CN107488103A - A kind of water azeotropic mixture extraction rectifying method - Google Patents
A kind of water azeotropic mixture extraction rectifying method Download PDFInfo
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present invention relates to a kind of water azeotropic mixture extraction rectifying method, water azeotropic mixture extraction rectifying method of the present invention is successional mode of operation, by selecting a variety of extractants, the product of the isopropyl alcohol and water of high-purity is obtained, and extractant can recycle.The maximum of the present invention is characterised by extraction except from conventional solvent, additionally use conventional solvent and the mixed extractant of ionic liquid composition, advantage is huge in terms of energy consumption, environmental pressure, product purity, it is particularly suitable for large-scale industrialization application, in particular for the separation of water azeotropic mixture, current technology blank has been filled up.
Description
Technical field
Separation method provided by the present invention is directed to water-azeotropic mixture, and ethylene glycol, second two is respectively adopted
The mixed solvent of alcohol and ionic liquid composition belongs to the extraction rectifying method of water-azeotropic mixture as extractant.
Background technology
In the separation method that chemical industry is commonly used, rectifying turns into the selection of numerous enterprises with the advantage of its own, still
Rectifying, which is meant that, needs energy consumption, therefore energy consumption cost also turns into the problem of enterprise needs emphasis to consider.With reference to country " 13
Five " planning and presently relevant industrial policy, energy-conservation, emission reduction turn into the most important thing of the chemical enterprise coming years.Adopted in the present invention
With extraction rectification technique, compared with traditional azeotropic distillation, significantly improved on energy consumption problem, and product purity is higher.This
The extractant used in invention, no longer it is simple organic solvent, but selects the mixing of organic solvent and ionic liquid composition
Extractant, it can substantially reduce the loss of extractant.
Ionic liquid refers to the salt compounds being in a liquid state at room temperature being made up of organic cation and anion, has
Steam forces down, fusing point is low, liquid journey is wide, easy to operate, soluble good and stablizes the advantages that high.Although ionic liquid has numerous excellent
Point, but because existing market is expensive, and the dosage of extractant is larger, causes production cost very high, therefore utilization rate
It is relatively low.Research finds, ionic liquid can form new ionic liquid with complexant, can effectively reduce industrial applications into
Originally, the advantages of and having both concurrently simultaneously, conventional complexant have ethylene glycol, glycerine etc., and the complexant that the present invention selects is second two
Alcohol, mixed solvent is formed with ionic liquid.The advantages of based on ionic liquid, can be used in rectification process conventional organic solvents with from
The mixed liquor of sub- liquid can effectively reduce the loss of conventional solvent as extractant（Ionic liquid is non-volatile, loss late pole
It is low, and recycle）, production cost is reduced, while product quality can be improved.
Isopropanol is widely used in the production of antibiotics as a kind of excellent organic solvent, therefore generates
Largely the industrial wastewater containing isopropanol needs to recycle.Due to isopropanol azeotrope with water（80.3 DEG C of azeotropic point, wherein isopropanol matter
Measure fraction 87.4%）, conventional distillation is difficult to obtain high-purity isopropanol, should use special extract rectification.At present, industrially frequently with extraction
Rectifying is taken to reclaim isopropanol from Iso-Propylalcohol wastewater.
A kind of methods of separating isopropanol-aqueous mixtures of Chinese patent CN103467246A, are disclosed using isopropanol-water
Mixture is raw material, and the double solvents formed using ionic liquid or ionic liquid with organic solvent is extractant, and raw material is by extraction
After taking stage of rectification and extractant recovery stage, isopropyl alcohol and water successively produces, and extractant is by recovery stage extraction Posterior circle
Use.The extractant wherein used has expensive, production cost height, and process energy consumption is big, is not easy to industrialize, installation cost
With it is high the shortcomings that.
Chinese patent CN102952004A proposes a kind of technique side of continuous azeotropic distillation separation glycol monoethyl ether-water
Method, entrainer is disposably added in kettle in the technique, using universal double tower reflux technique.The invention major defect is：Say
The compensation problem of entrainer is not referred in bright book, because the continuous operation cycle is longer, partially azeotropic agent can adopting with product
Go out and be lost in, cause azeotropic agent content in system constantly to reduce, cause the quality of product to be difficult to ensure that stabilization；Furthermore the technique is pressed
According to traditional reflux type, cause the increase of energy consumption；In addition the technique does not have the discharge for referring to entrainer recovery tower tower reactor water
Whether discharge standard is reached.In a word, how reducing loss of extractant and production cost, improving product purity is current rectification process
Need to solve the problems, such as.
The content of the invention
It is insufficient present in existing process the invention aims to overcome, and water-azeotropic mixture is directed to,
It is proposed that a kind of good separating effect, product purity are high, energy consumption is low, and extractant easily reclaims, is easy to industrialized separation method.The party
Method is mixed using ionic liquid or ionic liquid with the double solvents that organic solvent forms as extractant separation water-azeotropic
Thing, and provide the process units applied to this method.
In order to solve the above-mentioned technical problem, the present invention takes following technical scheme：
A kind of water-azeotropic mixture extraction rectifying method, it is characterised in that：This method is divided into continuity operation, wherein
Continuity operation includes extractive distillation column, solvent recovery tower, reboiler, condenser, and preheater.
Further, the continuity mode of operation mainly has following steps：
A. the mixture of water-isopropanol is entered in extractive distillation column tower by head tank or feed pump；
B. after overhead reflux stabilization is heated in extractive distillation column tower reactor, extractant passes through head tank or feed pump conveys
To preheater and enter in tower；
C. after gas-liquid composition is stable in extractive distillation column tower, tower top temperature is 80 ~ 85 DEG C and starts to produce isopropanol；
D. extractive distillation column kettle material is delivered to solvent recovery tower through delivery pump, after solvent recovery column overhead is stable, tower top temperature
Spend and return extractive distillation column for 101 ~ 105 DEG C of recovered waters, extractant and recycle.
Further, the continuity operation extractant is that the mixing of ethylene glycol or ethylene glycol and ionic liquid composition extracts
Take agent.
Further, the mixed extractant intermediate ion liquid is respectively N- picoline dimethyl phosphates salt, N- second
The one or two kinds of mixture of yl pyridines dimethyl phosphate salt.
Further, in the mixed extractant that the ethylene glycol forms with ionic liquid, ionic liquid mass fraction is
30wt%~40wt%。
Further, in the continuity mode of operation, the matter containing nano titanium oxide in the mixture of ionic liquid
Amount fraction is 5wt% ~ 8wt%.
Further, in the continuity mode of operation, the particle diameter of nano titanium oxide in the mixture of ionic liquid
For 60 ~ 80nm；
Further, under the continuity mode of operation, the operating condition of extractive distillation column is normal pressure, mixed extractant from 2 ~
10 blocks of column plates enter extractive distillation column, and raw material enters from 6 ~ 36 blocks of column plates；The operating condition of solvent recovery tower is decompression, and extraction is smart
Evaporate the tower bottoms of tower from the 10th ~ 40 block of column plate of solvent recovery tower tower to enter, tower top can obtain water, and the hybrid extraction of bottom of towe
Agent can return to extractive distillation column, recycle.
Further, extractive distillation column operating pressure described in the continuity operating process is 101.3kPa, backflow
Than being for 0.5-2.0, the addition of extractant and the mass ratio of raw material（0.1-2.0）：1;The solvent recovery tower operating pressure
For 55-98kPa.
Further, the main function of aforesaid operations is：
Extractant of the present invention is respectively that ethylene glycol, ethylene glycol and ionic liquid form mixed extractant, can be effective
Product purity and extraction efficiency are improved, reduces production cost.The ionic liquid that the present invention uses is respectively N- ethylpyridine phosphoric acid
Dimethyl ester salt, water-isopropanol N- picoline dimethyl phosphates salt, N- butyl-pyridinium dimethyl phosphate salt, are combined with ethanol, can
To effectively reduce the loss of conventional solvent, cost is reduced, while improve product quality.
5wt% ~ 8wt% nano titanium oxide is added in heretofore described ionic liquid so that ionic liquid is continuous
In rectifying extraction process, fully, heat is quickly absorbed, effectively heat transfer, the energy loss in diabatic process is reduced, to keep
Rectification system energy stabilization, extraction efficiency and product purity are improved, makes the fast and effective progress of separation process.
The mixture of reclaimed water-isopropanol of the present invention is directly entered in extractive distillation column tower by head tank or feed pump,
Preheating is required no, on the one hand can reduce the loss of raw material, improves extraction efficiency, on the other hand requiring no preheater can also
The energy is saved, reduces cost；Mixed extractant by preheater preheating by entering back into extractive distillation column, Ke Yibao in the present invention
Card extracts fast and effective progress so that azeotropic mixture and extractant faster merge, rapid extraction, avoid heat transfer loss and reduce to extract
Efficiency.
Another object of the present invention is to provide a kind of rectifying dress of method for separation water-azeotropic system
To put, the rectifier unit of the continuity operation includes extractive distillation column and solvent recovery tower equipped with 10-45 block theoretical cam curves,
The discharging opening of the tower reactor of the extractive distillation column is connected with the charging aperture of the solvent recovery tower, the solvent recovery tower bottom
Discharging opening be connected with the extractant feed mouth of the extractive distillation column；Material inlet, the extractant of the rectifying column enter
Material mouth is respectively arranged at the 2nd ~ 10 block of theoretical tray of the rectifying column and at the 6th ~ 36 block of theoretical tray；The recovery tower enters
Material mouth is located at the middle and lower part of the recovery tower.
It is an advantage of the invention that：
1. the double solvents that the present invention is formed with organic solvent using ionic liquid or ionic liquid is extractant, to production equipment without
Corrosion, it is pollution-free, it is lossless, easily recovery, it can be recycled, it is safe to use, the relative of isopropanol-water can be dramatically increased and waved
Hair degree realizes efficiently separating for thing system, while can reduce cost；Simultaneously nano titanium oxide is added in ionic liquid so that from
Sub- liquid fully, quickly absorbs heat in continuous rectification extraction process, effectively heat transfer, reduces the energy in diabatic process
Loss, to keep rectification system energy stabilization, extraction efficiency and product purity are improved, makes the fast and effective progress of separation process.
Solvent recovery tower of the present invention uses rectification under vacuum, can effectively reduce energy consumption, by improving the relatively volatile of raw material
Degree, by using rectification under vacuum, can reduce production cost to improve product purity by reducing the grade of heating agent
3. present invention process is simple, using double tower continuous rectification mode, it can be selected according to product yield requirement, be easy to grasp
Make, treating capacity is big, and energy consumption is low, good in economic efficiency while effectively reduce cost.
The method of the present invention can handle the isopropanol-water thing system of any composition, save because of original to material purity no requirement (NR)
Production cost and energy consumption caused by expecting concentrate, the isopropanol purity for making to be obtained by the present invention are more than 99.9%, and yield is more than
99.3%。
Brief description of the drawings
Fig. 1 is that the continuity for being used for separation water-azeotropic mixture in the present invention operates rectifier unit.
Marked in figure：T1- rectifying columns；T2- recovery towers；F1- rectifying column material inlets；F2- rectifying column extractant feeds
Mouthful；The tower top discharging opening of P1- rectifying columns；The tower top discharging opening of P2- recovery towers；S1- tower bottom of rectifying tower discharging openings；S2- recovery towers
Tower reactor discharging opening；1,2- tower reactor reboilers；3,4- overhead condensers；5- preheaters.
Embodiment
Embodiments of the invention are described in detail below, the present invention can be defined by the claims and cover a variety of
Various combination mode is implemented.
Experimental method in following embodiments, it is conventional method unless otherwise specified.Original used in following embodiments
Material, related dispensing etc., unless otherwise specified, are commercially available products.
Embodiment 1
（1）A kind of water-azeotropic mixture extraction rectifying method
The technological process as shown in accompanying drawing 1,
A. by the mixture of water-isopropanol（Isopropanol 45%, water 55%, mass fraction）A high position is passed through with 1000kg/hr flow
Groove or feed pump enter in extractive distillation column T1 towers from the 36th piece；
B. after overhead reflux stabilization is heated in extractive distillation column T1 tower reactors, N- picoline dimethyl phosphate salt and second two
Alcohol volume ratio 2：The extractant of 1 composition is delivered to preheater 5 by head tank or feed pump and entered from the 5th block of theoretical tray
In T1 towers；Atmospheric operation；
In aforesaid operations, the mass fraction containing nano titanium oxide is 5wt% in N- picoline dimethyl phosphate salt；Nanometer
The particle diameter of titanium dioxide is 60 ~ 80nm.
The addition of extractant and the mass ratio of raw material are 2.0, and reflux ratio 1, recovery tower T2 operating pressures are 98kPa,
After gas-liquid composition is stable in extractive distillation column T1 towers, T1 tower top temperatures are 80 DEG C and start to produce isopropanol, flow 446.8kg/
Hr, composition：Isopropanol 99.93%, water 0.07%, isopropanol yield 99.3%；
D. extractive distillation column T1 kettle materials are delivered to solvent recovery tower T2 through delivery pump S1, and solvent recovery tower T2 tower tops are stable
Afterwards, T2 tower top temperatures are 101 DEG C of recovered waters, and recovery tower T2 bottom of towe extraction extractant, water content 0.13%, it is smart that extractant returns extraction
Tower T1 is evaporated to recycle.
Embodiment 2
（1）A kind of water-azeotropic mixture extraction rectifying method
The technological process as shown in accompanying drawing 1,
A. by the mixture of water-isopropanol（Isopropanol 35%, water 65%, mass fraction）A high position is passed through with 1200kg/hr flow
Groove or feed pump enter in extractive distillation column T1 towers from the 26th piece；
B. after overhead reflux stabilization is heated in extractive distillation column T1 tower reactors, N- picoline dimethyl phosphates salt, N- second
Yl pyridines dimethyl phosphate salt and ethylene glycol volume ratio 1：1.5：The extractant of 1 composition is delivered to by head tank or feed pump
Preheater 5 simultaneously enters in T1 towers from the 3rd block of theoretical tray；Atmospheric operation；
Contain in aforesaid operations, in the mixture of N- picoline dimethyl phosphate salt and N- ethylpyridine dimethyl phosphate salt and receive
The mass fraction of rice titanium dioxide is 8wt%；The particle diameter of nano titanium oxide is 60 ~ 80nm.
The addition of extractant and the mass ratio of raw material are 1.6, reflux ratio 2.0, and recovery tower T2 operating pressures are
88kPa, after gas-liquid composition is stable in extractive distillation column T1 towers, T1 tower top temperatures are 81 DEG C and start to produce isopropanol, and flow is
416.2kg/hr, composition：Isopropanol 99.94%, water 0.06%, isopropanol yield 99.1%；
D. extractive distillation column T1 kettle materials are delivered to solvent recovery tower T2 through delivery pump S1, and solvent recovery tower T2 tower tops are stable
Afterwards, T2 tower top temperatures are 101.5 DEG C of recovered waters, and recovery tower T2 bottom of towe extraction extractant, water content 0.12%, extractant, which returns, to be extracted
Rectifying column T1 is recycled.
Embodiment 3
（1）A kind of water-azeotropic mixture extraction rectifying method
The technological process as shown in accompanying drawing 1,
A. by the mixture of water-isopropanol（Isopropanol 55%, water 45%, mass fraction）A high position is passed through with 1000kg/hr flow
Groove or feed pump enter in extractive distillation column T1 towers from the 32nd piece；
B. after overhead reflux stabilization is heated in extractive distillation column T1 tower reactors, N- picoline dimethyl phosphate salt and N- second
Yl pyridines dimethyl phosphate salt volume ratio 1.5：The extractant of 1 composition is delivered to preheater 5 simultaneously by head tank or feed pump
Enter from the 5th block of theoretical tray in T1 towers；Atmospheric operation；
Contain in aforesaid operations, in the mixture of N- picoline dimethyl phosphate salt and N- ethylpyridine dimethyl phosphate salt and receive
The mass fraction of rice titanium dioxide is 7wt%；The particle diameter of nano titanium oxide is 60 ~ 80nm.
The addition of extractant and the mass ratio of raw material are 1.2, reflux ratio 0.8, and recovery tower T2 operating pressures are
78kPa, after gas-liquid composition is stable in extractive distillation column T1 towers, T1 tower top temperatures are 81.9 DEG C and start to produce isopropanol；
546.7kg/hr, composition：Isopropanol 99.95%, water 0.05%, isopropanol yield 99.4%；
D. extractive distillation column T1 kettle materials are delivered to solvent recovery tower T2 through delivery pump S1, and solvent recovery tower T2 tower tops are stable
Afterwards, T2 tower top temperatures are 105 DEG C of recovered waters, and recovery tower T2 bottom of towe extraction extractant, water content 0.12%, it is smart that extractant returns extraction
Tower T1 is evaporated to recycle.
Embodiment 4
（1）A kind of water-azeotropic mixture extraction rectifying method
The technological process as shown in accompanying drawing 1,
A. by the mixture of water-isopropanol（Isopropanol 60%, water 40%, mass fraction）A high position is passed through with 1200kg/hr flow
Groove or feed pump enter in extractive distillation column T1 towers from the 32nd piece；
B. after overhead reflux stabilization is heated in extractive distillation column T1 tower reactors, N- ethylpyridine dimethyl phosphates salt composition
Extractant is delivered to preheater 5 by head tank or feed pump and entered from the 5th block of theoretical tray in T1 towers；Atmospheric operation；
In aforesaid operations, the mass fraction containing nano titanium oxide is 5wt% in N- ethylpyridine dimethyl phosphate salt；Nanometer
The particle diameter of titanium dioxide is 60 ~ 80nm.
The addition of extractant and the mass ratio of raw material are 1.0, reflux ratio 0.7, and recovery tower T2 operating pressures are
68kPa, after gas-liquid composition is stable in extractive distillation column T1 towers, T1 tower top temperatures are 85 DEG C and start to produce isopropanol, and flow is
715.0kg/hr, composition：Isopropanol 99.96%, water 0.04%, isopropanol yield 99.3%；
D. extractive distillation column T1 kettle materials deliver to solvent recovery tower T2 through the defeated S1 of delivery pump, and solvent recovery tower T2 tower tops are stable
Afterwards, T2 tower top temperatures are 103.6 DEG C of recovered waters, and recovery tower T2 bottom of towe extraction extractant, water content 0.11%, extractant, which returns, to be extracted
Rectifying column T1 is recycled.
Embodiment 5
（1）A kind of water-azeotropic mixture extraction rectifying method
The technological process as shown in accompanying drawing 1,
A. by the mixture of water-isopropanol（Isopropanol 75%, water 25%, mass fraction）A high position is passed through with 1000kg/hr flow
Groove or feed pump enter in extractive distillation column T1 towers from the 22nd piece；
B. after overhead reflux stabilization is heated in extractive distillation column T1 tower reactors, N- picoline dimethyl phosphate salt and second two
Alcohol volume ratio 1：The extractant of 1 composition is delivered to preheater 5 by head tank or feed pump and entered from the 5th block of theoretical tray
In T1 towers；Atmospheric operation；
In aforesaid operations, nano titanium oxide is free of in N- picoline dimethyl phosphate salt.
The addition of extractant and the mass ratio of raw material are 0.6, and reflux ratio 1, recovery tower T2 operating pressures are 88kPa,
After gas-liquid composition is stable in extractive distillation column T1 towers, T1 tower top temperatures are 84 DEG C and start to produce isopropanol；746.2kg/hr, group
Into：Isopropanol 98.93%, water 1.07%, isopropanol yield 98.5%；
D. extractive distillation column T1 kettle materials are delivered to solvent recovery tower T2 through delivery pump S1, and solvent recovery tower T2 tower tops are stable
Afterwards, T2 tower top temperatures are 102 DEG C of recovered waters, and recovery tower T2 bottom of towe extraction extractant, water content 0.08%, it is smart that extractant returns extraction
Tower T1 is evaporated to recycle.
Embodiment 6
（1）A kind of water-azeotropic mixture extraction rectifying method
The technological process as shown in accompanying drawing 1,
A. by the mixture of water-isopropanol（Isopropanol 95%, water 5%, mass fraction）Head tank is passed through with 1000kg/hr flow
Or feed pump enters in extractive distillation column T1 towers from the 26th piece；
B. after overhead reflux stabilization is heated in extractive distillation column T1 tower reactors, N- picoline dimethyl phosphates salt, N- second
Yl pyridines dimethyl phosphate salt and ethylene glycol volume ratio 2：1：The extractant of 1 composition is delivered to pre- by head tank or feed pump
Hot device 5 simultaneously enters in T1 towers from the 5th block of theoretical tray；Atmospheric operation；
Contain in aforesaid operations, in the mixture of N- picoline dimethyl phosphate salt and N- ethylpyridine dimethyl phosphate salt and receive
The mass fraction of rice titanium dioxide is 6%；The particle diameter of nano titanium oxide is 60 ~ 80nm.
The addition of extractant and the mass ratio of raw material are 2.0, and reflux ratio 1, recovery tower T2 operating pressures are 58kPa,
After gas-liquid composition is stable in extractive distillation column T1 towers, T1 tower top temperatures are 83.1 DEG C and start to produce isopropanol, and flow is
946.2kg/hr, composition：Isopropanol 99.98%, water 0.02%, isopropanol yield 99.6%；
D. extractive distillation column T1 kettle materials are delivered to solvent recovery tower T2 through delivery pump S1, and solvent recovery tower T2 tower tops are stable
Afterwards, T2 tower top temperatures are 102.5 DEG C of recovered waters, and recovery tower T2 bottom of towe extraction extractant, water content 0.08%, extractant, which returns, to be extracted
Rectifying column T1 is recycled.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
- A kind of 1. water-azeotropic mixture extraction rectifying method, it is characterised in that：This method is divided into continuity operation, its Middle continuity operation includes extractive distillation column, solvent recovery tower, reboiler, condenser, and preheater.
- 2. water according to claim 1-azeotropic mixture extraction rectifying method, it is characterised in that：It is described continuous Property mode of operation mainly has following steps：A. the mixture of water-isopropanol is entered in extractive distillation column tower by head tank or feed pump；B. after overhead reflux stabilization is heated in extractive distillation column tower reactor, extractant passes through head tank or feed pump conveys To preheater and enter in tower；C. after gas-liquid composition is stable in extractive distillation column tower, tower top temperature is 80 ~ 85 DEG C and starts to produce isopropanol；D. extractive distillation column kettle material is delivered to solvent recovery tower through delivery pump, after solvent recovery column overhead is stable, tower top temperature Spend and return extractive distillation column for 101 ~ 105 DEG C of recovered waters, extractant and recycle.
- 3. water according to claim 1-azeotropic mixture extraction rectifying method, it is characterised in that：It is described continuous Property operation extractant be ethylene glycol or ethylene glycol and ionic liquid composition mixed extractant.
- 4. water according to claim 1-azeotropic mixture extraction rectifying method, it is characterised in that：The mixing Extractant intermediate ion liquid is respectively N- picoline dimethyl phosphates salt, N- ethylpyridine dimethyl phosphates salt one kind or two The mixture of kind.
- 5. water according to claim 1-azeotropic mixture extraction rectifying method, it is characterised in that：The second two In the mixed extractant that alcohol forms with ionic liquid, ionic liquid mass fraction is 30wt% ~ 40wt%.
- 6. water according to claim 1-azeotropic mixture extraction rectifying method, it is characterised in that：It is described continuous In property mode of operation, the mass fraction containing nano titanium oxide is 5wt% ~ 8wt% in the mixture of ionic liquid.
- 7. water according to claim 1-azeotropic mixture extraction rectifying method, it is characterised in that：It is described continuous In property mode of operation, the particle diameter of nano titanium oxide is 60 ~ 80nm in the mixture of ionic liquid.
- 8. water according to claim 1-azeotropic mixture extraction rectifying method, it is characterised in that：It is described continuous Under property mode of operation, the operating condition of extractive distillation column is normal pressure, and mixed extractant enters extractive distillation column from 2 ~ 10 blocks of column plates, Raw material enters from 6 ~ 36 blocks of column plates；The operating condition of solvent recovery tower is decompression, and the tower bottoms of extractive distillation column is from solvent recovery 10th ~ 40 block of column plate of tower tower enters, and tower top can obtain water, and the mixed extractant of bottom of towe can return to extractive distillation column, follow Ring uses.
- 9. water according to claim 1-azeotropic mixture extraction rectifying method, it is characterised in that：It is described continuous Property operating process described in extractive distillation column operating pressure be 101.3kPa, reflux ratio 0.5-2.0, the addition of extractant with The mass ratio of raw material is（0.1-2.0）：1；The solvent recovery tower operating pressure is 55-98kPa.
- A kind of 10. rectifier unit for claim 1 methods described, it is characterised in that：The rectifying dress of the continuity operation Put and go out including extractive distillation column and solvent recovery tower equipped with 10-45 block theoretical cam curves, the tower reactor of the extractive distillation column Material mouth is connected with the charging aperture of the solvent recovery tower, discharging opening and the extractive distillation column of the solvent recovery tower bottom Extractant feed mouth be connected；Material inlet, the extractant feed mouth of the rectifying column are respectively arranged on the rectifying column At 2nd ~ 10 block of theoretical tray and at the 6th ~ 36 block of theoretical tray；Under the charging aperture of the recovery tower is located in the recovery tower Portion.
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| CN201710736333.4A CN107488103B (en) | 2017-08-24 | 2017-08-24 | Extraction and rectification method for water-isopropanol azeotropic mixture |
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| CN201710736333.4A CN107488103B (en) | 2017-08-24 | 2017-08-24 | Extraction and rectification method for water-isopropanol azeotropic mixture |
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| CN111662161A (en) * | 2020-06-28 | 2020-09-15 | 浙江工业大学 | Method for separating water-ethanol-isopropanol mixture by extractive distillation |
| CN113968773A (en) * | 2021-11-15 | 2022-01-25 | 江苏三贵资源再生有限公司 | Method for separating isopropanol and water by extractive distillation |
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