CN105274335B - A kind of segmentation flow pattern microfluid extract and separate copper and iron, the method for zinc - Google Patents
A kind of segmentation flow pattern microfluid extract and separate copper and iron, the method for zinc Download PDFInfo
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- CN105274335B CN105274335B CN201510739776.XA CN201510739776A CN105274335B CN 105274335 B CN105274335 B CN 105274335B CN 201510739776 A CN201510739776 A CN 201510739776A CN 105274335 B CN105274335 B CN 105274335B
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Abstract
The present invention relates to a kind of segmentation flow pattern microfluid extract and separate copper and iron, the method for zinc, belong to fluid extraction technology field.The sulfuric acid system of copper, iron, zinc will be contained as aqueous phase, the oil phase formed using 5 dodecylsalicylaldoximes and the nonylacetophenone oxime of 2 hydroxyl 5 as extractant and 260# solvent naphthas as diluent, aqueous phase and oil phase are entered into cross type microchannel by pump, coutroi velocity is 0.01mL/min~10mL/min, under the conditions of being 25~50 DEG C in temperature after segmentation stream reaction 0.1s~20s, exported in cross type microchannel and collect product and stratification, Cu2+Extraction enters organic phase, Fe3+、Fe2+、Zn2+Stay in aqueous phase, realize the separation of copper and iron zinc.This method has the advantages of efficient, safety, low cost, pollution-free, separation rate is high.
Description
Technical field
The present invention relates to a kind of segmentation flow pattern microfluid extract and separate copper and iron, the method for zinc, belong to fluid extraction technology
Field.
Background technology
Since the 1990s, an important trend of natural science and engineering development is to be miniaturized, chemical industry list
Blender, heat exchanger, absorber, extractor, reactor and control system required for atom operation etc. together form macro work
System.In whole micro- Chemical Engineering Technology, microreactor has microfluidic feature in occupation of core status, its flowing.Using micro-
Although reactor can not change reaction mechanism and intrinsic kinetics characteristic, but micro-fluidic technologies can be by changing fluid
Heat transfer, mass transfer and flow behavior strengthen chemical process.Traditional reactor is put step by step by lab scale-pilot scale-large-scale production
Big consersion unit realizes the raising of its disposal ability, and each passage in microfluidic reactor system is equivalent to one
Independent reactor, industry amplification increase superposition " Numbering-up " mode using the number of parallel work-flow, that is, pass through adding unit
Number improves disposal ability, and the microreactor amplified by this mode has many advantages, such as：The time of industry amplification contracts significantly
Short, actual production flexibility improves, and the security of production operation process improves, and reaches the requirement of commercial Application.If with routine
Yardstick reactor is compared, and the pico- refinement of characteristic dimension is just enough largely to improve micro- reaction system, such as big ratio
Surface area, greatly than phase contact area, small volume, directly parallel amplification, process is continuous, highly integrated, incorporation time is short, energy consumption is low,
Technique greenization etc..Being carried out continuously for chemical reaction is realized in the range of smaller size smaller, is significantly reduced in equipment volume
In the case of still ensure that large-scale industrial production, it is considered to be an important breakthrough of modern chemical industry idea of development.
Copper is heavy metal element, has red metallic luster, has excellent electrical and thermal conductivity performance.It is widely used in
Electrically, the field such as light industry, machine-building, building industry, national defense industry.For processing oxide ore, low-grade abandoned mine and complicated difficult
For ore dressing, mainly based on hydrometallurgy.And solvent extraction is wherein very important unit operation, but traditional solvent extracts
Method is taken to still suffer from the key issue that some needs solve：
A, extractant consumption is big
Because extraction, Stripping times are relatively long, multitple extraction is generally required, in order to adapt to extract mass transfer requirement, extraction
Agent dosage is big.In addition, extractant is big with air contact area, influenceed by environment temperature big, volatilization is serious, high-energy stirring process
Shearing force may destroy extractant molecules structure and the problems such as cause temperature rise.
B, co-extraction is serious, and extraction efficiency is low
Under strongly mixing condition, the co-extraction of main metal ion and foreign metal ion is serious, the poor selectivity of extraction, causes
Multistage washing and back extraction are also needed after extraction.Such as with Fe, Zn, Mn when extracting Co due to existing during P204 extract and separates Ni, Co
With Cu co-extraction, and make entirely to extract series and reach more than 18 grades, for another example with during P204 extract and separates In due to occur Fe,
Zn, Sb, Bi and Cl etc. co-extraction problem so that whole extraction series reaches more than 14 grades.This considerably increases cost of investment, drop
Low extraction efficiency.
C, easily there is emulsion
On producing the mechanism of emulsification in indium extraction process, all conduct in-depth research both at home and abroad at present, and propose
Many precautionary measures.But up to the present, emulsion can not avoid well.To find out its cause, it is due to for there are
Particle, certain metal ion species or the complicated solution system comprising surfactant, cause because the high energy of conventional extraction mixes
Extraction process is carried out very fully and rapid, but in phase separation, due to stability particle（Such as particle colloid）Absorption exists
Turn into stable protective layer on the liquid-liquid interface of emulsion particle so that two-phase droplet coalescence speed becomes very slowly even
Stop completely, and the energy removed from interface needed for a particle is very big.This is namely demulsified and difficulty and needs to input
The basic reason of big energy.
D, disaster hidden-trouble is big
Because the extraction process time is longer, it is necessary to build up volume larger tank diameter and depositing reservoir, whole extraction process will
Occupy very big place.And the exposure of organic phase large area is in atmosphere so that disaster hidden-trouble is larger.In recent years, Chinese large-sized
Just there occurs a lot of extraction plant fire casualties, the extraction process of some small-sized smelteries also takes place frequently fire incident for smeltery.
Therefore, these limitations of conventional extraction are urgently to be resolved hurrily, and the exploitation of closed, efficient extraction equipment is that solve this
The key point of one problem.Cross type microchannel, segmentation stream can be formed when two-phase current difference reaches certain value, due to liquid
The interface renewal speed of drop is fast, and it is big to compare the interfacial area of water-oil phase with laminar flow, causes mass transfer rate to increase, mixed so as to strengthen
Close, and conventional hybrid contrast, drop is uniform, without meticulous drop so as to avoiding emulsion.
Using the efficient of microreactor system, low consumption, it is safe the features such as it is single to transform the poorly efficient high consumption of conventional metallurgical industry
First process is such as extracted, exchanges heat and mixed, it is possible to new energy saving technique process is developed, so as to promote the industry of metallurgy industry
Upgrading.So far, there is not yet carrying out the research of copper, iron extract and separate with micro-fluidic technologies, the present invention provides a kind of micro- anti-
Answer the process route of extract and separate copper, iron in device.
The content of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of segmentation flow pattern microfluid extract and separate
Copper and iron, the method for zinc.This method overcomes that the extraction efficiency of conventional solvent extracting copper is low, solution easily emulsifies, copper and iron, zinc etc. are miscellaneous
Matter separation is difficult, and environmental pollution is serious, it is dangerous high the shortcomings of, this method have efficiently, safety, low cost, it is pollution-free, point
The advantages of high from rate, the present invention is achieved through the following technical solutions.
A kind of segmentation flow pattern microfluid extract and separate copper and iron, the method for zinc, the sulfuric acid system containing copper, iron, zinc is made
For aqueous phase, using 5- dodecylsalicylaldoximes and 2- hydroxyl -5- nonylacetophenone oximes as extractant and 260# solvent naphthas as
The oil phase of diluent composition, enters cross type microchannel, coutroi velocity 0.01mL/min by aqueous phase and oil phase by pump
~10mL/min, under the conditions of being 25~50 DEG C in temperature after segmentation stream reaction 0.1s~20s, exported in cross type microchannel
Collect product and stratification, Cu2+Extraction enters organic phase, Fe3+、Fe2+、Zn2+Stay in aqueous phase, realize point of copper and iron zinc
From.
It is described containing copper, iron, zinc sulfuric acid system in contain Cu2+0.01g/L~15g/L, full iron 0.01g/L~15g/L.
The percentage by volume of extractant is 5%~25% in the oil phase.
The volume ratio of 5- dodecylsalicylaldoximes and 2- hydroxyl -5- nonylacetophenone oximes is 1 in the extractant：1.
It is described that stratification is exported in cross type microchannel to stand 1s.
The cross type microchannel width is 100 μm~1000 μm, and depth is 50 μm~100 μm, length 100mm
~500mm.
Cross type microchannel material is dimethyl silicone polymer（PDMS）, processing mode is in microchannel template
On pour PDMS material, then treat PDMS solidification after be stripped, finally the PDMS after the demoulding is sealed with substrate.
The present invention inventive principle be：Because microchannel is in micron level, there is high specific surface area, diffusion length is short,
Concentration gradient is big, can be effectively promoted mass transfer and heat transfer, the time for reaching extraction equilibrium is improved an order of magnitude.In addition,
Because oil phase and aqueous phase convection current enter in cross type microchannel, aqueous phase can smash oil phase as many droplets, so as to
The segmentation stream that aqueous phase is continuous phase, oil phase is dispersed phase, and then two-phase contact area is considerably increased, specific surface area is improved,
Extraction mass transport process is enhanced significantly, it is reached extraction equilibrium in Millisecond.
The present invention uses cross type microchannel, two-phase liquid is kept segmentation in cross type microchannel
Stream, facilitated extraction reaction, collects in channel outlet and stands product, realizes copper, iron separation, Cu2+Extraction yield can reach 99%
More than, and the extraction yield of iron is below 1% entirely, the extraction yield of zinc is substantially zeroed, does not occur emulsion, so as to avoid conventional wet
A series of problems of extract and separate copper, iron in method metallurgy.Cross type microchannel progress copper, iron extract and separate specifically have superior
Performance, extraction efficiency is high, and strong to the selectivity of copper, split-phase is rapid, and single-stage extraction rate is high, and process is simple, easily controllable, is one
Green, efficient, the simple and direct extraction separating method of kind.
The beneficial effects of the invention are as follows：
1st, use of the present invention can produce the cross type microchannel progress copper of segmentation stream, iron extract and separate, and extraction is flat
The time of weighing apparatus shorten to bold and unconstrained second level scope, and single-stage extraction rate greatly reinforces up to more than 99% to the selectivity of copper, iron, zinc.
2nd, water-oil phase is rapidly separated, and does not occur emulsion.
3rd, due to shortening time of extraction equilibrium, the cycle-index of extractant is improved, reduces the consumption of extractant.
4th, extractive reaction is carried out in cross type microchannel, and condition controllability is strong, is avoided and is directly contacted with air,
Disaster hidden-trouble is eliminated, security improves.
5th, using there is PDMS（Dimethyl silicone polymer）For cross type microchannel material, cost is low, microchannel processing
Technique is simple, convenient operation, is easy to observe two phase flow signals online.
6th, segmentation stream caused by cross type microchannel, greatly improves the interfacial area of oil phase and aqueous phase, enhances extraction
Take mass transport process.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
The segmentation flow pattern microfluid extract and separate copper and iron, the method for zinc, by containing copper, iron, zinc sulfuric acid system（Contain
Cu2+3g/L, full iron 2g/L, Zn2+1g/L）As aqueous phase, regulation aqueous phase pH is 2, with 5- dodecylsalicylaldoximes and 2- hydroxyls
Base -5- nonylacetophenone oximes are as extractant（5- dodecylsalicylaldoximes and 2- hydroxyl -5- nonylacetophenone oximes in extractant
Volume ratio be 1：1）The oil phase formed with 260# solvent naphthas as diluent（The percentage by volume of extractant is in oil phase
25%）, by aqueous phase and oil phase（Aqueous phase and oil phase are in a ratio of 1 according to water oil：1）Cross type microchannel is entered by pump（Cross
Chiasma type microchannel width is 200 μm, and depth is 50 μm, length 100mm）Two entrances, coutroi velocity 0.05mL/
Min, under the conditions of being 25 DEG C in temperature after segmentation stream reaction 0.6s, collect product in the outlet of cross type microchannel and stand 1s
Layering, Cu2+Extraction enters organic phase, Fe3+、Fe2+、Zn2+Stay in aqueous phase, realize the separation of copper and iron zinc.
Do not occur emulsion in the experimentation of the present embodiment.Detection obtains Cu2+Extraction yield be 99.36%, full iron
Extraction yield is 0.089%, Zn2+Extraction yield be essentially 0, realize Cu2+With Fe2+、Fe3+、Zn2+Separation.
Embodiment 2
The segmentation flow pattern microfluid extract and separate copper and iron, the method for zinc, by containing copper, iron, zinc sulfuric acid system（Contain
Cu2+3g/L, full iron 2g/L, Zn2+1g/L）As aqueous phase, regulation aqueous phase pH is 2, with 5- dodecylsalicylaldoximes and 2- hydroxyls
Base -5- nonylacetophenone oximes are as extractant（5- dodecylsalicylaldoximes and 2- hydroxyl -5- nonylacetophenone oximes in extractant
Volume ratio be 1：1）The oil phase formed with 260# solvent naphthas as diluent（The percentage by volume of extractant is in oil phase
15%）, by aqueous phase and oil phase（Aqueous phase and oil phase are in a ratio of 1 according to water oil：1）Cross type microchannel is entered by pump（Cross
Chiasma type microchannel width is 300 μm, and depth is 100 μm, length 200mm）Two entrances, coutroi velocity 0.1mL/
Min, under the conditions of temperature is 50 DEG C, after segmentation stream reaction 1.8s, is exported in cross type microchannel and collect product and stand
1s is layered, Cu2+Extraction enters organic phase, Fe3+、Fe2+、Zn2+Stay in aqueous phase, realize the separation of copper and iron zinc.
Do not occur emulsion in the experimentation of the present embodiment.Detection obtains Cu2+Extraction yield be 99.15%, full iron
Extraction yield is 0.076%, Zn2+Extraction yield be essentially 0, realize Cu2+With Fe2+、Fe3+、Zn2+Separation.
Embodiment 3
The segmentation flow pattern microfluid extract and separate copper and iron, the method for zinc, by containing copper, iron, zinc sulfuric acid system（Contain
Cu2+3g/L, full iron 2g/L, Zn2+1g/L）As aqueous phase, regulation aqueous phase pH is 2, with 5- dodecylsalicylaldoximes and 2- hydroxyls
Base -5- nonylacetophenone oximes are as extractant（5- dodecylsalicylaldoximes and 2- hydroxyl -5- nonylacetophenone oximes in extractant
Volume ratio be 1：1）The oil phase formed with 260# solvent naphthas as diluent（The percentage by volume of extractant is in oil phase
15%）, by aqueous phase and oil phase（Aqueous phase and oil phase are in a ratio of 1 according to water oil：1）Cross type microchannel is entered by pump（Cross
Chiasma type microchannel width is 600 μm, and depth is 100 μm, length 300mm）Two entrances, coutroi velocity 0.15mL/
Min, under the conditions of being 50 DEG C in temperature after segmentation stream reaction 3.6s, collect product in the outlet of cross type microchannel and stand 1s
Layering, Cu2+Extraction enters organic phase, Fe3+、Fe2+、Zn2+Stay in aqueous phase, realize the separation of copper and iron zinc.
Do not occur emulsion in the experimentation of the present embodiment.Detection obtains Cu2+Extraction yield be 99.23%, full iron
Extraction yield is 0.095%, Zn2+Extraction yield be essentially 0, realize Cu2+With Fe2+、Fe3+、Zn2+Separation.
Embodiment 4
The segmentation flow pattern microfluid extract and separate copper and iron, the method for zinc, by containing copper, iron, zinc sulfuric acid system（Contain
Cu2+15g/L, full iron 15g/L, Zn2+1g/L）As aqueous phase, regulation aqueous phase pH is 2, with 5- dodecylsalicylaldoximes and 2- hydroxyls
Base -5- nonylacetophenone oximes are as extractant（5- dodecylsalicylaldoximes and 2- hydroxyl -5- nonylacetophenone oximes in extractant
Volume ratio be 1：1）The oil phase formed with 260# solvent naphthas as diluent（The percentage by volume of extractant is 5% in oil phase）,
By aqueous phase and oil phase（Aqueous phase and oil phase are in a ratio of 1 according to water oil：1）Cross type microchannel is entered by pump（Right-angled intersection
Type microchannel width is 100 μm, and depth is 80 μm, length 500mm）Two entrances, coutroi velocity 0.01mL/min,
Under the conditions of temperature is 40 DEG C after segmentation stream reaction 0.1s, collects product in the outlet of cross type microchannel and stand 1s layerings,
Cu2+Extraction enters organic phase, Fe3+、Fe2+、Zn2+Stay in aqueous phase, realize the separation of copper and iron zinc.
Do not occur emulsion in the experimentation of the present embodiment.Detection obtains Cu2+Extraction yield be 99.28%, full iron
Extraction yield is 0.086%, Zn2+Extraction yield be essentially 0, realize Cu2+With Fe2+、Fe3+、Zn2+Separation.
Embodiment 5
The segmentation flow pattern microfluid extract and separate copper and iron, the method for zinc, by containing copper, iron, zinc sulfuric acid system（Contain
Cu2+0.01g/L, full iron 0.01g/L, Zn2+1g/L）As aqueous phase, regulation aqueous phase pH is 2, with 5- dodecylsalicylaldoximes with
2- hydroxyl -5- nonylacetophenone oximes are as extractant（5- dodecylsalicylaldoximes and 2- hydroxyl -5- nonyl benzene second in extractant
The volume ratio of ketoxime is 1：1）The oil phase formed with 260# solvent naphthas as diluent（The percentage by volume of extractant is in oil phase
20%）, by aqueous phase and oil phase（Aqueous phase and oil phase are in a ratio of 1 according to water oil：1）Cross type microchannel is entered by pump（Cross
Chiasma type microchannel width is 1000 μm, and depth is 90 μm, length 400mm）Two entrances, coutroi velocity 10mL/
Min, under the conditions of being 40 DEG C in temperature after segmentation stream reaction 20s, collect product in the outlet of cross type microchannel and stand 1s
Layering, Cu2+Extraction enters organic phase, Fe3+、Fe2+、Zn2+Stay in aqueous phase, realize the separation of copper and iron zinc.
Do not occur emulsion in the experimentation of the present embodiment.Detection obtains Cu2+Extraction yield be 99.35%, full iron
Extraction yield is 0.018%, Zn2+Extraction yield be essentially 0, realize Cu2+With Fe2+、Fe3+、Zn2+Separation.
The embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula, in those of ordinary skill in the art's possessed knowledge, it can also make on the premise of present inventive concept is not departed from
Go out various change.
Claims (7)
1. a kind of segmentation flow pattern microfluid extract and separate copper and iron, the method for zinc, it is characterised in that：By containing copper, iron, zinc sulphur
Acid system is molten as extractant and 260# with 2- hydroxyl -5- nonylacetophenone oximes using 5- dodecylsalicylaldoximes as aqueous phase
Oil phase of the agent oil as diluent composition, enters cross type microchannel, coutroi velocity is by aqueous phase and oil phase by pump
0.01mL/min~10mL/min, under the conditions of being 25~50 DEG C in temperature after segmentation stream reaction 0.1s~20s, in cross type
Collect product and stratification, Cu in microchannel outlet2+Extraction enters organic phase, Fe3+、Fe2+、Zn2+Stay in aqueous phase, realize copper
With the separation of iron zinc.
2. segmentation flow pattern microfluid extract and separate copper according to claim 1 and iron, the method for zinc, it is characterised in that：Institute
State containing copper, iron, zinc sulfuric acid system in contain Cu2+0.01g/L~15g/L, full iron 0.01g/L~15g/L.
3. according to any described segmentation flow pattern microfluid extract and separate copper of claim 1 to 2 and iron, the method for zinc, its feature
It is：The percentage by volume of extractant is 5%~25% in the oil phase.
4. segmentation flow pattern microfluid extract and separate copper according to claim 3 and iron, the method for zinc, it is characterised in that：Institute
It is 1 to state the volume ratio of 5- dodecylsalicylaldoximes and 2- hydroxyl -5- nonylacetophenone oximes in extractant：1.
5. segmentation flow pattern microfluid extract and separate copper according to claim 1 and iron, the method for zinc, it is characterised in that：Institute
It is standing 1s to state in cross type microchannel outlet stratification.
6. segmentation flow pattern microfluid extract and separate copper according to claim 1 and iron, the method for zinc, it is characterised in that：Institute
Cross type microchannel width is stated as 100 μm~1000 μm, depth is 50 μm~100 μm, and length is 100mm~500mm.
7. segmentation flow pattern microfluid extract and separate copper according to claim 1 and iron, the method for zinc, it is characterised in that：Institute
It is dimethyl silicone polymer to state cross type microchannel material.
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| CN103146934B (en) * | 2013-03-11 | 2015-03-04 | 昆明理工大学 | Method for performing extraction separation on cobalt and nickel by using microfluid technology |
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