CN103240042A - Method for initiating droplet fusion by liquid infiltration - Google Patents
Method for initiating droplet fusion by liquid infiltration Download PDFInfo
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- CN103240042A CN103240042A CN2013101693915A CN201310169391A CN103240042A CN 103240042 A CN103240042 A CN 103240042A CN 2013101693915 A CN2013101693915 A CN 2013101693915A CN 201310169391 A CN201310169391 A CN 201310169391A CN 103240042 A CN103240042 A CN 103240042A
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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
Technical field
The invention belongs to drop and merge the field, particularly utilize the different single dispersant liquid drops of liquid-soaked initiation to merge the method that realizes little mixing or little reaction in a kind of microchannel.
Background technology
Microreactor is a kind of micro-scale reaction vessels of passing through the mixing realization response process of control trace reagent in the microchannel.Reaction vessel (as flask etc.) than routine, microreactor has higher specific area, as: the specific area that width is the microreactor passage of 100 μ m approximately is 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, little reaction is few to the demand of reagent, and is pollution-free substantially, 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.Though microreactor has above-mentioned advantage and wide application prospect, but the microreactor system build the cost height, flexibility is lower, and be difficult to effectively solve the problems such as obstruction of device microchannel when having precipitation to generate, this has limited the application of microreactor to a certain extent.One of effective ways that address this problem are to utilize the drop of motion as carrier in the microchannel, little mixing or little reaction between the material of realizing comprising in the drop by the fusion between different drops.Because the drop in the microchannel is in flow regime with continuous phase fluid, comprises whole little mixing and little course of reaction always, thereby can avoid the microchannel to stop up.
At present in the microchannel of report the fusion of drop to realize that the method for little mixing or little 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 that enlarges, flow velocity reduces, and mutual extrusion causes drop to merge the little mixing of realization or little reaction between drop.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 the microchannel, and this method is difficult to realize the fusion between the stable drop of surfactant, thereby its range of application is restricted.(2) wellability of change microfluidic device collecting pipe wall, design a slice hydrophilic region in hydrophobic collecting pipe for example, when two water drops are flowed through this hydrophilic region simultaneously, all can breakdown of emulsion and be attached at and collect on the tube wall, and then be sheared into drop, realize little mixing or little reaction.This method only is applicable to does not have the system that precipitation generates, if there is precipitation to generate in the emulsion droplet fusion process, precipitation will be adsorbed in together with drop and collect on the 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 the drop band, take place when charged drop collides in passage to merge and realize little mixing or little reaction.This 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, only is applicable to electrifiable system, and extra electric field may cause damage to the active material that comprises in the drop.
Summary of the invention
The objective 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 little mixing or little reaction, this method not only can realize the fusion between the stable drop of surfactant, and can avoid that the obstruction that precipitates microchannel when generating is arranged in the microreactor.
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: under normal pressure, room temperature water soluble emulsifier is added deionized water for stirring and evenly form the first disperse water phase fluid, 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: under normal pressure, room temperature water soluble emulsifier is added deionized water for stirring and evenly form the second disperse water phase fluid, the mass ratio of described water soluble emulsifier and deionized water is 0.005 ~ 0.01: 1;
The preparation of middle oil phase fluid: under normal pressure, room temperature oil soluble emulsifying agent is added the middle oil phase fluid of the formation that stirs in the soybean oil, 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: under normal pressure, room temperature surfactant is added the formation continuous phase fluid that stirs in the dimethicone, the mass ratio of described surfactant and dimethicone is 0.005 ~ 0.01: 1;
(2) drop merges the little mixing of realization
The second disperse water phase fluid of step (1) preparation is formed monodispersed water-in-oil emulsion drop with the different inlets that continuous phase fluid injects the single-stage droplet generator of microfluidic device respectively, meanwhile the first disperse water phase fluid, middle oil phase fluid and the continuous phase fluid of step (1) preparation injected the monodispersed oil bag of the different inlets formation water-in-oil emulsion drop of the two-stage droplet generator of microfluidic device respectively; 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, when 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 namely spreads into water-in-oil emulsion drop surface, water droplet in the oil bag water-in-oil emulsion drop and the oil reservoir between the water droplet in the water-in-oil emulsion drop are discharged from, and the water droplet in described two kinds of drops namely merges realizes little mixing;
Flow (the Q of the described 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 the described two-stage droplet generator
C1) be the flow (Q of continuous phase fluid in 300 ~ 400 μ L/h, the single-stage droplet generator
C2) be 300 ~ 500 μ L/h;
(3) collect the drop that merges formation
Introduced in the collection container by the efferent duct of microfluidic device with continuous phase fluid merging the emulsion droplet that forms in the step (2).
In the 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 the said method, described oil soluble emulsifying agent is the condensation product of poly-ricinoleic acid glyceride or alkyl phenol and oxirane.
In the said method, described surfactant is the mixture (Dow Corning 749) that trimethicone and cyclohexyl methyl siloxanes are formed, and the volume ratio of trimethicone and cyclohexyl methyl siloxanes is 1: 1.
In the said method, also contain water-soluble dye in the described second disperse water phase fluid, also contain oil-soluble dyes in the described middle oil phase fluid; 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 for use methylene blue as water-soluble dye to be, Lumogen F Red 300 is as oil-soluble dyes.
In the said method, also contain first reactant in the described first disperse water phase fluid, described second disperses aqueous phase also to contain second reactant, and the amount of described first reactant, second reactant is determined according to concrete chemical reaction; Water droplet in the oil bag water-in-oil emulsion drop and the water droplet in the water-in-oil emulsion drop are finished little reaction of first reactant and second reactant in little process of mixing, form little product or contain the emulsion droplet of little product, little product or the drop that contains little product are introduced in the collection container by the efferent duct of microfluidic device with continuous phase fluid, to collect liquid and remove oil phase with the degreaser washing, spend deionised water then and remove finish, continue after be drying to obtain little product.
In the said method, described first reactant and second reactant are water miscible material.
Liquid-soaked of the present invention causes different drops fusions and realizes that the mechanism of little mixing or little reaction is as follows: the thin-walled oil reservoir 1 of oil bag water-in-oil emulsion drop and the spreading coefficient of water droplet 2 in continuous phase fluid 3 in the water-in-oil emulsion drop are S
1=γ
23-(α γ
13+ γ
12), γ
IjBe the i phase interfacial tension (i ≠ j=1,2,3) alternate with j,
, R
1And R
2Be respectively the radius of the water droplet in oil bag water-in-oil emulsion drop and the water-in-oil emulsion drop, work as S
1＞0 o'clock, the thin-walled oil reservoir 1 of oil bag water-in-oil emulsion drop will soak into and spread into the water-in-oil emulsion drop
The surface of middle water droplet 2, water droplet 4 in the oil bag water-in-oil emulsion drop and the thin-walled oil reservoir between the water droplet 2 in the water-in-oil emulsion drop are discharged from, and the water droplet 2 in the water-in-oil emulsion drop contacts with the oily water droplet 4 that wraps in the water-in-oil emulsion drop to cause to merge realizes that little mixing or little reaction formation emulsion droplet 5(see Fig. 1).Can realize emulsion droplet merge with as the volume of the thin-walled oil reservoir of soakage layer and relevant by the size of infiltration drop, soaked into the drop surface when soakage layer spreads into fully, the liquid film between the drop of soakage layer institute embedding and the quilt infiltration drop is discharged fully namely causes the emulsion droplet fusion; If soakage layer is too thick or it is too little to be soaked into drop, after soakage layer spread into fully and soaked into the drop surface, the drop of soakage layer institute embedding and quilt soak into was still had soakage layer to exist between the drop, just two drops can not contact, can't realize merging.
Of the present inventionly can use various types of microfluidic devices, as PDMS device and capillary glass tube device etc., used microfluidic device has the droplet generator of a two-stage and droplet generator and public collecting pipe that contacts fusion for drop of a single-stage; The water-in-oil emulsion drop of the oil bag water-in-oil emulsion drop of the thin-walled of two-stage droplet generator preparation and the preparation of the single-stage droplet generator public collecting pipe of flowing through simultaneously, the thin-walled oil reservoir by oil bag water-in-oil emulsion drop in collecting pipe merges the water component that the infiltration of water-in-oil emulsion drop causes them; The preferred microfluidic device that uses following structure: described microfluidic device comprises slide, last cover glass, following cover glass, injection needle; The quantity of following cover glass is at least 9, each time cover glass determining deviation of being separated by is fixed on the slide and forms the microchannel that connects mutually, last cover glass covers the microchannel of described cover glass down formation and is fixed on down on the cover glass, the inlet of microchannel is eight, be provided with the expansion chamber in the collecting pipe, 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 fixedly there is efferent duct (construction method of described microfluidic device is referring to CN 102626602A) at the liquid outlet place of microchannel.
The structure of the microfluidic device with two droplet generators that the present invention adopts as shown in Figure 2, the schematic diagram that emulsion droplet is sprawled in its microchannel and the microchannel as shown in Figure 3, first microchannel, second microchannel and the 3rd microchannel constitute the two-stage droplet generator, and the 4th microchannel and the 5th microchannel constitute the 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 the susceptible to plugging problem in microchannel when having precipitation to generate in the microreactor, can produce continuously, is convenient to realize industrialization.
2, liquid-soaked of the present invention causes the method that different drops merge; the stable drop system of surfactant is suitable equally for having; and can protect the active material of institute's embedding in the drop effectively; widen the range of application of existing drop integration technology, be particularly useful for the preparation field of exact 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 little reaction between little drop, and is simple to operate, controllability good, and fusion process is spontaneous carrying out, and need not 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, saves cost.
Description of drawings
Fig. 1 is that drop soaks into the principle schematic that causes the drop fusion little mixing of realization or little reaction in the method for the invention;
Fig. 2 is the structural representation of the microfluidic device of the method for the invention employing;
Fig. 3 is microchannel and the interior different drop fusion process schematic diagrames of microchannel of the described microfluidic device of Fig. 2;
Fig. 4 is the high speed camera photo that has 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 the merge water droplets process is caused on water droplet surface in the water-in-oil emulsion drop;
Fig. 7 is that oil bag water-in-oil emulsion drop and Water-In-Oil drop enlarge collision in the chamber at collecting pipe but the high speed camera photo of fusion takes place in the Comparative Examples 1;
Fig. 8 is the high speed camera photo that the thin-walled oil of oil bag water-in-oil emulsion drop among the embodiment 2 spreads into the water droplet surface initiation merge water droplets process in the 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 among the embodiment 3 spreads into the water droplet surface initiation merge water droplets process in the water-in-oil emulsion drop;
Figure 10 is that liquid-soaked causes the high speed camera photo that drop merges the little prepared in reaction calcium carbonate granule of realization among the embodiment 4;
Figure 11 is the optical microscope photograph of the emulsion droplet that contains 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 among the 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 of precipitation polymerization method preparation in the Comparative Examples 2;
Among the figure, the drop of water droplet, 5-the fusions formation 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, the 4-oil bag water-in-oil emulsion drop, 6-slide, 7-following cover glass, 8-epoxide-resin glue, 9-injection needle, 10-upward cover glass, 11-efferent duct, 12-the first microchannel, 13-the second microchannel, 14-the three microchannel, 15-the four microchannel, 16-the five microchannel, 17-collecting pipe.
The specific embodiment
Also by reference to the accompanying drawings the method for the invention is described further below by embodiment.Among following each embodiment, described Dow Corning 749 is the mixture of the cyclohexyl methyl siloxanes of 50% trimethicone and percentage by volume 50% for percentage by volume, and Dow Corning 749 is its trade name, available from Dow Corning company; Described Lumogen F Red 300 is Yi Zhong perylene diimide compounds, and Lumogen F Red 300 is its trade name, available 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, available from Sigma company; Described medical soybean oil is the injection rank, available from Tieling Beiya Medical Oil Co., Ltd..
Embodiment 1
In the present embodiment, liquid-soaked causes different drops and merges the method that realizes little 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: under normal pressure, room temperature lauryl sodium sulfate (SDS) is added deionized water for stirring and evenly form the first disperse water phase fluid, the mass ratio of described SDS and deionized water is 0.01:1;
The preparation of the second disperse water phase fluid: under normal pressure, room temperature, SDS, methylene blue are added deionized water for stirring and evenly form the second disperse water phase fluid, 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: under normal pressure, room temperature, will gather ricinoleic acid glyceride (PGPR 90), Lumogen F Red 300(LR300) adds the middle oil phase fluid of formation that stirs in the medical soybean oil, 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 with Dow Corning 749(DC749) add the formation continuous phase fluid that stirs in the 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 merge the little mixing of realization
The microfluidic device that adopts in the present embodiment, its structure as shown in Figure 2, comprise slide 6, last cover glass 10, following cover glass 7 and injection needle 9, drop fusion process schematic diagram as shown in Figure 3 in its microchannel and the microchannel, first microchannel 12, second microchannel 13 and the 3rd microchannel 14 constitute the two-stage droplet generator, the 4th microchannel 15 and the 5th microchannel 16 constitute the single-stage droplet generator, the width of first microchannel 12 is 90 μ m, the width of 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, the 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, and minor axis is 600 μ m, and the height of each microchannel is about 150 μ m.
With the first disperse water phase fluid of step (1) preparation and continuous phase fluid injects the 4th microchannel 15 by the syringe that is connected with syringe pump respectively and the 5th microchannel 16 forms monodispersed water-in-oil emulsion drop (see figure 5), meanwhile the second disperse water phase fluid, middle oil phase fluid and the continuous phase fluid that step (1) is prepared injects first microchannel 12, second microchannel 13 and the 3rd microchannel 14 by the syringe that is connected with syringe pump respectively and forms 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, per 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 the oil bag water-in-oil emulsion drop and the thin-walled oil reservoir between the water droplet in the water-in-oil emulsion drop are discharged from, and the water droplet in described two kinds of drops namely merges realizes little mixing (see figure 6);
The flow Q of the described 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 continuous phase fluid flow Q in the two-stage droplet generator
C1=300 μ L/h, the flow Q in the single-stage droplet generator
C2=450 μ L/h;
(3) drop after collection is merged
Introduced in the collection container by the efferent duct 11 of microfluidic device with continuous phase fluid merging the emulsion droplet that forms in step (2) embodiment 1.
Comparative Examples 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 that adopts is identical with embodiment 1, with the first disperse water phase fluid of step (1) preparation and continuous phase fluid injects the 4th microchannel 15 by the syringe that is connected with syringe pump respectively and the 5th microchannel 16 forms monodispersed water-in-oil emulsion drop, the second disperse water phase fluid that step (1) is prepared meanwhile, middle oil phase fluid and continuous phase fluid inject first microchannel 12 by the syringe that is connected with syringe pump respectively, form monodispersed oil bag water-in-oil emulsion drop with thin-walled oil reservoir in second microchannel 13 and the 3rd microchannel 14; 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 continuous phase fluid flow Q in the two-stage droplet generator
C1=300 μ L/h, the flow Q in the 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 collision contacted in described water-in-oil emulsion drop, the expansion chamber of oil bag water-in-oil emulsion drop in collecting pipe 17, the water droplet in two drops does not merge realized little mixing (see figure 7).
Embodiment 2
In the present embodiment, liquid-soaked causes different drops and merges the method that realizes little 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: under normal pressure, room temperature SDS is added deionized water for stirring and evenly form the first disperse water phase fluid, the mass ratio of described SDS and deionized water is 0.005:1;
The preparation of the second disperse water phase fluid: under normal pressure, room temperature SDS is added deionized water for stirring and evenly form the second disperse water phase fluid, 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 the middle oil phase fluid of formation that stirs in the medical soybean oil, the amount of described PGPR 90 is 0.01 g in the medical soybean oil of every 1ml;
The preparation of continuous phase fluid: under normal pressure, room temperature DC749 is added the formation continuous phase fluid that stirs in the dimethicone, the mass ratio of described DC749 and dimethicone is 0.005: 1, and described dimethyl-silicon oil viscosity is 10 cSt;
(2) different drops merge the little mixing of realization
The microfluidic device that present embodiment adopts is identical with embodiment 1.
With the first disperse water phase fluid of step (1) preparation and continuous phase fluid injects the 4th microchannel 15 by the syringe that is connected with syringe pump respectively and the 5th microchannel 16 forms monodispersed water-in-oil emulsion drop, meanwhile the second disperse water phase fluid, middle oil phase fluid and the continuous phase fluid that step (1) is prepared injects first microchannel 12, second microchannel 13 and the 3rd microchannel 14 by the syringe that is connected with syringe pump respectively and forms 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 continuous phase fluid flow Q in the two-stage droplet generator
C1=300 μ L/h, the flow Q in the single-stage droplet generator
C2During=400 μ L/h, per 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 namely spreads into water-in-oil emulsion drop surface, water droplet in the oil bag water-in-oil emulsion drop and the thin-walled oil reservoir between the water droplet in the water-in-oil emulsion drop are discharged from, and the water droplet in described two kinds of drops namely merges realizes little mixing (see figure 8);
(3) drop after collection is merged
Introduced in the collection container by the efferent duct 11 of microfluidic device with continuous phase fluid merging the emulsion droplet that forms in the step (2).
Embodiment 3
In the present embodiment, liquid-soaked causes different drops and merges the method that realizes little 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: under normal pressure, room temperature SDS is added deionized water for stirring and evenly form the first disperse water phase fluid, the mass ratio of described SDS and deionized water is 0.01:1;
The preparation of the second disperse water phase fluid: under normal pressure, room temperature SDS is added deionized water for stirring and evenly form the second disperse water phase fluid, 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 the middle oil phase fluid of formation that stirs in the medical soybean oil, the amount of described PGPR 90 is 0.04 g in the medical soybean oil of every 1ml;
The preparation of continuous phase fluid: under normal pressure, room temperature DC749 is added the formation continuous phase fluid that stirs in the 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 merge the little mixing of realization
The microfluidic device that present embodiment adopts is identical with embodiment 1.
With the first disperse water phase fluid of step (1) preparation and continuous phase fluid injects the 4th microchannel 15 by the syringe that is connected with syringe pump respectively and the 5th microchannel 16 forms monodispersed water-in-oil emulsion drop, meanwhile the second disperse water phase fluid, middle oil phase fluid and the continuous phase fluid that step (1) is prepared injects first microchannel 12, second microchannel 13 and the 3rd microchannel 14 by the syringe that is connected with syringe pump respectively and forms 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 continuous phase fluid flow Q in the two-stage droplet generator
C1=300 μ L/h, the flow Q in the single-stage droplet generator
C2During=400 μ L/h, per 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 namely spreads into water-in-oil emulsion drop surface, water droplet in the oil bag water-in-oil emulsion drop and the thin-walled oil reservoir between the water droplet in the water-in-oil emulsion drop are discharged from, and the water droplet in described two kinds of drops namely merges realizes little mixing (see figure 9);
(3) drop after collection is merged
Introduced in the collection container by the efferent duct 11 of microfluidic device with continuous phase fluid merging the emulsion droplet that forms in the step (2).
Embodiment 4
In the present embodiment, utilize liquid-soaked to cause different drops and merge the little prepared in reaction nano-calcium carbonate particles of realization, processing step is as follows:
(1) preparation contains the middle oil phase of disperse water phase fluid, preparation and the continuous phase fluid of reactant
Contain the preparation of the disperse water phase fluid of calcium chloride: under normal pressure, room temperature, Pluronic F127, calcium chloride are added deionized water for stirring and evenly form the disperse water phase fluid that contains calcium chloride, 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: under normal pressure, room temperature, SDS, sodium carbonate are added deionized water for stirring and evenly form the disperse water phase fluid that contains sodium carbonate, 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 being added stirs in the medical soybean oil form in the middle of the 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: under normal pressure, room temperature DC749 is added the formation continuous phase fluid that stirs in the dimethicone, the mass ratio of described DC749 and dimethicone is 0.005: 1, and described dimethyl-silicon oil viscosity is 10 cSt;
(2) drop merges and causes little reaction
The microfluidic device that present embodiment adopts is identical with embodiment 1.
The disperse water phase fluid that contains sodium carbonate and the continuous phase fluid of step (1) preparation are formed the monodispersed water-in-oil emulsion drop that contains sodium carbonate by the 5th microchannel 16 and the 4th microchannel 15 of the syringe pump injection microfluidic device that is connected with syringe respectively, meanwhile with the disperse water phase fluid that contains calcium chloride of step (1) preparation, middle oil phase fluid and continuous phase fluid are injected first microchannel 12 of microfluidic device respectively by the syringe pump that is connected with syringe, form the monodispersed oil bag water-in-oil emulsion drop that contains calcium chloride with thin-walled oil reservoir in second microchannel 13 and the 3rd microchannel 14, the described water-in-oil emulsion drop that contains sodium carbonate enters with continuous phase fluid in the collecting pipe of microfluidic device with the oil bag water-in-oil emulsion drop that contains calcium chloride, as the flow Q of the disperse water phase fluid that contains calcium chloride
A=600 μ L/h contain 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 continuous phase fluid flow Q in the two-stage droplet generator
C1=300 μ L/h, the flow Q in the single-stage droplet generator
C2During=300 μ L/h, per 1 oil bag water-in-oil emulsion drop that contains calcium chloride contacts in the expansion chamber of collecting pipe 17 with 1 water-in-oil emulsion drop that contains sodium carbonate, the thin-walled oil reservoir that contains the oil bag water-in-oil emulsion drop surface of calcium chloride namely spreads into the water-in-oil emulsion drop surface that contains sodium carbonate, the thin-walled oil reservoir that contains the water droplet in the oil bag water-in-oil emulsion drop of calcium chloride and contain between water droplet in the water-in-oil emulsion drop of sodium carbonate is discharged from, described water droplet is finished little reaction of calcium chloride and sodium carbonate in the process of little mixing, form the emulsion droplet (see figure 10) that contains calcium carbonate granule;
(3) collect little product
The emulsion droplet that contains calcium carbonate granule that step (2) obtains is introduced in the collection container by the efferent duct 11 of microfluidic device with continuous phase fluid, contain calcium carbonate granule emulsion droplet optical microscope photograph as shown in figure 11, to collect liquid and remove oil phase with the degreaser washed with isopropyl alcohol, spend deionised water then and remove isopropyl alcohol, dry the stereoscan photograph of back gained calcium carbonate granule as shown in figure 12, its particle diameter is 200 ~ 800 nanometers.
Embodiment 5
In the present embodiment, utilize liquid-soaked to cause different drops and merge the little prepared in reaction chitosan microball of realization, processing step is as follows:
(1) preparation contains 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: under normal pressure, room temperature be that 5000 water soluble chitosan adds deionized water for stirring and evenly forms mixed liquor with Pluronic F127, weight average molecular weight, the sodium hydrate aqueous solution that adds concentration then in the described mixed liquor and be 1 mol/L is regulated its pH value to 6.7, namely gets 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;
Contain the preparation of the disperse water phase fluid of phthalaldehyde: under normal pressure, room temperature SDS, terephthalaldehyde are added deionized water for stirring and evenly form the disperse water phase fluid that contains phthalaldehyde, 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 being added stirs in the medical soybean oil form in the middle of the 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: under normal pressure, room temperature DC749 is added the formation continuous phase fluid that stirs in the dimethicone, the mass ratio of described DC749 and dimethicone is 0.01: 1, and described dimethyl-silicon oil viscosity is 10 cSt;
(2) drop merges and causes little reaction
The microfluidic device that present embodiment adopts is identical with embodiment 1.
The disperse water phase fluid that contains terephthalaldehyde and the continuous phase fluid of step (1) preparation are formed the monodispersed single water-in-oil emulsion drop that disperses that contains terephthalaldehyde by the 5th microchannel 16 and the 4th microchannel 15 of the syringe pump injection microfluidic device that is connected with syringe respectively, meanwhile with the disperse water phase fluid of the chitosan-containing of step (1) preparation, middle oil phase fluid and continuous phase fluid are respectively by first microchannel 12 that is injected microfluidic device by the syringe pump that is connected with syringe, form monodispersed oil bag water-in-oil emulsion drop with chitosan-containing of thin-walled oil reservoir in second microchannel 13 and the 3rd microchannel 14, described water-in-oil emulsion drop and oil bag water-in-oil emulsion drop enter with continuous phase fluid in the collecting pipe 17 of microfluidic device, as the flow Q of the disperse water phase fluid of chitosan-containing
A=400 μ L/h contain 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 continuous phase fluid flow Q in the two-stage droplet generator
C1=300 μ L/h, the flow Q in the single-stage droplet generator
C2During=400 μ L/h, the oil bag water-in-oil emulsion drop of per 1 chitosan-containing contacts in the expansion chamber of collecting pipe 17 with 1 water-in-oil emulsion drop that contains terephthalaldehyde, the thin-walled oil reservoir on the oil bag water-in-oil emulsion drop surface of chitosan-containing namely spreads into the water-in-oil emulsion drop surface that contains terephthalaldehyde, water droplet in the oil bag water-in-oil emulsion drop of chitosan-containing and the thin-walled oil reservoir that contains between water droplet in the water-in-oil emulsion drop of terephthalaldehyde are discharged from, described water droplet is finished little reaction of shitosan and terephthalaldehyde in the process of little mixing, form chitosan microball;
(3) collect little product
The chitosan microball that step (2) obtains is introduced in the 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 with the degreaser washed with isopropyl alcohol, spend deionised water then and remove isopropyl alcohol, dry the stereoscan photograph of back gained chitosan microball as shown in figure 14, this chitosan microball has good sphericity.
In the present embodiment, utilize liquid-soaked to cause different drops and merge the little prepared in reaction micron order hydroapatite particles of realization, processing step is as follows:
(1) preparation contains the middle oil phase of disperse water phase fluid, preparation and the continuous phase fluid of reactant
Contain the preparation of the disperse water phase fluid of calcium nitrate and phosphoric acid: (purity: 85%) the adding deionized water for stirring evenly forms the disperse water phase fluid that contains calcium nitrate and phosphoric acid with Pluronic F127, calcium nitrate tetrahydrate, phosphoric acid 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 nitrate is 1 mol/L, and described concentration of phosphoric acid is 0.7 mol/L;
Contain the preparation of the disperse water phase fluid of ammonium hydroxide: under normal pressure, room temperature with SDS, ammonium hydroxide (NH
4OH, 25 wt.%) add the even disperse water phase fluid that contains ammonium hydroxide that forms of deionized water for stirring, 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 being added stirs in the medical soybean oil form in the middle of the 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: under normal pressure, room temperature DC749 is added the formation continuous phase fluid that stirs in the dimethicone, the mass ratio of described DC749 and dimethicone is 0.01: 1, and described dimethyl-silicon oil viscosity is 10 cSt;
(2) drop merges and causes little reaction
The microfluidic device that adopts in the present embodiment is identical with embodiment 1.
The disperse water phase fluid that contains ammonium hydroxide and the continuous phase fluid of step (1) preparation are formed the monodispersed water-in-oil emulsion drop that contains ammonium hydroxide by the 5th microchannel 16 and the 4th microchannel 15 of the syringe pump injection microfluidic device that is connected with syringe respectively, meanwhile with the disperse water phase fluid that contains calcium nitrate and phosphoric acid of step (1) preparation, middle oil phase fluid and continuous phase fluid are respectively by first microchannel 12 that is injected microfluidic device by the syringe pump that is connected with syringe, form in second microchannel 13 and the 3rd microchannel 14 monodispersed have a thin-walled oil reservoir contain calcium nitrate and phosphoric acid oil bag water-in-oil emulsion drop, formed water-in-oil emulsion drop and 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 disperse water phase fluid that contains calcium nitrate and phosphoric acid
A=500 μ L/h contain 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 continuous phase fluid flow Q in the two-stage droplet generator
C1=400 μ L/h, the flow Q in the single-stage droplet generator
C2During=500 μ L/h, per 1 oil bag water-in-oil emulsion drop that contains calcium nitrate and phosphoric acid contacts in the expansion chamber of collecting pipe 17 with 1 water-in-oil emulsion drop that contains ammonium hydroxide, the thin-walled oil reservoir that contains the oil bag water-in-oil emulsion drop surface of calcium nitrate and phosphoric acid namely spreads into the water-in-oil emulsion drop surface that contains ammonium hydroxide, the thin-walled oil reservoir that contains the water droplet in the oil bag water-in-oil emulsion drop of calcium nitrate and phosphoric acid and contain between water droplet in the water-in-oil emulsion drop of ammonium hydroxide is discharged from, described water droplet is finished existing calcium nitrate in the process of little mixing, little reaction of phosphoric acid and ammonium hydroxide, the emulsion droplet of formation hydroxyl apatite particle;
(3) collect little product
The emulsion droplet of the hydroxyl apatite particle that step (2) is obtained is introduced in the collection containers by the efferent duct 11 of microfluidic device with continuous phase fluid, to collect liquid and remove oil phase with the degreaser washed with isopropyl alcohol, spend deionised water then and remove isopropyl alcohol, the stereoscan photograph of oven dry back gained hydroapatite particles as shown in figure 15, the particle diameter of the hydroapatite particles of this method preparation is about 10 microns as shown in Figure 15, uniform particles, and have flower-like structure.
Comparative Examples 2: precipitation polymerization method prepares hydroapatite particles
Disperse water phase fluid 10 mL that contain calcium nitrate and phosphoric acid of step (1) preparation among the embodiment 6 are added in the beaker of 50 mL and with the mixing speed with 120r/min on the magnetic stirring apparatus and stir, in described beaker, drip disperse water phase fluid 10 mL that contain ammonium hydroxide that step (1) is prepared among the embodiment 6 with glue head dropper then, leave standstill 2 h after keeping aforementioned mixing speed to continue to stir 1 h, isolate gained precipitate with deionized water cyclic washing 5 times to remove unreacted matters, the stereoscan photograph of oven dry back gained hydroxyapatite powder as shown in figure 16, the hydroxyapatite powder particle of precipitation polymerization method preparation is inhomogeneous as shown in Figure 16, and loosely organized.
Claims (9)
1. a 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: under normal pressure, room temperature water soluble emulsifier is added deionized water for stirring and evenly form the first disperse water phase fluid, 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: under normal pressure, room temperature water soluble emulsifier is added deionized water for stirring and evenly form the second disperse water phase fluid, the mass ratio of described water soluble emulsifier and deionized water is 0.005 ~ 0.01: 1;
The preparation of middle oil phase fluid: under normal pressure, room temperature oil soluble emulsifying agent is added the middle oil phase fluid of the formation that stirs in the soybean oil, 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: under normal pressure, room temperature surfactant is added the formation continuous phase fluid that stirs in the dimethicone, the mass ratio of described surfactant and dimethicone is 0.005 ~ 0.01: 1;
(2) drop merges the little mixing of realization
The second disperse water phase fluid of step (1) preparation is formed monodispersed water-in-oil emulsion drop with the different inlets that continuous phase fluid injects the single-stage droplet generator of microfluidic device respectively, meanwhile the first disperse water phase fluid, middle oil phase fluid and the continuous phase fluid of step (1) preparation injected the monodispersed oil bag of the different inlets formation water-in-oil emulsion drop of the two-stage droplet generator of microfluidic device respectively; 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, when 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 namely spreads into water-in-oil emulsion drop surface, water droplet in the oil bag water-in-oil emulsion drop and the oil reservoir between the water droplet in the water-in-oil emulsion drop are discharged from, and the water droplet in described two kinds of drops namely merges realizes little mixing;
Flow (the Q of the described 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 the described two-stage droplet generator
C1) be 300 ~ 400 μ L/h, the flow (Q of continuous phase fluid in the described single-stage droplet generator
C2) be 300 ~ 500 μ L/h;
(3) drop after collection is merged
Introduced in the collection container by the efferent duct of microfluidic device with continuous phase fluid merging the emulsion droplet that forms in the step (2).
2. cause the method that drop merges according to the described liquid-soaked of 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. cause the method that drop merges according to the described liquid-soaked of claim 1, it is characterized in that described oil soluble emulsifying agent is the condensation product of poly-ricinoleic acid glyceride or alkyl phenol and oxirane.
4. cause the method that drop merges according to the described liquid-soaked of claim 1, it is characterized in that described surfactant is the mixture that trimethicone and cyclohexyl methyl siloxanes are formed, the volume ratio of trimethicone and cyclohexyl methyl siloxanes is 1: 1.
5. cause the method that drop merges according to the described liquid-soaked of arbitrary claim in the claim 1 to 4, it is characterized in that also containing water-soluble dye in the described second disperse water phase fluid; Can also contain oil-soluble dyes in the oil phase fluid in the middle of described.
6. cause the method that drop merges according to the described liquid-soaked of arbitrary claim in the claim 1 to 4, it is characterized in that also containing first reactant in the described first disperse water phase fluid; Described second disperses aqueous phase also to contain second reactant; Water droplet in the oil bag water-in-oil emulsion drop and the water droplet in the water-in-oil emulsion drop are finished little reaction of first reactant and second reactant in little process of mixing.
7. cause the method that drop merges according to the described liquid-soaked of claim 5, it is characterized in that also containing first reactant in the described first disperse water phase fluid; Described second disperses aqueous phase also to contain second reactant; Water droplet in the oil bag water-in-oil emulsion drop and the water droplet in the water-in-oil emulsion drop are finished little reaction of first reactant and second reactant in little process of mixing.
8. cause the method that drop merges according to the described liquid-soaked of claim 6, it is characterized in that described first reactant and second reactant are water-soluble substances.
9. cause the method that drop merges according to the described liquid-soaked of claim 7, it is characterized in that described first reactant and second reactant are water-soluble substances.
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