CN103240042B - Method for initiating droplet fusion by liquid infiltration - Google Patents

Method for initiating droplet fusion by liquid infiltration Download PDF

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CN103240042B
CN103240042B CN201310169391.5A CN201310169391A CN103240042B CN 103240042 B CN103240042 B CN 103240042B CN 201310169391 A CN201310169391 A CN 201310169391A CN 103240042 B CN103240042 B CN 103240042B
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water
oil
phase fluid
drop
oil emulsion
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CN103240042A (en
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邓楠楠
褚良银
汪伟
巨晓洁
谢锐
D·A·威茨
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Sichuan University
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Sichuan University
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Abstract

The invention belongs to the field of droplet fusion, and particularly relates to a method for initiating different monodisperse droplet fusion by utilizing liquid wettability. The method comprises the processing steps of: (1) preparing disperse water phase, medium oil phase and continuous phase liquid; (2) injecting each disperse phase liquid into a micro-fluidic device to form water-in-oil emulsion droplets and oil-pocket water-in-oil emulsion droplets, enabling the formed water-in-oil emulsion droplets and the oil-pocket water-in-oil emulsion droplets to enter a collecting tube along with the continuous phase fluid; paving oil layers at the surfaces of the oil-pocket water-in-oil emulsion droplets at the surfaces of the water-in-oil emulsion droplets when the water-in-oil emulsion droplets contact the oil-pocket water-in-oil emulsion droplets in an expanded chamber of the collecting tube; and discharging the oil layers between water drops in the oil-pocket water-in-oil emulsion droplets and the water drops in the water-in-oil emulsion droplets, wherein the water drops in the two droplets are fused to achieve micro-mixing or micro-reaction; and (3) collecting the fused droplets.

Description

A kind of liquid-soaked causes the method that drop merges
Technical field
The invention belongs to drop and merge field, particularly in a kind of microchannel, utilize liquid-soaked to cause different single dispersant liquid drops and merge the method that realizes micro-mixing or micro-reaction.
Background technology
Microreactor is a kind of micro-scale reaction vessels of passing through the mixing realization response process of control trace reagent in microchannel.Than conventional reaction vessel (as flask etc.), microreactor has higher specific area, as: the specific area that width is the microreactor passage of 100 μ m is approximately 200 times of 100 mL flask specific areas, therefore microreactor is more conducive to the diffusion of molecule and the transmission of energy, can make that chemical reaction is faster, more effective to carry out, micro-reaction is few to the demand of reagent, substantially pollution-free, have better security, and with low cost.Therefore, the development of microreactor has caused that scientists pays close attention to greatly.Microreactor has been widely used in the research and development of chemical engineering process at present, and its main application fields comprises the preparation of organic building-up process, micron and nano material and the production of household chemicals etc.Although microreactor has above-mentioned advantage and wide application prospect, but microreactor system build that cost is high, flexibility is lower, and be difficult to effectively solve the problems such as obstruction that have precipitation to generate timer microchannel, this has limited the application of microreactor to a certain extent.One of effective ways that address this problem are in microchannel, to utilize the drop of motion as carrier, realize micro-mixing or micro-reaction between the material comprising in drop by the fusion between different drops.Due to the drop in microchannel with continuous phase fluid always in flow regime, comprise whole micro-mixing and micro-course of reaction, thereby can avoid microchannel to stop up.
The method that at present in the microchannel of report, the fusion of drop realizes micro-mixing or micro-reaction mainly contains following several: (1) designs the chamber of an expansion in the collecting pipe of microfluidic device, when drop flows in the chamber expanding, flow velocity reduces, and between drop, extruding causes drop fusion to realize micro-mixing or micro-reaction mutually.Because surfactant is widely used in stable emulsion drop interface in micro-fluidic technologies, prevent that emulsion droplet from carrying out uncontrollable spontaneous fusion (as the fusion between emulsion droplet of the same race) in microchannel, and the method is difficult to realize and has the fusion between the stable drop of surfactant, thereby its range of application is restricted.(2) change the wellability of microfluidic device collecting pipe wall, for example in hydrophobic collecting pipe, design a slice hydrophilic region, when two water drops are flowed through this hydrophilic region simultaneously, all can breakdown of emulsion and be attached at and collect on tube wall, and then be sheared into drop, realize micro-mixing or micro-reaction.The method is only applicable to the system generating without precipitation, if there is precipitation to generate in emulsion droplet fusion process, precipitation will be adsorbed in together with drop collects on tube wall, along with the carrying out of reaction, precipitates a large amount of accumulations and can cause passage to stop up.(3) extra electric field on microfluidic device, and allow different electric charge on drop band, when colliding in passage, charged drop occurs to merge to realize micro-mixing or micro-reaction.The method can accurately realize man-to-man fusion, but the manufacturing process of microfluidic device and the control procedure of drop are all quite complicated, production cost is too high, is only applicable to electrifiable system, and extra electric field may cause damage to the active material comprising in drop.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of liquid-soaked to cause different drops and merge the method that realizes micro-mixing or micro-reaction, the method not only can realize the fusion between the stable drop of surfactant, and can avoid having in microreactor the obstruction of microchannel while precipitating generation.
Liquid-soaked of the present invention causes the method that different drops merge, and processing step is as follows:
(1) preparation disperses water, middle oil phase and continuous phase fluid
The preparation of the first disperse water phase fluid: water soluble emulsifier is added deionized water for stirring evenly to form the first disperse water phase fluid under normal pressure, room temperature, the mass ratio of described water soluble emulsifier and deionized water is 0.005 ~ 0.01:1;
The preparation of the second disperse water phase fluid: water soluble emulsifier is added deionized water for stirring evenly to form the second disperse water phase fluid under normal pressure, room temperature, the mass ratio of described water soluble emulsifier and deionized water is 0.005 ~ 0.01: 1;
The preparation of middle oil phase fluid: stir in oil soluble emulsifying agent being added to soybean oil under normal pressure, room temperature and form middle oil phase fluid, the amount of described oil soluble emulsifying agent is 0.01 ~ 0.04 g in every 1ml soybean oil;
The preparation of continuous phase fluid: the formation continuous phase fluid that stirs in surfactant being added to dimethicone under normal pressure, room temperature, the mass ratio of described surfactant and dimethicone is 0.005 ~ 0.01: 1;
(2) drop fusion realizes micro-mixing
The different inlets of the single-stage droplet generator that the second disperse water phase fluid that step (1) is prepared and continuous phase fluid inject respectively microfluidic device form monodispersed water-in-oil emulsion drop, and the different inlets that meanwhile the first disperse water phase fluid, middle oil phase fluid and the continuous phase fluid of step (1) preparation injected respectively to the two-stage droplet generator of microfluidic device form monodispersed oil bag water-in-oil emulsion drop; Formed water-in-oil emulsion drop, oil bag water-in-oil emulsion drop enter in the collecting pipe of microfluidic device with continuous phase fluid, while contacting in the expansion chamber at described collecting pipe when water-in-oil emulsion drop and oily bag water-in-oil emulsion drop, the oil reservoir on oil bag water-in-oil emulsion drop surface spreads into water-in-oil emulsion drop surface, water droplet in oil bag water-in-oil emulsion drop and the oil reservoir between the water droplet in water-in-oil emulsion drop are discharged from, and the water droplet in described two kinds of drops merges realizes micro-mixing;
Flow (the Q of described the first disperse water phase fluid a) be 400 ~ 600 μ L/h, the flow (Q of the second disperse water phase fluid d) be 200 ~ 500 μ L/h, the flow (Q of middle oil phase fluid b) be 20 ~ 80 μ L/h, the flow (Q of continuous phase fluid in described two-stage droplet generator c1) be the flow (Q of continuous phase fluid in 300 ~ 400 μ L/h, single-stage droplet generator c2) be 300 ~ 500 μ L/h;
(3) collect and merge the drop forming
By merging the emulsion droplet forming in step (2), with continuous phase fluid, by the efferent duct of microfluidic device, introduced in collection container.
In said method, described water soluble emulsifier is the addition polymers (Pluronic F127) of lauryl sodium sulfate or a kind of polypropylene glycol and oxirane.
In said method, described oil soluble emulsifying agent is the condensation product of poly-ricinoleic acid glyceride or alkyl phenol and oxirane.
In said method, described surfactant is the mixture (Dow Corning 749) that trimethicone and cyclohexyl methyl siloxanes form, and the volume ratio of trimethicone and cyclohexyl methyl siloxanes is 1: 1.
In said method, in described the second disperse water phase fluid, also contain water-soluble dye, in described middle oil phase fluid, also contain oil-soluble dyes; The effect of described water-soluble dye and oil-soluble dyes is to dye to drop, its addition so that observe is limited, can use the dyestuff of various water-soluble or soybean oils, preferentially select methylene blue as water-soluble dye to be, Lumogen F Red 300 is as oil-soluble dyes.
In said method, in described the first disperse water phase fluid, also contain the first reactant, described second disperses also to contain the second reactant in water, and the amount of described the first reactant, the second reactant is determined according to concrete chemical reaction; Water droplet in oil bag water-in-oil emulsion drop completes the first reactant with the water droplet in water-in-oil emulsion drop and reacts with the micro-of the second reactant in micro-process of mixing, the emulsion droplet that forms micro-product or contain micro-product, by micro-product or containing the drop of micro-product, with continuous phase fluid, by the efferent duct of microfluidic device, introduced in collection container, to collect liquid and remove oil phase with degreaser washing, then with deionized water washing, remove finish, continue after be drying to obtain micro-product.
In said method, described the first reactant and the second reactant are water miscible material.
Liquid-soaked of the present invention causes different drops and merges that to realize the mechanism of micro-mixing or micro-reaction as follows: thin-walled oil reservoir 1 and the spreading coefficient of the water droplet 2 in water-in-oil emulsion drop in continuous phase fluid 3 of oil bag water-in-oil emulsion drop are S 123-(α γ 13+ γ 12), γ ijthe interfacial tension that i phase and j are alternate (i ≠ j=1,2,3), , R 1and R 2be respectively the radius of the water droplet in oil bag water-in-oil emulsion drop and water-in-oil emulsion drop, work as S 1during > 0, the thin-walled oil reservoir 1 of oil bag water-in-oil emulsion drop will infiltrate and spread into water-in-oil emulsion drop
The surface of middle water droplet 2, water droplet 4 in oil bag water-in-oil emulsion drop and the thin-walled oil reservoir between the water droplet 2 in water-in-oil emulsion drop are discharged from, and the water droplet 4 in the water droplet 2 in water-in-oil emulsion drop and oil bag water-in-oil emulsion drop contact and causes that fusion realizes micro-mixing or micro-reaction formation emulsion droplet 5(is shown in Fig. 1).Can realize emulsion droplet merges relevant with the size of quilt infiltration drop with the volume of thin-walled oil reservoir as soakage layer, when soakage layer spreads into the drip gauge face that infiltrated completely, the drop of soakage layer institute embedding causes emulsion droplet and merges with being discharged completely by the liquid film between infiltration drop; If soakage layer is too thick or it is too little to be infiltrated drop, soakage layer spreads into infiltrated after drip gauge face completely, and the drop of soakage layer institute embedding and quilt infiltrate between drop and still had soakage layer to exist, just two drops can not contact, cannot realize fusion.
Of the present inventionly can use various types of microfluidic devices, as PDMS device and capillary glass tube device etc., microfluidic device used has the droplet generator of a two-stage and the droplet generator of a single-stage and a public collecting pipe that contacts fusion for drop; The oil bag water-in-oil emulsion drop of thin-walled prepared by two-stage droplet generator and water-in-oil emulsion drop prepared by the single-stage droplet generator public collecting pipe of simultaneously flowing through, the water component that the thin-walled oil reservoir by oil bag water-in-oil emulsion drop in collecting pipe causes them to the infiltration of water-in-oil emulsion drop merges; Preferably use the microfluidic device of following structure: described microfluidic device comprises slide, upper cover glass, lower cover glass, injection needle; The quantity of lower cover glass is at least 9, each time cover glass determining deviation of being separated by is fixed on and on slide, forms the microchannel mutually connecting, upper cover glass covers the microchannel of described lower cover glass formation and is fixed on lower cover glass, the inlet of microchannel is eight, in collecting pipe, be provided with expansion chamber, the liquid outlet of microchannel is one; The quantity of injection needle is identical with the quantity of microchannel inlet, is separately fixed at the inlet place of microchannel, and the liquid outlet place of microchannel is fixed with efferent duct (construction method of described microfluidic device is referring to CN 102626602A).
The structure of the microfluidic device with two droplet generators that the present invention adopts as shown in Figure 2, the schematic diagram that in its microchannel and microchannel, emulsion droplet is sprawled as shown in Figure 3, the first microchannel, the second microchannel and the 3rd microchannel form two-stage droplet generator, and the 4th microchannel and the 5th microchannel form single-stage droplet generator.
The present invention has following beneficial effect:
1, liquid-soaked of the present invention causes the method that different drops merge, and has solved in microreactor and has had the susceptible to plugging problem in microchannel while generating that precipitates, and can produce continuously, is convenient to realize industrialization.
2, liquid-soaked of the present invention causes the method that different drops merge; for having, the stable drop system of surfactant is applicable equally; and can effectively protect the active material of institute's embedding in drop; widen the range of application of existing drop integration technology, be particularly useful for the preparation field of accurate chemical analysis, organic synthesis, micron and nano material.
3, liquid-soaked of the present invention causes the method that different drops merge, and can realize mixing or micro-reaction between micro-drop, simple to operate, controllability good, and fusion process is spontaneous carrying out, without extra energy supply, energy-conserving and environment-protective.
4, liquid-soaked of the present invention causes the method that different drops merge, and uses conventional equipment to realize, cost-saving.
Accompanying drawing explanation
Fig. 1 is that in the method for the invention, drop infiltrates the principle schematic that the fusion of initiation drop realizes micro-mixing or micro-reaction;
Fig. 2 is the structural representation of the microfluidic device of the method for the invention employing;
Fig. 3 is different drop fusion process schematic diagrames in the microchannel of microfluidic device described in Fig. 2 and microchannel;
Fig. 4 has the high speed camera photo of the oil bag water-in-oil emulsion drop preparation process of thin-walled oil reservoir in the embodiment 1 of embodiment 1;
Fig. 5 is the high speed camera photo of water-in-oil emulsion drop preparation process in the embodiment 1 of embodiment 1;
Fig. 6 is that the thin-walled oil of oil bag water-in-oil emulsion drop in the embodiment 1 of embodiment 1 spreads into the high speed camera photo that merge water droplets process is caused on water droplet surface in water-in-oil emulsion drop;
Fig. 7 is that in comparative example 1, oil bag water-in-oil emulsion drop and Water-In-Oil drop expand collision in chamber but the high speed camera photo of fusion does not occur at collecting pipe;
Fig. 8 is the high speed camera photo that the thin-walled oil of oil bag water-in-oil emulsion drop in embodiment 2 spreads into the water droplet surface initiation merge water droplets process in water-in-oil emulsion drop;
Fig. 9 is the high speed camera photo that the thin-walled oil of oil bag water-in-oil emulsion drop in embodiment 3 spreads into the water droplet surface initiation merge water droplets process in water-in-oil emulsion drop;
Figure 10 is that in embodiment 4, the fusion of liquid-soaked initiation drop realizes the high speed camera photo that calcium carbonate granule is prepared in micro-reaction;
Figure 11 is the optical microscope photograph of the emulsion droplet containing calcium carbonate granule of embodiment 4 preparations;
Figure 12 is the stereoscan photograph of the calcium carbonate granule of embodiment 4 preparations;
Figure 13 is the laser confocal microscope photo of chitosan-containing microballoon in continuous phase fluid in embodiment 5;
Figure 14 is the stereoscan photograph of the chitosan microball of embodiment 5 preparations;
Figure 15 is the photo of the ESEM of the hydroapatite particles of preparation in embodiment 6 embodiments 1;
Figure 16 is the photo of the ESEM of the hydroapatite particles that in comparative example 2 prepared by precipitation polymerization method;
In figure, drop, 6-slide, 7-lower cover glass, 8-epoxide-resin glue, 9-injection needle, 10-upper cover glass, 11-efferent duct, the 12-the first microchannel, the 13-the second microchannel, the 14-the three microchannel, the 15-the four microchannel, the 16-the five microchannel, 17-collecting pipe that water droplet, the 5-fusion in the thin-walled oil reservoir of 1-oil bag water-in-oil emulsion drop, the water droplet in 2-water-in-oil emulsion drop, 3-continuous phase fluid, 4-oil bag water-in-oil emulsion drop forms.
The specific embodiment
Below by embodiment, also by reference to the accompanying drawings the method for the invention is described further.In following each embodiment, described Dow Corning 749 is the mixture of the cyclohexyl methyl siloxanes of the percentage by volume trimethicone that is 50% and percentage by volume 50%, and Dow Corning 749 is its trade name, purchased from Dow Corning company; Described Lumogen F Red 300 is Yi Zhong perylene diimide compounds, and Lumogen F Red 300 is its trade name, purchased from BASF AG; Described Pluronic F127 is the addition polymers of a kind of polypropylene glycol and oxirane, and Pluronic F127 is its trade name, purchased from Sigma company; Described medical soybean oil is injection rank, purchased from Tieling Beiya Medical Oil Co., Ltd..
Embodiment 1
In the present embodiment, liquid-soaked causes different drops and merges the method that realizes micro-mixing, and processing step is as follows:
(1) preparation disperses water, middle oil phase and continuous phase fluid
The preparation of the first disperse water phase fluid: lauryl sodium sulfate (SDS) is added deionized water for stirring evenly to form the first disperse water phase fluid under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.01:1;
The preparation of the second disperse water phase fluid: SDS, methylene blue are added deionized water for stirring evenly to form the second disperse water phase fluid under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.01: 1, and the amount of described methylene blue is 2 mg in every 1ml deionized water;
The preparation of middle oil phase fluid: will gather ricinoleic acid glyceride (PGPR 90), Lumogen F Red 300(LR300 under normal pressure, room temperature) add in medical soybean oil and stir and form middle oil phase fluid, the amount of described PGPR 90 is 0.02 g in the medical soybean oil of every 1ml, and the amount of described LR300 is 1mg in the medical soybean oil of every 1ml;
The preparation of continuous phase fluid: under normal pressure, room temperature by Dow Corning 749(DC749) formation continuous phase fluid stirs in adding dimethicone, the mass ratio of described DC749 and dimethicone is 0.01: 1, and described dimethyl-silicon oil viscosity is 10 cSt;
(2) different drops fusions realize micro-mixing
The microfluidic device adopting in the present embodiment, its structure as shown in Figure 2, comprise slide 6, upper cover glass 10, lower cover glass 7 and injection needle 9, in its microchannel and microchannel, drop fusion process schematic diagram as shown in Figure 3, the first microchannel 12, the second microchannel 13 and the 3rd microchannel 14 form two-stage droplet generator, the 4th microchannel 15 and the 5th microchannel 16 form single-stage droplet generator, the width of the first microchannel 12 is 90 μ m, the width of the second microchannel 13 is 115 μ m, the width of the 3rd microchannel 14 is 150 μ m, the width of the 4th microchannel 15 is 150 μ m, the width of the 5th microchannel 16 is 90 μ m, collecting pipe width is 200 μ m, the floor projection of the expansion chamber of collecting pipe is oval, its major axis is 1.8mm, minor axis is 600 μ m, the height of each microchannel is about 150 μ m.
The first disperse water phase fluid of step (1) preparation and continuous phase fluid are formed to monodispersed water-in-oil emulsion drop (see figure 5) by syringe injection the 4th microchannel 15 and the 5th microchannel 16 that are connected with syringe pump respectively, meanwhile the second disperse water phase fluid, middle oil phase fluid and the continuous phase fluid of step (1) preparation are injected to the first microchannel 12, the second microchannel 13 and the 3rd microchannel 14 by the syringe being connected with syringe pump respectively and form the monodispersed oil bag water-in-oil emulsion drop (see figure 4) with thin-walled oil reservoir; Formed water-in-oil emulsion drop, oil bag water-in-oil emulsion drop enter in the collecting pipe 17 of microfluidic device with continuous phase fluid, every 1 oil bag water-in-oil emulsion drop contacts in the expansion chamber of collecting pipe 17 with 1 water-in-oil emulsion drop, the thin-walled oil reservoir on oil bag water-in-oil emulsion drop surface spreads into water-in-oil emulsion drop surface, water droplet in oil bag water-in-oil emulsion drop and the thin-walled oil reservoir between the water droplet in water-in-oil emulsion drop are discharged from, and the water droplet in described two kinds of drops merges realizes micro-mixing (see figure 6);
The flow Q of described the first disperse water phase fluid a=500 μ L/h, the flow Q of the second disperse water phase fluid d=200 μ L/h, the flow Q of middle oil phase fluid b=30 μ L/h, the flow Q of continuous phase fluid in two-stage droplet generator c1=300 μ L/h, the flow Q in single-stage droplet generator c2=450 μ L/h;
(3) collect the drop after merging
By merging the emulsion droplet forming in step (2) embodiment 1, with continuous phase fluid, by the efferent duct 11 of microfluidic device, introduced in collection container.
Comparative example 1
(1) preparation disperses water, middle oil phase and continuous phase fluid
The dispersion water of preparing, middle oil phase and continuous phase fluid are identical with embodiment 1.
(2) formation of different drops
The microfluidic device adopting is identical with embodiment 1, the first disperse water phase fluid of step (1) preparation and continuous phase fluid are formed to monodispersed water-in-oil emulsion drop by syringe injection the 4th microchannel 15 and the 5th microchannel 16 that are connected with syringe pump respectively, meanwhile by the second disperse water phase fluid of step (1) preparation, middle oil phase fluid and continuous phase fluid inject the first microchannel 12 by the syringe being connected with syringe pump respectively, in the second microchannel 13 and the 3rd microchannel 14, form the monodispersed oil bag water-in-oil emulsion drop with thin-walled oil reservoir, flow Q when the first disperse water phase fluid a=500 μ L/h, the flow Q of the second disperse water phase fluid d=200 μ L/h, the flow Q of middle oil phase fluid b=0 μ L/h, the flow Q of continuous phase fluid in two-stage droplet generator c1=300 μ L/h, the flow Q in single-stage droplet generator c2during=450 μ L/h, formed water-in-oil emulsion drop, oil bag water-in-oil emulsion drop enter in the collecting pipe 17 of microfluidic device with continuous phase fluid, when in described water-in-oil emulsion drop, the expansion chamber of oil bag water-in-oil emulsion drop in collecting pipe 17, collision contacts, the water droplet in two drops does not merge realizes micro-mixing (see figure 7).
Embodiment 2
In the present embodiment, liquid-soaked causes different drops and merges the method that realizes micro-mixing, and processing step is as follows:
(1) preparation disperses water, middle oil phase and continuous phase fluid
The preparation of the first disperse water phase fluid: SDS is added deionized water for stirring evenly to form the first disperse water phase fluid under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.005:1;
The preparation of the second disperse water phase fluid: SDS is added deionized water for stirring evenly to form the second disperse water phase fluid under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.01: 1;
The preparation of middle oil phase fluid: under normal pressure, room temperature, PGPR 90 is added in medical soybean oil and stir and form middle oil phase fluid, the amount of described PGPR 90 is 0.01 g in the medical soybean oil of every 1ml;
The preparation of continuous phase fluid: the formation continuous phase fluid that stirs in DC749 being added to dimethicone under normal pressure, room temperature, the mass ratio of described DC749 and dimethicone is 0.005: 1, described dimethyl-silicon oil viscosity is 10 cSt;
(2) different drops fusions realize micro-mixing
The microfluidic device that the present embodiment adopts is identical with embodiment 1.
The first disperse water phase fluid of step (1) preparation and continuous phase fluid are formed to monodispersed water-in-oil emulsion drop by syringe injection the 4th microchannel 15 and the 5th microchannel 16 that are connected with syringe pump respectively, meanwhile the second disperse water phase fluid, middle oil phase fluid and the continuous phase fluid of step (1) preparation are injected to the first microchannel 12, the second microchannel 13 and the 3rd microchannel 14 by the syringe being connected with syringe pump respectively and form the monodispersed oil bag water-in-oil emulsion drop with thin-walled oil reservoir; Formed water-in-oil emulsion drop, oil bag water-in-oil emulsion drop enter with continuous phase fluid in the collecting pipe of microfluidic device, as the flow Q of the first disperse water phase fluid a=400 μ L/h, the flow Q of the second disperse water phase fluid d=300 μ L/h, the flow Q of middle oil phase fluid b=20 μ L/h, the flow Q of continuous phase fluid in two-stage droplet generator c1=300 μ L/h, the flow Q in single-stage droplet generator c2during=400 μ L/h, every 1 oil bag water-in-oil emulsion drop contacts in the expansion chamber of collecting pipe 17 with 1 water-in-oil emulsion drop, the thin-walled oil reservoir on oil bag water-in-oil emulsion drop surface spreads into water-in-oil emulsion drop surface, water droplet in oil bag water-in-oil emulsion drop and the thin-walled oil reservoir between the water droplet in water-in-oil emulsion drop are discharged from, and the water droplet in described two kinds of drops merges realizes micro-mixing (see figure 8);
(3) collect the drop after merging
By merging the emulsion droplet forming in step (2), with continuous phase fluid, by the efferent duct 11 of microfluidic device, introduced in collection container.
Embodiment 3
In the present embodiment, liquid-soaked causes different drops and merges the method that realizes micro-mixing, and processing step is as follows:
(1) preparation disperses water, middle oil phase and continuous phase fluid
The preparation of the first disperse water phase fluid: SDS is added deionized water for stirring evenly to form the first disperse water phase fluid under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.01:1;
The preparation of the second disperse water phase fluid: SDS is added deionized water for stirring evenly to form the second disperse water phase fluid under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.005: 1;
The preparation of middle oil phase fluid: under normal pressure, room temperature, PGPR 90 is added in medical soybean oil and stir and form middle oil phase fluid, the amount of described PGPR 90 is 0.04 g in the medical soybean oil of every 1ml;
The preparation of continuous phase fluid: the formation continuous phase fluid that stirs in DC749 being added to dimethicone under normal pressure, room temperature, the mass ratio of described DC749 and dimethicone is 0.01: 1, described dimethyl-silicon oil viscosity is 10 cSt;
(2) different drops fusions realize micro-mixing
The microfluidic device that the present embodiment adopts is identical with embodiment 1.
The first disperse water phase fluid of step (1) preparation and continuous phase fluid are formed to monodispersed water-in-oil emulsion drop by syringe injection the 4th microchannel 15 and the 5th microchannel 16 that are connected with syringe pump respectively, meanwhile the second disperse water phase fluid, middle oil phase fluid and the continuous phase fluid of step (1) preparation are injected to the first microchannel 12, the second microchannel 13 and the 3rd microchannel 14 by the syringe being connected with syringe pump respectively and form the monodispersed oil bag water-in-oil emulsion drop with thin-walled oil reservoir; Formed water-in-oil emulsion drop, oil bag water-in-oil emulsion drop enter with continuous phase fluid in the collecting pipe of microfluidic device, as the flow Q of the first disperse water phase fluid a=450 μ L/h, the flow Q of the second disperse water phase fluid d=350 μ L/h, the flow Q of middle oil phase fluid b=20 μ L/h, the flow Q of continuous phase fluid in two-stage droplet generator c1=300 μ L/h, the flow Q in single-stage droplet generator c2during=400 μ L/h, every 1 oil bag water-in-oil emulsion drop contacts in the expansion chamber of collecting pipe with 1 water-in-oil emulsion drop, the thin-walled oil reservoir on oil bag water-in-oil emulsion drop surface spreads into water-in-oil emulsion drop surface, water droplet in oil bag water-in-oil emulsion drop and the thin-walled oil reservoir between the water droplet in water-in-oil emulsion drop are discharged from, and the water droplet in described two kinds of drops merges realizes micro-mixing (see figure 9);
(3) collect the drop after merging
By merging the emulsion droplet forming in step (2), with continuous phase fluid, by the efferent duct 11 of microfluidic device, introduced in collection container.
Embodiment 4
In the present embodiment, utilize liquid-soaked to cause different drops and merge and realize micro-reaction and prepare nano-calcium carbonate particles, processing step is as follows:
(1) preparation is containing the middle oil phase of disperse water phase fluid, preparation and the continuous phase fluid of reactant
The preparation of the disperse water phase fluid of chloride containing calcium: Pluronic F127, calcium chloride are added deionized water for stirring evenly to form the disperse water phase fluid of chloride containing calcium under normal pressure, room temperature, the mass ratio of described Pluronic F127 and deionized water is 0.005:1, and the concentration of described calcium chloride in deionized water is 0.2 mol/L;
Contain the preparation of the disperse water phase fluid of sodium carbonate: SDS, sodium carbonate are added deionized water for stirring evenly to form the disperse water phase fluid containing sodium carbonate under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.005: 1, and the concentration of described sodium carbonate in deionized water is 0.2mol/L;
The preparation of middle oil phase fluid: under normal pressure, room temperature, PGPR 90, LR300 are added in medical soybean oil and stir and form middle oil phase fluid, the amount of described PGPR 90 is 0.04 g in the medical soybean oil of every 1ml, and the amount of described LR300 is 1mg in the medical soybean oil of every 1ml;
The preparation of continuous phase fluid: the formation continuous phase fluid that stirs in DC749 being added to dimethicone under normal pressure, room temperature, the mass ratio of described DC749 and dimethicone is 0.005: 1, described dimethyl-silicon oil viscosity is 10 cSt;
(2) drop merges and causes micro-reaction
The microfluidic device that the present embodiment adopts is identical with embodiment 1.
The disperse water phase fluid containing sodium carbonate of step (1) preparation and continuous phase fluid are formed to the monodispersed water-in-oil emulsion drop containing sodium carbonate by the 5th microchannel 16 and the 4th microchannel 15 of the syringe pump injection microfluidic device being connected with syringe respectively, meanwhile by the disperse water phase fluid of the chloride containing calcium of step (1) preparation, middle oil phase fluid and continuous phase fluid are injected respectively the first microchannel 12 of microfluidic device by the syringe pump being connected with syringe, in the second microchannel 13 and the 3rd microchannel 14, form the monodispersed oil bag water-in-oil emulsion drop with the chloride containing calcium of thin-walled oil reservoir, describedly containing the water-in-oil emulsion drop of sodium carbonate and the oil bag water-in-oil emulsion drop of chloride containing calcium, with continuous phase fluid, enter in the collecting pipe of microfluidic device, flow Q when the disperse water phase fluid of chloride containing calcium a=600 μ L/h, containing the flow Q of the disperse water phase fluid of sodium carbonate d=350 μ L/h, the flow Q of middle oil phase fluid b=40 μ L/h, the flow Q of continuous phase fluid in two-stage droplet generator c1=300 μ L/h, the flow Q in single-stage droplet generator c2during=300 μ L/h, the oil bag water-in-oil emulsion drop of every 1 chloride containing calcium contacts in the expansion chamber of collecting pipe 17 with 1 water-in-oil emulsion drop containing sodium carbonate, the thin-walled oil reservoir on the oil bag water-in-oil emulsion drop surface of chloride containing calcium spreads into the water-in-oil emulsion drop surface containing sodium carbonate, water droplet in the oil bag water-in-oil emulsion drop of chloride containing calcium and the thin-walled oil reservoir containing between the water droplet in the water-in-oil emulsion drop of sodium carbonate are discharged from, described water droplet completes calcium chloride and reacts with the micro-of sodium carbonate in the process of micro-mixing, form the emulsion droplet (see figure 10) containing calcium carbonate granule,
(3) collect micro-product
The emulsion droplet containing calcium carbonate granule that step (2) is obtained is introduced in collection container by the efferent duct 11 of microfluidic device with continuous phase fluid, containing the optical microscope photograph of the emulsion droplet of calcium carbonate granule as shown in figure 11, to collect liquid and remove oil phase by degreaser washed with isopropyl alcohol, then with deionized water washing, remove isopropyl alcohol, after drying, as shown in figure 12, its particle diameter is 200 ~ 800 nanometers to the stereoscan photograph of gained calcium carbonate granule.
Embodiment 5
In the present embodiment, utilize liquid-soaked to cause different drops and merge and realize micro-reaction and prepare chitosan microball, processing step is as follows:
(1) preparation is containing the middle oil phase of disperse water phase fluid, preparation and the continuous phase fluid of reactant
The preparation of the disperse water phase fluid of chitosan-containing: the water soluble chitosan that is 5000 by Pluronic F127, weight average molecular weight under normal pressure, room temperature adds deionized water for stirring evenly to form mixed liquor, then to adding concentration in described mixed liquor, be that the sodium hydrate aqueous solution of 1 mol/L regulates its pH value to 6.7, obtain the disperse water phase fluid of chitosan-containing; The mass ratio of described Pluronic F127 and deionized water is that the mass ratio of 0.01:1, water soluble chitosan and deionized water is 0.02:1;
Preparation containing the disperse water phase fluid of phthalaldehyde: SDS, terephthalaldehyde are added deionized water for stirring evenly to form the disperse water phase fluid containing phthalaldehyde under normal pressure, room temperature, the mass ratio of described SDS and deionized water is that the mass ratio of 0.005: 1, terephthalaldehyde and deionized water is 0.001:1;
The preparation of middle oil phase fluid: under normal pressure, room temperature, PGPR 90, LR300 are added in medical soybean oil and stir and form middle oil phase fluid, the amount of described PGPR 90 is 0.01 g in the medical soybean oil of every 1ml, and the amount of described LR300 is 1mg in the medical soybean oil of every 1ml;
The preparation of continuous phase fluid: the formation continuous phase fluid that stirs in DC749 being added to dimethicone under normal pressure, room temperature, the mass ratio of described DC749 and dimethicone is 0.01: 1, described dimethyl-silicon oil viscosity is 10 cSt;
(2) drop merges and causes micro-reaction
The microfluidic device that the present embodiment adopts is identical with embodiment 1.
The disperse water phase fluid containing terephthalaldehyde of step (1) preparation and continuous phase fluid are formed to monodispersed single water-in-oil emulsion drop that disperses containing terephthalaldehyde by the 5th microchannel 16 and the 4th microchannel 15 of the syringe pump injection microfluidic device being connected with syringe respectively, meanwhile by the disperse water phase fluid of the chitosan-containing of step (1) preparation, middle oil phase fluid and continuous phase fluid are injected respectively the first microchannel 12 of microfluidic device by the syringe pump by being connected with syringe, in the second microchannel 13 and the 3rd microchannel 14, form the monodispersed oil bag water-in-oil emulsion drop with the chitosan-containing of thin-walled oil reservoir, described water-in-oil emulsion drop enters with continuous phase fluid in the collecting pipe 17 of microfluidic device with oil bag water-in-oil emulsion drop, flow Q when the disperse water phase fluid of chitosan-containing a=400 μ L/h, containing the flow Q of the disperse water phase fluid of terephthalaldehyde d=300 μ L/h, the flow Q of middle oil phase fluid b=20 μ L/h, the flow Q of continuous phase fluid in two-stage droplet generator c1=300 μ L/h, the flow Q in single-stage droplet generator c2during=400 μ L/h, the oil bag water-in-oil emulsion drop of every 1 chitosan-containing contacts in the expansion chamber of collecting pipe 17 with 1 water-in-oil emulsion drop containing terephthalaldehyde, the thin-walled oil reservoir on the oil bag water-in-oil emulsion drop surface of chitosan-containing spreads into the water-in-oil emulsion drop surface containing terephthalaldehyde, water droplet in the oil bag water-in-oil emulsion drop of chitosan-containing and the thin-walled oil reservoir containing between the water droplet in the water-in-oil emulsion drop of terephthalaldehyde are discharged from, described water droplet completes shitosan and reacts with the micro-of terephthalaldehyde in the process of micro-mixing, form chitosan microball,
(3) collect micro-product
The chitosan microball that step (2) is obtained is introduced in collection container by the efferent duct 11 of microfluidic device with continuous phase fluid, the optical microscope photograph of chitosan microball in continuous phase fluid as shown in figure 13, to collect liquid and remove oil phase by degreaser washed with isopropyl alcohol, then with deionized water washing, remove isopropyl alcohol, after drying, as shown in figure 14, this chitosan microball has good sphericity to the stereoscan photograph of gained chitosan microball.
Embodiment 6
In the present embodiment, utilize liquid-soaked to cause different drops and merge and realize micro-reaction and prepare micron order hydroapatite particles, processing step is as follows:
(1) preparation is containing the middle oil phase of disperse water phase fluid, preparation and the continuous phase fluid of reactant
Preparation containing the disperse water phase fluid of calcium nitrate and phosphoric acid: under normal pressure, room temperature by Pluronic F127, calcium nitrate tetrahydrate, phosphoric acid (purity: 85%) add deionized water for stirring evenly to form the disperse water phase fluid containing calcium nitrate and phosphoric acid; The mass ratio of described Pluronic F127 and deionized water is 0.005:1, and the concentration of described calcium nitrate is 1 mol/L, and the concentration of described phosphoric acid is 0.7 mol/L;
Preparation containing the disperse water phase fluid of ammonium hydroxide: under normal pressure, room temperature by SDS, ammonium hydroxide (NH 4oH, 25 wt.%) add deionized water for stirring evenly to form the disperse water phase fluid containing ammonium hydroxide, the mass ratio of described SDS and deionized water is 0.005: 1, the volumetric concentration of described ammonium hydroxide is 0.01 mL/L;
The preparation of middle oil phase fluid: under normal pressure, room temperature, PGPR 90, LR300 are added in medical soybean oil and stir and form middle oil phase fluid, the amount of described PGPR 90 is 0.01 g in the medical soybean oil of every 1ml, and the amount of described LR300 is 1mg in the medical soybean oil of every 1ml;
The preparation of continuous phase fluid: the formation continuous phase fluid that stirs in DC749 being added to dimethicone under normal pressure, room temperature, the mass ratio of described DC749 and dimethicone is 0.01: 1, described dimethyl-silicon oil viscosity is 10 cSt;
(2) drop merges and causes micro-reaction
The microfluidic device adopting in the present embodiment is identical with embodiment 1.
The disperse water phase fluid containing ammonium hydroxide of step (1) preparation and continuous phase fluid are formed to the monodispersed water-in-oil emulsion drop containing ammonium hydroxide by the 5th microchannel 16 and the 4th microchannel 15 of the syringe pump injection microfluidic device being connected with syringe respectively, meanwhile by the disperse water phase fluid containing calcium nitrate and phosphoric acid of step (1) preparation, middle oil phase fluid and continuous phase fluid are injected respectively the first microchannel 12 of microfluidic device by the syringe pump by being connected with syringe, in the second microchannel 13 and the 3rd microchannel 14, form monodispersed have thin-walled oil reservoir containing calcium nitrate and phosphoric acid oil bag water-in-oil emulsion drop, formed water-in-oil emulsion drop enters in the collecting pipe of microfluidic device with oil bag water-in-oil emulsion drop with continuous phase fluid, flow Q when the disperse water phase fluid containing calcium nitrate and phosphoric acid a=500 μ L/h, containing the flow Q of the disperse water phase fluid of ammonium hydroxide d=500 μ L/h, the flow Q of middle oil phase fluid b=80 μ L/h, the flow Q of continuous phase fluid in two-stage droplet generator c1=400 μ L/h, the flow Q in single-stage droplet generator c2during=500 μ L/h, every 1 oil bag water-in-oil emulsion drop containing calcium nitrate and phosphoric acid contacts in the expansion chamber of collecting pipe 17 with 1 water-in-oil emulsion drop containing ammonium hydroxide, the thin-walled oil reservoir that contains the oil bag water-in-oil emulsion drop surface of calcium nitrate and phosphoric acid spreads into the water-in-oil emulsion drop surface containing ammonium hydroxide, containing the water droplet in the oil bag water-in-oil emulsion drop of calcium nitrate and phosphoric acid and containing the thin-walled oil reservoir between the water droplet in the water-in-oil emulsion drop of ammonium hydroxide, be discharged from, described water droplet completes existing calcium nitrate in the process of micro-mixing, phosphoric acid reacts with the micro-of ammonium hydroxide, form the emulsion droplet of hydroxyl apatite particle,
(3) collect micro-product
The emulsion droplet of the hydroxyl apatite particle that step (2) is obtained is introduced in collection container by the efferent duct 11 of microfluidic device with continuous phase fluid, to collect liquid and remove oil phase by degreaser washed with isopropyl alcohol, then with deionized water washing, remove isopropyl alcohol, after drying, the stereoscan photograph of gained hydroapatite particles as shown in figure 15, the particle diameter of the hydroapatite particles that as shown in Figure 15 prepared by the method is 10 microns of left and right, uniform particles, and there is flower-like structure.
Comparative example 2: precipitation polymerization method is prepared hydroapatite particles
Disperse water phase fluid 10 mL containing calcium nitrate and phosphoric acid of step (1) preparation in embodiment 6 added in the beaker of 50 mL and stir by the mixing speed with 120r/min on magnetic stirring apparatus, then with glue head dropper, in described beaker, drip disperse water phase fluid 10 mL containing ammonium hydroxide that step in embodiment 6 (1) is prepared, keep aforementioned mixing speed continue to stir standing 2 h after 1 h, isolate gained precipitate with deionized water cyclic washing 5 times to remove unreacted material, after drying, the stereoscan photograph of gained hydroxyapatite powder as shown in figure 16, the hydroxyapatite powder particle that as shown in Figure 16 prepared by precipitation polymerization method is inhomogeneous, and loosely organized.

Claims (9)

1. liquid-soaked causes the method that drop merges, and it is characterized in that processing step is as follows:
(1) preparation disperses water, middle oil phase and continuous phase fluid
The preparation of the first disperse water phase fluid: water soluble emulsifier is added deionized water for stirring evenly to form the first disperse water phase fluid under normal pressure, room temperature, the mass ratio of described water soluble emulsifier and deionized water is 0.005 ~ 0.01:1;
The preparation of the second disperse water phase fluid: water soluble emulsifier is added deionized water for stirring evenly to form the second disperse water phase fluid under normal pressure, room temperature, the mass ratio of described water soluble emulsifier and deionized water is 0.005 ~ 0.01: 1;
The preparation of middle oil phase fluid: stir in oil soluble emulsifying agent being added to soybean oil under normal pressure, room temperature and form middle oil phase fluid, the amount of described oil soluble emulsifying agent is 0.01 ~ 0.04 g in every 1ml soybean oil;
The preparation of continuous phase fluid: the formation continuous phase fluid that stirs in surfactant being added to dimethicone under normal pressure, room temperature, the mass ratio of described surfactant and dimethicone is 0.005 ~ 0.01: 1;
(2) drop fusion realizes micro-mixing
The different inlets of the single-stage droplet generator that the second disperse water phase fluid that step (1) is prepared and continuous phase fluid inject respectively microfluidic device form monodispersed water-in-oil emulsion drop, and the different inlets that meanwhile the first disperse water phase fluid, middle oil phase fluid and the continuous phase fluid of step (1) preparation injected respectively to the two-stage droplet generator of microfluidic device form monodispersed oil bag water-in-oil emulsion drop; Formed water-in-oil emulsion drop, oil bag water-in-oil emulsion drop enter in the collecting pipe of microfluidic device with continuous phase fluid, while contacting in the expansion chamber at described collecting pipe when water-in-oil emulsion drop and oily bag water-in-oil emulsion drop, the oil reservoir on oil bag water-in-oil emulsion drop surface spreads into water-in-oil emulsion drop surface, water droplet in oil bag water-in-oil emulsion drop and the oil reservoir between the water droplet in water-in-oil emulsion drop are discharged from, and the water droplet in described two kinds of drops merges realizes micro-mixing;
Flow (the Q of described the first disperse water phase fluid a) be 400 ~ 600 μ L/h, the flow (Q of the second disperse water phase fluid d) be 200 ~ 500 μ L/h, the flow (Q of middle oil phase fluid b) be 20 ~ 80 μ L/h, the flow (Q of continuous phase fluid in described two-stage droplet generator c1) be 300 ~ 400 μ L/h, the flow (Q of continuous phase fluid in described single-stage droplet generator c2) be 300 ~ 500 μ L/h;
(3) collect the drop after merging
By merging the emulsion droplet forming in step (2), with continuous phase fluid, by the efferent duct of microfluidic device, introduced in collection container.
2. liquid-soaked causes the method that drop merges according to claim 1, it is characterized in that described water soluble emulsifier is the addition polymers of lauryl sodium sulfate or polypropylene glycol and oxirane.
3. liquid-soaked causes the method that drop merges according to claim 1, it is characterized in that described oil soluble emulsifying agent is for the condensation product of poly-ricinoleic acid glyceride or alkyl phenol and oxirane.
4. liquid-soaked causes the method that drop merges according to claim 1, it is characterized in that described surfactant is the mixture that trimethicone and cyclohexyl methyl siloxanes form, and the volume ratio of trimethicone and cyclohexyl methyl siloxanes is 1: 1.
5. according to liquid-soaked described in arbitrary claim in claim 1 to 4, cause the method that drop merges, it is characterized in that also containing water-soluble dye in described the second disperse water phase fluid; In described middle oil phase fluid, can also contain oil-soluble dyes.
6. according to liquid-soaked described in arbitrary claim in claim 1 to 4, cause the method that drop merges, it is characterized in that also containing the first reactant in described the first disperse water phase fluid; Described second disperses also to contain the second reactant in water; Water droplet in oil bag water-in-oil emulsion drop completes the first reactant with the water droplet in water-in-oil emulsion drop and reacts with the micro-of the second reactant in micro-process of mixing.
7. liquid-soaked causes the method that drop merges according to claim 5, it is characterized in that also containing the first reactant in described the first disperse water phase fluid; Described second disperses also to contain the second reactant in water; Water droplet in oil bag water-in-oil emulsion drop completes the first reactant with the water droplet in water-in-oil emulsion drop and reacts with the micro-of the second reactant in micro-process of mixing.
8. liquid-soaked causes the method that drop merges according to claim 6, it is characterized in that described the first reactant and the second reactant are water-soluble substances.
9. liquid-soaked causes the method that drop merges according to claim 7, it is characterized in that described the first reactant and the second reactant are water-soluble substances.
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