京化工大学 Method for extracting, distilling and separating alcohol-water solution through ethylene glycol and ionic liquid

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105061145A (en) * 2015-07-17 2015-11-18 济南大学 Batch distillation process for separating isopropanol-methyl isobutyrate azeotrope through mixed extraction agent
CN105541552A (en) * 2016-01-17 2016-05-04 济南大学 Glycol dimethyl ether-isopropanol azeotropic mixture extracting distillation method
CN105646146A (en) * 2016-01-17 2016-06-08 济南大学 Propyl alcohol-triethylamine azeotropic mixture extraction and rectification method
CN105646146B (en) * 2016-01-17 2017-12-01 济南大学 A kind of propyl alcohol triethylamine azeotropic mixture extraction rectifying method

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