CN207158995U - Ethane nitrile wastewater processing and recovery system - Google Patents
Ethane nitrile wastewater processing and recovery system Download PDFInfo
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- CN207158995U CN207158995U CN201720707896.6U CN201720707896U CN207158995U CN 207158995 U CN207158995 U CN 207158995U CN 201720707896 U CN201720707896 U CN 201720707896U CN 207158995 U CN207158995 U CN 207158995U
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Abstract
The utility model discloses a kind of processing of ethane nitrile wastewater and recovery system, including feed liquid pond, membrane separation device, condenser system, collecting tank, described feed liquid pond, membrane separation device, collecting tank are linked in sequence successively, and described collecting tank is provided with condenser system.The processing of ethane nitrile wastewater described in the utility model and recovery system can operate under low temperature, and temperature control is in normal temperature~60 DEG C, than sequence of constant boiling and rectification energy-conservation 1/2~2/3；And the decorum processing procedure is simple, system reliability and stability are higher, are advantageous to the industrialization of the recycling of ethane nitrile wastewater.
Description
Technical field
The processing of ethane nitrile wastewater and returned the present invention relates to a kind of Waste Water Treatment, more particularly in perfluor ketone production process
Receipts system, belongs to technical field of waste water processing.
Background technology
Perfluor ketone (C3F6O one industrial wastewater for containing high concentration acetonitrile, the typical water quality of waste water) are produced in production process
It is as follows：
| Sequence number | Test event | Unit | Scope | Certain water sample |
| 1 | pH | — | 2~9 | 4.92 |
| 2 | COD | mg/L | 10000~60000 | 17556.0 |
| 3 | BOD5 | mg/L | 200~6000 | 1419.8 |
| 4 | Acetonitrile | mg/L | 4000~45000 | 10348 |
| 5 | NH4 +-N | mg/L | 5~100 | 15.39 |
| 6 | TN | mg/L | 1000~20000 | 3749 |
| 7 | NO3 - | mg/L | 100~3000 | 582.2 |
| 8 | TDS | mg/L | 35000~400000 | 110000 |
| 9 | Solid content | % | 2~40 | 11.24 |
| 10 | Cl- | mg/L | 35000~500000 | 62841.5 |
| 11 | NO3 - | mg/L | 100~3000 | 582.2 |
| 12 | SO4 2- | mg/L | 200~6000 | 1348.2 |
| 13 | Na+ | mg/L | 7000~300000 | 47363.5 |
Ethane nitrile wastewater be poisonous organic industry sewage, it is necessary to carry out harmless treatment, next stage process could be entered or reached
Mark discharge.
The processing method of ethane nitrile wastewater mainly has the way of distillation, extraction, combustion method, Hydrolyze method and chemical oxidization method (to contain and urge
Change oxidation), the materilization freatment method such as electrolysis and biochemical method processing etc..The method of materializing strategy, ordinary disbursements are higher, simultaneously
Produce secondary pollution.The method of biological treatment, have usually using aerobic method to organonitrile compound processing, organonitrile compound
High toxicity, aerobic bioprocess would generally be limited；Aerobic method processing needs to be aerated, due to the height volatilization of organonitrile compound
Property, the stripping that can accelerate acetonitrile is aerated, acetonitrile is corresponding carboxylic acid and ammonia after domestication by Aerobic biological process, and carboxylic acid can enter
One step is oxidized to carbon dioxide and water.For the ethane nitrile wastewater of high concentration, the another question of Aerobic Process for Treatment is to produce
The ammonia nitrogen of high concentration, nitrification and denitrification process greatly add processing cost.In addition, the salt containing high concentration in waste water
Class, it also limit the application of biochemical treatment.
Patent CN101492391 discloses a kind of process extracted with rectifying separating ethane nitrile wastewater with combination, by second
Dichloromethane is added in nitrile waste water as extractant, after extracting stratification, upper strata raffinate phase is water, a small amount of acetonitrile, dichloromethane
Alkane, lower floor's extraction phase are dichloromethane, acetonitrile and a small amount of water.Lower floor's extraction phase is put into distillation system batch process, upper strata extraction
Remaining phase will also be put into distillation system processing, and a small amount of acetonitrile and dichloromethane are evaporated, the ethane nitrile content energy finally produced
Up to 99.5%, moisture is below 0.08%.The above method needs to use extractant, can bring new pollutant into.Duan Wanjun
(simulated wastewater [J] science and technology and engineering of the electrolysis of the iridium tantalum coatings such as Duan Wanjun, Chai Tao, Feng Yiwei dimensional stable anode containing acetonitrile,
2016,16(27):312-315) et al. employ iridium tantalum coating dimensional stable anode and carry out efficient degraded acetonitrile method, find when applying
The degradation effect of electrode pair acetonitrile of the layer containing iridium tantalum titanium elements is best, pH 6.60, and concentration is to contain 1.32ml per in 500ml water
Acetonitrile, voltage 4.10v, degradation rate is up to 69.0%.Above-mentioned electrolytic method energy consumption is very high, and removal efficiency only has
69%.Believe (letter prestige roc, the Zou Jie such as prestige roc；The Fenton reagent processing experimental study of pharmaceutical wastewater containing acetonitrile Liaoning chemical industry vol41
(5) 2,012 440~441) pharmaceutical wastewater containing acetone, acetonitrile and dichloromethane, reaction condition are contained using Fenton reagent processing
It is as follows：PH is 8~9；Reaction time is 60min；Ferrous sulfate dosage：2.5g/L；Hydrogen peroxide dosage：15mL/L.System
88% can be reached to the highest clearance of ethane nitrile wastewater.The above method will add substantial amounts of chemical agent, the use of hydrogen peroxide
Potential safety hazard be present.Applying Zheng Yu et al. (Tu Zhengyu, Xia Jun, Sun Yuchun, waits acetonitrile waste liquid osmotic, evaporating and dewatering processes to set
Meter, Nankai University's journal (natural science edition), 2,014 10 (6):53-58), handled with infiltration evaporation and the combined process of rectifying
Ethane nitrile wastewater has carried out design and calculated.When inlet amount is 100kg/h, using veneer, serial operation, series are infiltration evaporation step by step
31 grades, membrane area 12.4m2；In rectification working process, theoretical cam curve is 30 pieces, and pre-rectifying tower optimal point of operation reflux ratio is
0.5, feed tray is 11 layers, finished product rectifying column optimal point of operation reflux ratio 3.0, during 12 layers of feed tray, the product water of acetonitrile
Divide≤0.01%.The above method is the maturation process being dehydrated in acetonitrile.
Patent ZL200610095052.7 discloses a kind of processing method of difficult degradation nitrile contained organic sewage, contains in waste water
The difficult degradation such as hydroxyacetonitrile, aniline-acetonitrile organic matter containing nitrile, waste water are carried out using Fe-C weak electrolysis mechanisms in acid condition
Processing, adds ferrous sulfate and lime carries out precipitation process.In foregoing invention Fe-C light electrolysis post in use by
In Fe consumption, it may occur that hollow and percolation phenomenon, i.e. waste water flow directly out without Fe-C filler, another part Fe-C
The phenomenon of solidification caking can occur for post, be connected as a single entity with reactor, it is difficult to mobile.In addition, waste water after above-mentioned PROCESS FOR TREATMENT, is gone back
Substantial amounts of precipitation can be produced, turns into dangerous solid waste, it is necessary to be further processed.Treatment effect is bad in the invention,
Only 40% or so clearance.
The content of the invention
In order to overcome the shortcomings of above-mentioned technology, the purpose of this utility model is to provide the processing and recovery of a kind of ethane nitrile wastewater
Acetonitrile in waste water can be separated and removed by system, the system with salt, 5~20 times of isolated acetonitrile enrichment, be expected to realize
Reclaim acetonitrile.
To realize the above object, the utility model will take following technical scheme：
A kind of processing of ethane nitrile wastewater and recovery system, including feed liquid pond, membrane separation device, condenser system, collecting tank, institute
The feed liquid pond stated, membrane separation device, collecting tank are linked in sequence successively, and described collecting tank is provided with condenser system.
Further, described feed liquid pond passes sequentially through peristaltic pump and flowmeter and is connected with membrane separation device side.
Further, described collecting tank is connected by conveyance conduit with membrane separation device opposite side.
Further, vavuum pump is set on described collecting tank.
Further, described membrane separation device is made up of single membrane module.
Further, described membrane separation device is made up of the mode of multiple membrane module series, parallel or serial-parallel mirror.
Further, membrane module includes film, supporter, inlet tube and outlet, wherein, film be configured as doughnut or
Tubular structure, membrane material select hydrophobic non-porous infiltration evaporation membrane material, the preferably films of Switzerland Sulzer Pervap 4060
With the ceramic PDMS composite membranes of the Si Mo Science and Technology Ltd.s of Nanjing nine.
Further, described condenser system uses ice-water bath, ice salt bath or liquid nitrogen.
The running of said system is as follows：Ethane nitrile wastewater in perfluor ketone production process is continuously circulated through UF membrane
Device, while will transmit through with vavuum pump the acetonitrile steam of film in the opposite side of membrane separation device and be continuously pumped into collecting tank；Continuously
After operation 3~10 hours, collector is taken out, places 10~20min at normal temperatures, collector bottom is the liquid of acetonitrile.
Further, vacuum is maintained in acetonitrile collector, absolute pressure is 10~7000Pa.
Compared with prior art, the utility model has following beneficial effect：
(1) efficiently：The utility model expeditiously can separate acetonitrile and salt solution, and the salinity permeated in condensate liquid is 0,
Acetonitrile clearance in raw wastewater is more than 92%, and single-stage is with regard to that can reach very high separating degree.If using hydrophobic porous membrane material
Material, vaporization side can obtain concentrating more than 5 times of condensate liquid；Acetonitrile concentration reaches 5~20%；Using non-porous infiltration evaporation membrane material
Material, vaporization side can obtain concentrating more than 10 times of condensate liquid, and acetonitrile concentration reaches 5~60%.
(2) energy consumption is low：The recovery system that the utility model uses operates under low temperature, and temperature control is in normal temperature~60
DEG C, typically than sequence of constant boiling and rectification energy-conservation 1/2~2/3.
(3) recovery system of the present utility model is used, process is simple, and the reliability and stability of system are higher, are advantageous to
The industrialization of the recycling of ethane nitrile wastewater.
Brief description of the drawings
Fig. 1 is processing and the structural representation of recovery system of ethane nitrile wastewater described in the utility model.
Fig. 2 is acetonitrile concentration and the graph of relation of processing time in waste water described in the utility model.
Embodiment
The embodiment of the present invention is described in further detail below by specific embodiments and the drawings.
Principle of the present utility model is：Using film as contact medium, waste water is continuously circulated through membrane separation device, waste water
With a side contacts of membrane separation device, to be depressurized in the opposite side of membrane separation device, acetonitrile diffusion or dissolving diffuse through film medium,
Into in the collector of opposite side, collector keeps low temperature, and the acetonitrile and water vapour that diffusion and dissolving diffuse through are in low temperature
Condensation is as the solution of acetonitrile in collector, and according to the selective difference of membrane material, condensate liquid compares raw wastewater concentration 5~30
Times.Wherein, membrane material can use infiltrating and vaporizing membrane (such as PDMS membrane materials, the molecular screen membrane to acetonitrile with fine selectivity energy
Material, polyether-block-polyamide membrane material etc.).Acetonitrile is enriched with from weak solution, passes through infiltrating and vaporizing membrane under ultralow vacuum
The content of acetonitrile steam can reach more than 20%, in by frozen water or the acetonitrile collector of liquid nitrogen cooling, acetonitrile steam and water
Steam is condensed into as liquid or solid.Acetonitrile collector is taken out a period of time, the knot containing partial acetonitrile are placed under normal temperature
Brilliant water is dissolved as the bottom that acetonitrile solution is gathered in collector.
Such as Fig. 1, the processing of the ethane nitrile wastewater described in utility model and recovery system, including feed liquid pond 1, peristaltic pump 2, valve
3rd, flowmeter 4, membrane separation device 5, conveyance conduit 6, collecting tank 7, ice-water bath 8 and vavuum pump 9, feed liquid pond 1 and membrane separation device 5
Side be linked in sequence successively peristaltic pump 2, valve 3, flowmeter 4, collecting tank 7 sets ice-water bath 8, and connects vavuum pump 9, collects
Tank 7 is connected with the opposite side of membrane separation device 5 by conveyance conduit 6, and pressure vacuum gauge is provided with conveyance conduit 6.
The processing method of ethane nitrile wastewater, specifically comprises the following steps in perfluor ketone production process described in the utility model：
(1) the perfluor ketone waste water containing acetonitrile and high salinity is placed in material liquid tank 1, certain temperature is controlled, through entering peristaltic pump 2
Circulated in membrane separation device 5, valve 3 and flowmeter 4 can control the wastewater flow of waste water；
(2) perfluor ketone waste water in the circulating cycle, acetonitrile steam therein and part water vapor diffusion or dissolving diffuse through
Membrane separation device 5, the component for penetrating membrane separation device 5 are continuously fed into conveyance conduit 6 by the control pressure of vavuum pump 9,
Finally enter in collecting tank 7, collecting tank 7 sets ice-water bath 8, and acetonitrile steam and water vapour are condensed into collecting tank 7 as liquid
Body or solid, collecting tank 7 are taken out a period of time are placed under normal temperature, and the crystallization water containing partial acetonitrile is dissolved as acetonitrile solution and gathered
Collection is in the bottom of collecting tank 7.
Embodiment 1
It is 12327mg/L by concentration, the perfluor ketone 1L containing ethane nitrile wastewater that salt content is 20% is placed in wide-mouth bottle, passes through water
Bath is heated to 40 DEG C, solution is circulated into injection membrane separation device 5 with peristaltic pump 2, the membrane material used in membrane separation device 5 is auspicious
The infiltrating and vaporizing membranes of scholar Sulzer Pervap 4060, while the entrance of vavuum pump 9 is connected with collecting tank 7 and will transmit through the second of film
Nitrile steam is continuously pumped into, and maintains the vacuum in collecting tank 7 to be less than 20mbar, and temperature is less than 0 DEG C, after continuously running 3 hours, given up
Acetonitrile concentration in water is down to below 400mg/L, takes out collecting tank 7, after placing at room temperature, weighs, obtains 40g 30% second
The nitrile aqueous solution.
Embodiment 2
The acetonitrile solution 1L that concentration is 15012mg/L is placed in wide-mouth bottle, by heating water bath to 40 DEG C, uses peristaltic pump
Solution is circulated injection membrane separation device 5 by 2, and the membrane material used in membrane separation device 5 is the Si Mo Science and Technology Ltd. of Nanjing nine
Ceramic PDMS composite membranes, while the entrance of vavuum pump 9 is connected with collecting tank 7 and will transmit through the acetonitrile steam of film and is continuously taken out
Enter, maintain the vacuum in collecting tank 7 to be less than 15mbar, continuous operation takes out collecting tank 7 after 4 hours, after placing at room temperature, claims
Weight, obtains 58g 26.9% acetonitrile solution, and the acetonitrile concentration in waste water drops to below 100mg/L.
Embodiment 3
The acetonitrile solution 1L that concentration is 5913mg/L is placed in wide-mouth bottle, by heating water bath to 40 DEG C, with peristaltic pump 2
Solution is circulated into injection membrane separation device 5, the membrane material used in membrane separation device 5 oozes for Switzerland Sulzer Pervap 4060
Vaporization film thoroughly, while the entrance of vavuum pump is connected with collecting tank 7 and will transmit through the acetonitrile steam of film and is continuously pumped into, maintain collection
Vacuum in tank 7 is less than 35mbar, and continuous operation takes out collecting tank 7 after 2 hours, after placing at room temperature, weighs, obtains 30g
17.2% acetonitrile solution.Now the acetonitrile solution concentration in waste water is about 400mg/L, then is injected waste water with peristaltic pump 2
Membrane separation device 5, continue to run with 1 hour, the acetonitrile concentration in waste water drops to below 20mg/L.
Fig. 2 be acetonitrile initial concentration be 12327mg/L waste water, acetonitrile concentration versus time curve, raw wastewater second
Nitrile concentration be 12327mg/L waste water, circulated by membrane treatment appts, wastewater treatment after 2 hours acetonitrile concentration drop to 2265mg/
L, acetonitrile concentration drops to 72mg/L after 4 hours.
Claims (9)
1. ethane nitrile wastewater processing and recovery system, it is characterised in that including feed liquid pond, membrane separation device, condenser system, collection
Tank, described feed liquid pond, membrane separation device, collecting tank are linked in sequence successively, and described collecting tank is provided with condenser system.
2. the system as claimed in claim 1, it is characterised in that described feed liquid pond passes sequentially through peristaltic pump and flowmeter and film
Separator side connects.
3. the system as claimed in claim 1, it is characterised in that described collecting tank is another with membrane separation device by conveyance conduit
Side connects.
4. the system as claimed in claim 1, it is characterised in that be provided with vavuum pump on described collecting tank.
5. the system as claimed in claim 1, it is characterised in that described membrane separation device is made up of single membrane module.
6. the system as claimed in claim 1, it is characterised in that described membrane separation device is by multiple membrane module series, parallel
Or the mode of serial-parallel mirror forms.
7. the system as described in claim 5 or 6, it is characterised in that membrane module includes film, supporter, inlet tube and outlet,
Wherein, film is configured as doughnut or tubular structure, and membrane material is from hydrophobic nonporous vaporization membrane material.
8. system as claimed in claim 7, it is characterised in that membrane material selects the films of Switzerland Sulzer Pervap 4060 or south
The ceramic PDMS composite membranes of Jing Jiusimo Science and Technology Ltd.s.
9. the system as claimed in claim 1, it is characterised in that described condenser system uses ice-water bath, ice salt bath or liquid
Nitrogen.
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| CN201720707896.6U CN207158995U (en) | 2017-06-16 | 2017-06-16 | Ethane nitrile wastewater processing and recovery system |
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| CN201720707896.6U CN207158995U (en) | 2017-06-16 | 2017-06-16 | Ethane nitrile wastewater processing and recovery system |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109113159A (en) * | 2018-10-11 | 2019-01-01 | 盐城道泽环保科技有限公司 | A kind of reverse-flow type exempts from automatically controlling liquid transportation integration apparatus |
| CN109231635A (en) * | 2018-11-20 | 2019-01-18 | 江苏九天高科技股份有限公司 | A kind of dichloroethanes/ethane nitrile wastewater New Process for Treatment |
| CN111302422A (en) * | 2020-03-12 | 2020-06-19 | 上一环保科技（杭州）有限公司 | Concentration and reduction device and method for high-salt high-concentration organic wastewater |
-
2017
- 2017-06-16 CN CN201720707896.6U patent/CN207158995U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109113159A (en) * | 2018-10-11 | 2019-01-01 | 盐城道泽环保科技有限公司 | A kind of reverse-flow type exempts from automatically controlling liquid transportation integration apparatus |
| CN109231635A (en) * | 2018-11-20 | 2019-01-18 | 江苏九天高科技股份有限公司 | A kind of dichloroethanes/ethane nitrile wastewater New Process for Treatment |
| CN109231635B (en) * | 2018-11-20 | 2023-05-09 | 江苏九天高科技股份有限公司 | Wastewater treatment process |
| CN111302422A (en) * | 2020-03-12 | 2020-06-19 | 上一环保科技（杭州）有限公司 | Concentration and reduction device and method for high-salt high-concentration organic wastewater |
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