CN1317049C - Batch extractive distillation separating method of acetonitrile-methylbenzene azeotropic mixtrue - Google Patents
Batch extractive distillation separating method of acetonitrile-methylbenzene azeotropic mixtrue Download PDFInfo
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- CN1317049C CN1317049C CNB2005100146358A CN200510014635A CN1317049C CN 1317049 C CN1317049 C CN 1317049C CN B2005100146358 A CNB2005100146358 A CN B2005100146358A CN 200510014635 A CN200510014635 A CN 200510014635A CN 1317049 C CN1317049 C CN 1317049C
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- toluene
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Abstract
The present invention discloses a method for the batch extractive distillation and separation of acetonitrile-toluene azeotrope, which belongs to the separation technique of acetonitrile-toluene azeotrope. In the method, propyl benzene, butylbenzene, isobutylbenzene, sec-butylbenzene, tert-butylbenzene, p-diethyl benzene or p-tert-butyl toluene is used as anextraction agent, the mass ratio of the extraction agent to distillate at the tower top is from 2: 1 to 10: 1 under the operating conditions of normal pressure and pressure reduction of an extractive rectifying tower, the feeding temperature of the extraction agent is from 25 DEG C to 80 DEG C, the different temperature and the different reflux ratios of the top of the extractive rectifying tower are controlled, and then an acetonitrile products, a transition section I with low acetonitrile content, a toluene product and a toluene-extraction agent transition section II are respectively produced at the top of the extractive rectifying tower; when the constitutes of the extraction agent in a heating kettle reach the requirements, the extraction agent is pumped into a high-position storage tank, materials are fed, and then the next batch extractive distillation and separation is carried out. The present invention has the advantages of separation of high-purity acetonitrile and toluene products, flexible single-tower operation and low equipment cost due to the adoption of the extraction agent to destroy an acetonitrile-toluene azeotropic system.
Description
Technical field
The present invention relates to the intermittent extraction, distillation and separation method of a kind of acetonitrile-methylbenzene azeotropic mixture, belong to the isolation technics of acetonitrile-methylbenzene azeotropic mixture.
Background technology
Extracting rectifying is a kind of extraordinary rectifying isolation technics, is fit to the separation of azeotropic system.Add extractant continuously by top and reach the separation purpose with the relative volatility that changes between stock blend toward rectifying column.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 equipment investment is little, is suitable for separating of the small lot azeotropic system and the system of closely boiling.Acetonitrile and toluene are solvents commonly used in the pharmaceuticals industry, acetonitrile-the toluene mixture of Chan Shenging in process of production, owing to forming azeotropic mixture, acetonitrile-toluene is difficult to separate, as not reclaiming, not only pollute the environment, and the increase production cost, the separation method of therefore developing acetonitrile-methylbenzene azeotropic mixing has important meaning.About the article and the patent of extracting rectifying aspect a lot, the data of the acetonitrile that Shang Weijian publishes-methylbenzene azeotropic system extracting rectifying separation 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-methylbenzene azeotropic mixture.With the isolated acetonitrile of this method, toluene product purity height.
The present invention is realized by following technical proposals.Employing comprises extractive distillation column, heating kettle, and condenser, high-order storage tank, the extracting rectifying device that receiving tank and product jar constitute, batch extracting rectified separating acetonitrile-methylbenzene azeotropic mixture is characterized in that comprising following process:
With propyl benzene, n-butyl benzene, isobutylbenzene, sec-butylbenzene, tert-butyl benzene, p-diethylbenzene or p-tert-butyltoluene is extractant, extractive distillation column is operated with following condition, under normal pressure and decompression, entering the extractant of extractive distillation column and the mass ratio of this overhead is 2: 1-10: 1, and the feeding temperature of extractant is 25-80 ℃.When extracting rectifying cat head temperature is 81-83 ℃, with reflux ratio 1: 1-5: 1 by the qualified acetonitrile product of cat head extraction ethane nitrile content; When extracting rectifying cat head temperature is 83-110 ℃, with reflux ratio 8: 1-10: 1 by the low changeover portion I of cat head extraction ethane nitrile content, and stops to add extractant; When extracting rectifying cat head temperature is 110-112 ℃, with reflux ratio 3: 1-8: 1 by cat head extraction toluene; When extracting rectifying cat head temperature surpasses 112 ℃,,, select decompression operation for use if the boiling point of extractant equals and is higher than 160 ℃ by cat head extraction toluene-extractant changeover portion II; Form when reaching requirement when the extractant of heating kettle, the cooling of stopping pumps into high-order storage tank with extractant, heating kettle pack into new a collection of acetonitrile-toluene mixture and changeover portion I and changeover portion II, following batch of batch extracting rectified separation.
Idiographic flow (seeing accompanying drawing): acetonitrile-toluene mixture adds in the heating kettle 3, open the thermal source of heating kettle and the low-temperature receiver of condenser 4, after treating that the extracting rectifying cat head refluxes, extractant is introduced into extractive distillation column 2 tops from high-order storage tank 1, infinite reflux a period of time, discharging when ethane nitrile content reaches requirement, enter acetonitrile product jar 5, when ethane nitrile content is lower than product requirement in the extracting rectifying cat head distillate, the material of cat head extraction enters changeover portion I receiving tank 6 (when ethane nitrile content is formed less than azeotropic in the extracting rectifying cat head distillate, stop to add extractant), when toluene level reaches the finished product requirement in the extracting rectifying cat head distillate, the material of extraction enters toluene jar 7, when toluene level is lower than the finished product requirement in the extracting rectifying cat head distillate, the material of extraction enters changeover portion II receiving tank 8, when the composition of heating kettle extractant reaches requirement, stops.Heating kettle is high-purity extractant, squeezes into high-order storage tank and recycles.The material of two changeover portions is put in the heating kettle when next group distills.
The invention has the advantages that and adopt extractant to destroy acetonitrile-methylbenzene azeotropic system, isolate high-purity acetonitrile, toluene 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: the high-order storage tank of 1-, 2-extractive distillation column, 3-heating kettle, 4-condenser, 5-acetonitrile product jar, 6-changeover portion I receiving tank, 7-toluene product jar, 8-changeover portion II receiving tank.
The specific embodiment
Embodiment one
Adopt batch extraction rectification device, acetonitrile-(wherein acetonitrile 73% for the methylbenzene azeotropic mixture to drop into 500ml at heating kettle, toluene 27%, be mass percent), testing selected extractant is propyl benzene, open heating kettle thermal source and condenser low-temperature receiver, then extractive distillation column brings into operation, and treats that the extracting rectifying cat head has backflow, add extractant, the cat head place is being closed in the extractant feed position, and the control extractant adds speed 800ml/h, total reflux operation, when extracting rectifying cat head temperature is 81.5-82 ℃, ethane nitrile content in the distillate 〉=99% beginning discharging, reflux ratio is 3: 1, discharging speed is 200ml/h.When extracting rectifying cat head temperature is 83-110 ℃ of extraction acetonitrile-toluene changeover portion, and stop to add extractant, reflux ratio is 10: 1, when extracting rectifying cat head temperature is 110-112 ℃, toluene level in the overhead 〉=99% o'clock receives toluene, and reflux ratio is 5: 1, when extracting rectifying cat head temperature is higher than 112 ℃, reflux ratio is 8: 1, and extraction toluene-propyl benzene changeover portion is when propyl benzene content in the extracting rectifying cat head distillate 〉=99.5%, stop, heating kettle is high-purity propyl benzene.
Embodiment two
Adopt batch extraction rectification device, acetonitrile-(wherein acetonitrile 73% for the methylbenzene azeotropic mixture to drop into 500ml at heating kettle, toluene 27%, be mass percent), testing selected extractant is p-tert-butyltoluene, unlatching heating kettle thermal source and condenser low-temperature receiver then rectifying column bring into operation, treat that the extracting rectifying cat head has backflow, add extractant, the cat head place is being closed in the extractant feed position, the control extractant adds speed 1200ml/h, total reflux operation, when extracting rectifying cat head temperature is 81.5-82 ℃, ethane nitrile content in the overhead 〉=99% beginning discharging, reflux ratio is 2: 1, and discharging speed is at 150ml/h.When extracting rectifying cat head temperature is 83-110 ℃ of extraction acetonitrile-toluene changeover portion, and stop to add extractant, reflux ratio is 10: 1, when extracting rectifying cat head temperature is 110-112 ℃, and toluene level in the overhead 〉=99% o'clock, receive toluene, reflux ratio is 5: 1, and when extracting rectifying cat head temperature was higher than 112 ℃, reflux ratio was 10: 1, extraction toluene-p-tert-butyltoluene changeover portion, when the heating kettle temperature surpasses 160 ℃, stop, naturally cooling, when still temperature to be heated drops to 140 ℃, open heating kettle, decompression operation, vacuum degree control is at 0.079MPa, behind the overhead reflux, total reflux operation ten minutes is with reflux ratio discharging in 15: 1, when p-tert-butyltoluene content in the extracting rectifying cat head distillate 〉=99.5%, stop, heating kettle is high-purity p-tert-butyltoluene.
Embodiment three
Experimental provision and method of operating are with embodiment one, and extractant adopts mesitylene
Embodiment four
Experimental provision and method of operating are with embodiment two, and extractant adopts n-butyl benzene.
Embodiment five
Experimental provision and method of operating are with embodiment two, and extractant adopts isobutylbenzene.
Embodiment six
Experimental provision and method of operating are with embodiment two, and extractant adopts sec-butylbenzene.
Embodiment seven
Experimental provision and method of operating are with embodiment two, and extractant adopts tert-butyl benzene.
Embodiment eight
Experimental provision and method of operating are with embodiment two, and extractant adopts p-diethylbenzene.
Claims (1)
1. the intermittent extraction, distillation and separation method of an acetonitrile-methylbenzene azeotropic mixture, this method adopts and comprises extractive distillation column, heating kettle, condenser, high-order storage tank, the extracting rectifying device that receiving tank and product jar constitute, batch extracting rectified separating acetonitrile-methylbenzene azeotropic mixture, it is characterized in that comprising following process: with propyl benzene, n-butyl benzene, isobutylbenzene, sec-butylbenzene, tert-butyl benzene, p-diethylbenzene or p-tert-butyltoluene are extractant, extractive distillation column is operated with following condition, under normal pressure or decompression, entering the extractant of extractive distillation column and the mass ratio of this overhead is 2: 1-10: 1, the feeding temperature of extractant is 25-80 ℃, and when extracting rectifying cat head temperature is 81-83 ℃, with reflux ratio 1: 1-5: 1 by the qualified acetonitrile product of cat head extraction ethane nitrile content; When extracting rectifying cat head temperature is 83-110 ℃, with reflux ratio 8: 1-10: 1 by the low changeover portion I of cat head extraction ethane nitrile content, and stops to add extractant; When extracting rectifying cat head temperature is 110-112 ℃, with reflux ratio 3: 1-8: 1 by cat head extraction toluene; When extracting rectifying cat head temperature surpasses 112 ℃,,, select decompression operation for use if the boiling point of extractant equals and is higher than 160 ℃ by cat head extraction toluene-extractant changeover portion II; Form when reaching requirement when the extractant of heating kettle, the cooling of stopping pumps into high-order storage tank with extractant, heating kettle pack into new a collection of acetonitrile-methylbenzene mixture and changeover portion I and changeover portion II, following batch of batch extracting rectified separation.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100146358A CN1317049C (en) | 2005-07-26 | 2005-07-26 | Batch extractive distillation separating method of acetonitrile-methylbenzene azeotropic mixtrue |
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| CNB2005100146358A CN1317049C (en) | 2005-07-26 | 2005-07-26 | Batch extractive distillation separating method of acetonitrile-methylbenzene azeotropic mixtrue |
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| CN1317049C true CN1317049C (en) | 2007-05-23 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100427468C (en) * | 2006-05-29 | 2008-10-22 | 天津大学 | Apparatus and method for separating 5-bromo-2-methyl pyridine isomer by intermittent rectification under vacuum |
| CN101830830B (en) * | 2009-03-13 | 2013-04-24 | 中国石油天然气股份有限公司 | Method for separating acetonitrile-toluene by extractive distillation through dividing wall rectifying tower |
| CN104829437A (en) * | 2015-05-26 | 2015-08-12 | 济南大学 | Intermittent extractive distillation and separation method of acetonitrile-methyl tertiary-butyl ether azeotropic mixture |
| CN105175280B (en) * | 2015-06-17 | 2017-06-23 | 济南大学 | Acetonitrile-tert-butyl alcohol azeotropic mixture continuous extraction distillation and separation method |
| CN108373426A (en) * | 2018-03-13 | 2018-08-07 | 索闻特环保科技(上海)有限公司 | The separation method of acetonitrile and toluene mixture liquid |
| CN111362831B (en) * | 2020-04-25 | 2022-06-28 | 青岛科技大学 | Heterogeneous batch rectification separation process of cyclohexane-acetonitrile-toluene azeotrope |
| CN113461477A (en) * | 2021-06-24 | 2021-10-01 | 索闻特环保科技(上海)有限公司 | Method for treating mixed liquid containing acetonitrile and n-heptane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106710A (en) * | 1994-11-18 | 1995-08-16 | 天津大学 | Single-tower atmospheric intermittent extractive rectification method |
| JP2001004030A (en) * | 1999-04-19 | 2001-01-09 | Nok Corp | Separate plate and manufacture thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106710A (en) * | 1994-11-18 | 1995-08-16 | 天津大学 | Single-tower atmospheric intermittent extractive rectification method |
| JP2001004030A (en) * | 1999-04-19 | 2001-01-09 | Nok Corp | Separate plate and manufacture thereof |
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Assignee: RIONLON TIANJIN CHEMICAL Co.,Ltd. Assignor: Tianjin University Contract fulfillment period: 2009.3.2 to 2015.3.1 Contract record no.: 2009120000246 Denomination of invention: Batch extractive distillation separating method of acetonitrile-methylbenzene azeotropic mixtrue Granted publication date: 20070523 License type: Exclusive license Record date: 20091022 |
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Assignee: RIONLON TIANJIN CHEMICAL Co.,Ltd. Assignor: Tianjin University Contract record no.: 2009120000246 Date of cancellation: 20130828 |
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