CN86101730B - Electrostatic quasi-liquid film separation method and device - Google Patents
Electrostatic quasi-liquid film separation method and device Download PDFInfo
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- CN86101730B CN86101730B CN86101730A CN86101730A CN86101730B CN 86101730 B CN86101730 B CN 86101730B CN 86101730 A CN86101730 A CN 86101730A CN 86101730 A CN86101730 A CN 86101730A CN 86101730 B CN86101730 B CN 86101730B
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- 238000000926 separation method Methods 0.000 title claims description 14
- 239000007788 liquid Substances 0.000 title description 28
- 238000000605 extraction Methods 0.000 claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 29
- 230000008878 coupling Effects 0.000 claims abstract description 4
- 238000010168 coupling process Methods 0.000 claims abstract description 4
- 238000005859 coupling reaction Methods 0.000 claims abstract description 4
- 239000006185 dispersion Substances 0.000 claims abstract 2
- 239000007864 aqueous solution Substances 0.000 claims description 25
- 208000035126 Facies Diseases 0.000 claims description 20
- 238000000151 deposition Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 12
- 239000012141 concentrate Substances 0.000 claims description 9
- 230000005684 electric field Effects 0.000 claims description 8
- 230000005686 electrostatic field Effects 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 7
- 239000000284 extract Substances 0.000 claims description 6
- 239000008346 aqueous phase Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 230000005484 gravity Effects 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 3
- 230000008929 regeneration Effects 0.000 claims description 3
- 238000011069 regeneration method Methods 0.000 claims description 3
- 230000002411 adverse Effects 0.000 claims description 2
- 239000011810 insulating material Substances 0.000 claims description 2
- 239000007769 metal material Substances 0.000 claims description 2
- 238000005192 partition Methods 0.000 claims 1
- 229910021645 metal ion Inorganic materials 0.000 abstract description 3
- 239000003758 nuclear fuel Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract 2
- 239000011148 porous material Substances 0.000 abstract 2
- 238000010924 continuous production Methods 0.000 abstract 1
- 238000005272 metallurgy Methods 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 10
- 239000000839 emulsion Substances 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 6
- 239000012528 membrane Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 210000000481 breast Anatomy 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 229920005479 Lucite® Polymers 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000009854 hydrometallurgy Methods 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000007762 w/o emulsion Substances 0.000 description 2
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000000409 membrane extraction Methods 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
- Electrostatic Separation (AREA)
Abstract
A continuous process of extraction-back extraction is carried out by using pore space on electrode in middle of reaction tank to make organic solution containing extractant flow freely through pore space, and using electrostatic phase dispersion mode to apply force directly to dispersed water drop without turbulent motion of continuous oil phase. The water baffle is arranged on the electrode, so that water drops containing solute to be extracted on one side of the electrode are effectively separated from back extraction water drops on the other side of the electrode, and the coupling of an extraction-back extraction process in the reaction tank is ensured. It is suitable for the processes of extracting metal ions from water metallurgy (including nuclear fuel circulation), treating waste water and the like.
Description
The present invention relates to a kind of chemical separation technology, the specific solute in this technology energy separation, purifying and the concentrated aqueous solution.Be applicable to that (comprising nuclear fuel cycle) in the hydrometallurgy process from the aqueous solution extracts useful metal, and be applicable to aspect such as wastewater treatment.
Solvent extraction technology is a kind of separation method that this century, the forties grew up, and has become the representative art of hydrometallurgy at present.Solvent extraction is made up of the extraction and two processes of stripping, because the separation process of every grade of extraction and reextraction is subjected to the restriction of chemical balance, so required separation progression is more, the consumption of reagent is bigger.In addition, the reagent entrainment loss is also relatively more serious.
Liquid film separating method is a kind of new technology that middle nineteen sixties grows up, and it also is made up of the extraction and two processes of stripping.But, in liquid film separating method, the organic solution that contains extractant will contain and remain the aqueous solution and the stripping aqueous solution of extract solutes and separate, and make the extracting-back extraction process of getting obtain coupling at inside reactor, be the extracting-back extraction process of getting is carried out simultaneously, a step finishes, this just broken solvent extraction process intrinsic extraction equilibrium, this nonequilibrium behavior of liquid film makes required separation progression reduce, and has saved the consumption of reagent.
Liquid film technology can be divided into emulsion liquid membrane and support two kinds of liquid films by configuration.Emulsion liquid membrane is by propositions such as United States Patent (USP)s 3779907,4014785, its principle is, the aqueous solution that will contain reextraction reagent is made water in oil emulsion with the organic solution that contains extractant and surfactant, again this emulsion is remained the aqueous solution of extracting metals ion and mixes with containing, form the compound emulsion of water-oil-water type.In this system, the metal ion of aqueous phase sees through oil film and concentrates in disperseing aqueous phase continuously.After stopping to stir, water-in-oil emulsion promptly with continuous water layering.The mass transfer specific area of this method is big, and mass transport process is fast.But this method uses surfactant to stablize liquid film, and this has just increased operations such as system breast, breakdown of emulsion, makes whole process more complicated, is difficult to realize continued operation.
The supporting liquid film (ISEC, Membrane Extraction Session 12, P.80, and 1980) liquid film material (oil solution that promptly contains extractant) dipping hydrophobicity porosu solid film to be made, the porosu solid film here is the supporting mass of liquid film.This liquid film placed contain when remaining between the aqueous solution of extracting metals ion and the stripping workshop, metal ion just is extracted in the film in a side of film, is diffused into opposite side and is stripped in another aqueous solution in film.
The process of supporting liquid film is simple, is easy to realize serialization, but owing to adopt the porosu solid film to make supporting mass, resistance to mass tranfer is bigger.Simultaneously, the liquid film material is difficult to securely in the hole attached to support membrane, and promptly the stability problem of film is difficult to solve.
The object of the present invention is to provide a kind of new separation method and device, it can develop the characteristics of liquid Membrane Separation Technique non-equilibrium extraction, can overcome or improve the above-mentioned shortcoming of liquid film technology again.Its main feature is to utilize the hole that is positioned on the middle electrode of reactive tank, the oil solution of these electrode both sides can be flowed freely by hole, and utilize static phase dispersing mode that active force is directly put on and disperseed water droplet and do not make the violent turbulence of oil-continuous phase, on electrode, install water fender, effectively the water droplet of these electrode both sides is separated, thereby guaranteed the coupling of extraction and reextraction process in reactive tank inside.Above-mentioned feature embodies by following process: will contain and remain the aqueous solution of extract solutes and contact with the organic solution of being opened by the electrode separation of crack with holes and water fender that contains extractant respectively with aqueous solution of back extraction, organic solution can flow freely by hole, contain and remain the aqueous solution and the aqueous solution of back extraction of extract solutes and separated by water fender, the aqueous solution that will be in the organic facies with the high-voltage electrostatic field is dispersed into droplet, in the extraction side, treat that the solute in the aqueous phase extracted droplet is extracted to continuous organic facies, the complex compound that is generated is under the promotion of its concentration gradient, spread to the back extraction side by the electrode hole, in the back extraction side, solute by back extraction in the aqueous solution of back extraction droplet, extractant in the organic facies obtains regeneration continuously, extractant spreads back the extraction side by the electrode hole under the ordering about of its concentration gradient, so circulation is laterally being carried out the extracting-back extraction process of getting continuously.Meanwhile, above-mentioned two kinds of water droplets of extraction side and reextraction side are under the gravity effect, sinking in the organic facies continuously respectively, form the extraction and the reextraction process of adverse current, the water droplet sinks to the bottom, break away from strong electrostatic field, under weak electric field and gravity effect,, obtain raffinate and concentrate respectively with the organic facies layering.Because this method both belonged to non-equilibrium system, exempted system breast, breakdown of emulsion operation again, therefore, not only have fast, efficient, energy-saving advantages, and have that flow process is simple, process is easy to realize advantages such as serialization and automation.
Said process is to finish in the specific device of the present invention a kind of being suitable for.This device is the improvement to liquid film extraction equipment.
Fig. 1 is separation process principle of the present invention and device schematic diagram.
Fig. 2 is the structural representation of the electrode of band water fender.
Device among Fig. 1 comprises a reactive tank (1), and its top is separated into abstraction pool (3) and reextraction pond (4) by electrode (2), and its bottom is separated into extraction depositing reservoir (12) and back extraction depositing reservoir (14) by water-stop sheet (13).Abstraction pool (3) and extraction depositing reservoir (12) are full communicating, and reextraction pond (4) and reextraction depositing reservoir (14) also are communicated with fully.Water-stop sheet (13) is bonded on reactive tank (1) base plate, and bonding with the groove two side, and bonding portion will guarantee not leak, and prevents that the both sides water from going here and there mutually.
Hole (5) is arranged on the electrode (2), and water fender (6) is housed, organic solution in abstraction pool (3) and reextraction pond (4) can flow freely by hole (5), and the water droplet that is dispersed in the organic facies of abstraction pool (3) and reextraction pond (4) is separated by water fender (6).Electrode (2) constitutes two pairs of electric fields with the electrode (7) that is contained in reactive tank (1) both sides and (8), is applied to respectively on abstraction pool (3) and reextraction pond (4).
Raffinate in the extraction depositing reservoir (12) is drawn by conduit (11), concentrate in the reextraction depositing reservoir (14) is drawn by conduit (15), and an end of conduit (11) and (15) links to each other with the bottom of extraction depositing reservoir (12) and reextraction depositing reservoir (14) respectively.
In order to prevent interelectrode short circuit, have at least one to be insulating electrode in every pair of electrode, bare electrode (being on-insulated electrode) is if using resistant material in Korrosionsmedium makes, as corrosion resistant plate etc.In order to keep higher electrode efficiency, the porosity on the electrode should be less than 40%.In order to shorten the distance of complex compound and extractant horizontal proliferation, improve mass-transfer efficiency, interelectrode distance is the smaller the better, takes into account the feasibility on the charge door frame for movement, and general optional interelectrode distance is 5～20mm.
Reactive tank (1), water fender (6) and water-stop sheet (13) are all made with insulating materials.
During work, the organic solution that will contain extractant is filled with reactive tank (1), and on abstraction pool (3) and reextraction pond (4), apply the ac high-voltage electrostatic field simultaneously, contain and remain the feed liquid of extract solutes and add abstraction pool (3) along the indicated direction of arrow (9), strip liquor adds reextraction pond (4) along direction shown in the arrow (10).
According to principles of electrostatics, the water droplet in the dielectric solution is outside under the effect of electric field, will produce induced dipole and distorts, and the distortion degree increases with the increase of electric-field intensity.When electric-field intensity surpasses a certain critical value, water droplet just is dispersed into countless droplets.The present invention adds the feed liquid of abstraction pool (3) and the strip liquor of reextraction pond (4) and is being dispersed into countless droplets respectively in the organic facies continuously under the effect of suitable high-voltage electrostatic field.In abstraction pool (3), treat that the solute in the aqueous phase extracted droplet is extracted to continuous organic facies, the complex compound in the organic facies spreads to reextraction pond (4) by the hole (5) on the electrode (2) under the promotion of the concentration gradient of himself continuously.In reextraction pond (4), when the solute in the continuous organic facies by after back extraction is in the strip aqueous droplet, extractant in the organic facies just obtains regeneration continuously, the concentration gradient of extractant itself is ordered about it again and is spread back abstraction pool (3) by the hole (5) on the electrode (2), proceeds said process.Meanwhile, the above-mentioned two kinds of water droplets in abstraction pool (3) and reextraction pond (4) are sinking in the organic facies respectively under the gravity effect continuously, form counter-current extraction and countercurrent reextraction and get process.Two kinds of water droplets sink to reactive tank (1) bottom and just break away from electrostatic field and enter extraction depositing reservoir (12) and reextraction depositing reservoir (14) respectively, then with the organic facies layering, and then obtain raffinate and concentrate.
Mixed liquor in the abstraction pool (3) has an interface with the raffinate of extraction depositing reservoir (12), and the height at this interface can be controlled by the height of delivery port of adjusting conduit (11).Equally, between the concentrate of mixed liquor in reextraction pond (4) and reextraction depositing reservoir (14) interface is arranged also, its height is controlled by the height of the delivery port of regulating conduit (15).
In sum, technology proposed by the invention, it has kept, and liquid film technology separation progression is few, and advantages such as reagent consumption province have been avoided the system breast in the emulsion liquid membrane technology, breakdown of emulsion operation again, make the process simplification and are easy to realize serialization and automation.It is compared with the supporting liquid film, because of having saved the porosu solid film as the liquid film supporting mass, thereby resistance to mass tranfer is greatly reduced, and has avoided the staining of stability, film of film, the problems such as obstruction of micropore.In addition, because present technique adopts electrostatic field to make water be dispersed into droplet, this phase dispersing mode is not realize under the situation of violent turbulence in continuous phase, so can adopt the water of simple water fender in will extracting and strip to separate in this technology.Saved mechanical driving part in the static phase process for dispersing, simplified equipment, and obtained the good effect that energy consumption is low, the reagent entrainment loss is few, this is particularly suitable for operation of handling radioactive liquid.
The embodiment of the invention is as follows:
Reactive tank (1) is square, and its appearance and size is that 40(is long) * 100(is wide) * the 150(height) mm, make with lucite.The wide 75mm of electrode (2), high 100mm in the middle of the reactive tank (1), this electrode is made with stainless steel material, electrode (2) is supported by water-stop sheet (13), hole (5) and water fender (6) are arranged on the electrode (2), hole (5) is highly to be the rectangle of 2mm, vertically arranges two span 12mm.The water fender position is shown in Fig. 2 (A) or Fig. 2 (B).Electrode (2) can be made into double-plate, and as Fig. 2 (A) or one-board, as Fig. 2 (B), the double-plate structure is complicated, but water fender (6) does not influence electrode efficiency.Electrode (7), (8) they are insulating electrode, make with the common metal material, and the polyester film of external pasting 0.05 * 2mm, and be separately fixed at the two side of reactive tank (1), can be screwed.Distance is 10mm between electrode (2) and electrode (7), (8), and electrode is connected on the adjustable high-voltage ac power.Water-stop sheet (13) separates raffinate and concentrate, makes with lucite.
Utilize said apparatus from the aqueous solution, to extract cobalt (Co).Feed liquid is the aqueous solution that contains 1000ppm Co and 0.1M CHCOONa, and its initial pH value transfers to 5.0.Anti-stripping agent is the 1.0M HSO aqueous solution.Organic facies is for containing the 10%(volume) the hydrogenation kerosin of di-(2-ethylhexyl)phosphoric acid (extractant).Apply voltage 3kV in the experiment, recording electric current is 650 μ A.The feed liquid flow is 150ml/h, and the anti-stripping agent flow is 10ml/h, and recording the time of staying of water droplet in electric field in the experiment is 4s.At last, the concentration that obtains cobalt in the raffinate is 5ppm, and the concentration of cobalt is near 15000ppm in the concentrate, and the concentration of cobalt is lower than 200ppm in the organic facies, and total enrichment factor is near 3000.
Claims (6)
1, a kind of method of from the aqueous solution, removing specific solute, this method has the extraction and two processes of stripping, the organic solution that contains extractant will contain the aqueous solution and the aqueous solution of back extraction that remain to be extracted and separate, and make the extracting-back extraction process of getting realize coupling at inside reactor, become that the extracting-back extraction process of getting is carried out simultaneously and a step finishes, it is characterized in that to contain and remain the aqueous solution of extract solutes and contact with the organic solution of opening by the electrode separation of crack with holes and water fender that contains extractant respectively with aqueous solution of back extraction, the aqueous solution that adopts the high-voltage electrostatic field will be in the organic facies is dispersed into droplet, in the extraction side, treat that the solute in the aqueous phase extracted droplet is extracted to continuous organic facies, complex compound is under the promotion of its concentration gradient, hole by electrode spreads to the back extraction side, in the back extraction side, solute by back extraction in the stripping aqueous solution droplet, extractant in the organic facies obtains regeneration continuously, extractant spreads back the extraction side by the electrode hole under the ordering about of its concentration gradient, so circulation, the extracting-back extraction process of getting is laterally being carried out continuously, meanwhile, above-mentioned two kinds of water droplets of extraction side and back extraction side are under the gravity effect, sinking in the organic facies continuously respectively, form the extraction and the reextraction process of adverse current, the water droplet sinks to the bottom, break away from electrostatic field, with the organic facies layering, obtain raffinate and concentrate respectively.
2, the device of the described partition method of a kind of claim 1, constitute by reactive tank, it is characterized in that reactive tank (1) is separated into abstraction pool (3) and reextraction pond (4) by electrode (2), electrode (2) is supported by water-stop sheet (13), water-stop sheet (13) is divided into extraction depositing reservoir (12) and reextraction depositing reservoir (14) to reactive tank (1) lower part, have on the electrode (2) and allow the free-pouring hole of organic solution (5) and separate the water fender (6) that wait to come together water-soluble drop and stripping aqueous solution drip, electrode (2) is with the electrode (7) in abstraction pool (3) and reextraction pond (4) and (8) constitute two pairs of electric fields that are used for electrostatic dispersion respectively, having one in every pair of electric field at least is insulating electrode, be connected with a conduit (11) of drawing raffinate in extraction depositing reservoir (12) bottom, be connected with a conduit (15) of drawing concentrate, reactive tank (1) in back extraction depositing reservoir (14) bottom, water fender (6) and water-stop sheet (13) are made with insulating materials.
3, separator as claimed in claim 2 is characterized in that the hole on the middle electrode (2) of reactive tank (1) is a rectangle, and porosity is less than 40%.
4, as claim 2,3 described separators, it is characterized in that electrode (2) is a bare electrode, make with corrosion resistant metal material, as corrosion resistant plate, electrode (7), (8) they are insulating electrode.
5, as claim 2,3 described separators, the spacing that it is characterized in that two electrodes is 5～20mm.
6, separator as claimed in claim 4, the spacing that it is characterized in that two electrodes is 5～20mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86101730A CN86101730B (en) | 1986-03-19 | 1986-03-19 | Electrostatic quasi-liquid film separation method and device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86101730A CN86101730B (en) | 1986-03-19 | 1986-03-19 | Electrostatic quasi-liquid film separation method and device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86101730A CN86101730A (en) | 1987-09-16 |
| CN86101730B true CN86101730B (en) | 1987-09-23 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN86101730A Expired CN86101730B (en) | 1986-03-19 | 1986-03-19 | Electrostatic quasi-liquid film separation method and device |
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| Country | Link |
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| CN (1) | CN86101730B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1125664C (en) * | 2000-04-07 | 2003-10-29 | 清华大学 | Dispersive film extractor |
| CN1125665C (en) * | 2000-06-16 | 2003-10-29 | 清华大学 | In-line membrane extractor used in conjuction with electrospray mass spectroscope |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034716C (en) * | 1992-09-03 | 1997-04-30 | 中国原子能科学研究院 | Electrostatic quasi-liquid membrane efficient concentration method |
| GB9523542D0 (en) * | 1995-11-17 | 1996-01-17 | British Nuclear Fuels Plc | Separation method and apparatus |
| GB9609025D0 (en) * | 1996-04-30 | 1996-07-03 | British Nuclear Fuels Plc | Separation method and apparatus |
| CN110745900B (en) * | 2019-11-04 | 2022-05-10 | 西安建筑科技大学 | A kind of separation method of heavy metal hexavalent chromium and divalent cadmium |
| 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 |
-
1986
- 1986-03-19 CN CN86101730A patent/CN86101730B/en not_active Expired
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1125664C (en) * | 2000-04-07 | 2003-10-29 | 清华大学 | Dispersive film extractor |
| CN1125665C (en) * | 2000-06-16 | 2003-10-29 | 清华大学 | In-line membrane extractor used in conjuction with electrospray mass spectroscope |
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| Publication number | Publication date |
|---|---|
| CN86101730A (en) | 1987-09-16 |
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