CN102120194A - Magnetic-particle in-situ separation device for magnetic stabilization fluidized bed - Google Patents
Magnetic-particle in-situ separation device for magnetic stabilization fluidized bed Download PDFInfo
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- CN102120194A CN102120194A CN2010100338611A CN201010033861A CN102120194A CN 102120194 A CN102120194 A CN 102120194A CN 2010100338611 A CN2010100338611 A CN 2010100338611A CN 201010033861 A CN201010033861 A CN 201010033861A CN 102120194 A CN102120194 A CN 102120194A
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Abstract
The invention provides a magnetic-particle in-situ separation device for a magnetic stabilization fluidized bed, which comprises a magnetic stabilization fluidized bed and is characterized by also comprising a permanent magnet in-situ separation system positioned inside the magnetic stabilization fluidized bed, wherein the in-situ separation system comprises an isolation cylinder provided with a sealing bottom, the center of the isolation cylinder is provided with a discharging hole, and the isolation cylinder is nested and fixed on an upper port of a sleeve; two coaxially arranged annular permanent magnets are placed in the isolation cylinder; the two annular permanent magnets are respectively fixed on the bottom ends of crank connecting links of two crank-link mechanisms through fixed shaft sleeves, the upper ends of the crank connecting links are connected with disks rotating around a shaft, and the two disks are driven synchronously and reversely by a motor to carry out up and down periodical reciprocating motion in a reverse direction; and a tapered reducing hopper is arranged under the isolation cylinder, an arc-shaped baffle plate is arranged at the undermost of the tapered reducing hopper, and the arc-shaped baffle plate is connected with a guide pipe at the tail end of the tapered reducing hopper through a connecting rod.
Description
Technical field
The present invention relates to a kind of magnetic-particle separator, specially refer to a kind of magnetic stabilization fluid bed magnetic-particle in-situ separating device that is used for.
Background technology
Super-paramagnetism nano/micron particles is owing to have very big surface area, and surface-active is very high, and is therefore very unstable on thermodynamics, is easy to conglomerate.In order to prevent the cohesion between the magnetic-particle, make it form stable colloidal solution, need in preparation process, modify the magnetic-particle surface, should have more rich activity functional groups through the magnetic-particle surface of modifying, as-NH2 ,-COOH ,-OH and-CHO etc., so that conjugated biological molecules and affinity ligand, obtain being fit to the suitable magnetic carrier of various application.Magnetic particle is contained in magnetic-particle inside, has superparamagnetism, shows magnetic preferably under the externally-applied magnetic field when having, and after removing externally-applied magnetic field, the remanent magnetism of magnetic-particle is zero, thereby it can be controlled under the effect of externally-applied magnetic field and separate easily.This magnetic-particle surface itself has or has by surface modification the functional group of various active, can carry out the separation of bioactivator (as protein, nucleic acid, enzyme etc.), can come the big molecule of selectivity ground separating bio by coupling specificities molecule (as ligands specific, antibody, antigen etc.), also can carry out the immobilization of enzyme and carry out corresponding enzymic catalytic reaction.In addition, super-paramagnetism nano/micron particles is after the process finishing, and the chemical reaction catalyst that can be directly used in chemical synthesis, field of petrochemical industry carries out the chemical catalysis reaction.Thereby super-paramagnetism nano/micron carrier has a wide range of applications in fields such as the separation of biological product, enzymatic, chemical catalysis.
Magnetic field fluidized bed (Magnetically Fluidized Bed, MFB) be that common fluid bed is introduced in the magnetic field that will add, adopt the solid-liquid phase treatment system of magnetosensitive particle as the bed medium, being the product that fluidization technology combines with electromagnetic technique, is a kind of novel, fluidization technology efficiently.And magnetic stabilization fluid bed (MagneticallyStabilized Fluidized Bed MSFB) is the special shape of MFB, and it forms, has only the stable bed of faint motion under axial time-independent uniform magnetic field.MFB and MSFB have that vibration is little, noise is little, good stability, opereating specification is wide and characteristics such as wide adaptability, integrates the advantage of fixed bed and traditional fluid bed simultaneously: solid particle is easy to loading and unloading, can be recycled; Mass-and heat-transfer speed is high, has very high exploitation to be worth and wide application prospect.
In order to satisfy the demands of applications of super-paramagnetism nano/micron particles, magnetic stabilization fluid bedly used widely in fields such as the separation of biological product, enzymatic, chemical catalysis.Yet along with the development of material science, the magnetic-particle of employing all is nanoscale or the micron particles with large surface area, and this causes magnetic-particle very easily to be overflowed from magnetic field fluidized bed.Magnetic stabilization fluid bed general employing solenoid produces magnetic field, exists following problems in magnetic stabilization fluid bed actual application: a small amount of thin magnetic-particle support/catalyst is flowed out by liquid entrainment from reactor exit, causes the loss of separating medium; Be Anti-lost, usually the voltage and current that adds solenoid by increase strengthens magnetic field intensity, this way not only can increase the energy consumption of magnetic field fluidized bed operation, and under high-intensity magnetic field, the magnetic stabilization fluid bed freezing zone that is in, the magnetic absorption carrier is chain, channeling occurs in the bed, the fluid skewness causes mass-transfer efficiency to reduce.
Summary of the invention
The objective of the invention is to, be the magnetic stabilization fluid bed defective that exists of carrier of separating/catalyst for overcoming above-mentioned having now, thereby a kind of magnetic stabilization fluid bed magnetic-particle in-situ separating device that is used for is provided with super-paramagnetism nano/micron particles.
The device that the present invention proposes can be realized effective separation of magnetic field fluidized bed middle effusion nanoscale/micron order magnetic-particle, and will recycle in the magnetic-particle Returning reactor, and simple in structure, easy to operate.
To achieve these goals, a kind of magnetic stabilization fluid bed magnetic-particle in-situ separating device that is used for of the present invention, this device comprises one magnetic stabilization fluid bed 9, described magnetic stabilization fluid bed 9 comprise: a sleeve 6, described sleeve 6 comprises the cylindrical drum part on top and the conical section of bottom, the cylindrical drum part on described top and the conical section of bottom are cut apart by liquid distributing board 10, the bottom center of the conical section of described bottom has a liquid inlet opening 11, and the outside of described sleeve 6 is installed with one group of solenoid group 8; It is characterized in that,
Described device comprises that also one is positioned at the permanent magnet original position piece-rate system 17 of magnetic stabilization fluid bed 9 inside, and this permanent magnet original position piece-rate system 17 comprises:
One has the isolating cylinder 5 that the sealing end and center have discharging opening 14, the described isolating cylinder 5 nested upper port that are fixed on sleeve 6; Place the annular permanent magnet 15 of two coaxial arrangement in the described isolating cylinder 5, the magnetic field intensity of described annular permanent magnet is 2000~4000 oersteds; Described two annular permanent magnets 15 are fixed on the bottom of the crank connecting link 4 of two toggles 2 respectively by fixed hub 3, crank connecting link 4 upper ends link to each other with the disk 1 that pivots, two disks 1 are driven by motor 13 synchronous backwards, and then described two annular permanent magnets carry out rightabout cyclic movement up and down; Be provided with cone hopper 19 under the described isolating cylinder 5, the below of described cone hopper 19 is provided with a circular arc baffle plate 22, described circular arc baffle plate 22 links to each other with the mozzle 20 of cone hopper 19 ends by connecting rod 21, and the lower edge circle diameter of described circular arc baffle plate 22 is 1: 1.1~1.3 with mozzle 20 diameters ratio.
As an improvement of the present invention, be positioned at isolating cylinder 5 belows on the inwall of described sleeve 6 and be provided with ring baffle 7, the outer wall that the interior anchor ring of this ring baffle 7 is positioned at isolating cylinder 5 along the line in; This ring baffle 7 is used to prevent that magnetic-particle from entering the annular space that forms between isolating cylinder 5 outer walls and sleeve 6 inwalls and partly forming the dead angle.
Described cone hopper 19 is fixed in ring baffle 7 belows by fixed bar 18, and its upper edge is positioned at the top of the solenoid 8 of peripheral hardware, its upper edge circumference be positioned at the outer wall circumference of isolating cylinder 5 along the line beyond.
As another improvement of the present invention, also be fixed with the boad which can insolate flux 16 of a coaxial layout in the described isolating cylinder 5, form double-layer sleeve structure, this double-layer sleeve structure is used for placing respectively the annular permanent magnet 15 of two coaxial arrangement.Described boad which can insolate flux 16 is made by the plastics with separated magnetic effect, and the upper edge circumference of the top cylindrical drum of the upper edge circumference of described isolating cylinder 5 and sleeve 6 is in same horizontal plane.
The material of described sleeve 6, isolating cylinder 5, cone hopper 19 or ring baffle 7 is stainless steel, glass or plastics.
The invention has the advantages that the continuous piece-rate system 17 of described permanent magnet original position is positioned at magnetic field fluidized bed inside, can realize that the original position of magnetic-particle is separated, simplicity of design, easy and simple to handle; The design of circular arc baffle plate 22 can effectively realize the recycling of magnetic-particle, prevents the interference of ascending fluid to decline magnetic-particle in the mozzle 20, alleviates decline magnetic-particle in the mozzle 20 to magnetic stabilization fluid bed 9 disturbance; By the periodic motion of annular permanent magnet 15, can under the prerequisite that guarantees magnetic field fluidized bed continuous running, realize continuous separation to the effusion magnetic-particle.In addition, the continuous permanent magnet continuous separation device of magnetic-particle of the present invention is used for carrying out the magnetic stabilization fluid bed of solid-liquid two phase reaction, cyclic movement by annular permanent magnet 15, the absorption and the disengaging of magnetic-particle hocket, can reach catching and discharge to nanoscale/micron order magnetic-particle, and enter recycling, help improving magnetic stabilization fluid bed operational efficiency.
Description of drawings
Fig. 1 is the structural representation of magnetic-particle permanent magnet in-situ separating device of the present invention;
Fig. 2 is a kind of user mode schematic diagram of magnetic-particle permanent magnet in-situ separating device of the present invention;
Fig. 3 is the another kind of user mode schematic diagram of magnetic-particle permanent magnet in-situ separating device of the present invention.
The accompanying drawing sign
1, disk 2, toggle 3, fixed hub
4, crank connecting link 5, isolating cylinder 6, sleeve
7, ring baffle 8, solenoid 9, magnetic stabilization fluid bed
10, liquid distributing board 11, liquid inlet opening 12, driving-belt
13, direct current generator 14, discharging opening 15, annular permanent magnet
16, boad which can insolate flux 17, the continuous piece-rate system 18 of permanent magnet original position, fixed bar
19, cone hopper 20, mozzle 21, connecting rod
22, curved baffle 23, magnetic-particle
The specific embodiment
Below in conjunction with the drawings and specific embodiments, device of the present invention and result of use thereof are described.
As shown in Figure 1, of the present invention magnetic stabilization fluid bed 9 and permanent magnet original position piece-rate system 17.
Wherein, magnetic stabilization fluid bed 9 have a sleeve 6, and sleeve 6 bottoms are taper, the barrel of sleeve 6 is provided with ring baffle 7, below the fluid bed the inside liquid distributing board 10 is housed, the fluid bed bottom center has a liquid inlet opening 11, and magnetic stabilization fluid bed 9 outside is provided with one group of solenoid 8.
One permanent magnet original position piece-rate system 17, have one to have the isolating cylinder 5 that seals the end, the isolating cylinder 5 inner coaxial boad which can insolate flux 16 that set firmly, the double-decker that composition is made of two concentric different radii cylinders, a discharging opening 14 is established at isolating cylinder 5 centers, isolating cylinder 5 is fixedly mounted on the center on sleeve 6 tops, place the annular permanent magnet 15 of two coaxial arrangement in the isolating cylinder 5, annular permanent magnet 15 is fixed on the bottom of the crank connecting link 4 of two toggles 2, fasten dead axle cover 3 on the crank connecting link 4 and its upper end links to each other with the disk 1 that pivots, two disks 1 are by a direct current motor 13 driven in synchronism, isolating cylinder 5 belows are provided with cone hopper 19, cone hopper 19 is fixed on the ring baffle 7 by fixed bar 18, the below of cone hopper 19 is provided with a circular arc baffle plate 22, and circular arc baffle plate 22 links to each other with the end of cone hopper 19 by connecting rod 21.
Described boad which can insolate flux 16 is made by the plastics with separated magnetic effect;
The radius difference of described two annular permanent magnets 15, size matches with the size of isolating cylinder 5, and its magnetic field intensity is 2800 oersteds.
The lower edge circle diameter of described circular arc baffle plate 22 is 1: 1.2 with the mozzle 20 diameters ratio of cone hopper 19;
The material of described magnetic field fluidized bed sleeve 6, isolating cylinder 5, cone hopper 19, baffle plate is stainless steel, glass or plastics.
The course of work of this device is: see also Fig. 2 and Fig. 3, magnetic-particle 23 in magnetic stabilization fluid bed 9 is in stable state, a small amount of magnetic-particle 23 is along with the isolating cylinder 5 of the continuous piece-rate system 17 of permanent magnet original position of the present invention of being flowed through by the liquid that flows out in the fluid bed, when annular permanent magnet 15 is in position among Fig. 2, magnetic-particle 23 is under the effect of interior ring annular permanent magnet 15, can being captured also at the outer low side of isolating cylinder 5, coalescence becomes piece, when annular permanent magnet 15 carries out misorientation motion and is in the position of Fig. 3, the effect that coalescence becomes the magnetic-particle 23 of piece to break away from magnetic field, become graininess under the effect of gravity, to fall in the cone hopper 19 again, and and then enter mozzle 20, after circular arc baffle plate 22 disperses, enter magnetic field fluidized bed by mozzle 20, participation recycles, simultaneously, to the flow through magnetic-particle 23 of isolating cylinder 5 of outer shroud annular permanent magnet 15 is caught, and become piece at the outer low side coalescence of isolating cylinder 5, when annular permanent magnet 15 carries out misorientation motion once more and is in the position of Fig. 2, the effect that coalescence becomes the magnetic-particle 23 of piece to break away from magnetic field is fallen in the cone hopper 19, and participation recycles, interior ring annular permanent magnet 15 carries out the seizure of magnetic-particle 23 again, when annular permanent magnet 15 moves back and forth, the continuous piece-rate system 17 of permanent magnet original position can be carried out continuous separation to the magnetic-particle 23 that flows out in magnetic stabilization fluid bed 9, and makes it reenter magnetic stabilization fluid bed 9 to participate in and recycle.When described annular permanent magnet 15 moves back and forth: owing to be provided with the annular permanent magnet 15 that links with toggle 2 in the isolating cylinder 5, two annular permanent magnets 15 are set to as Fig. 2 or original state shown in Figure 3, toggle 2 is driven by direct current generator 13, and through fixed hub 3 rotation is changed into and to pump, make two annular permanent magnets 15 can produce the reciprocating motion of misorientation up and down, thereby realize the mutual conversion of this device between Fig. 2 and Fig. 3 two states.
The magnetic-particle 23 of present embodiment is with magnetic polyvinyl acetate microsphere surface grafting methyl propenoic acid glycidyl fat and the synthetic Cu of iminodiacetic acid
2+The affine absorption magnetic microsphere (PVA-g-GMA-IDA-Cu of chelating
2+), experimental results show that this magnetic microsphere has superparamagnetism.
In device of the present invention, carry out magnetic microsphere (PVA-g-GMA-IDA-Cu
2+) reaction of absorption laccase albumen, 25 ℃ of normal temperature, magnetic microsphere (PVA-g-GMA-IDA-Cu
2+) as absorption carrier, magnetic microsphere concentration 100mg/ml in magnetic stabilization fluid bed 9, liquid inlet opening 11 protein concentration 0.1mg/ml carry out magnetic microsphere (PVA-g-GMA-IDA-Cu according to the method described above
2+) the continuous in-situ lock out operation, at discharging opening 14 timing samplings, the outflow situation of centrifugal mensuration magnetic-particle 23 does not see that obvious magnetic microsphere flows out in the adsorption process.
Embodiment 2
The magnetic-particle 23 of present embodiment is active Ni catalyst, experimental results show that this magnetic microsphere has superparamagnetism.
In device of the present invention, carry out the reaction of caprolactam catalytic hydrogenation, 80 ℃ of reaction temperatures, the active Ni of magnetic is as catalyst, catalyst concn 20% (w/v) in magnetic stabilization fluid bed 9, liquid inlet opening 11 contains the caprolactam water solution concentration 32% (w/v) of dissolved hydrogen, carries out the continuous in-situ lock out operation of active Ni in magnetic stabilization fluid bed 9 according to the method described above, in the adsorption process at discharging opening 14 timing samplings, the outflow situation of the active Ni of centrifugal mensuration does not see that obvious active Ni flows out.
It should be noted last that above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although the present invention is had been described in detail with reference to embodiment, those of ordinary skill in the art is to be understood that, technical scheme of the present invention is made amendment or is equal to replacement, do not break away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (10)
1. one kind is used for magnetic stabilization fluid bed magnetic-particle in-situ separating device, this device comprises one magnetic stabilization fluid bed (9), described magnetic stabilization fluid bed (9) comprise: a sleeve (6), described sleeve (6) comprises the cylindrical drum part on top and the conical section of bottom, the cylindrical drum part on described top and the conical section of bottom are cut apart by liquid distributing board (10), the bottom center of the conical section of described bottom has a liquid inlet opening (11), and the outside of described sleeve (6) is installed with one group of solenoid group (8); It is characterized in that,
Described device comprises that also one is positioned at magnetic stabilization fluid bed (9) inner permanent magnet original position piece-rate system (17), and this permanent magnet original position piece-rate system (17) comprises:
One has the isolating cylinder (5) that the sealing end and center have discharging opening (14), the nested upper port that is fixed on sleeve (6) of described isolating cylinder (5); Place the annular permanent magnet (15) of two coaxial arrangement in the described isolating cylinder (5);
Described two annular permanent magnets (15) are fixed on the bottom of the crank connecting link (4) of two toggles (2) respectively by fixed hub (3), crank connecting link (4) upper end links to each other with the disk that pivots (1), two disks (1) are driven by motor (13) synchronous backward, and then described two annular permanent magnets carry out rightabout cyclic movement up and down;
Be provided with cone hopper (19) under the described isolating cylinder (5), the below of described cone hopper (19) is provided with a circular arc baffle plate (22), and described circular arc baffle plate (22) links to each other by the mozzle (20) of connecting rod (21) with cone hopper (19) end.
2. according to claim 1ly be used for magnetic stabilization fluid bed magnetic-particle in-situ separating device, it is characterized in that, be positioned at isolating cylinder (5) below on the inwall of described sleeve (6) and be provided with ring baffle (7), the outer wall that the interior anchor ring of this ring baffle (7) is positioned at isolating cylinder (5) along the line in; This ring baffle (7) is used to prevent that magnetic-particle from entering the annular space that forms between isolating cylinder (5) outer wall and sleeve (6) inwall and partly forming the dead angle.
3. according to claim 2ly be used for magnetic stabilization fluid bed magnetic-particle in-situ separating device, it is characterized in that described cone hopper (19) is fixed in ring baffle (7) below by fixed bar (18).
4. describedly be used for magnetic stabilization fluid bed magnetic-particle in-situ separating device according to claim 1 or 3, it is characterized in that, the upper edge of described cone hopper (19) is positioned at the top of the solenoid (8) of peripheral hardware, its upper edge circumference be positioned at the outer wall circumference of isolating cylinder (5) along the line beyond.
5. according to claim 1ly be used for magnetic stabilization fluid bed magnetic-particle in-situ separating device, it is characterized in that, also be fixed with the boad which can insolate flux (16) of a coaxial layout in the described isolating cylinder (5), form double-layer sleeve structure, this double-layer sleeve structure is used for placing respectively the annular permanent magnet (15) of two coaxial arrangement.
6. according to claim 5ly be used for magnetic stabilization fluid bed magnetic-particle in-situ separating device, it is characterized in that described boad which can insolate flux (16) is made by the plastics with separated magnetic effect.
7. according to claim 1ly be used for magnetic stabilization fluid bed magnetic-particle in-situ separating device, it is characterized in that the upper edge circumference of the top cylindrical drum of the upper edge circumference of described isolating cylinder (5) and sleeve (6) is in same horizontal plane.
8. according to claim 1ly be used for magnetic stabilization fluid bed magnetic-particle in-situ separating device, it is characterized in that the magnetic field intensity of described annular permanent magnet is 2000~4000 oersteds.
9. according to claim 1ly be used for magnetic stabilization fluid bed magnetic-particle in-situ separating device, it is characterized in that the lower edge circle diameter of described circular arc baffle plate (22) and mozzle (20) diameter ratio are 1: 1.1~1.3.
10. according to claim 1ly be used for magnetic stabilization fluid bed magnetic-particle in-situ separating device, it is characterized in that the material of described sleeve (6), isolating cylinder (5), cone hopper (19) or ring baffle (7) is stainless steel, glass or plastics.
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Cited By (7)
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CN105057097A (en) * | 2015-09-16 | 2015-11-18 | 重庆市九瑞粉末冶金有限责任公司 | Waterfall type separation device for magnetic iron powder particles |
CN105344467A (en) * | 2014-08-21 | 2016-02-24 | 扬州市大洋水务设备有限公司 | Novel magnetic separation settler |
CN106573215A (en) * | 2014-06-24 | 2017-04-19 | 巴斯夫欧洲公司 | Method for self-regulation of a system |
CN108176504A (en) * | 2017-12-27 | 2018-06-19 | 武汉科技大学 | A kind of magnetic powder superposed layer forming apparatus |
CN108500852A (en) * | 2018-05-31 | 2018-09-07 | 富士和机械工业(湖北)有限公司 | A kind of precision casting sanding system |
CN110684655A (en) * | 2019-10-18 | 2020-01-14 | 江苏大学 | Microalgae separation gradient magnetic stabilization fluidized bed device and microalgae harvesting method thereof |
CN111215240A (en) * | 2019-11-13 | 2020-06-02 | 鞍钢集团矿业有限公司 | Multilayer magnetic system selection magnetic separator |
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Cited By (9)
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CN106573215A (en) * | 2014-06-24 | 2017-04-19 | 巴斯夫欧洲公司 | Method for self-regulation of a system |
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CN110684655A (en) * | 2019-10-18 | 2020-01-14 | 江苏大学 | Microalgae separation gradient magnetic stabilization fluidized bed device and microalgae harvesting method thereof |
CN110684655B (en) * | 2019-10-18 | 2023-03-17 | 江苏大学 | Microalgae separation gradient magnetic stabilization fluidized bed device and microalgae harvesting method thereof |
CN111215240A (en) * | 2019-11-13 | 2020-06-02 | 鞍钢集团矿业有限公司 | Multilayer magnetic system selection magnetic separator |
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