CN103060559A - Microfluid extraction method for extracting and separating In, Fe and Zn - Google Patents
Microfluid extraction method for extracting and separating In, Fe and Zn Download PDFInfo
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- 238000000605 extraction Methods 0.000 title claims abstract description 55
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 48
- 229910052738 indium Inorganic materials 0.000 title claims abstract description 38
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000012071 phase Substances 0.000 claims abstract description 57
- 239000011701 zinc Substances 0.000 claims abstract description 47
- 239000012074 organic phase Substances 0.000 claims abstract description 43
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 31
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 230000005501 phase interface Effects 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 24
- 230000008569 process Effects 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 15
- 238000009854 hydrometallurgy Methods 0.000 claims description 9
- 239000008346 aqueous phase Substances 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 230000005514 two-phase flow Effects 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims 1
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- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
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- 239000000284 extract Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention provides a microfluid extraction method for extracting and separating In, Fe and Zn. The microfluid extraction method comprises the steps of: using a sulfuric acid system solution containing indium, ferrum and zinc as a water phase and a P204 extracting agent diluted through solvent oil as an organic phase, which are respectively fed into two flow pumps, wherein the outlet end of the flow pump is connected with an inlet of a microreactor; simultaneously, observing a two-phase laminar flow phase interface formed inside a microchannel through an optical microscope, so that two phases flow in parallel and then begins to be separated when reaching a Y-type fork at the outlet of the microchannel, and the two phases flow out of the microreactor from outlets of the two phases; respectively collecting the two phases; and extracting indium to enter the organic phase and leaving ferrum and zinc in the water phase, so that the separation of indium, ferrum and zinc is realized. The extraction rate of In can be up to more than 90%, but ions of Fe and Zn are not extracted completely; moreover, no emulsion appears; and reaction time is greatly shortened, the using amount and consumption of the extracting agent can be reduced, the condition controllability is high, the safety is high, and extracted organic solvent is prevented from being exposed in the air.
Description
Technical field
The present invention relates to a kind of microreactor system that utilizes to the method that valuable metal extracts, belong to the micro-fluidic technologies field.
Background technology
The extraction separation process of hydrometallurgy can directly carry out separating-purifying with many kinds of metal ions from solution, having avoided the separation processes such as precipitation, crystallization or reduction to produce waste residue and solution and arrived the various operation of solution to slag again, is the key means of metallurgy solution system isolation of purified.But still there are some key issues that need to solve in the traditional extraction process:
A, extraction agent consumption are large
Because extraction, the back extraction time is relatively long, often needs multistage even ten multi-stage solvent extractions, in order to adapt to the requirement of extraction mass transfer, Solvent quantity is large.In addition, extraction agent and contact with air area are large, are subjected to the impact of envrionment temperature large, and volatilization is serious, and the shearing force of high-energy stirring process may be destroyed the extractant molecules structure and cause the problem such as temperature rise.
B, the common extraction seriously, extraction efficiency is low
Under strongly mixing condition, the common extraction of main metal ion and foreign metal ion is serious, and the poor selectivity of extraction causes also needing multistage washing and back extraction after the extraction.As with in P204 extracting and separating Ni, the Co process because the common extraction of Fe, Zn, Mn and Cu when having extraction Co, and whole extraction progression is reached more than 18 grades, for another example with in the P204 extracting and separating In process owing to the common extraction problem of Fe, Zn, Sb, Bi and Cl etc. occurs, so that whole extraction progression reaches more than 14 grades.This has increased cost of investment greatly, has reduced extraction efficiency.
C, be prone to emulsion
About producing the mechanism of emulsification in the indium extraction process, all conduct in-depth research both at home and abroad at present, and proposed a lot of preventive measures.But up to the present, emulsion can not well be avoided.Trace it to its cause; because for having particle, certain metal ion species or comprising the omplicated solution system of tensio-active agent; what extraction process carried out because the high energy of conventional extraction mixes is very abundant and rapid; but in phase separation; because being adsorbed on the liquid-liquid interface of emulsion particle, stable particle (such as the particle colloid) becomes stable protective layer; very slowly even fully stopping so that two-phase droplet coalescence speed becomes, is very large and remove a required energy of particle from the interface.This is breakdown of emulsion difficulty and the basic reason that needs the large energy of input namely.
D, disaster hidden-trouble are large
Because the extraction process time is longer, need to build up the larger steel basin of volume and settling pond, whole extraction process will occupy very large place.And the organic phase big area is exposed in the air, so that disaster hidden-trouble is larger.In recent years, a lot of extraction plant fire casualties have just occured in the Chinese large-sized smeltery, the extraction process of the smeltery that some the are small-sized fire failure that also takes place frequently.
Therefore, these limitation of conventional extraction need to be resolved hurrily, and exploitation airtight, efficient extraction equipment is the key point that addresses this problem.
The poor efficiency high consumption unit process such as extraction, heat exchange and the mixing etc. that utilize the characteristics such as efficient, low consumption, safety of microreactor system to transform traditional Metallurgical industry might be developed the energy-saving technique process that makes new advances, thus the industrial upgrading of promotion metallurgy industry.
Because effective passage of microreactor or the physical size of chamber narrow down to micron even Nano grade, so that the gradient of fluid physics amount such as temperature, pressure, concentration and density etc. sharply increases, cause the greatly increase of heat and mass impellent, can make heat transfer coefficient improve an order of magnitude and order of magnitude of mass transfer reaction time reduction.The advantage of bringing thus also shows: because the raising of speed of response, conversion unit and reaction system can be reduced greatly, so that the security of reaction process improves greatly, the land used investment is saved greatly, and materials consumption reduces greatly; There is the reaction of toxicity for raw material, reaction process or product, can be by adopting the small-sized distributed mode of production in subregion, thus avoid the risk of poisonous and harmful raw produce; raw products transportation; Its processing power can improve by the number (Numbering-up) that increases functional unit, and does not need step by step iodine equipment.Advanced micro-fabrication technology is promoting the fast development of microreactor at present, and the focus in this field all concentrates on the research of the diffusion mass transfer of immiscible liquid-liquid two-phase extraction separation in a large number.
In the microfluid field, solvent extraction is very efficient, because it has the feature of the specific surface area that can provide very high and the diffusion length of lacking.The rate of mass transfer that is conducive to reduce the path length of diffusion and increases two-phase interface, thus chemical reaction rate improved.In addition, the phase mass transfer under the laminar flow control can avoid emulsification to occur.By " quantity stack " Numbering-up(parallel processing for example) technology for the increase of microfluid technological process output provide a kind of new may.This also so that batch operation (mixing/reaction/separation) can carry out continuously.Therefore, under the microchemistry system, can reach simultaneously the target that simplification of flowsheet prevents emulsification generation and Reaction time shorten.
Summary of the invention
The impurity separation difficulty such as the extraction efficiency that technical problem to be solved by this invention is to overcome the conventional solvent extraction of indium is low, the easy emulsification of solution, indium and iron, zinc, environmental pollution is serious, the shortcomings such as dangerous height, the microfluid extracting process of a kind of extracting and separating In and Fe, Zn is provided, and is a kind of efficient, safe, pollution-free, novel method that separation rate is high.
The present invention realizes by following technical proposal: the microfluid extracting process of a kind of extracting and separating In and Fe, Zn, and following each step of process:
The sulfuric acid system solution that (1) will contain indium, iron, zinc is as water, pass into respectively as organic phase in two flow pumps through the P204 extraction agent of solvent oil dilution, and the exit end of flow pump connects the microreactor entrance;
(2) open first organic phase flow pump, enter the microchannel of microreactor until organic phase after, pressing 0.65 times of the organic phase flow sets and open water phase flow rate pump again, (microscope is overlooked observation can see that water and organic phase are in the microchannel that the left and right sides is parallel advances to two-phase laminar flow phase interface by forming in the observation by light microscope microchannel simultaneously, two-phase laminar flow phase interface is the contact surface of water and organic phase), regulate during this time the flow of two-phase, make the two-phase split flow;
Begin to separate when (3) two phase flow is to the place, Y type fork of microchannel outlet, flow out microreactor from outlet separately, and two-phase is collected respectively, indium is extracted and enters organic phase, and iron and zinc are kept aqueous phase, has realized separating of indium and iron, zinc.
The described sulfuric acid system solution that contains indium, iron, zinc is the leach liquor in the hydrometallurgy zinc process.
Described solvent oil is conventional solvent oil, such as No. 260 solvent oils.
The characteristic dimension of described microchannel is 160～800 μ m(internal diameters), length is 80～480mm.
The duration of contact of described two-phase in the microchannel is 0.01～10s.
Inventive principle: because the long-pending ratio with the two-phase mass transfer degree of depth of two-phase interface in the microreactor, the object element concentration gradient is very large in the two-phase, causes the extraction impellent greatly to improve, and mass-transfer efficiency often improves an order of magnitude than traditional operation.So immiscible two-phase can be in the microchannel, carry out quick mass transfer in the situation of the Laminar Flow contact by the short period of time.Its feature is to have strengthened the metallurgical operations unit process, raises the efficiency, reduces energy consumption.
Micro-fluidic technologies is the technology of control under microscopic dimensions, operation and detection of complex fluid, is a brand-new cross discipline that grows up on little chemical industry, micromechanics, biotechnology and nanotechnology basis.The in recent years fast development of micro-fluidic technologies causes revolutionary impact in fields such as chemistry, medicine and life sciences.At present, at chemistry and chemical field, synthetic etc. such as gas processing, chemosynthesis and particle, micro-fluidic technologies can reach produces several tons production capacity per year.Therefore, micro-fluidic technologies is applied to the hydrometallurgy field, may at the aspects such as security of the emulsion that improves the hydrometallurgical solvent extraction process, reduction Solvent quantity and raising extracting operation, plays a significant role.
The present invention uses micro-fluidic technologies, make two-phase liquid in the microchannel, keep Laminar Flow, by Y type outlet sharp separation, the In percentage extraction can reach more than 90%, Fe and Zn ion then are not extracted fully, and emulsion do not occur, thereby avoided traditional extraction to contain the series of problems of In, Fe and Zn solution.Have following effect and advantage:
1, the present invention is directed to In metal in the zinc hydrometallurgy leach liquor, adopt the microfluid solvent extraction technology to reclaim, organic efficiency is high, and the reaction required time shortens greatly.
2, the present invention is because extraction process weak point consuming time by improving cycle index, can greatly reduce consumption and the consumption of extraction agent.
3, the present invention adopts and carries out selective extraction under the microfluid laminar flow condition, can avoid extraction process emulsion to occur.
4, the invention enables the foreign metal high efficiency separation such as In and Fe and Zn, extraction selectivity is very superior.
5, the present invention carries out in closed system in the assurance reaction, and the condition controllability is strong, and is safe, avoided the extraction organic solvent to be exposed in the air, produces the danger of volatilization and fire.
Description of drawings
Fig. 1 is the device synoptic diagram of microreactor of the present invention;
Fig. 2 is the schematic cross-section of embodiment 1 microchannel.
Embodiment
The present invention will be further described below by embodiment.
Embodiment 1
The sulfuric acid system solution (leach liquor in the hydrometallurgy zinc process) that (1) will contain indium 4.52g/L, iron, zinc is as water, pass into respectively in two flow pumps as organic phase through the P204 extraction agent (30% volume fraction P204+70% volume fraction solvent oil) of No. 260 solvent oil dilutions, and the exit end of flow pump connects the microreactor entrance;
(2) open first organic phase flow pump, (characteristic dimension is 160 μ m to treat organic phase to enter the microchannel of microreactor, length is 380mm) after, pressing 0.65 times of the organic phase flow sets and open water phase flow rate pump again, (microscope is overlooked observation can see that water and organic phase are in the microchannel that the left and right sides is parallel advances to two-phase laminar flow phase interface by forming in the observation by light microscope microchannel simultaneously, two-phase laminar flow phase interface is the contact surface of water and organic phase), regulate during this time the flow of two-phase, make the two-phase split flow, the duration of contact of two-phase in the microchannel is 1.49s;
Begin to separate when (3) two phase flow is to the place, Y type fork of microchannel outlet, flow out microreactor from outlet separately, and two-phase is collected respectively, indium is extracted and enters organic phase, and iron and zinc are kept aqueous phase, has realized separating of indium and iron, zinc.Detection obtains 92.50% In percentage extraction, and system is without the emulsification phenomenon.
Embodiment 2
The sulfuric acid system solution (leach liquor in the hydrometallurgy zinc process) that (1) will contain indium 3.17g/L, iron 3.42g/L, zinc 52.82g/L is as water, pass into respectively in two flow pumps as organic phase through the P204 extraction agent (30% volume fraction P204+70% volume fraction solvent oil) of conventional solvent oil dilution, and the exit end of flow pump connects the microreactor entrance;
(2) open first organic phase flow pump, (characteristic dimension is 200 μ m to treat organic phase to enter the microchannel of microreactor, length is 80mm) after, pressing 0.65 times of the organic phase flow sets and open water phase flow rate pump again, (microscope is overlooked observation can see that water and organic phase are in the microchannel that the left and right sides is parallel advances to two-phase laminar flow phase interface by forming in the observation by light microscope microchannel simultaneously, two-phase laminar flow phase interface is the contact surface of water and organic phase), regulate during this time the flow of two-phase, make the two-phase split flow, the duration of contact of two-phase in the microchannel is 0.69s;
Begin to separate when (3) two phase flow is to the place, Y type fork of microchannel outlet, flow out microreactor from outlet separately, and two-phase is collected respectively, indium is extracted and enters organic phase, and iron and zinc are kept aqueous phase, has realized separating of indium and iron, zinc.Detection obtains 90.80% In percentage extraction, and the percentage extraction of Fe, Zn is 0, and system is without the emulsification phenomenon.
Embodiment 3
The sulfuric acid system solution (leach liquor in the hydrometallurgy zinc process) that (1) will contain indium 4.12g/L, iron, zinc is as water, pass into respectively as organic phase in two flow pumps through the P204 extraction agent of conventional solvent oil dilution, and the exit end of flow pump connects the microreactor entrance;
(2) open first organic phase flow pump, (characteristic dimension is 800 μ m to treat organic phase to enter the microchannel of microreactor, length is 90mm) after, pressing 0.65 times of the organic phase flow sets and open water phase flow rate pump again, (microscope is overlooked observation can see that water and organic phase are in the microchannel that the left and right sides is parallel advances to two-phase laminar flow phase interface by forming in the observation by light microscope microchannel simultaneously, two-phase laminar flow phase interface is the contact surface of water and organic phase), regulate during this time the flow of two-phase, make the two-phase split flow, the duration of contact of two-phase in the microchannel is 0.01s;
Begin to separate when (3) two phase flow is to the place, Y type fork of microchannel outlet, flow out microreactor from outlet separately, and two-phase is collected respectively, indium is extracted and enters organic phase, and iron and zinc are kept aqueous phase, has realized separating of indium and iron, zinc.Detection obtains 92.10% In percentage extraction, and system is without the emulsification phenomenon.
Embodiment 4
The sulfuric acid system solution (leach liquor in the hydrometallurgy zinc process) that (1) will contain indium 3.92g/L, iron, zinc is as water, pass into respectively as organic phase in two flow pumps through the P204 extraction agent of No. 260 solvent oil dilutions, and the exit end of flow pump connects the microreactor entrance;
(2) open first organic phase flow pump, (characteristic dimension is 700 μ m to treat organic phase to enter the microchannel of microreactor, after length is 480mm, pressing 0.65 times of the organic phase flow sets and open water phase flow rate pump again, (microscope is overlooked observation can see that water and organic phase are in the microchannel that the left and right sides is parallel advances to two-phase laminar flow phase interface by forming in the observation by light microscope microchannel simultaneously, two-phase laminar flow phase interface is the contact surface of water and organic phase), regulate during this time the flow of two-phase, make the two-phase split flow, the duration of contact of two-phase in the microchannel is 10s;
Begin to separate when (3) two phase flow is to the place, Y type fork of microchannel outlet, flow out microreactor from outlet separately, and two-phase is collected respectively, indium is extracted and enters organic phase, and iron and zinc are kept aqueous phase, has realized separating of indium and iron, zinc.Detection obtains 91.86% In percentage extraction, and system is without the emulsification phenomenon.
Claims (5)
1. the microfluid extracting process of an extracting and separating In and Fe, Zn is characterized in that through following each step:
The sulfuric acid system solution that (1) will contain indium, iron, zinc is as water, pass into respectively as organic phase in two flow pumps through the P204 extraction agent of solvent oil dilution, and the exit end of flow pump connects the microreactor entrance;
(2) open first organic phase flow pump, enter the microchannel of microreactor until organic phase after, pressing 0.65 times of the organic phase flow sets and open water phase flow rate pump again, pass through simultaneously the two-phase laminar flow phase interface of formation in the observation by light microscope microchannel, regulate during this time the flow of two-phase, make the two-phase split flow;
Begin to separate when (3) two phase flow is to the place, Y type fork of microchannel outlet, flow out microreactor from outlet separately, and two-phase is collected respectively, indium is extracted and enters organic phase, and iron and zinc are kept aqueous phase, has realized separating of indium and iron, zinc.
2. the microfluid extracting process of extracting and separating In according to claim 1 and Fe, Zn, it is characterized in that: the described sulfuric acid system solution that contains indium, iron, zinc is the leach liquor in the hydrometallurgy zinc process.
3. the microfluid extracting process of extracting and separating In according to claim 1 and Fe, Zn, it is characterized in that: described solvent oil is conventional solvent oil.
4. the microfluid extracting process of extracting and separating In according to claim 1 and Fe, Zn, it is characterized in that: the characteristic dimension of described microchannel is 160～800 μ m, and length is 80～480mm.
5. the microfluid extracting process of extracting and separating In according to claim 1 and Fe, Zn is characterized in that: the duration of contact of described two-phase in the microchannel is 0.01～10s.
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| CN103667697A (en) * | 2013-12-11 | 2014-03-26 | 昆明理工大学 | Method for extracting zinc from low-concentration zinc sulfate solution |
| CN104232895A (en) * | 2014-09-05 | 2014-12-24 | 昆明理工大学 | Method of extracting indium from solution by adopting impinging stream-rotating packed bed extractor |
| CN105112658A (en) * | 2015-08-28 | 2015-12-02 | 昆明理工大学 | Method for extracting rare-earth elements through micro channels |
| WO2016004458A1 (en) * | 2014-07-08 | 2016-01-14 | University Of South Australia | Extraction of precious metals |
| CN105274335A (en) * | 2015-11-04 | 2016-01-27 | 昆明理工大学 | Method for extracting and separating copper from iron and zinc through segmented flow type micro-fluid |
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| CN103667697A (en) * | 2013-12-11 | 2014-03-26 | 昆明理工大学 | Method for extracting zinc from low-concentration zinc sulfate solution |
| CN103667697B (en) * | 2013-12-11 | 2015-09-16 | 昆明理工大学 | A kind of method of extracting zinc from low-concentration sulfuric acid zinc solution |
| WO2016004458A1 (en) * | 2014-07-08 | 2016-01-14 | University Of South Australia | Extraction of precious metals |
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| CN105112658A (en) * | 2015-08-28 | 2015-12-02 | 昆明理工大学 | Method for extracting rare-earth elements through micro channels |
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| CN105598464B (en) * | 2016-01-06 | 2017-10-24 | 哈尔滨工业大学（威海） | The in-situ preparation method of copper nano-wire in a kind of microchannel |
| CN105598464A (en) * | 2016-01-06 | 2016-05-25 | 哈尔滨工业大学（威海） | In-situ preparation method of copper nanowires in microchannel |
| CN106902544A (en) * | 2017-03-23 | 2017-06-30 | 昆明理工大学 | A kind of continuous polyfunctional reactant device of microfluid extraction back extraction and its application process |
| CN108359811A (en) * | 2018-03-07 | 2018-08-03 | 昆明理工大学 | A method of being stripped cobalt using micro-fluidic technologies |
| CN108771884A (en) * | 2018-05-08 | 2018-11-09 | 昆明理工大学 | A kind of combined type hybrid extraction device and method |
| CN111185029A (en) * | 2020-01-09 | 2020-05-22 | 昆明理工大学 | Multi-metal ion extraction device and method based on micro-fluidic chip and extraction rate calculation method |
| CN113392596A (en) * | 2021-04-25 | 2021-09-14 | 四川大学 | Method for extracting and separating scandium-iron solution by using microchannel reactor |
| CN116251380A (en) * | 2023-03-16 | 2023-06-13 | 福州大学 | Extraction method for high-phase-ratio system |
| CN116251380B (en) * | 2023-03-16 | 2024-06-04 | 福州大学 | Extraction method for high-phase-ratio system |
| CN117438123A (en) * | 2023-12-22 | 2024-01-23 | 中国核电工程有限公司 | Method and device for determining uranium extraction zone in extraction column and method for controlling position of uranium extraction zone |
| CN117438123B (en) * | 2023-12-22 | 2024-05-07 | 中国核电工程有限公司 | Method and device for determining uranium extraction zone in extraction column and method for controlling position of uranium extraction zone |
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