CN101352669B - Multichannel electrode with same variable electric field force - Google Patents

Multichannel electrode with same variable electric field force Download PDF

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CN101352669B
CN101352669B CN200710158289XA CN200710158289A CN101352669B CN 101352669 B CN101352669 B CN 101352669B CN 200710158289X A CN200710158289X A CN 200710158289XA CN 200710158289 A CN200710158289 A CN 200710158289A CN 101352669 B CN101352669 B CN 101352669B
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electrode
electric field
channel
low pressure
passage
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CN101352669A (en
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马小军
谢威扬
于炜婷
张家明
朱静
吴伟
王乐群
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Zhangjiagang Institute Of Industrial Technology Dalian Institute Of Chemical Physics China Academy Of Sciences
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Dalian Institute of Chemical Physics of CAS
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Abstract

The invention relates to a multi-channel high-efficiency electrode which can generate same change electric field force simultaneously, comprising a high-volage multi-channel electrode fixed on a support plate of a bracket. The high-voltage multi-channel electrode is of a closed tubular structure, the upper end of which is provided with an air intake and a feed inlet and the bottom of which is a slab shape; the lower part of a slab is provided with 2 or more than 2 metal hollow acerose channels which are electrically connected with the anode end of an external high-voltage pulse power source; the lower end ports of both the metal hollow acerose channels are positioned at a same plane; a low-voltage board electrode is arranged correspondingly below the high-voltage multi-channel electrode, and is of the slab-shaped structure; the low-voltage board electrode corresponding to the lower ends of the metal hollow acerose channels is provided with round holes, the circumferences of which are provided with metal circular rings which are electrically connected with an external high-voltage negative pulse power source; the low-voltage board electrode is connected with the bracket in a sliding way. The multi-channel high-efficiency electrode used in a method of electrostatic atomization can prepare biologic microcapsules with controllable and uniform grain diameters.

Description

A kind of multi-channel electrode with same variable electric field force
Technical field
The present invention relates to a kind of multichannel high-efficient electrode that can produce same variable electric field force simultaneously.But this electrode is used for the bio-microcapsule of the controlled and homogeneous of electrostatic atomization method scale preparation particle diameter.[Proc.R.Soc.A 1964,280:383-397 for document 1.Taylor G I, Disintegration of water drops in an electric field]
Background technology
Microcapsules are micron order size capsule carriers that a kind of utmost point has application prospect, are widely used in the research of biomedicine, organizational project and pharmaceutical fields such as cell cultivation, medicine sustained and controlled release formulation, cellular transplantation therapy, PCI and gene delivery vehicle.Scale preparation uniform particle diameter microcapsules device is the key equipment of large-scale production microcapsule product.
In many preparation methods of microcapsules, the electrostatic atomization method is one of gentle process of preparation microcapsules and bio-microcapsule living body biological product.
But the use of electrostatic atomization method at present is confined to single channel and prepares microcapsules [document 2.UnitedStates Patent 4744933,1988], can't carry out large-scale production.Common way is to connect high voltage pulse, do ground electrode with stainless steel ring or hole sheet with syringe, leaps high in ten thousand deep-sited pulses and depresses controlled, the good biological protomere of monodispersity [document 3. Chinese utility model patents, patent No. ZL 002 53538.6] of preparation particle diameter.
Though existing at present bibliographical information electrostatic atomization method adopts multi-channel electrode can prepare microcapsules [document 4.D.Poncelet, B.Bugarski, B.G.Amsden, J.Zhu, R.Neufeld, M.F.A.Goosen, " A Parallel Plate electrostatic droplet generation:parameters affecting microbead size; " Appl Microbiol Biotechnol (1994) 42:251-255], but be difficult to accomplish that the product grain is through homogeneous.Due to the reason of searching to the bottom, the field intensity phase mutual interference that this kind electrode forms at each interchannel, electric field force inequality.The locus of each passage in any case arrange all can't obtain an equivalent electric field force [document 5. Chinese invention patents, patent No. ZL01120095.2] that changes simultaneously at the Exit to all routes end.
Summary of the invention
At the multichannel high-efficient electrode present situation that still lacks same variable electric field force in the present electrostatic atomization technical process, the present invention has carried out brand-new design on electrode structure.The object of the present invention is to provide a kind of can the scale preparation microcapsules and the multichannel high-efficient electrode of the microcapsules uniform particle diameter of preparation.Can set up the electric field of the minimum and synchronous variation of the mutual interference mutually more than 2 or 2 between each access port place that the present invention is embodied in the high pressure multi-channel electrode and the low pressure plate electrode alone, guarantee the uniformity that the electric field force of each passage changes.In the design, reduced electric field force size influencing each other between arranging with number of poles, electrode plane geometry to greatest extent.
For achieving the above object, the technical solution used in the present invention is:
A kind of multichannel high-efficient electrode with same variable electric field force comprises support, is provided with stent bearing plank in the middle and upper part of support, is fixed with the high pressure multi-channel electrode on the stent bearing plank;
The high pressure multi-channel electrode is the tubular structure of sealing, its upper end is provided with air inlet and charge door, its bottom surface is dismountable annular plate, turning in one's mind one in the ring-type bottom surface of high pressure multi-channel electrode is provided with the multichannel needle plate of the metal hollow needle-like passage more than 2 or 2, and the cavity in the hollow bulb of multichannel needle plate and the tubular structure is communicated with; Metal hollow needle-like passage is electrically connected with extraneous high-voltage pulse power source positive terminal; The lower port of each hollow needle-like passage is in same plane; Its air inlet links to each other with accurate constant voltage source of the gas by wireway;
Be provided with the low pressure plate electrode in high pressure multi-channel electrode below, the low pressure plate electrode is a plate-like structure, and its size and dimension is corresponding with the planar bottom surface of high pressure multi-channel electrode, and the position parallels; The pairing low pressure plate electrode in hollow spicule lower end is provided with circular hole, is provided with and the concentric metal ring of metal hollow needle-like passage around the circular hole, and metal ring is electrically connected with extraneous high pressure negative pulse power supply; Low pressure plate electrode and support are for slidably being connected.
Support is provided with stepper motor.The stepper motor transmission is connected with the low pressure plate electrode, and the low pressure plate electrode can slide up and down along support.
Between described multichannel needle plate and ring-type bottom surface for removably connecting.This multichannel needle plate is an installation, dismantles assembly very easily, according to different preparation demands (as capsule grain diameter scope and productive rate etc.), can adjust the hollow spicule internal diameter and the quantity of needle plate at any time.
The external diameter of metal hollow needle-like passage is controlled between 0.5~2.0 millimeter of the Φ, and rigidity is strong and be difficult for flexural deformation; Hollow spicule internal diameter can satisfy the multiple demand of preparation particle diameter at 100~5000 microns microcapsules between 0.10~0.80 millimeter.
Between high pressure multi-channel electrode and low pressure plate electrode, be provided with electric field near high pressure multi-channel electrode side and strengthen the utmost point, it is a plate-like structure, and parallel with the low pressure plate electrode, electric field strengthens the utmost point and is provided with and the corresponding aperture of metal hollow needle-like passage, and metal hollow needle-like passage is set in the electric field enhancing by aperture and extremely goes up.
The present invention has following advantage:
1. the uniformity that changes of each passage electric field force, the protomere uniform particle diameter of preparation.The hollow needle-like passage of high pressure multi-channel electrode of the present invention and the circular hole on the low pressure plate electrode adopt the concentric structure design, guarantee between multichannel port and low pressure plate electrode, to produce a kind of electric field force of equivalent variations, make the field intensity between each passage disturb the negligible degree that reduces to.It is multi-channel electrode can the scale preparation uniform particle diameter, the basic fundamental of the microcapsules of good dispersion guarantees.
High pressure multi-channel electrode outer shape of the present invention can be just, can justify; Its number of channels, arrangement mode are not subject to how much and are symmetrically distributed.
2. material flow is easy to dismounting through accessory, is easy to high-temperature sterilization.High pressure multi-channel electrode overall structure is the cylindrical container of a sealing, and its lower end is the multichannel needle plate of metal hollow needle-like; And needle plate is an installation, dismantles assembly very easily.According to different preparation demands (as capsule grain diameter scope and productive rate etc.), can adjust the hollow spicule internal diameter and the quantity of needle plate at any time.Insert the positive pole of high-voltage pulse power source and the accurate constant voltage source of the gas of adjustable seamless power during actual the use.
3. the low pressure plate electrode adopts resistant to elevated temperatures nontoxic polymer composite to form through special process processing, processing and fabricating.Use this kind electrode can reduce the encystation magnitude of voltage significantly, relatively its operating voltages such as flush type ground electrode or ring electrode can reduce about 30~60% of encystation voltage; And the fragment that can reduce microcapsules significantly generates.When the preparation bio-microcapsule, this electrode can satisfy demands such as high-temperature sterilization.
4. electric field strengthens the utmost point and adopts dielectric constant big and quick detachable and can satisfy the material making of high-temperature sterilization requirement.Its effect is exactly the field intensity that strengthens each access port zone.
5. the field intensity secondary is controlled, has not only reduced operating voltage but also kept the organism activity.The control step motor is used for fine adjustment high-low pressure electrode spacing, can carry out under the constant situation of external condition that secondary is accurate to be adjusted to field intensity, finally the encystation electric field force that obtains suiting at the place, Exit to all routes.This adjusting device has adopted the stepping regulation technology, can be by the control of on-site manual or computer remote, and its electrode spacing control accuracy can reach ± and 0.005 millimeter.Electrode resets and the position adjustment, can on-site manual or computer remote control.
6. can change the passage number and the aperture of multichannel needle plate arbitrarily, its processing and fabricating can be realized series specification.As the metal hollow needle-like passage of high pressure multi-channel electrode, its external diameter is unified between 0.5~2.0 millimeter of the Φ, and rigidity is strong and be difficult for flexural deformation; Hollow spicule internal diameter can satisfy the multiple demand of preparation particle diameter at 100~5000 microns microcapsules between 0.10~0.80 millimeter.
7. Precision Machining such as numerical control machining center positions, cuts, boring are adopted in the making of electrode of the present invention; Ultrasonic wave boundling processing method is adopted in the inside and outside surface grinding of each metal hollow needle-like passage, and the processing of needle plate is manufactured error is controlled within the reasonable range; The inner surface of hollow needle-like passage adopts and is coated with membrane treatment process, reduces the surface tension in the passage to greatest extent.
The high efficiency of the accuracy on this electrode structure, use determined that it has can be continuously, the practicality of stable operation.
In a word, the present invention regulates the size of electric field force by relative position secondary between the adjusting electrode, thereby reduces operating voltage significantly, satisfies biotechnology industries such as pharmaceutical preparation, food, feed and prepares the active demand of microcapsule product; This electrode can change the number and the aperture of passage arbitrarily, and accessory is dismantled easily, and material flow can make things convenient for high-temperature sterilization through part; After the transformation, can be used for the spray-drying parts and prepare functional powder.
Electrode design of the present invention use to confirm through reality: the size of electric field force and number of poles and the plane location independent of arranging.But continous-stable operation in the process of the biological protomere of electrostatic atomization method scale preparation therefore can more extensive according to demand amplification.
Description of drawings
Fig. 1 is the multichannel high-efficient electrode structural representation; Wherein, 1 stepper motor, 2 air inlets, 3 charging apertures, 4 stent bearing planks, 5 high pressure multi-channel electrode, 6 electric fields strengthen the utmost point, 7 metal hollow needle-like passages, 8 low pressure plate electrodes, 9 gel liquid baths, 10 supports;
Fig. 2 is the observations of embodiment 1 protomere D750 μ m 40 power microscope forms;
Fig. 3 is the observations of embodiment 2 protomere D295 μ m 40 power microscope forms;
Fig. 4 is embodiment 1 protomere particle size distribution measuring result;
Fig. 5 is embodiment 2 protomere particle size distribution measuring results;
Fig. 6-1 prepares the observation of protomere 40 power microscope forms for embodiment 3 buried electrodes;
Fig. 6-2 is embodiment 3 electrode preparation protomere 40 power microscope forms observations of the present invention.
The specific embodiment
A kind of multichannel high-efficient electrode with same variable electric field force,
Comprise support 10, be provided with stent bearing plank 4, be fixed with high pressure multi-channel electrode 5 on the stent bearing plank 4 in the middle and upper part of support 10;
High pressure multi-channel electrode 5 is the tubular structure of sealing, its upper end is provided with air inlet 2 and charge door 3, its bottom surface is dismountable annular plate, turning in one's mind one in the ring-type bottom surface of high pressure multi-channel electrode 5 is provided with the multichannel needle plate of the metal hollow needle-like passage more than 2 or 2, and the cavity in the hollow bulb of multichannel needle plate and the tubular structure is communicated with; Metal hollow needle-like passage 7 is electrically connected with extraneous high-voltage pulse power source positive terminal; The lower port of each hollow needle-like passage is in same plane; Its air inlet 2 links to each other with accurate constant voltage source of the gas by wireway;
Be provided with low pressure plate electrode 8 in high pressure multi-channel electrode 5 belows; Low pressure plate electrode 8 is a plate-like structure, and material of main part is made of epoxy resin or polyflon, and its size and dimension is corresponding with the planar bottom surface of high pressure multi-channel electrode, and the position parallels; The low pressure plate electrode is electrically connected with extraneous high-voltage pulse power source positive terminal; The pairing low pressure plate electrode in hollow needle-like passage lower end is provided with circular hole, is provided with metal ring around the circular hole, and metal ring is electrically connected with extraneous high-voltage pulse power source negative pole end; Low pressure plate electrode 8 and support 10 are for slidably being connected.
Support 10 is provided with stepper motor 1, and low pressure plate electrode 8 is in transmission connection with stepper motor 1, and low pressure plate electrode 8 can slide up and down along support 10.
The external diameter of metal hollow needle-like passage 7 is controlled between 0.5~2.0 millimeter of the Φ, and rigidity is strong and be difficult for flexural deformation; Hollow spicule internal diameter can satisfy the multiple demand of preparation particle diameter at 100~5000 microns microcapsules between 0.10~0.80 millimeter.
Between high pressure multi-channel electrode 5 and low pressure plate electrode 8, be provided with electric field near high pressure multi-channel electrode 5 sides and strengthen the utmost point 6, it parallels for plate-like structure and with the low pressure plate electrode, electric field strengthens the utmost point and is provided with and the corresponding aperture of metal hollow needle-like passage, and metal hollow needle-like passage is set in the electric field enhancing by aperture and extremely goes up.
What present embodiment 1. and embodiment 2. adopted is 19 channel electrodes, and embodiment 3. is seven channel electrodes.
The high-voltage pulse power source that present embodiment uses is conventional microcapsules preparing instrument.
The sodium alginate soln that concentration is certain imports in the high pressure multi-channel electrode after impurity elimination etc. is handled after filtration.Open preparation system switch and intake valve, under the effect of high-voltage electrostatic field, sodium alginate soln forms the awl jet by the orifice of high pressure multi-channel electrode, splashes into and is solidified into the calcium alginate micro gel bead in the coagulation bath.
Embodiment 1
1. sodium alginate is dispersed in and forms 1.5% (w/v) sodium alginate material liquid in 0.9% physiological saline; 1.11% (w/v) CaCl 2Solution is coagulation bath.
2. under the situation of high-voltage pulse+Upp=5.0kV, frequency f=110Hz, pulsewidth 4ms, threshold voltage U=1000V, the sodium alginate material liquid flows out from internal diameter is the orifice of 19 passages of Φ 0.4mm under the pressure of 0.075MPa, falling into coagulation bath solidifies, forming particle diameter is the calcium alginate micro gel bead of 750 μ m, and output is 2000ml/h.
3. prepared micro gel bead is observed spherical attitude (as Fig. 2) through the Japanese biological inverted microscope CK40 of Olympus company type.
4. adopt the U.S. LS-100 Q of Beckman-Coulter company type laser particle analyzer to measure the particle diameter and the particle diameter distribution (as Fig. 4) of composite macromolecule microsphere.
5. measure the micro gel bead volume of collecting within a certain period of time, calculate output.
Embodiment 2
1. sodium alginate is dispersed in and forms 1.0% (w/v) sodium alginate material liquid in 0.9% physiological saline; 1.11% (w/v) CaCl 2Solution is coagulation bath.
2. at high-voltage pulse Upp=6.8kV, frequency f=140Hz, pulsewidth 5ms, under the situation of threshold voltage U=0V, the sodium alginate material liquid flows out from internal diameter is the orifice of 19 passages of Φ 0.17mm under the pressure of 0.085MPa, falling into coagulation bath solidifies, forming particle diameter is the calcium alginate micro gel bead of 300 μ m,, output is 400ml/h.
3. same with embodiment 1, the results are shown in Figure 3.
4. same with embodiment 1, the results are shown in Figure 5.
5. same with embodiment 1.
Embodiment 3
In the existing document is ground electrode with the formed buried electrode of the becket that places coagulation bath all, with the experiment of comparing of this buried electrode and this electrode:
1. sodium alginate is dispersed in and forms 1.5% (w/v) sodium alginate material liquid in 0.9% physiological saline; 1.11% (w/v) CaCl 2Solution is coagulation bath.
2. parameter comparison:
Electrode form Pulse voltage (kv) Pulse frequency (Hz) Pulse width (ms) Threshold voltage (v) Gas force (MPa) Micro gel bead particle diameter (μ m)
Buried electrode 7.25? 160? 4? 0? 0.02? 400~500?
This electrode 2.75? 100? 4? 0? 0.02? 500?
3. prepared micro gel bead is observed spherical attitude through the Japanese biological inverted microscope CK40 of Olympus company type and is seen Fig. 6 for details.Use this electrode to reduce in pulse voltage at 62% o'clock, the microcapsules form of generation is more excellent.

Claims (5)

1. multi-channel electrode with same variable electric field force is characterized in that:
Comprise support (10), be provided with stent bearing plank (4), be fixed with high pressure multi-channel electrode (5) on the stent bearing plank (4) in the middle and upper part of support (10);
High pressure multi-channel electrode (5) is the tubular structure of sealing, its upper end is provided with air inlet (2) and charge door (3), its bottom surface is dismountable annular plate, be provided with the multichannel needle plate of the metal hollow needle-like passage more than 2 or 2 one of the ring-type bottom surface of high pressure multi-channel electrode (5) liner, the hollow bulb of multichannel needle plate is communicated with cavity in the tubular structure; Metal hollow needle-like passage (7) is electrically connected with extraneous high-voltage pulse power source positive terminal; The lower port of each hollow needle-like passage is in same plane; Its air inlet (2) links to each other with accurate constant voltage source of the gas by wireway;
Be provided with low pressure plate electrode (8) in high pressure multi-channel electrode (5) below;
Low pressure plate electrode (8) is a plate-like structure, and material of main part is made of epoxy resin or polyflon, and its size and dimension is corresponding with the planar bottom surface of high pressure multi-channel electrode, and the position parallels; The low pressure plate electrode is electrically connected with extraneous high-voltage pulse power source positive terminal; The pairing low pressure plate electrode in hollow needle-like passage lower end is provided with circular hole, is provided with metal ring around the circular hole, and metal ring is electrically connected with extraneous high-voltage pulse power source negative pole end; Low pressure plate electrode (8) and support (10) are for slidably being connected.
2. according to the described multi-channel electrode of claim 1 with same variable electric field force, it is characterized in that: support (10) is provided with stepper motor (1), low pressure plate electrode (8) is in transmission connection with stepper motor (1), and low pressure plate electrode (8) can slide up and down along support (10).
3. according to the described multi-channel electrode of claim 1 with same variable electric field force, it is characterized in that: between described multichannel needle plate and ring-type bottom surface for removably connecting, this multichannel needle plate is an installation, dismantles assembly very easily, according to different preparation demands, can adjust the hollow spicule internal diameter and the quantity of needle plate at any time.
4. according to the described multi-channel electrode with same variable electric field force of claim 1, it is characterized in that: the external diameter of metal hollow needle-like passage (7) is controlled between 0.5~2.0 millimeter of the Φ, and rigidity is strong and be difficult for flexural deformation; Hollow spicule internal diameter can satisfy the multiple demand of preparation particle diameter at 100~5000 microns microcapsules between 0.10~0.80 millimeter.
5. according to the described multi-channel electrode of claim 1 with same variable electric field force, it is characterized in that: between high pressure multi-channel electrode (5) and low pressure plate electrode (8), be provided with electric field near high pressure multi-channel electrode (5) side and strengthen the utmost point (6), it parallels for plate-like structure and with the low pressure plate electrode, electric field strengthens the utmost point and is provided with and the corresponding aperture of metal hollow needle-like passage, and metal hollow needle-like passage is set in the electric field enhancing by aperture and extremely goes up.
CN200710158289XA 2007-11-14 2007-11-14 Multichannel electrode with same variable electric field force Active CN101352669B (en)

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CN1395987A (en) * 2001-07-13 2003-02-12 中国科学院大连化学物理研究所 System for preparing gel beads

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US4744933A (en) * 1984-02-15 1988-05-17 Massachusetts Institute Of Technology Process for encapsulation and encapsulated active material system
CN1395987A (en) * 2001-07-13 2003-02-12 中国科学院大连化学物理研究所 System for preparing gel beads

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