CN105498656B - Preparing device of shell-core functional material - Google Patents
Preparing device of shell-core functional material Download PDFInfo
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- CN105498656B CN105498656B CN201511009230.5A CN201511009230A CN105498656B CN 105498656 B CN105498656 B CN 105498656B CN 201511009230 A CN201511009230 A CN 201511009230A CN 105498656 B CN105498656 B CN 105498656B
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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
-
- 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 employing microfluidic methods prepare the device of shell kernel function material, belong to double-deck emulsion and prepare skill
Art field.
Background technology
Double emulsion is the nested structure heterogeneous system that a kind of outer drop of dispersion phase is wrapped in less interior drop, double emulsion
This unique shell core micro structure can be effectively isolated the contact with continuously of interior drop, so be widely used in micro-
In the preparation of the functional materials such as memorizer, microreactor, tiny segregator and microstructure unit.The system of the double emulsion commonly used at present
Preparation Method generally has that complex process, efficiency be low and waste of raw materials, and to each phase stream due to during
Body lacks effectively regulation and control, causes that obtained double emulsion sphericity is high, concentricization degree is poor, so as to cause double emulsion
The functional modification difficulty of the microsphere surface that solidification is generated further is increased, and this all significantly impacts the preparation effect of functionalization material
Rate.For this purpose, in the urgent need to the art methods to preparing shell kernel function material based on double emulsion are improved optimization, developing
The novel processing step of high-quality shell kernel function material, so as to improve the preparation efficiency of functional material.
The content of the invention
The technical problem to be solved be it is above-mentioned it is existing prepare shell kernel function materials process dispersion, low production efficiency
And double emulsion yield poorly, ropy shortcoming, and provide and a kind of ensureing that double emulsion sphericity, concentricity and size are equal
The preparation efficiency of functional material is greatly improved under conditions of one property, scale, the continuous metaplasia for possessing excellent controllability is realized
Produce.
To solve above-mentioned technical problem, the technical solution used in the present invention is:
A kind of preparation facilitiess of shell kernel function material, including micro-fluidic integrated chip, microfluid drive and shell core
Functional material catcher, described microfluid drive includes external fluid phase syringe pump and syringe, middle phase fluid injection
Pump and syringe, internal phase fluid syringe pump and syringe, described micro-fluidic integrated chip includes foreign minister's input channel, mesophase
Input channel, interior phase input channel, double emulsion generate micro structure and functional material output channel, are input in described foreign minister
Passage connects foreign minister's syringe, in described mesophase input channel connection mesophase syringe, described interior phase input channel
Phase syringe in connection, in the described shell kernel function material collector of the exit connection of described functional material output channel,
It is characterized in that:Described micro-fluidic integrated chip also includes that being located at the double emulsion generates micro structure and functional material output
Bionical division array, dielectrophoresises regulation of mental activities micro unit, liquid film solidification micro unit between passage, the micro- list of microsphere outer surface functionalization
Unit and functional stuffing loading and homogenizing micro unit, the double emulsion generates micro structure, bionical division array, dielectrophoresises regulation of mental activities
Micro unit, liquid film solidification micro unit, microsphere outer surface functionalization micro unit and functional stuffing loading and homogenizing micro unit are by defeated
Wan access is sequentially connected, and described bionical division array includes main channel, at least two-stage level separation lanes and converging channel, institute
The level separation lanes stated are biomimetic features microchannel, and described converging channel is funnel-shaped structure, and described dielectrophoresises are adjusted
Heart micro unit includes multigroup regulation of mental activities electrode arranged side by side and capture, release electrode.
The level separation lanes are square-section, and every grade of level separation lanes are that division number is 2, each separation lanes bag
Include access ramp and be connected to the parallel channels of access ramp rear end, the parallel channels are parallel with main channel, between two inclined tube
Angle be 60 degree, n-th grade of level separation lanes is highly consistent with the 0th grade of level separation lanes, and the relation of width is Dn/D0
=2-n/p, wherein, p > 1;N-th grade of level separation lanes is L with the relation of the 0th grade of level separation lanes lengthn/L0=2-n/q,
Wherein 1<q<2.
To target sizes, multiplication produces of the same size double newborn described level separation lanes homolysis mother's double emulsion
Liquid, described converging channel is funnel-shaped structure, for collecting the target double emulsion after dividing.Described bionical division array
The production efficiency of the double emulsions of the target that raising size is homogeneous, monodispersity is good that can double.
Described dielectrophoresises regulation of mental activities micro unit also includes a gripper shoe, and described support plate surface uniformly lead by one layer of coating
Conductive film adopts high frequency inhomogeneous field, conductive filament electrode, underlying parallel-plate is put from above as dielectric layer, described regulation of mental activities electrode
Electrode is constituted;Described release electrode adopts uniform electric field, is made up of preposition parallel-plate electrode, rearmounted parallel-plate electrode, described
Preposition parallel-plate electrode and described rearmounted parallel-plate electrode by micro motor control be opened and closed.
The capture of regulation of mental activities electrode structure, release electrode structure described in each group adopts single output control, by described
Controller is controlled, and realizes independent regulation of mental activities.
Described liquid film solidification micro unit includes solvent exchange microchannel, is dried microchannel, cooling microchannel, the micro- electricity of high temperature
Hot plate and multigroup miniature valve, described high temperature micro-electric hot plate is arranged in and described is dried microchannel bottom.
Described solvent exchange microchannel is snakelike densely covered arrangement, and described is dried microchannel and described cooling microchannel
Gather for meander and arrange, make full use of micro-fluidic chip space, increase solvent exchange and liquid film drying time.Described high temperature is micro-
Electric hot plate be arranged in it is described be dried microchannel bottom, accelerate liquid film drying.Described miniature valve is connected with described controller,
Described controller output corresponding signal, micro-valve is opened and closed under electric current driving, effectively connects or isolate microchannel, and control is anti-
Between seasonable.After described liquid film solidification micro structure, the high double emulsion of concentricity and sphericity solidify to form shell core microsphere.
Described microsphere outer surface functionalization micro unit includes microsphere outer surface functionalization microchannel and multigroup miniature valve, institute
The microsphere outer surface functionalization microchannel stated be it is snakelike it is densely covered arrangement and multiple individual passages are isolated into by described miniature valve,
Fill abluent and initiator solution in different passages respectively.
Shell core microsphere respectively with abluent, initiator for reaction after, finally microsphere outer surface coat a layer function material draw
Agent is sent out, microsphere functionalization characteristic is induced.The microsphere response time in the channel is by miniature valve control.
Described functional stuffing loading and homogenizing micro unit is micro- comprising functional stuffing loading microchannel and functional stuffing homogenizing
Passage, constant temperature micro-electric hot plate and multigroup miniature valve, described functional stuffing loading microchannel and functional stuffing homogenizing microchannel is
Meander is gathered and is arranged, and described thermostatic electrothermal plate is arranged in described functional stuffing homogenizing microchannel bottom, and described function is filled out
Functional filler in material loading microchannel;The described miniature valve control shell core microsphere response time.
Functionalized microsphere is fully contacted in the channel reaction with functional stuffing, functional stuffing is loaded, then in described work(
Can filler loading microchannel in by described constant temperature micro-electric hot plate thermal induction functional material characteristic and the surface for making function material
Material is uniformly distributed in gradually dry run.
It is typical diesis shape microchannel that described double emulsion generates micro structure, and directly processing is in described digitized
In micro-fluidic integrated chip.Described miniature valve individually controls opening and closing by the control circuit in described controller, described
The micro-fluidic integrated chip of digitized according to differences such as working condition, fluid properties, size can be controlled in several square centimeters
Left and right, material can select silicon chip, glass, silicone rubber, plastic or other material as substrate, by the side such as etching, photoetching or die
Method processes microchannel.
When described microfluid drive runs, large volume of double emulsion generates micro- in described double emulsion
Generate in structure, along with flow of fluid, into described bionical division array, single large volume double emulsion is just split into
4,8 ... .2nIndividual homogeneity is good, the high double emulsion of quality.Described dielectrophoresises regulation of mental activities micro unit is subsequently entered, by non-equal
Even electric field regulation of mental activities, obtains good sphericity, the high double emulsion of concentricity, simultaneously because the joule heating effect of electrophoresis accelerates dual breast
Pension gelation, becomes gelation macromolecular structure.Subsequently in described liquid film solidification micro unit, first in described solvent exchange
Solvent exchange is carried out in microchannel, then rapid draing in microchannel is dried described, it is then micro- by described cooling again
Passage becomes solid-state-microspherical.By transfer passages, solid-state-microspherical is transported to into described microsphere outer surface functionalization micro unit and is entered
Row outer surface functionalization, finally continues optimizing surface material knot in described functional stuffing loading and homogenizing micro unit
Structure, finally enters described shell kernel function material collector from the functional material output channel described in end, obtains high-quality
Shell kernel function material.
Beneficial effect:
A kind of device for preparing high-quality shell kernel function material according to the present invention, makes full use of digitized microflow control technique
Advantage, double emulsion is generated into micro structure, bionical division array, dielectrophoresises regulation of mental activities micro unit, liquid film solidification micro unit, micro-
Outer surface of ball functionalization micro unit and functional stuffing loading and homogenizing micro unit are integrated on a micro-fluidic chip, using dual
Break emulsions method quickly prepares the good double emulsion of homogeneity, using the sphericity of the double emulsions of high frequency inhomogeneous field regulation and control and same
Heart degree accelerates emulsion gel simultaneously, and efficiently realizes liquid film solidification, the loading of microsphere surface functionalization material and homogenizing, real
The quick preparation of high-quality shell kernel function material is showed.Further, since introducing the spy of bionical division array in division array
Structure is levied, the double emulsion that the generation quantity that can efficiently double is more, homogeneity is good, monodispersity is good, using dielectrophoresises skill
Art aids in the quick-gelatinizing of double emulsion.The above factor, not only makes full use of the space of micro-fluidic chip so that chip
Topology layout compact and reasonable, also achieves purpose that is quick, efficiently preparing high-quality shell kernel function material.
Description of the drawings
Fig. 1 is the structural representation of the present invention.
Fig. 2 is micro-fluidic integrated chip schematic diagram of the invention.
Fig. 3 is bionical division array schematic diagram of the invention.
Fig. 4 is regulation of mental activities electrode of the present invention and capture, release electrode schematic diagram.
1. external fluid phase syringe pumps and syringe in figure;2. middle phase fluid syringe pump and syringe;3. internal phase fluid is noted
Penetrate pump and syringe;4. foreign minister's input channel;5. mesophase input channel;6. in phase input channel and;7. digitized is micro-fluidic
Integrated chip;8. functional material output channel;9. shell kernel function material collector;10. controller;11. double emulsions generate micro-
Structure;12. bionical division arrays;13. dielectrophoresises regulation of mental activities micro units;14. solvent exchange microchannels;15. are dried microchannel;
16. cooling microchannels;17. high temperature micro-electric hot plates;18. microsphere outer surface functionalization micro units;The loading of 19. functional stuffings is micro- logical
Road;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. is rearmounted parallel
Plate electrode;30. gripper shoes.
Specific embodiment
Further described in detail below in conjunction with the accompanying drawings:
Fig. 1 gives the system diagram of the present invention, a kind of existing device of preparation of high-quality shell kernel function material, concrete structure bag
Include external fluid phase syringe pump and syringe 1, middle phase fluid syringe pump and syringe 2, internal phase fluid syringe pump and syringe 3,
Foreign minister's input channel 4, mesophase input channel 5, the micro-fluidic integrated chip 7, functional material of interior phase input channel 6, digitized are defeated
Go out the key components such as passage 8, shell kernel function material collector 9, controller 10.External fluid phase, middle phase fluid, indraft
Body is respectively in external fluid phase syringe pump and syringe 1, middle phase fluid syringe pump and syringe 2, internal phase fluid syringe pump and note
Emitter 3 drives in the micro-fluidic integrated chip 7 of lower inflow digitized and forms double emulsion, and in the micro-fluidic integrated chip 7 of digitized
It is middle to solidify and functional material loading procedure through division, with one heart regulation and control and quick-gelatinizing, liquid film, it is finally defeated from functional material
Go out in passage 8 and flow into shell kernel function material collector 9, wherein, controller 10 is micro- by the different signal digital control of output
Various micromodule equipments in stream control integrated chip 7.
Fig. 2 gives digitized micro-fluidic integrated chip schematic diagram, concrete structure include figure in foreign minister's input channel 4, in
Between phase input channel 5, interior phase input channel 6, functional material output channel 8, double emulsion generate micro structure 11;Bionical division battle array
Row 12;Dielectrophoresises regulation of mental activities micro unit 13;Solvent exchange microchannel 14;It is dried microchannel 15;Cooling microchannel 16;The micro- electricity of high temperature
Hot plate 17;Microsphere outer surface functionalization micro unit 18;Functional stuffing loads microchannel 19;Functional material homogenizing microchannel 20;It is permanent
Warm micro-electric hot plate 21;Miniature valve 22;Deng key component, from foreign minister's input channel 4, mesophase input channel 5, the input of interior phase
The fluid that stream enters in Digital microfluidic chips in passage 6, generates in micro structure 11, due to the shearing force of fluid in double emulsion
With the effect of fluid interfacial surface tension, the double emulsions of large volume are generated, subsequently bionical division array 12 is flowed into flowing, so as to reality
A double emulsion homolysis is showed and has adjusted into dielectrophoresises for two, four, eight ... the double emulsions after division
In heart micro unit 13, double emulsion regulation of mental activities are realized, and have adjusted sphericity, while under electrophoretic action, accelerating gel.Gel
Afterwards, double emulsion has reformed into gel macromolecule double emulsion, subsequently carries out fast solvent exchange in solvent exchange microchannel 14,
Swap time is controlled by 4 groups of miniature valves 22, and double emulsion shell becomes plastic macromolecule thin film, in microchannel 15 is dried,
It is rapid to be dried because the high temperature micro-electric hot plate 17 for being dried the bottom of microchannel 15 is heated, subsequently into cooling in cooling microchannel 16,
Flexible polymer films microsphere is thus obtained, the flash cure process of double emulsion is realized, the response time in solidification
Controlled by miniature valve 22.Then flexible polymer films microsphere is inserted in microsphere outer surface functionalization micro unit 18, in microsphere
In outer surface functionalization micro unit 18, microsphere is set to be reacted with abluent, initiator successively in the channel, by miniature valve 22
In the control response time, finally a layer function material initiator is coated in microsphere outer surface, induce microsphere functionalization characteristic.Subsequent work(
Microsphere can be changed and be fully contacted reaction with functional stuffing therein in functional stuffing loading microchannel 19, be carried out loading function and fill out
Material, it is special by thermal induction functional material by the constant temperature micro-electric hot plate 21 of bottom subsequently into functional stuffing homogenizing microchannel 20
The functional material on property and the surface for making is uniformly distributed in gradually dry run, and the wherein response time of passage is controlled by miniature valve 22
System, with regard to this, continuously obtains high-quality shell kernel function material in the micro-fluidic integrated chip of digitized.
Fig. 3 gives bionical division array schematic diagram, and concrete structure includes main channel 23, level separation lanes 24, converges
The grade key component of passage 25, double emulsions flow into level separation lanes 24 after generating in main channel 23, by uniformly successively
Two, four, eight, 16 ... individual uniform double emulsions are split into, is finally converged in converging channel 25.Thus obtain
The even, double emulsion that monodispersity is good.
Fig. 4 gives regulation of mental activities electrode and capture, release electrode structure schematic diagram, and concrete structure includes preposition parallel-plate electrode
26th, the key components such as conductive filament electrode 27, underlying parallel-plate electrode 28, rearmounted parallel-plate electrode 29, gripper shoe 30 are put on,
Wherein gripper shoe 30 needs to coat layer of conductive film as dielectric layer.When a number of target double emulsion enters into regulation of mental activities
When in structure, preposition parallel-plate electrode 26 opens in passage, and rearmounted parallel-plate electrode 29 is conductive, captures target double emulsion.So
Afterwards by the closing passage of preposition parallel-plate electrode 26, subsequently on to put conductive filament electrode 27, underlying parallel-plate electrode 28 conductive, carry out double
Emulsion regulation of mental activities, obtains good sphericity, and after the high double emulsion of concentricity, rearmounted parallel-plate electrode 29 opens passage, preposition parallel
Plate electrode 26 is conductive, discharges target double emulsion.Thus obtain the high double emulsion of good sphericity, concentricity.
Claims (6)
1. a kind of preparation facilitiess of shell kernel function material, including micro-fluidic integrated chip, microfluid drive and shell core work(
Energy material collector, described microfluid drive includes external fluid phase syringe pump and syringe, middle phase fluid syringe pump
And syringe, internal phase fluid syringe pump and syringe, described micro-fluidic integrated chip includes that foreign minister's input channel, mesophase are defeated
Enter passage, interior phase input channel, double emulsion and generate micro structure and functional material output channel, it is logical in described foreign minister's input
Road connects foreign minister's syringe, and in described mesophase input channel connection mesophase syringe, described interior phase input channel connects
Interior phase syringe is connect, in the described shell kernel function material collector of the exit connection of described functional material output channel, its
It is characterised by:Described micro-fluidic integrated chip also includes being located at double emulsion generation micro structure and functional material output is logical
Bionical division array, dielectrophoresises regulation of mental activities micro unit, liquid film solidification micro unit between road, microsphere outer surface functionalization micro unit
With functional stuffing loading and homogenizing micro unit, it is micro- that the double emulsion generates micro structure, bionical division array, dielectrophoresises regulation of mental activities
Unit, liquid film solidification micro unit, microsphere outer surface functionalization micro unit and functional stuffing loading and homogenizing micro unit are by transporting
Passage is sequentially connected, and described bionical division array includes main channel, at least two-stage level separation lanes and converging channel, described
Level separation lanes be biomimetic features microchannel, described converging channel is funnel-shaped structure, described dielectrophoresises regulation of mental activities
Micro unit includes multigroup regulation of mental activities electrode arranged side by side and capture, release electrode;The level separation lanes be square-section, every grade of level
It is 2 that separation lanes are division number, and each separation lanes includes access ramp and is connected to the parallel channels of access ramp rear end, described flat
Row of channels is parallel with main channel, and the angle between two access ramps is 60 degree, and n-th grade of level separation lanes divides with the 0th grade of level
Passage it is highly consistent, the relation of width is Dn/D0=2-n/p, wherein, p > 1;N-th grade of level separation lanes and the 0th grade of level
The relation of separation lanes length is Ln/L0=2-n/q, wherein 1<q<2;Described regulation of mental activities electrode adopts high frequency inhomogeneous field, by
On put conductive filament electrode, underlying parallel-plate electrode composition.
2. preparation facilitiess according to claim 1, it is characterised in that:Described dielectrophoresises regulation of mental activities micro unit also includes one
Gripper shoe, described support plate surface uniformly coats layer of conductive film as dielectric layer;Described release electrode is using uniform
Electric field, is made up of preposition parallel-plate electrode, rearmounted parallel-plate electrode, and described preposition parallel-plate electrode is rearmounted parallel with described
Plate electrode is opened and closed by micro motor control.
3. preparation facilitiess according to claim 1, it is characterised in that:Described liquid film solidification micro unit includes solvent exchange
Microchannel, microchannel, cooling microchannel, high temperature micro-electric hot plate and multigroup miniature valve are dried, described high temperature micro-electric hot plate arrangement
Microchannel bottom is dried in described.
4. preparation facilitiess according to claim 3, it is characterised in that:Described solvent exchange microchannel is snakelike densely covered row
Row, described be dried microchannel and described cooling microchannel is the densely covered arrangement of meander.
5. preparation facilitiess according to claim 1, it is characterised in that:Described microsphere outer surface functionalization micro unit includes
Microsphere outer surface functionalization microchannel and multigroup miniature valve, described microsphere outer surface functionalization microchannel is snakelike densely covered arrangement
And multiple individual passages are isolated into by described miniature valve, fill abluent and initiator solution respectively in different channels.
6. preparation facilitiess according to claim 1, it is characterised in that:Described functional stuffing is loaded and homogenizing micro unit bag
Microchannel and functional stuffing homogenizing microchannel, constant temperature micro-electric hot plate and multigroup miniature valve, described function are loaded containing functional stuffing
It is the densely covered arrangement of meander that filler loads microchannel and functional stuffing homogenizing microchannel, and described constant temperature micro-electric hot plate is arranged in described
Functional stuffing homogenizing microchannel bottom, functional filler in described functional stuffing loading microchannel;Described miniature valve control
The shell core microsphere response time processed.
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CN103285947A (en) * | 2013-05-27 | 2013-09-11 | 苏州扬清芯片科技有限公司 | Droplet micro-fluidic chip and operation method thereof |
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