CN104829437A - Intermittent extractive distillation and separation method of acetonitrile-methyl tertiary-butyl ether azeotropic mixture - Google Patents
Intermittent extractive distillation and separation method of acetonitrile-methyl tertiary-butyl ether azeotropic mixture Download PDFInfo
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- CN104829437A CN104829437A CN201510273140.0A CN201510273140A CN104829437A CN 104829437 A CN104829437 A CN 104829437A CN 201510273140 A CN201510273140 A CN 201510273140A CN 104829437 A CN104829437 A CN 104829437A
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- acetonitrile
- butyl ether
- methyl tertiary
- extraction
- extractive distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
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- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an intermittent extractive distillation and separation method of an acetonitrile-methyl tertiary-butyl ether azeotropic mixture, and belongs to a separation technology of the acetonitrile-methyl tertiary-butyl ether azeotropic mixture. The intermittent extractive distillation and separation method of the acetonitrile-methyl tertiary-butyl ether azeotropic mixture comprises the following steps of using dimethyl sulfoxide (DMSO), N, N-dimethylformamide or a mixture of the dimethyl sulfoxide and the N, N-dimethylformamide at an optional proportion as an extraction agent under the condition that the operation pressure of an extractive distillation tower is constant pressure or reduced pressure; controlling different temperatures and different reflux ratios of the extractive distillation tower and respectively extracting methyl tertiary-butyl ethers, methyl tertiary-butyl ether-acetonitrile transition section 1, acetonitrile and acetonitrile-extracting agent transition section 2 under the condition that the mass ratio of the extracting agent to distillation of a tower roof is 0.5:1-10:1; and pumping the extracting agent into a high-position storing tank to be used circularly when composition of the extracting agent of a tower reactor meets requirements. The intermittent extractive distillation and separation method of the acetonitrile-methyl tertiary-butyl ether azeotropic mixture has the advantages that the acetonitrile-methyl tertiary-butyl ether azeotropic system is damaged by the extracting agent so as to extract high-purity methyl tertiary-butyl ether products and acetonitrile products. The single tower is operated flexibly, and the cost of equipment is low.
Description
Technical field
The present invention relates to a kind of acetonitrile-methyl tertiary butyl ether azeotropic mixture intermittent extraction, distillation and separation method, belong to the isolation technique of acetonitrile-methyl tertiary butyl ether azeotropic mixture.
Background technology
Extracting rectifying is a kind of special extract rectification isolation technique, is applicable to the separation of azeotropic system.To reach the object of separation with the relative volatility changed between stock blend by adding extraction agent continuously toward rectifying tower top.Batch extracting rectifiedly merged the advantage of batch fractionating and extracting rectifying, flexible operation, can be separated multiple component by a tower, facility investment is little, is applicable to being separated of short run azeotropic system and system of closely boiling.The chemical structural formula of methyl tertiary butyl ether is: CH
3oC (CH3)
3.Be a kind of high-octane rating (research octane number (RON) 115) gasoline dope, chemical oxygen content is much lower compared with methyl alcohol, and be beneficial to warming up and fuel economy, vaporization heat is low, favourable to cold start-up, is usually used in the blending of white gasoline and low lead oil.Also again iso-butylene can be cracked into, as the raw material of rubber and other Chemicals.And in the industry, because acetonitrile is as the extraction agent in C4 separation, be difficult to be separated, if do not reclaimed so easily form azeotrope (molar fraction of acetonitrile is 0.12) with methyl tertiary butyl ether in process of production, not only pollute the environment, and can production cost be increased.Therefore develop a kind of separation method being separated this azeotrope to have great importance.About the article of extracting rectifying aspect and patent a lot, the data of the acetonitrile not yet published-methyl tertiary butyl ether 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 acetonitrile-methyl tertiary butyl ether azeotropic mixture, the product purity of the isolated acetonitrile of the method, methyl tertiary butyl ether is high.
Of the present inventionly to be achieved through the following technical solutions.Adopt the extracting rectifying device comprising extractive distillation column, heating kettle, condenser, high-order storage tank, receiving tank and products pot and form, batch extracting rectified separating acetonitrile-methyl tertiary butyl ether azeotropic mixture, its feature comprises following process:
With dimethyl sulfoxide (DMSO) (DMSO), N, N-dimethylformamide (DMF) or the two with arbitrary proportion mixing composition mixture for extraction agent, the concrete operations condition of extractive distillation column is as follows: under normal or reduced pressure, the mass ratio of the extraction agent and this overhead product that enter extraction tower is 0.5:1-10:1, and the feeding temperature of extraction agent is 30---65 DEG C.When the tower top temperature of extractive distillation column is 50-55 DEG C, with reflux ratio 1:1-6:1 extraction acetonitrile-methyl tertiary butyl ether transition section 1; When the temperature of extracting rectifying tower top is 55-60 DEG C, take reflux ratio as 1:1-5:1 extraction methyl tertiary butyl ether, and stop adding extraction agent; When the temperature of extracting rectifying tower top is 75-80 DEG C, with reflux ratio 2:1-7:1 extraction acetonitrile; When extracting rectifying tower top temperature >=82 DEG C, with reflux ratio 1:1-10:1 by overhead extraction acetonitrile-extraction agent transition section 2.When tower top extraction agent composition reaches requirement, stop and cooling, extraction agent infusion is entered high-order storage tank.Load new a collection of acetonitrile-MTBE mixtures and transition section 1 and transition section 2 in heating kettle at the bottom of tower, carry out lower batch of batch extracting rectified separation.
Idiographic flow (see photo): the azeotropic mixture of acetonitrile-methyl tertiary butyl ether is loaded in tower top heating kettle 3, open the thermal source of overhead condenser 4 and heating kettle, rectifying tower top to be extracted have backflow and temperature keep stable after, extraction agent is introduced in the top of extractive distillation column 2 from high-order storage tank 1, after during total reflux one section, the receiving tank 5 when extracting rectifying tower top overhead product is less than the purity of methyl tertiary butyl ether, extraction material being entered transition section 1 when tower top temperature be 55-60 DEG C, the purity of methyl tertiary butyl ether reaches requirement, be introduced into receiving tank 6(when the content of extracting rectifying tower top methyl tertiary butyl ether is less than azeotropic composition, stop adding extraction agent), when in overhead product, the content of acetonitrile reaches requirement, material will be distillated and enter receiving tank 7, when the requirement lower than product of the content of acetonitrile in extracting rectifying tower top overhead product, the material of extraction enters transition section 2 receiving tank 8, when the composition of heating kettle extraction agent reaches requirement, stop.It is high purity extraction agent in heating kettle at the bottom of tower.Squeezed into high-order storage tank 1 with pump to recycle.The material of transition section 1 and transition section 2 again next batch rectifying time put in heating kettle.
The invention has the advantages that and use rational extraction agent to break the azeotropic system of acetonitrile-methyl tertiary butyl ether, isolate highly purified acetonitrile, methyl tert-butyl ether product.Single tower flexible operation, cost of equipment is low, efficiency high.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention and schematic flow sheet, in figure: Fig. 1 is apparatus of the present invention and schematic flow sheet.In figure: 1-high-order storage tank, 2-extractive distillation column, 3-heating kettle, 4-condenser, 5-transition section 1 receiving tank, 6-methyl tertiary butyl ether receiving tank, 7-acetonitrile receiving tank, 8-transition section 2 receiving tank.
Embodiment
Embodiment 1: adopt batch extraction rectification device, azeotropic mixture (the wherein methyl tertiary butyl ether 12% of 500L acetonitrile-methyl tertiary butyl ether is dropped in heating kettle, acetonitrile 88%, being molecular fraction) the selected extraction agent of experiment is N, N-dimethylformamide, open overhead condensation water and heating kettle thermal source, after rectifying tower top to be extracted has the also tower top temperature maintenance that refluxes stable, add extraction agent, tower top place is being closed in extractant feed position, the input speed controlling extraction agent is 500L/h, total reflux operation, when the tower top temperature of extractive distillation column is 50-55 DEG C, with reflux ratio 4:1 extraction acetonitrile-methyl tertiary butyl ether transition section 1, and be incorporated into receiving tank 5, when extracting rectifying tower top temperature is 55-60 DEG C, in overhead product, the content of methyl tertiary butyl ether is greater than 99% beginning discharging, and reflux ratio is 2:1, and discharging speed is 200L/h, overhead product is incorporated into products pot 6, and stops adding extraction agent, when the temperature of extractive distillation column is 75-82 DEG C, when the content of the acetonitrile in overhead product is greater than 99%, receive acetonitrile, reflux ratio is 5:1, when extracting rectifying tower top temperature is more than 82 DEG C, reflux ratio is 4:1, extraction acetonitrile-transition section 2, when the extraction agent in overhead product reaches requirement, obtain high-purity extraction agent in heating kettle at the bottom of tower, after cooling of stopping, be driven into high-order storage tank with pump, add fresh material Posterior circle and use.
Embodiment 2: experimental installation and working method are with embodiment one, and extraction agent adopts dimethyl sulfoxide (DMSO).
Embodiment 3: experimental installation and working method with embodiment one, extraction agent adopt dimethyl sulfoxide (DMSO) and N, N-dimethylformamide etc. the mixture of quality.
Claims (3)
1. the intermittent extraction, distillation and separation method of acetonitrile-methyl tertiary butyl ether azeotropic mixture thing, the method adopts the extracting rectifying device comprising extractive distillation column, heating kettle, condenser, high-order storage tank, receiving tank and products pot and form, batch extracting rectified separating acetonitrile-methyl tertiary butyl ether azeotropic mixture.
2. the intermittent extraction, distillation and separation method of the azeotropic mixture of a kind of acetonitrile-methyl tertiary butyl ether according to claim 1, it is characterized in that with dimethyl sulfoxide (DMSO) (DMSO), N, N-dimethylformamide or the two with arbitrary proportion composition mixture for extraction agent.
3. its feature of intermittent extraction, distillation and separation method of the azeotropic mixture of a kind of acetonitrile-methyl tertiary butyl ether according to claim 2 comprises following process: with dimethyl sulfoxide (DMSO) (DMSO), N, N-dimethylformamide (DMF) or the two with arbitrary proportion mixing composition mixture for extraction agent, the concrete operations condition of extractive distillation column is as follows: under normal or reduced pressure, the mass ratio of the extraction agent and this overhead product that enter extraction tower is 0.5:1-10:1, and the feeding temperature of extraction agent is 30---65 DEG C; When the tower top temperature of extractive distillation column is 50-55 DEG C, with reflux ratio 1:1-6:1 extraction acetonitrile-methyl tertiary butyl ether transition section 1; When the temperature of extracting rectifying tower top is 55-60 DEG C, take reflux ratio as 1:1-5:1 extraction methyl tertiary butyl ether, and stop adding extraction agent; When the temperature of extracting rectifying tower top is 75-80 DEG C, with reflux ratio 2:1-7:1 extraction acetonitrile; When extracting rectifying tower top temperature >=82 DEG C, with reflux ratio 1:1-10:1 by overhead extraction acetonitrile-extraction agent transition section 2; When tower top extraction agent composition reaches requirement, stop and cooling, extraction agent infusion is entered high-order storage tank; Load new a collection of acetonitrile-MTBE mixtures and transition section 1 and transition section 2 in heating kettle at the bottom of tower, carry out lower batch of batch extracting rectified separation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106220532A (en) * | 2016-07-21 | 2016-12-14 | 青岛科技大学 | A kind of separation of extractive distillation acetonitrile and the method for triethylamine |
| CN108273280A (en) * | 2018-02-08 | 2018-07-13 | 凯莱英医药集团（天津）股份有限公司 | The separator and method of acetonitrile-methyl tertiary butyl ether(MTBE)-aqueous systems |
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| CN1736529A (en) * | 2005-07-26 | 2006-02-22 | 天津大学 | Batch extractive distillation separating method of acetonitrile-methylbenzene azeotropic mixtrue |
| CN103159598A (en) * | 2013-03-26 | 2013-06-19 | 沈阳化工大学 | Batch extractive distillation separation method of isopropyl ether-isopropanol mixture |
| CN103304373A (en) * | 2013-06-27 | 2013-09-18 | 济南大学 | Batch extraction-rectification-separation method of dichloromethane-methanol azeotropic mixture |
| CN103601653A (en) * | 2013-11-22 | 2014-02-26 | 天津大学 | Method for extracting, rectifying and separating acetonitrile-water azeotropic mixture |
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- 2015-05-26 CN CN201510273140.0A patent/CN104829437A/en active Pending
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| CN1736529A (en) * | 2005-07-26 | 2006-02-22 | 天津大学 | Batch extractive distillation separating method of acetonitrile-methylbenzene azeotropic mixtrue |
| CN103159598A (en) * | 2013-03-26 | 2013-06-19 | 沈阳化工大学 | Batch extractive distillation separation method of isopropyl ether-isopropanol mixture |
| CN103304373A (en) * | 2013-06-27 | 2013-09-18 | 济南大学 | Batch extraction-rectification-separation method of dichloromethane-methanol azeotropic mixture |
| CN103601653A (en) * | 2013-11-22 | 2014-02-26 | 天津大学 | Method for extracting, rectifying and separating acetonitrile-water azeotropic mixture |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220532A (en) * | 2016-07-21 | 2016-12-14 | 青岛科技大学 | A kind of separation of extractive distillation acetonitrile and the method for triethylamine |
| CN106220532B (en) * | 2016-07-21 | 2018-06-22 | 青岛科技大学 | A kind of method of separation of extractive distillation acetonitrile and triethylamine |
| CN108273280A (en) * | 2018-02-08 | 2018-07-13 | 凯莱英医药集团（天津）股份有限公司 | The separator and method of acetonitrile-methyl tertiary butyl ether(MTBE)-aqueous systems |
| CN108273280B (en) * | 2018-02-08 | 2023-10-27 | 凯莱英医药集团（天津）股份有限公司 | Separation device and method for acetonitrile-methyl tertiary butyl ether-water system |
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