CN115254222B - Method for preparing monodisperse non-Newtonian fluid droplets based on asymmetric parallel microchannels - Google Patents
Method for preparing monodisperse non-Newtonian fluid droplets based on asymmetric parallel microchannels Download PDFInfo
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- 229920001223 polyethylene glycol Polymers 0.000 claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims description 8
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 7
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 4
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
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- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 4
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- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 4
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- 239000005662 Paraffin oil Substances 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 2
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 claims description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 2
- 239000005543 nano-size silicon particle Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
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- 239000000230 xanthan gum Substances 0.000 claims description 2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/02—Burettes; Pipettes
- B01L3/0241—Drop counters; Drop formers
- B01L3/0265—Drop counters; Drop formers using valves to interrupt or meter fluid flow, e.g. using solenoids or metering valves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502769—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements
- B01L3/502784—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements specially adapted for droplet or plug flow, e.g. digital microfluidics
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Abstract
The invention discloses a method for preparing monodisperse non-Newtonian fluid droplets based on asymmetric parallel microchannels, and belongs to the technical field of micro-chemical industry. The micro-channel device consists of an upper cover plate and a bottom plate, wherein the upper cover plate is provided with two-phase liquid inlet holes and liquid outlet holes communicated to the micro-channel bottom plate. The lower bottom plate consists of a fluid distributing pipe, a parallel branch, two T-shaped knots and a liquid drop collecting pipe. The method for preparing the monodisperse non-Newtonian fluid liquid drops based on the asymmetric parallel micro-channels improves the production efficiency of liquid drop preparation, can conveniently realize the regulation and control of the liquid drop size through the change of the two-phase flow, and has good stability and uniform liquid drop size in the liquid drop preparation process. Has wide application value in the fields of fine chemical industry, biological medicine, materials, food and the like.
Description
Technical Field
The invention belongs to the technical field of micro-chemical industry, and particularly relates to a method for preparing monodisperse non-Newtonian fluid droplets based on an asymmetric parallel microchannel device.
Background
The micro-droplets can provide relatively independent micro-reaction, micro-mixing and micro-differential space for the fields of chemical reaction, biosynthesis, material preparation and the like. The uniformity of the droplet size is a necessary condition to ensure efficient performance of the corresponding process. The traditional method for preparing the micro-droplets mainly comprises a mechanical stirring method and a membrane emulsification method, however, the method consumes large amount of reagent, and the prepared micro-droplets have poor monodispersity and instability in size. The micro-chemical technology has excellent characteristic of accurate control, which makes it have absolute advantage in preparing uniform liquid drops. However, the production flux of a single-pipeline microchannel is small, and the mass preparation of micro-droplets is severely restricted. Patent CN107511189B discloses a preparation method of monodisperse micro-droplets based on capillary, which has small production flux and cannot realize continuous preparation. The microchannel apparatus for preparing monodisperse non-newtonian fluid droplets using acoustic radiation in CN114160218A also has only a single tube, and the problem of small production throughput is also present.
During the amplification process, the fluid flow distribution conditions in the parallel lines affect droplet size uniformity and even do not generate droplets when a cross flow occurs. In addition, the flowing medium used in the micro-channel usually contains substances such as polymers, and the fluid has complex nonlinear fluid rheological characteristics, such as fluid viscosity and elasticity, which are closely related to deformation rate during the flowing process, so that the fluid distribution and the monodispersity of liquid drops are seriously affected. Therefore, high throughput preparation of uniform microdroplets based on parallel amplification is one of the focus of attention. Patent CN113304790a discloses a microchannel basic unit and array group thereof for realizing high-throughput preparation of micro-droplets. The basic unit is a similar-Chinese character 'Hui' structure with two focusing structures, the structure is complex, and the requirements on processing and manufacturing are very high.
Current parallel micro-channels can be structurally divided into symmetrical parallel micro-channels and asymmetrical parallel micro-channels. The patent CN110624616A adopts a three-dimensional tree-shaped symmetrical parallel amplifying mode to improve the yield of micro liquid drops, and in the micro channels, uneven fluid distribution can be caused by the difference of pipeline processing precision and pipeline surface roughness, and the space utilization rate is lower. The asymmetric parallel micro-channel has the advantages of strong disturbance resistance, compact arrangement, easy integration, high space utilization rate and the like, and the key point of preparing uniform liquid drops by the asymmetric parallel micro-channel is reasonable structural layout and size design.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for preparing monodisperse non-Newtonian fluid droplets based on asymmetric parallel microchannels, so as to solve the problems of low droplet production efficiency and uneven droplet size in the prior art.
The technical scheme of the invention is as follows:
an asymmetric parallel microchannel consists of an upper cover plate and a lower bottom plate, wherein the upper cover plate is provided with a two-phase liquid inlet and a liquid outlet which are communicated with the lower bottom plate, the lower bottom plate is etched with a main body structure of the microchannel, and the two main body structures are tightly bonded by bolts to ensure the tightness of the microchannel; the microchannel device body comprises: the device comprises a continuous phase inlet, a parallel channel for transporting continuous phase fluid, a disperse phase inlet, a main channel for transporting disperse phase fluid, a parallel channel for transporting disperse phase fluid, two T-shaped structures, a parallel channel for transporting liquid drops, a liquid drop collecting main channel and a liquid drop discharging outlet, wherein the continuous phase fluid inlet is connected with the parallel channel for transporting continuous phase fluid, the disperse phase fluid inlet is connected with the main channel for transporting disperse phase fluid, the main channel is vertically connected with the parallel channel for transporting disperse phase fluid, the parallel channel for transporting continuous phase fluid, the parallel channel for transporting disperse phase fluid and the parallel channel for transporting liquid drops are connected through the T-shaped structures, the other end of the parallel channel for transporting liquid drops is vertically connected with the liquid drop collecting main channel, and the liquid discharging outlet is positioned at the tail end of the liquid drop collecting main channel.
The parallel channels for transporting the continuous phase fluid have the same length and are 50-100 times the height of the micro-channels, the height of the micro-channels is 50-1000 mu m, and the aspect ratio is 0.1-10.
The disperse phase liquid inlet is positioned at one side of the micro-channel, the width of the main channel for transporting the disperse phase fluid is 1-30 times of the height of the micro-channel, and the lengths of the parallel channels for transporting the disperse phase fluid are the same and are 10-20 times of the height of the micro-channel.
The width of the liquid drop collecting main channel is 1-30 times of the height of the micro channel, the liquid drop discharging outlet is positioned at the opposite side of the disperse phase inlet side, and the liquid drop collecting main channel and the liquid drop discharging outlet are in a zigzag shape.
The number of parallel channels for transporting the disperse phase fluid is consistent with that of parallel channels for transporting the continuous phase fluid, and the specific number is set according to the requirement and is more than or equal to 2.
A method for preparing monodisperse non-Newtonian fluid liquid drops based on asymmetric parallel micro-channels comprises the steps that a continuous phase and a disperse phase are respectively injected into the asymmetric parallel micro-channels through a continuous phase inlet and a disperse phase inlet, mutually-immiscible two phases are contacted at a T-shaped structure, the disperse phase generates liquid drops under the action of extrusion force and shearing force of the continuous phase, then the liquid drops are discharged out of the micro-channels through a liquid outlet, and the liquid drops with different sizes are prepared through two-phase flow regulation.
The continuous phase is one of cyclohexane, n-butane, paraffin oil and silicone oil which are organic solvents.
The disperse phase is one of aqueous solution of sodium carboxymethyl cellulose, xanthan gum, polyethylene oxide and polyacrylamide or polyethylene glycol solution added with nano silicon dioxide, the concentration of polymer added in the aqueous solution is 0.003-4%, and the concentration of silicon dioxide added in polyethylene glycol with the particle size of 15nm is 5-15%.
The continuous phase or the disperse phase contains one of surfactants Span40, span80, span85, tween 20 and Tween 80, and the addition amount of the surfactant is 2-7%.
The invention has the following beneficial effects:
the device and the method complete the preparation of uniform non-Newtonian fluid drops, can realize the continuous preparation of drops with different sizes through two-phase flow regulation, and are accurate in control and simple and convenient in operation. By arranging the asymmetric parallel micro-pipelines, the liquid drop preparation efficiency is improved, the system immunity is enhanced, the space utilization rate of the micro-channel chip is improved, the material cost is reduced, and the processing and the manufacturing are facilitated. The uniformity of the droplets prepared in the two lines was good. The production flux of the micro-channel basic units can be further improved through the array arrangement of the micro-channel basic units.
Drawings
FIG. 1 is a schematic view of a microchannel structure according to the present invention;
wherein: 1-continuous phase inlet; 2-parallel channels for transporting the continuous phase fluid; 3-disperse phase inlet; 4-a main channel for transporting the dispersed phase fluid; 5-parallel channels for transporting the dispersed phase fluid; a 6-T structure; 7-parallel channels for transporting droplets; 8-a main droplet collection channel; 9, a liquid outlet;
in FIG. 2 (a), (b) and (c) are Q respectively d =60 μl/min, disperse phase flow Q c Uniform non-Newtonian liquid drops with different sizes, which are prepared at 200 mu L/min,300 mu L/min and 400 mu L/min respectively;
FIG. 3 is a graph showing the droplet size distribution prepared using the present microchannel at a dispersed phase injection flow rate of 60. Mu.L/min and a dispersed phase injection flow rate of 200. Mu.L/min.
The specific embodiment is as follows:
the method of preparing monodisperse non-Newtonian droplets based on asymmetric parallel microchannels according to the invention is described in further detail below with reference to the accompanying drawings and examples.
Example 1:
and (3) preparing polyacrylamide and deionized water according to a mass ratio of 1:10000 at normal temperature, and stirring for 10 hours to fully dissolve the high polymer substances to prepare a disperse phase. The surfactant span85 and cyclohexane are fully mixed according to the mass ratio of 5:100, and a continuous phase is prepared. The width of the main channel for transporting the disperse phase is 20 times of the height, and the aspect ratio of other pipelines is 1. The continuous phase and the disperse phase were injected from inlets 1 and 3 of the micro channel, respectively, with an injection flow rate of 50. Mu.L/min for the disperse phase and 800. Mu.L/min for the continuous phase. After meeting at the T-shaped junction, the two liquid drops are generated under the action of extrusion force and shearing force of continuous phase fluid, the non-Newtonian liquid drops with the diameter of 480 mu m flow out of the micro-channel from the discharge outlet after being generated, and then flow into the collecting device.
Example 2:
and preparing sodium carboxymethylcellulose and deionized water according to a mass ratio of 1:100 at normal temperature, and stirring for 10 hours to fully dissolve the high molecular substances to prepare a disperse phase. The surfactant span85 and cyclohexane are fully mixed according to the mass ratio of 5:100, and a continuous phase is prepared. The main channel for transporting the disperse phase and the main channel for collecting liquid drops are 20 in width-to-height ratio, and the aspect ratio of other pipelines is 1. The continuous phase and the disperse phase were injected from inlets 1 and 3 of the micro channel, respectively, with an injection flow rate of 250. Mu.L/min for the disperse phase and 200. Mu.L/min for the continuous phase. After meeting at the T-shaped junction, under the action of extrusion force and shearing force of continuous phase fluid, non-Newtonian liquid drops with the diameter of 740 mu m are generated, and after the liquid drops are generated, the liquid drops flow out of the micro-channel from the outlet and enter the collecting device.
Example 3:
and preparing sodium carboxymethylcellulose and deionized water according to a mass ratio of 0.1:100 at normal temperature, and stirring for 10 hours to fully dissolve the high polymer substances to prepare a disperse phase. The surfactant span85 and cyclohexane are fully mixed according to the mass ratio of 5:100, and a continuous phase is prepared. The main droplet collecting channel has a width to height ratio of 20 and the other channels have an aspect ratio of 1. The continuous phase and the disperse phase were injected from inlets 1 and 3 of the micro channel, respectively, with an injection flow rate of 20. Mu.L/min for the disperse phase and 400. Mu.L/min for the continuous phase. After meeting at the T-shaped junction, the two liquid drops with the diameter of 520 mu m are generated under the action of the extrusion force and the shearing force of the continuous phase fluid, and the liquid drops flow out of the micro-channel from the outlet after being generated and enter the collecting device.
Example 4:
and (3) preparing polyacrylamide and deionized water according to a mass ratio of 1:10000 at normal temperature, and stirring for 10 hours to fully dissolve the high polymer substances to prepare a disperse phase. The surfactant span85 and cyclohexane are fully mixed according to the mass ratio of 5:100, and a continuous phase is prepared. The aspect ratio of all the channels in the microchannel is 1. The continuous phase and the disperse phase were injected from inlets 1 and 3 of the micro channel, respectively, with an injection flow rate of 250. Mu.L/min for the disperse phase and 400. Mu.L/min for the continuous phase. After meeting at the T-shaped junction, the two liquid drops with the diameter of 600 mu m are generated under the action of the extrusion force and the shearing force of the continuous phase fluid, and the liquid drops flow out of the micro-channel from the discharge outlet after being generated and enter the collecting device.
Example 5:
and (3) preparing polyacrylamide and deionized water according to a mass ratio of 0.3:10000 at normal temperature, and stirring for 10 hours to fully dissolve the high polymer substances to prepare a disperse phase. The surfactant span85 and cyclohexane are fully mixed according to the mass ratio of 5:100, and a continuous phase is prepared. The main droplet collecting channel has a width to height ratio of 20 and the other channels have an aspect ratio of 1. The continuous phase and the disperse phase were injected from inlets 1 and 3 of the micro channel, respectively, with an injection flow rate of 350. Mu.L/min for the disperse phase and 400. Mu.L/min for the continuous phase. After meeting at the T-shaped junction, the two liquid drops with the diameter of 616 mu m are generated under the action of the extrusion force and the shearing force of the continuous phase fluid, and the liquid drops flow out of the micro-channel from the discharge outlet after being generated and enter the collecting device.
Example 6:
and preparing the silicon dioxide nano particles and polyethylene glycol according to the mass ratio of 8:100, adding 4% tween 20, and fully stirring to fully mix the silicon dioxide particles and the polyethylene glycol to prepare a disperse phase. The continuous phase is silicone oil with the viscosity of 10 mPas. The main droplet collecting channel has a width to height ratio of 20 and the other channels have an aspect ratio of 1. The continuous phase and the disperse phase were injected from the inlets 1 and 3 of the micro channel, respectively, the injection flow rate of the disperse phase was 40. Mu.L/min, and the injection flow rate of the continuous phase was 50. Mu.L/min. After meeting at the T-shaped junction, the two liquid drops with the diameter of 500 mu m are generated under the action of the extrusion force and the shearing force of the continuous phase fluid, and the liquid drops flow out of the micro-channel from the discharge outlet after being generated and enter the collecting device.
Example 7:
and preparing the silicon dioxide nano particles and polyethylene glycol according to the mass ratio of 10:100, adding 4% tween 20, and fully stirring to fully mix the silicon dioxide particles and the polyethylene glycol to prepare a disperse phase. The continuous phase is silicone oil with the viscosity of 10 mPas. The main droplet collecting channel has a width to height ratio of 20 and the other channels have an aspect ratio of 1. The continuous phase and the disperse phase were injected from the inlets 1 and 3 of the micro channel, respectively, the injection flow rate of the disperse phase was 10. Mu.L/min, and the injection flow rate of the continuous phase was 50. Mu.L/min. After meeting at the T-shaped junction, the two liquid drops with the diameter of 385 microns are generated under the action of the extrusion force and the shearing force of the continuous phase fluid, and the liquid drops flow out of the micro-channel from the discharge outlet after being generated and enter the collecting device.
The foregoing is merely exemplary of the present invention and is not intended to limit the scope of the invention in any way. Any simple modification, substitution, improvement, etc. made by those skilled in the relevant art in view of the technical spirit of the present invention still fall within the scope of the technical proposal of the present invention.
Claims (6)
1. The asymmetric parallel micro-channel is characterized by comprising an upper cover plate and a lower bottom plate, wherein the upper cover plate is provided with a two-phase liquid inlet and a liquid outlet which are communicated to the lower bottom plate, the lower bottom plate is etched with a main body structure of the micro-channel, and the two main body structures are tightly bonded by bolts to ensure the tightness of the micro-channel; the microchannel device body comprises: the device comprises a continuous phase inlet (1), a parallel channel (2) for transporting continuous phase fluid, a disperse phase inlet (3), a main channel (4) for transporting disperse phase fluid, a parallel channel (5) for transporting disperse phase fluid, two T-shaped structures (6), a parallel channel (7) for transporting liquid drops, a liquid drop collecting main channel (8) and a liquid drop discharging port (9); the continuous phase inlet (1) is connected with a parallel channel (2) for transporting continuous phase fluid, the disperse phase inlet (3) is connected with a main channel (4) for transporting disperse phase fluid, the main channel (4) for transporting disperse phase fluid is vertically connected with a parallel channel (5) for transporting disperse phase fluid, the parallel channel (2) for transporting continuous phase fluid, the parallel channel (5) for transporting disperse phase fluid and a parallel channel (7) for transporting liquid drops are connected through a T-shaped structure (6), the other end of the parallel channel (7) for transporting liquid drops is vertically connected with a liquid drop collecting main channel (8), and a liquid drop outlet (9) is positioned at the tail end of the liquid drop collecting main channel (8);
the lengths of the parallel channels (2) for transporting the continuous phase fluid are the same, the lengths are 50-100 times of the heights of the micro channels, the heights of the micro channels are 50-1000 mu m, and the aspect ratio is 0.1-10;
the disperse phase liquid inlet is positioned at one side of the micro-channel, the width of the main channel (4) for transporting the disperse phase fluid is 1-30 times of the height of the micro-channel, and the lengths of the parallel channels (5) for transporting the disperse phase fluid are the same and are 10-20 times of the height of the micro-channel;
the width of the liquid drop collecting main channel (8) is 1-30 times of the height of the micro channel, the liquid drop discharging outlet (9) is positioned at the opposite side of the disperse phase inlet side, and the liquid drop collecting main channel and the liquid drop discharging outlet are in a zigzag shape.
2. The asymmetric parallel microchannel according to claim 1, wherein the number of parallel channels for transporting the dispersed phase fluid is equal to or greater than 2, and the specific number is set according to the requirement.
3. A method for preparing monodisperse non-newtonian fluid droplets based on asymmetric parallel micro-channels, which is characterized in that a continuous phase and a disperse phase are respectively injected into the asymmetric parallel micro-channels according to any one of claims 1-2 through a continuous phase inlet (1) and a disperse phase inlet (3), mutually-immiscible two phases are contacted at a T-shaped structure (6), the disperse phase generates droplets under the action of extrusion force and shearing force of the continuous phase, and then the droplets are discharged from the micro-channels through a droplet discharge outlet (9), and droplets with different sizes are prepared through two-phase flow regulation.
4. A method for preparing monodisperse non-newtonian fluid droplets based on asymmetric parallel micro channels according to claim 3, wherein the continuous phase is one of the organic solvents cyclohexane, n-butane, paraffin oil, silicone oil.
5. The method for preparing monodisperse non-Newtonian fluid droplets based on asymmetric parallel microchannels according to claim 3, wherein the disperse phase is an aqueous solution of sodium carboxymethyl cellulose, xanthan gum, polyethylene oxide and polyacrylamide or a polyethylene glycol solution added with nano silicon dioxide, the concentration of the polymer added in the aqueous solution is 0.003% -4%, and the concentration of the silicon dioxide added in the polyethylene glycol with the particle size of 15nm is 8% -15%.
6. The method for preparing monodisperse non-newtonian fluid droplets based on asymmetric parallel micro channels according to claim 3, wherein the continuous phase or the disperse phase contains one of surfactants Span40, span80, span85, tween 20 and tween 80, and the addition amount of the surfactant is 2% -7%.
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| JP2005297150A (en) * | 2004-04-14 | 2005-10-27 | Tosoh Corp | Microscopic flow passage structure and droplet generating method using this structure |
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