CN105503524B - A kind of butanol butyl formate azeotropic mixture extraction rectifying method - Google Patents
A kind of butanol butyl formate azeotropic mixture extraction rectifying method Download PDFInfo
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- CN105503524B CN105503524B CN201610026619.9A CN201610026619A CN105503524B CN 105503524 B CN105503524 B CN 105503524B CN 201610026619 A CN201610026619 A CN 201610026619A CN 105503524 B CN105503524 B CN 105503524B
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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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by 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
- 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
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Abstract
A kind of butanol butyl formate 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 butyl formate azeotropic mixture extraction rectifying method, by selecting a variety of extractants, the butanol and butyl formate 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 butyl formate azeotropic system, current technology blank has been filled up.
Description
Technical field
Separation method provided by the present invention is directed to butanol-butyl formate azeotropic system, and ethylene glycol, second is respectively adopted
The mixed solvent of glycol and ionic liquid composition belongs to the extracting rectifying side of butanol-butyl formate azeotropic system as extractant
Method.
Background technology
The raw material being related in the present invention is butanol and butyl formate, both material common in chemical industry.Fourth
Alcohol(C4H10O), also known as tyrosol, the third carbinol, it is the solvent of multiple coating and plasticizer phthalic acid dibutyl ester processed(See adjacent benzene two
Formic acid esters)Raw material, be also used for manufacturing butyl acrylate, butyl acetate, butyl glycol ether and as organic synthesis intermediate
With the extractant of biochemical medicine, it is additionally operable to manufacture surfactant.Butyl formate(C5H10O2), as lacquer solvent, manufacture
Solvent during film, it is additionally operable to artificial leather, spices manufacture, organic synthesis, chemical reagent etc..
Butanol not only has important application with butyl formate in petrochemical industry, and also has inside other industry
It is quite extensive to use.But but there is azeotropism in two kinds of materials so that the difficulty for separating both greatly increases.For having
The recovery of solvent, it is industrial it is widely used be distillation or rectifying processing mode, but for azeotropic system, the country is adopted
With it is more be azeotropic distillation method.But azeotropic distillation has the limitation of its own:In terms of energy consumption, cost is compared with other method
It is higher, 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-butyl formate azeotropic system, not correlation.
The content of the invention
It is insufficient present in existing process the invention aims to overcome, and it is directed to butanol-butyl formate azeotropic body
System, propose 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-butyl formate has azeotropism(It can be seen that butanol-butyl formate in accompanying drawing 1
Azeotropic point be present).
In order to solve the above technical problems, the technical solution adopted by the present invention is:A kind of butanol-butyl formate azeotropic mixture
Extraction rectifying method, 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-butyl formate azeotropic mixture extraction rectifying method continuity operating procedure is such as
Under:
1)Butanol is continuously added to butyl formate mixture by T101 middle and lower parts by feed system, and extractant is from tower top
Add, feeding temperature is all normal temperature, and T101 operating pressures are 0.3atm(Absolute pressure);
2)T101 tower tops can obtain the butyl formate 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 butyl formate, T102 operating pressures are 0.1atm(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-butyl formate azeotropic mixture extraction rectifying method continuity operation, the continuity
Operating important technological parameters is:
1)T101 technical parameters:Theoretical cam curve=35 ~ 55;Reflux ratio=3.5:1~5:1, 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%);Charge ratio=0.8 ~ 1.8 of extractant and raw material:1, feeding temperature=30 DEG C ~ 40 DEG C, pressure=0.11MPa, raw material is
Butanol(17.9wt%)With butyl formate(82.1wt%)Nearly azeotropic composition, feeding temperature=30 DEG C ~ 40 DEG C, pressure=0.11MPa;
Bottom temperature=118 DEG C ~ 120 DEG C, tower top temperature=68 DEG C ~ 71 DEG C.Extracted feed position is 3 ~ 9 blocks of column plates, feedstock position
28 ~ 45 blocks of column plates;
2)T102 technical parameters:Theoretical cam curve=40 ~ 60;Reflux ratio=0.5:1~1.5:1, operating pressure=0.1atm;Tower
Kettle temperature degree=130 DEG C ~ 139 DEG C, tower top temperature=62 DEG C ~ 68 DEG C, feed entrance point are 23 ~ 36 blocks of column plates.
A kind of butanol of the present invention-butyl formate azeotropic mixture extraction rectifying method intermittent operation step is such as
Under:
1)Butanol disposably squeezes into tower bottom of rectifying tower E1 with butyl formate mixture 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 60 DEG C, detection, tower top butyl formate content is more than 99%, with reflux ratio(3~5):1 extraction
Butyl formate product is to V3(With the rise of tower top temperature, reflux ratio is accordingly improved to 5:1);
4)When tower top temperature is more than 70 DEG C, and detect that butyl formate content starts to reduce, close extraction, carry out infinite reflux
0.5h is operated, is started afterwards with reflux ratio(2~5):1 extraction butyl formate-butanol changeover portion to V2(With the liter of tower top temperature
Height, reflux ratio are accordingly improved to 5:1);
5)When tower top temperature reaches 82 DEG C, detection, tower top butanol content is more than 99%, with reflux ratio(2~4):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(0.5~1.3):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-butyl formate azeotropic mixture extraction rectifying method intermittent operation step, the operation
The main important technological parameters of step are
1)Extractive distillation column theoretical cam curve=35 ~ 65;Operating pressure is 0.3atm;
2)The charge ratio of extractant and raw material=(1.5 ~ 4):1.
Beneficial effects of the present invention:The present invention can make butanol-butyl formate 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 butyl formate 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-butyl formate.
Fig. 2 is that butanol-butyl formate 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 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 80kg/h;Feed throughput is 100kg/h, and raw material composition is butanol
(18wt%)With butyl formate(82wt%).The T101 numbers of plates are 55, and extractant feed position is in the 5th block of column plate, feedstock position
Put in 45 blocks of column plates.Reflux ratio is set as 4:1, overhead extraction speed is 82kg/h, and obtained butyl formate purity is 99.7%.
The T102 numbers of plates are 50, and 5. feed entrance point is the 7th block of column plate to stream stock, reflux ratio 0.5:1, overhead extraction speed is 18kg/h,
Obtained butanol purity is 99.6%.Bottom of towe extractant flows back, the supplement as solvent.
Embodiment two
Extractant selects ethylene glycol, dosage 180kg/hr, T101 reflux ratio is set into 5:1, T102 reflux ratio is set
For 1.5:1, other conditions such as embodiment one.Obtained butanol is with butyl formate 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 300kg;Feed throughput is 100kg/h, and raw material composition is butanol
(18wt%)With butyl formate(82wt%);Extracting rectifying column plate number is 55, and extractant feed position is in the 5th block of column plate;Butanol with
Butyl formate mixture disposably squeezes into tower bottom of rectifying tower E1 by raw material pump P2, opens heating;It is complete to return when condensate liquid occurs in tower top
Stream operation, and extractant is continuously added in tower by pump P1, and continue total reflux operation;When tower top temperature reaches 60 DEG C, inspection
Survey, tower top butyl formate content is more than 99%, with reflux ratio(3~5):1 produces butyl formate product to V3(With tower top temperature
Rise, reflux ratio are accordingly improved to 5:1);When tower top temperature is more than 70 DEG C, and detect that butyl formate content starts to reduce, close
Extraction is closed, total reflux operation 0.5h is carried out, starts afterwards with reflux ratio(2~5):1 extraction butyl formate-butanol changeover portion to V2
(With the rise of tower top temperature, reflux ratio is accordingly improved to 5:1);When tower top temperature reaches 82 DEG C, detection, tower top butanol content
More than 99%, with reflux ratio(2~4):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 is more than 90 DEG C, and detect that butanol content starts to reduce, stop adding extractant and simultaneously close extraction, complete time
Flow 0.2h, start afterwards with(0.5~1.3):1 extraction butanol-ethylene glycol changeover portion to V4;When tower top temperature is more than 120 DEG C, stop
Only heat, after the cooling of tower reactor extractant, it is standby to be discarded to V1.
Example IV
Extractant selects ethylene glycol, and dosage 200kg, other conditions such as embodiment three, obtained butanol is with butyl formate
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)
- A kind of 1. butanol-butyl formate azeotropic mixture extraction rectifying method, it is characterised in that:This method is divided into continuity operation Or intermittent operation, wherein continuity operation include extractive distillation column (T101) and solvent recovery tower (T102), raw material butanol and The mixture of butyl formate adds in extractive distillation column (T101) middle and lower part, and extractant adds from extractive distillation column (T101) top Enter, butyl formate is in extractive distillation column (T101) overhead extraction, and extractant is with butanol mixture by extractive distillation column (T101) tower Enter after the extraction of bottom in the middle part of solvent recovery tower (T102), butanol is adopted from solvent recovery tower (T102) overhead extraction, bottom of towe extractant Go out Posterior circle utilization;Intermittent operation includes butanol and disposably squeezes into tower bottom of rectifying tower (E1) with butyl formate mixture material, Extractant is continuously added to by tower top, first overhead extraction for butyl formate, it is different according to temperature afterwards, produce first successively Acid butyl ester-butanol interim fraction, butanol, butanol-extractant interim fraction, tower reactor extraction extractant recycle;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:Theoretical cam curve=35~55;Reflux ratio=3.5:1~5:1, operating pressure =0.3atm;Charge ratio=0.8~1.8 of extractant and raw material:1, feeding temperature=30 DEG C~40 DEG C, pressure=0.11MPa, Raw material is butanol and butyl formate, feeding temperature=30 DEG C~40 DEG C, pressure=0.11MPa;Extracted feed position is 3~9 pieces Column plate, 28~45 blocks of feedstock position column plate, bottom temperature are 118 DEG C~120 DEG C, and tower top temperature is 68 DEG C~71 DEG C;2) solvent recovery tower (T102) technical parameter:Theoretical cam curve=40~60;Reflux ratio=0.5:1~1.5:1, operation pressure Power=0.1atm, feed entrance point are 23~36 blocks of column plates, and bottom temperature is 130 DEG C~139 DEG C, and tower top temperature is 62 DEG C~68 ℃;Under intermittent operation mode, important technological parameters are:Extractive distillation column theoretical cam curve=35~65;The charge ratio of extractant and raw material is 1.5:1~4:1;Full tower operation pressure Power is 0.3atm.
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Citations (3)
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 |
CN103159586A (en) * | 2013-03-26 | 2013-06-19 | 沈阳化工大学 | Continuous extractive distillation separation method of dimethyl carbonate-methanol azeotropic mixture |
CN103467286A (en) * | 2013-08-20 | 2013-12-25 | 天津科林泰克科技有限公司 | Method for separating ethyl acetate-ethyl alcohol compound |
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Patent Citations (3)
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 |
CN103159586A (en) * | 2013-03-26 | 2013-06-19 | 沈阳化工大学 | Continuous extractive distillation separation method of dimethyl carbonate-methanol azeotropic mixture |
CN103467286A (en) * | 2013-08-20 | 2013-12-25 | 天津科林泰克科技有限公司 | Method for separating ethyl acetate-ethyl alcohol compound |
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