CN206858474U - A kind of ethyl acetate dehydration device - Google Patents
A kind of ethyl acetate dehydration device Download PDFInfo
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- CN206858474U CN206858474U CN201720515040.9U CN201720515040U CN206858474U CN 206858474 U CN206858474 U CN 206858474U CN 201720515040 U CN201720515040 U CN 201720515040U CN 206858474 U CN206858474 U CN 206858474U
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- ethyl acetate
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Abstract
The utility model provides a kind of ethyl acetate dehydration device, including the ethyl acetate rectifying and dewatering unit and ethyl acetate film dewatering unit being interconnected with pipeline；The ethyl acetate rectifying and dewatering unit includes ethyl acetate dehydrating tower, reboiler and penetrating fluid preheater；The tower top of the ethyl acetate dehydrating tower and bottom are respectively equipped with material inlet and penetrating fluid charging aperture；Penetrating fluid charging aperture connects with the hot side discharging opening of penetrating fluid preheater, and the air inlet of ethyl acetate dehydrating tower lower end connects with the gaseous phase outlet of reboiler, and the liquid-phase outlet of reboiler connects with the charging aperture of penetrating fluid preheater hot side；The delivery port of ethyl acetate dehydration tower bottom connects with the fluid inlet of technique waste water receiving unit and reboiler.A kind of ethyl acetate dehydration device described in the utility model, flow is simple, and energy consumption is low, can reduce production cost.
Description
Technical field
The utility model belongs to chemical products separation and purification field, more particularly, to a kind of ethyl acetate dehydration device.
Background technology
Ethyl acetate is a kind of important industrial chemicals, and boiling point is 77.1 DEG C, can be big with alcohol, ether, chloroform, acetone, benzene etc.
Most immiscible organic solvents, there is excellent solvability, toxicity is smaller, and volatilization is very fast, is the aliphatic acid being most widely used
One of ester, it is industrial important solvent.The product purity of ethyl acetate, particularly water content are generally proposed in commercial Application
Higher requirement, therefore, the refining process technology of water content≤0.5wt% ethyl acetate product are taken seriously.Due to normal pressure
Lower ethyl acetate and water form azeotropic mixture, and its azeotropic mixture boiling point is 70.4 DEG C, and water content is 6.1wt% during azeotropic, common
The product that ethyl acetate water content is less than azeotropic composition is hardly resulted under the conditions of distillation operation, and uses liquid-liquid extraction, azeotropic to steam
Evaporate, saline extraction and azeotropic water removed the methods of extracting rectifying, the problems such as high energy consumption, complex process be present.Ethyl acetate-water body
The technology that efficiently separates of system is that ethyl acetate is used as product or the wide variety of basis of solvent, development technology flow is succinct, it is efficient,
Green and the ethyl acetate separating and dehydrating technique of low-carbon are to production of ethyl and efficiently using significant.
The content of the invention
In view of this, the utility model is directed to a kind of ethyl acetate dehydration device, the defects of to overcome prior art,
Flow is simple, and energy consumption is low, and production cost and equipment investment can decline.
To reach above-mentioned purpose, what the technical solution of the utility model was realized in：
A kind of ethyl acetate dehydration device, including the ethyl acetate rectifying and dewatering unit and acetic acid second being interconnected with pipeline
Ester film dewatering unit, valve is equipped with each pipeline；
The ethyl acetate rectifying and dewatering unit includes ethyl acetate dehydrating tower, reboiler and penetrating fluid preheater；It is described
The top and bottom of ethyl acetate dehydrating tower are respectively equipped with material inlet and penetrating fluid charging aperture；Penetrating fluid charging aperture and infiltration
The hot side discharging opening connection of liquid preheater, the air inlet of ethyl acetate dehydrating tower lower end connect with the gaseous phase outlet of reboiler, then
The liquid-phase outlet of boiling device connects with the charging aperture of penetrating fluid preheater hot side；Ethyl acetate is dehydrated the delivery port and technique of tower bottom
Waste water receiving unit connects with the fluid inlet of reboiler；
The ethyl acetate film dewatering unit includes membrane separator, and charging aperture and the ethyl acetate of the membrane separator are dehydrated
The discharging opening connection of top of tower；The discharging opening of the infiltration evaporation side of membrane separator and the inlet of the cold side of penetrating fluid preheater connect
Logical, the discharging opening of the upstream feed liquid side of membrane separator connects with ethyl acetate product tank.
Further, the ethyl acetate film dewatering unit also includes vacuum system and infiltration vapour condenser；The film point
From the inlet communication vacuum system of the infiltration evaporation side of device, the discharging opening connection infiltration vapour condensation of the infiltration evaporation side of membrane separator
The charging aperture of device；Permeate the inlet of the liquid outlet connection infiltration flow container of vapour condenser.
Further, the ethyl acetate film dewatering unit also includes ethyl acetate product condenser and feed preheater；
The charging aperture and raw material of the hot side of the discharging opening connection ethyl acetate product condenser of the upstream feed liquid side of the membrane separator are pre-
The charging aperture of the hot side of hot device；The discharging opening connection ethyl acetate product tank of the hot side of the ethyl acetate product condenser enters
Material mouth；The charging aperture connection cooling medium source of the cold side of the ethyl acetate product condenser；The hot side of the feed preheater
Discharging opening connection ethyl acetate product tank charging aperture, the charging aperture connection aquifer ethyl of the cold side of feed preheater is former
Material source, the discharging opening of the cold side of feed preheater connect the material inlet at the top of ethyl acetate dehydrating tower.
Further, ethyl acetate dehydrating tower is high-efficiency packing tower and plate column combination tower；The penetrating fluid charging aperture with
On at least provided with one layer of Gas distribution column plate；Fed below penetrating fluid charging aperture and below material inlet at least provided with one layer
By liquid column plate, improve the separating capacity of ethyl acetate dehydrating tower and the reliability of equipment, separating capacity improves, operating pressure and
Operation temperature reduces, stable operation；Gas distribution column plate and charging are respectively positioned in ethyl acetate dehydrating tower described ooze by liquid column plate
Pump is connected with pipeline between transparent liquid tank and penetrating fluid preheater.
Further, Gas distribution column plate and charging are entered above penetrating fluid charging aperture with penetrating fluid respectively by liquid column plate
At the 300mm-500mm of below material mouth or material inlet lower section；Being provided with the membrane separator can be carried out to ethyl acetate and water
The membrane module of selectively penetrating separation；The membrane module is hydrophilic organic film or inoranic membrane.
A kind of method that integrated ethyl acetate and water are separated using ethyl acetate dehydration device as described above, utilization are above-mentioned
Ethyl acetate dehydration device, 1~15wt% ethyl acetate raw material, i.e. aquifer ethyl are formed close to azeotropic with aqueous concentration
Raw material, is evaporated using ethyl acetate raw material and the ethyl acetate infiltration fluid dewatering rich in water concentrates the multi-functional acetic acid second being integrated
Ester dehydrating tower, infiltration evaporation UF membrane, energy multi-level multiple-effect such as utilize at technology, the second that production water content is 0.03~0.5wt%
Acetoacetic ester product, production procedure is simple and direct, and energy consumption is low.
To reach above-mentioned purpose, what the technical solution of the utility model was realized in：
A kind of method that integrated ethyl acetate and water are separated using ethyl acetate dehydration device as described above, including from second
The material inlet of acetoacetic ester dehydrating tower introduces the ethyl acetate raw material that water content is 1~15wt%, and is fed from penetrating fluid
Mouth is introduced into the penetrating fluid of caused two strands of ethyl acetate rich in water in membrane separator UF membrane operating process, passes through acetic acid
The integrated operating process of ethyl ester rectifying and dewatering unit and ethyl acetate film dewatering unit, obtains 0.03~0.5wt%'s of water content
The step of ethyl acetate product.
Preferably, the method for the integrated ethyl acetate of described separation and water, in addition to the second to water content for 1~15wt%
The step of acetoacetic ester raw material is preheated before entrance ethyl acetate dehydrating tower using feed preheater；Heat Jie of feed preheater
Matter is the retentate material of membrane separator discharge, and the multiple-effect that ethyl acetate dehydrating tower material steam heat energy can be achieved utilizes；Aqueous second
Preheating temperature of the acetoacetic ester raw material in feed preheater can be by adjusting ethyl acetate product condenser cooling medium consumption control
System.
Preferably, the method for the integrated ethyl acetate of described separation and water, in addition to the step of acquisition penetrating fluid；UF membrane
The infiltration vapour of ethyl acetate rich in water caused by device UF membrane operating process, permeated after infiltration vapour condenser condensation
Liquid.
Preferably, the method for the integrated ethyl acetate of described separation and water, in addition to penetrating fluid into ethyl acetate
The step of before dehydrating tower using the preheating of penetrating fluid preheater；The heating medium of penetrating fluid preheater is reboiler heating vapour-condensing
Liquid, realize the Multi-class propagation of reboiler heating vapour-condensing liquid heat energy.Penetrating fluid enters acetic acid second after the preheating of penetrating fluid preheater
Ester dehydrating tower hypomere charging aperture, realize that the vaporization of aquifer ethyl raw material and penetrating fluid take off simultaneously using ethyl acetate dehydrating tower
Water Sproading, the integrated operation of ethyl acetate need not set aquifer ethyl feed vaporization device and infiltration fluid dewatering to return respectively
Receive Ethyl Acetate Plant.
The operating pressure (gauge pressure) of ethyl acetate dehydrating tower is 0~0.1MPa, and temperature is 71~102 DEG C；Ethyl acetate film
The operating pressure (gauge pressure) of the infiltration evaporation of the membrane separator film of dewatering unit is -0.05~-0.095MPa.
A kind of operation and control that integrated ethyl acetate and water method are separated using ethyl acetate dehydration device as described above
Conditional statement processed is as follows：
Aqueous 1~15wt% ethyl acetate raw material is delivered to after feed preheater preheats at the top of ethyl acetate dehydrating tower
Material inlet, the raw material preheating temperature of aquifer ethyl is by adjusting ethyl acetate product condenser cooling medium consumption control
System, at the same by caused by membrane separating process be rich in water ethyl acetate penetrating fluid by penetrating fluid preheater preheat after, deliver to second
The penetrating fluid charging aperture of acetoacetic ester dehydrating tower bottom, the heating medium of penetrating fluid preheater is reboiler heating vapour-condensing liquid.
Ethyl acetate dehydrating tower provides heat by the heating steam of reboiler, and aquifer ethyl raw material is in ethyl acetate
Realize vaporization in dehydrating tower, at the same the penetrating fluid of the ethyl acetate rich in water in tower by mass transfer and heat transfer effect, realize second
Acetoacetic ester vaporizes and concentration, technique waste water are discharged from ethyl acetate dehydrating tower bottom of towe, and the discharge of ethyl acetate dehydrating tower column overhead is dense
The material steam close to aquifer ethyl raw material is spent, the operating pressure (gauge pressure) of ethyl acetate dehydrating tower is 0~0.1MPa, temperature
About 71~101 DEG C of degree.
Equipped with the membrane module that selectively penetrating separation can be carried out to ethyl acetate and water in membrane separator, membrane module is parent
Water-based organic film or inoranic membrane.The ethyl acetate material steam of ethyl acetate dehydration column overhead discharge delivers to membrane separator,
For hydrone in membrane separator in material stream due to the hydrophilic interaction of membrane material, selective is preferential rich on membrane material surface
Collection, in the presence of the vapor partial pressure difference of the film both sides of membrane separator, hydrone preferentially passes through film, infiltration evaporation side by diffusion
By connecting vacuum system, the molecule of infiltration is vaporized in downstream penetration film surface, subsequently enter the condenser condensation of infiltration vapour
Penetrating fluid is obtained, delivers to infiltration flow container, penetrating fluid is pressurized the return ethyl acetate after the preheating of penetrating fluid preheater by pump and taken off
Water tower dehydration recovery ethyl acetate, penetrating fluid preheater heating medium is reboiler steam condensate.
Retentate material after the dehydration of the upstream feed liquid side of membrane separator, while deliver to ethyl acetate product condenser and original
Expect preheater, realize that the multiple-effect of ethyl acetate dehydrating tower material steam heat energy utilizes, aquifer ethyl raw material preheating temperature leads to
The control of ethyl acetate product condenser cooling medium consumption is overregulated, it is 0.03~0.5% that water content is obtained after condensation cooling
Ethyl acetate product delivers to ethyl acetate product tank.The infiltration evaporation behaviour of the operating pressure of membrane separator, i.e. downstream penetration vapour side
It is -0.07~-0.095MPa to make pressure.
Relative to prior art, a kind of ethyl acetate dehydration device described in the utility model has the advantage that：
(1) a kind of ethyl acetate dehydration device described in the utility model, the disjoint set for ethyl acetate-aqueous systems
Into ethyl acetate dehydrating tower can integrate raw material evaporation and the ethyl acetate infiltration fluid dewatering concentration rich in water, raw material preheating
The setting of device, penetrating fluid preheater etc., the recycling of feasible system internal heat, reduce the energy consumption of whole system.
(2) a kind of ethyl acetate dehydration device described in the utility model, ethyl acetate dehydrating tower have high-efficiency packing tower
With the compound tower structure of plate column, more than penetrating fluid charging aperture at least provided with one layer of Gas distribution column plate, aquifer ethyl raw material
Fed below charging aperture and at least provided with one layer below penetrating fluid charging aperture by liquid column plate, enable the separation of ethyl acetate dehydrating tower
The reliability of power and equipment improves, and separating capacity improves, and operating pressure and operation temperature reduce, stable operation.
Relative to prior art, one kind described in the utility model is separated using ethyl acetate dehydration device as described above
The method of integrated ethyl acetate and water has the advantage that：
It is described in the utility model it is a kind of using the integrated ethyl acetate of ethyl acetate dehydration device as described above separation and
The method of water, the aquifer ethyl raw material using water content as 1~15wt%, can obtain 0.03~0.5wt% of water content second
Acetoacetic ester product, the saturated vapor using steam pressure as 0.6Mpa calculate, and the steam consumption of production ton ethyl acetate product is
0.25~0.36 ton.
It is described in the utility model it is a kind of using the integrated ethyl acetate of ethyl acetate dehydration device as described above separation and
The method of water, efficiently solve the aquifer ethyl raw material separation removal azeotropic water close to ethyl acetate azeotrope with water composition
Technique, due to complex process, steam consumption, the problems such as equipment investment is big and running cost is high, can not use conventional rectification technique,
The problem of the methods of extraction, extracting rectifying, azeotropic distillation can not be used.By aquifer ethyl feedstock evaporation process with
Permeate the coupling integration of fluid dewatering rectification-recovery process；Retentate material after dehydration preheats aquifer ethyl through feed preheater
Raw material, realize that the multiple-effect of reboiler heating steam energy utilizes；Penetrating fluid is heated through reboiler heating vapour-condensing liquid, and realization is boiled again
The Multi-class propagation of device heating vapour-condensing liquid energy, these measures make one kind of the present invention utilize ethyl acetate as described above
The method of the integrated ethyl acetate of dehydration device separation and water has flow simple, and functions of the equipments are more, and energy consumption is low, production cost and sets
The features such as standby investment declines, has stronger market promotion prospect.
Brief description of the drawings
Fig. 1 is a kind of simple structure schematic diagram of ethyl acetate dehydration device described in the utility model embodiment 1.
Reference：
1- ethyl acetate dehydrating towers；2- reboilers；4- penetrating fluid preheaters；5- membrane separators；6- ethyl acetate produces
Product condenser；7- feed preheaters；8- ethyl acetate product tanks；9- permeates vapour condenser；10- permeates flow container；11- techniques
Waste water receiving unit；12- vacuum systems；13- Gas distribution column plates；14- is fed by liquid column plate；15- aquifer ethyl raw materials
Source.
Embodiment
In addition to being defined, technical term used has and the utility model one of ordinary skill in the art in following examples
The identical meanings being commonly understood by.Test reagent used, is routine biochemistry reagent unless otherwise specified in following examples；
The experimental method, it is conventional method unless otherwise specified.
The utility model is described in detail with reference to embodiment and accompanying drawing.
Embodiment 1
As shown in figure 1, a kind of ethyl acetate dehydration device, including the ethyl acetate rectifying and dewatering list being interconnected with pipeline
Member and ethyl acetate film dewatering unit, valve is equipped with each pipeline；
The ethyl acetate rectifying and dewatering unit includes ethyl acetate dehydrating tower 1, reboiler 2 and penetrating fluid preheater 4；Institute
State the top of ethyl acetate dehydrating tower 1 and bottom and be respectively equipped with material inlet and penetrating fluid charging aperture；Penetrating fluid charging aperture with
The hot side discharging opening connection of penetrating fluid preheater 4, the air inlet of the lower end of ethyl acetate dehydrating tower 1 and the gaseous phase outlet of reboiler 2
Connection, the liquid-phase outlet of reboiler 2 connect with the charging aperture of the hot side of penetrating fluid preheater 4；The bottom of ethyl acetate dehydrating tower 1 goes out
The mouth of a river connects with the fluid inlet of technique waste water receiving unit 11 and reboiler 2；
The ethyl acetate film dewatering unit includes membrane separator 5, and the charging aperture of the membrane separator 5 takes off with ethyl acetate
The discharging opening connection at the top of water tower 1；The discharging opening of infiltration evaporation side of membrane separator 5 and entering for the cold side of penetrating fluid preheater 4
Liquid mouth connects, and the discharging opening of the upstream feed liquid side of membrane separator 5 connects with ethyl acetate product tank 8.
The ethyl acetate film dewatering unit also includes vacuum system 12 and infiltration vapour condenser 9；The membrane separator 5
The inlet communication vacuum system 12 of infiltration evaporation side, the discharging opening connection infiltration vapour condenser 9 of the infiltration evaporation side of membrane separator 5
Charging aperture；Permeate the inlet of the liquid outlet connection infiltration flow container 10 of vapour condenser 9.
The ethyl acetate film dewatering unit also includes ethyl acetate product condenser 6 and feed preheater 7；The film point
From the charging aperture and feed preheater 7 of the hot side of the discharging opening connection ethyl acetate product condenser 6 of the upstream feed liquid side of device 5
The charging aperture of hot side；The charging of the discharging opening connection ethyl acetate product tank 8 of the hot side of the ethyl acetate product condenser 6
Mouthful；The charging aperture connection cooling medium source of the cold side of the ethyl acetate product condenser 6；The hot side of the feed preheater 7
Discharging opening connection ethyl acetate product tank 8 charging aperture, the charging aperture connection aquifer ethyl of the cold side of feed preheater 7
Raw material source 15, the material inlet at the top of discharging opening connection ethyl acetate dehydrating tower 1 of the cold side of feed preheater 7.
Ethyl acetate dehydrating tower 1 is high-efficiency packing tower and plate column combination tower；More than the penetrating fluid charging aperture it is provided with 1 layer
Gas distribution column plate 13；1 layer of charging is equipped with below penetrating fluid charging aperture and below material inlet by liquid column plate 14；Gas phase point
Cloth column plate 13 and charging are respectively positioned on the infiltration flow container 10 and penetrating fluid preheater 4 in ethyl acetate dehydrating tower 1 by liquid column plate 14
Between pipeline on be connected with pump.
Gas distribution column plate 13 and charging are located at respectively by liquid column plate 14 above penetrating fluid charging aperture and penetrating fluid charging aperture
Below lower section or material inlet at 300mm；Selectively penetrating can be carried out to ethyl acetate and water by being provided with the membrane separator 5
The membrane module of separation；The membrane module is hydrophilic organic film, and specially polyvinyl alcohol (PVA)/polyacrylonitrile (PAN) is compound
Film.
The ethyl acetate raw material that integrated water content is 15wt% is separated using above-mentioned ethyl acetate dehydration device, to produce water
Content is as follows for the operating method and control condition of 0.5wt% ethyl acetate product：
Aquifer ethyl raw material delivers to the feedstock at the top of ethyl acetate dehydrating tower 1 after the preheating of feed preheater 7
Mouthful, aquifer ethyl raw material preheating temperature is controlled by adjusting the cooling medium consumption of ethyl acetate product condenser 6, simultaneously will
Ethyl acetate penetrating fluid rich in water caused by membrane separating process delivers to ethyl acetate dehydration after the preheating of penetrating fluid preheater 4
The penetrating fluid charging aperture of the bottom of tower 1, the heating medium of penetrating fluid preheater 4 is reboiler heating vapour-condensing liquid.
Ethyl acetate dehydrating tower 1 provides heat by the heating steam of reboiler 2, and aquifer ethyl raw material is in acetic acid second
Vaporization is realized in ester dehydrating tower 1, while the penetrating fluid of the ethyl acetate rich in water passes through mass transfer and heat transfer effect, realization in tower
Ethyl acetate vaporizes and concentration, technique waste water are discharged from the bottom of towe of ethyl acetate dehydrating tower 1, the tower top of ethyl acetate dehydrating tower tower 1 row
Go out concentration close to the material steam of aquifer ethyl raw material, the operating pressure (gauge pressure) of ethyl acetate dehydrating tower 1 is 0MPa, temperature
About 71 DEG C of degree.
The ethyl acetate material steam of the tower top of ethyl acetate dehydrating tower 1 discharge delivers to membrane separator 5, in membrane separator 5
Equipped with the membrane module that Selective Separation can be carried out to ethyl acetate and water, the membrane module in membrane separator 5 is hydrophilic organic
Film.In membrane separator 5, the hydrone in material stream is due to the hydrophilic interaction of membrane material, selective preferential dissolving absorption
In membrane material surface, film is preferentially passed through by diffusion in the presence of the vapor partial pressure difference of film both sides, infiltration evaporation side passes through connection
Vacuum system 12, the molecule of infiltration is set to subsequently enter the condensation of infiltration vapour condenser 9 and be permeated in downstream side form surface vaporization
Liquid, delivers to infiltration flow container 10, and penetrating fluid returns to ethyl acetate dehydrating tower 1 after the preheating of penetrating fluid preheater 4 and is dehydrated recovery second again
Acetoacetic ester, it is the steam condensation water of reboiler 2 that penetrating fluid preheater 4, which heats medium, the retentate material after the dehydration of feed liquid side, is sent simultaneously
To ethyl acetate product condenser 6 and feed preheater 7, the ethyl acetate product obtained after condensation cooling delivers to ethyl acetate production
Product tank 8.The vacuumizing pressure (gauge pressure) of membrane separator 5 is 0.05MPa.
According to the operating process of the separation integrated approach of a kind of ethyl acetate and water described above, processing water content is
15wt% aquifer ethyl raw material, can obtain water content 0.5wt% ethyl acetate product, using steam pressure as 0.6Mpa
Saturated vapor calculate, production ton ethyl acetate product steam consumption be 0.36 ton.
Embodiment 2
A kind of ethyl acetate dehydration device described in the present embodiment is substantially the same manner as Example 1, and difference is：It is described
Membrane module is hydrophilic inoranic membrane, specially porous aluminium oxide loaded NaA molecular sieve membrane；Ethyl acetate dehydrating tower 1 has height
Packed tower and the compound tower structure of plate column are imitated, more than penetrating fluid charging aperture distance 500mm sets 1 layer of Gas distribution column plate 13, contains
Distance 500mm below distance 500mm below water ethyl acetate material inlet and penetrating fluid charging aperture sets 2 layers of charging by liquid tower
Plate 14.
The ethyl acetate raw material that integrated water content is 1wt% is separated using above-mentioned ethyl acetate dehydration device, to produce water
Content is as follows for the operating method and control condition of 0.03wt% ethyl acetate product：
Aquifer ethyl raw material delivers to the feedstock at the top of ethyl acetate dehydrating tower 1 after the preheating of feed preheater 7
Mouthful, aquifer ethyl raw material preheating temperature is controlled by adjusting the cooling medium consumption of ethyl acetate product condenser 6, simultaneously will
Ethyl acetate penetrating fluid rich in water caused by membrane separating process delivers to ethyl acetate dehydration after the preheating of penetrating fluid preheater 4
The penetrating fluid charging aperture of the bottom of tower 1, the heating medium of penetrating fluid preheater 4 is the heating vapour-condensing liquid of reboiler 2.
Ethyl acetate dehydrating tower 1 provides heat by the heating steam of reboiler 2, and aquifer ethyl raw material is in acetic acid second
Vaporization is realized in ester dehydrating tower 1, while the penetrating fluid of the ethyl acetate rich in water passes through mass transfer and heat transfer effect, realization in tower
Ethyl acetate vaporizes and concentration, technique waste water are discharged from the bottom of towe of ethyl acetate dehydrating tower 1, the column overhead of ethyl acetate dehydrating tower 1 row
Go out concentration is close to the material steam of aquifer ethyl raw material, the operating pressure (gauge pressure) of ethyl acetate dehydrating tower 1
0.01MPa, about 102 DEG C of temperature.
The ethyl acetate material steam of the tower top of ethyl acetate dehydrating tower 1 discharge delivers to membrane separator 5, in membrane separator 5
Equipped with the membrane module that Selective Separation can be carried out to ethyl acetate and water, the membrane module in membrane separator 5 is hydrophilic inorganic
Film.In membrane separator 5, the hydrone in material stream is due to the hydrophilic interaction of membrane material, selective preferential dissolving absorption
In membrane material surface, film is preferentially passed through by diffusion in the presence of the vapor partial pressure difference of film both sides, infiltration evaporation side passes through connection
Vacuum system 12, the molecule of infiltration is set to subsequently enter the condensation of infiltration vapour condenser 9 and be permeated in downstream side form surface vaporization
Liquid, delivers to infiltration flow container 10, and penetrating fluid returns to ethyl acetate dehydrating tower 1 after the preheating of penetrating fluid preheater 4 and is dehydrated recovery second again
Acetoacetic ester, it is the steam condensation water of reboiler 2 that penetrating fluid preheater 4, which heats medium, the retentate material after the dehydration of feed liquid side, is sent simultaneously
To ethyl acetate product condenser 6 and feed preheater 7, the ethyl acetate product obtained after condensation cooling delivers to ethyl acetate production
Product tank 8.The vacuumizing pressure (gauge pressure) of membrane separator 5 is 0.095MPa.
According to the operating process of the separation integrated approach of a kind of ethyl acetate and water described above, processing water content is
1wt% aquifer ethyl raw material, can obtain water content 0.03wt% ethyl acetate product, using steam pressure as 0.6Mpa
Saturated vapor calculate, production ton ethyl acetate product steam consumption be 0.25 ton.
Embodiment 3
A kind of ethyl acetate dehydration device described in the present embodiment is substantially the same manner as Example 2, and difference is：It is described
Membrane module is hydrophilic organic film, specially polyvinyl alcohol (PVA)/polyacrylonitrile (PAN) composite membrane.
The ethyl acetate raw material that integrated water content is 8.1wt% is separated using above-mentioned ethyl acetate dehydration device, with production
Water content is as follows for the operating method and control condition of 0.1wt% ethyl acetate product：
Aquifer ethyl raw material delivers to the feedstock at the top of ethyl acetate dehydrating tower 1 after the preheating of feed preheater 7
Mouthful, aquifer ethyl raw material preheating temperature is controlled by adjusting the cooling medium consumption of ethyl acetate product condenser 6, simultaneously will
Ethyl acetate penetrating fluid rich in water caused by membrane separating process delivers to ethyl acetate dehydration after the preheating of penetrating fluid preheater 4
The penetrating fluid charging aperture of the bottom of tower 1, the heating medium of penetrating fluid preheater 4 is the heating vapour-condensing liquid of reboiler 2.
Ethyl acetate dehydrating tower 1 provides heat by the heating steam of reboiler 2, and aquifer ethyl raw material is in acetic acid second
Vaporization is realized in ester dehydrating tower 1, while the penetrating fluid of the ethyl acetate rich in water passes through mass transfer and heat transfer effect, realization in tower
Ethyl acetate vaporizes and concentration, technique waste water are discharged from the bottom of towe of ethyl acetate dehydrating tower 1, the column overhead of ethyl acetate dehydrating tower 1 row
Go out concentration is close to the material steam of aquifer ethyl raw material, the operating pressure (gauge pressure) of ethyl acetate dehydrating tower 1
0.05MPa, about 90 DEG C of temperature.
The ethyl acetate material steam of the tower top of ethyl acetate dehydrating tower 1 discharge delivers to membrane separator 5, in membrane separator 5
Equipped with the membrane module that Selective Separation can be carried out to ethyl acetate and water, the membrane module in membrane separator 5 is hydrophilic organic
Film.In membrane separator 5, the hydrone in material stream is due to the hydrophilic interaction of membrane material, selective preferential dissolving absorption
In membrane material surface, film is preferentially passed through by diffusion in the presence of the vapor partial pressure difference of film both sides, infiltration evaporation side passes through connection
Vacuum system 12, the molecule of infiltration is set to subsequently enter the condensation of infiltration vapour condenser 9 and be permeated in downstream side form surface vaporization
Liquid, delivers to infiltration flow container 10, and penetrating fluid returns to ethyl acetate dehydrating tower 1 after the preheating of penetrating fluid preheater 4 and is dehydrated recovery second again
Acetoacetic ester, it is the steam condensation water of reboiler 2 that penetrating fluid preheater 4, which heats medium, the retentate material after the dehydration of feed liquid side, is sent simultaneously
To ethyl acetate product condenser 6 and feed preheater 7, the ethyl acetate product obtained after condensation cooling delivers to ethyl acetate production
Product tank 8.The vacuumizing pressure (gauge pressure) of membrane separator 5 is 0.09MPa.
According to the operating process of the separation integrated approach of a kind of ethyl acetate and water described above, processing water content is
8.1wt% aquifer ethyl raw material, can obtain water content 0.1wt% ethyl acetate product, using steam pressure as
0.6Mpa saturated vapor calculates, and the steam consumption of production ton ethyl acetate product is 0.32 ton.
The system and method that the utility model is disclosed and proposed, those skilled in the art can be fitted by using for reference present disclosure
When the links such as feed change, technological parameter, structure design are realized.The method of the present invention has been entered by preferred embodiment with technology
Gone description, person skilled substantially can not depart from present invention, in spirit and scope to method described herein and
Technology is modified or suitably changed with combining, to realize the technology of the present invention.
Preferred embodiment of the present utility model is the foregoing is only, it is all at this not to limit the utility model
Within the spirit and principle of utility model, any modification, equivalent substitution and improvements made etc., the utility model should be included in
Protection domain within.
Claims (7)
- A kind of 1. ethyl acetate dehydration device, it is characterised in that：Including the ethyl acetate rectifying and dewatering list being interconnected with pipeline Member and ethyl acetate film dewatering unit, valve is equipped with each pipeline；The ethyl acetate rectifying and dewatering unit includes ethyl acetate dehydrating tower (1), reboiler (2) and penetrating fluid preheater (4)； The tower top of the ethyl acetate dehydrating tower (1) and tower bottom are respectively equipped with material inlet and penetrating fluid charging aperture；Penetrating fluid enters Material mouth connects with the hot side discharging opening of penetrating fluid preheater (4), the air inlet and reboiler of ethyl acetate dehydrating tower (1) lower end (2) gaseous phase outlet connection, the liquid-phase outlet of reboiler (2) connect with the charging aperture of penetrating fluid preheater (4) hot side；Acetic acid second The delivery port of ester dehydrating tower (1) bottom connects with the fluid inlet of technique waste water receiving unit (11) and reboiler (2)；The ethyl acetate film dewatering unit includes membrane separator (5), and the charging aperture of the membrane separator (5) takes off with ethyl acetate Discharging opening connection at the top of water tower (1)；The discharging opening of the infiltration evaporation side of membrane separator (5) is cold with penetrating fluid preheater (4) The inlet connection of side, the discharging opening of the upstream feed liquid side of membrane separator (5) connect with ethyl acetate product tank (8).
- 2. ethyl acetate dehydration device according to claim 1, it is characterised in that：The ethyl acetate film dewatering unit is also Including vacuum system (12) and infiltration vapour condenser (9)；The inlet communication vacuum system of the infiltration evaporation side of the membrane separator (5) Unite (12), the charging aperture of the discharging opening connection infiltration vapour condenser (9) of the infiltration evaporation side of membrane separator (5)；Permeate vapour condensation The inlet of the liquid outlet connection infiltration flow container (10) of device (9).
- 3. ethyl acetate dehydration device according to claim 1, it is characterised in that：The ethyl acetate film dewatering unit is also Including ethyl acetate product condenser (6) and feed preheater (7)；The discharging opening of the upstream feed liquid side of the membrane separator (5) Connect the charging aperture of the hot side of ethyl acetate product condenser (6) and the charging aperture of the hot side of feed preheater (7)；The acetic acid The charging aperture of the discharging opening connection ethyl acetate product tank (8) of the hot side of ethyl ester product condenser (6)；The ethyl acetate product The charging aperture connection cooling medium source of the cold side of condenser (6)；The discharging opening connection acetic acid of the hot side of the feed preheater (7) The charging aperture of ethyl ester product tank (8), the charging aperture connection aquifer ethyl raw material source (15) of the cold side of feed preheater (7), The material inlet of discharging opening connection ethyl acetate dehydrating tower (1) tower top of the cold side of feed preheater (7).
- 4. ethyl acetate dehydration device according to claim 2, it is characterised in that：Ethyl acetate dehydrating tower (1) is efficient Packed tower and plate column combination tower；Pump is connected with pipeline between the infiltration flow container (10) and penetrating fluid preheater (4).
- 5. ethyl acetate dehydration device according to claim 1, it is characterised in that：More than the penetrating fluid charging aperture at least Provided with one layer of Gas distribution column plate (13)；Below penetrating fluid charging aperture and material inlet below at least provided with one layer charging by Liquid column plate (14)；Gas distribution column plate (13) and charging are respectively positioned in ethyl acetate dehydrating tower (1) by liquid column plate (14).
- 6. ethyl acetate dehydration device according to claim 5, it is characterised in that：Gas distribution column plate (13) and charging by Liquid column plate (14) is respectively positioned at penetrating fluid charging aperture top and penetrating fluid charging aperture lower section or material inlet lower section 300mm- At 500mm.
- 7. ethyl acetate dehydration device according to claim 1, it is characterised in that：Being provided with the membrane separator (5) can The membrane module of selectively penetrating separation is carried out to ethyl acetate and water；The membrane module is hydrophilic organic film or inoranic membrane.
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| CN201720515040.9U CN206858474U (en) | 2017-05-10 | 2017-05-10 | A kind of ethyl acetate dehydration device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201720515040.9U CN206858474U (en) | 2017-05-10 | 2017-05-10 | A kind of ethyl acetate dehydration device |
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