CN103044215A - Intermittent extractive distillation and separation method for isopropyl ether-isopropanol mixture - Google Patents
Intermittent extractive distillation and separation method for isopropyl ether-isopropanol mixture Download PDFInfo
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- CN103044215A CN103044215A CN2012105497859A CN201210549785A CN103044215A CN 103044215 A CN103044215 A CN 103044215A CN 2012105497859 A CN2012105497859 A CN 2012105497859A CN 201210549785 A CN201210549785 A CN 201210549785A CN 103044215 A CN103044215 A CN 103044215A
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Abstract
The invention provides an intermittent extractive distillation and separation method for an isopropyl ether-isopropanol mixture and relates to a distillation and separation method. A device used by the method comprises an extractive distillation tower, a heating kettle and a distillation device, wherein the heating kettle is arranged at the bottom of the extractive distillation tower; and the distillation device is connected to the top of the extractive distillation tower and comprises a condensing device and a receiving tank. The technical process comprises the following steps: adding raw materials at a normal pressure at one time, continuously adding ethylene glycol monomethyl ether to the raw materials as an extracting agent, carrying out intermittent operation on the raw materials by using the extractive distillation tower, controlling a temperature and a reflux ratio at the top of the tower, and extracting isopropyl ether and isopropanol in sequence. The intermittent extractive distillation and separation method for the isopropyl ether-isopropanol mixture, provided by the invention, has the advantages as follows: through using the ethylene glycol monomethyl ether as the extracting agent, the relative volatility of an isopropyl ether-isopropanol system is enhanced, the problem that the solubility is poor when the traditional ethylene glycol is used as the extracting agent is avoided, convenient operation and easy control are achieved, solvents are recycled, energy consumption is reduced, the cost is reduced, a better separating effect and very good economic efficiency are obtained, and the intermittent extractive distillation and separation method is beneficial for environmental protection.
Description
Technical field
The present invention relates to a kind of distillation and separation method, particularly relate to a kind of intermittent extraction, distillation and 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; Also be 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 conventional distillation can't be finished in the industries such as chemical industry, pharmacy, oil deep processing and separate, have academic research and actual application value concurrently.Batch extracting rectified is by disposable adding raw material, then adds continuously the solvent of suitable flow from the cat head somewhere, increases the relative volatility between separated component, thereby reaches the purpose of effective separation 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 present invention adopts ethylene glycol monomethyl ether to improve the relative volatility of isopropyl ether-Isopropanol Solvent, the problem of poor solubility when having avoided traditional ethylene glycol to be extraction agent as extraction agent.
The objective of the invention is to be achieved through the following technical solutions:
A kind of intermittent extraction, distillation and separation method of isopropyl ether-isopropanol mixture, described method comprises following process:
1) with at the bottom of isopropyl ether and the disposable adding tower of Virahol raw material, opening power to the heating jacket voltage of reboiler, begins heating;
2) solvent-free total reflux, give the plated film heat tracing cover tube voltage of rectifying tower, guarantee that material was unlikely to the cold internal reflux that forms in rectifying, open water coolant, prepare the condensation material, waited to reflux when occurring, keep total reflux, tower top temperature is stabilized in azeotropic temperature, and note the liquid level of tower reactor this moment, makes it keep liquid level;
3) have continuous solvent to add total reflux, solvent-free total reflux begins to add extraction agent, again total reflux;
4) the cat head 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 with the reflux ratio discharging, note the size of quantity of reflux in this process, control the flow of extraction agent according to quantity of reflux; And control cat head reflux ratio, determine the composition of cut according to cat head drop temperature and stratographic analysis result, and change in time receiving bottle to receive the cut of different concns;
5) solvent-free adding when tower top temperature reaches preset temperature, stops solubilizing agent with the difficult volatiles of reflux ratio extraction, changes receiving bottle, collects difficult volatiles; When the extraction agent of interim fraction in the holding tank dense, can stop.
The intermittent extraction, distillation and separation method of described a kind of isopropyl ether-isopropanol mixture, the device that the method adopts comprises extractive distillation column, heating kettle at the bottom of the extracting rectifying Tata, the rectifier unit that the condensing works that the extracting rectifying column overhead connects and receiving tank consist of, periodical operation separates isopropyl ether-isopropanol mixture.
Advantage of the present invention and effect are:
The present invention adopts 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 schematic flow sheet of the present invention.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
Among the 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.
The method adopts and comprises extractive distillation column, the extractive distillation column overhead condenser, and the device that heating kettle and header tank and receiving tank consist of at the bottom of the extracting rectifying Tata 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, when the cut content of overhead extraction is lower than 98.5%, stop to collect isopropyl ether when namely reaching 70-80 ℃ on the tower top temperature, then collect the interim fraction I.When temperature rises to 82.4 ℃, stop to add extraction agent, with reflux ratio 2 ~ 4, reach 99.5% Virahol from the overhead collection massfraction, when the cut content of overhead extraction is lower than 98.5%, stop to collect Virahol, then collect the interim fraction II.When the cut content of overhead extraction reaches 98%, stop to collect stopped heating.Last again reclaim and utilize the ethylene glycol monomethyl ether of tower reactor as the extraction agent of next batch periodical operation.
Embodiment:
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 the tower reactor comes to life, observe the thermometer registration of cat head, 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 cat head from extracting rectifying begins the extraction massfraction, and collect with isopropyl ether holding tank 7.When being lower than 98.5%, the isopropyl ether massfraction of overhead fraction extraction stops to collect isopropyl ether, the holding tank of migrating 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 to collect the interim fraction I, stop to add 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.When being lower than 98.5%, the Virahol massfraction of overhead fraction extraction stops to collect Virahol, 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 the 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 cat head 150mm place,, Virahol-(wherein isopropyl ether 83.7%, isopropyl ether 16.3% for the isopropyl ether mixture to add 1500ml 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 the 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 is lower than 98.5%, stop to collect 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 to add extraction agent, with reflux ratio 2:1 from extractive distillation column overhead collection Virahol, when the isopropanol content of extraction is lower than 98.5%, stop to collect 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 was higher than 98%, stopped heating also made the ethylene glycol monomethyl ether cooling, and 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 cat head 150mm place,, Virahol-(wherein isopropyl ether 85.5%, isopropyl ether 14.5% for the isopropyl ether mixture to add 1500ml 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 the 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 is lower than 98.5%, stop to collect 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 to add extraction agent, with reflux ratio 2:1 from extractive distillation column overhead collection Virahol, when the isopropanol content of extraction is lower than 98.5%, stop to collect 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 was higher than 98%, stopped heating also made the ethylene glycol monomethyl ether cooling, and 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 (2)
1. the intermittent extraction, distillation and separation method of an isopropyl ether-isopropanol mixture is characterized in that, described method comprises following process:
1) with at the bottom of isopropyl ether and the disposable adding tower of Virahol raw material, opening power to the heating jacket voltage of reboiler, begins heating;
2) solvent-free total reflux, give the plated film heat tracing cover tube voltage of rectifying tower, guarantee that material was unlikely to the cold internal reflux that forms in rectifying, open water coolant, prepare the condensation material, waited to reflux when occurring, keep total reflux, tower top temperature is stabilized in azeotropic temperature, and note the liquid level of tower reactor this moment, makes it keep liquid level;
3) have continuous solvent to add total reflux, solvent-free total reflux begins to add extraction agent, again total reflux;
4) the cat head 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 with the reflux ratio discharging, note the size of quantity of reflux in this process, control the flow of extraction agent according to quantity of reflux; And control cat head reflux ratio, determine the composition of cut according to cat head drop temperature and stratographic analysis result, and change in time receiving bottle to receive the cut of different concns;
5) solvent-free adding when tower top temperature reaches preset temperature, stops solubilizing agent with the difficult volatiles of reflux ratio extraction, changes receiving bottle, collects difficult volatiles; When the extraction agent of interim fraction in the holding tank dense, can stop.
2. the intermittent extraction, distillation and separation method of a kind of isopropyl ether-isopropanol mixture according to claim 1, it is characterized in that, the device that the method adopts comprises extractive distillation column, heating kettle at the bottom of the extracting rectifying Tata, the rectifier unit that the condensing works that the extracting rectifying column overhead connects and receiving tank consist of, periodical operation separates isopropyl ether-isopropanol mixture.
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Cited By (6)
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| CN103159598A (en) * | 2013-03-26 | 2013-06-19 | 沈阳化工大学 | Batch extractive distillation separation method of 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 |
| 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 |
| CN107759449A (en) * | 2017-09-30 | 2018-03-06 | 绍兴明业化纤有限公司 | A kind of separation method of the cyclobutenyl ether of 1,1 dimethylallyl, 3 first 2 and 3 methyl, 2 butylene 1 alcohol |
| CN111377804A (en) * | 2020-03-27 | 2020-07-07 | 山东省特种设备检验研究院潍坊分院 | Device and method for separating diisopropyl ether-isopropanol mixture by binary mixed extractant |
| CN112619195A (en) * | 2020-12-30 | 2021-04-09 | 中冶焦耐(大连)工程技术有限公司 | Refined phenol intermittent distillation control process |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159598A (en) * | 2013-03-26 | 2013-06-19 | 沈阳化工大学 | Batch extractive distillation separation method of 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 |
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| 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 |
| CN107759449A (en) * | 2017-09-30 | 2018-03-06 | 绍兴明业化纤有限公司 | A kind of separation method of the cyclobutenyl ether of 1,1 dimethylallyl, 3 first 2 and 3 methyl, 2 butylene 1 alcohol |
| CN107759449B (en) * | 2017-09-30 | 2020-12-15 | 绍兴明业化纤有限公司 | Separation method of 1, 1-dimethylallyl 3-methyl-2-butenyl ether and 3-methyl-2-butene-1-ol |
| CN111377804A (en) * | 2020-03-27 | 2020-07-07 | 山东省特种设备检验研究院潍坊分院 | Device and method for separating diisopropyl ether-isopropanol mixture by binary mixed extractant |
| CN112619195A (en) * | 2020-12-30 | 2021-04-09 | 中冶焦耐(大连)工程技术有限公司 | Refined phenol intermittent distillation control process |
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Application publication date: 20130417 |