CN105503501B - A kind of butanol hexamethylene azeotropic mixture extraction rectifying method - Google Patents

A kind of butanol hexamethylene azeotropic mixture extraction rectifying method Download PDF

Info

Publication number
CN105503501B
CN105503501B CN201610026620.1A CN201610026620A CN105503501B CN 105503501 B CN105503501 B CN 105503501B CN 201610026620 A CN201610026620 A CN 201610026620A CN 105503501 B CN105503501 B CN 105503501B
Authority
CN
China
Prior art keywords
butanol
extractant
tower
hexamethylene
extractive distillation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201610026620.1A
Other languages
Chinese (zh)
Other versions
CN105503501A (en
Inventor
姜占坤
刘顺江
孙国新
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Jinan
Original Assignee
University of Jinan
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Jinan filed Critical University of Jinan
Priority to CN201610026620.1A priority Critical patent/CN105503501B/en
Publication of CN105503501A publication Critical patent/CN105503501A/en
Application granted granted Critical
Publication of CN105503501B publication Critical patent/CN105503501B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/04—Purification; Separation; Use of additives by distillation
    • C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
    • C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
    • 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
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

A kind of butanol hexamethylene azeotropic mixture extraction rectifying method, butanol of the present invention includes the mode of operation or decompression intermittent operation mode of decompressing and continuous with hexamethylene azeotropic mixture extraction rectifying method, by selecting a variety of extractants, the butanol and cyclohexane product of high-purity are 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 butanol hexamethylene azeotropic system, current technology blank has been filled up.

Description

A kind of butanol-hexamethylene azeotropic mixture extraction rectifying method
Technical field
Separation method provided by the present invention is directed to butanol-hexamethylene azeotropic system, and ethylene glycol, second two is respectively adopted The mixed solvent of alcohol and ionic liquid composition belongs to the extraction rectifying method of butanol-hexamethylene azeotropic system as extractant.
Background technology
The raw material being related in the present invention is butanol and hexamethylene, both material common in chemical industry.Butanol （C4H10O）, also known as tyrosol, the third carbinol, it is the solvent of multiple coating and plasticizer phthalic acid dibutyl ester processed（See O-phthalic Acid esters）Raw material, be also used for manufacturing butyl acrylate, butyl acetate, butyl glycol ether and as organic synthesis intermediate and The extractant of biochemical medicine, it is additionally operable to manufacture surfactant.Hexamethylene（C6H12）, it is mainly used as rubber, coating, varnish Solvent, the diluent of adhesive, oil extraction agent.Because of the small toxicity of hexamethylene, therefore benzene is often replaced to be used for de-oiling fat, de- lubricating grease And depainting.It is also commonly used for manufacturing monomer adipic acid, hexamethylene diamine and the caprolactam of nylon, also serves as manufacture cyclohexanol, cyclohexanone Raw material.
Butanol not only has important application with hexamethylene in petrochemical industry, and also has phase inside other industry Used when extensive.But but there is azeotropism in two kinds of materials so that the difficulty for separating both greatly increases.For organic The recovery of solvent, it is industrial it is widely used be distillation or rectifying processing mode, but for azeotropic system, the country uses More is azeotropic distillation method.But azeotropic distillation has the limitation of its own：In terms of energy consumption, cost is compared with other method more Height, in equipment investment, also tend to bigger compared with other method, and product purity is difficult to ensure that.
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.It was discovered by researchers that ionic liquid can form new ionic liquid with complexant, industrial applications can be effectively reduced Cost, and the advantages of have both concurrently simultaneously, conventional complexant has ethylene glycol, glycerine etc., and the complexant that the present invention selects is Ethylene glycol, mixed solvent is formed with ionic liquid.
The advantages of based on ionic liquid, the mixed liquor conduct of conventional organic solvents and ionic liquid can be used in rectification process Extractant, the loss of conventional solvent can be effectively reduced（Ionic liquid is non-volatile, loss late is extremely low, and recycles）, drop Low production cost, while product quality can be improved.
Existing azeotropic system separation means are divided into two classes substantially：Azeotropic distillation and extracting rectifying.Extracting rectifying is in product There is advantage compared with azeotropic distillation in terms of purity, energy consumption.And at present in the selection of extractant, substantially using conventional solvent conduct Extractant directly uses ion liquid abstraction agent, a kind of sides of continuous extraction separation mixed alcohol-water of CN103193590A in other words A kind of technique of separation of extractive distillation Ethyl formate-alcohol-water of method, CN102627556A makees extractant using ethylene glycol； The method of CN103193590A ion liquid abstractions rectifying separation Acetic Acid-Water uses ionic liquid as extractant.The former is extracting Take low in efficiency, and the latter is then much bigger in cost of investment.Sum it up, how to reduce loss of extractant and be produced into Originally the problem of product purity is current rectification process urgent need to resolve, is improved.
At present, the document or report of the separation on butanol-hexamethylene azeotropic system, not correlation.
The content of the invention
It is insufficient present in existing process the invention aims to overcome, and butanol-hexamethylene azeotropic system 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.Pass through T-x-y phasors, it can be seen that butanol-hexamethylene has azeotropism（It can be seen that butanol-hexamethylene has azeotropic in accompanying drawing 1 Point）.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of butanol-hexamethylene azeotropic mixture extraction Rectificating method is taken, this method is operated using continuity or intermittent operation.
Extractant described in the invention is respectively ethylene glycol, ethylene glycol and ionic liquid（40wt%~50wt%）Formed mixed Extractant is closed, product purity and extraction efficiency can be effectively improved, reduces production cost.Inventing the ionic liquid used is respectively N- ethylpyridine dimethyl phosphate salt（[epy][DMP]）, N- picoline dimethyl phosphate salt（[mpy][DMP]）, N- butyl Pyridine dimethyl phosphate salt（[bpy][DMP]）.
A kind of butanol of the present invention-hexamethylene azeotropic mixture extraction rectifying method continuity operating procedure is as follows：
1）Butanol is continuously added to cyclohexane mixtures by T101 middle and lower parts by feed system, and extractant adds from tower top Enter, feeding temperature is all normal temperature, and T101 operating pressures are 0.3atm（Absolute pressure）；
2）T101 tower tops can obtain the cyclohexane product of product purity more than 99.9%, and bottom of towe is butanol and extractant；
3）T101 tower base streams enter T102 middle part, and the butanol product of purity more than 99.9%, tower are obtained in T102 tower tops Bottom residue extractant and micro butanol and hexamethylene, T102 operating pressures are 0.3atm（Absolute pressure）；
4）T102 tower base streams are incorporated to extractant feed pipeline, are supplemented as extractant.
Based on a kind of above-mentioned butanol-hexamethylene azeotropic mixture extraction rectifying method continuity operation, continuity behaviour It is as important technological parameters：
1）T101 technical parameters：Tower theoretical cam curve=35 ~ 60；Reflux ratio=2:1~4:1, operating pressure=0.3atm；Extraction Agent is respectively the mixed extractant of ethylene glycol, ethylene glycol and ionic liquid composition（Wherein ionic liquid be content 40wt% ~ 50wt% N- ethylpyridine dimethyl phosphate salt（[epy][DMP]）, N- picoline dimethyl phosphate salt（[mpy][DMP]）、 N- butyl-pyridinium dimethyl phosphate salt（[bpy][DMP]））；Charge ratio=1.5 of extractant and raw material:1~5:1, feeding temperature= 30 DEG C ~ 40 DEG C, pressure=0.11MPa, raw material is butanol（93wt%）With hexamethylene（7wt%）Nearly azeotropic composition, feeding temperature= 30 DEG C ~ 40 DEG C, pressure=0.11MPa；Bottom temperature=125 DEG C ~ 131 DEG C, tower top temperature=44 DEG C ~ 49 DEG C.Extracted feed position is 3 ~ 9 blocks of column plates, 28 ~ 45 blocks of feedstock position column plate；
2）T102 technical parameters：Theoretical cam curve=30 ~ 45；Reflux ratio=1:1~4:1, operating pressure=0.3atm；Tower reactor temperature =161 DEG C ~ 167 DEG C of degree, tower top temperature=85 DEG C ~ 90 DEG C, feed entrance point is 23 ~ 36 blocks of column plates.
A kind of butanol of the present invention-hexamethylene azeotropic mixture extraction rectifying method intermittent operation step is as follows：
1）Butanol disposably squeezes into tower bottom of rectifying tower E1 with cyclohexane mixtures by raw material pump P2, opens heating；
2）When condensate liquid, total reflux operation occurs in tower top, and extractant is continuously added in tower by pump P1, and continued complete Reflux operation；
3）When tower top temperature reaches 43 DEG C, detection, tower top cyclohexane content is more than 99%, with reflux ratio（2~4）:1 extraction ring Hexane product is to V3（With the rise of tower top temperature, reflux ratio is accordingly improved to 4:1）；
4）When tower top temperature is more than 50 DEG C, and detect that cyclohexane content starts to reduce, close extraction, carry out infinite reflux behaviour Make 0.5h, start afterwards with reflux ratio（2~5）:1 extraction hexamethylene-butanol changeover portion to V2（With the rise of tower top temperature, return Stream is improved to 5 than corresponding:1）；
5）When tower top temperature reaches 82 DEG C, detection, tower top butanol content is more than 99%, with reflux ratio（1~4）:1 extraction butanol Product is to V5（With the rise of tower top temperature, reflux ratio is accordingly improved to 4:1）；
6）When tower top temperature is more than 90 DEG C, and detect that butanol content starts to reduce, stop adding extractant and closing adopting Go out, infinite reflux 0.2h, start afterwards with（2~4）:1 extraction butanol-ethylene glycol changeover portion to V4；
7）When tower top temperature is more than 120 DEG C, stopping is heated, and after the cooling of tower reactor extractant, it is standby to be discarded to V1.
Based on a kind of above-mentioned butanol-hexamethylene azeotropic mixture extraction rectifying method intermittent operation step, operation step Suddenly main important technological parameters are
1）Extractive distillation column theoretical cam curve=38 ~ 55, operating pressure 0.3atm；
2）The charge ratio of extractant and raw material=(1.5 ~ 5):1.
Beneficial effects of the present invention：The present invention can make butanol-hexamethylene azeotropism disappear by adding extractant （Azeotropic point disappears in accompanying drawing 2）.
The novelty of the present invention is with advantage：
1）The separation of butanol and hexamethylene azeotropic system, separating technology there is no to report or deliver at present；
2）It is various using a variety of extractants, selectivity；
3）Using rectification under vacuum, energy consumption can be effectively reduced, it is pure to improve product by improving the relative volatility of raw material Degree, and by using rectification under vacuum, production cost can be reduced by reducing the grade of heating agent；
4）Ionic liquid is being with the addition of in extractant, it is possible to increase the service efficiency of extractant, reduces cost；
5）Technique is simple, using double tower continuous rectification mode（T101 towers are extractive distillation column, and T102 towers are solvent recovery Tower）Or single column batch fractionating mode, it can be selected according to product yield requirement, operation is flexible, while effectively reduces cost.
Brief description of the drawings
Fig. 1 is the T-x-y phasors of butanol-hexamethylene.
Fig. 2 is that butanol-hexamethylene adds the T-x-y phasors after extractant.
Fig. 3 is continuity operation device of the present invention and flow chart.
Fig. 4 is intermittent operation device of the present invention and flow chart.
Fig. 3 mainly flows stock explanation：1.-extractant enters tower stream stock；2.-raw material enters tower stream stock；3. extractive distillation column flows back Flow stock；4.-extractive distillation column extraction stream stock；5.-solvent recovery tower enters stream stock；6.-solvent recovery tower backflow stream stock； 7.-solvent recovery tower extraction stream stock；8.-extractant extraction stream stock.
Fig. 3 capital equipment explanations：T101-extractive distillation column；T102-solvent recovery tower；E101, E103-condenser； E102, E103-reboiler；P101-material pump.
Fig. 4 is intermittent operation device of the present invention and schematic flow sheet.
Fig. 4 symbol descriptions：P1-extractant feed pump；P2-feedstock pump；E1-tower reactor；E2-condenser（Containing catching Storage）；V1 ~ V5 be respectively extractant recycling can, interim fraction tank 1., products pot 1., interim fraction tank 2., products pot 2..
Embodiment
It is that the invention will be further described for combination specific implementation case below, but does not limit the scope of protection of the invention.
Embodiment one
The implementation case is continuous extraction distillation operation mode, and as shown in Figure 3, extractant selects ethylene glycol and N- methyl Pyridine dimethyl phosphate salt（[mpy][DMP]）, dosage 150kg/h；Feed throughput is 100kg/h, and raw material composition is butanol （93wt%）With hexamethylene（7wt%）.The T101 numbers of plates are 55, and in the 5th block of column plate, feedstock position exists for extractant feed position 45 blocks of column plates.Reflux ratio is set as 4:1, overhead extraction speed is 93kg/h, and obtained cyclohexane purity is 99.7%.T102 towers Plate number is 35, and 5. feed entrance point is the 7th block of column plate to stream stock, reflux ratio 2:1, overhead extraction speed is 7kg/h, obtained butanol Purity is 99.6%.Bottom of towe extractant flows back, the supplement as solvent.
Embodiment two
Extractant selects ethylene glycol, dosage 400kg/hr, T101 reflux ratio is set into 3:1, T102 reflux ratio is set For 4:1, other conditions such as embodiment one.Obtained butanol is with cyclohexane product purity more than 99.9%.
Embodiment three
The implementation case is batch extracting rectified mode of operation, and as shown in Figure 4, extractant selects ethylene glycol and N- methyl Pyridine dimethyl phosphate salt（[mpy][DMP]）, dosage 500kg；Feed throughput is 100kg, and raw material composition is butanol （93wt%）With hexamethylene（7wt%）.Extracting rectifying column plate number is 55, and extractant feed position is in the 5th block of column plate；Butanol and hexamethylene Alkane mixture disposably squeezes into tower bottom of rectifying tower E1 by raw material pump P2, opens heating；When condensate liquid, infinite reflux behaviour occurs in tower top Make, and extractant is continuously added in tower by pump P1, and continue total reflux operation；When tower top temperature reaches 43 DEG C, detection, tower Apical ring hexane content is more than 99%, with reflux ratio（2~4）:1 produces cyclohexane product to V3（With the rise of tower top temperature, backflow Improved than corresponding to 4:1）；When tower top temperature is more than 50 DEG C, and detect that cyclohexane content starts to reduce, close extraction, carry out Total reflux operation 0.5h, start afterwards with reflux ratio（2~5）:1 extraction hexamethylene-butanol changeover portion to V2（With tower top temperature Rise, reflux ratio accordingly improved to 5:1）；When tower top temperature reaches 82 DEG C, detection, tower top butanol content is more than 99%, to return Stream ratio（1~4）:1 produces butanol product to V5（With the rise of tower top temperature, reflux ratio is accordingly improved to 4:1）；When tower top temperature Degree detects that butanol content starts to reduce more than 90 DEG C, stops adding extractant and closes extraction, infinite reflux 0.2h, afterwards Start with（2~4）:1 extraction butanol-ethylene glycol changeover portion to V4；When tower top temperature is more than 120 DEG C, stopping heating, tower reactor extracts After agent cooling, it is standby to be discarded to V1.
Example IV
Extractant selects ethylene glycol, dosage 400kg, other conditions such as embodiment three.Obtained butanol produces with hexamethylene Product purity is more than 99%.
Described above is the preferable case of effect in the present invention, but the content is only presently preferred embodiments of the present invention, no The practical range for being defined the present invention can be used for.

Claims (1)

  1. A kind of 1. butanol-hexamethylene azeotropic mixture extraction rectifying method, it is characterised in that：This method be divided into continuity operation or The operation of intermittent operation, wherein continuity includes extractive distillation column (T101) and solvent recovery tower (T102), raw material butanol and ring The mixture of hexane adds in extractive distillation column (T101) middle and lower part, and extractant adds from extractive distillation column (T101) top, ring Hexane is after extractive distillation column (T101) overhead extraction, extractant and butanol mixture are produced by extractive distillation column (T101) bottom of towe In the middle part of into solvent recovery tower (T102), butanol produces Posterior circle from solvent recovery tower (T102) overhead extraction, bottom of towe extractant Utilize；Intermittent operation includes butanol and disposably squeezes into tower bottom of rectifying tower (E1) with cyclohexane mixtures raw material, and extractant passes through Tower top is continuously added to, first overhead extraction for hexamethylene, it is different according to temperature afterwards, produce hexamethylene-butanol mistake successively Cut, butanol, butanol-extractant interim fraction are crossed, tower reactor extraction extractant recycles；
    Continuity or intermittent operation extractant are the mixed extractant of ethylene glycol and ionic liquid composition；
    Mixed extractant intermediate ion liquid be respectively N- picoline dimethyl phosphates salt, N- ethylpyridine dimethyl phosphates salt, N- butyl-pyridinium dimethyl phosphate salt；
    In the mixed extractant that ethylene glycol forms with ionic liquid, ionic liquid mass fraction is 40wt%~50wt%；
    Under continuity mode of operation, important technological parameters are：
    1) extractive distillation column (T101) technical parameter：Tower theoretical cam curve=35~60；Reflux ratio=2:1~4:1, operating pressure =0.3atm；Charge ratio=1.5 of extractant and raw material:1~5:1, feeding temperature=30 DEG C~40 DEG C, pressure=0.11MPa, Raw material is butanol and hexamethylene, feeding temperature=30 DEG C~40 DEG C, pressure=0.11MPa；Extracted feed position is 3~9 pieces of towers Plate, 28~45 blocks of feedstock position column plate, bottom temperature are 125 DEG C~131 DEG C, and tower top temperature is 44 DEG C~49 DEG C；
    2) solvent recovery tower (T102) technical parameter：Theoretical cam curve=30~45；Reflux ratio=1:1~4:1, operating pressure= 0.3atm；Feed entrance point is 23~36 blocks of column plates, and bottom temperature is 161 DEG C~167 DEG C, and tower top temperature is 85 DEG C~90 DEG C；
    Under intermittent operation mode, important technological parameters are：Extractive distillation column theoretical cam curve=38~55；Extractant and raw material Charge ratio be 1.5:1~5:1；Full tower operating pressure is 0.3atm.
CN201610026620.1A 2016-01-17 2016-01-17 A kind of butanol hexamethylene azeotropic mixture extraction rectifying method Expired - Fee Related CN105503501B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610026620.1A CN105503501B (en) 2016-01-17 2016-01-17 A kind of butanol hexamethylene azeotropic mixture extraction rectifying method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610026620.1A CN105503501B (en) 2016-01-17 2016-01-17 A kind of butanol hexamethylene azeotropic mixture extraction rectifying method

Publications (2)

Publication Number Publication Date
CN105503501A CN105503501A (en) 2016-04-20
CN105503501B true CN105503501B (en) 2017-12-12

Family

ID=55711879

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610026620.1A Expired - Fee Related CN105503501B (en) 2016-01-17 2016-01-17 A kind of butanol hexamethylene azeotropic mixture extraction rectifying method

Country Status (1)

Country Link
CN (1) CN105503501B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105906479B (en) * 2016-05-24 2019-01-22 济南大学 A kind of separation method of butanol-butyronitrile mixture
CN106008159B (en) * 2016-05-24 2019-01-22 济南大学 A kind of separation method of isopropanol-propionitrile mixture
CN110052052A (en) * 2019-05-29 2019-07-26 天津赫普菲乐新材料有限公司 Multicomponent batch fractionating intelligence control system and control method
CN114805025A (en) * 2022-05-27 2022-07-29 辽宁石油化工大学 Separation and purification method of cyclohexanol and butyl cyclohexyl ether

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102180791A (en) * 2011-04-13 2011-09-14 天津大学 Method for separating methyl acetate-methanol mixture by ionic liquid intermittent extractive rectification
CN103896713A (en) * 2014-04-17 2014-07-02 河北工业大学 Process for extracting, rectifying and separating cyclohexane-ethanol system by using ionic liquid
CN104774130A (en) * 2015-03-12 2015-07-15 浙江大学 Extraction and rectification method for separating mixture of cyclohexane and isopropanol
CN104774132A (en) * 2015-03-12 2015-07-15 浙江大学 Extraction and rectification method for separating mixture of cyclohexane and n-propanol

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
USD399193S (en) * 1997-07-25 1998-10-06 Sailing Strong International Co., Ltd. Removable hard disk drive holder and cassette

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102180791A (en) * 2011-04-13 2011-09-14 天津大学 Method for separating methyl acetate-methanol mixture by ionic liquid intermittent extractive rectification
CN103896713A (en) * 2014-04-17 2014-07-02 河北工业大学 Process for extracting, rectifying and separating cyclohexane-ethanol system by using ionic liquid
CN104774130A (en) * 2015-03-12 2015-07-15 浙江大学 Extraction and rectification method for separating mixture of cyclohexane and isopropanol
CN104774132A (en) * 2015-03-12 2015-07-15 浙江大学 Extraction and rectification method for separating mixture of cyclohexane and n-propanol

Also Published As

Publication number Publication date
CN105503501A (en) 2016-04-20

Similar Documents

Publication Publication Date Title
CN105693446B (en) A kind of isopropanol triethylamine azeotropic mixture extraction rectifying method
CN105503501B (en) A kind of butanol hexamethylene azeotropic mixture extraction rectifying method
CN113214039B (en) Extractive distillation process for separating ternary complex azeotropic mixture cyclohexane/normal propyl alcohol/water
CN105523889B (en) A kind of tert-butyl alcohol triethylamine azeotropic mixture extraction rectifying method
CN104230657A (en) Novel energy-saving three-tower continuous extractive distillation technology and extractive distillation system thereof
CN107935807A (en) A kind of system and method for recycling refined methyl cyclopentane and application thereof
CN106220532A (en) A kind of separation of extractive distillation acetonitrile and the method for triethylamine
CN103055530A (en) Solvent reinforced transformation thermal coupling rectification system for separating cyclohexanone and phenol
CN105646146B (en) A kind of propyl alcohol triethylamine azeotropic mixture extraction rectifying method
CN112745208B (en) Cyclohexanone recovery and separation process and system
CN113214049A (en) Method for separating isopropanol and isopropyl ether by liquid-liquid extraction-flash evaporation
CN109534998B (en) Energy-saving process for separating ethyl acetate-ethanol by pressure swing distillation with side extraction
CN105001055B (en) Based on mixed solvent as extractant isopropanol acetonitrile azeotropic mixture distillation and separation method
CN105541552B (en) A kind of glycol dimethyl ether azeotropic mixture extraction rectifying method
CN112661593A (en) Method for separating benzene, cyclohexene and cyclohexane by extractive distillation of mixed solvent containing ionic liquid
CN102093176B (en) Method for extracting and separating methylal-methanol mixture by using continuous countercurrent rotating disk
CN105669369B (en) A kind of tert-butyl alcohol-propyl formate azeotropic mixture extraction rectifying method
CN103288584B (en) Reformed arene C 10the processing method of middle extraction high-purity beta-methylnaphthalene
CN105503524B (en) A kind of butanol butyl formate azeotropic mixture extraction rectifying method
CN104829426A (en) Continuous isopropyl ether-isopropyl alcohol azeotrope extraction and rectification technology based on choline chloride/urea low-co-melting solvent
CN115093326A (en) Method for separating ethyl acetate-ethanol-butanone mixture by extraction pressure swing distillation
CN115028523A (en) Pressure-variable-heterogeneous azeotropic rectification separation method for butanone dehydration
CN103772325A (en) Novel method for separating and purifying 1,2-epoxybutane
CN105384594B (en) Method for extracting m-diethylbenzene and p-diethylbenzene from diethylbenzene by three times of successive extractive distillation
CN113185409A (en) Method for extracting and separating n-heptane-dimethyl carbonate by ionic liquid

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20171212

Termination date: 20220117

CF01 Termination of patent right due to non-payment of annual fee