CN101417208A - Extractive agent recovering method in water phase using film isolation technique - Google Patents
Extractive agent recovering method in water phase using film isolation technique Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention provides a method used for recovering extractant in water phase by film separation technique; the water phase is defined as entrainment flowing out of an extraction system and extraction raffinate and strip liquor where the extractant is dissolved; diluent used in water phase and the extraction system respectively flows at two sides of the film; by the adsorption of the film material on the extractant and the extraction of the diluent on the extractant, the extractant is transferred from the water phase to diluent phase. During practical operation, the flowing speed of the water phase has large influence on the separation effect and directly decides the disposal quantity; furthermore, the flowing speed of the diluent has relatively small influence; the pressure difference between the water phase and the diluent phase keeps in proper range; and the diluent rich in extractant can be re-used for recovering the extractant and can be also returned to the organic phase of the extraction system.
Description
Background technology
The present invention relates to the method that a kind of aqueous phase from solvent extraction system reclaims extractant.
In fields such as petrochemical industry, metallurgy, wastewater treatment, obtained using widely as the solvent extraction technology of a unit process.General extracting operation comprises extraction and two stages of back extraction.By extraction process, extract is transferred to the organic facies from water, and the water after extraction is called extraction raffinate; Back extraction is that the organic facies with the enrichment extract contacts with the another one water, and the extract in the organic facies is separated, and organic facies obtains regeneration and enter extracting system recycling, and enrichment the water of extract be called as strip liquor.In the method, comprise extraction raffinate and strip liquor two parts as the water of handling object.
In the actual extraction process, need adopt internals and energy input for improving mass-transfer efficiency, so water is very serious to carrying secretly of organic facies, can cause the pollution of water, and will constantly be supplemented with the machine phase.In extraction process, the expense of organic facies loss generally accounts for about 10% of product cost.Production with copper is example, and practice confirms for many years both at home and abroad: the loss of organic facies accounts for 10% of smelting copper totle drilling cost.Wherein, water carries secretly and dissolves and account for 46% of organic facies evapotranspiration.
From the process reaction of chemical extraction, extractant can be divided three classes: acidic extractant (as di-(2-ethylhexyl)phosphoric acid, i.e. P204), basic extractant (as trioctylamine) and neutral extractant (as tributyl phosphate, i.e. TBP).In chemical extraction, extractant is to be dissolved in the organic facies that is configured for solvent extraction system in the diluent, and the main effect of diluent is a rerum natura of improving organic facies, as density, viscosity etc.Diluent is and the not miscible liquid flux of water the complex that its energy dissolution extraction agent and extractant and the solute that is extracted form.The example of diluent comprises: kerosene, normal heptane, toluene, dimethylbenzene, ethylene dichloride etc.
From the above mentioned as can be known, in the extraction process, solution not only has extractant with after organic facies contacts in extraction raffinate and the strip liquor, also has diluent.Though most of extractants belong to low toxicity or non-toxic type material, if enter environment, still can pollute natural stream networks, as increasing discharge water chemical oxygen consumption (COC) etc.In addition, the extractant that aqueous phase is carried secretly may impact next step flow process, and the extractant of carrying secretly as extraction raffinate returns the rubber lining of understanding the corrosion leaching tanks when leaching again; The organic facies that strip liquor is taken away tends to be deposited on the electrolytic element, pollutes electrolytic element, influences the quality of product.Therefore, reclaim extractant in the solvent-extracted actual production and mainly contain three purposes: reduce investment cost, reduce the pollution of environment and guarantee product quality.
Many extractants in actual production with physical method recovery aqueous phase, the simplest method is a defecator after adding again behind the defecator, increases settling time; This method is consuming time longer, and efficient is low; To stable emulsion, effect is bad during if any surfactant.Size droplet diameter during less than 100 microns the simple settled process that uses be difficult to phase-splitting, need to adopt additive method, as absorption method, floatation, fibre deposition bed, lamella knockouts, filtration method etc.In the absorption method, active carbon and polystyrene resin are often used as adsorbent, but the extractant that is adsorbed is difficult for recovery, and the regeneration of adsorbent is very difficult, and the treating capacity of adsorption column is restricted.Floatation is utilized the surface-active of extractant, makes extractant attached on the interface, with bubble floating, with moisture be that to produce the needed energy consumption of bubble bigger from, the problem of this method.Fibre deposition bed and lamella coalescent filter all are to accelerate owing to being subjected to flowing space obstruction flow velocity when utilizing feed liquid to flow through, and the shearing force of the surface of solids has increased the disturbance of oil droplet in the water, quickens coalescence and phase-splitting, and the effect of breakdown of emulsion is arranged.This method is difficult to reclaim the extractant of solubilised state, need comprehensively use in conjunction with additive method.Additive method also has filtration method, centrifugal process etc., because inconvenient operation, and problem such as energy consumption is bigger, to use aspect the extractant be not very extensive reclaiming.
Traditional recovery extractant method wants multiple arrangement to be used because single assembly efficient is lower, causes flow process complicated, the equipment investment height.The flowsheet synthesis of the recovery extractant of Spasic (Chemical Engineering Science, Vol.52, No.5, pp.651-675,1997) test has used the lamella coalescent filter, floatation, settled process and absorption method etc.Experimental result shows that the efficient of lamella coalescent filter is 62%, and the efficient of floatation is 77%, and the efficient of adsorbent equipment is 63%, and the separation of whole flow process is 92%.
Summary of the invention
The objective of the invention is to propose a kind of efficient, easy extractant recovery method, reduce the expense and the energy consumption that reclaim extractant, and can combine preferably with existing extracting system.Technology of the present invention is that water is contacted by film with diluent, by the absorption on film surface and " extraction " effect of diluent, extractant is transferred to the diluent from water; Described diluent is an employed diluent in the extracting system.Diluent rich in extractant can be used to reclaim extractant once more, also can be incorporated in the organic facies of extracting system.
Technical scheme of the present invention is as follows:
A kind of membrane separating method that reclaims the aqueous phase extractant, it is characterized in that this method utilizes the film device to separate, make the water that contains extractant and diluent respectively from two side flow of film, water contacts by film with diluent, and extractant is transferred to the diluent from water; Described water is extraction raffinate and the strip liquor in the chemical extraction system; Described diluent is an employed diluent in the extracting system; For the hydrophobic membrane device, the static pressure of water one side should be higher than the diluent static pressure of a side mutually; Then opposite for the hydrophilic membrane device; But this pressure reduction can not be above penetrating pressure.
Film device of the present invention adopts hollow fiber module, rolling or board-like film device; The size that requires fenestra is between 100nm-100 μ m.If adopt hollow fiber module, the water that then contains extractant flows in the tube side of hollow fiber module, and diluent flows in the shell side of hollow fiber module; Water in the tube side and the contact form of the diluent in the shell side is and stream or adverse current.
Technical characterictic of the present invention also is: post-treatment aqueous phase can be circulated, to prolong the time of contact of water and diluent.
The present invention has the following advantages and the high-lighting effect: compare with traditional processing method, method of the present invention only just can realize the high efficiente callback of extractant with the film apparatus, simple, the easy operating of method, and energy consumption is low, and by diluent with the good and former extracting system combination of this recovery method.And this method helps preventing that diluent from entering water, and this has just effectively been avoided secondary pollution.
Description of drawings
Fig. 1 carries out the flow chart of the embodiment of film separating and recovering extractant for adopting hollow fiber module.
Fig. 2 is the cross-sectional view of hollow fiber module.
Among the figure: 1-hollow fiber module shell; 2-hollow-fibre membrane; 3-film organ pipe journey inlet; The outlet of 4-film organ pipe journey; 5-film device shell side inlet; The outlet of 6-film device shell side; 7-pump; 8-Pressure gauge; 9-valve.
The specific embodiment
The membrane separating method of recovery aqueous phase extractant provided by the invention makes the water that contains extractant and diluent respectively from two side flow of film, and water contacts by film with diluent, and extractant is transferred to the diluent from water; Described water is extraction raffinate and the strip liquor in the chemical extraction system; Described diluent is an employed diluent in the extracting system; The diluent that extracting system adopts usually has kerosene, normal heptane, toluene, dimethylbenzene, ethylene dichloride etc.Diluent rich in extractant can be used to reclaim extractant once more, also can be incorporated in the organic facies of extracting system.
In order to prevent the interpenetrative generation of water and diluent, alternately should keep certain pressure reduction in two of film both sides, the pressure that does not soak into a phase of membrane micropore should be higher than the pressure that soaks into membrane micropore one phase, for example, for the hydrophobic membrane device, the static pressure of water one side should be higher than the diluent static pressure of a side mutually; Then opposite for the hydrophilic membrane device.But there is a critical value in this pressure reduction, is called to penetrate pressure, and pressure reduction can not surpass this critical value.If hypothesis membrane micropore road is parallel even cylindrical bore, then penetrating of microporous barrier pressed Δ p
CrCan be expressed as:
Δp
cr＝2γcosθ
c/r
P
Wherein, γ is the interfacial tension of two-phase, r
PBe fenestra radius, θ
cBe the feeler that joins, refer to fenestra road wall and be angle between the tangent line of nose end two-phase interface of starting point with liquid-liquid-solid three-phase junction.
In principle, to the flow velocity of two-phase without limits, but these two flow velocitys are influential to separating effect.Flow velocity increases, and can strengthen convective mass transfer.One timing of film device specification, the flow velocity increase can make diminish time of contact, thereby influences separating effect.To determine suitable two-phase flow velocity according to concrete processing requirements and film device specification
The film device that the present invention uses can be a hollow fiber module, rolling or board-like film device etc.; The size that requires fenestra is between 100nm-100 μ m.The specification of the gross area of film, film device will be by the treating capacity decision of water.When adopting hollow fiber module to separate, the water that contains extractant flows in the tube side of hollow fiber module, and diluent flows in the shell side of hollow fiber module, the water in the tube side and the contact form of the diluent in the shell side is and stream or adverse current.In order to reach better separating effect, post-treatment aqueous phase can be circulated, to prolong the time of contact of water and diluent.
The film device that embodiment among Fig. 1 is selected for use is a hollow fiber module.Hollow fiber module is that many hollow-fibre membrane silks are seated in the housing, and its cross section as shown in Figure 2.Concrete diluent and the diluent in the extraction system are identical, are beneficial to return extracting system and use.Contain tube side inlet 3 inflows of the water of extractant from hollow fiber module 1, diluent enters from shell side inlet 5, the contact form that two-phase adopts and flows, and final post-treatment aqueous phase exports 4 from tube side and flows out, and diluent rich in extractant is from shell side outlet 6 outflows.
The parameter of used film device is among the embodiment: membrane material is PVDF; Effective dimensions (φ * L (mm)) is 42 * 313; The average pore size of film is 0.1 μ m; Total membrane area is 0.2m
2Doughnut inside/outside footpath (mm) is 0.8/1.4, and number of fiber is 254.
In the following example, be diluent, reclaim typical acidic extractant P204 and neutral extractant TBP with the normal heptane.In the actual extraction process, aqueous phase not only has extractant, also has diluent.In the present embodiment, aqueous phase contains extractant, diluent normal heptane and low quantity of surfactant Triton X-114.Each organic initial concentration of aqueous phase is decided with reference to the typical extraction process of reality.The computational methods of the rate of recovery of extractant are:
The rate of recovery=1-outlet water extractant concentration/initial water extractant concentration
Embodiment 1: reclaim acidic extractant P204 (once by the film device)
Initial three kinds of organic concentration: P204 of aqueous phase are 97.7mg/L, and normal heptane is 160.2mg/L, and Triton X-114 is 6.1mg/L.Aqueous phase flow rate is 0.0014m/s in the hollow fiber module tube side; The flow velocity of normal heptane is 0.0004m/s in the shell side; Pressure reduction from the tube side to the shell side is 0.4kPa.Water does not circulate in the experiment, and promptly the water that initial concentration is constant continues to enter film organ pipe journey.
The P204 concentration of film device outlet water and the device relation of running time in table 1. example 1
| Time/min | 0 | 5 | 10 | 20 | 40 | 80 | 100 | 120 | 140 |
| P204 concentration/mg/L | 24.4 | 26.2 | 34.4 | 36.8 | 39.6 | 40.4 | 42.3 | 45.3 | 45.8 |
| The P204 rate of recovery | 0.750 | 0.732 | 0.648 | 0.623 | 0.595 | 0.586 | 0.567 | 0.536 | 0.531 |
Can see that from top result film device outlet P204 concentration has a process that rises and afterwards tend towards stability earlier in time, the corresponding recovery takes the lead in tending towards stability the separating effect when this value is this film device stable operation after the decline.Rate of recovery when it is initial and stable is respectively about 0.750 and 0.531.
Embodiment 2: the tube side flow velocity is to the influence (once by the film device) of separating effect
Other conditions are identical with example 1, and example 2 is investigated the influence of tube side aqueous phase flow rate to separating effect, and aqueous phase flow rate in the hollow fiber module tube side is become 0.00073m/s.
The P204 concentration of film device outlet water and the device relation of running time in table 2. example 2
| Time/min | 0 | 5 | 10 | 20 | 40 | 60 | 80 | 100 | 120 |
| P204 concentration/mg/L | 14.3 | 27.6 | 25.3 | 26.3 | 25.7 | 33.0 | 33.0 | 38.2 | 38.7 |
| The P204 rate of recovery | 0.854 | 0.718 | 0.741 | 0.731 | 0.737 | 0.662 | 0.662 | 0.609 | 0.604 |
The result of embodiment 2 and embodiment 1 compared can see that aqueous phase flow rate diminishes in the tube side, it is big that the rate of recovery becomes, and this is elongated cause time of contact of water.But its stable separating effect is still good inadequately.
More than the final removal effect of two examples be subjected to the restriction of film device length, cause the time of contact can not long enough.For overcoming the restriction of film device length, in two following examples water is circulated, i.e. the water of film organ pipe journey outlet enters the film device from import again, and we just can investigate the best separating effect that can reach like this.
Embodiment 3: reclaim acidic extractant P204 (water circulation)
The composition of initial water is consistent with example 1.Aqueous phase flow rate is 0.0125m/s in the hollow fiber module tube side; The flow velocity of normal heptane is 0.0004m/s in the shell side; Pressure reduction from the tube side to the shell side is 0.4kPa.
The P204 concentration of film device outlet water and the device relation of running time in table 3. example 3
| Time/min | 0 | 5 | 10 | 30 | 50 | 70 | 90 | 110 | 130 |
| P204 concentration/mg/L | 69.7 | 71.7 | 63.4 | 28.3 | 18.0 | 14.3 | 12.9 | 12.1 | 10.4 |
| The P204 rate of recovery | 0.287 | 0.266 | 0.351 | 0.71 | 0.816 | 0.854 | 0.868 | 0.876 | 0.894 |
Can see that from separating effect increased time of contact by the circulation water, last separating effect is near 90%.In actual applications, can be by using long film device or several film device series connection being reached higher separating effect.
Embodiment 4: pressure reduction is to the influence (water circulation) of separating effect
Other conditions are identical with example 3, and the pressure reduction of example 4 investigations from the tube side to the shell side becomes 0.8kPa to the influence of separating effect with this pressure reduction.
The P204 concentration of film device outlet water and the device relation of running time among table 4. embodiment 4
| Time/min | 0 | 5 | 10 | 30 | 50 | 60 | 80 | 100 | 120 |
| P204 concentration/mg/L | 71.2 | 62.4 | 40.6 | 27.7 | 20.8 | 19.4 | 17.7 | 16.4 | 15.3 |
| The P204 rate of recovery | 0.271 | 0.361 | 0.584 | 0.716 | 0.787 | 0.801 | 0.819 | 0.832 | 0.843 |
The separating effect of example 4 is compared with example 3 and be there is no much variations, and visible pressure reduction is not clearly to the influence of separating effect.
Embodiment 5: reclaim neutral extractant TBP (water circulation)
Initial each organic consisting of: TBP259.7mg/L of aqueous phase, normal heptane 173.1mg/L, Triton X-114 are 43.3mg/L.Aqueous phase flow rate is 0.0125m/s in the hollow fiber module tube side; The normal heptane flow velocity is 0.0004m/s in the shell side; Pressure reduction from the tube side to the shell side is 0.4kPa.Water circulates in the experiment.
The TBP concentration of film device outlet water and the device relation of running time in table 5. example 5
| Time/min | 0 | 5 | 10 | 20 | 30 | 40 | 50 | 60 |
| TBP concentration/mg/L | 150.9 | 94.1 | 74.4 | 60.1 | 59.2 | 58.3 | 57.0 | 56.9 |
| The TBP rate of recovery | 0.419 | 0.638 | 0.714 | 0.769 | 0.772 | 0.776 | 0.781 | 0.781 |
Can see that from the example of above three waters circulation the concentration of film device outlet extractant finally reach a lower value, and the rate of recovery of extractant increases in time on the whole, reaches a higher value at last on the whole along with the time constantly reduces.As to P204, ult rec is 89.4%; To TBP, ult rec is 78.1%.This result shows that this process has good recovering effect to extractant as long as guarantee time of contact.Reclaim the process of extractant with people such as Spasic and compare, the extraction yield recovering effect of our circulation experiment is lower than the separating effect of its whole flow process, but is higher than the separating effect of its any one separate processes; And the process energy consumption is low, and is simple to operate, is easy to realize.
Claims (5)
1. method of utilizing membrane separation technique to reclaim the aqueous phase extractant, it is characterized in that this method utilizes the film device to separate, make the water that contains extractant and diluent respectively from two side flow of film, water contacts by film with diluent, and extractant is transferred to the diluent from water; Described water is extraction raffinate and the strip liquor in the chemical extraction system; Described diluent is an employed diluent in the extracting system; For the hydrophobic membrane device, the static pressure of water one side should be higher than the diluent static pressure of a side mutually; Then opposite for the hydrophilic membrane device; But this pressure reduction can not be above penetrating pressure.
2. according to the described a kind of method of utilizing membrane separation technique to reclaim the aqueous phase extractant of claim 1, it is characterized in that: described film device adopts hollow fiber module, rolling or board-like film device, and the size of fenestra is between 100nm-100 μ m.
3. according to the described a kind of method of utilizing membrane separation technique to reclaim the aqueous phase extractant of claim 2, it is characterized in that: when adopting hollow fiber module to separate, the water that contains extractant flows in the tube side of hollow fiber module, and diluent flows in the shell side of hollow fiber module.
4. according to the described a kind of method of utilizing membrane separation technique to reclaim the aqueous phase extractant of claim 3, it is characterized in that: the water in the tube side and the contact form of the diluent in the shell side are and stream or adverse current.
5. according to claim 1,2,3 or 4 described a kind of methods of utilizing membrane separation technique to reclaim the aqueous phase extractant, it is characterized in that: post-treatment aqueous phase is circulated, to prolong the time of contact of water and diluent.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829436A (en) * | 2010-05-27 | 2010-09-15 | 南京工业大学 | Large liquid membrane continuous reaction device |
| CN102459662A (en) * | 2009-06-11 | 2012-05-16 | 奥图泰有限公司 | Method and apparatus for regeneration of extraction solution in metal extraction processes |
| CN104001345A (en) * | 2013-02-25 | 2014-08-27 | 刘钢 | Nano-fibrous tubular membrane extraction apparatus |
| CN107441963A (en) * | 2017-08-10 | 2017-12-08 | 武汉纺织大学 | A kind of preparation method of aqueous phase polymeric hollow fiber array material |
| CN108367244A (en) * | 2015-07-29 | 2018-08-03 | 格雷迪安特公司 | Osmosis method for desalination and related system |
| CN108367943A (en) * | 2015-12-18 | 2018-08-03 | 苏伊士集团 | Method for treating water, correlation module and equipment |
| CN109897958A (en) * | 2019-04-16 | 2019-06-18 | 中国恩菲工程技术有限公司 | The recovery method of copper in phosphoric acid kind of extractants solution |
| CN110358111A (en) * | 2019-08-21 | 2019-10-22 | 蒋遂安 | A kind of system and method for coal mining waste harmless resource production humic acid |
| CN112007381A (en) * | 2020-09-08 | 2020-12-01 | 绍兴市九鑫环保有限公司 | Continuous extraction device and extraction method for phosphorus-containing waste acid |
| CN114534498A (en) * | 2022-01-06 | 2022-05-27 | 中国原子能科学研究院 | Device and method for trapping residual TBP in aqueous phase |
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2008
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| CN102459662A (en) * | 2009-06-11 | 2012-05-16 | 奥图泰有限公司 | Method and apparatus for regeneration of extraction solution in metal extraction processes |
| CN102459662B (en) * | 2009-06-11 | 2014-02-19 | 奥图泰有限公司 | Method and apparatus for regeneration of extraction solution in metal extraction processes |
| CN101829436B (en) * | 2010-05-27 | 2012-06-27 | 南京工业大学 | Large liquid membrane continuous reaction device |
| CN101829436A (en) * | 2010-05-27 | 2010-09-15 | 南京工业大学 | Large liquid membrane continuous reaction device |
| CN104001345A (en) * | 2013-02-25 | 2014-08-27 | 刘钢 | Nano-fibrous tubular membrane extraction apparatus |
| US11400416B2 (en) | 2015-07-29 | 2022-08-02 | Gradiant Corporation | Osmotic desalination methods and associated systems |
| CN108367244A (en) * | 2015-07-29 | 2018-08-03 | 格雷迪安特公司 | Osmosis method for desalination and related system |
| CN108367943A (en) * | 2015-12-18 | 2018-08-03 | 苏伊士集团 | Method for treating water, correlation module and equipment |
| CN107441963A (en) * | 2017-08-10 | 2017-12-08 | 武汉纺织大学 | A kind of preparation method of aqueous phase polymeric hollow fiber array material |
| CN107441963B (en) * | 2017-08-10 | 2019-09-24 | 武汉纺织大学 | A kind of preparation method of water phase polymeric hollow fiber array material |
| US11629072B2 (en) | 2018-08-22 | 2023-04-18 | Gradiant Corporation | Liquid solution concentration system comprising isolated subsystem and related methods |
| CN109897958A (en) * | 2019-04-16 | 2019-06-18 | 中国恩菲工程技术有限公司 | The recovery method of copper in phosphoric acid kind of extractants solution |
| CN110358111A (en) * | 2019-08-21 | 2019-10-22 | 蒋遂安 | A kind of system and method for coal mining waste harmless resource production humic acid |
| CN112007381A (en) * | 2020-09-08 | 2020-12-01 | 绍兴市九鑫环保有限公司 | Continuous extraction device and extraction method for phosphorus-containing waste acid |
| US11667549B2 (en) | 2020-11-17 | 2023-06-06 | Gradiant Corporation | Osmotic methods and systems involving energy recovery |
| CN114534498A (en) * | 2022-01-06 | 2022-05-27 | 中国原子能科学研究院 | Device and method for trapping residual TBP in aqueous phase |
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