CN102895927B - Grain size controllable monodisperse polyvinyl alcohol gel microsphere, preparation method thereof - Google Patents
Grain size controllable monodisperse polyvinyl alcohol gel microsphere, preparation method thereof Download PDFInfo
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- CN102895927B CN102895927B CN201210407133.1A CN201210407133A CN102895927B CN 102895927 B CN102895927 B CN 102895927B CN 201210407133 A CN201210407133 A CN 201210407133A CN 102895927 B CN102895927 B CN 102895927B
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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 the nontoxic and good feature of biocompatibility, is widely used in and controls drug releasing rate, extends action effective, to aspects such as particular organization and the releases of organ target.The using emulsion polymerization techniques such as Zhao great Qing, taking aldehyde or borax as crosslinking agent, obtain PVA gel micro-ball, but this technology can only be used the PVA solution of low concentration, causes the mechanical property deficiency of PVA gel micro-ball.Gao Suzhao etc. adopt high voltage electrostatic technique to obtain 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.
PVA gel micro-ball is also 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 supply artery of the tumor locking, cut off the nutrition of tumour cell is caused to tumor tissue necrosis.If contain antineoplastic in microballoon, 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 μ m scope average diameters.The PVA gel micro-ball particle diameter that Boschetti etc. (US Patent No. 7,670,592) are prepared taking formaldehyde as crosslinking agent with emulsion polymerization method reaches hundreds of microns, adopts mechanical mixing method formation W/O emulsion crosslinking curing to become microballoon.This emulsion polymerization method is in the time preparing tens of extremely hundreds of microns of microballoons, and the difficulty that generates the uniform drop of particle diameter due to control is larger, solidifies rear thus obtained microsphere particle diameter wider distribution, is difficult to obtain the mono-dispersion microballoon of size homogeneous.And particle diameter is difficult for by cytophagy at tens polymer microballoons to hundreds of micron, the pharmaceutical release time with targeting and load is long, has advantage as the pharmaceutical carrier in 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.
The single dispersion polyethylene alcogel microballoon that provides a kind of particle diameter controlled is provided.
An also object of the present invention is to provide the above-mentioned particle diameter of preparation controlled single dispersion polyethylene alcogel microballoon device used.
In order to realize object 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, control flow velocity and the viscosity of 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 obtain the controlled single dispersion polyethylene alcogel microballoon of particle diameter.
More specifically, the method comprises the following steps:
(1) preparation of coagulating bath solution: in proportion boron-containing compound is added in the mixed liquor of alcohol and amino alcohol, magnetic agitation heating are dissolved it, preparation boron compound concentration is 0.005 ~ 0.050gmL
-1coagulating bath solution;
(2) preparation of decentralized photo and continuous phase: appropriate polyvinyl alcohol is added in deionized water, and magnetic agitation heating are dissolved it, the decentralized photo solution that preparation polyvinyl alcohol percentage by weight is 2% ~ 10%; Low polar compound is mixed with alcohol, prepare low polar compound and alcohol volume ratio and be 100: 0 ~ 250 continuous phase solution;
(3) flow velocity and the viscosity of adjustment decentralized photo and continuous phase: controlling decentralized photo flow rates is 20 ~ 300mmmin
-1, continuous phase flow rates is 20 ~ 300mmmin
-1, dispersed phase viscosity scope is 1 ~ 500mPas, 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 coagulating bath solution, after curing reaction, gained drop can be solidified into the controlled single dispersion polyethylene alcohol hydrogel microsphere of particle diameter.
Wherein, the boron compound described in 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 alcohol and amino alcohol is preferably 2: 1; Described heating refers to and is slowly heated to 60 DEG C.
Wherein, described in step (2), low polar compound is preferably silicone oil, soybean oil or salad oil, more preferably silicone oil; Described alcohol is preferably one or both in isoamyl alcohol, isooctanol, more preferably isoamyl alcohol and isooctanol mixture; Described heating refers to and is slowly heated to 90 DEG C.
The time of curing reaction described in step (5) is 2 ~ 8 hours.
Described preparation method also comprises the post processing of step (6) polyvinyl alcohol hydrogel microballoon: by the polyvinyl alcohol hydrogel microballoon of step (5) gained through filtration or decantation (decant) after, organic solvent washing several for residual organic solution, be placed in water-soluble solvent and soak a couple of days, elimination solvent, dry, obtain 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 of the water-soluble solvent composition 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 prepared by said method.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 microfluidic control device used, 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 arranged on respectively on decentralized photo syringe pump and 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 continuous phase syringe is cured flow into returnable after this conduit collects in.
Wherein, in three of described T-shaped threeway ports, be provided with internal thread; Described continuous phase syringe is provided with the outside, termination of T-shaped threeway connecting duct the external screw thread matching well mutually with T-shaped threeway port internal thread;
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 outside, one end that closed casing is connected with T-shaped threeway is provided with the external screw thread matching 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 match; Described capillary is inserted in the conduit being communicated with described T-shaped threeway the 3rd port through described closed casing;
The outside, termination of the 3rd port connecting tube of described T-shaped threeway is provided with the external screw thread matching 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 is prepared the controlled single dispersion polyethylene alcogel microballoon of particle diameter is as follows: the decentralized photo solution preparing and continuous phase solution are respectively charged in decentralized photo and continuous phase syringe, and be placed in respectively on decentralized photo and 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 microfluidic control device to prepare the controlled single dispersion polyethylene alcogel microballoon of particle diameter.As the poly-vinyl alcohol solution of decentralized photo the promotion of syringe pump dirty enter in capillary in microfluidic controller, in outflow port capillaceous, in the time that decentralized photo liquid flows out, surface tension interaction result between viscous force and the liquid of mobile continuous phase causes decentralized photo liquid to be sheared into drop at outflow port place, the diameter of drop is subject 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, after cross-linking reaction, can obtain the polyvinyl alcohol gel microballoon of monodispersity.Reduce capillary diameter, increase flow velocity or the viscosity of continuous phase, reduce decentralized photo flow velocity, can cause also corresponding the reducing of size of the final polyvinyl alcohol gel microballoon obtaining, therefore 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 prepared by the present invention 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 in microfluidic controller, decentralized photo is flowed through, continuous phase and decentralized photo flow velocity and viscosity, can regulate and control the size of prepared microballoon easily.Microballoon does not need heating can to solidify by Quick cross-linking at normal temperatures, and energy consumption is little, and consuming time short, cost is low, has widened the application of PVA gel micro-ball at field of medicaments.
Brief description of the drawings
Fig. 1 is the optical microphotograph picture of the polyvinyl alcohol microparticles prepared of embodiment 1, and scale is 200 μ m;
Fig. 2 is the optical microphotograph picture of the polyvinyl alcohol microparticles prepared of embodiment 2, and scale is 200 μ m;
Fig. 3 is the optical microphotograph picture of the polyvinyl alcohol microparticles prepared of embodiment 3, and scale is 200 μ m;
Fig. 4 is the optical microphotograph picture of the polyvinyl alcohol microparticles prepared of embodiment 4, and scale is 200 μ m;
Fig. 5 is the optical microphotograph picture of the polyvinyl alcohol microparticles prepared of embodiment 5, 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;
In figure, 1-1 continuous phase syringe pump; 1-2 decentralized photo syringe pump; 2-1 continuous phase syringe; 2-2 decentralized photo syringe; 3-capillary; 4-continuous phase conduit; The threeway of 5-T type; 6-output duct; 7-poly-vinyl alcohol solution drop; 8-returnable; 9-coagulating bath; 10-closed casing; 11-dispersant liquid drop.
Detailed description of the invention
Below in conjunction with specific embodiment, further set forth related content of the present invention.It is to be noted, these embodiment are only not used in and limit the scope of the invention for the present invention is described, and, after having read content of the present invention, relevant technical staff in the field can make various changes or amendment to the present invention, and these equivalent form of values fall into the application's appended claims limited range equally.
Embodiment 1
0.5g borax is joined in the mixture of 10mL isoamyl alcohol and 5mL triethanolamine, magnetic agitation is also slowly heated to 60 DEG C dissolves it, is mixed with coagulating bath solution.
1.0g polyvinyl alcohol is joined in the beaker that contains 12.5mL deionized water, magnetic agitation is also slowly heated to 90 DEG C dissolves it, makes decentralized photo solution; 30mL silicone oil is mixed with 20mL isooctanol, obtain continuous phase solution.
Above-mentioned decentralized photo solution and continuous phase solution are respectively charged in the syringe of 1mL and 50mL, are placed on two boost pumps, connect microfluidic controller, it is 26mmmin that decentralized photo flow velocity is set
-1, viscosity 160mPas, continuous phase flow velocity is 200mmmin
-1, viscosity 540mPas, capillary size is: external diameter/internal diameter 165/98 μ m, open microfluidic control device, prepare single dispersion polyethylene alcoholic solution drop; Collect the drop generating in the culture dish of above-mentioned coagulating bath solution is housed, slowly stir curing reaction 4h under room temperature, drop can be solidified into polyvinyl alcohol hydrogel microballon.After simple decantation, residual organic solution is washed 4 times with 1: 1 (volume ratio) mixed liquor of chloroform and ethanol, then with after ethanol washing 2 times, is placed in ethanol and soaks 4 days, and elimination ethanol is dry, obtains single dispersion polyethylene alcogel microballoon.Fig. 1 is the optical microphotograph picture of thus obtained microsphere, can find out microspherulite diameter homogeneous, has monodispersity, and particle diameter is 50 μ m.
Embodiment 2
0.5g borax is joined in the mixture of 10mL isoamyl alcohol and 5mL triethanolamine, magnetic agitation is also slowly heated to 60 DEG C dissolves it, is mixed with coagulating bath solution.
1.0g polyvinyl alcohol is joined in the beaker that contains 12.5mL deionized water, magnetic agitation is also slowly heated to 90 DEG C dissolves it, makes decentralized photo solution; 30mL silicone oil is mixed with 20mL isooctanol, obtain continuous phase solution.
Above-mentioned decentralized photo solution and continuous phase solution are respectively charged in the syringe of 1mL and 50mL, are placed on two boost pumps, connect after micro passage reaction, it is 72mmmin that decentralized photo flow velocity is set
-1, viscosity 160mPas, continuous phase flow velocity is 127mmmin
-1, viscosity 540mPas, capillary size is: external diameter/internal diameter 245/98 μ m, open microfluidic control device, prepare single dispersion polyethylene alcoholic solution drop; Collect the drop generating in the culture dish of above-mentioned coagulating bath solution is housed, slowly stir curing reaction 4h under room temperature, drop can be solidified into polyvinyl alcohol hydrogel microballon.After simple decantation, residual organic solution is washed 4 times times with 1: 1 (volume ratio) mixed liquor of chloroform and ethanol, then with after ethanol washing 2 times, being placed in ethanol soaks 4 days, elimination ethanol, dry, obtain single dispersion polyethylene alcogel microballoon.Fig. 2 is the optical microphotograph picture of thus obtained microsphere, can find out microspherulite diameter homogeneous, has monodispersity, and particle diameter is 270 μ m.
Embodiment 3
0.5g borax is joined in the mixture of 10mL isoamyl alcohol and 5mL triethanolamine, magnetic agitation is also slowly heated to 60 DEG C dissolves it, is mixed with coagulating bath solution.
1.0g polyvinyl alcohol is joined in the beaker that contains 12.5mL deionized water, magnetic agitation is also slowly heated to 90 DEG C dissolves it, makes decentralized photo solution; 30mL silicone oil is mixed with 20mL isooctanol, obtain continuous phase solution.
Above-mentioned decentralized photo solution and continuous phase solution are respectively charged in the syringe of 1mL and 50mL, are placed on two boost pumps, connect after micro passage reaction, it is 264mmmin that decentralized photo flow velocity is set
-1, viscosity 160mPas, continuous phase flow velocity is 46mmmin
-1, viscosity 540mPas, capillary size is: external diameter/internal diameter 360/225 μ m, open microfluidic control device, prepare single dispersion polyethylene alcoholic solution drop; Collect the drop generating in the culture dish of above-mentioned coagulating bath solution is housed, slowly stir curing reaction 4h under lower room temperature, drop can be solidified into polyvinyl alcohol hydrogel microballon.After simple decantation, residual organic solution is washed 4 times times with 1: 1 (volume ratio) mixed liquor of chloroform and ethanol, then with after ethanol washing 2 times, being placed in ethanol soaks 4 days, elimination ethanol, dry, obtain single dispersion polyethylene alcogel microballoon.Fig. 3 is the optical microphotograph picture of thus obtained microsphere, can find out microspherulite diameter homogeneous, has monodispersity, and particle diameter is 580 μ m.
Embodiment 4
0.5g borax is joined in the mixture of 10mL isoamyl alcohol and 5mL diethanol amine, magnetic agitation is also slowly heated to 60 DEG C dissolves it, is mixed with coagulating bath solution.
1.0g polyvinyl alcohol is joined in the beaker that contains 10mL deionized water, magnetic agitation is also slowly heated to 90 DEG C dissolves it, makes decentralized photo solution; 30mL soybean oil is mixed with 30mL isoamyl alcohol, obtain continuous phase solution.
Above-mentioned decentralized photo solution and continuous phase solution are respectively charged in the syringe of 1mL and 50mL, are placed on two boost pumps, connect microfluidic controller, it is 72mmmin that decentralized photo flow velocity is set
-1, viscosity 110mPas, continuous phase flow velocity is 140mmmin
-1, viscosity 540mPas, capillary size is: external diameter/internal diameter 245/98 μ m, open microfluidic control device, prepare single dispersion polyethylene alcoholic solution drop; Collect the drop generating in the culture dish of above-mentioned coagulating bath solution is housed, slowly stir curing reaction 5h under room temperature, drop can be solidified into polyvinyl alcohol hydrogel microballon.After simple decantation, residual organic solution is washed 4 times with 1: 1 (volume ratio) mixed liquor of chloroform and ethanol, then with after ethanol washing 2 times, is placed in ethanol and soaks 4 days, and elimination ethanol is dry, obtains single dispersion polyethylene alcogel microballoon.Fig. 4 is the optical microphotograph picture of thus obtained microsphere, can find out microspherulite diameter homogeneous, has monodispersity, and particle diameter is 240 μ m.
Embodiment 5
0.5g borax is joined in the mixture of 50mL isoamyl alcohol and 25mL triethanolamine, magnetic agitation is also slowly heated to 60 DEG C dissolves it, is mixed with coagulating bath solution.
1.0g polyvinyl alcohol is joined in the beaker that contains 12.5mL deionized water, magnetic agitation is also slowly heated to 90 DEG C dissolves it, makes decentralized photo solution; 30mL salad oil is mixed with 30mL isooctanol, obtain continuous phase solution.
Above-mentioned decentralized photo solution and continuous phase solution are respectively charged in the syringe of 1mL and 50mL, are placed on two boost pumps, connect microfluidic controller, it is 72mmmin that decentralized photo flow velocity is set
-1, viscosity 75mPas, continuous phase flow velocity is 140mmmin
-1, viscosity 540mPas, capillary size is: external diameter/internal diameter 245/98 μ m, open microfluidic control device, prepare single dispersion polyethylene alcoholic solution drop; Collect the drop generating in the culture dish of above-mentioned coagulating bath solution is housed, slowly stir curing reaction 3h under room temperature, drop can be solidified into polyvinyl alcohol hydrogel microballon.After simple decantation, residual organic solution is washed 4 times with 1: 1 (volume ratio) mixed liquor of chloroform and ethanol, then with after ethanol washing 2 times, is placed in ethanol and soaks 4 days, and elimination ethanol is dry, obtains single dispersion polyethylene alcogel microballoon.Fig. 5 is the optical microphotograph picture of thus obtained microsphere, can find out microspherulite diameter homogeneous, has monodispersity, and particle diameter is 315 μ m.
Embodiment 6
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 arranged on respectively decentralized photo syringe pump 1-2 and continuous phase syringe pump 1-1 is upper, and is 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 continuous phase syringe flows into returnable after collecting in this conduit.
Wherein, in 5 three ports of described T-shaped threeway, be provided with internal thread; Described continuous phase syringe 2-1 is provided with the outside, termination of T-shaped threeway 5 connecting ducts the external screw thread matching well mutually with T-shaped threeway 5 port internal threads;
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 outside, one end that closed casing 10 is connected with T-shaped threeway 5 is provided with the external screw thread matching 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 match;
The outside, termination of the 3rd port connecting tube of described T-shaped threeway 5 is provided with the external screw thread matching well mutually with T-shaped threeway 5 port internal threads.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of 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 (8)
1. a preparation method for the controlled single dispersion polyethylene alcogel microballoon of particle diameter, its step is as follows:
(1) preparation of coagulating bath solution: in proportion boron-containing compound is added in the mixed liquor of alcohol and amino alcohol, magnetic agitation heating are dissolved it, preparation boron compound concentration is 0.005～0.050gmL
-1coagulating bath solution;
(2) preparation of decentralized photo and continuous phase: appropriate polyvinyl alcohol is added in deionized water, and magnetic agitation heating are dissolved it, the decentralized photo solution that preparation polyvinyl alcohol percentage by weight is 2%～10%; Low polar compound is mixed with alcohol, prepare low polar compound and alcohol volume ratio and be 100: 0～250 continuous phase solution;
(3) flow velocity and the viscosity of adjustment decentralized photo and continuous phase: controlling decentralized photo flow rates is 20～300mmmin
-1, continuous phase flow rates is 20～300mmmin
-1, dispersed phase viscosity scope is 1～500mPas, 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: in the coagulating bath solution that the drop of collection step (4) gained prepares in step (1), after curing reaction, drop can be solidified into the controlled single dispersion polyethylene alcogel microballoon of particle diameter.
2. the method for claim 1, 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 alcohol and amino alcohol is 2: 1; The described heating of step (1) refers to and is slowly heated to 60 DEG C.
3. the method for claim 1, is characterized in that, described in step (2), low polar compound is silicone oil, soybean oil or salad oil; Described alcohol is one or both in isoamyl alcohol, isooctanol; The described heating of step (2) refers to and is slowly heated to 90 DEG C.
4. the method for claim 1, is characterized in that, the time of curing reaction described in step (5) is 2～8 hours.
5. the method for claim 1, it is characterized in that, described preparation method also comprises the post processing of step (6) polyvinyl alcohol gel microballoon: by the polyvinyl alcohol gel microballoon of step (5) gained through filtration or decantation after, organic solvent washing several for residual organic solution, be placed in water-soluble solvent and soak a couple of days, elimination solvent, dry, obtain monodispersity polyvinyl alcohol gel microballoon.
6. method as claimed in claim 5, is characterized in that, described water-soluble solvent is one or more in methyl alcohol, ethanol, acetone; Described organic solvent refers to nonpolar and weakly polar organic solvent.
7. the controlled single dispersion polyethylene alcogel microballoon of particle diameter that described in claim 1～6 any one, preparation method obtains.
8. single dispersion polyethylene alcogel microballoon as claimed in claim 7, 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%.
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| CN113855848B (en) * | 2021-10-18 | 2022-11-01 | 四川大学 | Monodisperse boric acid crosslinked polyvinyl alcohol embolism microsphere and preparation method thereof |
| CN115301170A (en) * | 2022-08-08 | 2022-11-08 | 广东工业大学 | Method for regulating viscosity of paraffin phase-change microcapsule suspension |
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| CN101249410A (en) * | 2008-04-10 | 2008-08-27 | 华东理工大学 | Preparation of organic-inorganic composite microballoons |
| CN101279232A (en) * | 2008-01-11 | 2008-10-08 | 东南大学 | Preparation of microballoons based on microfluid |
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| CN101279232A (en) * | 2008-01-11 | 2008-10-08 | 东南大学 | Preparation of microballoons based on microfluid |
| CN101249410A (en) * | 2008-04-10 | 2008-08-27 | 华东理工大学 | Preparation of organic-inorganic composite microballoons |
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