CN105498656A - Preparing device of shell-core functional material - Google Patents
Preparing device of shell-core functional material Download PDFInfo
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- CN105498656A CN105498656A CN201511009230.5A CN201511009230A CN105498656A CN 105498656 A CN105498656 A CN 105498656A CN 201511009230 A CN201511009230 A CN 201511009230A CN 105498656 A CN105498656 A CN 105498656A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00851—Additional features
- B01J2219/00871—Modular assembly
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/0095—Control aspects
- B01J2219/00984—Residence time
Abstract
The invention discloses a preparing device of a shell-core functional material, which comprises a microfluidics integrated chip, a microfluidics drive device and a shell-core functional material collector; the microfluidics integrated chip comprises an outer phase input passage, a middle phase input passage, an inner phase input passage, a double emulsion generating micro structure, and a functional material output passage, and further comprises a bionic splitting array, a dielectrophoresis tuning micro unit, a liquid membrane curing micro unit, a microsphere external surface functionalized micro unit and a functional filler loading and homogenizing micro unit, which are arranged between the double emulsion generating micro structure and the functional material output passage. The preparing device can fully use the space of the microfluidics integrated chip, enables the chip to be compactly and reasonably configured and realizes the aim of fast and efficiently preparing the high quality shell-core functional material, thus greatly improving the preparing efficiency of the functional material under the conditions of ensuring degree of sphericity, concentricity and size uniformity of double emulsion, and realizing scaled and continuous production with excellent controllability.
Description
Technical field
The present invention relates to a kind of device adopting microfluidic methods to prepare shell kernel function material, belong to double-deck emulsion preparing technical field.
Background technology
Double emulsion is the nested structure heterogeneous system that the outer drop of a kind of decentralized photo is wrapped in less interior drop, the shell core micro-structural of this uniqueness of double emulsion can isolate interior drop and contact continuously, effectively so be widely used in the preparation of the functional materials such as microstorage, microreactor, tiny segregator and microstructure unit.The preparation method of at present conventional double emulsion also exists the problems such as the low and waste of raw materials of complex process, efficiency is serious usually, and owing to lacking effective regulation and control to each phase fluid in process, cause that obtained double emulsion sphericity is not high, concentricization degree is poor, thus cause double emulsion to solidify the functional modification difficulty of microsphere surface generated to strengthen further, this is the extreme influence preparation efficiency of functionalization material all.For this reason, in the urgent need to improving and optimizating the art methods preparing shell kernel function material based on double emulsion, the novel processing step of development high-quality shell kernel function material, thus improve the preparation efficiency of functional material.
Summary of the invention
Technical problem to be solved by this invention be above-mentioned existing prepare shell kernel function materials process dispersion, production efficiency is low and double emulsion yields poorly, ropy shortcoming; and significantly improve the preparation efficiency of functional material under providing a kind of condition ensureing double emulsion sphericity, concentricity and dimensional homogeneity, achieve possess excellent controllability scale, continuous prodution.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of preparation facilities of shell kernel function material, comprise micro-fluidic integrated chip, microfluid drive and shell kernel function material collector, described microfluid drive comprises external fluid phase syringe pump and syringe, mesophase spherule fluid injecting pump and syringe, internal phase fluid syringe pump and syringe, described micro-fluidic integrated chip comprises foreign minister's input channel, mesophase spherule input channel, interior phase input channel, double emulsion generates micro-structural and functional material output channel, foreign minister's syringe is connected in described foreign minister's input channel, mesophase spherule syringe is connected in described mesophase spherule input channel, phase syringe in described interior phase input channel connects, shell kernel function material collector described in connecting in the exit of described functional material output channel, it is characterized in that: described micro-fluidic integrated chip also comprises the bionical division array between described double emulsion generation micro-structural and functional material output channel, dielectrophoresis aligning micro unit, liquid film solidification micro unit, microballoon outer surface functionalization micro unit and functional stuffing load and homogenizing micro unit, described double emulsion generates micro-structural, bionical division array, dielectrophoresis aligning micro unit, liquid film solidification micro unit, microballoon outer surface functionalization micro unit is loaded with functional stuffing and is connected successively by transfer passages with homogenizing micro unit, described bionical division array comprises main channel, at least two-stage level separation lanes and converging channel, described level separation lanes is biomimetic features microchannel, described converging channel is funnel-shaped structure, described dielectrophoresis aligning micro unit comprises many groups aligning electrode arranged side by side and catches, release electrode.
Described level separation lanes is square-section, every grade of level separation lanes is division number is 2, each separation lanes comprises access ramp and is connected to the parallel channels of access ramp rear end, described parallel channels is parallel with main channel, angle between described two inclined tubes is 60 degree, n-th grade of level separation lanes is consistent with the height of the 0th grade of level separation lanes, and the pass of width is D
n/ D
0=2
-n/p, wherein, p > 1; The pass of n-th grade of level separation lanes and the 0th grade of level separation lanes length is L
n/ L
0=2
-n/q, wherein 1<q<2.
The female double emulsion of described level separation lanes homolysis is to target sizes, and multiplication produces of the same size pair of emulsion, and described converging channel is funnel-shaped structure, for collecting the target double emulsion after division.The production efficiency of the two emulsion of the target that raising size is homogeneous, monodispersity is good that described bionical division array can double.
Described dielectrophoresis aligning micro unit also comprises a gripper shoe, and described gripper shoe surface uniform coating layer of conductive film is as dielectric layer, and described aligning electrode adopts high frequency inhomogeneous field, puts conductive filament electrode, underlying parallel-plate electrode forms from above; Described release electrode adopts uniform electric field, and be made up of preposition parallel-plate electrode, rearmounted parallel-plate electrode, described preposition parallel-plate electrode and described rearmounted parallel-plate electrode control opening and closing by micro motor.
Aligning electrode structure described in each group is caught, discharge electrode structure all adopts independent output to control, and is controlled, realize independent aligning by described controller.
Described liquid film solidification micro unit comprises exchange of solvent microchannel, dry microchannel, cooling microchannel, high temperature micro-electric hot plate and organizes miniature valve more, and described high temperature micro-electric hot plate is arranged in described bottom, dry microchannel.
Described exchange of solvent microchannel is snakelike densely covered arrangement, and described dry microchannel and described cooling microchannel are the densely covered arrangement of meander, make full use of micro-fluidic chip space, increase exchange of solvent and liquid film drying time.Described high temperature micro-electric hot plate is arranged in described bottom, dry microchannel, accelerates liquid film drying.Described miniature valve is connected with described controller, and described controller exports corresponding signal, the opening and closing under electric current drives of micro-valve, and effective connection or isolation microchannel, control the reaction time.After described liquid film solidification micro-structural, concentricity and the high double emulsion of sphericity solidify to form shell core microballoon.
Described microballoon outer surface functionalization micro unit comprises microballoon outer surface functionalization microchannel and organizes miniature valve more, described microballoon outer surface functionalization microchannel is snakelike densely covered arrangement and is isolated into multiple individual passage by described miniature valve, fills cleaning agent and initiator solution respectively in different channels.
Shell core microballoon respectively with cleaning agent, initiator for reaction after, finally at microballoon outer surface one deck functional material initator, induction microballoon functionalization characteristic.The microballoon reaction time is in the channel controlled by miniature valve.
Described functional stuffing loads and homogenizing micro unit comprises functional stuffing loading microchannel and functional stuffing homogenizing microchannel, constant temperature micro-electric hot plate and organizes miniature valve more, it is the densely covered arrangement of meander that described functional stuffing loads microchannel and functional stuffing homogenizing microchannel, described thermostatic electrothermal plate is arranged in described bottom, functional stuffing homogenizing microchannel, and described functional stuffing loads in microchannel functional stuffing; Described miniature valve controls the shell core microballoon reaction time.
Functionalized microsphere is the abundant haptoreaction with functional stuffing in the channel, value-added tax function filler, then to load in microchannel by described constant temperature micro-electric hot plate thermal induction functional material characteristic and the functional material on the surface made is uniformly distributed in dry run gradually at described functional stuffing.
It is typical diesis shape microchannel that described double emulsion generates micro-structural, and directly processing is on the micro-fluidic integrated chip of described digitlization.Described miniature valve all controls opening and closing separately by the control circuit in described controller, the micro-fluidic integrated chip of described digitlization is according to the difference such as condition of work, fluid properties, size can control at about several square centimeters, material can select silicon chip, glass, silicon rubber, plastic or other material as substrate, by method processing microchannels such as etching, photoetching or dies.
When described microfluid drive runs, the double emulsion of larger volume generates in micro-structural at described double emulsion and generates, and along with fluid flowing, enter described bionical division array, single large volume double emulsion is just split into 4,8 ... .2
nindividual homogeneity is good, the double emulsion that quality is high.Enter described dielectrophoresis aligning micro unit subsequently, by inhomogeneous field aligning, obtain good sphericity, the double emulsion that concentricity is high, simultaneously because the joule heating effect of electrophoresis accelerates double emulsion gelation, become gelation macromolecular structure.Subsequently in described liquid film solidification micro unit, first in described exchange of solvent microchannel, carry out exchange of solvent, then rapid draing in described dry microchannel, and then become solid-state-microspherical by described cooling microchannel.Pass through transfer passages, solid-state-microspherical is transported to described microballoon outer surface functionalization micro unit and carries out outer surface functionalization, finally load at described functional stuffing and continue optimizing surface material structure in homogenizing micro unit, finally enter described shell kernel function material collector from the functional material output channel described in end, obtain high-quality shell kernel function material.
Beneficial effect:
A kind of device preparing high-quality shell kernel function material that the present invention relates to, make full use of the advantage of digitlization microflow control technique, double emulsion is generated micro-structural, bionical division array, dielectrophoresis aligning micro unit, liquid film solidification micro unit, microballoon outer surface functionalization micro unit and functional stuffing load and homogenizing micro unit is integrated on a micro-fluidic chip, double emulsion disintegrating method is utilized to prepare the good double emulsion of homogeneity fast, use the sphericity of the two emulsion of high frequency inhomogeneous field regulation and control and concentricity to accelerate emulsion gel simultaneously, and realize liquid film solidification efficiently, microsphere surface functionalization material loads and homogenizing, achieve the quick preparation of high-quality shell kernel function material.In addition, owing to introducing the feature structure of bionical division array in division array, the double emulsion that the generation quantity that can efficiently double is many, homogeneity good, monodispersity is good, utilizes dielectrophoresis technology to assist the quick-gelatinizing of double emulsion.These factors above, not only make full use of the space of micro-fluidic chip, make chip structure compact in design reasonable, also achieve fast, efficiently prepare the object of high-quality shell kernel function material.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Fig. 2 is the micro-fluidic integrated chip schematic diagram of the present invention.
Fig. 3 is the present invention's bionical division array schematic diagram.
Fig. 4 is aligning electrode of the present invention and catches, discharges electrode schematic diagram.
1. external fluid phase syringe pump and syringes in figure; 2. mesophase spherule fluid injecting pump and syringe; 3. internal phase fluid syringe pump and syringe; 4. foreign minister's input channel; 5. mesophase spherule input channel; 6. in phase input channel and; 7. the micro-fluidic integrated chip of digitlization; 8. functional material output channel; 9. shell kernel function material collector; 10. controller; 11. double emulsions generate micro-structural; 12. bionical division arrays; 13. dielectrophoresis aligning micro units; 14. exchange of solvent microchannels; 15. dry microchannels; 16. cooling microchannels; 17. high temperature micro-electric hot plates; 18. microballoon outer surface functionalization micro units; 19. functional stuffings load microchannel; 20. functional material homogenizing microchannels; 21 constant temperature micro-electric hot plates; 22. miniature valves; 23. main channels; 24. level separation lanes; 25. converging channels; 26. preposition parallel-plate electrodes; Conductive filament electrode is put on 27.; 28. underlying parallel-plate electrodes; 29. rearmounted parallel-plate electrodes; 30. gripper shoes.
Detailed description of the invention
Further describe in detail below in conjunction with accompanying drawing:
Fig. 1 gives system diagram of the present invention, the existing device of preparation of high-quality shell kernel function material, concrete structure comprises the chief component such as external fluid phase syringe pump and syringe 1, mesophase spherule fluid injecting pump and syringe 2, internal phase fluid syringe pump and syringe 3, foreign minister's input channel 4, mesophase spherule input channel 5, interior phase input channel 6, the micro-fluidic integrated chip 7 of digitlization, functional material output channel 8, shell kernel function material collector 9, controller 10.External fluid phase, mesophase spherule fluid, interior to fluid respectively at external fluid phase syringe pump and syringe 1, mesophase spherule fluid injecting pump and syringe 2, internal phase fluid syringe pump and syringe 3 drive lower inflow in the micro-fluidic integrated chip 7 of digitlization to form double emulsion, and through division in the micro-fluidic integrated chip 7 of digitlization, concentric regulation and control and quick-gelatinizing, liquid film solidification and functional material loading procedure, finally from functional material output channel 8, flow into shell kernel function material collector 9, wherein, controller 10 is by exporting the multiple micromodule equipment in the different micro-fluidic integrated chips of signal digital control 7.
Fig. 2 gives digitlization micro-fluidic integrated chip schematic diagram, and concrete structure comprises foreign minister's input channel 4 in figure, mesophase spherule input channel 5, interior phase input channel 6, functional material output channel 8, double emulsion generation micro-structural 11, bionical division array 12, dielectrophoresis aligning micro unit 13, exchange of solvent microchannel 14, dry microchannel 15, cooling microchannel 16, high temperature micro-electric hot plate 17, microballoon outer surface functionalization micro unit 18, functional stuffing loads microchannel 19, functional material homogenizing microchannel 20, constant temperature micro-electric hot plate 21, miniature valve 22, Deng chief component, from foreign minister's input channel 4, mesophase spherule input channel 5, the fluid in Digital microfluidic chips is flow in interior phase input channel 6, generate in micro-structural 11 at double emulsion, due to the shearing force of fluid and the effect of fluid interfacial surface tension, generate the two emulsion of large volume, bionical division array 12 is flowed into subsequently with flowing, thus to achieve a double emulsion homolysis be two, four, eight ... double emulsion after division is entering in dielectrophoresis aligning micro unit 13, achieve two emulsion aligning, and have adjusted sphericity, simultaneously under electrophoretic action, accelerate gel.After gel, double emulsion just becomes gel macromolecule double emulsion, fast solvent exchange is carried out subsequently in exchange of solvent microchannel 14, swap time is controlled by 4 groups of miniature valves 22, double emulsion shell becomes plastic macromolecule film, in dry microchannel 15, because the high temperature micro-electric hot plate 17 bottom dry microchannel 15 heats, rapid drying, then cooling in cooling microchannel 16 is entered, so just obtain flexible polymer films microballoon, achieve the flash cure process of double emulsion, the reaction time in solidification is controlled by miniature valve 22.Then flexible polymer films microballoon is inserted in microballoon outer surface functionalization micro unit 18, in microballoon outer surface functionalization micro unit 18, microballoon is reacted with cleaning agent, initator in the channel successively, the reaction time is controlled by miniature valve 22, final at microballoon outer surface one deck functional material initator, induction microballoon functionalization characteristic.The functionalized microsphere abundant haptoreaction of functional stuffing in functional stuffing loading microchannel 19 and wherein subsequently, carry out value-added tax function filler, then entered function filler homogenizing microchannel 20, by the constant temperature micro-electric hot plate 21 of bottom, by thermal induction functional material characteristic and the functional material on the surface made be uniformly distributed in dry run gradually, wherein the reaction time of passage is controlled by miniature valve 22, at this point, obtains high-quality shell kernel function material in the micro-fluidic integrated chip of digitlization continuously.
Fig. 3 gives bionical division array schematic diagram, concrete structure comprises the chief components such as main channel 23, level separation lanes 24, converging channel 25, level separation lanes 24 is flowed into after two emulsion generates in main channel 23, split into two, four, eight, 16 successively uniformly ... individual uniform double emulsion, finally converges in converging channel 25.So just obtain the double emulsion uniform, monodispersity is good.
Fig. 4 gives aligning electrode and catches, discharges electrode structure schematic diagram, concrete structure comprise preposition parallel-plate electrode 26, on put the chief components such as conductive filament electrode 27, underlying parallel-plate electrode 28, rearmounted parallel-plate electrode 29, gripper shoe 30, wherein gripper shoe 30 need coating layer of conductive film as dielectric layer.When the target double emulsion of some enters into aligning structure, passage is opened by preposition parallel-plate electrode 26, and rearmounted parallel-plate electrode 29 conducts electricity, target acquisition double emulsion.Then by preposition parallel-plate electrode 26 closing passage, put conductive filament electrode 27 subsequently, underlying parallel-plate electrode 28 conducts electricity, carry out two emulsion aligning, obtain good sphericity, after the double emulsion that concentricity is high, rearmounted parallel-plate electrode 29 opens passage, and preposition parallel-plate electrode 26 conducts electricity, release target double emulsion.So just obtain good sphericity, double emulsion that concentricity is high.
Claims (7)
1. the preparation facilities of a shell kernel function material, comprise micro-fluidic integrated chip, microfluid drive and shell kernel function material collector, described microfluid drive comprises external fluid phase syringe pump and syringe, mesophase spherule fluid injecting pump and syringe, internal phase fluid syringe pump and syringe, described micro-fluidic integrated chip comprises foreign minister's input channel, mesophase spherule input channel, interior phase input channel, double emulsion generates micro-structural and functional material output channel, foreign minister's syringe is connected in described foreign minister's input channel, mesophase spherule syringe is connected in described mesophase spherule input channel, phase syringe in described interior phase input channel connects, shell kernel function material collector described in connecting in the exit of described functional material output channel, it is characterized in that: described micro-fluidic integrated chip also comprises the bionical division array between described double emulsion generation micro-structural and functional material output channel, dielectrophoresis aligning micro unit, liquid film solidification micro unit, microballoon outer surface functionalization micro unit and functional stuffing load and homogenizing micro unit, described double emulsion generates micro-structural, bionical division array, dielectrophoresis aligning micro unit, liquid film solidification micro unit, microballoon outer surface functionalization micro unit is loaded with functional stuffing and is connected successively by transfer passages with homogenizing micro unit, described bionical division array comprises main channel, at least two-stage level separation lanes and converging channel, described level separation lanes is biomimetic features microchannel, described converging channel is funnel-shaped structure, described dielectrophoresis aligning micro unit comprises many groups aligning electrode arranged side by side and catches, release electrode.
2. preparation facilities according to claim 1, it is characterized in that: described level separation lanes is square-section, every grade of level separation lanes is division number is 2, each separation lanes comprises access ramp and is connected to the parallel channels of access ramp rear end, described parallel channels is parallel with main channel, angle between described two inclined tubes is 60 degree, and n-th grade of level separation lanes is consistent with the height of the 0th grade of level separation lanes, and the pass of width is D
n/ D
0=2
-n/p, wherein, p > 1; The pass of n-th grade of level separation lanes and the 0th grade of level separation lanes length is L
n/ L
0=2
-n/q, wherein 1<q<2.
3. preparation facilities according to claim 1, it is characterized in that: described dielectrophoresis aligning micro unit also comprises a gripper shoe, described gripper shoe surface uniform coating layer of conductive film is as dielectric layer, described aligning electrode adopts high frequency inhomogeneous field, puts conductive filament electrode, underlying parallel-plate electrode forms from above; Described release electrode adopts uniform electric field, and be made up of preposition parallel-plate electrode, rearmounted parallel-plate electrode, described preposition parallel-plate electrode and described rearmounted parallel-plate electrode control opening and closing by micro motor.
4. preparation facilities according to claim 1, it is characterized in that: described liquid film solidification micro unit comprises exchange of solvent microchannel, dry microchannel, cooling microchannel, high temperature micro-electric hot plate and organizes miniature valve more, and described high temperature micro-electric hot plate is arranged in described bottom, dry microchannel.
5. preparation facilities according to claim 4, is characterized in that: described exchange of solvent microchannel is snakelike densely covered arrangement, and described dry microchannel and described cooling microchannel are the densely covered arrangement of meander.
6. preparation facilities according to claim 1, it is characterized in that: described microballoon outer surface functionalization micro unit comprises microballoon outer surface functionalization microchannel and organizes miniature valve more, described microballoon outer surface functionalization microchannel is snakelike densely covered arrangement and is isolated into multiple individual passage by described miniature valve, fills cleaning agent and initiator solution respectively in different channels.
7. preparation facilities according to claim 1, it is characterized in that: described functional stuffing loads and homogenizing micro unit comprises functional stuffing loading microchannel and functional stuffing homogenizing microchannel, constant temperature micro-electric hot plate and organizes miniature valve more, it is the densely covered arrangement of meander that described functional stuffing loads microchannel and functional stuffing homogenizing microchannel, described thermostatic electrothermal plate is arranged in described bottom, functional stuffing homogenizing microchannel, and described functional stuffing loads in microchannel functional stuffing; Described miniature valve controls the shell core microballoon reaction time.
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| CN106311367A (en) * | 2016-09-29 | 2017-01-11 | 东南大学 | Firm-core-containing duplex-emulsion preparation micro fluid control device and preparation method thereof |
| CN106492716A (en) * | 2016-12-20 | 2017-03-15 | 中国工程物理研究院激光聚变研究中心 | Integral dual milk particle generating meanss and its processing method |
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