CN103240043B - Preparation method of monodisperse multicomponent multiple emulsion - Google Patents

Preparation method of monodisperse multicomponent multiple emulsion Download PDF

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CN103240043B
CN103240043B CN201310169399.1A CN201310169399A CN103240043B CN 103240043 B CN103240043 B CN 103240043B CN 201310169399 A CN201310169399 A CN 201310169399A CN 103240043 B CN103240043 B CN 103240043B
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phase fluid
oil
water
drop
emulsion
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CN103240043A (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 relates to a preparation method of monodisperse multicomponent multiple emulsion. The preparation method comprises the steps as follows: (1) preparing a disperse phase fluid and a continuous phase fluid; (2) preparing monodisperse multicomponent multiple emulsion droplets by the following steps: filling the fluids prepared in the step (1) into different droplet generators of a microfluid device to form emulsion droplets, wherein the emulsion droplets formed in the different droplet generators are contacted in an expanded cavity and the emulsion droplets formed in one droplet generator are spread on the emulsion droplets formed in another droplet generator to form the multiple emulsion droplets; and (3) collecting the monodisperse multicomponent multiple emulsion.

Description

A kind of single preparation method who disperses multicomponent multiple emulsion
Technical field
The invention belongs to single multiple emulsion preparation field of disperseing, particularly a kind of microflow control technique that utilizes is prepared single method of disperseing multicomponent multiple emulsion.
Background technology
Multiple emulsion (Multiple Emulsions), claim again the emulsion in emulsion (Emulsions of Emulsions), a kind of by oil-in-water (Oil-in-Water, O/W) type and Water-In-Oil (Water-in-Oil, W/O) type emulsion are further emulsified in the compound emulsion forming in another continuous phase.The emulsion that the oil droplet that contains water droplet is formed in water by suspended dispersed is called W/O/W (W/O/W) type double emulsion, it is Water-In-Oil bag oil (O/W/O) type double emulsion that the water droplet that contains oil droplet is suspended in the emulsion forming in oil phase, is three-phase system.W/O/W type emulsion is again distributed to and in oil, forms Water-In-Oil bag Water-In-Oil (W/O/W/O) type triple emulsion, O/W/O type emulsion is again distributed to and in water, forms W/O/W bag oil (O/W/O/W) type triple emulsion.In like manner, also can form quadruple, five heavy even more multiple emulsions.Multicomponent multiple emulsion has the structure of Various Complex, can protection package be embedded in active material wherein, thereby is widely used in the fields such as the synthetic and microreactor of the embedding, drug delivery, Chemical Decomposition, template of nutriment and food additives.
At present the preparation method of the multiple emulsion of report has several as follows: (1) overall multistep emulsion process, as utilize mechanical agitation, colloid mill, the ultrasonic homogenizer etc. of involving to realize emulsification by the difference of interfacial tension between shearing force and profit two-phase.The method operation is fairly simple, can be fast the large batch of multiple emulsion of preparing also, but because the shearing force in whole system is inhomogeneous, be difficult to carry out meticulous control, the multiple emulsion particle diameter that therefore prepared by the method is distributed more widely, and is difficult to control structure and the size of multiple emulsion.(2) multistep film emulsion process, to decentralized photo liquid pressurization, make it see through the perforated membrane with equal equal aperture, form micro-drop and be distributed to and in continuous phase, form elementary emulsion, using elementary emulsion as decentralized photo, pressurization makes it to see through perforated membrane and makes multiple emulsion.The method can be prepared multiple emulsion in enormous quantities, and prepared by the more overall multistep emulsion process of decentralized photo of the multiple emulsion preparing good, but still can not accurately control the internal structure of multiple emulsion, as the number that comprises drop etc.(3) microflow control technique emulsion process, utilize heterogeneous fluid in microchannel, to carry out repeatedly emulsification pretreatment and form multiple emulsion, the method can accurately be controlled size and the structure of multiple emulsion, the multiple emulsion of preparation has good monodispersity, but be difficult to prepare the multicomponent emulsion with ultra-thin-wall structure, simultaneously the method needs to carry out in microchannel repeatedly emulsification pretreatment, poor stability.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of and prepare single method of disperseing multicomponent multiple emulsion by mutually infiltrating between emulsion droplet, the method can not only accurately be controlled size and the internal structure of multiple emulsion, and can prepare the multicomponent emulsion with ultra-thin-wall structure.
Single preparation method who disperses multicomponent multiple emulsion of the present invention, processing step is as follows:
(1) preparation decentralized photo and continuous phase fluid
The preparation of the first dispersed phase fluid: water soluble emulsifier is added deionized water for stirring evenly to form the first dispersed 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 dispersed phase fluid: stir in oil soluble emulsifying agent being added to soybean oil under normal pressure, room temperature and form the second dispersed phase fluid, the amount of described oil soluble emulsifying agent is 0.005～0.02g in every 1ml soybean oil;
The preparation of the 3rd dispersed phase fluid: under normal pressure, room temperature by n-octyl alcohol and soybean oil by volume 1:3 mix to obtain mixed liquor, then in described mixed liquor, add oil soluble emulsifying agent, stir and form the 3rd dispersed phase fluid, the amount of described oil soluble emulsifying agent is 0.005～0.02g in the mixed liquor of every 1ml n-octyl alcohol and soybean oil;
The preparation of the 4th dispersed phase fluid: identical with the compound method of described the 3rd dispersed phase fluid;
The preparation of the 5th dispersed phase fluid: identical with the compound method of described the second dispersed phase fluid;
The preparation of the 6th dispersed phase fluid: light trigger 2-hydroxy-2-methyl propiophenone is added in ethoxylated trimethylolpropane triacrylate (its number-average molecular weight Mn is 692) under normal pressure, room temperature, stir and form the 6th dispersed phase fluid, the volume ratio of described 2-hydroxy-2-methyl propiophenone and ETPTA is 1:100;
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) the single multicomponent multiple emulsion drop that disperses of preparation
One of adopt with the following method the single multicomponent multiple emulsion drop that disperses of preparation:
Method one: the single multicomponent oil bag water-in-oil emulsion drop that disperses of preparation
The different inlets that the second dispersed phase fluid that step (1) is prepared and continuous phase fluid inject respectively the first single-stage droplet generator of microfluidic device form single dispersed oil bag fat liquor drop, and the different inlets that the first dispersed phase fluid of meanwhile step (1) being prepared and continuous phase fluid inject respectively the second single-stage droplet generator of microfluidic device form single water-in-oil emulsion drops that disperse; The oil bag fat liquor drop forming, water-in-oil emulsion drop enters microfluidic device collecting pipe with continuous phase fluid, when oil bag fat liquor drop contacts with the expansion chamber of water-in-oil emulsion drop at described collecting pipe, oil bag fat liquor drop spreads into the single multicomponent oil bag water-in-oil emulsion drop that disperses of formation on water-in-oil emulsion drop;
Flow (the Q of described the first dispersed phase fluid b) be 100～300 μ L/h, the flow (Q of described the second dispersed phase fluid a1) be 20～80 μ L/h, the flow (Q of described continuous phase fluid in the first single-stage droplet generator c1) be 40～200 μ L/h, flow (Q in the second single-stage droplet generator c2) be 200～500 μ L/h;
Method two: the single multicomponent Water-In-Oil bag fat liquor drop that disperses of preparation
The different inlets that the 3rd dispersed phase fluid that step (1) is prepared and continuous phase fluid inject respectively the first single-stage droplet generator of microfluidic device form single dispersed oil bag fat liquor drop, and the different inlets that the first dispersed phase fluid of meanwhile step (1) being prepared and continuous phase fluid inject respectively the second single-stage droplet generator of microfluidic device form single water-in-oil emulsion drops that disperse; The water-in-oil emulsion drop forming, oil bag fat liquor drop enters microfluidic device collecting pipe with continuous phase fluid, when water-in-oil emulsion drop contacts with the expansion chamber of oil bag fat liquor drop at described collecting pipe, water-in-oil emulsion drop spreads into the single multicomponent Water-In-Oil bag fat liquor drop that disperses of formation on oil bag fat liquor drop;
Flow (the Q of described the first dispersed phase fluid b) be 100～150 μ L/h, the flow (Q of described the 3rd dispersed phase fluid a2) be 50～90 μ L/h, the flow (Q of described continuous phase fluid in the first single-stage droplet generator c1) be 100～150 μ L/h, flow (Q in the second single-stage droplet generator c2) be 200～400 μ L/h;
Method three: the single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse of preparation
The different inlets that the 3rd dispersed phase fluid, the 4th dispersed phase fluid and the continuous phase fluid of step (1) preparation injected respectively to the first single-stage droplet generator of microfluidic device form two kinds of single dispersed oil bag fat liquor drops simultaneously, and the different inlets that the first dispersed phase fluid of simultaneously step (1) being prepared and continuous phase fluid inject respectively the second single-stage droplet generator of microfluidic device form single water-in-oil emulsion drops that disperse; Two kinds of single dispersed oil bag fat liquor drops that form, single collecting pipe that disperses water-in-oil emulsion drop to enter microfluidic device with continuous phase fluid, when water-in-oil emulsion drop contacts with the expansion chamber of two kinds of oil bag fat liquor drops at described collecting pipe, water-in-oil emulsion drop spreads into the single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse of formation on two kinds of oil bag fat liquor drops;
Flow (the Q of described the 3rd dispersed phase fluid a2) be 20 μ L/h, the flow (Q of described the 4th dispersed phase fluid a3) be 20 μ L/h, the flow (Q of described the first dispersed phase fluid b) be 150 μ L/h, the flow (Q of described continuous phase fluid in the first single-stage droplet generator c1) be 200 μ L/h, flow (Q in the second single-stage droplet generator c2) be 400 μ L/h;
Or adopt the single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse of following methods preparation:
The different inlets of the 4th dispersed phase fluid that step (1) is prepared, the single-stage droplet generator that continuous phase fluid injects respectively microfluidic device form oil bag fat liquor drops, and the different inlets that meanwhile the 3rd dispersed phase fluid of step (1) preparation respectively injected to the two-stage droplet generator of microfluidic device as middle phase, continuous phase fluid as foreign minister as interior phase, the first dispersed phase fluid form Water-In-Oil bag fat liquor drop; The Water-In-Oil bag fat liquor drop forming, oil bag fat liquor drop enters microfluidic device collecting pipe with continuous phase fluid, when Water-In-Oil bag fat liquor drop contacts with the expansion chamber of oil bag fat liquor drop at described collecting pipe, the water layer of Water-In-Oil bag fat liquor drop spreads into the single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse of formation on oil bag fat liquor drop;
Flow (the Q of described the first dispersed phase fluid b) be 150 μ L/h, the flow (Q of described the 3rd dispersed phase fluid a2) be 150 μ L/h, the flow (Q of described the 4th dispersed phase fluid a3) be 50～200 μ L/h, the flow (Q of described continuous phase fluid in single-stage droplet generator c4) be 100～300 μ L/h, flow (Q in two-stage droplet generator c3) be 300 μ L/h;
Method four: the single multicomponent oil bag Water-In-Oil bag fat liquor drop that disperses of preparation
The different inlets of the 5th dispersed phase fluid that step (1) is prepared, the single-stage droplet generator that continuous phase fluid injects respectively microfluidic device form oil bag fat liquor drops, and the different inlets that meanwhile the 3rd dispersed phase fluid of step (1) preparation respectively injected to the two-stage droplet generator of microfluidic device as middle phase, continuous phase fluid as foreign minister as interior phase, the first dispersed phase fluid form Water-In-Oil bag fat liquor drop; The Water-In-Oil bag fat liquor drop forming, oil bag fat liquor drop enters microfluidic device collecting pipe with continuous phase fluid, when oil bag fat liquor drop contacts with the expansion chamber of Water-In-Oil bag fat liquor drop at described collecting pipe, oil bag fat liquor drop spreads into the single multicomponent oil bag Water-In-Oil bag fat liquor drop that disperses of formation on Water-In-Oil bag fat liquor drop;
Flow (the Q of described the first dispersed phase fluid b) be 100～150 μ L/h, the flow (Q of described the 3rd dispersed phase fluid a2) be 150 μ L/h, the flow (Q of described the 5th dispersed phase fluid a4) be 150～200 μ L/h, the flow (Q of described continuous phase fluid in single-stage droplet generator c4) be 200～220 μ L/h, flow (Q in two-stage droplet generator c3) be 300～500 μ L/h;
(3) collect single multicomponent multiple emulsion that disperses
Single multicomponent multiple emulsion drop that disperses that step (2) is formed is introduced in collection container by the efferent duct of microfluidic device together with continuous phase, obtains single multicomponent multiple emulsion that disperses of respective type.
In said method, described water soluble emulsifier is the addition polymers of lauryl sodium sulfate or 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) of trimethicone and cyclohexyl methyl siloxanes composition, and the volume ratio of trimethicone and cyclohexyl methyl siloxanes is 1:1.
In said method, can also contain dyestuff described in step in the 4th dispersed phase fluid and the 5th dispersed phase fluid, the effect of described dyestuff is to drop dyeing, and its addition so that observe is limited, and can use the various dyestuffs that are dissolved in soybean oil, preferentially selects f Red300.
Single external diameter that disperses emulsion droplet in multicomponent multiple emulsion prepared by said method is 100～500 μ m.
Single preparation method who disperses multicomponent multiple emulsion of the present invention is microflow control technique emulsification-infusion method, form the principle of multiple emulsion based on mutually infiltrating between two or more emulsion droplets: Fig. 1 is shown in by single formation schematic diagram that disperses multicomponent double emulsion, immiscible the first emulsion droplet 1 and the second emulsion droplet 2 are dispersed in the another kind of continuous phase fluid 3 not dissolving each other with it, when sprawling coefficient S 1when >0, the first emulsion droplet 1 will spread into and on the second emulsion droplet 2, form 2/1/3 type emulsion; When sprawling coefficient S 2when >0, the second emulsion droplet 2 will spread into and on the first emulsion droplet 1, form 1/2/3 type emulsion; Spreading coefficient S 1=γ 23-(α 1γ 13+ γ 12), S 2=γ 13-(α 2γ 23+ γ 12), γ ijthe interfacial tension that i phase and j are alternate (i ≠ j=1,2,3), α 1 = [ 1 + ( R 1 R 2 ) 3 ] 2 3 - ( R 1 R 2 ) 2 , α 2 = [ 1 + ( R 2 R 1 ) 3 ] 2 3 - ( R 2 R 1 ) 2 , R 1and R 2be respectively the radius of the first emulsion droplet 1 and the second emulsion droplet 2.In the present invention, Fig. 2 is shown in by single multicomponent formation schematic diagram dual and triple emulsion that disperses.Therefore, any three kinds of immiscible fluids, as long as interfacial tension adjusting is suitable between three-phase, also can prepare single multicomponent multiple emulsion that disperses according to the principle mutually infiltrating between emulsion droplet.
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 public collecting pipe that two droplet generators contact for drop with; Two droplet generators are prepared two kinds of different emulsion droplets, and the emulsion droplet public collecting pipe of flowing through is realized and mutually infiltrated the more complicated emulsion of preparation in collecting pipe; 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 7, each lower cover glass determining deviation of being separated by is fixed on slide and 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 six or 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 CN102626602A).
The structure of the microfluidic device with two single-stage droplet generators that the present invention adopts as shown in Figure 3, the schematic diagram that in its microchannel and microchannel, emulsion droplet is sprawled is as Fig. 4～Fig. 6, the first microchannel and the second microchannel form the first single-stage droplet generator, and the 3rd microchannel and the 4th microchannel form the second single-stage droplet generator; The structure of the microfluidic device with a two-stage droplet generator and a single-stage droplet generator that the present invention adopts as shown in Figure 7, the schematic diagram that in its microchannel and microchannel, emulsion droplet is sprawled as shown in Figure 8, Figure 9, the 5th microchannel, the 6th microchannel and the 7th microchannel form two-stage droplet generator, and the 8th microchannel and the 9th microchannel form single-stage droplet generator.
The present invention has following beneficial effect:
1, the present invention adopts the single multicomponent multiple emulsion that disperses of microflow control technique emulsification-infusion method preparation, for single preparation that disperses multicomponent multiple emulsion provides a kind of new method.
2, the method for the invention not only can accurately be controlled internal structure and the size of multiple emulsion, and can prepare the multicomponent emulsion with ultra-thin-wall structure, and in principle, the wall thickness of described multiple emulsion can be a monomolecular thickness.
3, the multiple emulsion that the method for the invention prepares has good monodispersity, thus can be by the method the collaborative control delivery for the preparation of complicated multicomponent pharmaceutical or active material.
4, the method for the invention simple to operate, be easy to control and regulate, and adopt conventional equipment can realize, cost-saving, be easy to realize suitability for industrialized production.
Brief description of the drawings
Fig. 1 is single formation schematic diagram that disperses multicomponent double emulsion in the method for the invention;
Fig. 2 is single formation schematic diagram that disperses the dual and triple emulsion of multicomponent in the method for the invention;
Fig. 3 is the structural representation of the microfluidic device with two single-stage droplet generators of the method for the invention employing;
Fig. 4 is that in the microchannel of microfluidic device described in Fig. 3 and microchannel, oil bag fat liquor drop spreads into the schematic diagram on water-in-oil emulsion drop;
Fig. 5 is that in the microchannel of microfluidic device described in Fig. 3 and microchannel, water-in-oil emulsion drop spreads into the schematic diagram on oil bag fat liquor drop;
Fig. 6 is that in the microchannel of microfluidic device described in Fig. 3 and microchannel, water-in-oil emulsion drop spreads into the schematic diagrames on different oil bag fat liquor drops simultaneously;
Fig. 7 is the structural representation of the microfluidic device with a two-stage droplet generator and a single-stage droplet generator of the method for the invention employing;
Fig. 8 is that in the microchannel of microfluidic device described in Fig. 7 and microchannel, Water-In-Oil bag fat liquor drop spreads into the schematic diagram on oil bag fat liquor drop;
Fig. 9 is that in the microchannel of microfluidic device described in Fig. 7 and microchannel, oil bag fat liquor drop spreads into the schematic diagram on Water-In-Oil bag fat liquor drop;
Figure 10 is that in the embodiment 1 of embodiment 1, oil bag fat liquor drop spreads into and on water-in-oil emulsion drop, forms single high speed camera photo that disperses multicomponent W/O/O emulsion droplet process;
Figure 11 is that in the embodiment 2 of embodiment 1, oil bag fat liquor drop spreads into and on water-in-oil emulsion drop, forms single high speed camera photo that disperses multicomponent W/O/O emulsion droplet process;
Figure 12 is that in the embodiment 3 of embodiment 1, oil bag fat liquor drop spreads into and on water-in-oil emulsion drop, forms single high speed camera photo that disperses multicomponent W/O/O emulsion droplet process;
Figure 13 is single optical microscope photograph that disperses multicomponent W/O/O emulsion prepared by the embodiment 1 of embodiment 1;
Figure 14 is that in the embodiment 1 of embodiment 2, oil bag fat liquor drop spreads into the single high speed camera photo that disperses multicomponent oil bag water-in-oil emulsion drop process that forms monokaryon on water-in-oil emulsion drop completely;
Figure 15 is that in the embodiment 2 of embodiment 2, oil bag fat liquor drop spreads into the single high speed camera photo that disperses multicomponent oil bag water-in-oil emulsion drop process that forms double-core on water-in-oil emulsion drop completely;
Figure 16 is that in the embodiment 3 of embodiment 2, oil bag fat liquor drop spreads into the single high speed camera photo that disperses multicomponent oil bag water-in-oil emulsion drop process that forms three cores on water-in-oil emulsion drop completely;
Figure 17 is that in the embodiment 4 of embodiment 2, oil bag fat liquor drop spreads into the single high speed camera photo that disperses multicomponent W/O/O emulsion droplet process that forms monokaryon on water-in-oil emulsion drop completely;
Figure 18 is that in the embodiment 5 of embodiment 2, oil bag fat liquor drop spreads into the single high speed camera photo that disperses multicomponent W/O/O emulsion droplet process that forms double-core on water-in-oil emulsion drop completely;
Figure 19 is that in the embodiment 1 of embodiment 3, water-in-oil emulsion drop spreads into the single high speed camera photo that disperses multicomponent O/W/O emulsion droplet process that forms monokaryon on oil bag fat liquor drop completely;
Figure 20 is that in the embodiment 2 of embodiment 3, water-in-oil emulsion drop spreads into the single high speed camera photo that disperses multicomponent O/W/O emulsion droplet process that forms double-core on oil bag fat liquor drop completely;
Figure 21 is that in the embodiment 3 of embodiment 3, water-in-oil emulsion drop spreads into the single high speed camera photo that disperses multicomponent O/W/O emulsion droplet process that forms three cores on oil bag fat liquor drop completely;
Figure 22 is that in embodiment 4, water-in-oil emulsion drop spreads into the high speed camera photo that forms the different oily core multiple emulsion drop processes of single dispersion multicomponent Water-In-Oil bag on two kinds of oil bag fat liquor drops completely;
Figure 23 is the high speed camera photo of Water-In-Oil bag fat liquor drop forming process in the embodiment of the present invention 5;
Figure 24 is the high speed camera photo of oil bag fat liquor drop forming process in the embodiment of the present invention 5;
Figure 25 is that the water layer of oil bag water-in-oil emulsion drop in the embodiment 1 of embodiment 5 spreads into completely on oil bag fat liquor drop and forms single high speed camera photo that disperses two the oily core multiple emulsion of difference drop processes of multicomponent Water-In-Oil bag;
Figure 26 is that the water layer of oil bag water-in-oil emulsion drop in the embodiment 2 of embodiment 5 spreads into completely on oil bag fat liquor drop and forms single high speed camera photo that disperses three oily core multiple emulsion drop processes of multicomponent Water-In-Oil bag;
Figure 27 is that the water layer of oil bag water-in-oil emulsion drop in the embodiment 3 of embodiment 5 spreads into completely on oil bag fat liquor drop and forms single high speed camera photo that disperses four oily core multiple emulsion drop processes of multicomponent Water-In-Oil bag;
Figure 28 is single optical microscope photograph that disperses the different oily core multiple emulsions of multicomponent Water-In-Oil bag prepared by the embodiment 1 of embodiment 5;
Figure 29 is that in the embodiment 1 of embodiment 6, oil bag fat liquor drop spreads into the high speed camera photo that forms the O/W/O/O emulsion droplet process that includes a Water-In-Oil bag fat liquor drop on Water-In-Oil bag fat liquor drop completely;
Figure 30 is that in the embodiment 2 of embodiment 6, oil bag fat liquor drop spreads into the high speed camera photo that forms the O/W/O/O emulsion droplet process that includes two Water-In-Oil bag fat liquor drops on Water-In-Oil bag fat liquor drop completely;
Figure 31 is the single optical microscope photograph that disperses multicomponent O/W/O/O emulsion that includes a Water-In-Oil bag fat liquor drop prepared by the embodiment 1 of embodiment 6;
Figure 32 is the stereoscan photograph of the ethoxylated trimethylolpropane triacrylate micro-capsule prepared of embodiment 7;
Figure 33 is the stereoscan photograph of the ethoxylated trimethylolpropane triacrylate micro-capsule wall thickness prepared of embodiment 7.
In figure, the 1-the first emulsion droplet, the 2-the second emulsion droplet, 3-continuous phase fluid, the 4-the three emulsion droplet, 5-slide, 6-lower cover glass, 7-epoxide-resin glue, 8-injection needle, 9-upper cover glass, 10-efferent duct, the 11-the first microchannel, the 12-the second microchannel, the first inlet of 12-1-the second microchannel 12, the second inlet of 12-2-the second microchannel 12, the 13-the three microchannel, the 14-the four microchannel, the 15-the five microchannel, the 16-the six microchannel, the 17-the seven microchannel, the 18-the eight microchannel, the 19-the nine microchannel, 20-collecting pipe.
Detailed description of the invention
Also by reference to the accompanying drawings single preparation method who disperses multicomponent multiple emulsion of the present invention is described further below by embodiment.In following each embodiment, described Dow Corning749 is that percentage by volume is the mixture of the cyclohexyl methyl siloxanes of 50% trimethicone and percentage by volume 50%, and Dow Corning749 is its trade name, purchased from Dow Corning company; Described dyestuff f Red300 is Yi Zhong perylene diimide compounds, f Red300 is its trade name, purchased from BASF AG; Described medical soybean oil is injection rank, purchased from Tieling Beiya Medical Oil Co., Ltd..
Embodiment 1
The present embodiment adopts single multicomponent oil bag Water-In-Oil (W/O/O) emulsion of disperseing of the method for the invention preparation, and processing step is as follows:
(1) preparation decentralized photo and continuous phase fluid
The preparation of the first dispersed phase fluid: lauryl sodium sulfate (SDS) is added deionized water for stirring evenly to form the first dispersed 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 dispersed phase fluid: will gather ricinoleic acid glyceride (PGPR90) and add to stir in medical soybean oil and form the second dispersed phase fluid under normal pressure, room temperature, the amount of described PGPR90 is 0.005g in the medical soybean oil of every 1ml;
The preparation of continuous phase fluid: formation continuous phase fluid stirs in Dow Corning749 (DC749) being added to dimethicone under normal pressure, room temperature, the mass ratio of described DC749 and dimethicone is 0.005:1, and described dimethyl-silicon oil viscosity is 10cSt.
(2) the single multicomponent W/O/O emulsion droplet that disperses of preparation
The present embodiment uses the microfluidic device with two single-stage droplet generators, its structure as shown in Figure 3, comprise slide 5, upper cover glass 9, lower cover glass 6 and injection needle 8, oil bag fat liquor drop spreads into schematic diagram on water-in-oil emulsion drop as shown in Figure 4 in its microchannel and microchannel, the first microchannel 11 and the second microchannel 12 form the first single-stage droplet generator, the 3rd microchannel 13 and the 4th microchannel 14 form the second single-stage droplet generator, the width of the first microchannel 11 is 80 μ m, the width of the second microchannel 12 is 120 μ m, the width of the 3rd microchannel 13 is 120 μ m, the width of the 4th microchannel 14 is 80 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 2.5mm, minor axis is 260 μ m, the height of each microchannel is about 150 μ m.
The first microchannel 11 and the second microchannel 12 that the second dispersed phase fluid of step (1) preparation and continuous phase fluid are injected to microfluidic device the first single-stage droplet generator by the syringe 8 being connected with syringe pump respectively form single dispersed oil bag fat liquor drop, and the 3rd microchannel 13 and the 4th microchannel 14 that meanwhile the first dispersed phase fluid of step (1) preparation and continuous phase fluid are injected to microfluidic device the second single-stage droplet generator by the syringe 8 being connected with syringe pump respectively form single water-in-oil emulsion drop that disperses; The oil bag fat liquor drop forming, water-in-oil emulsion drop enters microfluidic device collecting pipe 20 with continuous phase fluid, when oil bag fat liquor drop contacts with the expansion chamber of water-in-oil emulsion drop at collecting pipe, oil bag fat liquor drop spreads into the single multicomponent W/O/O emulsion droplet that disperses of formation on water-in-oil emulsion drop;
Embodiment 1: as the flow Q of the first dispersed phase fluid b=200 μ L/h, the flow Q of the second dispersed phase fluid a1=20 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=40 μ L/h, flow Q in the second single-stage droplet generator c2=300 μ L/h, described oil bag fat liquor drop meets each oil bag fat liquor drop and contact with a water-in-oil emulsion drop in the expansion chamber of collecting pipe 20 with water-in-oil emulsion drop, oil bag fat liquor drop spreads into formation list dispersion multicomponent W/O/O emulsion droplet (seeing Figure 10) on water-in-oil emulsion drop;
Embodiment 2: as the flow Q of the first dispersed phase fluid b=150 μ L/h, the flow Q of the second dispersed phase fluid a1=80 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=70 μ L/h, flow Q in the second single-stage droplet generator c2=300 μ L/h, described oil bag fat liquor drop and water-in-oil emulsion drop enter and in the expansion chamber of collecting pipe 20, meet each oil bag fat liquor drop and contact with a water-in-oil emulsion drop, and oil bag fat liquor drop spreads into formation list dispersion multicomponent W/O/O emulsion droplet (seeing Figure 11) on water-in-oil emulsion drop;
Embodiment 3: as the flow Q of the first dispersed phase fluid b=150 μ L/h, the flow Q of the second dispersed phase fluid a1=40 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=40 μ L/h, flow Q in the second single-stage droplet generator c2=500 μ L/h, described oil bag fat liquor drop meets each oil bag fat liquor drop and contact with a water-in-oil emulsion drop in the expansion chamber of collecting pipe 20 with water-in-oil emulsion drop, oil bag fat liquor drop spreads into formation list dispersion multicomponent W/O/O emulsion droplet (seeing Figure 12) on water-in-oil emulsion drop.
(3) collect single multicomponent W/O/O emulsion of disperseing
The single multicomponent W/O/O emulsion droplet that disperses forming in step (2) embodiment 1～3 is introduced in collection container by the efferent duct 10 of microfluidic device together with continuous phase, obtained corresponding single multicomponent W/O/O emulsion of disperseing.
The optical microscope photograph of single dispersion multicomponent W/O/O emulsion of preparing according to embodiment 1 conditional as shown in figure 13.
Embodiment 2
The present embodiment adopts single multicomponent oil bag Water-In-Oil (W/O/O) emulsion of disperseing of the method for the invention preparation, and processing step is as follows:
(1) preparation decentralized photo and continuous phase fluid
The preparation of the first dispersed phase fluid: SDS is added deionized water for stirring evenly to form the first dispersed 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 dispersed phase fluid: under normal pressure, room temperature, PGPR90 is added in medical soybean oil and stir and form the second dispersed phase fluid, the amount of described PGPR90 is 0.02g in the medical soybean oil of every 1ml;
The preparation of the 5th dispersed phase fluid: PGPR90 is added to the formation mixed liquor that stirs in medical soybean oil under normal pressure, room temperature, then form the 5th dispersed phase fluid to adding in described mixed liquor fluorescent dye LR300 to stir, the amount of described PGPR90 is 0.005g in the medical soybean oil of every 1ml, and the amount of described LR300 is 1mg in the medical soybean oil of 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 10cSt.
(2) the single multicomponent W/O/O emulsion droplet that disperses of preparation
In the present embodiment, the single microfluidic device of multicomponent W/O/O emulsion droplet that disperses of preparation is with embodiment 1;
Method one: the second dispersed phase fluid of step (1) preparation is formed to single dispersed oil bag fat liquor drop by the first microchannel 11 and second microchannel 12 of syringe injection microfluidic device the first single-stage droplet generator being connected with syringe pump respectively with continuous phase fluid, meanwhile the first dispersed phase fluid of step (1) preparation is formed to single water-in-oil emulsion drop that disperses by the 3rd microchannel 13 and the 4th microchannel 14 of syringe injection microfluidic device the second single-stage droplet generator being connected with syringe pump respectively with continuous phase fluid; The oil bag fat liquor drop forming, water-in-oil emulsion drop enters microfluidic device collecting pipe 20 with continuous phase fluid, when oil bag fat liquor drop contacts with the expansion chamber of water-in-oil emulsion drop at collecting pipe, oil bag fat liquor drop spreads into the single multicomponent W/O/O emulsion droplet that disperses of formation on water-in-oil emulsion drop;
Embodiment 1: as the flow Q of the second dispersed phase fluid a1=50 μ L/h, the flow Q of the first dispersed phase fluid b=200 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=200 μ L/h, flow Q in the second single-stage droplet generator c2=200 μ L/h, described oil bag fat liquor drop meets each oil bag fat liquor drop and contacts with a water-in-oil emulsion drop in the expansion chamber of collecting pipe 20 with water-in-oil emulsion drop, oil bag fat liquor drop spreads into the single multicomponent W/O/O emulsion droplet (seeing Figure 14) that disperses that forms monokaryon on water-in-oil emulsion drop;
Embodiment 2: as the flow Q of the second dispersed phase fluid a1=50 μ L/h, the flow Q of the first dispersed phase fluid b=300 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=100 μ L/h, flow Q in the second single-stage droplet generator c2=200 μ L/h, described oil bag fat liquor drop meets each oil bag fat liquor drop and contacts with two water-in-oil emulsion drops in the expansion chamber of collecting pipe 20 with water-in-oil emulsion drop, oil bag fat liquor drop spreads into the single multicomponent W/O/O emulsion droplet (seeing Figure 15) that disperses that forms double-core on water-in-oil emulsion drop;
Embodiment 3: as the flow Q of the second dispersed phase fluid a1=50 μ L/h, the flow Q of the first dispersed phase fluid b=300 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=200 μ L/h, flow Q in the second single-stage droplet generator c2=200 μ L/h, described oil bag fat liquor drop meets each oil bag fat liquor drop and contacts with three water-in-oil emulsion drops in the expansion chamber of collecting pipe with water-in-oil emulsion drop, oil bag fat liquor drop spreads into the single multicomponent W/O/O emulsion droplet (seeing Figure 16) that disperses that forms three cores on water-in-oil emulsion drop;
Method two: the 5th dispersed phase fluid of step (1) preparation is formed to single dispersed oil bag fat liquor drop by the first microchannel 11 and second microchannel 12 of syringe injection microfluidic device the first single-stage droplet generator being connected with syringe pump respectively with continuous phase fluid, the first dispersed phase fluid of step (1) preparation is formed to single water-in-oil emulsion drop that disperses by the 3rd microchannel 13 and the 4th microchannel 14 of syringe injection microfluidic device the second single-stage droplet generator being connected with syringe pump respectively with continuous phase fluid simultaneously; The oil bag fat liquor drop forming, water-in-oil emulsion drop enters microfluidic device collecting pipe 20 with continuous phase fluid, when oil bag fat liquor drop contacts with the expansion chamber of water-in-oil emulsion drop at collecting pipe 20, oil bag fat liquor drop spreads into the single multicomponent W/O/O emulsion droplet that disperses of formation on water-in-oil emulsion drop;
Embodiment 1: as the flow Q of the 5th dispersed phase fluid a4=80 μ L/h, the flow Q of the first dispersed phase fluid b=150 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=150 μ L/h, flow Q in the second single-stage droplet generator c2=250 μ L/h, described oil bag fat liquor drop meets each oil bag fat liquor drop and contacts with a water-in-oil emulsion drop in the expansion chamber of collecting pipe 20 with water-in-oil emulsion drop, oil bag fat liquor drop spreads into the single multicomponent W/O/O emulsion droplet (seeing Figure 17) that disperses that forms monokaryon on water-in-oil emulsion drop;
Embodiment 2: as the flow Q of the 5th dispersed phase fluid a4=40 μ L/h, the flow Q of the first dispersed phase fluid b=100 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=100 μ L/h, flow Q in the second single-stage droplet generator c2=200 μ L/h, described oil bag fat liquor drop meets each oil bag fat liquor drop and contacts with two water-in-oil emulsion drops in the expansion chamber of collecting pipe 20 with water-in-oil emulsion drop, oil bag fat liquor drop spreads into the single multicomponent W/O/O emulsion droplet (seeing Figure 18) that disperses that forms double-core on water-in-oil emulsion drop.
(3) collect single multicomponent W/O/O emulsion of disperseing
Single multicomponent W/O/O emulsion droplet connection continuous phase fluid that disperses that step (2) is formed is introduced in collection container by the efferent duct 10 of microfluidic device together, obtains corresponding single multicomponent W/O/O emulsion of disperseing.
Embodiment 3
The present embodiment adopts single multicomponent Water-In-Oil bag oil (O/W/O) emulsion of disperseing of the method for the invention preparation, and processing step is as follows:
(1) preparation decentralized photo and continuous phase fluid
The preparation of the first dispersed phase fluid: SDS is added deionized water for stirring evenly to form the first dispersed phase fluid under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.005:1;
The preparation of the 3rd dispersed phase fluid: under normal pressure, room temperature by n-octyl alcohol and medical soybean oil by volume 1:3 mix to obtain mixed liquor, then in described mixed liquor, add PGPR90, stir and form the 3rd dispersed phase fluid, the amount of described PGPR90 is 0.005g in the mixed liquor of every 1ml n-octyl alcohol and medical soybean oil;
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 10cSt.
(2) the single multicomponent O/W/O emulsion droplet that disperses of preparation
The microfluidic device adopting in the present embodiment, its structure as shown in Figure 3, comprise slide 5, upper cover glass 9, lower cover glass 6 and injection needle 8, water-in-oil emulsion drop spreads into schematic diagram on oil bag fat liquor drop as shown in Figure 5 in its microchannel and microchannel, the first microchannel 11 and the second microchannel 12 form the first single-stage droplet generator, the 3rd microchannel 13 and the 4th microchannel 14 form the second single-stage droplet generator, the width of the first microchannel 11 is 100 μ m, the width of the second microchannel 12 is 150 μ m, the width of the 3rd microchannel 13 is 150 μ m, the width of the 4th microchannel 14 is 100 μ m, collecting pipe width is 180 μ m, the floor projection of the expansion chamber of collecting pipe is oval, its major axis is 1.5mm, minor axis is 600 μ m, the height of each microchannel is about 150 μ m.
The first microchannel 11 and the second microchannel 12 that the 3rd dispersed phase fluid of step (1) preparation and continuous phase fluid are injected to the first single-stage droplet generator of microfluidic device by the syringe being connected with syringe pump respectively form single dispersed oil bag fat liquor drop, and the 3rd microchannel 13 and the 4th microchannel 14 that the syringe meanwhile the first dispersed phase fluid of step (1) preparation being connected due to syringe pump respectively with continuous phase fluid injects the second single-stage droplet generator of microfluidic device form single dispersion water-in-oil emulsion drops; The water-in-oil emulsion drop, the oil bag fat liquor drop that form enter collecting pipe 20 with continuous phase fluid, when water-in-oil emulsion drop contacts with the expansion chamber of oil bag fat liquor drop at collecting pipe 20, water-in-oil emulsion drop spreads into the single multicomponent O/W/O emulsion droplet that disperses of formation on oil bag fat liquor drop;
Embodiment 1: as the flow Q of the first dispersed phase fluid b=100 μ L/h, the flow Q of the 3rd dispersed phase fluid a2=50 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=100 μ L/h, flow Q in the second single-stage droplet generator c2=200 μ L/h, described water-in-oil emulsion drop meets each water-in-oil emulsion drop with oil bag fat liquor drop and contacts with an oil bag fat liquor drop in the expansion chamber of collecting pipe 20, and water-in-oil emulsion drop spreads into the single multicomponent O/W/O emulsion droplet (seeing Figure 19) that disperses that forms monokaryon on oil bag fat liquor drop;
Embodiment 2: as the flow Q of the first dispersed phase fluid b=100 μ L/h, the flow Q of the 3rd dispersed phase fluid a2=80 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=150 μ L/h, flow Q in the second single-stage droplet generator c2=400 μ L/h, described water-in-oil emulsion drop meets each water-in-oil emulsion drop with oil bag fat liquor drop and contacts with two oil bag fat liquor drops in the expansion chamber of collecting pipe 20, and water-in-oil emulsion drop spreads into the single multicomponent O/W/O emulsion droplet (seeing Figure 20) that disperses that forms double-core on oil bag fat liquor drop;
Embodiment 3: as the flow Q of the first dispersed phase fluid b=150 μ L/h, the flow Q of the 3rd dispersed phase fluid a2=90 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=150 μ L/h, flow Q in the second single-stage droplet generator c2=200 μ L/h, described water-in-oil emulsion drop meets each water-in-oil emulsion drop with oil bag fat liquor drop and contacts with three oil bag fat liquor drops in the expansion chamber of collecting pipe 20, and water-in-oil emulsion drop spreads into the single multicomponent O/W/O emulsion droplet (seeing Figure 21) that disperses that forms three cores on oil bag fat liquor drop.
(3) collect single multicomponent O/W/O emulsion of disperseing
Single multicomponent O/W/O emulsion droplet that disperses that step (2) is formed is introduced in collection container by the efferent duct 10 of microfluidic device together with continuous phase, obtains corresponding single multicomponent O/W/O emulsion of disperseing.
Embodiment 4
The present embodiment adopts the single different oily core multiple emulsions of multicomponent Water-In-Oil bag that disperse of the method for the invention preparation, and processing step is as follows:
The preparation of the first dispersed phase fluid: SDS is added deionized water for stirring evenly to form the first dispersed phase fluid under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.01:1;
The preparation of the 3rd dispersed phase fluid: under normal pressure, room temperature by n-octyl alcohol and medical soybean oil by volume 1:3 mix to obtain mixed liquor, then in described mixed liquor, add PGPR90, stir and form the 3rd dispersed phase fluid, the amount of described PGPR90 is 0.02g in the mixed liquor of every 1ml n-octyl alcohol and medical soybean oil;
The preparation of the 4th dispersed phase fluid: under normal pressure, room temperature by n-octyl alcohol and medical soybean oil by volume 1:3 mix to obtain mixed liquor, then in described mixed liquor, add PGPR90 and fluorescent dye LR300, the amount of described PGPR90 is 0.02g in every 1ml mixed liquor, and the amount of described LR300 is 1mg in the mixed liquor of 1ml n-octyl alcohol and medical soybean oil;
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 10cSt.
(2) the single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse of preparation
In the present embodiment, the single microfluidic device of the different oily core multiple emulsion drops of multicomponent Water-In-Oil bag that disperses of preparation is with embodiment 3, and in its microchannel and microchannel, water-in-oil emulsion drop spreads into schematic diagram on different oil bag fat liquor drops as shown in Figure 6 simultaneously;
By the 3rd dispersed phase fluid of step (1) preparation, the 4th dispersed phase fluid and continuous phase fluid are injected respectively the first inlet 12-1 of the second microchannel 12 of the first single-stage droplet generator of microfluidic device by the syringe being connected with syringe pump, the second inlet 12-2 and the first microchannel 11 form two kinds of single dispersed oil bag fat liquor drops simultaneously, the first dispersed phase fluid of meanwhile step (1) being prepared and continuous phase fluid inject respectively the 3rd microchannel 13 and the single water-in-oil emulsion drops that disperse of the 4th microchannel 14 formation of microfluidic device the second single-stage droplet generator by syringe pump, the two kinds of single dispersed oil bag fat liquor drops, the single water-in-oil emulsion drop that disperses that form enter collecting pipe 20 with continuous phase fluid and expand in chamber and contact at it, when a water-in-oil emulsion drop and two kinds oil bag fat liquor drop each one while contact, water-in-oil emulsion drop spreads on two kinds of oil bag fat liquor drops and forms single multicomponent Water-In-Oil bag oily core emulsion droplets of difference (seeing Figure 22) that disperse, the flow Q of described the first dispersed phase fluid bthe flow Q of=150 μ L/h, the 3rd dispersed phase fluid a2the flow Q of=20 μ L/h, the 4th dispersed phase fluid a3=20 μ L/h, the flow Q in the first single-stage droplet generator of continuous phase fluid c1=200 μ L/h, flow Q in the second single-stage droplet generator c2=400 μ L/h,
(3) collect single different oily core multiple emulsions of multicomponent Water-In-Oil bag that disperse
Single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse that step (2) is formed are introduced in collection container by the efferent duct 10 of microfluidic device together with continuous phase, obtain single different oily core emulsions of multicomponent Water-In-Oil bag of disperseing.
Embodiment 5
The present embodiment adopts the single different oily core multiple emulsions of multicomponent Water-In-Oil bag that disperse of the method for the invention preparation, and processing step is as follows:
(1) preparation decentralized photo and continuous phase fluid
The preparation of the first dispersed phase fluid: SDS is added deionized water for stirring evenly to form the first dispersed phase fluid under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.01:1;
The preparation of the 3rd dispersed phase fluid: under normal pressure, room temperature by n-octyl alcohol and medical soybean oil by volume 1:3 mix to obtain mixed liquor, then in described mixed liquor, add PGPR90, stir and form the 3rd dispersed phase fluid, the amount of described PGPR90 is 0.005g in the mixed liquor of every 1ml n-octyl alcohol and medical soybean oil;
The preparation of the 4th dispersed phase fluid: under normal pressure, room temperature by n-octyl alcohol and medical soybean oil by volume 1:3 mix to obtain mixed liquor, then in described mixed liquor, add PGPR90 and fluorescent dye LR300, the amount of described PGPR90 is 0.005g in the mixed liquor of every 1ml n-octyl alcohol and medical soybean oil, and the amount of described LR300 is 1mg in the mixed liquor of 1ml n-octyl alcohol and medical soybean oil;
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 10cSt.
(2) the single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse of preparation
The microfluidic device that the present embodiment uses, its structure as shown in Figure 7, comprise slide 5, upper cover glass 9, lower cover glass 6 and injection needle 8, Water-In-Oil bag fat liquor drop spreads into schematic diagram on oil bag fat liquor drop as shown in Figure 8 in its microchannel and microchannel, the 5th microchannel 15, the 6th microchannel 16 and seven microchannels 17 form a two-stage droplet generator, and the 8th microchannel 18 and the 9th microchannel 19 form a single-stage droplet generator; The width of the 5th microchannel 15 is 90 μ m, the width of the 6th microchannel 16 is 115 μ m, the width of the 7th microchannel 17 is 150 μ m, the width of the 8th microchannel 18 is 150 μ m, and the width of the 9th microchannel 18 is 90 μ m, and 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.
By the 4th dispersed phase fluid of step (1) preparation, the 9th microchannel 19 and the 8th microchannel 18 that continuous phase fluid injects the described single-stage droplet generator of microfluidic device by the syringe that is connected with syringe pump respectively form oil bag fat liquor drop (Figure 24 is shown in by the high speed camera photo of the present embodiment embodiment 1 oil bag fat liquor drop preparation process), meanwhile using the 3rd dispersed phase fluid of step (1) preparation as interior phase, the first dispersed phase fluid is as middle phase, continuous phase fluid is injected respectively the 5th microchannel 15 of the described two-stage droplet generator of microfluidic device by the syringe being connected with syringe pump as foreign minister, the 6th microchannel 16, seven microchannels 17 form Water-In-Oil bag fat liquor drop (in the present embodiment, in embodiment 1, Figure 23 is shown in by the high speed camera photo of Water-In-Oil bag fat liquor drop preparation process), the Water-In-Oil bag fat liquor drop, the oil bag fat liquor drop that form enter collecting pipe 20 with continuous phase fluid, when Water-In-Oil bag fat liquor drop contacts with the expansion chamber of oil bag fat liquor drop at collecting pipe 20, the water layer of Water-In-Oil bag fat liquor drop spreads into the single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse of i.e. formation on oil bag fat liquor drop,
Embodiment 1: as the flow Q of the first dispersed phase fluid b=150 μ L/h, the flow Q of the 3rd decentralized photo phase fluid a2=150 μ L/h, the flow Q of the 4th dispersed phase fluid a3=50 μ L/h, the flow Q of continuous phase fluid in described single-stage droplet generator c4=100 μ L/h, flow Q in described two-stage droplet generator c3=300 μ L/h, described Water-In-Oil bag fat liquor drop meets each Water-In-Oil bag fat liquor drop with oil bag fat liquor drop and contacts with an oil bag fat liquor drop in the expansion chamber of collecting pipe 20, and the water layer of Water-In-Oil bag fat liquor drop spreads on oil bag fat liquor drop and form single multicomponent Water-In-Oil bag oily core emulsion droplets of two differences (seeing Figure 25) that disperse;
Embodiment 2: as the flow Q of the first dispersed phase fluid b=150 μ L/h, the flow Q of the 3rd decentralized photo phase fluid a2=150 μ L/h, the flow Q of the 4th dispersed phase fluid a3=200 μ L/h, the flow Q of continuous phase fluid in described single-stage droplet generator c4=200 μ L/h, flow Q in described two-stage droplet generator c3=300 μ L/h, described Water-In-Oil bag fat liquor drop meets each Water-In-Oil bag fat liquor drop with oil bag fat liquor drop and contacts with two oil bag fat liquor drops in the expansion chamber of collecting pipe 20, and the water layer of Water-In-Oil bag fat liquor drop spreads on oil bag fat liquor drop and form single multicomponent Water-In-Oil three oily core emulsion droplets of bag (seeing Figure 26) that disperse;
Embodiment 3: as the flow Q of the first dispersed phase fluid b=150 μ L/h, the flow Q of the 3rd decentralized photo phase fluid a2=150 μ L/h, the flow Q of the 4th dispersed phase fluid a3=200 μ L/h, the flow Q of continuous phase fluid in described single-stage droplet generator c4=300 μ L/h, flow Q in described two-stage droplet generator c3=300 μ L/h, described Water-In-Oil bag fat liquor drop meets each Water-In-Oil bag fat liquor drop with oil bag fat liquor drop and contacts with three oil bag fat liquor drops in the expansion chamber of collecting pipe 20, and the water layer of Water-In-Oil bag fat liquor drop spreads on oil bag fat liquor drop and form single multicomponent Water-In-Oil four oily core emulsion droplets of bag (seeing Figure 27) that disperse;
(3) collect single different oily core multiple emulsions of multicomponent Water-In-Oil bag that disperse
Single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse that step (2) is formed are introduced in collection container by the efferent duct 10 of microfluidic device together with continuous phase, obtain single different oily core emulsions of multicomponent Water-In-Oil bag of disperseing.The optical microscope photograph of the different oily core emulsions of single dispersion multicomponent Water-In-Oil bag prepared by embodiment 1 as shown in figure 28.
Embodiment 6
The present embodiment adopts single multicomponent oil bag Water-In-Oil bag oil (O/W/O/O) emulsion of disperseing of the method for the invention preparation, and processing step is as follows:
(1) preparation decentralized photo and continuous phase fluid
The preparation of the first dispersed phase fluid: SDS is added deionized water for stirring evenly to form the first dispersed phase fluid under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.01:1;
The preparation of the 3rd dispersed phase fluid: under normal pressure, room temperature by n-octyl alcohol and medical soybean oil by volume 1:3 mix to obtain mixed liquor, then in described mixed liquor, add PGPR90, stir and form the 3rd dispersed phase fluid, the amount of described PGPR90 is 0.02g in the mixed liquor of every 1ml n-octyl alcohol and medical soybean oil;
The preparation of the 5th dispersed phase fluid: PGPR90 is added to the formation mixed liquor that stirs in medical soybean oil under normal pressure, room temperature, then form the 5th dispersed phase fluid to adding in described mixed liquor fluorescent dye LR300 to stir, the amount of described PGPR90 is 0.02g in the medical soybean oil of every 1ml, and the amount of described LR300 is 1mg in the medical soybean oil of 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 10cSt.
(2) the single multicomponent O/W/O/O emulsion droplet that disperses of preparation
In the present embodiment, the microfluidic device adopting is identical with embodiment 5, and oil bag fat liquor drop spreads into schematic diagram on Water-In-Oil bag fat liquor drop as shown in Figure 9 in its microchannel and microchannel.
By the 5th dispersed phase fluid of step (1) preparation, the 9th microchannel 19 and the 8th microchannel 18 that continuous phase fluid injects the described single-stage droplet generator of microfluidic device by the syringe that is connected with syringe pump respectively form oil bag fat liquor drop, meanwhile using the 3rd dispersed phase fluid of step (1) preparation as interior phase, the first dispersed phase fluid is as middle phase, continuous phase fluid is injected respectively the 5th microchannel 15 of the described two-stage droplet generator of microfluidic device by the syringe being connected with syringe pump as foreign minister, the 6th microchannel 16 and the 7th microchannel 17 form Water-In-Oil bag fat liquor drop, the Water-In-Oil bag fat liquor drop, the oil bag fat liquor drop that form enter collecting pipe 20 with continuous phase fluid, when oil bag fat liquor drop contacts with the expansion chamber of Water-In-Oil bag fat liquor drop at collecting pipe 20, oil bag fat liquor drop spreads into the single multicomponent O/W/O/O emulsion droplet that disperses of formation on Water-In-Oil bag fat liquor drop,
Embodiment 1: as the flow Q of the first dispersed phase fluid b=150 μ L/h, the flow Q of the 3rd dispersed phase fluid a2=150 μ L/h, the flow Q of the 5th dispersed phase fluid a4=200 μ L/h, the flow Q of continuous phase fluid in described two-stage droplet generator c3=200 μ L/h, flow Q in described single-stage droplet generator c4=300 μ L/h, described oil bag fat liquor drop meets each oil bag fat liquor drop with Water-In-Oil bag fat liquor drop and contact with a Water-In-Oil bag fat liquor drop in the expansion chamber of collecting pipe 20, the oily O/W/O/O emulsion droplet (seeing Figure 29) that wraps fat liquor drop and spread into formation on Water-In-Oil bag fat liquor drop and include a Water-In-Oil bag fat liquor drop;
Embodiment 2: as the flow Q of the first dispersed phase fluid b=100 μ L/h, the flow Q of the 3rd dispersed phase fluid a2=150 μ L/h, the flow Q of the 5th dispersed phase fluid a4=150 μ L/h, the flow Q of continuous phase fluid in described two-stage droplet generator c3=220 μ L/h, flow Q in described single-stage droplet generator c4=500 μ L/h, described oil bag fat liquor drop meets each oil bag fat liquor drop with Water-In-Oil bag fat liquor drop and contact with a Water-In-Oil bag fat liquor drop in the expansion chamber of collecting pipe 20, and oil bag fat liquor drop spreads into formation on Water-In-Oil bag fat liquor drop and include the list dispersion multicomponent O/W/O/O emulsion droplet (seeing Figure 30) of two Water-In-Oil bag fat liquor drops.
(3) collect single multicomponent O/W/O/O emulsion of disperseing
In single dispersion that step (2) is formed, the O/W/O/O emulsion droplet of the different emulsions of bag is introduced in collection container by the efferent duct 10 of microfluidic device together with continuous phase, obtains single multicomponent O/W/O/O emulsion of disperseing.The optical microscope photograph that prepared by embodiment 1 include a Water-In-Oil bag fat liquor drop single disperses multicomponent O/W/O/O emulsion as shown in figure 31.
Embodiment 7
The present embodiment adopts the method for the invention to prepare single dispersed oil bag Water-In-Oil (W/O/O) emulsion of ultra-thin-wall, and synthesize ethoxylated trimethylolpropane triacrylate (ETPTA) micro-capsule with ultra-thin-wall taking it as template, processing step is as follows:
(1) preparation decentralized photo and continuous phase fluid
The preparation of the first dispersed phase fluid: SDS is added deionized water for stirring evenly to form the first dispersed phase fluid under normal pressure, room temperature, the mass ratio of described SDS and deionized water is 0.01:1;
The preparation of the 6th dispersed phase fluid: light trigger 2-hydroxy-2-methyl propiophenone is added in ethoxylated trimethylolpropane triacrylate (its number-average molecular weight Mn is 692) under normal pressure, room temperature, stir and form the 6th dispersed phase fluid, the volume ratio of described 2-hydroxy-2-methyl propiophenone and ETPTA is 1:100;
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 10cSt.
(2) the single W/O/O emulsion droplet that disperses of preparation
In the present embodiment, the microfluidic device adopting is with embodiment 1.
The first microchannel 11 and the second microchannel 12 that the 6th dispersed phase fluid of step (1) preparation and continuous phase fluid are injected to microfluidic device the first single-stage droplet generator by the syringe 8 being connected with syringe pump respectively form single dispersed oil bag fat liquor drop, and the 3rd microchannel 13 and the 4th microchannel 14 that the first dispersed phase fluid of step (1) preparation and continuous phase fluid are injected to microfluidic device the second single-stage droplet generator by the syringe 8 being connected with syringe pump respectively form single water-in-oil emulsion drop that disperses simultaneously; The oil bag fat liquor drop forming, water-in-oil emulsion drop enters microfluidic device collecting pipe 20 with continuous phase fluid, as the flow Q of the first dispersed phase fluid b=300 μ L/h, the flow Q of the 6th dispersed phase fluid a5=40 μ L/h, the flow Q of continuous phase fluid in the first single-stage droplet generator c1=300 μ L/h, flow Q in the second single-stage droplet generator c2=300 μ L/h, described oil bag fat liquor drop meets each oil bag fat liquor drop and contacts with a water-in-oil emulsion drop in the expansion chamber of collecting pipe 20 with water-in-oil emulsion drop, oil bag fat liquor drop spreads on water-in-oil emulsion drop and forms the single W/O/O of dispersion emulsion droplet, and wherein the middle oil reservoir of W/O/O emulsion droplet is ETPTA and light trigger 2-hydroxy-2-methyl propiophenone;
(3) collecting list disperses W/O/O emulsion and causes ETPTA to aggregate into micro-capsule
The single W/O/O of dispersion emulsion droplet that step (2) is formed is introduced in collection container by the efferent duct 10 of microfluidic device together with continuous phase, obtains the single W/O/O of dispersion emulsion.Then gained list disperses W/O/O emulsion to be placed in to irradiate 5min under the uviol lamp of 200W to be solidified into ETPTA micro-capsule, and its stereoscan photograph is shown in Figure 32 and Figure 33, the ETPTA micro-capsule of preparing taking W/O/O emulsion as template there is ultra-thin-wall structure, its wall thickness is only 300nm.

Claims (5)

1. a single preparation method who disperses multicomponent multiple emulsion, is characterized in that processing step is as follows:
(1) preparation decentralized photo and continuous phase fluid
The preparation of the first dispersed phase fluid: water soluble emulsifier is added deionized water for stirring evenly to form the first dispersed 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 dispersed phase fluid: stir in oil soluble emulsifying agent being added to soybean oil under normal pressure, room temperature and form the second dispersed phase fluid, the amount of described oil soluble emulsifying agent is 0.005～0.02g in every 1ml soybean oil;
The preparation of the 3rd dispersed phase fluid: under normal pressure, room temperature by n-octyl alcohol and soybean oil by volume 1:3 mix to obtain mixed liquor, then in described mixed liquor, add oil soluble emulsifying agent, stir and form the 3rd dispersed phase fluid, the amount of described oil soluble emulsifying agent is 0.005～0.02g in the mixed liquor of every 1ml n-octyl alcohol and soybean oil;
The preparation of the 4th dispersed phase fluid: identical with the compound method of described the 3rd dispersed phase fluid, in described the 4th dispersed phase fluid and the 5th dispersed phase fluid, also contain dyestuff;
The preparation of the 5th dispersed phase fluid: identical with the compound method of described the second dispersed phase fluid;
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) the single multicomponent multiple emulsion drop that disperses of preparation
One of adopt with the following method the single multicomponent multiple emulsion drop that disperses of preparation:
Method one: the single multicomponent oil bag water-in-oil emulsion drop that disperses of preparation
The different inlets that the second dispersed phase fluid that step (1) is prepared and continuous phase fluid inject respectively the first single-stage droplet generator of microfluidic device form single dispersed oil bag fat liquor drop, and the different inlets that the first dispersed phase fluid of meanwhile step (1) being prepared and continuous phase fluid inject respectively the second single-stage droplet generator of microfluidic device form single water-in-oil emulsion drops that disperse; The oil bag fat liquor drop forming, water-in-oil emulsion drop enters microfluidic device collecting pipe with continuous phase fluid, when oil bag fat liquor drop contacts with the expansion chamber of water-in-oil emulsion drop at described collecting pipe, oil bag fat liquor drop spreads into the single multicomponent oil bag water-in-oil emulsion drop that disperses of formation on water-in-oil emulsion drop;
Flow (the Q of described the first dispersed phase fluid b) be 100～300 μ L/h, the flow (Q of described the second dispersed phase fluid a1) be 20～80 μ L/h, the flow (Q of described continuous phase fluid in the first single-stage droplet generator c1) be 40～200 μ L/h, flow (Q in the second single-stage droplet generator c2) be 200～500 μ L/h;
Method two: the single multicomponent Water-In-Oil bag fat liquor drop that disperses of preparation
The different inlets that the 3rd dispersed phase fluid that step (1) is prepared and continuous phase fluid inject respectively the first single-stage droplet generator of microfluidic device form single dispersed oil bag fat liquor drop, and the different inlets that the first dispersed phase fluid of meanwhile step (1) being prepared and continuous phase fluid inject respectively the second single-stage droplet generator of microfluidic device form single water-in-oil emulsion drops that disperse; The water-in-oil emulsion drop forming, oil bag fat liquor drop enters microfluidic device collecting pipe with continuous phase fluid, when water-in-oil emulsion drop contacts with the expansion chamber of oil bag fat liquor drop at described collecting pipe, water-in-oil emulsion drop spreads into the single multicomponent Water-In-Oil bag fat liquor drop that disperses of formation on oil bag fat liquor drop;
Flow (the Q of described the first dispersed phase fluid b) be 100～150 μ L/h, the flow (Q of described the 3rd dispersed phase fluid a2) be 50～90 μ L/h, the flow (Q of described continuous phase fluid in the first single-stage droplet generator c1) be 100～150 μ L/h, flow (Q in the second single-stage droplet generator c2) be 200～400 μ L/h;
Method three: the single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse of preparation
The different inlets that the 3rd dispersed phase fluid, the 4th dispersed phase fluid and the continuous phase fluid of step (1) preparation injected respectively to the first single-stage droplet generator of microfluidic device form two kinds of single dispersed oil bag fat liquor drops simultaneously, and the different inlets that the first dispersed phase fluid of simultaneously step (1) being prepared and continuous phase fluid inject respectively the second single-stage droplet generator of microfluidic device form single water-in-oil emulsion drops that disperse; Two kinds of single dispersed oil bag fat liquor drops that form, single collecting pipe that disperses water-in-oil emulsion drop to enter microfluidic device with continuous phase fluid, when water-in-oil emulsion drop contacts with the expansion chamber of two kinds of oil bag fat liquor drops at described collecting pipe, water-in-oil emulsion drop spreads into the single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse of formation on two kinds of oil bag fat liquor drops;
Flow (the Q of described the 3rd dispersed phase fluid a2) be 20 μ L/h, the flow (Q of described the 4th dispersed phase fluid a3) be 20 μ L/h, the flow (Q of described the first dispersed phase fluid b) be 150 μ L/h, the flow (Q of described continuous phase fluid in the first single-stage droplet generator c1) be 200 μ L/h, flow (Q in the second single-stage droplet generator c2) be 400 μ L/h;
Or adopt the single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse of following methods preparation:
The different inlets of the 4th dispersed phase fluid that step (1) is prepared, the single-stage droplet generator that continuous phase fluid injects respectively microfluidic device form oil bag fat liquor drops, and the different inlets that meanwhile the 3rd dispersed phase fluid of step (1) preparation respectively injected to the two-stage droplet generator of microfluidic device as middle phase, continuous phase fluid as foreign minister as interior phase, the first dispersed phase fluid form Water-In-Oil bag fat liquor drop; The Water-In-Oil bag fat liquor drop forming, oil bag fat liquor drop enters microfluidic device collecting pipe with continuous phase fluid, when Water-In-Oil bag fat liquor drop contacts with the expansion chamber of oil bag fat liquor drop at described collecting pipe, the water layer of Water-In-Oil bag fat liquor drop spreads into the single different oily core emulsion droplets of multicomponent Water-In-Oil bag that disperse of formation on oil bag fat liquor drop;
Flow (the Q of described the first dispersed phase fluid b) be 150 μ L/h, the flow (Q of described the 3rd dispersed phase fluid a2) be 150 μ L/h, the flow (Q of described the 4th dispersed phase fluid a3) be 50～200 μ L/h, the flow (Q of described continuous phase fluid in single-stage droplet generator c4) be 100～300 μ L/h, flow (Q in two-stage droplet generator c3) be 300 μ L/h;
Method four: the single multicomponent oil bag Water-In-Oil bag fat liquor drop that disperses of preparation
The different inlets of the 5th dispersed phase fluid that step (1) is prepared, the single-stage droplet generator that continuous phase fluid injects respectively microfluidic device form oil bag fat liquor drops, and the different inlets that meanwhile the 3rd dispersed phase fluid of step (1) preparation respectively injected to the two-stage droplet generator of microfluidic device as middle phase, continuous phase fluid as foreign minister as interior phase, the first dispersed phase fluid form Water-In-Oil bag fat liquor drop; The Water-In-Oil bag fat liquor drop forming, oil bag fat liquor drop enters microfluidic device collecting pipe with continuous phase fluid, when oil bag fat liquor drop contacts with the expansion chamber of Water-In-Oil bag fat liquor drop at described collecting pipe, oil bag fat liquor drop spreads into the single multicomponent oil bag Water-In-Oil bag fat liquor drop that disperses of formation on Water-In-Oil bag fat liquor drop;
Flow (the Q of described the first dispersed phase fluid b) be 100～150 μ L/h, the flow (Q of described the 3rd dispersed phase fluid a2) be 150 μ L/h, the flow (Q of described the 5th dispersed phase fluid a4) be 150～200 μ L/h, the flow (Q of described continuous phase fluid in single-stage droplet generator c4) be 200～220 μ L/h, flow (Q in two-stage droplet generator c3) be 300～500 μ L/h;
(3) collect single multicomponent multiple emulsion that disperses
Single multicomponent multiple emulsion drop that disperses that step (2) is formed is introduced in collection container by the efferent duct of microfluidic device together with continuous phase, obtains single multicomponent multiple emulsion that disperses of respective type.
2. the preparation method who singly disperses according to claim 1 multicomponent multiple emulsion, is characterized in that described water soluble emulsifier is the addition polymers of lauryl sodium sulfate or polypropylene glycol and oxirane.
3. singly disperse according to claim 1 the preparation method of multicomponent multiple emulsion, 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. singly disperse according to claim 1 the preparation method of multicomponent multiple emulsion, it is characterized in that described surfactant is the mixture of trimethicone and cyclohexyl methyl siloxanes composition, the volume ratio of trimethicone and cyclohexyl methyl siloxanes is 1:1.
5. according to single preparation method who disperses multicomponent multiple emulsion described in arbitrary claim in claim 1 to 4, it is characterized in that single external diameter that disperses emulsion droplet in multicomponent multiple emulsion prepared by the method is 100～500 μ m.
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