CN102895927A - Grain size controllable monodisperse polyvinyl alcohol gel microsphere, preparation method thereof and applied device - Google Patents
Grain size controllable monodisperse polyvinyl alcohol gel microsphere, preparation method thereof and applied device Download PDFInfo
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Abstract
The invention relates to a preparation method for a grain size controllable monodisperse polyvinyl alcohol gel microsphere. The preparation method comprises the following steps: preparing a disperse phase solution and a continuous phase solution; controlling the flowing speed, flow and viscosity of the disperse phase and the continuous phase; obtaining polyvinyl alcohol solution drops in different grain sizes and in uniform diameter size after converging the disperse phase with the continuous phase; and solidifying the drops, thereby obtaining the grain size controllable monodisperse polyvinyl alcohol gel microspheres. The invention also relates to a preparation device for the grain size controllable monodisperse polyvinyl alcohol gel microsphere and the prepared monodisperse polyvinyl alcohol gel microsphere. The microsphere prepared according to the invention has a better surface morphology and a grain size range of 50-600 microns. The preparation device is convenient to assemble and disassemble; the size controllable preparation for a monodisperse polyacrylamide microsphere is realized by changing the size of a capillary tube or controlling the flowing speed or viscosity of the disperse phase and the continuous phase; and the grain size distribution coefficient CV is less than 5%.
Description
Technical field
The present invention relates to the preparation field of mono-dispersion microballoon, relate in particular to controlled single dispersion polyethylene alcogel microballoon of a kind of particle diameter and preparation method thereof and equipment therefor.
Background technology
Polyvinyl alcohol (PVA) gel micro-ball has nontoxic and good characteristics of biocompatibility, is widely used in the control drug releasing rate, prolongs action effective, to aspects such as particular organization and the releases of organ target.The using emulsion polymerization techniques such as Zhao Daqing take aldehyde or borax as crosslinking agent, obtain the PVA gel micro-ball, but this technology can only be used the PVA solution of low concentration, cause the mechanical property of PVA gel micro-ball not enough.Gao Suzhao etc. adopt high voltage electrostatic technique to obtain the PVA gel micro-ball for the preparation of porous three-dimensional cytoskeleton, and this method gained PVA microballoon is physical crosslinking, can again be dissolved in the water through microwave treatment.
The PVA gel micro-ball also is widely used in and carries out arterial embolism, treatment malignant tumour, fibroid, hepatic hemangioma, hyperthyroidism, acute gastrointestinal bleeding etc.By the super arterial embolism of selecting, make the supply artery of the tumor locking, the nutrition of cutting off tumour cell causes tumor tissue necrosis.If contain antineoplastic in the microballoon, then can greatly improve the curative effect of medicine, reduce its toxic and side effect for some inoperable malignant tumor patients, technique has more special meaning.Wei Shuli etc. have prepared PVA microballoon and 5 FU 5 fluorouracil PVA microballoon with emulsion polymerization method, and 90.2% microsphere diameter of PVA microballoon is 71.5 μ m in 50 ~ 100 mu m range average diameters.The PVA gel micro-ball particle diameter that Boschetti etc. (US Patent No. 7,670,592) prepare take formaldehyde as crosslinking agent with emulsion polymerization method reaches hundreds of microns, adopts mechanical mixing method formation W/O emulsion and crosslinking curing to become microballoon.This emulsion polymerization method because the difficulty of the uniform drop of control generation particle diameter is larger, solidifies rear thus obtained microsphere particle diameter wider distribution when the tens of extremely hundreds of microns microballoons of preparation, be difficult to obtain the mono-dispersion microballoon of size homogeneous.And particle diameter is difficult for by cytophagy at tens polymer microballoons to the hundreds of micron, and the pharmaceutical release time with targeting and load is long, has advantage as the pharmaceutical carrier in the oncotherapy.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide the preparation method of the controlled single dispersion polyethylene alcogel microballoon of a kind of particle diameter.
Single dispersion polyethylene alcogel microballoon of providing a kind of particle diameter controlled is provided.
An also purpose of the present invention is to provide the above-mentioned particle diameter of preparation the controlled used device of single dispersion polyethylene alcogel microballoon.
In order to realize purpose of the present invention, the invention provides the preparation method of the controlled single dispersion polyethylene alcogel microballoon of a kind of particle diameter, its step is as follows: preparation coagulating bath solution, decentralized photo solution and continuous phase solution, flow velocity and the viscosity of control decentralized photo and continuous phase, after decentralized photo and continuous phase are converged, obtain the poly-vinyl alcohol solution drop of particle diameter difference and diameter dimension homogeneous, described drop is by solidifying to get the controlled single dispersion polyethylene alcogel microballoon of particle diameter.
More specifically, the method may further comprise the steps:
(1) preparation of coagulating bath solution: in proportion boron-containing compound is added in the mixed liquor of pure and mild amino alcohol, magnetic agitation and heating make its dissolving, and preparation boron compound concentration is 0.005 ~ 0.050gmL
-1Coagulating bath solution;
(2) preparation of decentralized photo and continuous phase: an amount of polyvinyl alcohol is added in the deionized water, and magnetic agitation and heating make its dissolving, and preparation polyvinyl alcohol percentage by weight is 2% ~ 10% decentralized photo solution; To hang down polar compound and mix with alcohol, the low polar compound of preparation and pure volume ratio are 100: 0 ~ 250 continuous phase solution;
(3) flow velocity and the viscosity of adjustment decentralized photo and continuous phase: control decentralized photo flow rates is 20 ~ 300mmmin
-1, the continuous phase flow rates is 20 ~ 300mmmin
-1, the dispersed phase viscosity scope is 1 ~ 500mPas, the continuous phase range of viscosities is 50 ~ 2500mPas;
(4) formation of polyvinyl alcohol drop: after step (2) gained decentralized photo solution and continuous phase solution are converged, can obtain the poly-vinyl alcohol solution drop of particle diameter difference and diameter dimension homogeneous;
(5) drop is solidified into microballoon: the drop of collecting step (4) gained in step (1) prepare in the coagulating bath solution, behind the curing reaction, the gained drop can be solidified into the controlled single dispersion polyethylene alcohol hydrogel microsphere of particle diameter.
Wherein, the boron compound described in the step (1) is preferably borax or boric acid; Alcohol is preferably isoamyl alcohol, isooctanol or hexanol; Amino alcohol is preferably triethanolamine or diethanol amine; The volume ratio of pure and mild amino alcohol is preferably 2: 1; Described heating refers to slowly be heated to 60 ℃.
Wherein, low polar compound is preferably silicone oil, soybean oil or salad oil, more preferably silicone oil described in the step (2); Described alcohol is preferably one or both in isoamyl alcohol, the isooctanol, more preferably isoamyl alcohol and isooctanol mixture; Described heating refers to slowly be heated to 90 ℃.
The time of curing reaction described in the step (5) is 2 ~ 8 hours.
Described preparation method also comprises the post processing of step (6) polyvinyl alcohol hydrogel microballoon: after the filtration of polyvinyl alcohol hydrogel microballoon process or decantation (decant) with step (5) gained, residual organic solution with organic solvent washing for several times, place water-soluble solvent to soak a couple of days, the elimination solvent, drying namely gets monodispersity polyvinyl alcohol gel microballoon.
Described organic solvent refers to nonpolar and weakly polar organic solvent, is preferably hexane, benzinum, carrene, chloroform, or the mixed solvent that forms of the water-soluble solvents such as hexane, benzinum, carrene, chloroform and methyl alcohol, ethanol, acetone.
The present invention further provides the controlled single dispersion polyethylene alcogel microballoon of particle diameter of said method preparation.The particle size range of described single dispersion polyethylene alcogel microballoon is 50 ~ 600 μ m, and coefficient of dispersion CV is less than 5%.
The present invention further provides above-mentioned preparation method used microfluidic control device, it comprises decentralized photo syringe, continuous phase syringe, decentralized photo syringe pump, continuous phase syringe pump, T-shaped threeway, returnable, described decentralized photo syringe and continuous phase syringe are installed in respectively on decentralized photo syringe pump and the continuous phase syringe pump, and are connected with two ports of T-shaped threeway by conduit respectively; The 3rd port of described T-shaped threeway is communicated with conduit, and the liquid in described decentralized photo syringe and the continuous phase syringe flows in the returnable after this conduit compiles and is cured.
Wherein, be provided with internal thread in three of described T-shaped threeway ports; Described continuous phase syringe is provided with the external screw thread that matches well mutually with T-shaped threeway port internal thread with the outside, termination of T-shaped threeway connecting duct;
The conduit that described decentralized photo syringe is connected with T-shaped threeway is capillary, described decentralized photo syringe is provided with closed casing with the interface that T-shaped threeway is connected, the end outside that closed casing is connected with T-shaped threeway is provided with the external screw thread that matches well mutually with T-shaped threeway port internal thread, the end face of closed casing is the sealing surface with a through hole, and the diameter of described through hole and overall diameter capillaceous are complementary; Described capillary passes described closed casing and is inserted in the conduit that is communicated with described T-shaped threeway the 3rd port;
The outside, termination of the 3rd port connecting tube of described T-shaped threeway is provided with the external screw thread that matches well mutually with T-shaped threeway port internal thread.
Preferably, described connecting duct is preferably polyfluortetraethylene pipe;
Preferred, the conduit external diameter that described continuous phase syringe is connected with T-shaped threeway is 1600um, and internal diameter is 1000um; The conduit capillary external diameter that described decentralized photo syringe is connected with T-shaped threeway is 160 ~ 750um, and internal diameter is 20 ~ 540um; The conduit external diameter that the 3rd port of described T-shaped threeway is communicated with is 1600 ~ 3200 μ m, and internal diameter is 500～1600 μ m.
The principle that said apparatus prepares the controlled single dispersion polyethylene alcogel microballoon of particle diameter is as follows: the decentralized photo solution and the continuous phase solution that prepare are respectively charged in decentralized photo and the continuous phase syringe, and place respectively on decentralized photo and the continuous phase syringe pump, by adjusting fltting speed and the decentralized photo size capillaceous of syringe pump, control flow velocity, flow and the viscosity of decentralized photo and continuous phase, can obtain the poly-vinyl alcohol solution drop of particle diameter difference and diameter dimension homogeneous.
The present invention adopts the microfluidic control device to prepare the controlled single dispersion polyethylene alcogel microballoon of particle diameter.As the poly-vinyl alcohol solution of decentralized photo in the dirty capillary that enters in the microfluidic controller of the promotion of syringe pump, in outflow port capillaceous, when decentralized photo liquid flows out, the viscous force of the continuous phase that flows causes decentralized photo liquid to be sheared into drop at the outflow port place with the surface tension interaction result between the liquid, the diameter of drop is subjected to the surface tension of decentralized photo and continuous phase, viscosity, flow velocity, the impact of the factors such as capillary outlet end size, under fixing above-mentioned preparation parameter, can obtain continuously the poly-vinyl alcohol solution drop of size homogeneous, through obtaining the polyvinyl alcohol gel microballoon of monodispersity after the cross-linking reaction.Reduce capillary diameter, increase flow velocity or the viscosity of continuous phase, reduce the decentralized photo flow velocity, the size that can cause the final polyvinyl alcohol gel microballoon that obtains is corresponding reducing also, so can be simply and easily by changing capillary size, continuous phase and decentralized photo flow velocity and viscosity realize the controlled preparation of single dispersion polyethylene alcogel microballoon.
Single dispersion polyethylene alcogel microsphere surface form of the present invention's preparation is better, and particle size range is 50 ~ 600 μ m; This preparation facilities assembles and dismantles easy, and by adjusting the capillary size that decentralized photo is flowed through in the microfluidic controller, continuous phase and decentralized photo flow velocity and viscosity can be regulated and control the size of prepared microballoon easily.Microballoon need not heat at normal temperatures and can solidify by Quick cross-linking, and energy consumption is little, weak point consuming time, and cost is low, has widened the application of PVA gel micro-ball at field of medicaments.
Description of drawings
Fig. 1 is the optical microphotograph picture of the polyvinyl alcohol microparticles of embodiment 1 preparation, and scale is 200 μ m;
Fig. 2 is the optical microphotograph picture of the polyvinyl alcohol microparticles of embodiment 2 preparations, and scale is 200 μ m;
Fig. 3 is the optical microphotograph picture of the polyvinyl alcohol microparticles of embodiment 3 preparations, and scale is 200 μ m;
Fig. 4 is the optical microphotograph picture of the polyvinyl alcohol microparticles of embodiment 4 preparations, and scale is 200 μ m;
Fig. 5 is the optical microphotograph picture of the polyvinyl alcohol microparticles of embodiment 5 preparations, and scale is 200 μ m;
Fig. 6 is microfluidic control device schematic diagram of the present invention;
Fig. 7 is microfluidic control device A of the present invention position enlarged diagram;
Among the figure, 1-1 continuous phase syringe pump; 1-2 decentralized photo syringe pump; 2-1 continuous phase syringe; 2-2 decentralized photo syringe; The 3-capillary; 4-continuous phase conduit; The threeway of 5-T type; The 6-output duct; 7-poly-vinyl alcohol solution drop; The 8-returnable; The 9-coagulating bath; The 10-closed casing; The 11-dispersant liquid drop.
The specific embodiment
Below in conjunction with specific embodiment, further set forth related content of the present invention.It is to be noted, these embodiment only are not used in for explanation the present invention and limit the scope of the invention, and, after having read content of the present invention, the relevant technical staff in the field can make various changes or modification to the present invention, and these equivalent form of values fall into the application's appended claims limited range equally.
Embodiment 1
The 0.5g borax is joined in the mixture of 10mL isoamyl alcohol and 5mL triethanolamine, also slowly be heated to 60 ℃ makes its dissolving to magnetic agitation, is mixed with coagulating bath solution.
The 1.0g polyvinyl alcohol is joined in the beaker that contains the 12.5mL deionized water, and also slowly be heated to 90 ℃ makes its dissolving to magnetic agitation, makes decentralized photo solution; 30mL silicone oil and 20mL isooctanol are mixed, obtain continuous phase solution.
Above-mentioned decentralized photo solution and continuous phase solution are respectively charged in the syringe of 1mL and 50mL, place on two boost pumps, connect microfluidic controller, it is 26mmmin that the decentralized photo flow velocity is set
-1, viscosity 160mPas, continuous phase flow velocity are 200mmmin
-1, viscosity 540mPas, capillary size is: external diameter/internal diameter 165/98 μ m, open the microfluidic control device, prepare single dispersion polyethylene alcoholic solution drop; Collect the drop of generation in the culture dish that above-mentioned coagulating bath solution is housed, slowly stir curing reaction 4h under the room temperature, drop can be solidified into the polyvinyl alcohol hydrogel microballon.Through behind the simple decantation, residual organic solution is washed 4 times with 1: 1 (volume ratio) mixed liquor of chloroform and ethanol, with after the ethanol washing 2 times, places ethanol to soak 4 days again, elimination ethanol, and drying namely gets single dispersion polyethylene alcogel microballoon.Fig. 1 is the optical microphotograph picture of thus obtained microsphere, can find out the microspherulite diameter homogeneous, has monodispersity, and particle diameter is 50 μ m.
Embodiment 2
The 0.5g borax is joined in the mixture of 10mL isoamyl alcohol and 5mL triethanolamine, also slowly be heated to 60 ℃ makes its dissolving to magnetic agitation, is mixed with coagulating bath solution.
The 1.0g polyvinyl alcohol is joined in the beaker that contains the 12.5mL deionized water, and also slowly be heated to 90 ℃ makes its dissolving to magnetic agitation, makes decentralized photo solution; 30mL silicone oil and 20mL isooctanol are mixed, obtain continuous phase solution.
Above-mentioned decentralized photo solution and continuous phase solution are respectively charged in the syringe of 1mL and 50mL, place on two boost pumps, behind the connection micro passage reaction, it is 72mmmin that the decentralized photo flow velocity is set
-1, viscosity 160mPas, continuous phase flow velocity are 127mmmin
-1, viscosity 540mPas, capillary size is: external diameter/internal diameter 245/98 μ m, open the microfluidic control device, prepare single dispersion polyethylene alcoholic solution drop; Collect the drop of generation in the culture dish that above-mentioned coagulating bath solution is housed, slowly stir curing reaction 4h under the room temperature, drop can be solidified into the polyvinyl alcohol hydrogel microballon.Through behind the simple decantation, residual organic solution is washed 4 times times with 1: 1 (volume ratio) mixed liquor of chloroform and ethanol, with after the ethanol washing 2 times, places ethanol to soak 4 days again, elimination ethanol, and drying namely gets single dispersion polyethylene alcogel microballoon.Fig. 2 is the optical microphotograph picture of thus obtained microsphere, can find out the microspherulite diameter homogeneous, has monodispersity, and particle diameter is 270 μ m.
The 0.5g borax is joined in the mixture of 10mL isoamyl alcohol and 5mL triethanolamine, also slowly be heated to 60 ℃ makes its dissolving to magnetic agitation, is mixed with coagulating bath solution.
The 1.0g polyvinyl alcohol is joined in the beaker that contains the 12.5mL deionized water, and also slowly be heated to 90 ℃ makes its dissolving to magnetic agitation, makes decentralized photo solution; 30mL silicone oil and 20mL isooctanol are mixed, obtain continuous phase solution.
Above-mentioned decentralized photo solution and continuous phase solution are respectively charged in the syringe of 1mL and 50mL, place on two boost pumps, behind the connection micro passage reaction, it is 264mmmin that the decentralized photo flow velocity is set
-1, viscosity 160mPas, continuous phase flow velocity are 46mmmin
-1, viscosity 540mPas, capillary size is: external diameter/internal diameter 360/225 μ m, open the microfluidic control device, prepare single dispersion polyethylene alcoholic solution drop; Collect the drop of generation in the culture dish that above-mentioned coagulating bath solution is housed, slowly stir curing reaction 4h under the lower room temperature, drop can be solidified into the polyvinyl alcohol hydrogel microballon.Through behind the simple decantation, residual organic solution is washed 4 times times with 1: 1 (volume ratio) mixed liquor of chloroform and ethanol, with after the ethanol washing 2 times, places ethanol to soak 4 days again, elimination ethanol, and drying namely gets single dispersion polyethylene alcogel microballoon.Fig. 3 is the optical microphotograph picture of thus obtained microsphere, can find out the microspherulite diameter homogeneous, has monodispersity, and particle diameter is 580 μ m.
Embodiment 4
The 0.5g borax is joined in the mixture of 10mL isoamyl alcohol and 5mL diethanol amine, also slowly be heated to 60 ℃ makes its dissolving to magnetic agitation, is mixed with coagulating bath solution.
The 1.0g polyvinyl alcohol is joined in the beaker that contains the 10mL deionized water, and also slowly be heated to 90 ℃ makes its dissolving to magnetic agitation, makes decentralized photo solution; 30mL soybean oil and 30mL isoamyl alcohol are mixed, obtain continuous phase solution.
Above-mentioned decentralized photo solution and continuous phase solution are respectively charged in the syringe of 1mL and 50mL, place on two boost pumps, connect microfluidic controller, it is 72mmmin that the decentralized photo flow velocity is set
-1, viscosity 110mPas, continuous phase flow velocity are 140mmmin
-1, viscosity 540mPas, capillary size is: external diameter/internal diameter 245/98 μ m, open the microfluidic control device, prepare single dispersion polyethylene alcoholic solution drop; Collect the drop of generation in the culture dish that above-mentioned coagulating bath solution is housed, slowly stir curing reaction 5h under the room temperature, drop can be solidified into the polyvinyl alcohol hydrogel microballon.Through behind the simple decantation, residual organic solution is washed 4 times with 1: 1 (volume ratio) mixed liquor of chloroform and ethanol, with after the ethanol washing 2 times, places ethanol to soak 4 days again, elimination ethanol, and drying namely gets single dispersion polyethylene alcogel microballoon.Fig. 4 is the optical microphotograph picture of thus obtained microsphere, can find out the microspherulite diameter homogeneous, has monodispersity, and particle diameter is 240 μ m.
Embodiment 5
The 0.5g borax is joined in the mixture of 50mL isoamyl alcohol and 25mL triethanolamine, also slowly be heated to 60 ℃ makes its dissolving to magnetic agitation, is mixed with coagulating bath solution.
The 1.0g polyvinyl alcohol is joined in the beaker that contains the 12.5mL deionized water, and also slowly be heated to 90 ℃ makes its dissolving to magnetic agitation, makes decentralized photo solution; 30mL salad oil and 30mL isooctanol are mixed, obtain continuous phase solution.
Above-mentioned decentralized photo solution and continuous phase solution are respectively charged in the syringe of 1mL and 50mL, place on two boost pumps, connect microfluidic controller, it is 72mmmin that the decentralized photo flow velocity is set
-1, viscosity 75mPas, continuous phase flow velocity are 140mmmin
-1, viscosity 540mPas, capillary size is: external diameter/internal diameter 245/98 μ m, open the microfluidic control device, prepare single dispersion polyethylene alcoholic solution drop; Collect the drop of generation in the culture dish that above-mentioned coagulating bath solution is housed, slowly stir curing reaction 3h under the room temperature, drop can be solidified into the polyvinyl alcohol hydrogel microballon.Through behind the simple decantation, residual organic solution is washed 4 times with 1: 1 (volume ratio) mixed liquor of chloroform and ethanol, with after the ethanol washing 2 times, places ethanol to soak 4 days again, elimination ethanol, and drying namely gets single dispersion polyethylene alcogel microballoon.Fig. 5 is the optical microphotograph picture of thus obtained microsphere, can find out the microspherulite diameter homogeneous, has monodispersity, and particle diameter is 315 μ m.
As shown in Figure 6 and Figure 7, a kind of microfluidic control device, it comprises decentralized photo syringe 2-2, continuous phase syringe 2-1, decentralized photo syringe pump 1-2, continuous phase syringe pump 1-1, T-shaped threeway 5, returnable 8, described decentralized photo syringe 2-2 and continuous phase syringe 2-1 are installed in respectively on decentralized photo syringe pump 1-2 and the continuous phase syringe pump 1-1, and are connected with two ports of T-shaped threeway 5 by conduit respectively; Wherein, the 3rd port of T-shaped threeway 5 is communicated with conduit, and the liquid in described decentralized photo syringe and the continuous phase syringe flows into returnable after compiling in this conduit.
Wherein, be provided with internal thread in 5 three ports of described T-shaped threeway; Described continuous phase syringe 2-1 is provided with the external screw thread that matches well mutually with T-shaped threeway 5 port internal threads with the outside, termination of T-shaped threeway 5 connecting ducts;
The conduit that described decentralized photo syringe 2-2 is connected with T-shaped threeway 5 is capillary 3, described decentralized photo syringe 2-2 is provided with closed casing 10 with the interface that T-shaped threeway 5 is connected, the end outside that closed casing 10 is connected with T-shaped threeway 5 is provided with the external screw thread that matches well mutually with T-shaped threeway 5 port internal threads, the end face of closed casing 10 is the sealing surface with a through hole, and the diameter of described through hole and overall diameter capillaceous are complementary;
The outside, termination of the 3rd port connecting tube of described T-shaped threeway 5 is provided with the external screw thread that matches well mutually with T-shaped threeway 5 port internal threads.
The above only is preferred embodiment of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. the preparation method of the controlled single dispersion polyethylene alcogel microballoon of a particle diameter, its step is as follows: preparation coagulating bath solution, decentralized photo solution and continuous phase solution, flow velocity and the viscosity of control decentralized photo and continuous phase, after decentralized photo and continuous phase are converged, obtain the poly-vinyl alcohol solution drop of particle diameter difference and diameter dimension homogeneous, described drop is by solidifying to get the controlled single dispersion polyethylene alcogel microballoon of particle diameter.
2. the method for claim 1, it specifically may further comprise the steps:
(1) preparation of coagulating bath solution: in proportion boron-containing compound is added in the mixed liquor of pure and mild amino alcohol, magnetic agitation and heating make its dissolving, and preparation boron compound concentration is 0.005 ~ 0.050gmL
-1Coagulating bath solution;
(2) preparation of decentralized photo and continuous phase: an amount of polyvinyl alcohol is added in the deionized water, and magnetic agitation and heating make its dissolving, and preparation polyvinyl alcohol percentage by weight is 2% ~ 10% decentralized photo solution; To hang down polar compound and mix with alcohol, the low polar compound of preparation and pure volume ratio are 100: 0 ~ 250 continuous phase solution;
(3) flow velocity and the viscosity of adjustment decentralized photo and continuous phase: control decentralized photo flow rates is 20 ~ 300mmmin
-1, the continuous phase flow rates is 20 ~ 300mmmin
-1, the dispersed phase viscosity scope is 1 ~ 500mPas, the continuous phase range of viscosities is 50 ~ 2500mPas;
(4) formation of polyvinyl alcohol drop: after step (2) gained decentralized photo solution and continuous phase solution are converged, can obtain the poly-vinyl alcohol solution drop of particle diameter difference and diameter dimension homogeneous;
(5) drop is solidified into microballoon: collect the drop of step (4) gained in the coagulating bath solution that step (1) prepares, behind the curing reaction, drop can be solidified into the controlled single dispersion polyethylene alcogel microballoon of particle diameter.
3. method as claimed in claim 2 is characterized in that, the described boron compound of step (1) is borax or boric acid; Alcohol is isoamyl alcohol, isooctanol or hexanol; Amino alcohol is triethanolamine or diethanol amine; The volume ratio of pure and mild amino alcohol is 2: 1; The described heating of step (1) refers to slowly be heated to 60 ℃.
4. method as claimed in claim 2 is characterized in that, low polar compound is silicone oil, soybean oil or salad oil described in the step (2); Described alcohol is one or both in isoamyl alcohol, the isooctanol; The described heating of step (2) refers to slowly be heated to 90 ℃.
5. method as claimed in claim 2 is characterized in that, the time of curing reaction described in the step (5) is 2 ~ 8 hours.
6. method as claimed in claim 2, it is characterized in that, described preparation method also comprises the post processing of step (6) polyvinyl alcohol hydrogel microballoon: after the filtration of polyvinyl alcohol hydrogel microballoon process or decantation with step (5) gained, residual organic solution with organic solvent washing for several times, place water-soluble solvent to soak a couple of days, the elimination solvent, drying namely gets monodispersity polyvinyl alcohol gel microballoon.
7. method as claimed in claim 6 is characterized in that, described water-soluble solvent is one or more in methyl alcohol, ethanol, the acetone; Described organic solvent refers to nonpolar and weakly polar organic solvent.
8. the controlled single dispersion polyethylene alcogel microballoon of particle diameter that obtains of the described preparation method of claim 1 ~ 7 any one.
9. single dispersion polyethylene alcogel microballoon as claimed in claim 8 is characterized in that the particle size range of described single dispersion polyethylene alcogel microballoon is 50 ~ 600 μ m, and coefficient of dispersion CV is less than 5%.
10. prepare the used microfluidic control device of the described gel micro-ball of claim 8, it comprises decentralized photo syringe, continuous phase syringe, decentralized photo syringe pump, continuous phase syringe pump, T-shaped threeway, returnable, described decentralized photo syringe and continuous phase syringe are installed in respectively on decentralized photo syringe pump and the continuous phase syringe pump, and are connected with two ports of T-shaped threeway by conduit respectively; The 3rd port of described T-shaped threeway is communicated with conduit, and the liquid in described decentralized photo syringe and the continuous phase syringe flows into returnable and is cured after this conduit compiles.
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