CN107803050B - A kind of dynamic magnetic particle combined films extraction equipment and extracting process - Google Patents

A kind of dynamic magnetic particle combined films extraction equipment and extracting process Download PDF

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Publication number
CN107803050B
CN107803050B CN201711295003.2A CN201711295003A CN107803050B CN 107803050 B CN107803050 B CN 107803050B CN 201711295003 A CN201711295003 A CN 201711295003A CN 107803050 B CN107803050 B CN 107803050B
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magnetic particle
extraction
magnet
combined films
phase
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CN107803050A (en
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杨良嵘
冯冬
惠俊峰
安震涛
刘会洲
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Institute of Process Engineering of CAS
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Institute of Process Engineering of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0419Solvent extraction of solutions which are liquid in combination with an electric or magnetic field or with vibrations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0426Counter-current multistage extraction towers in a vertical or sloping position
    • B01D11/043Counter-current multistage extraction towers in a vertical or sloping position with stationary contacting elements, sieve plates or loose contacting elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0484Controlling means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The present invention provides a kind of dynamic magnetic particle combined films extraction equipment and extracting process.The extraction equipment, including tower body, extraction phase storage room, porous sieve plate, dynamic magnetic particle combined films, magnet and magnet actuator;Extraction phase storage room is located at below tower body, is disposed with porous sieve plate and dynamic magnetic particle combined films between extraction phase storage room and tower body from the bottom to top, is placed with magnet and magnet actuator below extraction phase storage room.Dynamic magnetic particle combined films extraction equipment of the invention, magnet actuator band moving magnet moves up and down, the magnetic thin layer of particulate in combination dynamic magnetic particle combined films is constantly rearranged, extraction phase constantly forms fine drop and is scattered in feed liquid phase, will not block or fluid distrbution is uneven;Magnetic particle, which draws close movement to magnetic field again, has fragmentation to dispersed phase drop, conducive to the formation of fine drop, while the phenomenon that can effectively prevent channel, improves extraction efficiency.

Description

A kind of dynamic magnetic particle combined films extraction equipment and extracting process
Technical field
The invention belongs to magnetic particle combined films extraction and separation technology fields, are related to a kind of dynamic magnetic particle combination membrane extraction dress It sets and extracting process.
Background technique
In recent years, with the development of industry, abstraction technique is in chemical engineering industry, and pharmaceuticals industry, the fields such as petroleum industry obtain It is widely applied, but simultaneously traditional extraction technology is also increasingly difficult to meet the needs of development of modern industry.Traditional extraction Equipment is taken to be generally divided into mixer-settler extractor, extraction tower and centrifugal extractor, there is mass-transfer efficiencies for mixer-settler extraction process Height, but the problems such as occupation area of equipment is big;Traditional extraction tower type is more, wherein widely used is filler extraction Tower, oscillating screen plate tower, mechanical stirring extraction tower and pulsed extraction tower, it is a series of that extraction tower is usually present that the device is complicated etc. Problem, such as turntable extracting tower are the widely used one kind of mechanical stirring extraction tower, but have more serious amplification Effect especially becomes apparent when being applied to the fields such as system more complicated pharmacy and petrochemical industry, mass transfer is caused to be imitated Rate is low.
Membrane extraction technology is a kind of new separation technology for combining membrane process and liquid-liquid extraction, has been received since proposition Greatly concern and attention.Compared with traditional abstraction technique, since membrane extraction technology without two alternate dispersions and coalesced Journey, so greatly reducing the entrainment loss of extractant;And relax physical property to extractant density, viscosity, interfacial tension etc. It is required that expanding the application range of extractant.
For this purpose, film dispersion extraction becomes a kind of completely new research hotspot.Membrane extraction equipment is using microporous barrier as phase point One phase is distributed in another phase under conditions of film pressure at both sides difference is greater than and penetrates pressure, realizes mass transfer point by scattered medium From.
Ma Wei, Shen Dianbang (physics, magnetic field is applied in metallurgy and Exploration of Mechanism, 430-432,1969) have studied magnetic field and exist When effect in the Waste acid recovery technology containing arsenic, discovery magnetic field improves the extraction yield of TBP (tributyl phosphate) extraction arsenic 3%-5%, made further research with infrared spectroscopy and nuclear magnetic resonance the result shows that, magnetic field is in the feelings not changed to extraction mechanism Under condition, but change extraction efficiency, while finding solution concentration difference, the extraction yield variation degree of physical parameter is not yet It is identical.
Currently, the extraction efficiency of extraction separation device existing in the prior art needs to be further increased.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of dynamic magnetic particle combined films extraction equipment, Avoid fixed magnetic particle combined films be used for a long time it is possible that fluid distrbution it is uneven, and fixed magnetic particle combined films The problem of blocking inside magnetic thin layer of particulate because of organic phase accumulation, improves extraction efficiency.
To achieve this purpose, the present invention adopts the following technical scheme:
A kind of dynamic magnetic particle combined films extraction equipment, described device include tower body, extraction phase storage room, porous sieve plate, Dynamic magnetic particle combined films, magnet and magnet actuator;Wherein, the extraction phase storage room is located at below tower body, the extraction It takes and is disposed with porous sieve plate and dynamic magnetic particle combined films between phase storage room and tower body from the bottom to top, the extraction phase storage It deposits and is placed with the magnet and magnet actuator below room, the magnet is connected with the magnet actuator.
In the present invention, the magnet actuator includes the first crank connecting link, fixed hub, the second crank connecting link and direct current Motor, one end of first crank connecting link pass through the fixed hub and connect with the magnet, first crank connecting link The other end is flexibly connected with one end of second crank connecting link, the other end and the direct current generator of second crank connecting link It connects and is rotated under the drive of the direct current generator.
In the present invention, the amplitude of the magnet actuator is 8~12cm, for example, magnet actuator amplitude be 8cm, 9cm、10cm、11cm、12cm。
Preferably, the rotational frequency of the magnet actuator is 20~50 revs/min, such as the rotation of magnet actuator Frequency is 20 revs/min, 25 revs/min, 30 revs/min, 35 revs/min, 40 revs/min, 45 revs/min, 50 revs/min.
In the present invention, the dynamic magnetic particle combined films include magnetic particle and film, and the magnetic particle is in the magnet In the top dynamic arrangement of the film under magnetic fields, the magnetic particle is containing Fe3O4Magnetic particle.
Preferably, the magnetic particle dynamic arrangement with a thickness of 3~5mm.
Preferably, the partial size of the magnetic particle is 300~600 μm.
Preferably, the aperture of the film is 1~80 μm.
Preferably, dynamic magnetic particle combined films extraction equipment of the invention further includes being located at the extraction phase to store Base support below room, the magnet are set to the inside of the base support, and the volume of the base support is greater than described The volume of magnet.
Extraction phase material mouth is arranged in the extraction phase storage room, and the material mouth is connected with extraction phase slot.
Preferably, pressure gauge and electromagnetic dosing pump are successively connected between the extraction phase storage room and extraction phase slot.
Wherein, the bottom of the tower body is connect by pipeline with raffinate phase collector.
In the present invention, the top of the tower body is connect by pipeline with material liquid phase groove.
Preferably, the top of the tower body is connect by pipeline with extraction phase collector.
In the present invention, sequentially connected feed liquid phase peristaltic pump and pressure are additionally provided between the material liquid phase groove and the tower body Power meter, so that the feed liquid in the material liquid phase groove mutually enters the tower body.
The height of the extraction phase storage room is 10~15mm.
Preferably, the porous sieve plate is the porous sieve plate of organic glass material, the aperture of the porous sieve plate is 2~ 6mm。
Preferably, the porosity of the porous sieve plate is 20~30%.
Preferably, the magnet is cylinder-shaped magnet, and the S grade of the cylinder-shaped magnet or N grades are upward.
The second object of the present invention is to provide a kind of dynamic magnetic particle combined films extracting process, the extracting process are as follows: To contain the aqueous solution of object ion as feed liquid phase, to contain the mixed solution of extractant and diluent as extraction phase, institute It states extraction phase and forms uniformly tiny droplet distribution in the feed liquid phase across the dynamic magnetic particle combined films, the feed liquid It is mutually adverse current with the type of flow of the extraction phase;Object ion mass transfer in the feed liquid phase is into the drop of the extraction phase It is extracted.
The extraction phase is squeezed into the feed liquid phase by extrapolability, and the extrapolability is not more than the lower section of feed liquid phase storage room Magnet to the magnetic force of the magnetic particles of magnetic particle combined films;Such as extraction phase is squeezed into the outer of feed liquid phase by electromagnetic dosing pump Thrust is not greater than the cylinder-shaped magnet below feed liquid phase storage room to the magnetic force of magnetic particle, and otherwise magnetic particle can be divided Dephasing is related to be dispersed among continuous phase, and feed liquid is caused mutually to pollute and the loss of magnetic particle.Just because of magnetic particle in magnetic field There is following characteristics under effect, i.e., existing for the magnetic field under the conditions of, when magnetic field, the attraction to magnetic particle is greater than fluid to magnetic When the impact force of particle, even if the extraction phase to be dispersed is under flow regime, magnetic particle can still draw close movement to magnetic field, then Generate coalescence.
In the present invention, the magnetic particle is under the magnetic fields of the magnet in the top dynamic arrangement of the film, institute Stating magnetic particle is containing Fe3O4Magnetic particle;
In the present invention, the magnetic particle dynamic arrangement with a thickness of 3~5mm, such as magnetic particle dynamic arrangement with a thickness of 3mm、3.5mm、4mm、4.5mm、5mm。
In the present invention, such as the partial size of magnetic particle is 300 μm, 350 μm, 400 μm, 450 μm, 500 μm, 550 μm, 600 μm.
It is further preferred that the aperture of the film is 1~80 μm, such as the aperture of film is 1 μm, 5 μm, 10 μm, 20 μ m、30μm、40μm、50μm、60μm、70μm、80μm。
In the present invention, the film is thin layer place mat, plays the purpose of support magnetic particle and dispersion extraction phase.The film Aperture be 1~80 μm, such as film aperture be 1 μm, 5 μm, 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm;Thin layer place mat membrane pore size is several microns to tens microns, and thin layer place mat aperture should not be too large, also unsuitable too small, aperture mistake It is easy to cause the omission of magnetic-particle, the too small easy thin layer place mat blocking in aperture greatly.
Preferably, the thin layer place mat is silk, common cloth or steel wire, plays support magnetic thin layer of particulate and prevents magnetic The effect that grain is omitted.
The extraction phase is used as dispersed phase, the volume of the extractant and the diluent in magnetic particle combination membrane extraction Than for (1~5): (5~10), such as the volume ratio of extractant and diluent is 1:1,1:2,1:3,1:4,1:5,1:6,1:7,1: 8、1:9、1:10、2:3、2:5、2:7、2:9、3:5、3:7、3:8、3:10、4:5、4:7、4:9、5:6、5:7、5:8、5:9。
Preferably, the extractant is tributyl phosphate (TBP);It is further preferred that the diluent is sulfonated kerosene (No. 260 solvent naphthas).
The feed liquid is mutually used as continuous phase in magnetic particle combination membrane extraction, and the object ion is propionic acid, 3- hydroxyl third Acid and one of 2 hydroxy propanoic acid or at least two mixture.Compared with prior art, the invention has the benefit that
(1) dynamic magnetic particle combined films extraction equipment of the invention, magnet actuator band moving magnet move up and down, constantly Rearrange combination dynamic magnetic particle combined films in magnetic thin layer of particulate so that the gap between magnetic particle constantly replace it is loose with Fine and close state, can be effectively prevented tiny dispersed phase drop and deposits blocking between magnetic thin layer of particulate gap, it is ensured that point Dephasing drop constantly passes through magnetic thin layer of particulate, will not there is a situation where blocking or fluid distrbution are uneven;Magnetic particle exists simultaneously Under magnetic force again to magnetic field draw close movement can play the role of to dispersed phase drop it is broken, conducive to the formation of fine drop, The phenomenon that channel can be effectively prevent simultaneously.
(2) dynamic magnetic particle combined films extracting process of the invention can by constantly moving up and down cylinder-shaped magnet rapidly To achieve the purpose that constantly to rearrange combination magnetic thin layer of particulate, dispersed phase can constantly form uniform particle sizes under flow regime Fine drop, and even fluid distribution.Size droplet diameter is tens microns between millimeter, since size droplet diameter is small, so phase There is very big mass transfer area compared with traditional extraction, is conducive to mass transfer.
(3) dynamic magnetic particle combined films extraction equipment of the invention passes through design dynamic magnetic thin layer of particulate and thin layer place mat Film combines, and under magnetic force and fluid impingement force effect, constantly springs up out the tiny dispersed phase drop point of uniform particle sizes It dissipates among continuous phase, by magnetic fields, under conditions of not changing extraction mechanism, improves extraction efficiency, film is extracted It takes and possesses good application prospect in the industry.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of dynamic magnetic particle combined films extraction equipment of the invention;
Fig. 2 is the structural schematic diagram of the magnet actuator in dynamic magnetic particle combined films extraction equipment of the invention;
Fig. 3 is dynamic magnetic particle combined films extraction equipment operation principle schematic diagram of the invention;
One when Fig. 4 (a) is the magnet actuator work in dynamic magnetic particle combined films extraction equipment of the invention Working state structure schematic diagram;
It is another when Fig. 4 (b) is the magnet actuator work in dynamic magnetic particle combined films extraction equipment of the invention A working state structure schematic diagram.
Appended drawing reference is as follows:
1- extraction phase slot;2- electromagnetic dosing pump;3- pressure gauge;4- base support;5- magnet;6- extraction phase storage room;7- Porous sieve plate;8- film;9- magnetic particle;10- raffinate phase collector;11- tower body;12- expects liquid phase groove;13- feed liquid phase peristaltic pump; 14- extraction phase collector;15- magnet actuator;The first crank connecting link of 15a-;15b- fixed hub;The second crank of 15c- connects Bar;15d- direct current generator.
Specific embodiment
1-4 with reference to the accompanying drawing, and pass through specific embodiment to further illustrate the technical scheme of the present invention.
Such as attached drawing 1, dynamic magnetic particle combined films extraction equipment of the invention, device includes tower body 11, extraction phase storage room 6, porous sieve plate 7, dynamic magnetic particle combined films, magnet 5 and magnet actuator 15;Wherein, extraction phase storage room 6 is located at tower body 11 lower sections, are disposed with porous sieve plate 7 from the bottom to top and dynamic magnetic particle combine between extraction phase storage room 6 and tower body 11 Film, the lower section of extraction phase storage room 6 are placed with magnet 5 and magnet actuator 15, and magnet 5 is connected with magnet actuator 15 It connects.As shown in Fig. 2, magnet actuator 15 include the first crank connecting link 15a, fixed hub 15b, the second crank connecting link 15c and Direct current generator 15d, wherein fixed hub 15b plays the role of positioning, direct current generator 15d to the movement of the first crank connecting link 15a Power is provided;One end of first crank connecting link 15a passes through fixed hub 15b and connect with magnet 2, and the first crank connecting link 15a's is another One end is flexibly connected with one end of the second crank connecting link 15c, and the other end of the second crank connecting link 15c is connect with direct current generator 15d And it is rotated under the drive of direct current generator 15d.The second crank connecting link 15c is driven to move after direct current generator 15d starting, the second crank Connecting rod 15c drives the first crank connecting link 15a movement, and the first crank connecting link 15a is moved up and down under the positioning of fixed hub 15b to be made Magnet 5 moves up and down simultaneously;The up and down motion band moving magnet 5 of magnet actuator 15 is constantly mobile, dynamic magnetic particle combined films In magnetic particle 9 combination is constantly rearranged under the active force in magnetic field so that the gap between magnetic particle 9 constantly replace it is loose With densifie state, so that extraction phase is constantly formed fine drop under flow regime and is become dispersed phase and be scattered in feed liquid phase, guarantees Fine drop dispersed phase constantly passes through magnetic thin layer of particulate, will not there is a situation where blocking or fluid distrbution are uneven;Magnetic simultaneously Grain under magnetic force again to magnetic field draw close movement can play the role of to dispersed phase drop it is broken, conducive to the shape of fine drop At, while the phenomenon that channel can be effectively prevent, improve extraction efficiency.
Extraction phase is broken up into fine drop via porous sieve plate 7, dynamic magnetic particle combined films by extraction phase storage room 6 Dispersed phase enters tower body 11, and 15 morning of magnet actuator movement band moving magnet is mobile, can constantly rearrange dynamic magnetic The built-up sequence of magnetic particle in particle combined films, so that loose and fine and close state is constantly replaced in the gap between magnetic particle, Tiny dispersed phase drop can be effectively prevented and deposit blocking between magnetic thin layer of particulate gap, it is ensured that dispersed phase drop is continuous Ground passes through magnetic thin layer of particulate, will not there is a situation where blocking or fluid distrbution are uneven;Magnetic particle is under magnetic force simultaneously Again dispersed phase drop can be played the role of broken by drawing close movement to magnetic field, conducive to the formation of fine drop, while can effectively be prevented Only the phenomenon that channel.
As the embodiment of the present invention, dynamic magnetic particle combined films include magnetic particle 9 and film 8, and magnetic particle 9 is in film 8 Top arrange straticulation, dynamic magnetic particle combined films include magnetic particle 9 and film 8, magnetic force of the magnetic particle 9 in magnet Under film 8 top dynamic arrangement, i.e., band moving magnet 5 moves when magnet actuator 15 moves, to make the dynamic of magnetic particle 9 Movement, magnetic particle 9 are containing Fe3O4Magnetic particle;Magnetic grain diameter can be adjusted more according to designed size droplet diameter size dimension It changes, magnetic grain diameter has to be larger than thin layer place mat aperture, to prevent containing Fe3O4Magnetic grain diameter because it is too small to caused by omit damage It loses.Magnetic-particle is evenly distributed on above thin layer place mat, and thickness is certain.Thin layer place mat membrane pore size is several microns micro- to tens Rice, thin layer place mat aperture should not be too large, also unsuitable too small, the excessive omission for being easy to cause magnetic-particle in aperture, the too small appearance in aperture Easy thin layer place mat blocking.Preferably, the thin layer place mat be silk, common cloth or steel wire, rise support magnetic thin layer of particulate and The effect for preventing magnetic particle from omitting.Magnetic thin layer of particulate is blocked up to be easy to cause dispersed phase drop to cannot pass through particle gap and increase The consequence of resistance, excessively thin may rearrange to magnetic thin layer of particulate of magnetic thin layer of particulate have some impact on, and are easy to appear a small amount of Magnetic particle is superimposed the phenomenon for causing part thin layer place mat exposed.Preferably, magnetic particle dynamic arrangement with a thickness of 3~5mm, such as Magnetic particle dynamic arrangement with a thickness of 3mm, 3.5mm, 4mm, 4.5mm, 5mm.It is excessively thin to be easy to appear extraction phase to break through magnetic particle thin It is the phenomenon that layer, blocked up to be easy to cause top magnetic particle small by magnetic force, loss is mutually washed away to easily be extracted, while blocked up May also lead to extraction phase drop cannot pass through the consequence of fine grained thin layer.Preferably, the partial size of magnetic particle is 300~600 μm, Such as the partial size of magnetic particle is 300 μm, 350 μm, 400 μm, 450 μm, 500 μm, 550 μm, 600 μm.Magnetic mean particle size must The aperture of film must be greater than, to prevent containing Fe3O4Magnetic grain diameter because it is too small to caused by omit.Preferably, the aperture of film is 1~80 μm, such as the aperture of film is 1 μm, 5 μm, 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm.Thin layer Place mat membrane pore size is several microns to tens microns, and thin layer place mat aperture should not be too large, and also unsuitable too small, aperture is excessive to be easy to lead Cause the omission of magnetic-particle, the too small easy thin layer place mat blocking in aperture.Preferably, the thin layer place mat be silk, common cloth or Steel wire plays a part of to support magnetic thin layer of particulate and prevents magnetic particle from omitting.
As a preferred solution of the present invention, extraction phase material mouth, material mouth and extraction phase slot 1 is arranged in extraction phase storage room 6 It is connected;Pressure gauge 3 and electromagnetic dosing pump 2 are successively connected between extraction phase storage room 6 and extraction phase slot 1.The bottom of tower body 11 is logical Pipeline is crossed to connect with raffinate phase collector 10.The top of tower body 11 is connect by pipeline with material liquid phase groove 12;The top of tower body 11 It is connect by pipeline with extraction phase collector 14.It is mutually compacted that sequentially connected feed liquid is additionally provided between material liquid phase groove 12 and tower body 11 Dynamic pump 13 and pressure gauge 3, so that the feed liquid in material liquid phase groove 12 mutually enters tower body 11.Expect the feed liquid in liquid phase groove 12 mutually in feed liquid Phase peristaltic pump 13 and the effect of pressure gauge 3 are lower into tower body 11;Extraction phase enters extraction phase storage room 6 through extraction phase slot 1, in pressure Across porous sieve plate 7, film 8 under the effect of the pressure of meter 3 and electromagnetic dosing pump 2, the gap across dynamic magnetic particle 9 is formed The fine drop dispersed phase of uniform particle diameter enters in feed liquid phase, and the flow direction of feed liquid phase and dispersed phase is reflux type, complete At mass transport process, by multitple extraction and split-phase, last extraction phase collector 14 is from 11 collected overhead extraction phase of tower body, raffinate phase Collector 10 is from 11 bottom collection raffinate phase of tower body.
When dynamic magnetic particle combined films extraction equipment of the invention works, magnet 5 is under the action of magnet actuator 15 It constantly moves up and down, extraction phase enters extraction phase storage room 6 by extraction phase slot 1 under extrapolability, passes through porous sieve plate 7, film 8 With magnetic particle 9, becomes the feed liquid phase that the dispersed phase of fine drop enters in tower body 11 and move upwards, feed liquid is mutually by material liquid phase groove Enter in tower body 11 in 12 and move downward, the motion mode with dispersed phase is adverse current, and dispersed phase passes through to the mesh in feed liquid phase Mark particle is extracted, and last extraction phase collector 14 is from 11 collected overhead extraction phase of tower body, and raffinate phase collector 10 is from tower body 11 bottom collection raffinate phases, as shown in Figure 3.
Two working conditions when magnet actuator work are shown such as Fig. 4 (a), 4 (b), are made in magnet actuator Under, magnet quickly moves up and down and the magnetic particle constantly rise and fall under the impact force action of fluid, and magnetic particle is thin Layer is rearranged, and the fine drop of uniform particle sizes out is efficiently uninterruptedly dispersed.
Preferably, the amplitude of magnet actuator 15 and frequency have certain requirement, certain amplitude with Rotational frequency moves up and down cylinder-shaped magnet quickly, guarantees magnetic thin layer of particulate in continuous under the magnetic force of Strength Changes Dynamic arrangement state.The amplitude of magnet actuator 15 is 8~12cm;Preferably, the rotational frequency of magnet actuator 15 It is 20~50 revs/min.
As further preferred scheme, dynamic magnetic particle combined films extraction equipment of the invention further includes being located at extraction phase The base support 4 of 6 lower section of storage room, magnet 5 are set to the inside of base support 4, and the volume of base support 4 is greater than magnet 5 Volume.Preferably, magnet 5 is cylinder-shaped magnet, and the S grade of cylinder-shaped magnet or N grades are upward.Base support volume is greater than magnet, Magnet is facilitated flexibly to move up and down;Magnet is cylinder-shaped magnet, and N grades or S grades upwards, guarantees the same water above thin layer place mat Square to the magnetic force that is subject to of magnetic particle it is uniform.
The height of extraction phase storage room 6 be 10~15mm, such as extraction phase storage room height be 10mm, 11mm, 12mm, 13mm, 14mm, 15mm, height can not be excessively high, in order to guarantee that magnet and magnetic particle have sufficiently strong magnetic field.
Preferably, porous sieve plate 7 is the porous sieve plate of organic glass material, and the aperture of porous sieve plate 7 is 2~6mm, such as The aperture of porous sieve plate is 2mm, 3mm, 4mm, 5mm, 6mm;Preferably, the porosity of the porous sieve plate is 20~30%.Hole Spacing can not be excessive, too small apart from the too long porosity that will cause, but be easy to cause if too short between sieve plate pore and break It is broken, cause damages of screen deck.It is further preferred that the porosity of porous sieve plate 7 is 20~30%.
The extraction phase is used as dispersed phase, the extractant and the diluent in dynamic magnetic particle combination membrane extraction Volume ratio is (1~5): (5~10), such as the volume ratio of extractant and diluent is 1:1,1:2,1:3,1:4,1:5,1:6,1: 7、1:8、1:9、1:10、2:3、2:5、2:7、2:9、3:5、3:7、3:8、3:10、4:5、4:7、4:9、5:6、5:7、5:8、5:9。 Preferably, the extractant is tributyl phosphate (TBP);It is further preferred that the diluent is that (No. 260 molten for sulfonated kerosene Agent oil).The feed liquid is mutually used as continuous phase in dynamic magnetic particle combination membrane extraction, and the object ion is propionic acid, 3- hydroxyl One of propionic acid and 2 hydroxy propanoic acid or at least two mixture.
The extracting process of dynamic magnetic particle combined films extraction equipment of the invention are as follows: made with the aqueous solution containing object ion For feed liquid phase, the mixed solution to contain extractant and diluent is opened on magnet actuator band moving magnet as extraction phase Lower movement, the magnetic particle in dynamic magnetic particle combined films dynamically rearrange combination, and the extraction phase passes through the dynamic magnetic The magnetic particle of the dynamic mobile of particle combined films formed uniformly tiny droplet distribution in the feed liquid phase, the feed liquid phase with The type of flow of the extraction phase is adverse current;Object ion mass transfer in the feed liquid phase is carried out into the drop of the extraction phase Extraction.
By designing dynamic magnetic thin layer of particulate in conjunction with thin layer place mat film in dynamic magnetic particle combined films, so that magnetic particle Between gap constantly replace loose with fine and close state, tiny dispersed phase drop can be effectively prevented in magnetic thin layer of particulate gap Between deposit blocking, it is ensured that dispersed phase drop constantly passes through magnetic thin layer of particulate, will not occur blocking or fluid distrbution Uneven situation;Magnetic particle draws close movement to magnetic field again under magnetic force simultaneously can broken work to dispersed phase drop With conducive to the formation of fine drop, while the phenomenon that channel can be effectively prevent;It is acted in magnetic force and fluid impingement force Under, the tiny dispersed phase drop for constantly springing up out uniform particle sizes is scattered among feed liquid phase, by magnetic fields, is not being changed Under conditions of extraction mechanism, raising extraction efficiency is improved.
Embodiment 1
In the present embodiment, TBP extractant and sulfonated kerosene diluent volume ratio are 2:8, mixing composition organic extraction phase.Material Liquid phase is the aqueous solution containing propionic acid, propionate concentration 0.405mol/L, solution ph 2.63.Wherein, dynamic magnetic particle combines In film, the magnetic particle used is containing Fe304Magnetic particle, the partial size of magnetic particle 9 is about 500 μm, and the thickness of magnetic particle is about 3mm; Using steel wire as thin layer place mat, aperture is 10 μm;It uses sieve plate for organic glass, is covered with the pore that aperture is 5mm, hole Gap rate is 24%, thin layer place mat effective area 20.25cm2;The amplitude of magnet actuator be 10cm, rotational frequency be 20 turns/ Point, the magnet used is cylinder-shaped magnet, and S grades are upwards, and the magnetic numerical density in same level direction is uniform above thin layer place mat, and And the magnetic force that bottom magnetic particle is subject to is greater than the magnetic force that magnetic particle in upper layer is subject to.The extraction efficiency of the present embodiment It is 55%.
Embodiment 2
In the present embodiment, TBP extractant and sulfonated kerosene diluent volume ratio are 3:7, mixing composition organic extraction phase.Material Liquid phase is the aqueous solution containing propionic acid, propionate concentration 0.405mol/L, solution ph 2.63.Wherein, dynamic magnetic particle combines In film, the magnetic particle used is containing Fe304Magnetic particle, the partial size of magnetic particle 9 is about 500 μm, and the thickness of magnetic particle is about 3mm; Using steel wire as thin layer place mat, aperture is 10 μm;It uses sieve plate for organic glass, is covered with the pore that aperture is 5mm, hole Gap rate is 24%, thin layer place mat effective area 20.25cm2;The amplitude of magnet actuator be 12cm, rotational frequency be 40 turns/ Point, the magnet used is cylinder-shaped magnet, and S grades are upwards, and the magnetic numerical density in same level direction is uniform above thin layer place mat, and And the magnetic force that bottom magnetic particle is subject to is greater than the magnetic force that magnetic particle in upper layer is subject to.The extraction efficiency of the present embodiment It is 62%.
Embodiment 3
In the present embodiment, TBP extractant and sulfonated kerosene diluent volume ratio are 4:6, mixing composition organic extraction phase.Material Liquid phase is the aqueous solution containing propionic acid, propionate concentration 0.405mol/L, solution ph 2.63.Wherein, dynamic magnetic particle combines In film, the magnetic particle used is containing Fe304Magnetic particle, the partial size of magnetic particle 9 is about 500 μm, and the thickness of magnetic particle is about 3mm; Using steel wire as thin layer place mat, aperture is 10 μm;It uses sieve plate for organic glass, is covered with the pore that aperture is 5mm, hole Gap rate is 24%, thin layer place mat effective area 20.25cm2;The amplitude of magnet actuator be 8cm, rotational frequency be 50 turns/ Point, the magnet used is cylinder-shaped magnet, and S grades are upwards, and the magnetic numerical density in same level direction is uniform above thin layer place mat, and And the magnetic force that bottom magnetic particle is subject to is greater than the magnetic force that magnetic particle in upper layer is subject to.The extraction efficiency of the present embodiment It is 73%.
Comparative example
Compared with Example 1, the magnetic numerical density in same level direction is uniform above the thin layer place mat of this comparative example, and The magnetic force that bottom magnetic particle is subject to is greater than the magnetic force that magnetic particle in upper layer is subject to, the difference is that extraction phase squeezes into material Extrapolability in liquid phase is greater than magnet to the magnetic force of magnetic particle, other extraction conditions are identical as embodiment 1, this comparison The extraction efficiency of example is 47.6%.
Above embodiments are only used to illustrate method detailed of the invention, and the invention is not limited to above-mentioned method detaileds, i.e., Do not mean that the invention must rely on the above detailed methods to implement.It should be clear to those skilled in the art, right Any improvement of the invention, the addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, the selection of concrete mode Deng all of which fall within the scope of protection and disclosure of the present invention.

Claims (31)

1. a kind of dynamic magnetic particle combined films extraction equipment, which is characterized in that described device includes tower body (11), extraction phase storage Room (6), porous sieve plate (7), dynamic magnetic particle combined films, magnet (5) and magnet actuator (15);Wherein, the extraction phase Storage room (6) is located at below tower body (11), is disposed with from the bottom to top between the extraction phase storage room (6) and tower body (11) Porous sieve plate (7) and dynamic magnetic particle combined films are placed with the magnet (5) and magnetic below the extraction phase storage room (6) Iron transmission device (15), the magnet (5) are connected with the magnet actuator (15).
2. dynamic magnetic particle combined films extraction equipment according to claim 1, which is characterized in that the magnet actuator (15) described including the first crank connecting link (15a), fixed hub (15b), the second crank connecting link (15c) and direct current generator (15d) One end of first crank connecting link (15a) passes through the fixed hub (15b) and connect with the magnet (2), and first crank connects The other end of bar (15a) is flexibly connected with one end of second crank connecting link (15c), second crank connecting link (15c) The other end connect with the direct current generator (15d) and rotates under the drive of the direct current generator (15d).
3. dynamic magnetic particle combined films extraction equipment according to claim 1 or 2, which is characterized in that the magnet transmission The amplitude of device (15) is 8~12cm.
4. dynamic magnetic particle combined films extraction equipment according to claim 1 or 2, which is characterized in that the magnet transmission The rotational frequency of device (15) is 20~50 revs/min.
5. dynamic magnetic particle combined films extraction equipment according to claim 1, which is characterized in that the dynamic magnetic particle group Closing film includes magnetic particle (9) and film (8), and the magnetic particle (9) is under the magnetic fields of the magnet (5) in the film (8) top dynamic arrangement, the magnetic particle (9) are containing Fe3O4Magnetic particle.
6. dynamic magnetic particle combined films extraction equipment according to claim 5, which is characterized in that the magnetic particle (9) is dynamic State arrangement with a thickness of 3~5mm.
7. dynamic magnetic particle combined films extraction equipment according to claim 5, which is characterized in that the partial size of the magnetic particle It is 300~600 μm.
8. dynamic magnetic particle combined films extraction equipment according to claim 5, which is characterized in that the aperture of the film is 1~80 μm.
9. dynamic magnetic particle combined films extraction equipment according to claim 1, which is characterized in that described device further includes position Base support (4) below the extraction phase storage room (6), the magnet (5) are set to the interior of the base support (4) Portion, the volume of the base support (4) are greater than the volume of the magnet (5).
10. dynamic magnetic particle combined films extraction equipment according to claim 9, which is characterized in that the extraction phase storage Extraction phase material mouth is arranged in room (6), and the material mouth is connected with extraction phase slot (1).
11. dynamic magnetic particle combined films extraction equipment according to claim 9, which is characterized in that the extraction phase storage Pressure gauge (3) and electromagnetic dosing pump (2) are successively connected between room (6) and extraction phase slot (1).
12. dynamic magnetic particle combined films extraction equipment according to claim 1, which is characterized in that the tower body (11) Bottom is connect by pipeline with raffinate phase collector (10).
13. dynamic magnetic particle combined films extraction equipment according to claim 1, which is characterized in that the tower body (11) Top is connect by pipeline with material liquid phase groove (12).
14. dynamic magnetic particle combined films extraction equipment according to claim 1, which is characterized in that the tower body (11) Top is connect by pipeline with extraction phase collector (14).
15. dynamic magnetic particle combined films extraction equipment according to claim 13, which is characterized in that the material liquid phase groove (12) sequentially connected feed liquid phase peristaltic pump (13) and pressure gauge (3) are additionally provided between the tower body (11), so that described Feed liquid in material liquid phase groove (12) mutually enters the tower body (11).
16. dynamic magnetic particle combined films extraction equipment according to claim 1, which is characterized in that the extraction phase storage The height of room (6) is 10~15mm.
17. dynamic magnetic particle combined films extraction equipment according to claim 1, which is characterized in that the porous sieve plate (7) For the porous sieve plate of organic glass material, the aperture of the porous sieve plate (7) is 2~6mm.
18. dynamic magnetic particle combined films extraction equipment according to claim 17, which is characterized in that the porous sieve plate (7) porosity is 20~30%.
19. dynamic magnetic particle combined films extraction equipment according to claim 1, which is characterized in that the magnet (5) is circle Cylindrical magnetic iron, the S grade of the cylinder-shaped magnet or N grades are upwards.
20. a kind of extracting process using dynamic magnetic particle combined films extraction equipment described in one of claim 1-19, special Sign is, the extracting process are as follows: to contain the aqueous solution of object ion as feed liquid phase, with containing extractant and diluent Mixed solution as extraction phase, the extraction phase pass through the dynamic magnetic particle combined films formed uniformly tiny droplet distribution in In the feed liquid phase, the type of flow of the feed liquid phase and the extraction phase is adverse current;Object ion in the feed liquid phase passes Matter is extracted into the drop of the extraction phase.
21. extracting process according to claim 20, which is characterized in that the extraction phase squeezes into the feed liquid by extrapolability Xiang Zhong, the extrapolability no more than the lower section of feed liquid phase storage room magnet to the magnetic fields of the magnetic particles of magnetic particle combined films Power.
22. extracting process according to claim 21, which is characterized in that magnetic fields of the magnetic particle in the magnet Under the film top dynamic arrangement, the magnetic particle be containing Fe3O4Magnetic particle.
23. extracting process according to claim 22, which is characterized in that the magnetic particle dynamic arrangement with a thickness of 3~ 5mm。
24. extracting process according to claim 22, which is characterized in that the partial size of the magnetic particle is 300~600 μm.
25. extracting process according to claim 22, which is characterized in that the aperture of the film is 1~80 μm.
26. extracting process according to claim 22, which is characterized in that the film is thin layer place mat.
27. extracting process according to claim 26, which is characterized in that the thin layer place mat is silk, common cloth or steel Silk screen.
28. extracting process according to claim 20, which is characterized in that the volume ratio of the extractant and the diluent For (1~5): (5~10).
29. extracting process according to claim 20, which is characterized in that the extractant is tributyl phosphate.
30. extracting process according to claim 20, which is characterized in that the diluent is sulfonated kerosene.
31. extracting process according to claim 20, which is characterized in that the feed liquid is mutually in magnetic particle combination membrane extraction As continuous phase, the object ion is the mixing of one of propionic acid, 3- hydracrylic acid and 2 hydroxy propanoic acid or at least two Object.
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CN102233200A (en) * 2010-09-15 2011-11-09 中国科学院过程工程研究所 Vibrating screen plate tower for continuous production of liquid-liquid-liquid three-phase extraction
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US2614064A (en) * 1949-10-31 1952-10-14 Phillips Petroleum Co Method of and apparatus for liquid-liquid contacting
GB737789A (en) * 1952-08-20 1955-10-05 Atomic Energy Authority Uk Improvements in or relating to columns for liquid-liquid extraction processes
CN1142783A (en) * 1993-12-10 1997-02-12 英国核子燃料公司 Separation of liquids
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