CN103159598A - Batch extractive distillation separation method of isopropyl ether-isopropanol mixture - Google Patents
Batch extractive distillation separation method of isopropyl ether-isopropanol mixture Download PDFInfo
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- CN103159598A CN103159598A CN2013100980486A CN201310098048A CN103159598A CN 103159598 A CN103159598 A CN 103159598A CN 2013100980486 A CN2013100980486 A CN 2013100980486A CN 201310098048 A CN201310098048 A CN 201310098048A CN 103159598 A CN103159598 A CN 103159598A
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Abstract
The invention discloses a batch extractive distillation separation method of isopropyl ether-isopropanol mixture, and relates to a batch extractive distillation method of isopropyl ether. In the method, an extractive distillation tower, a heating kettle at the bottom of the extractive distillation tower, a condensing unit connected to the top of the extractive distillation tower and a distillation device composed of a receiving tank are adopted. The technological process of the method is as follows: adding raw materials at normal pressure in one step; and continuously adding ethylene glycol monomethyl ether serving as an extraction agent, performing batch operation of the extractive distillation tower, controlling the temperature of the top of the tower and a reflux ratio, and sequentially extracting isopropyl ether and isopropanol. The batch extractive distillation separation method has the advantages that by taking ethylene glycol monomethyl ether as an extraction agent, relative volatility of an isopropyl ether-isopropanol is improved, the problem of poor solubility when ethanediol is taken as the extraction agent, the operation is convenient and easy to control, the cyclic utilization of a solvent is realized, the energy consumption is reduced, the cost is reduced and the separation effect is good, so that the method has good economy and is favorable for environmental friendliness.
Description
Technical field
The present invention relates to a kind of method of batch extracting rectified isopropyl ethers, particularly a kind of separation method of isopropyl ether-isopropanol mixture.
Background technology
Isopropyl ether is the good solvent of animal, plant and mineral grease, can be used for extracting Nicotine from tobacco; Be also the good solvent of resin in chemical engineering industry, and often will be applied to dewaxing technique.Diisopropyl ether has higher octane value and frost resistance, can be used as the gasoline dopant.At present, the method for preparing diisopropyl ether has: separating isopropanol by product method, propylene direct hydration method, alfin synthesis method.These methods all contain Virahol, and diisopropyl ether and Virahol can form the polarity azeotrope under normal pressure, can not separate with general rectificating method.Isopropyl ether-Isopropanol Solvent, conventional separation method are to adopt atmospheric distillation, but when the massfraction of isopropyl ether reached 83.7%, relative volatility was near 1, are difficult to obtain purity greater than 90% isopropyl ether with the separation method of routine.
Batch extracting rectified is an emerging research topic, it possesses the practicality of handiness, economy and the extracting rectifying of batch fractionating simultaneously, be applicable to the system that in the industries such as chemical industry, pharmacy, oil deep processing, conventional distillation can't be completed and separate, have academic research and actual application value concurrently.Batch extracting rectified is by the disposable raw material that adds, and then adds continuously the solvent of suitable flow from the tower top somewhere, increases the relative volatility between separated component, thereby reaches the purpose of effectively separating between the weight component.Compare with continuous extraction rectifying, batch extracting rectified have a less investment, flexible operation, it is the plurality of advantages such as a plurality of products that the tower of trying one's best few of available relative continuous rectification separates multicomponent mixture, and, chemical industry begins to transform to production short run high value-added product now, more and more receives researchist's concern.
Summary of the invention
The object of the present invention is to provide a kind of intermittent extraction, distillation and separation method of isopropyl ether-isopropanol mixture, the method adopts ethylene glycol monomethyl ether as extraction agent, improved the relative volatility of isopropyl ether-Isopropanol Solvent, the problem of poor solubility when having avoided traditional ethylene glycol to be extraction agent, the isopropyl ether product purity of separating is high, simple to operate.
The present invention is realized by following technical proposals:
The intermittent extraction, distillation and separation method of isopropyl ether-isopropanol mixture said method comprising the steps of:
With isopropyl ether and the Virahol raw material is disposable add tower at the bottom of, opening power begins heating for the heating jacket of reboiler;
Solvent-free total reflux; Give the plated film heat tracing sleeve pipe heating of rectifying tower, guarantee that material was unlikely to the cold internal reflux that forms in rectifying, open water coolant, prepare the condensation material; When having backflow to occur, keep total reflux, tower top temperature is stabilized in azeotropic temperature;
There is continuous solvent to add total reflux, after solvent-free total reflux, begins to add extraction agent, then total reflux;
The tower top discharging that has continuous solvent to add has continuous solvent to add total reflux, after tower top temperature is stable, open trim the top of column than controller after discharging; Note the size of quantity of reflux in this process, control the flow of extraction agent according to quantity of reflux; And control the tower top reflux ratio, determine the composition of cut according to tower top drop temperature and stratographic analysis result, and change in time receiving bottle to receive the cut of different concns;
Solvent-free adding with the difficult volatiles of reflux ratio extraction; When tower top temperature reaches preset temperature, stop solubilizing agent, change receiving bottle, collect difficult volatiles;
Stop, when the extraction agent of interim fraction in holding tank dense, can stop.Advantage of the present invention is to adopt ethylene glycol monomethyl ether to improve the relative volatility of isopropyl ether-Isopropanol Solvent as extraction agent, the problem of poor solubility when having avoided traditional ethylene glycol to be extraction agent, easy to operate, be easy to control, realized the recycle of solvent, energy expenditure reduces, cost, and also separating effect is better, have good economy, and be conducive to environmental protection.
Description of drawings
Fig. 1 is for realizing extracting rectifying device schematic flow sheet of the present invention.
Embodiment
The inventive method adopts and comprises extractive distillation column, the extractive distillation column overhead condenser, and the device that at the bottom of the extractive distillation column tower, heating kettle and header tank and receiving tank consist of carries out batch extracting rectified operation.Separation method comprises following process: the employing ethylene glycol monomethyl ether is extraction agent, with the disposable tower reactor that joins rectifying tower of raw material, the temperature of controlling tower reactor under normal pressure is 60-85 ℃ and carried out total reflux operation lasting 1-2 hour, then ethylene glycol monomethyl ether is preheating to the top that is incorporated into continuously tower after 40-60 ℃ from header tank as extraction agent, the quality of extraction agent is 2 ~ 4 times of mixture to be separated, and tower top temperature is controlled to be 68.47 ℃ and lasting total reflux 1-2 hour.Then with reflux ratio 1 ~ 4, be 99.5% isopropyl ether product from the overhead extraction massfraction, lower than 98.5%, stop collecting isopropyl ether when the cut content of overhead extraction when namely reaching 70-80 ℃ on tower top temperature, then collect the interim fraction I.When temperature rises to 82.4 ℃, stop adding extraction agent, with reflux ratio 2 ~ 4, reach 99.5% Virahol from the overhead collection massfraction, stop collecting Virahol when the cut content of overhead extraction lower than 98.5% the time, then collect the interim fraction II.When the cut content of overhead extraction reaches 98%, stop collecting stopped heating.At last again reclaim and utilize the ethylene glycol monomethyl ether of tower reactor as the extraction agent of next batch periodical operation.
Adopt device shown in Figure 1 to carry out detailed explanation below in conjunction with the present invention.
In figure: 1-header tank, 2-extractive distillation column, 3-heating kettle, 4-interim fraction II holding tank, 5-Virahol holding tank, 6-interim fraction I holding tank, 7 – isopropyl ether holding tanks, 8-condenser.
In the disposable tower reactor that joins extractive distillation column 2 of the mixture of isopropyl ether-Virahol, opening power is opened electric heating cover 3, pass into water of condensation, after the raw material in tower reactor comes to life, observe the thermometer registration of tower top, slowly improve the voltage of heating jacket, total reflux operation.After full tower is stable (tower top temperature is 66 ℃), the extraction agent ethylene glycol monomethyl ether that preheating temperature is reached 40-60 ℃ adds and is incorporated into the top of extractive distillation column 2 from header tank 1, and extractive distillation column carries out total reflux operation.When the tower top temperature of extractive distillation column is stabilized in 68.47 ℃, continue total reflux operation 1-2 hour, then reach 99.5% isopropyl ether take reflux ratio as 1 ~ 4 tower top from extracting rectifying begins the extraction massfraction, and collect with isopropyl ether holding tank 7.Stop collecting isopropyl ether lower than 98.5% the time when the isopropyl ether massfraction of overhead fraction extraction, the conversion holding tank is collected the excessive cut I of isopropyl ether-Virahol, be tower top temperature when reaching 70-80 ℃, enter into interim fraction I holding tank 6 from the excessive cut I of the overhead extraction isopropyl ether-Virahol of extractive distillation column.When the tower top temperature of extractive distillation column is stabilized in 82.4 ℃, stop collecting the interim fraction I, stop adding extraction agent, with reflux ratio 2 ~ 4 extraction Virahols, enter into Virahol holding tank 5 from the Virahol of the overhead extraction of extractive distillation column.Stop collecting Virahol lower than 98.5% the time when the Virahol massfraction of overhead fraction extraction, then collect the interim fraction II, enter into interim fraction II holding tank 4. when the ethylene glycol monomethyl ether content of overhead extraction reaches 98% from the Virahol-ethylene glycol monomethyl ether of the overhead extraction of extractive distillation column, stop extraction, stopped heating also makes ethylene glycol monomethyl ether cooling, ethylene glycol monomethyl ether is pumped into header tank, the heating kettle new a collection of isopropyl ether-isopropanol mixture of packing into, lower batch of batch extracting rectified separation.
Embodiment one:
Raw material to be separated: isopropyl ether (99.9%), Virahol (99.9%)
Extraction agent: ethylene glycol monomethyl ether (99.8%)
Adopt batch extracting rectified tower (packing tower): the technique of implementing separation is as follows:
Tower internal diameter: in-built θ 4 * 4 net ring fillers of Φ 40mm() solvent ratio: 3:1
Reflux ratio: 1 ~ 4
Tower husband tower reactor temperature: 60 ~ 125 ℃
With flow path device shown in Figure 1, adopt periodical operation to separate isopropyl ether-isopropanol mixture, detailed process is as follows: the diameter of phi 40mm of the extractive distillation column of employing, and in-built Dixon ring filler, packing layer are 2000mm, the extraction agent import is at distance tower top 150mm place,, (wherein isopropyl ether 83.7%, isopropyl ether 16.3% to add 1500ml Virahol-isopropyl ether mixture in the heating tower reactor, be massfraction), join header tank after the preheating of extraction agent ethylene glycol monomethyl ether.Open heating kettle power supply and logical water of condensation.After material in tower reactor comes to life, slowly improve heater voltage.Total reflux operation is until full tower is in steady state, when namely tower top temperature is stabilized in 66 ℃.Then the extraction agent after preheating is incorporated into the top of extractive distillation column from header tank, the quality of extraction agent is 3 times of raw material, total reflux operation.when the tower top temperature of extractive distillation column is stabilized in 68.47 ℃, stop total reflux, take reflux ratio 3:1 as 99.5% isopropyl ether from extractive distillation column overhead collection massfraction, when the isopropyl ether content of extraction lower than 98.5% the time, stop collecting isopropyl ether, with reflux ratio 3:1 from extractive distillation column overhead collection isopropyl ether-Virahol interim fraction I, when the tower top temperature of extractive distillation column is stabilized in 82.4 ℃, stop adding extraction agent, with reflux ratio 2:1 from extractive distillation column overhead collection Virahol, when the isopropanol content of extraction lower than 98.5% the time, stop collecting Virahol, with reflux ratio 2:1 from extractive distillation column overhead collection Virahol-ethylene glycol monomethyl ether interim fraction II, when the content of ethylene glycol monomethyl ether in the interim fraction of extraction higher than 98% the time, stopped heating also makes ethylene glycol monomethyl ether cooling, ethylene glycol monomethyl ether is pumped into header tank, the heating kettle new a collection of isopropyl ether-isopropanol mixture of packing into, lower batch of batch extracting rectified separation.
Embodiment two:
Raw material to be separated: isopropyl ether (99.9%), Virahol (99.9%)
Extraction agent: ethylene glycol monomethyl ether (99.8%)
Adopt batch extracting rectified tower (packing tower): the technique of implementing separation is as follows:
Tower internal diameter: in-built θ 4 * 4 net ring fillers of Φ 40mm()
Solvent ratio: 3:1
Reflux ratio: 1 ~ 4
Tower husband tower reactor temperature: 60 ~ 125 ℃
With flow path device shown in Figure 1, adopt periodical operation to separate isopropyl ether-isopropanol mixture, detailed process is as follows: the diameter of phi 40mm of the extractive distillation column of employing, and in-built Dixon ring filler, packing layer are 2000mm, the extraction agent import is at distance tower top 150mm place,, (wherein isopropyl ether 85.5%, isopropyl ether 14.5% to add 1500ml Virahol-isopropyl ether mixture in the heating tower reactor, be massfraction), join header tank after the preheating of extraction agent ethylene glycol monomethyl ether.Open heating kettle power supply and logical water of condensation.After material in tower reactor comes to life, slowly improve heater voltage.Total reflux operation is until full tower is in steady state, when namely tower top temperature is stabilized in 66 ℃.Then the extraction agent after preheating is incorporated into the top of extractive distillation column from header tank, the quality of extraction agent is 4 times of raw material, total reflux operation.when the tower top temperature of extractive distillation column is stabilized in 68.47 ℃, stop total reflux, take reflux ratio 3:1 as 99.5% isopropyl ether from extractive distillation column overhead collection massfraction, when the isopropyl ether content of extraction lower than 98.5% the time, stop collecting isopropyl ether, with reflux ratio 3:1 from extractive distillation column overhead collection isopropyl ether-Virahol interim fraction I, when the tower top temperature of extractive distillation column is stabilized in 82.4 ℃, stop adding extraction agent, with reflux ratio 2:1 from extractive distillation column overhead collection Virahol, when the isopropanol content of extraction lower than 98.5% the time, stop collecting Virahol, with reflux ratio 2:1 from extractive distillation column overhead collection Virahol-ethylene glycol monomethyl ether interim fraction II, when the content of ethylene glycol monomethyl ether in the interim fraction of extraction higher than 98% the time, stopped heating also makes ethylene glycol monomethyl ether cooling, ethylene glycol monomethyl ether is pumped into header tank, the heating kettle new a collection of isopropyl ether-isopropanol mixture of packing into, lower batch of batch extracting rectified separation.
Claims (1)
1. the intermittent extraction, distillation and separation method of isopropyl ether-isopropanol mixture, is characterized in that, said method comprising the steps of:
1) with isopropyl ether and the Virahol raw material is disposable add tower at the bottom of, opening power begins heating for the heating jacket of reboiler;
2) solvent-free total reflux; Give the plated film heat tracing sleeve pipe heating of rectifying tower, guarantee that material was unlikely to the cold internal reflux that forms in rectifying, open water coolant, prepare the condensation material; When having backflow to occur, keep total reflux, tower top temperature is stabilized in azeotropic temperature;
3) there is continuous solvent to add total reflux, after solvent-free total reflux, begins to add extraction agent, then total reflux;
4) the tower top discharging that has continuous solvent to add has continuous solvent to add total reflux, after tower top temperature is stable, open trim the top of column than controller after discharging; Note the size of quantity of reflux in this process, control the flow of extraction agent according to quantity of reflux; And control the tower top reflux ratio, determine the composition of cut according to tower top drop temperature and stratographic analysis result, and change in time receiving bottle to receive the cut of different concns;
5) solvent-free adding with the difficult volatiles of reflux ratio extraction; When tower top temperature reaches preset temperature, stop solubilizing agent, change receiving bottle, collect difficult volatiles;
6) stop, when the extraction agent of interim fraction in holding tank dense, can stop.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044215A (en) * | 2012-12-18 | 2013-04-17 | 沈阳化工大学 | Intermittent extractive distillation and separation method for isopropyl ether-isopropanol mixture |
| 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 |
| CN104860797A (en) * | 2015-05-21 | 2015-08-26 | 济南大学 | Isopropyl ether-isopropyl alcohol azeotrope distillation separation method based on choline chloride deep eutectic solvent |
| CN105037112A (en) * | 2015-05-21 | 2015-11-11 | 济南大学 | Batch extractive distillation separation method of ethyl tert-butyl ether/tert-butyl alcohol azeotropic mixture |
| CN105348098A (en) * | 2015-08-06 | 2016-02-24 | 青岛科技大学 | Method for rectifying and separating methyl formate, methanol and water by intermittent reaction |
| CN106518618A (en) * | 2016-10-08 | 2017-03-22 | 济南大学 | Method for continuously extracting, rectificating and separating isopropanol-isopropyl ether azeotrope by mixed solvent |
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| CN101792367A (en) * | 2010-03-12 | 2010-08-04 | 江苏工业学院 | Intermittent extraction, distillation and separation method of isopropanol-diisopropyl ether-water mixture |
| CN103044215A (en) * | 2012-12-18 | 2013-04-17 | 沈阳化工大学 | Intermittent extractive distillation and separation method for isopropyl ether-isopropanol mixture |
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2013
- 2013-03-26 CN CN2013100980486A patent/CN103159598A/en active Pending
Patent Citations (2)
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| CN101792367A (en) * | 2010-03-12 | 2010-08-04 | 江苏工业学院 | Intermittent extraction, distillation and separation method of isopropanol-diisopropyl ether-water mixture |
| CN103044215A (en) * | 2012-12-18 | 2013-04-17 | 沈阳化工大学 | Intermittent extractive distillation and separation method for isopropyl ether-isopropanol mixture |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044215A (en) * | 2012-12-18 | 2013-04-17 | 沈阳化工大学 | Intermittent extractive distillation and separation method for isopropyl ether-isopropanol mixture |
| CN104860797A (en) * | 2015-05-21 | 2015-08-26 | 济南大学 | Isopropyl ether-isopropyl alcohol azeotrope distillation separation method based on choline chloride deep eutectic solvent |
| CN105037112A (en) * | 2015-05-21 | 2015-11-11 | 济南大学 | Batch extractive distillation separation method of ethyl tert-butyl ether/tert-butyl alcohol azeotropic mixture |
| 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 |
| CN105348098A (en) * | 2015-08-06 | 2016-02-24 | 青岛科技大学 | Method for rectifying and separating methyl formate, methanol and water by intermittent reaction |
| CN105348098B (en) * | 2015-08-06 | 2017-03-22 | 青岛科技大学 | Method for rectifying and separating methyl formate, methanol and water by intermittent reaction |
| CN106518618A (en) * | 2016-10-08 | 2017-03-22 | 济南大学 | Method for continuously extracting, rectificating and separating isopropanol-isopropyl ether azeotrope by mixed solvent |
| CN106518618B (en) * | 2016-10-08 | 2019-03-29 | 济南大学 | A kind of method of mixed solvent continuous extraction rectifying separating isopropanol-isopropyl ether azeotropic mixture |
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Application publication date: 20130619 |