CN208166883U - A kind of system of separating alcohol, ethyl acetate and aqueous mixtures - Google Patents
A kind of system of separating alcohol, ethyl acetate and aqueous mixtures Download PDFInfo
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- CN208166883U CN208166883U CN201820456402.6U CN201820456402U CN208166883U CN 208166883 U CN208166883 U CN 208166883U CN 201820456402 U CN201820456402 U CN 201820456402U CN 208166883 U CN208166883 U CN 208166883U
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Abstract
The system that the utility model discloses a kind of separating alcohol, ethyl acetate and aqueous mixtures, pretreatment unit obtains ethyl alcohol under normal pressure by pretreater, the azeotropic mixtures of at least any two kinds of compositions of ethyl acetate and water are transported to coalescence phase-splitter split-phase as oil mutually and heavy phase, the oil of acquisition is mutually transported to ethyl acetate product unit, and the heavy phase of acquisition is transported to ethyl alcohol recovery unit；The azeotropic mixture that the weight-removing column tower top of de- weight unit acquires at least any two kinds of compositions of ethyl acetate, second alcohol and water continues to return to coalescence phase-splitter split-phase, the oily ethyl acetate product unit that mutually enters obtains ethyl acetate product, and weight-removing column tower reactor obtains heavy phase and is transported to ethyl alcohol recovery unit；The degreasing tower of ethyl alcohol recovery unit utilizes the degreasing tower reboiler of ethanol tower overhead vapours, and degreasing tower reboiler and ethyl alcohol tower reboiler form economic benefits and social benefits coupling.The utility model flexible operation, improves thermodynamic efficiency, and thermal energy can make full use of.
Description
Technical field
The utility model relates to the systems of a kind of separating alcohol, ethyl acetate and aqueous mixtures, belong to chemical materials rectifying
Purification technique field.
Background technique
Ethyl alcohol colorless clear liquid has calcination taste, easily flows, moisture is easily absorbed from air, can be with water and chloroform, second
A variety of organic solvents such as ether are dissolved each other with arbitrary proportion, can form azeotropic mixture (aqueous 4.43%), azeotropic point 78.15 with water
℃.Relative density 0.789,78.5 DEG C of boiling point, is important organic solvent by -114.1 DEG C of fusing point, be widely used in medicine, coating,
The every field such as amenities, cosmetics, grease.
Ethyl acetate is also known as ethyl acetate, and pure ethyl acetate is the colorless and transparent liquid with penetrating odor, tool
There are excellent dissolubility, quick-drying, it is widely used, it is a kind of very important Organic Chemicals and fabulous industrial solvent,
It is widely used in acetate fiber, ethyl cellulose, chlorinated rubber, vinyl, acetate fiber resin, synthetic rubber, coating and oil
In the production process of paint etc..
Currently, the industrial production of domestic ethyl acetate, is mainly condensed into a molecule second using esterification process and two molecules of acetaldehyde
The acetaldehyde condensation method of acetoacetic ester.Esterification process produce ethyl acetate raw material be acetic acid and ethyl alcohol, sulfuric acid, phosphoric acid, solid acid or
Occur esterification in the presence of the catalyst such as highly acidic resin, main component to be separated is ethyl acetate, second in crude product
Alcohol and water.The Chinese patent of Publication No. CN201410210484.2 discloses a kind of differential pressure rectifying separating acetic acid ethyl ester and ethyl alcohol
The method of azeotropic mixture, by carrying out distillation under pressure in treating column for thick ester continuous feed, steaming thing enters back through treating column jacking
Tower reboiler is received, is condensed in recycling tower reboiler, condensate liquid enters phase-splitter split-phase, and ester phase is returned treating column reflux, maintained just
Normal rectifying state, heavy phase enter recycle section, refine tower reactor continuous discharge, obtain ethyl acetate；Waste water continuous feed is being returned
It receives tower to be evaporated under reduced pressure, steams material and enter the condensation of recovery tower overhead condenser, condensate liquid enters recovery tower backflash, flows back
Slot condensate liquid is divided into two strands, one is sent into rectifying state of the recovery tower to maintain recovery tower, one extraction deesterify system is returned
It receives tower reactor and continuously goes out waste water.Although the technique can be realized the separation to ethyl alcohol, ethyl acetate and water, but operating flexibility
Difference cannot achieve the different flexible choice processing modes of the difference or material content according to treating capacity, while vapor consumes
Amount is big, and the dosage and power consumption of cooling water are more, and distillation process heat can not make full use of.
Utility model content
The utility model is in view of the deficienciess of the prior art, provide a kind of separating alcohol, ethyl acetate and aqueous mixtures
System, compared with conventional solution, operability is more flexible, can be according to the difference or material content for the treatment of capacity not
With flexible choice processing mode, vapor consumption is greatly reduced, reduces the dosage and power consumption of cooling water, improves thermodynamics effect
Rate, so that distillation process thermal energy can make full use of.
The technical solution that the utility model solves above-mentioned technical problem is as follows：The utility model provide a kind of separating alcohol,
The system of ethyl acetate and aqueous mixtures, the system comprises pretreatment units, ethyl acetate product unit, ethyl acetate product
Refined unit, de- weight unit, ethyl alcohol recovery unit；
The pretreatment unit includes pretreater, pretreater condenser, pretreater reboiler and coalescence phase-splitter；
The pretreater tower reactor is heated by the pretreater reboiler using a heat source；The pretreater condenser connection
In the pretreater tower top, the coalescence phase-splitter connects the pretreater, and coalescence phase-splitter is used for the pretreatment
The azeotropic mixture split-phase of at least any two kinds of compositions for ethyl alcohol, ethyl acetate and the water that column overhead obtains is oil phase and heavy phase；
The ethyl acetate product unit includes ethyl acetate product tower, ethyl acetate product tower reboiler and knockout tower,
The coalescence phase-splitter of the pretreatment unit is connected in the ethyl acetate product tower tower；The ethyl acetate product tower reboiler
It is connected to the ethyl acetate product tower tower reactor；Ethyl acetate product tower connects the ethyl acetate product essence through the knockout tower
Unit processed；
The ethyl acetate product refined unit includes molecular sieve adsorber and product purification condenser, and the molecular sieve is inhaled
Adnexa and product purification condenser are separately connected the knockout tower of the ethyl acetate product unit；
The de- heavy unit includes weight-removing column, weight-removing column reboiler and weight-removing column condenser；The weight-removing column tower reactor is through institute
State the ethyl acetate product column overhead that weight-removing column reboiler connects the ethyl acetate product unit；Weight-removing column tower top is through described de-
Weight tower condenser is connected to the coalescence phase-splitter of the pretreatment unit；
The ethyl alcohol recovery unit include degreasing tower, degreasing tower reboiler, degreasing tower condenser, ethanol tower and ethanol tower again
Boil device；Heavy phase pipeline after connecting the coalescence phase-splitter split-phase of the pretreatment unit in the degreasing tower tower；The degreasing tower
Reboiler is connected to the degreasing tower tower reactor, and degreasing tower reboiler forms economic benefits and social benefits through the ethanol tower and the ethyl alcohol tower reboiler
Coupling；The degreasing tower condenser is connected to the degreasing column overhead.
The system of a kind of separating alcohol, ethyl acetate and aqueous mixtures as described above, the ethyl acetate product unit
Ethyl acetate product tower reboiler utilize primary steam, take off weight unit weight-removing column reboiler utilize ethyl acetate product tower tower
It pushes up steam and heat source is provided, ethyl acetate product unit forms economic benefits and social benefits with de- weight unit and couples.
The system of a kind of separating alcohol, ethyl acetate and aqueous mixtures as described above, the ethyl acetate product unit
It operates, is interlocked certainly by the pneumatic control valve and tower top pressure transmitter of ethyl acetate product column overhead gaseous phase outlet under elevated pressure
Dynamic to adjust pressure, ethyl acetate product tower tower pressure interior force is 0.2-0.5MPa, and ethyl acetate product column overhead is connected to described poly-
Phase-splitter is tied, ethyl acetate product tower is also used to return to the extraction of tower top after coalescence phase-splitter split-phase obtains oily phase and repeats to convey
To ethyl acetate product unit.
The system of a kind of separating alcohol, ethyl acetate and aqueous mixtures, the ethyl alcohol recovery unit include as described above
Rectifying still, rectifying column, recycling condenser and reflux ratio distributor；The rectifying still connects the coalescence split-phase of the pretreatment unit
Heavy phase pipeline after device split-phase；The rectifying column connects the rectifying still, and the ethyl alcohol that rectifying column is used to steam rectifying still carries out
Purification；The recycling condenser is connected to described the top of the distillation column, and the reflux ratio distributor is connected to described the top of the distillation column.
The utility model relates to separating alcohol, ethyl acetate and aqueous mixtures process, including be successively set on
Pretreatment unit, ethyl acetate product unit, ethyl acetate product refined unit, de- weight unit, ethyl alcohol recovery unit, it is described
Pretreatment unit is steamed ethyl acetate and ethyl alcohol by pretreater, and ethyl alcohol, ethyl acetate and the water under acquisition normal pressure are extremely
The azeotropic mixture of few any two kinds of compositions, the azeotropic mixture of at least any two kinds of compositions of acquisition are transported to coalescence phase-splitter split-phase as oil
Mutually and heavy phase, the oil of acquisition are mutually transported to the ethyl acetate product unit, and it is single that the heavy phase of acquisition is transported to the ethyl alcohol recycling
Member；The oil that the ethyl acetate product unit obtains pretreatment unit communicates gas phase after peracetic acid ethyl ester product tower is handled
Extraction is delivered to after ethyl acetate refined unit obtains anhydrous ethyl acetate, or condensation and directly produces product, ethyl acetate product
Column overhead Produced Liquid is transported to de- weight unit and is carried out dehydrating；The ethyl acetate product refined unit uses molecular sieve, film
The moisture of absorption or rectificating method removal PPM rank；The weight-removing column tower top of the de- heavy unit acquire ethyl acetate, ethyl alcohol and
The azeotropic mixture of at least any two kinds of compositions of water continues to return to coalescence phase-splitter split-phase or ethyl acetate product tower, and then oil mutually enters
Ethyl acetate product unit obtains ethyl acetate product, and weight-removing column tower reactor obtains heavy phase and is transported to ethyl alcohol recovery unit；The second
De- ester of the alcohol recovery unit according to the difference for the treatment of capacity, using continuous coupled operation or intermittently operated, in continuous coupled operation
Tower utilizes the de- ester tower reboiler of ethanol tower overhead vapours, and ethanol tower is equipped with to be boiled again using the ethanol tower that primary steam is heat source
Device, takes off ester tower reboiler and ethyl alcohol tower reboiler forms economic benefits and social benefits coupling；When intermittently operated, raw material is added at one time to rectifying still,
The top of the distillation column successively produces ethyl acetate, the ternary azeotrope of second alcohol and water, interim fraction and alcohol product.
The process of a kind of separating alcohol, ethyl acetate and aqueous mixtures as described above, the ethyl acetate product
The ethyl acetate product tower of unit is equipped with the ethyl acetate product tower reboiler using primary steam, and the weight-removing column of de- weight unit is set
Have and provides the weight-removing column reboiler of heat source, ethyl acetate product unit and de- weight unit using ethyl acetate product column overhead steam
Form economic benefits and social benefits coupling；The ethyl acetate product unit operates under elevated pressure, passes through ethyl acetate product column overhead gaseous phase outlet
Pneumatic control valve and tower top pressure transmitter interlock automatic pressure regulation, be forced into 0.2-0.5MPa, ethyl acetate product tower
Overhead extraction return coalescence phase-splitter split-phase obtains oily mutually repetition and is delivered to ethyl acetate product unit.
Further, the ethyl acetate product unit is coupled with de- weight unit economic benefits and social benefits using fair current coupling rectification technique, institute
It is as follows to state fair current coupling rectification process：
(1) ethyl acetate of the oil phase through ethyl acetate product unit that the coalescence phase-splitter split-phase of preprocessed unit obtains
Charging in the middle part of product tower；
(2) after oil mutually enters ethyl acetate product unit ethyl acetate product, by providing heat source with primary steam
The heating of ethyl acetate product tower reboiler, steam rise to ethyl acetate product column overhead, ethyl acetate product column overhead steam
After de- weight unit weight-removing column reboiler heat exchange cooling, liquid a part of condensation is back to ethyl acetate product tower as reflux
Tower top realizes the mass-and heat-transfer of ethyl acetate product Ta Tanei, another part extraction；
(3) ethyl acetate product column overhead Produced Liquid enters in de- weight unit weight-removing column, by with ethyl acetate product
Column overhead steam is after the weight-removing column reboiler heating of heat source vaporizes, and steam rises to de- weight unit weight-removing column tower top, weight-removing column
For overhead vapours after the condensation of weight-removing column condenser, a part is back to de- weight unit weight-removing column tower top as reflux, realizes de- weight
The mass-and heat-transfer of Ta Tanei, another part extraction are back to ethyl acetate product unit and continue rectifying；
(4) it takes off weight unit weight-removing column tower bottoms and goes to ethyl alcohol recovery unit, recycling obtains 95% ethyl alcohol.
The process of a kind of separating alcohol, ethyl acetate and aqueous mixtures as described above, the ethyl alcohol recovery unit
The pressurization of degreasing tower or normal pressing operation, become by the pneumatic control valve of degreasing column overhead gaseous phase outlet and degreasing column overhead pressure
It send device to interlock automatic pressure regulation, is forced into 0-0.5MPa, ethanol tower uses normal pressure or negative-pressure operation；The de- heavy unit takes off
Weight tower uses normal pressure or negative-pressure operation.
The process of a kind of separating alcohol, ethyl acetate and aqueous mixtures as described above, the pretreatment unit
The obtained heavy phase of coalescence phase-splitter split-phase, and the weight-removing column tower reactor of de- weight unit obtain heavy phase and are delivered to ethyl alcohol recovery unit obtaining
95% ethyl alcohol.
The process of a kind of separating alcohol, ethyl acetate and aqueous mixtures as described above, the ethyl alcohol recovery unit
Using coupling reverse rectification process, the coupling reverse rectification technique is as follows：
(1) richness of the heavy phase that the coalescence phase-splitter split-phase of preprocessed unit obtains and de- weight unit weight-removing column tower reactor extraction
Kettle liquid containing ethyl alcohol, the degreasing tower middle part charging through ethyl alcohol recovery unit；
(2) after heavy phase enters degreasing tower, by adding with the degreasing tower reboiler of ethanol tower overhead vapours offer heat source
Heat, steam rise to degreasing column overhead, and for overhead vapours after condensing, a part is back to degreasing column overhead as reflux, realize
The mass-and heat-transfer of degreasing Ta Tanei, another part extraction；
(3) degreasing column overhead Produced Liquid enters in ethanol tower, by using primary steam as the ethyl alcohol tower reboiler of heat source
After heating vaporization, steam rises to ethyl alcohol column overhead, and after the heat exchange condensation of degreasing tower reboiler, a part is returned as reflux
To ethyl alcohol column overhead, the mass-and heat-transfer in tower is realized, another part extraction is returned；
(4) ethyl alcohol tower bottoms goes to wastewater treatment.
For the utility model compared with conventional solution, operability is more flexible, can according to the difference for the treatment of capacity or
The different flexible choice processing modes of material content, while vapor consumption can also be greatly reduced, reduce the use of cooling water
Amount and power consumption improve thermodynamic efficiency, so that distillation process thermal energy can make full use of.Compared with conventional distillation, this is practical
Novel used technology mode saving energy 50% or so, and anhydrous ethyl acetate, dehydrated alcohol can be obtained, ethyl acetate in water
And ethanol content is positively retained at 300PPM hereinafter, reducing sewage treatment difficulty.
Detailed description of the invention
Fig. 1 be separating alcohol, ethyl acetate and aqueous mixtures technique in pretreatment unit, ethyl acetate product unit,
Ethyl acetate product refined unit and de- weight cell schematics；
Fig. 2 be separating alcohol, in ethyl acetate and aqueous mixtures technique continuous coupled operation the signal of ethyl alcohol recovery unit
Figure；
Fig. 3 be separating alcohol, in ethyl acetate and aqueous mixtures technique intermittently operated ethyl alcohol recovery unit schematic diagram.
Specific embodiment
To keep the above objects, features, and advantages of the utility model more obvious and easy to understand, with reference to the accompanying drawing to this
The specific embodiment of utility model is described in detail.Many details are explained in the following description in order to abundant
Understand the utility model.But the utility model can be implemented with being much different from other way described herein, this field
Technical staff can do similar improvement without prejudice to the utility model connotation, therefore the utility model is not by following public affairs
The limitation for the specific embodiment opened.
Unless otherwise defined, all technical and scientific terms used herein are led with the technology for belonging to the utility model
The normally understood meaning of the technical staff in domain is identical.Terminology used in the description of the utility model herein only be
The purpose of description specific embodiment, it is not intended that in limitation the utility model.Term as used herein "and/or" packet
Include any and all combinations of one or more related listed items.
Referring to figure 1, figure 2 and figure 3, the utility model provides the system of a kind of separating alcohol, ethyl acetate and aqueous mixtures,
The system comprises pretreatment unit, ethyl acetate product unit, ethyl acetate product refined unit, de- weight unit, ethyl alcohol to return
Receive unit；
The pretreatment unit includes pretreater 12, pretreater condenser 13, pretreater reboiler 11 and coalescence
Phase-splitter 14；12 tower reactor of pretreater is heated by the pretreater reboiler 11 using a heat source；The pre- place
Reason tower condenser 13 is connected to 12 tower top of pretreater, and the coalescence phase-splitter 14 connects the pretreater 12, coalescence
At least any two kinds of compositions for ethyl alcohol, ethyl acetate and the water that phase-splitter 14 is used to obtain the tower top of the pretreater 12
Azeotropic mixture split-phase is oil phase and heavy phase；
The ethyl acetate product unit includes ethyl acetate product tower 22, ethyl acetate product tower reboiler 21 and separation
Tower 23 connects the coalescence phase-splitter 14 of the pretreatment unit in 22 tower of ethyl acetate product tower；The ethyl acetate produces
Product tower reboiler 21 is connected to 22 tower reactor of ethyl acetate product tower；Ethyl acetate product tower 22 is connected through the knockout tower 23
The ethyl acetate product refined unit；
The ethyl acetate product refined unit includes molecular sieve adsorber 31 and product purification condenser 32, the molecule
Sieve absorber 31 and product purification condenser 32 are separately connected the knockout tower 23 of the ethyl acetate product unit；
The de- weight unit includes weight-removing column 42, weight-removing column reboiler 41 and weight-removing column condenser 43；The weight-removing column 42
Tower reactor connects 22 tower top of ethyl acetate product tower of the ethyl acetate product unit through the weight-removing column reboiler 41；Weight-removing column
42 tower tops are connected to the coalescence phase-splitter 14 of the pretreatment unit through the weight-removing column condenser 43；
The ethyl alcohol recovery unit includes degreasing tower 52, degreasing tower reboiler 51, degreasing tower condenser 53,55 and of ethanol tower
Ethyl alcohol tower reboiler 54；Heavy phase pipe after connecting coalescence 14 split-phase of phase-splitter of the pretreatment unit in 52 tower of degreasing tower
Line；The degreasing tower reboiler 51 is connected to 52 tower reactor of degreasing tower, and degreasing tower reboiler 51 is through the ethanol tower 55 and institute
It states ethyl alcohol tower reboiler 54 and forms economic benefits and social benefits coupling；The degreasing tower condenser 53 is connected to 52 tower top of degreasing tower；
In one embodiment of the system of separating alcohol, ethyl acetate and aqueous mixtures, the ethyl acetate product unit
Ethyl acetate product tower reboiler 21 utilize primary steam, take off weight unit weight-removing column reboiler 41 utilize ethyl acetate product
22 overhead vapours of tower provides heat source, and ethyl acetate product unit forms economic benefits and social benefits with de- weight unit and couples.
In one embodiment of the system of separating alcohol, ethyl acetate and aqueous mixtures, the ethyl acetate product unit
It operates under elevated pressure, the pneumatic control valve and tower top pressure transmitter exported by 22 top gaseous phase of ethyl acetate product tower interlocks
Automatic pressure regulation, 22 tower pressure interior force of ethyl acetate product tower are 0.2-0.5MPa, and 22 tower top of ethyl acetate product tower is connected to
The coalescence phase-splitter 14, ethyl acetate product tower 22, which is also used to returning to the extraction of tower top into coalescence 14 split-phase of phase-splitter, obtains oil
It repeats to be delivered to ethyl acetate product unit after phase.
In one embodiment of the system of separating alcohol, ethyl acetate and aqueous mixtures, the ethyl alcohol recovery unit includes
Rectifying still 61, rectifying column 62, recycling condenser 63 and reflux ratio distributor 64；The rectifying still 61 connects the pretreatment unit
Coalescence 14 split-phase of phase-splitter after heavy phase pipeline；The rectifying column 62 connects the rectifying still 61, and rectifying column 62 is used for essence
The ethyl alcohol that kettle 61 steams is evaporated to be purified；The recycling condenser 63 is connected to 62 tower top of rectifying column, the reflux score
Orchestration 64 is connected to 62 tower top of rectifying column.
The utility model relates to separating alcohol, ethyl acetate and aqueous mixtures process, including be successively set on
Pretreatment unit, ethyl acetate product unit, ethyl acetate product refined unit, de- weight unit, ethyl alcohol recovery unit, it is described
At least any two kinds azeotropic formed that pretreatment unit passes through ethyl alcohol, ethyl acetate and water under the acquisition normal pressure of pretreater 12
Object, the azeotropic mixture of at least any two kinds of compositions of acquisition are transported to coalescence 14 split-phase of phase-splitter as oil phase and heavy phase, the oil of acquisition
It is mutually transported to the ethyl acetate product unit, the heavy phase of acquisition is transported to the ethyl alcohol recovery unit；The ethyl acetate produces
The oil that article unit obtains pretreatment unit communicates gas phase extraction after peracetic acid ethyl ester product tower 22 is handled and is delivered to acetic acid
Ethyl ester refined unit directly produces product, 22 overhead extraction liquid of ethyl acetate product tower after obtaining anhydrous ethyl acetate, or condensation
De- weight unit is transported to be carried out dehydrating；The ethyl acetate product refined unit is using molecular sieve, film absorption or rectifying side
The moisture of method removal PPM rank；It is at least any that 42 tower top of weight-removing column of the de- weight unit acquires ethyl acetate, second alcohol and water
The azeotropic mixture of two kinds of compositions continues to return to coalescence 14 split-phase of phase-splitter, and then the oily ethyl acetate product unit that mutually enters obtains acetic acid
Ethyl ester product, 42 tower reactor of weight-removing column obtain heavy phase and are transported to ethyl alcohol recovery unit；The ethyl alcohol recovery unit is according to treating capacity
Difference, using continuous coupled operation or intermittently operated, the de- ester tower 52 in continuous coupled operation is steamed using 55 tower top of ethanol tower
The de- ester tower reboiler 51 of vapour, ethanol tower 55 are equipped with the ethyl alcohol tower reboiler 54 using primary steam for heat source, and de- ester tower boils again
Device 51 and ethyl alcohol tower reboiler 54 form economic benefits and social benefits coupling；When intermittently operated, raw material is added at one time to rectifying still 61, rectifying column 62
Tower top successively produces ethyl acetate, the ternary azeotrope of second alcohol and water, interim fraction and alcohol product.
In one embodiment of the process of separating alcohol, ethyl acetate and aqueous mixtures, the ethyl acetate product
The ethyl acetate product tower 22 of unit is equipped with the ethyl acetate product tower reboiler 21 using primary steam, takes off the de- weight of weight unit
Tower 42, which is equipped with, provides the weight-removing column reboiler 41 of heat source, ethyl acetate product unit using 22 overhead vapours of ethyl acetate product tower
Economic benefits and social benefits are formed with de- heavy unit to couple；The ethyl acetate product unit operates under elevated pressure, passes through ethyl acetate product tower 22
The pneumatic control valve and tower top pressure transmitter of top gaseous phase outlet interlock automatic pressure regulation, are forced into 0.2-0.5MPa, second
22 overhead extraction of acetoacetic ester product tower return coalescence 14 split-phase of phase-splitter obtains oily mutually repetition and is delivered to ethyl acetate product unit.
The ethyl acetate product unit is coupled with de- weight unit economic benefits and social benefits using fair current coupling rectification technique, the fair current coupling
It is as follows to close rectification technique：
(1) acetic acid second of the oil phase through ethyl acetate product unit that coalescence 14 split-phase of phase-splitter of preprocessed unit obtains
It is fed in the middle part of ester product tower 22；
(2) after oil mutually enters ethyl acetate product unit ethyl acetate product, by providing heat source with primary steam
Ethyl acetate product tower reboiler 21 heats, and steam rises to 22 tower top of ethyl acetate product tower, 22 tower of ethyl acetate product tower
Steam is pushed up after the de- heat exchange of weight unit weight-removing column reboiler 41 cooling, liquid a part of condensation is back to acetic acid second as reflux
22 tower top of ester product tower realizes the mass-and heat-transfer in 22 tower of ethyl acetate product tower, another part extraction；
(3) 22 overhead extraction liquid of ethyl acetate product tower enters in de- weight unit weight-removing column 42, by with ethyl acetate
22 overhead vapours of product tower is after the heating of weight-removing column reboiler 41 of heat source vaporizes, and steam rises to de- 42 tower of weight unit weight-removing column
Top, for 42 overhead vapours of weight-removing column after the condensation of weight-removing column condenser 43, a part is back to de- weight unit weight-removing column as reflux
42 tower tops, realize the mass-and heat-transfer in 42 tower of weight-removing column, and another part extraction is back to ethyl acetate product unit and continues rectifying；
(4) it takes off 42 tower bottoms of weight unit weight-removing column and goes to ethyl alcohol recovery unit, recycling obtains 95% ethyl alcohol.
In one embodiment of the process of separating alcohol, ethyl acetate and aqueous mixtures, the ethyl alcohol recovery unit
Degreasing tower 52 pressurization or normal pressing operation, pass through 52 top gaseous phase of degreasing tower export pneumatic control valve and 52 tower top of degreasing tower
Pressure transmitter interlocks automatic pressure regulation, is forced into 0-0.5MPa, and ethanol tower 55 uses normal pressure or negative-pressure operation；The de- weight
The weight-removing column 42 of unit uses normal pressure or negative-pressure operation.
In one embodiment of the process of separating alcohol, ethyl acetate and aqueous mixtures, the pretreatment unit
42 tower reactor of weight-removing column of heavy phase and de- weight unit that coalescence 14 split-phase of phase-splitter obtains obtains heavy phase and is delivered to ethyl alcohol recovery unit
Obtain 95% ethyl alcohol.
In one embodiment of the process of separating alcohol, ethyl acetate and aqueous mixtures, the ethyl alcohol recovery unit
Using coupling reverse rectification process, the coupling reverse rectification technique is as follows：
(1) heavy phase and the extraction of de- 42 tower reactor of weight unit weight-removing column that coalescence 14 split-phase of phase-splitter of preprocessed unit obtains
The kettle liquid rich in ethyl alcohol, feed in the middle part of the degreasing tower 52 through ethyl alcohol recovery unit；
(2) after heavy phase enters degreasing tower 52, by providing the degreasing tower reboiler of heat source with 55 overhead vapours of ethanol tower
51 heating, steam rise to 52 tower top of degreasing tower, and for overhead vapours after condensing, a part is back to degreasing tower 52 as reflux
Tower top realizes the mass-and heat-transfer in 52 tower of degreasing tower, another part extraction；
(3) 52 overhead extraction liquid of degreasing tower enters in ethanol tower 55, by using primary steam as the ethanol tower of heat source again
After boiling the heating vaporization of device 54, steam rises to 55 tower top of ethanol tower, and after the heat exchange condensation of degreasing tower reboiler 51, a part is made
It is back to 55 tower top of ethanol tower for reflux, realizes the mass-and heat-transfer in tower, another part extraction is returned；
(4) 55 kettle liquid of ethanol tower goes to wastewater treatment.
Using the process and system of the utility model separating alcohol, ethyl acetate and aqueous mixtures, 10t/h is fed,
Feed composition：Ethyl acetate 70%, ethyl alcohol 12.35%, water 16.65%, reboiling 1% are fed in the middle part of pretreater 12, pre-
It handles under the heating of tower reboiler 11, atmospheric operation controls 70-71 DEG C of 12 tower top temperature of pretreater, bottom temperature 101-103
DEG C, reflux ratio 0.5-2,12 tower reactor of pretreater extraction 1t/h waste water goes to waste water treatment plant, 12 overhead extraction 9t/h of pretreater,
Then coalescence 14 split-phase of phase-splitter is gone, upper oil phase (ethyl acetate 86.5%, ethyl alcohol 8%, water 5.5%) and lower layer's heavy phase are obtained
(ethyl acetate 9.56%, ethyl alcohol 14.95%, water 75.5%), oil mutually enter ethyl acetate product tower 22, pass through tower top regulating valve
With tower top pressure interlocking automatic control, tower pressure interior force 0.4MPa is adjusted, 122-123 DEG C of tower top temperature, bottom temperature is 130-140 DEG C,
Reflux ratio 0.5-2,
22 tower reactor of ethyl acetate product tower produces vapor phase acetic acid ethyl ester (aqueous≤200PPM) with the flow of 6.75t/h, so
After go ethyl acetate product refined unit to be dehydrated through molecular sieve or film, obtain anhydrous ethyl acetate product；Ethyl acetate product tower
The mixture of 22 overhead extractions is fed in the middle part of weight-removing column 42,42 atmospheric operation of weight-removing column, 70 DEG C of 42 tower top temperature of weight-removing column, tower
82 DEG C of kettle, reflux ratio 0.5-2, at least any two kinds azeotropic mixtures returns formed of ethyl acetate, ethyl alcohol, water that tower top obtains
14 split-phase of phase-splitter is coalesced, the heavy phase that the water and ethyl alcohol and coalescence 14 split-phase of phase-splitter that tower reactor obtains obtain goes ethyl alcohol recycling single
Member recycles ethyl alcohol.
Coalescence 14 lower layer's heavy phase of phase-splitter and 42 tower reactor of weight-removing column obtain heavy phase mixture about 2.2t/h, recycle from ethyl alcohol single
It feeds, is heated by degreasing tower reboiler 51,72 DEG C of tower top temperature, 82 DEG C of bottom temperature, reflux ratio 1- in the middle part of first degreasing tower 52
8, overhead extraction 350Kg/h, ethanol tower 55 adjust tower pressure interior force by tower top regulating valve and tower top pressure interlocking automatic control
0.1MPa, 97 DEG C of tower top temperature, 121 DEG C of bottom temperature, reflux ratio 0.5-2, overhead extraction amount 1200Kg/h.
In another implementation process, using the technique side of the utility model separating alcohol, ethyl acetate and aqueous mixtures
Method and system feed 5t/h, feed composition：Ethyl acetate 50%, ethyl alcohol 10.82%, water 39.18%, reboiling 1%.From pre-
It is fed in the middle part of reason tower 12, under the heating of pretreater reboiler 11, atmospheric operation controls 70-71 DEG C of tower top temperature, bottom temperature
101-103 DEG C, reflux ratio 0.5-2,12 tower reactor of pretreater extraction 1.68t/h waste water removes waste water treatment plant, 12 tower of pretreater
Top extraction 3.32t/h, then goes coalescence 14 split-phase of phase-splitter, obtains upper oil phase (ethyl acetate 86.5%, ethyl alcohol 8%, water
5.5%) and lower layer's heavy phase (ethyl acetate 9.56%, ethyl alcohol 14.95%, water 5.5%), oil mutually enter ethyl acetate product tower
22, by tower top regulating valve and tower top pressure interlocking automatic control, adjust tower pressure interior force 0.4MPa, 120-125 DEG C of tower top temperature, tower reactor
Temperature is 130-140 DEG C, reflux ratio 0.5-2, and 22 tower reactor of ethyl acetate product tower produces vapor phase acetic acid second with the flow of 4.85t/h
Ester (aqueous≤200PPM) then goes ethyl acetate product refined unit to be dehydrated through molecular sieve or film, obtains anhydrous ethyl acetate
Product；The mixture of 22 overhead extraction of ethyl acetate product tower returns to coalescence 14 split-phase of phase-splitter, and oil mutually continues into ethyl acetate
Product unit separation.
Coalescence 14 lower layer's heavy phase of phase-splitter and 42 tower reactor of weight-removing column obtain heavy phase mixture and are once quantitatively adding rectifying still 61,
It being heated using external steam, 62 tower top of rectifying column successively produces the mixture (70-71 DEG C) of ethyl acetate, second alcohol and water, and 95%
Ethyl alcohol (78 DEG C), interim fraction are produced to interim fraction tank, are returned to rectifying still 61 with lower batch materials and are continued rectifying, when rectifying still 61
In be free of ethyl acetate and ethyl alcohol when, waste water from 61 bottom of rectifying still be discharged.
For the utility model compared with conventional solution, operability is more flexible, can according to the difference for the treatment of capacity or
The different flexible choice processing modes of material content, while vapor consumption can also be greatly reduced, reduce the use of cooling water
Amount and power consumption improve thermodynamic efficiency, so that distillation process thermal energy can make full use of.Compared with conventional distillation, this is practical
Novel used technology mode saving energy 50% or so, and anhydrous ethyl acetate, dehydrated alcohol can be obtained, ethyl acetate in water
And ethanol content can keep 300PPM hereinafter, reducing sewage treatment difficulty.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
Above-described embodiments merely represent several embodiments of the utility model, the description thereof is more specific and detailed,
But it cannot be understood as the limitations to utility model patent range.It should be pointed out that for the common skill of this field
For art personnel, without departing from the concept of the premise utility, various modifications and improvements can be made, these are belonged to
The protection scope of the utility model.Therefore, the scope of protection shall be subject to the appended claims for the utility model patent.
Claims (4)
1. the system of a kind of separating alcohol, ethyl acetate and aqueous mixtures, it is characterised in that：It is single that the system comprises pretreatments
Member, ethyl acetate product unit, ethyl acetate product refined unit, de- weight unit, ethyl alcohol recovery unit；
The pretreatment unit includes pretreater, pretreater condenser, pretreater reboiler and coalescence phase-splitter；It is described
Pretreater tower reactor is heated by the pretreater reboiler using a heat source；The pretreater condenser is connected to institute
Pretreater tower top is stated, the coalescence phase-splitter connects the pretreater, and coalescence phase-splitter is used for the pretreater tower
The azeotropic mixture split-phases of at least any two kinds of compositions for ethyl alcohol, ethyl acetate and the water that top obtains are oil phase and heavy phase；
The ethyl acetate product unit includes ethyl acetate product tower, ethyl acetate product tower reboiler and knockout tower, described
The coalescence phase-splitter of the pretreatment unit is connected in ethyl acetate product tower tower；The ethyl acetate product tower reboiler connection
In the ethyl acetate product tower tower reactor；Ethyl acetate product tower connects the ethyl acetate product through the knockout tower and refines list
Member；
The ethyl acetate product refined unit includes molecular sieve adsorber and product purification condenser, the molecular sieve adsorber
The knockout tower of the ethyl acetate product unit is separately connected with product purification condenser；
The de- heavy unit includes weight-removing column, weight-removing column reboiler and weight-removing column condenser；The weight-removing column tower reactor is through described de-
Weight tower reboiler connects the ethyl acetate product column overhead of the ethyl acetate product unit；Weight-removing column tower top is through the weight-removing column
Condenser is connected to the coalescence phase-splitter of the pretreatment unit；
The ethyl alcohol recovery unit includes that degreasing tower, degreasing tower reboiler, degreasing tower condenser, ethanol tower and ethanol tower boil again
Device；Heavy phase pipeline after connecting the coalescence phase-splitter split-phase of the pretreatment unit in the degreasing tower tower；The degreasing tower is again
Boiling device is connected to the degreasing tower tower reactor, and degreasing tower reboiler forms economic benefits and social benefits coupling through the ethanol tower and the ethyl alcohol tower reboiler
It closes；The degreasing tower condenser is connected to the degreasing column overhead.
2. the system of a kind of separating alcohol according to claim 1, ethyl acetate and aqueous mixtures, it is characterised in that：Institute
The ethyl acetate product tower reboiler of ethyl acetate product unit is stated using primary steam, takes off the weight-removing column reboiler benefit of weight unit
Heat source is provided with ethyl acetate product column overhead steam, ethyl acetate product unit forms economic benefits and social benefits with de- weight unit and couples.
3. the system of a kind of separating alcohol according to claim 1, ethyl acetate and aqueous mixtures, it is characterised in that：Institute
It states ethyl acetate product unit to operate under elevated pressure, passes through the pneumatic control valve and tower of ethyl acetate product column overhead gaseous phase outlet
It presses power transmitter and interlocks automatic pressure regulation, ethyl acetate product tower tower pressure interior force is 0.2-0.5MPa, ethyl acetate product
Column overhead is connected to the coalescence phase-splitter, and ethyl acetate product tower is also used to returning to the extraction of tower top into coalescence phase-splitter split-phase
It repeats to be delivered to ethyl acetate product unit after obtaining oily phase.
4. the system of a kind of separating alcohol according to claim 1, ethyl acetate and aqueous mixtures, it is characterised in that：Institute
Stating ethyl alcohol recovery unit includes rectifying still, rectifying column, recycling condenser and reflux ratio distributor；The rectifying still connection is described pre-
Heavy phase pipeline after the coalescence phase-splitter split-phase of processing unit；The rectifying column connects the rectifying still, and rectifying column is used for essence
The ethyl alcohol that kettle steams is evaporated to be purified；The recycling condenser is connected to described the top of the distillation column, and the reflux ratio distributor connects
It connects in described the top of the distillation column.
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| CN201820456402.6U CN208166883U (en) | 2018-04-03 | 2018-04-03 | A kind of system of separating alcohol, ethyl acetate and aqueous mixtures |
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| CN201820456402.6U CN208166883U (en) | 2018-04-03 | 2018-04-03 | A kind of system of separating alcohol, ethyl acetate and aqueous mixtures |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112358397A (en) * | 2020-11-24 | 2021-02-12 | 浙江台州市联创环保科技股份有限公司 | Equipment and method for rectifying and separating ethyl acetate and ethanol azeotrope |
| CN114100176A (en) * | 2021-12-09 | 2022-03-01 | 江苏恒兴新材料科技股份有限公司 | Compound ethyl butyrate purification tower, separation and refining system and separation process thereof |
-
2018
- 2018-04-03 CN CN201820456402.6U patent/CN208166883U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112358397A (en) * | 2020-11-24 | 2021-02-12 | 浙江台州市联创环保科技股份有限公司 | Equipment and method for rectifying and separating ethyl acetate and ethanol azeotrope |
| CN112358397B (en) * | 2020-11-24 | 2024-01-16 | 浙江台州市联创环保科技股份有限公司 | Equipment and method for rectifying and separating ethyl acetate and ethanol azeotrope |
| CN114100176A (en) * | 2021-12-09 | 2022-03-01 | 江苏恒兴新材料科技股份有限公司 | Compound ethyl butyrate purification tower, separation and refining system and separation process thereof |
| CN114100176B (en) * | 2021-12-09 | 2022-12-09 | 江苏恒兴新材料科技股份有限公司 | Compound ethyl butyrate purification tower, separation and refining system and separation process thereof |
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