CN209161729U - A kind of dichloroethanes/ethane nitrile wastewater processing unit - Google Patents
A kind of dichloroethanes/ethane nitrile wastewater processing unit Download PDFInfo
- Publication number
- CN209161729U CN209161729U CN201821916615.9U CN201821916615U CN209161729U CN 209161729 U CN209161729 U CN 209161729U CN 201821916615 U CN201821916615 U CN 201821916615U CN 209161729 U CN209161729 U CN 209161729U
- Authority
- CN
- China
- Prior art keywords
- tank
- acetonitrile
- dichloroethanes
- processing unit
- wastewater processing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The utility model relates to a kind of dichloroethanes/ethane nitrile wastewater processing units.This device includes extractive distillation column, distillate drum, molecular screen membrane equipment, washing kettle.Extractive distillation column is operated using first continuous, rear interval two ways, and the distillate under different operation mode is collected into respectively in different distillate drums, and binding molecule sieve membrane separation equipment is dehydrated, and obtains water content≤0.05wt.% acetonitrile solvent, acetonitrile purity >=99.5%.The present apparatus is combined with molecular screen membrane separation equipment using extractive distillation column, and it is big to solve in line environmental hazard, and it is big to separate and recover difficulty, the not high problem of acetonitrile purity.
Description
Technical field
The utility model relates to a kind of dichloroethanes/ethane nitrile wastewater processing units.
Background technique
In chemical production process, dichloroethanes and acetonitrile are chiefly used in the dissolution and purification of organic chemicals, after use
Solvent dichloroethanes and acetonitrile mix, and water content is higher, cannot reach reuse standard.Waste liquid generates in production process
Amount is big, and in line environmental hazard is big, high production cost, can additionally increase production cost again as sewage treatment.Dichloroethanes,
Acetonitrile, with three kinds of components of water azeotropic two-by-two, separation cannot achieve using single tower distillation, use at present more for multitower rectifying work
Skill, intermediate treatment is cumbersome, and recycling acetonitrile purity is low.
Summary of the invention
The purpose of the utility model is to provide a kind of dichloroethanes/ethane nitrile wastewater processing unit, can solve dichloroethanes/
Ethane nitrile wastewater separates and recovers the problem that difficulty is big, acetonitrile purity is not high.
The technical solution of the utility model is as follows:
Dichloroethanes/ethane nitrile wastewater processing unit, including extractive distillation column, distillate drum, molecular screen membrane equipment, washing kettle；
Extracting rectifying tower bottom connects reboiler, and top connects tower top first-stage condenser and tower top secondary condenser；Distillate drum includes back
Stream tank, front-end volatiles tank, midbarrel tank, acetonitrile distillate flow container and tails tank；Tower top first-stage condenser and tower top B-grade condensation
Device is connected with return tank import, and return tank outlet is divided into two-way, connects tower top, another way and front-end volatiles tank, midbarrel all the way
Tank, acetonitrile distillate flow container and the respective import of tails tank is separately connected；Front-end volatiles are kept in front-end volatiles tank, and front-end volatiles are main
For dichloroethanes, acetonitrile and water；Acetonitrile distillate is distillated in flow container in acetonitrile and is kept in；Front-end volatiles tank connects washing kettle, washing kettle
Outlet connection dichloroethanes storage tank and water phase storage tank, organic phase are collected in dichloroethanes storage tank, and water phase is received in water phase storage tank
Collection；Acetonitrile distillates flow container outlet connection molecule sieve membrane equipment, separates by membrane module, and water phase enters water phase receiving tank, acetonitrile into
Enter finished pot.
Wherein:
Water is fed as extractive distillation column extractant from the middle and upper part of tower.
Pans outlet is connected with mother liquor tank.The outlet of tails tank is connected with rectifying column.
Molecular screen membrane equipment includes membrane module, evaporator, film feed preheater, film finished product condenser, permeate condenser.
Contain multiple membrane modules in molecular screen membrane equipment, membrane module is serial or parallel connection form.
Washing kettle two, switching uses, and is easily formed stable phase interface.Liquid separating port design in washing kettle bottom has anti-vortex to keep off
Plate, liquid separating port liquid down-comer road are equipped with conductivity meter.
The connect outlet of closed cans and tails tank of water phase storage tank, film water is connected with tower feed preheater respectively, as extraction
Agent is recycled.
The utility model has the advantages that
1, the present apparatus is using extractive distillation column-membrane separation plant-washing kettle joint, and the acetonitrile purity of separation and recovery >=
99.5%, water content≤0.05wt.%.
2, water is as extractant, safety and environmental protection.Compared to conventional method, simple process, low energy consumption.
3, using molecular screen membrane equipment, good separating effect.
4, extractive distillation column completes separation using first continuous, rear interval two ways operation in an extractive distillation column,
Without using two extractive distillation columns, equipment investment is saved.
5, tails tank is set, acetonitrile yield is improved, reduces content of organics in kettle raffinate.
Detailed description of the invention
Fig. 1 is 1 schematic device of embodiment, in which:
E101- reboiler, E102- tower top first-stage condenser, E103- tower top secondary condenser, E104- tower feeding preheating
Device, E105- gaseous effluent cooler, E106- distillate cooler, E107- film feed preheater, E108- film finished product condenser,
E109- evaporator, E110- permeate condenser.
P101- reflux pump, P102- front-end volatiles transfering material pump, P103- acetonitrile distillate transfering material pump, P104- vacuum pump.
V101- return tank, V102- front-end volatiles tank, V103- midbarrel tank, V104- acetonitrile distillate flow container, evaporate after V105-
Point tank, V106- finished pot, V107- film water connect closed cans, V108- dichloroethanes storage tank, V109- water phase storage tank.
T101- rectifying column, S101- washing kettle, N101- molecular screen membrane equipment.
Fig. 2 is 2 schematic device of embodiment, in which:
E101- reboiler, E102- tower top first-stage condenser, E103- tower top secondary condenser, E104- gaseous effluent cooler,
E105- distillate cooler, E106- film feed preheater, E107- film finished product condenser, E108- evaporator, E109- penetrating fluid
Condenser.
P101- reflux pump, P102- front-end volatiles transfering material pump, P103- acetonitrile distillate transfering material pump, P104- vacuum pump.
V101- return tank, V102- front-end volatiles tank, bis- rectifying front-end volatiles tanks of V103-, bis- rectifying tails of V104-
Tank, V105- midbarrel tank, V106- acetonitrile distillate flow container, V107- tails tank, V108- finished pot, and V109- film water connects
Closed cans, V110- dichloroethanes storage tank, V111- water phase storage tank.
T101- rectifying column, S101- washing kettle, N101- molecular screen membrane equipment.
Specific embodiment
The present invention is done below with reference to embodiment and is further explained.The following example is merely to illustrate the present invention, but
It is not used to limit practical range of the invention.
Dichloroethanes/ethane nitrile wastewater processing unit, including extractive distillation column, distillate drum, molecular screen membrane equipment, washing kettle；
Extracting rectifying tower bottom connects reboiler, and top connects tower top first-stage condenser and tower top secondary condenser；Distillate drum includes back
Stream tank, front-end volatiles tank, midbarrel tank, acetonitrile distillate flow container and tails tank；Tower top first-stage condenser and tower top B-grade condensation
Device is connected with return tank import, and return tank outlet is divided into two-way, connects tower top, another way and front-end volatiles tank, midbarrel all the way
The import that tank, acetonitrile distillate flow container and tails tank is separately connected；Front-end volatiles are kept in front-end volatiles tank, and front-end volatiles are mainly two
Chloroethanes, acetonitrile and water；Acetonitrile distillate is distillated in flow container in acetonitrile and is kept in；Front-end volatiles tank connects washing kettle, washing kettle outlet
Connection dichloroethanes storage tank and water phase storage tank, organic phase are collected in dichloroethanes storage tank, and water phase is collected in water phase storage tank；Second
Nitrile distillates flow container outlet connection molecule sieve membrane equipment, separates by membrane module, water phase enters water phase receiving tank, and acetonitrile enters finished product
Tank.
Wherein, water is fed as extractive distillation column extractant from the middle and upper part of tower.Pans outlet is connected with mother liquor tank.
The outlet of tails tank is connected with rectifying column.Molecular screen membrane equipment includes membrane module, evaporator, film feed preheater, and film finished product is cold
Condenser, permeate condenser.Contain multiple membrane modules in molecular screen membrane equipment, membrane module is serial or parallel connection form.Washing kettle two
Platform, switching use, and are easily formed stable phase interface.Washing kettle bottom liquid separating port, which designs, anti-swirl baffle, under liquid separating port liquid
It drops pipeline and conductivity meter is housed.The connect outlet difference rectifying column of closed cans and tails tank of water phase storage tank, film water is connected, as extraction
Agent is taken to be recycled.
Embodiment 1
As shown in Figure 1, acetonitrile/dichloroethanes is delivered in reboiler E101 through tower feed pump, the middle and upper part rectifying column T101
Extractant (process water) is continuously conveyed to enter in tower, the continuous operation of rectifying column T101 normal pressure, after infinite reflux stable operation, rectifying
Extraction front-end volatiles steam in the top tower T101 flows into back after tower top first-stage condenser E102 and tower top secondary condenser E103 condensation
It flows in tank V101, is conveyed through reflux pump P101, is partly refluxed at the top of rectifying column T101, another part passes through distillate cooler
E106 is produced into front-end volatiles tank V102, and content of organics≤0.05wt.% waste water is continuously discharged in tower reactor.Rectifying column T101 is set
There is tower feed preheater E104.Solvent quantity is definite value when continuous extraction distillation operation, and mother liquor amount mass ratio about 1:
1.After charging, rectifying column T101 switchs to batch fractionating, acetonitrile of the overhead extraction containing a small amount of dichloroethanes by continuous rectification
Steam, extraction is into midbarrel tank V103 after condensing.As dichloroethane content≤0.5wt.% in return tank of top of the tower V101
Afterwards, tower top start collect acetonitrile distillate to acetonitrile distillate in flow container V104.When acetonitrile distillate water content is higher than 20wt.%
Distillate switches to tails tank V105, stops distillation operation in tower reactor waste water when ethane nitrile content < 0.1wt.%, and tower reactor discharge is useless
Water is cooling through tower feed preheater E104 and gaseous effluent cooler E105.Midbarrel composition is close with mother liquor, is back to mother liquor tank,
Extracting rectifying operation is carried out again.The a certain amount of laggard rectifying column T101 of tails accumulation concentrates dehydration.
Dichloroethanes distillate is delivered in washing kettle S101 by front-end volatiles transfering material pump P102, and the water that 4 times of quality are added carries out
Layering, the bottom washing kettle S101 are discharged organic phase and water phase, are stored respectively to dichloroethanes storage tank V108 and water phase storage tank V109.
Organic phase composition about dichloroethanes 81wt.%, acetonitrile 18wt.%, water 1wt.%.Water phase forms about dichloroethanes 1wt.%, acetonitrile
7wt.%, water 92wt.% can also enter tails tank V105 and accumulate directly as extractive distillation column T101 extractant reuse
Processing.
Acetonitrile distillates the distillate in flow container V104 and is delivered to film feed preheater by acetonitrile distillate transfering material pump P103
E107 be preheated to about 70-80 DEG C after enter evaporator E109, about 110 DEG C of evaporator E109 outlet steam temperature, through superheater mistake
Heat enters molecular screen membrane equipment N101, complete equipment operating pressure about 0.2MPa(G to 125 DEG C in the form of superheated steam), film
Component is by 7 10m2Component is in series.Moisture and a small amount of acetonitrile in raw material infiltrate into downstream by upstream side through membrane module
Side, film upstream side obtain water content≤0.05wt.% acetonitrile finished product.Take the mode for vacuumizing plus condensing with shape in film downstream side
The vapor partial pressure for the upstream and downstream two sides component that forms a film is poor.Prime osmotic lateral pressure is 3KPa, and rear class osmotic lateral pressure is 500Pa.It seeps
Transparent liquid steam enters permeate condenser E110 under vacuum pump set suction, and condensed penetrating fluid is back to film water and connects closed cans
V107, as extractive distillation column T101 extractant reuse.Air into system is leaked by vacuum pump P104 extraction.It is dehydrated finished product warp
It stores after crossing film feed preheater E107 and film finished product condenser E108 heat exchange to finished pot V106.Each material composition is shown in Table 1 institute
Show.
Table 1 mainly flows stock ingredient and content
。
Embodiment 2
As shown in Fig. 2, acetonitrile/dichloroethanes is delivered in reboiler E101 through tower feed pump, between rectifying column T101 normal pressure
It has a rest operation, conveying extractant (process water) enters the middle and upper part rectifying column T101 after tower middle portion temperature rises, and stablizes through infinite reflux and grasps
After work, extraction front-end volatiles steam in the top rectifying column T101 is condensed through tower top first-stage condenser E102 and tower top secondary condenser E103
Afterwards, it flows into return tank V101, is conveyed through reflux pump P101, is partly refluxed at the top of rectifying column T101, another part is by evaporating
Liquid cooler E106 is produced into front-end volatiles tank V102 out, and rectifying distillate switches to after ethane nitrile content rises in return tank of top of the tower
In midbarrel tank V105.After dichloroethane content≤0.5wt.% in return tank of top of the tower V101, tower top starts collection acetonitrile and evaporates
Liquid to acetonitrile distillates in flow container V106 out.When acetonitrile distillate water content is higher than 20wt.%, distillate switches to tails tank
V107 stops distillation operation in tower reactor waste water when ethane nitrile content < 0.1wt.%, it is cold through gaseous effluent cooler E104 that waste water is discharged in tower reactor
But.Front-end volatiles are again introduced into extractive distillation column T101 after accumulating several, tower top is first collected secondary rectifying front-end volatiles, produced afterwards secondary
Rectifying tails, secondary front-end volatiles are collected in secondary rectifying front-end volatiles tank V103, are conveyed by secondary front-end volatiles transfering material pump P102
Into washing kettle S101, the water that 4 times of quality are added is layered, and organic phase and water phase is discharged in the bottom washing kettle S101, is stored up respectively
It deposits to dichloroethanes storage tank V110 and water phase storage tank V111.Organic phase composition about dichloroethanes 87.3wt.%, acetonitrile 6.6wt.%,
Water 6.2wt.%.Water phase forms about dichloroethanes 0.6wt.%, acetonitrile 2.8wt.%, water 96.6wt.%, can be directly as extracting rectifying
Tower T101 extractant reuse；The feed liquid of secondary rectifying tails tank V104 and midbarrel tank V105 is back to mother liquor tank, again
Carry out extracting rectifying operation.Tails is as extractive distillation column T101 extractant reuse.
Acetonitrile distillates the distillate in flow container V106 and is delivered to film feed preheater by acetonitrile distillate transfering material pump P103
E106 be preheated to about 70-80 DEG C after enter evaporator E108, about 110 DEG C of evaporator E108 outlet steam temperature, through superheater mistake
Heat enters molecular screen membrane equipment N101, complete equipment operating pressure about 0.38MPa(G to 125 DEG C in the form of superheated steam),
Membrane module is by 7 10m2Modules in parallel is constituted.Moisture and a small amount of acetonitrile in raw material are infiltrated into down through membrane module by upstream side
Side is swum, film upstream side obtains water content≤0.05wt.% acetonitrile finished product.Film downstream side take vacuumize plus condensation mode with
The vapor partial pressure for forming film upstream and downstream two sides component is poor.Prime osmotic lateral pressure is 3KPa, and rear class osmotic lateral pressure is 500Pa.
Penetrating fluid steam enters permeate condenser E109 under vacuum pump set suction, and condensed penetrating fluid is back to film water Phase Receiver
Tank V109, as extractive distillation column T101 extractant reuse.Air into system is leaked by vacuum pump P104 extraction.It is dehydrated finished product
It stores after film feed preheater E106 and film finished product condenser E107 heat exchange to finished pot V108.Each material composition is shown in Table 2
It is shown.
Table 2 mainly flows stock ingredient and content
Claims (8)
1. dichloroethanes/ethane nitrile wastewater processing unit, it is characterised in that: set including extractive distillation column, distillate drum, molecular screen membrane
Standby, washing kettle；Extracting rectifying tower bottom connects reboiler, and top connects tower top first-stage condenser and tower top secondary condenser；It evaporates
Point tank includes that return tank, front-end volatiles tank, midbarrel tank, acetonitrile distillate flow container and tails tank；Tower top first-stage condenser and tower
Top secondary condenser is connected with return tank import, and return tank outlet is divided into two-way, connects tower top, another way and front-end volatiles all the way
Tank, midbarrel tank, acetonitrile distillate flow container and the respective import of tails tank is separately connected；Front-end volatiles are temporary in front-end volatiles tank
It deposits, front-end volatiles are mainly dichloroethanes, acetonitrile and water；Acetonitrile distillate is distillated in flow container in acetonitrile and is kept in；The connection of front-end volatiles tank
Washing kettle, washing kettle outlet connection dichloroethanes storage tank and water phase storage tank, organic phase are collected in dichloroethanes storage tank, and water phase exists
It is collected in water phase storage tank；Acetonitrile distillates flow container outlet connection molecule sieve membrane equipment, separates by membrane module, water phase enters water phase and connects
Closed cans, acetonitrile enter finished pot.
2. dichloroethanes according to claim 1/ethane nitrile wastewater processing unit, it is characterised in that: water is as extracting rectifying
Tower extractant is fed from the middle and upper part of tower.
3. dichloroethanes according to claim 1/ethane nitrile wastewater processing unit, it is characterised in that: pans outlet and mother
Flow container is connected.
4. dichloroethanes according to claim 1/ethane nitrile wastewater processing unit, it is characterised in that: molecular screen membrane equipment packet
Containing membrane module, evaporator, film feed preheater, film finished product condenser, permeate condenser.
5. dichloroethanes according to claim 1/ethane nitrile wastewater processing unit, it is characterised in that: in molecular screen membrane equipment
Containing multiple membrane modules, membrane module is serial or parallel connection form.
6. dichloroethanes according to claim 1/ethane nitrile wastewater processing unit, it is characterised in that: washing kettle two, switching
It uses, is easily formed stable phase interface.
7. dichloroethanes according to claim 1/ethane nitrile wastewater processing unit, it is characterised in that: water phase storage tank, film water phase
Receiving tank and tails tank are connected with rectifying column, can not only be used for extractant recycling, can also slightly steam receipts acetonitrile.
8. dichloroethanes according to claim 1/ethane nitrile wastewater processing unit, it is characterised in that: the liquid separation of washing kettle bottom
Mouth design has anti-swirl baffle, and liquid separating port liquid down-comer road is equipped with conductivity meter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821916615.9U CN209161729U (en) | 2018-11-20 | 2018-11-20 | A kind of dichloroethanes/ethane nitrile wastewater processing unit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821916615.9U CN209161729U (en) | 2018-11-20 | 2018-11-20 | A kind of dichloroethanes/ethane nitrile wastewater processing unit |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN209161729U true CN209161729U (en) | 2019-07-26 |
Family
ID=67339129
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201821916615.9U Active CN209161729U (en) | 2018-11-20 | 2018-11-20 | A kind of dichloroethanes/ethane nitrile wastewater processing unit |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN209161729U (en) |
-
2018
- 2018-11-20 CN CN201821916615.9U patent/CN209161729U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105418368B (en) | A kind of technique and device for producing high straight alcohol | |
| CN106431812A (en) | Method and device for separating methylbenzene-methanol-water azeotrope using extractive distillation | |
| CN105218317B (en) | The method and device that ethanol is reclaimed in a kind of hexanitrobibenzyl production | |
| CN106178571B (en) | Azeotrope separation process | |
| CN109231635A (en) | A kind of dichloroethanes/ethane nitrile wastewater New Process for Treatment | |
| CN110938047A (en) | Tetrahydrofuran-benzene-water mixture separation process and device | |
| CN104109078B (en) | A kind of method that in Sulpyrine production, ethanol reclaims | |
| CN110862330B (en) | Efficient energy-saving rectification process for recycling DMAC waste liquid | |
| CN107073353A (en) | The improvement related to oxirane recovery | |
| CN104926690B (en) | The recovery process for purification and device of acetonitrile in a kind of synthesis for Ceftriaxone Sodium | |
| CN106045872A (en) | System for recovering DMF (dimethylformamid) waste liquor with pervaporation method and method | |
| CN107998677B (en) | Environment-friendly cleaning device and process method for solvent recovery | |
| CN104193651A (en) | Refining method and device for synthesizing acetonitrile from acetic acid by ammoniation | |
| CN111517920B (en) | Process for separating tetrahydrofuran-methanol-water by three-tower batch rectification | |
| CN209161729U (en) | A kind of dichloroethanes/ethane nitrile wastewater processing unit | |
| CN104844420B (en) | The continuous treatment technique of neopentyl glycol condensation water cleaning mother liquor and device | |
| CN107998678B (en) | Environment-friendly cleaning device and process method for separating organic azeotrope | |
| CN205412296U (en) | Continuous rectification plant of nitromethane | |
| CN204727810U (en) | A kind of purification and recover device for acetonitrile in ceftriaxone sodium synthesis | |
| CN111909120B (en) | Energy-saving separation process of water-containing ternary azeotropic system | |
| CN113559536A (en) | System and method for recycling methanol from waste organic solvent | |
| CN106187767A (en) | A kind of process for purification and device removing alcohol for the dehydration of packages printing industry ethyl acetate waste liquid | |
| CN206940774U (en) | A kind of tetrahydrofuran dehydration device | |
| CN112694404A (en) | Method and device for purifying vinyl acetate in EVOH production process | |
| CN216798744U (en) | Intermittent rectification and purification device for dimethyl sulfoxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |