CN207713660U - A kind of energy-saving Synthesis Diethyl ether system - Google Patents
A kind of energy-saving Synthesis Diethyl ether system Download PDFInfo
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- CN207713660U CN207713660U CN201721752253.XU CN201721752253U CN207713660U CN 207713660 U CN207713660 U CN 207713660U CN 201721752253 U CN201721752253 U CN 201721752253U CN 207713660 U CN207713660 U CN 207713660U
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Abstract
The utility model discloses a kind of energy-saving Synthesis Diethyl ether systems, including moving towards sequentially connected raw material feed device according to process, esterification device, refining plant and products pot, raw material feed device includes ester alcohol head tank, it is dehydrated ester alcohol tank and acetic acid tank, esterification device includes pressing the sequentially connected esterification reboiler of reaction process, esterifying kettle, esterification column, esterification condensator and esterification layering tank, dehydration ester alcohol tank and acetic acid tank are connect with esterification reboiler respectively, sequentially connected feed vaporizer and raw material vapor permeable membrance component are set between ester alcohol head tank and dehydration ester alcohol tank；Sequentially connected esterification evaporator and esterification vapor permeable membrance component are set between esterification layering tank and esterification condensing unit, and the discharge port for being esterified the feed liquid side of vapor permeable membrance component is connect with esterification column overhead reflux mouth and refining plant feed inlet respectively through two pipelines.The utility model can reduce the energy consumption in building-up process.
Description
Technical field
The utility model is related to the synthesis systems of ethyl acetate, and in particular to a kind of energy-saving Synthesis Diethyl ether system
System.
Background technology
Acetic acid ethyl ester is a kind of important Organic Chemicals, can be used for manufacturing acetamide, acetoacetic ester etc., as work
Industry solvent can be used in the products such as paint, adhesive, ethyl cellulose, artificial leather, malthoid colorant, staple fibre；Make
For adhesive, the production for printing ink, olivet；As extractant, the production for products such as medicine, organic acids is simultaneously
In industries extensive uses such as essence and flavoring agent, medicine, advanced ink, pyroxylin, nitrocellulose, dyestuffs.
Lactate synthesis is the conventional production methods of ethyl acetate, and under the catalytic action of the concentrated sulfuric acid, ethyl alcohol and acetic acid are in ester
Change and reacted in kettle, is steamed from esterification tower top in the form of ethyl acetate, alcohol and water ternary azeotrope, the ester generated according to reaction
Water with from the point of view of ester water in azeotropic mixture, react the ester of generation and cannot take away moisture completely, in order to improve in actual production
Band water effect, often azeotropic mixture is after esterification overhead condensation cooling, band water in a part of ethyl acetate backflow to tower in upper layer, separately
To the refined purification for the treatment of column, lower layer's water phase to recovery tower is dehydrated to be recycled a part.Due to ethyl acetate-water-ethanol ternary azeotropic
The water content (about 5-6wt%) that moisture (about 9wt.%) is dissolved each other with room temperature lower part in object differs smaller, the band for the ester that flows back
Outlet capacity is poor, causes the reflux of esterification column bigger, is 95% ethyl alcohol in itself usually between 3-5, and in feed ethanol
Or the ethyl alcohol that other water content are larger, the moisture brought into kettle is more, needs more ethyl acetate backflows；Furthermore enter
The thick cruel middle water content for the treatment of column is relatively high, and water and ethyl alcohol are not contained in product to ensure that tower reactor produces, tower top ethyl acetate
Regurgitant volume is also higher, in addition, to reduce the consumption of ethyl alcohol, from refined overhead extraction containing ethyl acetate, second alcohol and water it is mixed
The organic phase isolated in conjunction object returns to esterification tower reactor and continues to participate in reaction, and a part of water is caused to be followed in esterification column and treating column
Ring, energy consumption are higher.
Utility model content
The purpose of this utility model is to provide a kind of energy-saving Synthesis Diethyl ether system.
The purpose of this utility model is achieved through the following technical solutions：A kind of energy-saving Synthesis Diethyl ether system
System, including sequentially connected raw material feed device, esterification device, refining plant and products pot are moved towards according to process,
The raw material feed device includes ester alcohol head tank, dehydration ester alcohol tank and acetic acid tank, and the esterification device includes by reaction
The sequentially connected esterification reboiler of process, esterifying kettle, esterification column, esterification condensator and esterification layering tank, the dehydration ester alcohol tank
It is connect respectively with esterification reboiler with acetic acid tank, wherein be arranged between the ester alcohol head tank and dehydration ester alcohol tank and be sequentially connected
Feed vaporizer and raw material vapor permeable membrance component, the ethyl alcohol from ester alcohol head tank by feed vaporizer evaporate vapour
Enter the diafiltration dehydration of raw material vapor permeable membrance component after change, enters later in dehydration ester alcohol tank and store；The esterification layering
Sequentially connected esterification evaporator and esterification vapor permeable membrance component, the esterification vapor permeable membrance group are set after tank
The discharge port of the feed liquid side of part is connect with esterification column overhead reflux mouth and refining plant feed inlet respectively through two pipelines, comes from ester
The organic phase for changing layering tank upper layer enters esterification vapor permeable membrance component diafiltration dehydration after being esterified evaporator carburation by evaporation,
Then being divided into two parts, refuxing esterification tower and entrance refining plant are refined respectively.
The raw material vapor permeable membrance component includes by shell and several infiltrations of shell and tube arrangement inside the shell
Vaporize the film group of membrane tube composition.As one embodiment, the infiltrating and vaporizing membrane group number is 6 or more, each infiltration evaporation
Film group area is 7cm2。
The esterification vapor permeable membrance component includes by shell and several infiltrations of shell and tube arrangement inside the shell
Vaporize the film group of membrane tube composition.As one embodiment, the infiltrating and vaporizing membrane group number is 10 or more, each infiltration evaporation
Film group area is 20cm2。
The refining plant includes treating column, the refined reboiler being connect with treating column bottom of tower, it is refined to be connect with tower top
Condenser and refined layering tank, the bottom of tower discharge port of the treating column are connect with products pot, and the refined layering tank top has
Machine phase discharge port is connect with treating column overhead reflux mouth and ester alcohol head tank respectively through two pipelines.
The utility model further includes device for recycling sewage, the raw material vapor permeable membrance component and esterification infiltration evaporation
The discharge port of the per-meate side of permeable membrane module is connect by condensing unit with device for recycling sewage respectively, under the refined layering tank
The water phase discharge port in portion is connect with device for recycling sewage, to carry out unified recovery processing to the waste water generated in technical process.
The device for recycling sewage includes Water Tank and sewage recovery tower, the raw material vapor permeable membrance component and ester
The discharge port for changing the per-meate side of vapor permeable membrance component is connected by the water inlet of vacuum plant and Water Tank respectively, described
The water phase discharge port of refined layering tank lower part and the water inlet of Water Tank connect, the Water Tank water outlet and sewage recovery tower
Water inlet connects, and the sewage of recycling is sent into sewage recovery tower and is handled, and it is cold that the sewage recycling column overhead connects back to receipts
Condenser and recycling layering tank, the organic phase outlet on recycling layering tank top with and ester alcohol head tank connect, the row of its underpart
The mouth of a river is connect with sewage recovery tower overhead reflux mouth.
The vacuum plant includes condenser, condensate liquid surge tank and vacuum pump, the leaving condenser water mouth and sewage
Tank connects, and the feed inlet of the cooling medium surge tank is connect with condenser discharge port respectively, the vacuum pump and cooling medium
Surge tank connects.
The beneficial effects of the utility model：
(1) sequentially connected feed vaporizer and original is arranged between ester alcohol head tank and dehydration ester alcohol tank in the utility model
Expect that vapor permeable membrance component, the ethyl alcohol from ester alcohol head tank enter raw material after feed vaporizer carburation by evaporation and permeate
The diafiltration dehydration of vaporation permeable membrane module, enters in dehydration ester alcohol tank and stores later；It is arranged after esterification is layered tank sequentially connected
It is esterified evaporator and esterification vapor permeable membrance component, the organic phase from esterification layering tank upper layer is through being esterified evaporator evaporation
Enter esterification vapor permeable membrance component diafiltration dehydration after vaporization, it is thick by the moisture and esterification tower top that control feed ethanol
The moisture of ethyl acetate, is not limited in synthesis technology by azeotropic, does not introduce third component, ensures yield and product purity, can
Continuous operation, and low energy consumption.
(2) the utility model removes feed ethanol by vapor permeable membrance component and is esterified the water of tower top ethyl acetate
Point, the regurgitant volume in reactive distillation and subtractive process is greatly reduced, the yield of product is improved.
Description of the drawings
Fig. 1 is the Synthesis Diethyl ether system of the utility model application.
Specific implementation mode
The utility model is described in further detail with reference to specific embodiments and the drawings.The present embodiment is with this reality
With being implemented under premised on new technique, detailed embodiment and specific operating process, but the utility model are now provided
Protection domain embodiment not limited to the following.
Synthesis Diethyl ether system as shown in Figure 1 is the embodiments of the present invention, by according to process trend according to
Secondary connection raw material feed device, esterification device, refining plant, sewage-treatment plant and products pot 20.
Raw material feed device is by ester alcohol head tank 1, feed vaporizer 2, raw material vapor permeable membrance component 3, dehydration ester
Alcohol tank 4 and acetic acid tank 5 are constituted.Ester alcohol head tank 1, feed vaporizer 2 and raw material vapor permeable membrance component 3 and dehydration ester alcohol
Tank 4 is sequentially connected, and it is saturating that the ethyl alcohol from ester alcohol head tank 1 enters raw material infiltration evaporation after 2 carburation by evaporation of feed vaporizer
Moisture film component 3 is percolated, and is entered after removing moisture in dehydration ester alcohol tank 4 and is stored.Be dehydrated the discharge port of ester alcohol tank 4 and acetic acid tank 5 with
The feed inlet of esterification device connects.
Esterification device is by esterification reboiler 11, esterifying kettle 10, esterification column 12, esterification condensator 13, esterification layering tank
14, it is esterified evaporator 15 and esterification vapor permeable membrance component 16 is sequentially connected.It is esterified feed inlet and the dehydration of reboiler 11
The discharge port of ester alcohol tank 4 and acetic acid tank 5 connects.The feed liquid side for being esterified vapor permeable membrance component 16 has discharge port, this goes out
Material mouth is connect with 12 overhead reflux mouth of esterification column and refining plant feed inlet respectively through two pipelines, on esterification layering tank 14
The organic phase of layer enters esterification vapor permeable membrance component 16 after being esterified 15 carburation by evaporation of evaporator and is percolated dehydration, then divides
At two parts, refuxing esterification tower 12 and entrance refining plant are refined respectively.The dewatered ethanol and second being dehydrated in ester alcohol tank 4
After being heated in being esterified reboiler 11 into esterifying kettle 10 esterification, product occur in the presence of a catalyst for the acetic acid of sour tank 5
Into being detached in esterification column 12, ethyl acetate, alcohol and water ternary azeotrope distillated from tower top condensed through esterification condensator 13 it is laggard
Enter esterification layering tank 14 to be layered, upper organic phase enters esterification vapor permeable membrance after entering esterification 15 carburation by evaporation of evaporator
16 infiltration evaporation of component obtains the trapped fluid of removing moisture.Trapped fluid flows back a part through return line by certain reflux ratio
To water entrainer, another part is used as in esterification column 12 then refining plant is sent into through product output pipe and is refined.
Refining plant is made for the treatment of column 22, refined condenser 23, refined layering tank 24, refined reboiler 21, treating column
22 bottom of tower discharge ports and 21 bottom discharge mouth of refined reboiler are connect with products pot 20.22 tower top exhaust outlet for the treatment of column is through refined
Condenser 23 connect with refined layering tank 24, refine be layered the discharge port on 24 top of tank by two pipelines respectively with treating column 22
The refluxing opening and ester alcohol head tank 1 of tower top connect, and a upper organic phase part for refined layering tank 24 is back to treating column
In, another part send to ester alcohol head tank 1 and is used as reaction raw materials.
Sewage-treatment plant includes sewage storage tank 7 and sewage recovery tower 26.Raw material vapor permeable membrance component 3 permeates
The discharge outlet of side is through the first vacuum plant and sewage storage tank 7, the discharge outlet of 16 per-meate side of esterification vapor permeable membrance component
Through the second vacuum plant and sewage storage tank 7, esterification layering tank 14 and the refined water outlet for being layered 24 bottom of tank respectively with sewage
Storage tank 7 connects.The water outlet of 7 bottom of sewage storage tank is connect with the water inlet of sewage recovery tower 26, and sewage is sent into sewage
It is handled in recovery tower 26.26 bottom of tower of sewage recovery tower is equipped with regenerator 25, and tower top is equipped with sequentially connected sewage condenser
27 and sewage be layered tank 28.The discharge port on the top of sewage layering tank 28 is connect with ester alcohol head tank 1, organic by what is separated
It mutually send to ester alcohol head tank 1 and is used as reaction raw materials；The discharge port of its bottom is connect with 26 overhead reflux mouth of sewage recovery tower, will under
Continue to handle in layer aqueous-phase reflux tower.
First vacuum plant and the second vacuum plant include condenser 6,17, condensate liquid surge tank 8,18 and vacuum pump
9,19.6,7 water outlet of condenser is connect with Water Tank 17, and condensate liquid surge tank 8,18 is connected with condenser 6,7, vacuum pump 9,
19 connect with surge tank 8,18.
In the present embodiment, raw material vapor permeable membrance component 6 includes that shell and tube arranges by shell and inside the shell
6 infiltrating and vaporizing membrane groups of membrane tube composition, each infiltrating and vaporizing membrane group area are 7cm2.It is esterified vapor permeable membrance component 16
Include by shell and 10 infiltrating and vaporizing membrane groups forming of membrane tube of shell and tube arrangement inside the shell, each infiltrating and vaporizing membrane group
Area is 20cm2。
Synthesis Diethyl ether working-flow and principle：Ethyl alcohol is pumped into feed vaporizer 2 from ester alcohol head tank 1, control
Temperature and boil-off pressure, into raw material vapor permeable membrance component 6, due to the water-wet behavior and pore size of film itself
It limits (molecule screening principle), compared to other organic molecules, hydrone is easier to penetrate this inoranic membrane, in the per-meate side of membrane tube
It is evacuated to vacuum using vacuum pump 9, so that the retention side of raw material vapor permeable membrance component 6 and per-meate side is formed pressure difference, gives moisture
Son provides motive force through membrane tube, to realize ethanol dehydration.Dehydration ester alcohol is drained into followed by 6 groups of dewatered ethyl alcohol of membrane tube
Tank 4, and the waste water infiltrated through membrane module is discharged to Water Tank 7 by the collection of condenser 6.
Be dehydrated in ester alcohol tank 4 in dewatered ethanol and acetic acid tank 5 acetic acid and sulfuric acid through be esterified 11 heating evaporation of reboiler into
Enter in esterifying kettle 10, control kettle temperature is reacted, and reaction vapor, which enters in esterification column 12, to be detached, and reaction product is with ethyl acetate-
The form of alcohol-water ternary azeotrope is condensed through esterification condensator 13 enters the esterification layering layering of tank 14, and lower layer's water phase is discharged to dirt
Water pot 7, upper organic phase are permeated through evaporator 15, control temperature, boil-off pressure and per-meate side vacuum pressure into esterification
Vaporation permeable membrane module 16 is dehydrated, and the penetrating fluid after UF membrane enters Water Tank 7 after the cooling of the second cooler 17, after dehydration
An ethyl acetate part return the reflux band water of esterification column 12, another part enters the refined purification for the treatment of column 22, dehydrated acetic acid ethyl ester
Since most of water is all stripped of, so comparing legacy system, regurgitant volume greatly reduces needed for esterification column 12, and enters treating column
Since water content reduces, reflux ratio also accordingly reduces by 22 ethyl acetate.
Dehydrated acetic acid ethyl ester detaches in treating column 22, and bottom of tower sintetics is discharged to products pot 20, and overhead vapours is with second
The form of acetoacetic ester-alcohol-water ternary azeotrope is layered through refining condenser 23 into refined layering tank 24, and lower layer's water phase is discharged to
Water Tank 7, a upper organic phase part return treating column 22 and flow back, and another part is discharged to ester alcohol head tank 1, is dehydrated through UF membrane
After reenter esterifying kettle 11 reaction.
7 raw material of Water Tank enters sewage recovery tower 26 and is recycled, and overhead vapours is total with ethyl acetate, alcohol and water ternary
The condensed device 27 of form for boiling object enters the sewage layering layering of tank 28, and lower layer's water phase is back in tower, and upper layer ester mutually drains into ester alcohol
Head tank 1 reenters the reaction of esterifying kettle 11 after UF membrane is dehydrated.26 bottom of tower sewerage of sewage recovery tower is at sewage plant
Reason.
Claims (8)
1. a kind of energy-saving Synthesis Diethyl ether system, including move towards sequentially connected raw material supply dress according to process
Set, esterification device, refining plant and products pot, the raw material feed device include ester alcohol head tank, dehydration ester alcohol tank and
Acetic acid tank, the esterification device include by the sequentially connected esterification reboiler of reaction process, esterifying kettle, esterification column, esterification
Condenser and esterification layering tank, the dehydration ester alcohol tank and acetic acid tank are connect with esterification reboiler respectively, characterized in that the ester
Sequentially connected feed vaporizer and raw material vapor permeable membrance component are set between raw polyol tank and dehydration ester alcohol tank；It is described
Sequentially connected esterification evaporator and esterification vapor permeable membrance component, the esterification infiltration evaporation are set after esterification layering tank
The discharge port of the feed liquid side of permeable membrane module connects with esterification column overhead reflux mouth and refining plant feed inlet respectively through two pipelines
It connects.
2. energy-saving Synthesis Diethyl ether system according to claim 1, characterized in that the raw material infiltration evaporation
Permeable membrane module includes by shell and the film group that forms of several infiltration evaporation membrane tubes of shell and tube arrangement inside the shell.
3. energy-saving Synthesis Diethyl ether system according to claim 2, characterized in that the infiltrating and vaporizing membrane group
Number is 6 or more, and each infiltrating and vaporizing membrane group area is 7cm2。
4. energy-saving Synthesis Diethyl ether system according to claim 1, characterized in that the esterification infiltration evaporation
Permeable membrane module include by shell and inside the shell shell and tube arrangement several infiltration evaporation membrane tubes film group.
5. energy-saving Synthesis Diethyl ether system according to claim 4, characterized in that the infiltrating and vaporizing membrane group
Number is 10 or more, and each infiltrating and vaporizing membrane group area is 20cm2。
6. energy-saving Synthesis Diethyl ether system according to claim 1, characterized in that the refining plant includes
Treating column, the refined reboiler being connect with treating column bottom of tower, the refined condenser being connect with tower top and refined layering tank, the essence
The bottom of tower discharge port of tower processed is connect with products pot, the organic phase discharge port on the refined layering tank top through two pipelines respectively with
Treating column overhead reflux mouth is connected with ester alcohol head tank.
7. energy-saving Synthesis Diethyl ether system according to claim 1, characterized in that further include sewage recycling dress
It sets, the discharge port of the per-meate side of the raw material vapor permeable membrance component and esterification vapor permeable membrance component passes through respectively
Condensing unit is connect with device for recycling sewage, and the water phase discharge port of the refined layering tank lower part is connect with device for recycling sewage,
To carry out unified recovery processing to the waste water generated in technical process.
8. energy-saving Synthesis Diethyl ether system according to claim 7, characterized in that the device for recycling sewage
Including Water Tank and sewage recovery tower, the raw material vapor permeable membrance component is oozed with esterification vapor permeable membrance component
The discharge port of saturating side is connected by the water inlet of condensing unit and Water Tank respectively, the water phase discharging of the refined layering tank lower part
Mouth is connect with the water inlet of Water Tank, and the Water Tank water outlet is connect with the water inlet of sewage recovery tower, by the sewage of recycling
It is sent into sewage recovery tower and is handled, the sewage recycling column overhead, which connects back to, receives condenser and recycling layering tank, described time
The organic phase outlet on contracture layer tank top with and ester alcohol head tank connect, the discharge outlet of its underpart and sewage recovery tower overhead reflux
Mouth connection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721752253.XU CN207713660U (en) | 2017-12-13 | 2017-12-13 | A kind of energy-saving Synthesis Diethyl ether system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721752253.XU CN207713660U (en) | 2017-12-13 | 2017-12-13 | A kind of energy-saving Synthesis Diethyl ether system |
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| Publication Number | Publication Date |
|---|---|
| CN207713660U true CN207713660U (en) | 2018-08-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201721752253.XU Expired - Fee Related CN207713660U (en) | 2017-12-13 | 2017-12-13 | A kind of energy-saving Synthesis Diethyl ether system |
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| Country | Link |
|---|---|
| CN (1) | CN207713660U (en) |
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2017
- 2017-12-13 CN CN201721752253.XU patent/CN207713660U/en not_active Expired - Fee Related
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Granted publication date: 20180810 Termination date: 20211213 |