CN102512848B - Large phase ratio liquid-liquid two-phase continuous extraction apparatus - Google Patents
Large phase ratio liquid-liquid two-phase continuous extraction apparatus Download PDFInfo
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Abstract
A large phase ratio liquid-liquid two-phase continuous extraction apparatus belongs to the field of liquid-liquid extraction and separation. The apparatus contains a tower body, a gas buffer chamber, a liquid film aggregation device, liquid film dispersers, a liquid film distributor, an air-pressure chamber and the like. The liquid film dispersers and the liquid film distributor can be combined together to realize dispersion of small-volume organic phase by the use of tiny bubbles, thus solving the problem that it is not easy to fully disperse small-volume organic phase by a traditional stirring mode. The phase ratio of a light phase to a heavy phase flowing upstream in the tower body can be adjusted by the interlayer gap of the liquid film distributor. The light phase and the heavy phase can be operated by counter current under the condition of super-large phase ratio. A liquid film disperser and a bubble connection cap are arranged at intervals in the tower body, so as to realize repeated coagulation and dispersion of rising bubbles and achieve high stage efficiency of height of mass transfer unit. A liquid film aggregation device on the top of the tower can be used for bubble coagulation and demulsification and is suitable for extraction operation of an easily-emulsified system. The apparatus provided by the invention is applicable to continuous countercurrent operation under the condition of multi-stage series connection.
Description
Technical field
The invention belongs to liquid liquid solvent extraction separation technology field, particularly relate to one and compare greatly liquid-liquid diphase continuous extraction apparatus.
Background technology
Solvent extraction is the important chemical separation technology of a class.In traditional organic phase-water two-phase extraction process, the selection of immiscible oil, water two-phase volume ratio (comparing) or flow-rate ratio (stream than) has often determined in two-phase mixed process which is as decentralized photo, and another is as continuous phase.Therefore, whether suitable the selection of comparing (or stream ratio) is, and the Separation Indexes of final goal thing is had to important impact.Normally, be applicable to the equipment that traditional liquid-liquid two-phase extraction separates, its structural design need to consider to be both conducive to the two-phase mass transport process of specific extraction system, is conducive to again mixed two-phase and is separated fast.Therefore, extraction system two-phase is compared or is flowed than unsuitable excessive.Otherwise, very easily cause two-phase to mix uneven, affect interphase mass transfer efficiency.To some easy emulsification and extraction systems, two-phase is compared or is flowed than excessive, very easily causes alternate carrying secretly especially, and extractant runs off, and extracting operation is restive.According to application target difference, common extraction equipment is mainly divided into three major types: mix-clarification extractor, tower or column extractor, centrifugal extractor.For the operation in mixing-settler extractor, excessive if profit two-phase is compared, certainly will require to increase speed of agitator in mixing chamber, fully disperse with the decentralized photo that ensures small size.So, the settling area of clarifying chamber also corresponding increase, the negative consequence of bringing to offset strong agitation, causes mixed settler extractor floor space excessive, internal solvent stagnant storage in clarifying chamber's is excessive, process operation cost is high.For common tower or column extractor, comparing greatly while operating under condition, the height that need to increase tower or post approaches mass transfer as far as possible and balances each other and realize two and be separated, and this just needs higher factory building.If two-phase flow ratio is excessive, is not especially suitable for extraction system or easy emulsifying system that some two-phase density contrasts are less, otherwise very easily causes the serious two phase flow axial backmixing of generation in extraction tower.Usually, in extraction tower, serious axial backmixing is caused by following factor: (1) continuous phase VELOCITY DISTRIBUTION on flow direction is inhomogeneous; (2) in continuous phase, have eddy current whirlpool, general goal is crossed by local velocity, may carry dispersed phase drop secretly, causes the back-mixing of decentralized photo; (3) droplet size is inhomogeneous, and dispersed phase drop VELOCITY DISTRIBUTION is inhomogeneous, causes the front mixed of part drop; (4), in the time that decentralized photo flow velocity is excessive, can cause the drop back-mixing of continuous phase liquid around.In addition, the extraneous input of extraction tower energy (stirring or pulse) strengthening turbulent flow, though there is the effect of pulverizing drop and strengthening mass transfer, in the time of excessive whipping, also can make back-mixing aggravation.Axial backmixing has a negative impact to the performance of extraction tower, and it has not only reduced mass transfer force, and has reduced the disposal ability of extraction tower.Adopt centrifugal extractor to replace the separation process of gravity hardening constituent with centrifugal force, although can solve the phase-splitting difficult problem that a part causes due to emulsification, but because centrifuge need operate under higher rotation speed, the time that contacts is short, if two-phase is compared excessive, very easily cause phase-splitting incomplete, phase entrainment loss is serious.
In recent years, along with the development of process industrial, traditional liquid-liquid two-phase solvent extraction equipment can not adapt to the application requirements of emerging separation system far away.For example, because of requirements such as financial cost, the extract and separate of biochemical system usually requires to operate comparing greatly under condition.Because the bioactivators such as protein usually have surface-active, extraction process very easily causes emulsification, causes phase process to be difficult to effective control.While comparing greatly lower operation, extractant difficulties in dispersion, phase continuity is restive, and extraction process is balanced each other and the restriction of mass-transfer efficiency is difficult to obtain satisfied separative efficiency.If extraction process is separated, effect is bad, and a part of dissolvent residual, in heavy phase, has not only caused the loss of extractant, and causes the secondary pollution to heavy phase.But improve the loss of its extraction efficiency and ability and minimizing extractant and to often existing contradiction between the secondary pollution of heavy phase, traditional two-phase extraction equipment is difficult to solve more satisfactorily, the separating-purifying of target product has become " bottleneck " of these industry developments of restriction, and its expense often accounts for the more than 50% of whole production cost.On the other hand, solvent extraction has been widely used in the separation and Extraction of each metal ion species as an important procedure in hydrometallurgy process.But in recent years, due to the dilution of resource, the concentration of metal ion in feed liquid to be extracted is more and more lower, cause extracting operation often to need in the face of larger water oil phase ratio.For example, rare earth extraction industry, the separation of middle heavy rare earth element usually needs to solve water oil phase than the difficulty that is greater than 200:1, and water oil two-phase volume ratio is sometimes even up to 1000:1.How to realize and to compare greatly extracting operation from the structural design of extraction and stripping apparatus, become a rare earth extraction separation industries difficult problem in the urgent need to address.
Certain of small size is treated to dispersing liquid is distributed in the immiscible liquid of another kind of large volume, general adopt be mechanical agitation dispersing mode (Fei Weiyang. Liquid-liquid Extraction Processes and equipment. Beijing: Atomic Energy Press, 1993), but the scope of comparing that the method is suitable for little.For easy emulsifying system, the method is more inapplicable.Chinese patent (ZL99122873.1) discloses a kind of liquid injecting mixed device, and a kind of liquid winding-up is separated into small sized particles, is mixed with emulsion with another kind of immiscible liquid (setting it as continuous phase).This invention is not also suitable for and compares greatly operation, and needs to introduce in addition the granule liquid of surfactant with stable dispersion.CN101862549A disclose a kind of large phase ratio easy emulsifying system without clarifying chamber's continuous extraction apparatus.The maximum feature of this device is, has designed a kind of self-priming agitator that disperses mutually.Utilize the rotary centrifugal force of self-absorbing type stirrer, make the decentralized photo for the treatment of of small size pass the micropore dispersion being arranged on a series of hollow concentric circles barrels in the continuous phase of large volume.This invention has solved traditional agitating mode processing and in the time of dispersing liquid small volume, has been difficult for a difficult problem of fully disperseing.Because self-absorbing type stirrer shearing force is low, be specially adapted to the stirring extraction of easy emulsifying system.But while using this self-absorbing type stirrer to promote liquid, comparing or flowing of weight two-phase should not be excessive than still.Particularly compare and be greater than 200 for weight two-phase, even larger extraction system, this device cannot normally be worked.In order to promote the dispersing liquid for the treatment of of micro volume, self-absorbing type stirrer need to be worked under higher rotating speed, and this has just run counter to the design original intention that prevents originally emulsification.Can adapt to although reduce agitator size the demand that small volumes of liquids disperses, the mismatch contradiction of tower body cavity size and little agitator size becomes again outstanding, reduces tower body cavity size and only can cause further reducing for the treatment of capacity.In addition, for the dispersing liquid for the treatment of of unusual small size, self-absorbing type stirrer cannot be differentiated weight two-phase, is usually that two-phase is raised together, causes subsequent operation to be difficult to effective control.
Summary of the invention
For the deficiencies in the prior art, one of object of the present invention is to provide one to compare greatly liquid-liquid diphase continuous extraction apparatus, the difficulty while operation under super large is compared condition to solve weight two-phase.
Principle of the present invention is, adopt a kind of mode that blasts micro-bubble, utilize bubble surface easily to adsorb the principle of hydrophobic organic compound, by dispersed the hydrophobicity organic phase of the small size bubble surface that is adsorbed on, the organic phase that realizes small size is dispersed in the continuous water of large volume with the form of micro-bubble liquid film.Bubble is in the process rising, and its surperficial organic phase liquid film contacts with the continuous water of large volume extraction mass transfer occurs.When the bubble rising is encountered a kind of lipophile porous material surface, bubble breaks, and surperficial organic phase liquid film is sprawled coalescence at porous hydrophobic material surface, thus and aqueous phase separation.
Described one is compared greatly liquid-liquid diphase continuous extraction apparatus and is comprised tower body, gas buffer chamber, liquid film coalescence device, liquid film disperser, liquid film distributor, air-pressure chamber, and its concrete structure is:
Tower body 10 is cavity structure, gas buffer chamber 4 is positioned at tower body 10 tops, gas buffer chamber (4) closing cap for upper end (1) sealing, liquid film coalescence device 21 is positioned at the intersection of tower body 10 tower bodies 10 and gas buffer chamber 4, between liquid film coalescence device 21 or liquid film disperser 8 and tower body 10 inwalls, leave heavy phase channels, tower body 10 is separated into bubble dispersing chambers 20 at different levels by liquid film disperser 8; Liquid film distributor 11 is positioned at tower body 10 bottoms, and liquid film distributor 11 tops are connected and communicate with the liquid film disperser 8 of tower body 10 bottommosts, and liquid film distributor 11 belows are air-pressure chamber 17, and air-pressure chamber 17 is connected with air-blowing device; Light phase entrance 12 is positioned on liquid film distributor hollow cylinder 31 sidewalls, light phase entrance (12) communicates with interlayer space 29, light phase export 22 is positioned on 4 sidewalls of gas buffer chamber, and heavy liquid inlet 6 is positioned on tower body 10 top sidewalls, and heavy out 19 is positioned on tower body 10 bottom sidewalls.
Preferably, have heavy phase guiding gutter 7 in tower body 10, as water conservancy diversion heavy phase, heavy phase flows into next stage bubble dispersing chamber from upper level bubble dispersing chamber in heavy phase guiding gutter, forms countercurrent mass transfer with the organic light phase bubble rising; Heavy phase guiding gutter 7 is disk-like structure, center drilling, be provided with the vertical slot 7 of an open at both ends equating with ring width on one end ring limit, vertical slot 7 is close to tower body inwall cavity, heavy phase guiding gutter 7 is connected with liquid film coalescence device 21 or liquid film disperser 8 lower ends, its diameter equals liquid film coalescence device 21 or liquid film disperser 8, and external diameter equals tower body 10 inwall cavity internal diameters; Tower body 10 is separated into bubble dispersing chambers 20 at different levels by liquid film disperser 8 and heavy phase guiding gutter 7, further preferably, liquid film disperser 8 and heavy phase guiding gutter 7 are no less than 1 group in tower body, and for example 1 group, 2 groups, 3 groups, 5 groups, 10 groups etc., one of ordinary skill in the art can select as required; When tower body 10 is interior while there is heavy phase guiding gutter 7, between liquid film coalescence device 21 or liquid film disperser 8 and tower body 10 inwalls, no longer leave heavy phase channels, all heavy phase components flow into next stage bubble dispersing chamber by heavy phase guiding gutter 7 from upper level bubble dispersing chamber, form countercurrent mass transfer with the organic light phase bubble rising.
Preferably, described gas buffer chamber 4 can be that upper and lower footpath is consistent, also can be upper and lower footpath inconsistent, its typical but non-limiting example has: the large truncated cone-shaped structure in little inverted round stage structure, little Xia footpath, upper footpath, great Xia footpath, upper footpath, upper and lower footpath is consistent but drum organization that middle part diameter is larger etc., or other can play the arbitrary shape of the effect of collecting the light phase of overflowing from liquid film coalescence device 21.
Preferably, 4 lower ends, gas buffer chamber are provided with contraction section 5, and the end opening of contraction section 5 is connected and communicates with tower top liquid film coalescence device 21 upper ends; Described contraction section 5 is up big and down small structure, its typical but non-limiting example has: the up big and down small shape of falling truncated rectangular pyramids, up big and down small many terrace with edges shape, up big and down small reverse frustoconic etc., further preferably, light phase export 22 is positioned on contraction section 5 walls of lower end, gas buffer chamber.
Preferably, liquid film coalescence device 21 is or/and liquid film disperser 8 lower ends are connected with the collection bubble-cap 9 of open at both ends, the effect of collection bubble-cap 9 is to collect the bubble rising, collection bubble-cap 9 top diameters with liquid film coalescence device 21 or/and liquid film disperser 8 is identical, between below external diameter and tower body 10 cavity internal diameters, leave space, as heavy phase channels, further preferred, liquid film disperser 8 and collection bubble-cap 9 are no less than 1 group, for example 1 group, 2 groups, 3 groups, 5 groups, 10 groups etc. in tower body.
Do not connect collection bubble-cap 9 in liquid film disperser 8 lower ends of tower body bottommost.
The object that liquid film disperser and collection bubble-cap are set in tower body is, the bubble rising is collected through collection bubble-cap, assembles in liquid film disperser bottom, part bubble generation coalescence, breaks, the organic light phase liquid film coalescence of bubble surface, forms an organic light phase of thin layer again in liquid film disperser bottom.Now, a large amount of bubbles that rise, when through this layer of liquid film, are pressed into the micro channel of liquid film disperser again, bubble surface is carrying organic light phase, through these micro channels, from the ejection of liquid film disperser upper end jet, again form the air bubble liquid-membrane of organic light phase.So iterative cycles, under the effect of every grade of liquid film disperser and collection bubble-cap, is all concatenated to form the coalescence of bubble, the effect of then disperseing again.
Preferably, collection bubble-cap 9 upper ends are connected with liquid film coalescence device 21 or liquid film disperser 8, between below external diameter and tower body 10 cavity internal diameters, leave space, the width in space equals the width of heavy phase guiding gutter 7, be connected with heavy phase guiding gutter 7, heavy phase guiding gutter 7 center drillings, be provided with the vertical slot 7 of an open at both ends equating with ring width on one end ring limit, vertical slot 7 is close to tower body inwall cavity, its internal diameter equals to collect bubble-cap 9 maximum gauges, external diameter equals tower body 10 inwall cavity diameters, further preferred liquid film disperser 8, collection bubble-cap 9 and heavy phase guiding gutter 7 are no less than 1 group in tower body, for example 1 group, 2 groups, 3 groups, 5 groups, 10 groups etc., one of ordinary skill in the art can select as required.
Preferably, be provided with an exhaust outlet 2 on 4 sidewalls of gas buffer chamber, further preferably exhaust outlet 2 is connected with an air pressure valve, and particularly preferably described exhaust outlet 2 is connected with unidirectional air pressure valve 3 use pipelines, and described exhaust outlet 2 is positioned at closing cap 1 below.
Preferably, liquid film disperser 8 is disk-like structure, has the micropore 24 running through, and penetrates the micro channel 25 through the fixing open at both ends of through hole of liquid film disperser 8.
Preferably, liquid film disperser 8 vertical tube internal channel diameters are 0.1mm-6mm, and more preferably 0.3mm-3mm, is particularly preferably 0.5mm-2mm; Vertical tube length is preferably 1mm-30mm, and more preferably 3mm-25mm, is particularly preferably 5mm-20mm.
Preferably, liquid film distributor 11 lower ends connect seal closure 18, seal closure 18 effects are to separate air-pressure chamber and tower body cavity, prevent that the liquid in tower body cavity from flowing into air-pressure chamber, the osculum end of seal closure 18 is connected with liquid film distributor 11, its diameter equals liquid film distributor 11 diameters, and the big opening end of seal closure 18 is communicated with air-pressure chamber, and its diameter equals tower body 10 internal diameters.
Preferably, described air-blowing device is pulsed or lasting air supply system, further preferably formed by gas buffer tank (13) and feeder (14), described feeder can be air compressor machine or high-pressure cylinder or other air supply systems, and one of ordinary skill in the art can select according to the professional knowledge of its grasp.
Preferably, in liquid film distributor 11, establish the dish 28 of two formed objects, on two dishes, all have many through holes 26, through hole 26 structures of upper and lower two dishes 28 are identical, upper and lower hole site correspondence, between two dishes, leave certain interlayer space 29, interlayer space 29 Height Adjustable, between adjustment disk, interlayer space 29 height objects are, adjusting enters the amount of organic light phase in interlayer space 29 between dish, thereby it is organic light compared with the heavy phase aqueous solution that control enters in tower body, preferably the height in interlayer space 29 is regulated by one group of bolt 30.
Preferably, the material of two dishes 28 of composition sandwich-type liquid film distributor 11 is lipophile macromolecular material, it act as and enters the organic of interlayer space 29 and be on good terms rapidly at panel surface drawout, form organic liquid film at dish tapping, under air-blowing gas pressure, organic liquid film forms bubble through liquid film distributor, enters top and is attached thereto logical liquid film disperser 8.
Preferably, be connected with a mozzle 27 with light phase entrance 12, mozzle 27 is connected with outside through tower body 10 cavity inner wall perforates, organic light interlayer space 29 that is pressed into mozzle and pumps into liquid film distributor 11 through high pressure, described high pressure is greater than tower spirit pressure chamber 17 air pressure, and can be provided by pump, to prevent that organic phase from flowing backwards.
Preferably, air-pressure chamber 17 bottoms are provided with a collecting tank 15, it act as the liquid of collecting to be got off by top sandwich-type liquid film distributor diafiltration, further preferably, valve 16 is established in collecting tank 15 belows, for deriving the liquid of collection, the typical but non-limiting example of described valve 16 has: ball valve, needle valve, diaphragm valve, plug valve etc.
Tower body 10 be shaped as the arbitrary shape that is conducive to extraction process, can be designed as required by one of ordinary skill in the art, its typical but non-limiting example has: cylinder, cuboid, Elliptic Cylinder etc., for example gas buffer chamber 4 of other parts of extraction equipment, liquid film coalescence device 21, liquid film disperser 8, heavy phase guiding gutter 7, liquid film distributor 11, air-pressure chamber 17 grades are according to its shape adjustments, as long as can ensure interface size, shape can be combined closely mutually, for example, in the time that tower body 10 is elliptical cylinder-shape cavity structure, gas buffer chamber 4 can be elliptical cylinder-shape cavity structure, also can be up big and down small oval ladder cavity structure, liquid film coalescence device 21 is Elliptic Cylinder structure, liquid film disperser 8 is oval plate structure, heavy phase guiding gutter 7 can be elliptical ring dish, liquid film distributor 11 can be the structure of hollow ellipse cylinder open at both ends, inside establish the oval plate of two same diameter, air-pressure chamber can be half ellipsoidal structure, particularly preferably tower body 10 is cylinder barrel shaped cavity structure, gas buffer chamber 4 is cylinder barrel shaped cavity structure, contraction section 5 is reverse frustoconic, liquid film coalescence device 21 is cylindrical structure, liquid film disperser 8 is disc structure, and heavy phase guiding gutter 7 is circle ring disk, and liquid film distributor 11 is the circular hollow cylinder 31 of hollow cylinder open at both ends, inside establish the disk 28 of two same diameter, air-pressure chamber 17 is a hemispherical dome structure.
Preferably, in the time that tower body 10 is cylinder barrel shaped cavity structure, the diameter of tower body 10 is 1/60～1/15, more preferably 1/50～1/20 of its height, is particularly preferably 1/40～1/25.
Described heavy liquid inlet 6 and heavy out 19 can external pipes, and it act as and imports or derive the mobile heavy phase of tower body inner chamber.
The material of tower body can be affiliated field conventional material, one of ordinary skill in the art can select according to the professional knowledge of its grasp, be preferably metal or/and glass or/and Polymer Materials ' Structure material, particularly preferably inner surface do antiseptic metal or/and glass or/and Polymer Materials ' Structure material.
Preferably, tower body outer surface is provided with form, and further preferably the material of form is transparent material, as glass, in the time that tower body uses the structural material (as glass) of transparent material, without form.
Light phase export 22, can external pipe, and it act as overflow at contraction section 5 or/and the organic light phase that assemble gas buffer chamber 4.
Preferably, liquid film coalescence device 21 inner fillings have silk screen 32, further preferably silk screen is lipophile material, or the conducting metal material of external high-pressure electrostatic, particularly preferably silk screen is lipophile high molecular polymer material, or the conducting metal material of external high-pressure electrostatic, the bubble that is conducive to rise breaks in its surface cohesion, organic light phase liquid film coalescence in silk screen after breaking, organic gently mutually through liquid film coalescence device silk screen, from overhead gas surge chamber or/and contraction section overflow.
Described liquid film disperser, under air-blowing effect, bubble is carrying organic light phase, through these micro channels 25, sprays from liquid film disperser upper end micropore 24, forms the air bubble liquid-membrane of organic light phase.Owing to keeping certain distance between each micro channel, and micro channel 25 has certain length, and the bubble of ejection forms jet, is not easy coalescence.Therefore, can obtain homodisperse bubble.Air Bubble Size is by decisions such as the surperficial hydrophilic and hydrophobics of micro channel diameter, air-blowing air pressure, micro channel wall material.Bubble rising velocity is by decisions such as the micro channel wall material surface hydrophilic and hydrophobics of air-blowing air pressure, liquid film disperser.Liquid film disperser is located at tower body inside, at least 1 (comprising 1), for example 2,3,5 etc.
Preferably, liquid film disperser, micro channel Facing material, for having hydrophilic material, comprise stainless steel or high molecular polymer etc., and it act as the air bubble liquid-membrane that prevents organic light phase in its surface adhesion, under air-blowing effect, can pass rapidly microchannel.
One of object of the present invention is also to provide a kind of described using method of comparing greatly liquid-liquid diphase continuous extraction apparatus, and described device can carry out single-stage continuous extraction operation, also can carry out the operation of plural serial stage counter current continuous extraction.
It is 1:1500～1:30 that the applicable profit two phase countercurrent flow mass transfer of described device is compared scope, is particularly preferably 1:1000～1:50.
Concrete operation method is:
(1) while carrying out single-stage extraction operation, organicly gently carry light phase entrance 12 from being positioned at tower bottom to pump into the interlayer space 29 of liquid film distributor 11 through mozzle 27 by pump 23, organic phase is coiled 28 surface spreadings at liquid film distributor 11 and is opened, and forms organic liquid film at dish 28 tappings.Be attached thereto under logical air-pressure chamber 17 air-blowing gas pressures in lower end, organic liquid film forms bubble through liquid film distributor 11, enters top and is attached thereto logical liquid film disperser 8.Under air-blowing effect, bubble is carrying organic light phase, through the micro channel 25 of liquid film disperser 8 vertical tubes, spray from liquid film disperser 8 upper end micropores 24, form the air bubble liquid-membrane of organic light phase, be dispersed in the bubble dispersing chamber 20 in tower body 10, contact countercurrent mass transfer with heavy phase.The bubble rising is collected through upper level collection bubble-cap 9, assembles in upper level liquid film disperser 8 bottoms, part bubble generation coalescence, breaks, and the organic light phase liquid film coalescence of bubble surface, forms an organic light phase of thin layer again in liquid film disperser 8 bottoms.Now, a large amount of bubbles that rise are when through this layer of liquid film, be pressed into again the micro channel 25 of liquid film disperser 8, bubble surface has adsorbed organic light phase, through after these micro channels 25, be jet-like ejection from liquid film disperser 8 upper end micropores 24, again form the air bubble liquid-membrane of organic light phase.So iterative cycles, under the effect of every grade of liquid film disperser 8 and collection bubble-cap 9, is all concatenated to form the coalescence of bubble, then disperses again, enters the bubble dispersing chamber 20 in upper level tower body 10.The final liquid film coalescence device 21 that is positioned at tower top that arrives of bubble rising.Under inner lipophile silk screen 32 effects of liquid film coalescence device 21, bubble breaks in its surface cohesion.Organic light phase liquid film after breaking is in the interior coalescence of silk screen 32, organic gently mutually through liquid film coalescence device silk screen 32, overflows from overhead gas surge chamber 4 or contraction section 5.Organic light phase runs up to after certain volume therein, and tapping from its sidewall (light phase export 22) flows out.In the time that gas buffer chamber 4 internal gas pressures are greater than certain value, unidirectional air pressure valve 3 is opened exhaust.What form adverse current with organic light phase bubble is heavy phase liquid continuous phase, heavy phase enters tower body cavity from the perforate (heavy liquid inlet 6) that is positioned at tower body top, flow into bubble dispersing chamber 20 from heavy phase guiding gutter 7, form countercurrent mass transfer with the organic light phase bubble rising.Finally, heavy phase flows out from the perforate (heavy out 19) that is positioned at tower body bottom.
(2), while carrying out plural serial stage extracting operation, apparatus of the present invention are carried out plural serial stage.The organic light phase flowing out through upper level device tower body top light phase export 22, delivers into medial launder through pipeline, and then is pumped into the light phase entrance 12 of next stage device tower body bottom by pump, enters liquid film distributor 11 interlayer spaces 29.The heavy phase that upper level device tower body bottom heavy out 19 flows out, also delivers into another medial launder through pipeline, and then is pumped into the heavy liquid inlet 6 at next stage device tower body top by pump.So repeatedly, light, heavy two phase flow forms counter-current flow in the device of plural serial stage, thereby realizes the object of multiple stage continuous adverse current extraction.
The feature of apparatus of the present invention is:
(1) this device can be realized the organic light of small size disperseed by bubble.Organic light by being pumped into the liquid film distributor interlayer space that is positioned at device tower body bottom, organic phase, at liquid film distributor panel surface drawout, forms organic liquid film at dish tapping.Under air-pressure chamber air-blowing gas pressure, organic liquid film forms bubble through liquid film distributor, enters top and is attached thereto logical liquid film disperser.Bubble surface carries organic light phase, through the micro channel of liquid film disperser vertical tube, from the ejection of liquid film disperser riser upper end micro-hole jet, forms the air bubble liquid-membrane of organic light phase, is dispersed in the bubble dispersing chamber in tower body.The organic light phase air bubble liquid-membrane rising contacts in bubble dispersing chamber with the heavy phase flowing down from heavy phase guiding gutter, countercurrent mass transfer.Disperseed the thinking of small size organic phase by bubble, solved traditional agitating mode processing and treated a very hour difficult difficult problem of fully disperseing of dispersing liquid volume.In unit interval, the organic light phase phase volume of access to plant tower body can be controlled by liquid film distributor interlayer space.Like this, in device tower body the light phase of counter-current flow and heavy phase compare or flow-rate ratio can manual control, solved light phase and compared at super large with heavy phase a difficult problem for counter-current operation under condition.
(2) in this device tower body, every a segment distance, a liquid film disperser is set.The bubble rising, in the time flowing through every grade of liquid film disperser, is concatenated to form the coalescence of organic light phase air bubble liquid-membrane, the effect of then disperseing again.Can greatly improve like this stage efficiency of unit height of mass transfer in device tower body.Air Bubble Size and climbing speed can be by decisions such as the micro channel diameter of air-blowing air pressure, liquid film disperser, micro channel wall material surface hydrophilic and hydrophobics, effectively prevented the phenomenon of axial liquid stream back-mixing in tower body.
(3) this device tower body top arranges special liquid film coalescence device.Liquid film coalescence device inner filling has silk screen, and silk screen is lipophile high molecular polymer material, also can be conducting metal material, external high-pressure electrostatic, and the bubble that is conducive to rise breaks in its surface cohesion.In addition, even two phase countercurrent flow mass transfer generation emulsion, also breakdown of emulsion in liquid film coalescence device rapidly in tower body.Therefore, this device is also applicable to the extracting operation of easy emulsifying system.
Apparatus of the present invention are simple in structure, easily amplify, and are applicable to continuous operation, can plural serial stage, realize multistagely contact, the object of continuous countercurrent extraction.
Brief description of the drawings
Fig. 1 is a kind of structural representation of comparing greatly liquid-liquid diphase continuous extraction apparatus of the present invention.
Fig. 2 is the structural representation (wherein a is that top view, b are front view) of liquid film disperser 8 parts of apparatus of the present invention.
Fig. 3 is the structural representation (wherein a is that top view, b are front view) of sandwich-type liquid film distributor 11 parts at the bottom of the tower of apparatus of the present invention.
Fig. 4 is the structural representation (wherein a is that top view, b are front view) of tower top liquid film coalescence device 21 parts of apparatus of the present invention.
Fig. 5 is the truncated cone-shaped open at both ends of apparatus of the present invention structural representation that integrates bubble-cap 9 parts (wherein a as top view, b as front view).
Fig. 6 is the structural representation (wherein a is that top view, b are front view) of the hollow inside and outside circle barrel structure of the open at both ends of apparatus of the present invention formula heavy phase guiding gutter parts 7.
Reference numeral is expressed as follows:
1-closing cap; 2-gas buffer chamber exhaust outlet; 3-unidirectional air pressure valve;
4-gas buffer chamber; 5-contraction section; 6-heavy liquid inlet;
7-heavy phase guiding gutter; 8-liquid film disperser; 9-collection bubble-cap;
10-tower body; 11-liquid film distributor; 12-light phase entrance;
13-gas buffer tank; 14-feeder; 15-collecting tank;
16-valve; 17-air-pressure chamber; 18-seal closure;
19-heavy out; 20-bubble dispersing chamber; 21-liquid film coalescence device;
22-light phase export; 23-pump; 24-micropore;
25-micro channel; 26-through hole; 27-mozzle;
28-dish; 29-interlayer space; 30-bolt;
31-hollow cylinder; 32-silk screen.
Detailed description of the invention
Below in conjunction with accompanying drawing, the liquid-liquid diphase continuous extraction apparatus of comparing greatly of the present invention is described.Those skilled in the art should understand, described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
One of the present invention is compared greatly liquid-liquid diphase continuous extraction apparatus, is mainly made up of tower body 10, gas buffer chamber 4, liquid film coalescence device 21, liquid film disperser 8, liquid film distributor 11, air-pressure chamber 17 etc.
While carrying out single-stage continuous extraction operation, organicly gently carry light phase entrance 12 from being positioned at tower bottom to be pumped into the interlayer space 29 of sandwich-type liquid film distributor 11 through mozzle 27 by pump 23, organic phase is launched in the 28 inner surface tilings of liquid film distributor dish, and at dish, perforate 26 places form organic liquid film.Be attached thereto under logical air-pressure chamber 17 air-blowing gas pressures in lower end, organic liquid film forms bubble through liquid film distributor 11, enters top and is attached thereto logical liquid film disperser 8.Under air-blowing effect, bubble is carrying organic light phase, through the micro channel 25 of liquid film disperser 8, spray from liquid film disperser riser upper end micropore 24, form the air bubble liquid-membrane of organic light phase, be dispersed in the bubble dispersing chamber 20 in tower body, contact countercurrent mass transfer with heavy phase.The bubble rising is collected through upper level collection bubble-cap 9, assembles in upper level liquid film disperser 8 bottoms, part bubble generation coalescence, breaks, and the organic light phase liquid film coalescence of bubble surface, forms an organic light phase of thin layer again in liquid film disperser 8 bottoms.Now, a large amount of bubbles that rise are when through this layer of liquid film, be pressed into again the micro channel 25 of liquid film disperser 8, bubble surface has adsorbed organic light phase, through behind these microchannels, be jet-like ejection from liquid film disperser riser upper end micropore 24, again form the air bubble liquid-membrane of organic light phase.So iterative cycles, under the effect of every grade of liquid film disperser and collection bubble-cap, is all concatenated to form the coalescence of bubble, then disperses again, enters the bubble dispersing chamber 20 in upper level tower body.The final liquid film coalescence device 21 that is positioned at tower top that arrives of bubble rising.Under inner lipophile silk screen 32 effects of liquid film coalescence device, bubble breaks in its surface cohesion.Organic light phase liquid film coalescence in silk screen after breaking, organic gently mutually through liquid film coalescence device silk screen, overflow from overhead gas surge chamber 4 or contraction section 5.Organic light phase runs up to after certain volume therein, and tapping from its sidewall (light phase export 22) flows out.In the time that gas buffer chamber 4 internal gas pressures are greater than certain value, unidirectional air pressure valve 3 is opened exhaust.What form adverse current with organic light phase bubble is heavy phase liquid continuous phase, heavy phase enters tower body 10 from the perforate (heavy liquid inlet 6) that is positioned at tower body top, flow into bubble dispersing chamber 20 from heavy phase guiding gutter 7, form countercurrent mass transfer with the organic light phase bubble rising.Finally, heavy phase flows out from the perforate (heavy out 19) that is positioned at tower body bottom.
While carrying out plural serial stage extracting operation, the organic light phase flowing out through upper level device tower body top light phase export 22, delivers into a medial launder through pipeline, and then is pumped into the light phase entrance 12 of next stage device tower body bottom by pump, enters liquid film distributor 11 interlayers.The heavy phase that upper level device tower body bottom heavy out 19 flows out, also delivers into another medial launder through pipeline, and then is pumped into the heavy liquid inlet 6 at next stage device tower body top by pump.So repeatedly, light, heavy two phase flow forms counter-current flow in the device of plural serial stage, thereby realizes the object of multiple stage continuous adverse current extraction.
Embodiment 1
Organic phase is two-(2-ethylhexyl) phosphoric acid (P204), is dissolved in sulfonated kerosene, and the concentration of P204 in kerosene is 1mol/L.The attach most importance to aqueous solution of rare earth ion erbium, ytterbium, lutetium of water, pH4-4.5, rare earth ion total concentration 10mg/L.Organic phase volume is 10mL, and water volume to be extracted is 5L, water: oil is in a ratio of 500:1.Tower body cavity internal diameter 50mm, high 2000mm, arranges three groups of liquid film dispersers and collection bubble-cap, every group of spacing 500mm in tower body.Liquid film disperser vertical tube channel diameter is 1mm, and vertical tube length is 5mm.Organic phase is pumped into the interlayer space of sandwich-type liquid film distributor 11 at the bottom of tower by diaphragm metering pump.The air steel cylinder air pressure 1.0MPa communicating with tower spirit pressure chamber.Carry out single-stage continuous extraction operation, detect the water Rare Earth Metal Ions concentration that flow out at heavy out 19 places in tower body bottom, the extraction yield of three kinds of rare earth ions is respectively 90.8%, 82.5%, and 80.0%.
Embodiment 2
Organic phase is 15wt% aphthenic acids+10wt% mixed alcohol+75wt% sulfonated kerosene.Water is the mixed aqueous solution of yttrium, lanthanum, europium, gadolinium ion, pH4-4.5, rare earth ion total concentration 100mg/L.Organic phase volume is 100mL, and water volume to be extracted is 100L, water: oil is in a ratio of 1000:1.Tower body cavity internal diameter 50mm, high 2000mm, arranges three groups of liquid film dispersers and collection bubble-cap, every group of spacing 500mm in tower body.Liquid film disperser vertical tube channel diameter is 1.5mm, and vertical tube length is 10mm.Organic phase is pumped into the interlayer space of sandwich-type liquid film distributor 11 at the bottom of tower by diaphragm metering pump.The air steel cylinder air pressure 1.5MPa communicating with tower spirit pressure chamber.Carry out three grades of series connection continuous extraction operations, detect afterbody tower body bottom heavy out 19 places and flow out water Rare Earth Metal Ions concentration, extraction yield is respectively lanthanum 98.0%, yttrium 92.0%, europium 95.0%, gadolinium 93.5%.
Embodiment 3
Organic phase is the iso-octyl phosphine monooctyl acid monooctyl ester (P507) of part ammonification, is dissolved in sulfonated kerosene, and the concentration of P507 in kerosene is 1.5mol/L.Water is the mixed aqueous solution of lanthanum, europium, ytterbium ion, pH4-4.5, rare earth ion total concentration 100mg/L.Organic phase volume is 100mL, and water volume to be extracted is 10L, water: oil is in a ratio of 100:1.Tower body cavity internal diameter 50mm, high 2000mm, arranges three groups of liquid film dispersers and collection bubble-cap, every group of spacing 500mm in tower body.Liquid film disperser vertical tube channel diameter is 1mm, and vertical tube length is 10mm.Organic phase is pumped into the interlayer space of sandwich-type liquid film distributor 11 at the bottom of tower by diaphragm metering pump.The air steel cylinder air pressure 1.5MPa communicating with tower spirit pressure chamber.Carry out three grades of series connection continuous extraction operations, detect afterbody tower body bottom heavy out 19 places and flow out water Rare Earth Metal Ions concentration, extraction yield is respectively lanthanum 95.5%, europium 92.0%, ytterbium 83.0%.
Embodiment 4
Organic phase is the butyl acetate solution of 5.7wt% tributylphosphine oxide (TBPO), and water is the lactalbumin containing 1mg/mL, the benzylpenicillin potassium saline solution of 0.05M, pH=4.0.Organic phase volume is 50mL, and water volume to be extracted is 10L, water: oil is in a ratio of 200:1.Tower body cavity internal diameter 50mm, high 2000mm, arranges three groups of liquid film dispersers and collection bubble-cap, every group of spacing 500mm in tower body.Liquid film disperser vertical tube channel diameter is 1mm, and vertical tube length is 5mm.Organic phase is pumped into the interlayer space of sandwich-type liquid film distributor 11 at the bottom of tower by diaphragm metering pump.The air steel cylinder air pressure 1.5MPa communicating with tower spirit pressure chamber.Carry out three grades of series connection continuous extraction operations, detect the content of penicillin in afterbody tower body bottom heavy out 19 places' outflow waters, extraction yield 90.5%.
Embodiment 5
Organic phase is the butyl acetate solution of 5.7wt% tributylphosphine oxide (TBPO), and water is the lactalbumin containing 1mg/mL, the benzylpenicillin potassium saline solution of 0.05M, pH=4.0.Organic phase volume is 50mL, and water volume to be extracted is 10L, water: oil is in a ratio of 200:1.Tower body cavity internal diameter 50mm, high 2000mm, tower body is cylinder, and tower body top is directly connected with cylindrical gas surge chamber, and tower body inside arranges three liquid film dispersers, and liquid film disperser below does not connect collection bubble-cap, every two liquid film disperser spacing 500mm.Liquid film disperser vertical tube channel diameter is 1mm, and vertical tube length is 5mm.Organic phase is pumped into the interlayer space of sandwich-type liquid film distributor 11 at the bottom of tower by diaphragm metering pump.The air steel cylinder air pressure 1.5MPa communicating with tower spirit pressure chamber.Carry out three grades of series connection continuous extraction operations, detect the content of penicillin in afterbody tower body bottom heavy out 19 places' outflow waters, extraction yield 88.4%.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the each raw material of product of the present invention and the interpolation of auxiliary element, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (39)
1. compare greatly a liquid-liquid diphase continuous extraction apparatus, described device comprises tower body, gas buffer chamber, liquid film coalescence device, liquid film disperser, liquid film distributor, air-pressure chamber, and its concrete structure is:
Tower body (10) is cavity structure, gas buffer chamber (4) is positioned at tower body (10) top, gas buffer chamber (4) closing cap for upper end (1) sealing, liquid film coalescence device (21) is positioned at the intersection of tower body (10) tower body and gas buffer chamber, between liquid film coalescence device (21) or liquid film disperser (8) and tower body (10) inwall, leave heavy phase channels, tower body (10) is separated into bubble dispersing chambers at different levels (20) by liquid film disperser (8); Liquid film distributor (11) is positioned at tower body (10) bottom, liquid film distributor (11) top is connected and communicates with the liquid film disperser (8) of tower body (10) bottommost, liquid film distributor (11) below is air-pressure chamber (17), and air-pressure chamber (17) is connected with air-blowing device; In liquid film distributor (11), establish the dish (28) of two formed objects, on two dishes, all have many through holes (26), through hole (26) structure of upper and lower two dishes (28) is identical, upper and lower hole site correspondence, between two dishes, leave certain interlayer space (29), interlayer space (29) Height Adjustable; Light phase entrance (12) is positioned on liquid film distributor hollow cylinder (31) sidewall, light phase entrance (12) communicates with interlayer space (29), light phase export (22) is positioned on the sidewall of gas buffer chamber (4), heavy liquid inlet (6) is positioned on the sidewall of tower body (10) top, and heavy out (19) is positioned on the sidewall of tower body (10) bottom;
Lower end, gas buffer chamber (4) is provided with contraction section (5), and the end opening of contraction section (5) is connected and communicates with tower top liquid film coalescence device (21) upper end; Described contraction section (5) is up big and down small structure.
2. device as claimed in claim 1, it is characterized in that, in tower body (10), there is heavy phase guiding gutter (7), described heavy phase guiding gutter (7) is disk-like structure, center drilling, be provided with the vertical slot of an open at both ends equating with ring width on one end ring limit, vertical slot is close to tower body inwall cavity, heavy phase guiding gutter (7) is connected with liquid film coalescence device (21) or liquid film disperser (8) lower end, its diameter equals liquid film coalescence device (21) or liquid film disperser (8), and external diameter equals tower body (10) inwall cavity internal diameter; Tower body (10) is separated into bubble dispersing chambers at different levels (20) by liquid film disperser (8) and heavy phase guiding gutter (7);
Described gas buffer chamber (4) is that upper and lower footpath is consistent or upper and lower footpath is inconsistent.
3. device as claimed in claim 2, is characterized in that, liquid film disperser (8) and heavy phase guiding gutter (7) are no less than 1 group in tower body.
4. device as claimed in claim 1 or 2, is characterized in that, light phase export (22) is positioned on lower end, gas buffer chamber contraction section (5) wall.
5. device as claimed in claim 1 or 2, it is characterized in that, liquid film coalescence device (21) is or/and liquid film disperser (8) lower end is connected with the collection bubble-cap (9) of open at both ends, collection bubble-cap (9) top diameter with liquid film coalescence device (21) or/and liquid film disperser (8) is identical, between below external diameter and tower body (10) cavity internal diameter, leave heavy phase channels, liquid film disperser (8) and collection bubble-cap (9) are no less than 1 group in tower body;
Do not connect collection bubble-cap (9) in liquid film disperser (8) lower end of tower body bottommost.
6. the device as described in claim 1-3 any one, it is characterized in that, collection bubble-cap (9) upper end is connected with liquid film coalescence device (21) or liquid film disperser (8), between below external diameter and tower body (10) cavity internal diameter, leave space, the width in space equals the width of heavy phase guiding gutter (7), be connected with heavy phase guiding gutter (7), heavy phase guiding gutter (7) center drilling, be provided with the vertical slot of an open at both ends equating with ring width on one end ring limit, vertical slot is close to tower body inwall cavity, its internal diameter equals to collect bubble-cap (9) maximum gauge, external diameter equals tower body (10) inwall cavity diameter.
7. device as claimed in claim 6, is characterized in that, on the sidewall of gas buffer chamber (4), is provided with an exhaust outlet (2).
8. device as claimed in claim 7, is characterized in that, exhaust outlet (2) is connected with an air pressure valve.
9. device as claimed in claim 8, is characterized in that, described exhaust outlet (2) is connected with pipeline with a unidirectional air pressure valve (3), and described exhaust outlet (2) is positioned at closing cap (1) below.
10. the device as described in claim 1-3 any one, it is characterized in that, liquid film disperser (8) is disk-like structure, there is the micropore (24) running through, penetrate the micro channel (25) through the fixing open at both ends of through hole of liquid film disperser (8).
11. devices as claimed in claim 10, is characterized in that, liquid film disperser (8) vertical tube internal channel diameter is 0.1mm-6mm; Vertical tube length is 1mm-30mm.
12. devices as claimed in claim 11, is characterized in that, liquid film disperser (8) vertical tube internal channel diameter is 0.3mm-3mm.
13. devices as claimed in claim 12, is characterized in that, liquid film disperser (8) vertical tube internal channel diameter is 0.5mm-2mm.
14. devices as claimed in claim 11, is characterized in that, vertical tube length is 3mm-25mm.
15. devices as claimed in claim 14, is characterized in that, vertical tube length is 5mm-20mm.
16. devices as claimed in claim 1, it is characterized in that, liquid film distributor (11) lower end connects seal closure (18), the osculum end of seal closure (18) is connected with liquid film distributor (11), its diameter equals liquid film distributor (11) diameter, the big opening end of seal closure (18) is communicated with air-pressure chamber, and its diameter equals tower body (10) internal diameter.
17. devices as claimed in claim 1, is characterized in that, described air-blowing device is pulsed or lasting air supply system.
18. devices as claimed in claim 17, is characterized in that, described air-blowing device is made up of gas buffer tank (13) and feeder (14), and described feeder is air compressor machine or high-pressure cylinder or other air supply systems.
19. devices as claimed in claim 1, is characterized in that, the height of interlayer space (29) is regulated by one group of bolt (30).
20. devices as claimed in claim 1, is characterized in that, the material of two dishes (28) of composition sandwich-type liquid film distributor (11) is lipophile macromolecular material.
21. devices as described in claim 1-3 any one, it is characterized in that, be connected with a mozzle (27) with light phase entrance (12), mozzle (27) is connected with outside through tower body (10) cavity inner wall perforate, organic light interlayer space (29) that is pressed into mozzle and pumps into liquid film distributor (11) through high pressure, described high pressure is greater than tower spirit pressure chamber (17) air pressure, and is provided by pump.
22. devices as claimed in claim 21, is characterized in that, air-pressure chamber (17) bottom is provided with a collecting tank (15).
23. devices as claimed in claim 22, is characterized in that, valve (16) is established in collecting tank (15) below.
24. devices as described in claim 1-3 any one, it is characterized in that, tower body (10) be shaped as cylinder, cuboid, Elliptic Cylinder, the gas buffer chamber (4) of extraction equipment, liquid film coalescence device (21), liquid film disperser (8), heavy phase guiding gutter (7), liquid film distributor (11), air-pressure chamber (17) be according to tower body shape adjustments, as long as can ensure that interface size, shape can combine closely mutually.
25. devices as claimed in claim 24, it is characterized in that, tower body (10) is cylinder barrel shaped cavity structure, gas buffer chamber (4) is cylinder barrel shaped cavity structure, contraction section (5) is reverse frustoconic, liquid film coalescence device (21) is cylindrical structure, liquid film disperser (8) is disc structure, heavy phase guiding gutter (7) is circle ring disk, liquid film distributor (11) is the circular hollow cylinder (31) of hollow cylinder open at both ends, the disk (28) of inside establishing two same diameter, air-pressure chamber (17) is a hemispherical dome structure.
26. devices as claimed in claim 24, is characterized in that, in the time that tower body (10) is cylinder barrel shaped cavity structure, the diameter of tower body (10) is 1/60～1/15 of its height.
27. devices as claimed in claim 26, is characterized in that, the diameter of tower body (10) is 1/50～1/20 of its height.
28. devices as claimed in claim 27, is characterized in that, the diameter of tower body (10) is 1/40～1/25 of its height.
29. devices as described in claim 1-3 any one, is characterized in that, the material of tower body be metal or/and glass or/and Polymer Materials ' Structure material.
30. devices as claimed in claim 29, is characterized in that, the material of tower body be inner surface do antiseptic metal or/and glass or/and Polymer Materials ' Structure material.
31. devices as described in claim 1-3 any one, is characterized in that, tower body outer surface is provided with form, and the material of form is transparent material.
32. devices as claimed in claim 31, is characterized in that, the material of form is glass.
33. devices as described in claim 1-3 any one, is characterized in that, liquid film coalescence device (21) inner filling has silk screen (32).
34. devices as claimed in claim 33, is characterized in that, silk screen is lipophile material, or the conducting metal material of external high-pressure electrostatic.
35. devices as claimed in claim 34, is characterized in that, silk screen is lipophile high molecular polymer material, or the conducting metal material of external high-pressure electrostatic.
36. devices as described in claim 1-3 any one, is characterized in that, liquid film disperser is located at tower body inside, at least 1.
37. devices as described in claim 1-3 any one, is characterized in that, liquid film disperser, micro channel Facing material are for having hydrophilic material.
38. devices as claimed in claim 37, is characterized in that, liquid film disperser, micro channel Facing material are stainless steel or high molecular polymer.
39. compare greatly the using method of liquid-liquid diphase continuous extraction apparatus as described in claim 1-38 any one, it is characterized in that, described device carries out single-stage continuous extraction operation, or carries out the operation of plural serial stage counter current continuous extraction.
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| CN112604320B (en) * | 2020-11-30 | 2022-03-01 | 青岛理工大学 | Pre-dispersion micro-nano bubble supported liquid film generator |
| CN112604321B (en) * | 2020-11-30 | 2022-06-17 | 青岛理工大学 | Large-phase-ratio pre-dispersion micro-nano bubble supported liquid film extraction device |
| CN112704910B (en) * | 2021-01-14 | 2021-10-22 | 青岛理工大学 | Organic liquid membrane interface shearing updating extraction device and use method |
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