CN105274335A - Method for extracting and separating copper from iron and zinc through segmented flow type micro-fluid - Google Patents
Method for extracting and separating copper from iron and zinc through segmented flow type micro-fluid Download PDFInfo
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- CN105274335A CN105274335A CN201510739776.XA CN201510739776A CN105274335A CN 105274335 A CN105274335 A CN 105274335A CN 201510739776 A CN201510739776 A CN 201510739776A CN 105274335 A CN105274335 A CN 105274335A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 239000010949 copper Substances 0.000 title claims abstract description 73
- 239000011701 zinc Substances 0.000 title claims abstract description 54
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 52
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 48
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 36
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000012530 fluid Substances 0.000 title abstract description 4
- 238000000605 extraction Methods 0.000 claims abstract description 89
- 239000012071 phase Substances 0.000 claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 20
- UWGTVLYQSJNUFP-SILNSSARSA-N 4-dodecyl-2-[(Z)-hydroxyiminomethyl]phenol Chemical compound [H]\C(=N\O)C1=C(O)C=CC(CCCCCCCCCCCC)=C1 UWGTVLYQSJNUFP-SILNSSARSA-N 0.000 claims abstract description 15
- UHSURKDCQCGNGM-UHFFFAOYSA-N 5-(2-hydroxyimino-2-phenylethyl)nonan-2-ol Chemical compound CCCCC(CCC(C)O)CC(=NO)C1=CC=CC=C1 UHSURKDCQCGNGM-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000012074 organic phase Substances 0.000 claims abstract description 9
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000008346 aqueous phase Substances 0.000 claims description 35
- 230000011218 segmentation Effects 0.000 claims description 28
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 8
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 8
- KFZAUHNPPZCSCR-UHFFFAOYSA-N iron zinc Chemical compound [Fe].[Zn] KFZAUHNPPZCSCR-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 4
- 238000013517 stratification Methods 0.000 claims description 4
- -1 polydimethylsiloxane Polymers 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 238000000926 separation method Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000003085 diluting agent Substances 0.000 abstract 1
- 239000000839 emulsion Substances 0.000 description 12
- 230000008569 process Effects 0.000 description 11
- 238000012546 transfer Methods 0.000 description 8
- 238000001514 detection method Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010977 unit operation Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 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
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000005514 two-phase flow Effects 0.000 description 1
- 238000004148 unit process Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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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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- Manufacture And Refinement Of Metals (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a method for extracting and separating copper from iron and zinc through segmented flow type micro-fluid, and belongs to the technical field of fluid extraction. A sulfuric acid system containing the copper, the iron and the zinc is used as a water phase, and an oil phase is formed by taking 5-dodecyl salicylaldoxime and 2-hydroxy-5-nonylacetophenone oxime as extraction agents and number 260 solvent oil as a diluent; the water phase and the oil phase enter a cross type micro-channel through a pump, and the flow speed is controlled to be 0.01 mL/min-10 mL/min; after a segmented flow reaction is performed for 0.1-20 s under the condition that the temperature ranges from 25 DEG C to 50 DEG C, products are collected from the outlet of the cross type micro-channel and stand to be layered; and Cu2+ is extracted and enters an organic phase, Fe3+, Fe2+ and Zn2+ remain in the water phase, and thus the copper is separated from the iron and the zinc. The method has the advantages of being high in efficiency, safe, low in cost, free of pollution and high in separation rate.
Description
Technical field
The present invention relates to a kind of method of segmentation flow pattern microfluid extracting and separating copper and iron, zinc, belong to fluid extraction technology field.
Background technology
Since the nineties in 20th century, an important trend of natural science and engineering development is microminiaturized, and the mixing tank required for chemical engineering unit operation, interchanger, resorber, extractor, reactor and Controlling System etc. together form micro-chemical system.In whole micro-Chemical Engineering Technology, microreactor is in occupation of core status, and its flowing has microfluidic feature.Although utilize microreactor can not change reaction mechanism and intrinsic kinetics characteristic, but micro-fluidic technologies can strengthen chemical process by the heat transfer of alter, mass transfer and flow characteristics.Traditional reactor by lab scale-pilot scale-scale operation step by step iodine equipment realize the raising of its processing power, and each passage in microfluidic reactor system is all equivalent to an independently reactor, number increasing superposition " Numbering-up " mode adopting parallel work-flow is amplified in industry, namely processing power is improved by increasing number of unit, the microreactor amplified by this mode has plurality of advantages: the time that industry is amplified shortens greatly, actual production handiness improves, the security of production operation process improves, and reaches the requirement of industrial application.If compared with conventional yardstick reactor, the slight refinement of characteristic dimension is just enough to improve micro-reactive system to a great extent, as bigger serface, greatly than phase contact area, volume is little, directly parallel amplification, process are continuously, highly integrated, mixing time is short, energy consumption is low, technique greenization etc.Within the scope of smaller size smaller, achieve carrying out continuously of chemical reaction, still can ensure large-scale commercial production when equipment volume significantly reduces, be considered to an important breakthrough of modern chemical industry idea of development.
Copper is heavy metal element, has red metalluster, has excellent electrical and thermal conductivity performance.Be widely used in electrically, light industry, machinofacture, building industry, the field such as national defense industry.For process oxidized ore, low-grade abandoned mine and complicated difficult ore dressing, it is main for mainly smelting in a wet process.And solvent extraction is wherein very important unit operation, but still there is the key issue that some need to solve in traditional solvent extraction method:
A, extraction agent consumption are large
Due to extraction, Stripping times is relatively long, often needs multi-stage solvent extraction, and in order to adapt to the requirement of extraction mass transfer, Solvent quantity is large.In addition, extraction agent and air contact surfaces amass large, and the impact by envrionment temperature is large, and volatilization is serious, and the shearing force of high-energy stirring process may be destroyed extractant molecules structure and cause the problems such as temperature rise.
B, altogether extraction are serious, and 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 also needs multistage washing and back extraction after causing extraction.As with in P204 extracting and separating Ni, Co process due to exist extraction Co time Fe, Zn, Mn and Cu common extraction, and make whole extraction progression reach more than 18 grades, for another example with in P204 extracting and separating In process owing to there is the common extraction problem of Fe, Zn, Sb, Bi and Cl etc., make whole extraction progression reach more than 14 grades.This considerably increases cost of investment, reduce extraction efficiency.
C, easily there is emulsion
About the mechanism producing emulsification in indium extraction process, all conduct in-depth research both at home and abroad at present, and propose a lot of preventive measures.But up to the present, emulsion can not well be avoided.Trace it to its cause; due to for having particle, certain metal ion species or comprising the omplicated solution system of tensio-active agent; high energy mixing due to conventional extraction extraction process is carried out very fully and rapidly; but in phase separation; stable protective layer is become due on the liquid-liquid interface that stability particle (as particle colloid) is adsorbed on emulsion particle; two-phase droplet coalescence speed is become slowly stop even completely, and be very large from the interface energy removed needed for a particle.This namely breakdown of emulsion difficulty and need the basic reason inputting large energy.
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 organic phase big area exposes in atmosphere, makes disaster hidden-trouble larger.In recent years, Chinese large-sized smeltery just there occurs a lot of extraction plant fire casualty, and the extraction process of some small-sized smelteries also takes place frequently fire failure.
Therefore, these limitation of conventional extraction are urgently to be resolved hurrily, and the exploitation of airtight, efficient extraction equipment is the key point addressed this problem.Cross type microchannel, segmentation stream can be formed when two-phase current difference reaches certain value, because the interface renewal speed of drop is fast, the interfacial area comparing water-oil phase with laminar flow is large, rate of mass transfer is caused to increase, thus enhancing mixed, and conventional hybrid contrast, drop is even, does not have meticulous drop thus avoids emulsion.
Utilize the features such as efficient, the low consumption of microreactor system, safety to transform the poor efficiency high consumption unit process of conventional metallurgical industry as extraction, heat exchange and mixing etc., likely develop the energy-saving technique process made new advances, thus promote the industrial upgrading of metallurgy industry.Up to now, there is not yet the research carrying out copper, iron extracting and separating with micro-fluidic technologies, the invention provides a kind of operational path of extracting and separating copper, iron in microreactor.
Summary of the invention
For above-mentioned prior art Problems existing and deficiency, the invention provides a kind of method of segmentation flow pattern microfluid extracting and separating copper and iron, zinc.Present method overcomes that the extraction efficiency of conventional solvent extracting copper is low, the easy emulsification of solution, copper and the magazins' layout such as iron, zinc difficulty, environmental pollution is serious, the shortcomings such as dangerous height, present method has efficiently, safety, low cost, the advantage that pollution-free, separation rate is high, the present invention is achieved through the following technical solutions.
A kind of method of segmentation flow pattern microfluid extracting and separating copper and iron, zinc, using the sulfuric acid system containing copper, iron, zinc as aqueous phase, using the oil phase that 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime form as extraction agent and 260# solvent oil as thinner, aqueous phase and oil phase are entered cross type microchannel by pump, coutroi velocity is 0.01mL/min ~ 10mL/min, under temperature is 25 ~ 50 DEG C of conditions after segmentation stream reaction 0.1s ~ 20s, in cross type microchannel, outlet collects product and stratification, Cu
2+extraction enters organic phase, Fe
3+, Fe
2+, Zn
2+stay in aqueous phase, realize being separated of copper and iron zinc.
Containing Cu in the described sulfuric acid system containing copper, iron, zinc
2+0.01g/L ~ 15g/L, full iron 0.01g/L ~ 15g/L.
In described oil phase, the percent by volume of extraction agent is 5% ~ 25%.
In described extraction agent, the volume ratio of 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime is 1:1.
Described is standing 1s at cross type microchannel outlet stratification.
Described cross type microchannel width is 100 μm ~ 1000 μm, and the degree of depth is 50 μm ~ 100 μm, and length is 100mm ~ 500mm.
Described cross type microchannel material is polydimethylsiloxane (PDMS), and processing mode, for build PDMS material in the template of microchannel, is treated that PDMS carries out the demoulding after solidifying subsequently, finally the PDMS after the demoulding and substrate sealed.
Inventive principle of the present invention is: because microchannel is in micron level, and have high specific surface area, diffusion length is short, and concentration gradient is large, can effectively promote mass transfer and heat transfer, make the time reaching extraction equilibrium improve an order of magnitude.In addition, because oil phase and aqueous phase convection current enter in cross type microchannel, oil phase can smash by aqueous phase becomes many small dropletss, thus aqueous phase be external phase, oil phase is the segmentation stream of disperse phase, and then considerably increase two-phase contact area, improve specific surface area, greatly enhance extraction mass transfer process, make it reach extraction equilibrium at Millisecond.
The present invention uses cross type microchannel, makes two-phase liquid keep segmentation stream in cross type microchannel, and facilitated extraction reacts, and collects and leave standstill product in channel outlet, realizes copper, iron is separated, Cu
2+percentage extraction can reach more than 99%, and the percentage extraction of full iron is below 1%, and the percentage extraction of zinc is zero substantially, does not occur emulsion, thus avoids the series of problems of extracting and separating copper, iron in conventional wet metallurgy.Copper is carried out in cross type microchannel, iron extracting and separating specifically has superior performance, and extraction efficiency is high, and strong to the selectivity of copper, phase-splitting is rapid, and single-stage extraction rate is high, and process is simple, and being easy to control, is a kind of green, efficient, simple and direct extraction separating method.
The invention has the beneficial effects as follows:
1, the present invention adopts the cross type microchannel that can produce segmentation stream to carry out copper, iron extracting and separating, and the time shorten of extraction equilibrium is person of outstanding talent's level scope second, and single-stage extraction rate can reach more than 99%, greatly strengthens the selectivity of copper, iron, zinc.
2, water-oil phase is separated rapidly, does not occur emulsion.
3, owing to shortening the time of extraction equilibrium, improve the cycle index of extraction agent, reduce the consumption of extraction agent.
4, extractive reaction carries out in cross type microchannel, and condition controllability is strong, avoids and directly contacts with air, eliminate disaster hidden-trouble, and security improves.
5, employing has PDMS(polydimethylsiloxane) be cross type microchannel material, cost is low, and microchannel complete processing is simple, and handled easily, is easy to observe two phase flow signals online.
6, the segmentation stream of cross type microchannel generation, makes the interfacial area of oil phase and aqueous phase greatly improve, enhances extraction mass transfer process.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The method of this segmentation flow pattern microfluid extracting and separating copper and iron, zinc, by the sulfuric acid system containing copper, iron, zinc (containing Cu
2+3g/L, full iron 2g/L, Zn
2+1g/L) as aqueous phase, aqueous phase pH is regulated to be 2, using the oil phase (in oil phase, the percent by volume of extraction agent is for 25%) that 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime form as extraction agent (in extraction agent, the volume ratio of 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime is for 1:1) and 260# solvent oil as thinner, aqueous phase and oil phase (aqueous phase and oil phase are in a ratio of 1:1 according to water oil) are entered cross type microchannel by pump, and (cross type microchannel width is 200 μm, the degree of depth is 50 μm, length is 100mm) two entrances, coutroi velocity is 0.05mL/min, under temperature is 25 DEG C of conditions after segmentation stream reaction 0.6s, collect product in the outlet of cross type microchannel and leave standstill 1s layering, Cu
2+extraction enters organic phase, Fe
3+, Fe
2+, Zn
2+stay in aqueous phase, realize being separated of copper and iron zinc.
Emulsion is there is not in the experimentation of the present embodiment.Detection obtains Cu
2+percentage extraction be 99.36%, the percentage extraction of full iron is 0.089%, Zn
2+percentage extraction be 0 substantially, achieve Cu
2+with Fe
2+, Fe
3+, Zn
2+separation.
Embodiment 2
The method of this segmentation flow pattern microfluid extracting and separating copper and iron, zinc, by the sulfuric acid system containing copper, iron, zinc (containing Cu
2+3g/L, full iron 2g/L, Zn
2+1g/L) as aqueous phase, aqueous phase pH is regulated to be 2, using the oil phase (in oil phase, the percent by volume of extraction agent is for 15%) that 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime form as extraction agent (in extraction agent, the volume ratio of 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime is for 1:1) and 260# solvent oil as thinner, aqueous phase and oil phase (aqueous phase and oil phase are in a ratio of 1:1 according to water oil) are entered cross type microchannel by pump, and (cross type microchannel width is 300 μm, the degree of depth is 100 μm, length is 200mm) two entrances, coutroi velocity is 0.1mL/min, under temperature is 50 DEG C of conditions, after segmentation stream reaction 1.8s, collect product in the outlet of cross type microchannel and leave standstill 1s layering, Cu
2+extraction enters organic phase, Fe
3+, Fe
2+, Zn
2+stay in aqueous phase, realize being separated of copper and iron zinc.
Emulsion is there is not in the experimentation of the present embodiment.Detection obtains Cu
2+percentage extraction be 99.15%, the percentage extraction of full iron is 0.076%, Zn
2+percentage extraction be 0 substantially, achieve Cu
2+with Fe
2+, Fe
3+, Zn
2+separation.
Embodiment 3
The method of this segmentation flow pattern microfluid extracting and separating copper and iron, zinc, by the sulfuric acid system containing copper, iron, zinc (containing Cu
2+3g/L, full iron 2g/L, Zn
2+1g/L) as aqueous phase, aqueous phase pH is regulated to be 2, using the oil phase (in oil phase, the percent by volume of extraction agent is for 15%) that 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime form as extraction agent (in extraction agent, the volume ratio of 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime is for 1:1) and 260# solvent oil as thinner, aqueous phase and oil phase (aqueous phase and oil phase are in a ratio of 1:1 according to water oil) are entered cross type microchannel by pump, and (cross type microchannel width is 600 μm, the degree of depth is 100 μm, length is 300mm) two entrances, coutroi velocity is 0.15mL/min, under temperature is 50 DEG C of conditions after segmentation stream reaction 3.6s, collect product in the outlet of cross type microchannel and leave standstill 1s layering, Cu
2+extraction enters organic phase, Fe
3+, Fe
2+, Zn
2+stay in aqueous phase, realize being separated of copper and iron zinc.
Emulsion is there is not in the experimentation of the present embodiment.Detection obtains Cu
2+percentage extraction be 99.23%, the percentage extraction of full iron is 0.095%, Zn
2+percentage extraction be 0 substantially, achieve Cu
2+with Fe
2+, Fe
3+, Zn
2+separation.
Embodiment 4
The method of this segmentation flow pattern microfluid extracting and separating copper and iron, zinc, by the sulfuric acid system containing copper, iron, zinc (containing Cu
2+15g/L, full iron 15g/L, Zn
2+1g/L) as aqueous phase, aqueous phase pH is regulated to be 2, using the oil phase (in oil phase, the percent by volume of extraction agent is for 5%) that 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime form as extraction agent (in extraction agent, the volume ratio of 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime is for 1:1) and 260# solvent oil as thinner, aqueous phase and oil phase (aqueous phase and oil phase are in a ratio of 1:1 according to water oil) are entered cross type microchannel by pump, and (cross type microchannel width is 100 μm, the degree of depth is 80 μm, length is 500mm) two entrances, coutroi velocity is 0.01mL/min, under temperature is 40 DEG C of conditions after segmentation stream reaction 0.1s, collect product in the outlet of cross type microchannel and leave standstill 1s layering, Cu
2+extraction enters organic phase, Fe
3+, Fe
2+, Zn
2+stay in aqueous phase, realize being separated of copper and iron zinc.
Emulsion is there is not in the experimentation of the present embodiment.Detection obtains Cu
2+percentage extraction be 99.28%, the percentage extraction of full iron is 0.086%, Zn
2+percentage extraction be 0 substantially, achieve Cu
2+with Fe
2+, Fe
3+, Zn
2+separation.
Embodiment 5
The method of this segmentation flow pattern microfluid extracting and separating copper and iron, zinc, by the sulfuric acid system containing copper, iron, zinc (containing Cu
2+0.01g/L, full iron 0.01g/L, Zn
2+1g/L) as aqueous phase, aqueous phase pH is regulated to be 2, using the oil phase (in oil phase, the percent by volume of extraction agent is for 20%) that 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime form as extraction agent (in extraction agent, the volume ratio of 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime is for 1:1) and 260# solvent oil as thinner, aqueous phase and oil phase (aqueous phase and oil phase are in a ratio of 1:1 according to water oil) are entered cross type microchannel by pump, and (cross type microchannel width is 1000 μm, the degree of depth is 90 μm, length is 400mm) two entrances, coutroi velocity is 10mL/min, under temperature is 40 DEG C of conditions after segmentation stream reaction 20s, collect product in the outlet of cross type microchannel and leave standstill 1s layering, Cu
2+extraction enters organic phase, Fe
3+, Fe
2+, Zn
2+stay in aqueous phase, realize being separated of copper and iron zinc.
Emulsion is there is not in the experimentation of the present embodiment.Detection obtains Cu
2+percentage extraction be 99.35%, the percentage extraction of full iron is 0.018%, Zn
2+percentage extraction be 0 substantially, achieve Cu
2+with Fe
2+, Fe
3+, Zn
2+separation.
Above the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (7)
1. the method for a segmentation flow pattern microfluid extracting and separating copper and iron, zinc, it is characterized in that: using the sulfuric acid system containing copper, iron, zinc as aqueous phase, using the oil phase that 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime form as extraction agent and 260# solvent oil as thinner, aqueous phase and oil phase are entered cross type microchannel by pump, coutroi velocity is 0.01mL/min ~ 10mL/min, under temperature is 25 ~ 50 DEG C of conditions after segmentation stream reaction 0.1s ~ 20s, in cross type microchannel, outlet collects product and stratification, Cu
2+extraction enters organic phase, Fe
3+, Fe
2+, Zn
2+stay in aqueous phase, realize being separated of copper and iron zinc.
2. the method for segmentation flow pattern microfluid extracting and separating copper according to claim 1 and iron, zinc, is characterized in that: containing Cu in the described sulfuric acid system containing copper, iron, zinc
2+0.01g/L ~ 15g/L, full iron 0.01g/L ~ 15g/L.
3., according to the method for the arbitrarily described segmentation flow pattern microfluid extracting and separating copper of claims 1 to 3 and iron, zinc, it is characterized in that: in described oil phase, the percent by volume of extraction agent is 5% ~ 25%.
4. the method for segmentation flow pattern microfluid extracting and separating copper according to claim 4 and iron, zinc, is characterized in that: in described extraction agent, the volume ratio of 5-dodecylsalicylaldoxime and 2-hydroxyl-5-nonylacetophenone oxime is 1:1.
5. the method for segmentation flow pattern microfluid extracting and separating copper according to claim 1 and iron, zinc, is characterized in that: described at cross type microchannel outlet stratification for leaving standstill 1s.
6. the method for segmentation flow pattern microfluid extracting and separating copper according to claim 1 and iron, zinc, it is characterized in that: described cross type microchannel width is 100 μm ~ 1000 μm, the degree of depth is 50 μm ~ 100 μm, and length is 100mm ~ 500mm.
7. the method for segmentation flow pattern microfluid extracting and separating copper according to claim 1 and iron, zinc, is characterized in that: described cross type microchannel material is polydimethylsiloxane.
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