CN104147950A - Porous membrane used for emulsification, preparation method and application thereof - Google Patents
Porous membrane used for emulsification, preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a porous membrane of which a material is perfluoro plastic. The porous membrane, which is prepared with the perfluoro plastic as a substrate, has a pore size controllable performance and can achieve a large pore size, thereby obtaining large-particle-size microspheres. A result in an embodiment in the invention proves that with a circular porous membrane as an emulsification membrane, polylactic acid microspheres of which an average particle size is 75 [mu]m can be obtained, and with a tubular porous membrane as an emulsification membrane, microshperes of which the average particle size is 115 [mu]m and particle sizes are uniform can be obtained. The porous membrane used for emulsification is obtained by forming penetrating holes in the substrate through a machining method with the perfluoro plastic as the substrate. A preparation method of the porous membrane is easy to carry out and is beneficial to large-scale industrial production.
Description
Technical field
The present invention relates to film emulsifying technology field, relate in particular to a kind of perforated membrane for emulsification, its preparation method and application thereof.
Background technology
Emulsification is that a kind of liquid is evenly dispersed in the effect in immiscible another kind of liquid with fine droplet, is chemistry, chemical industry, food, medicine, the important operation unit in the fields such as biochemistry.Traditional emulsifying manner is mainly by mechanical agitation, high speed shear etc.Emulsion droplet particle diameter breadth coefficient prepared by these traditional methods is larger, for particle diameter being required to strict product, need to introduce loaded down with trivial details post processing and extra separation equipment, has also wasted a large amount of raw materials simultaneously.
Film emulsion process is the new method of preparing homogeneous latex emulsion occurring the nearly more than ten years, on the perforated membrane that film emulsion process is used, a large amount of evenly holes can be seen micro-distributor as, film both sides are respectively decentralized photo and continuous phase, film external and internal pressure is poor is mass transfer force, decentralized photo forms drop growth by the film surface at opposite side after micropore under pressure, while growing to a certain size owing to being subject to the effect of swiftly flowing continuous phase shearing force stripping film surface, thereby form oil-in-water or water-in-oil emulsion, also can prepare compound emulsion.Compared with conventional method, film emulsification method is simple to operate, energy consumption is low, dosage of surfactant is few, emulsion is more even, therefore all has potential application prospect in every profession and trade.
What adopt in the market that film emulsion process prepares that uniform microsphere generally adopts is SPG film emulsifying technology.SPG film is a kind of cellular glass film, and its exemplary aperture is between 0.1 μ m～20 μ m.Its operation principle is to adopt hydrophilic micropore glass film, and oil phase is entered to water by the mould of size uniform, obtains the drop of size uniform.In emulsion process, be the interfacial tension of utilizing between oil phase and hydrophilic membrane, make oil phase grow into a drop at the opening part of film, work as interfacial tension, film Emulsification pressure, when the power of dragging of continuous phase etc. reaches balance, drop splits away off.
And the SPG film that SPG membrane emulsifier adopts in the market, its typical aperture is generally less than 20 μ m, on the large-sized microballoon of preparation, also can have some restrictions.Such as, its average grain diameter of Risperidone microballoon of selling in the market, at 90 μ m, adopts common SPG film emulsification to be just difficult to realize.
Summary of the invention
The object of the present invention is to provide a kind of perforated membrane for emulsification, its preparation method and application thereof, perforated membrane provided by the invention aperture has good adjustability, thereby obtains the microballoon of greater particle size.
The invention provides a kind of perforated membrane for emulsification, the material of described perforated membrane is perfluor plastics.
Preferably, the material of described perforated membrane is polytetrafluoroethylene (PTFE), perfluor (ethylene, propylene) copolymer, poly-perfluoroalkoxy resin.
Preferably, the thickness of described perforated membrane is 0.1mm～3mm.
Preferably, the surface of described perforated membrane is hydrophilic.
The preparation method who the invention provides a kind of perforated membrane for emulsification, comprising:
Taking perfluor plastics as matrix, adopt the method for machining, on described matrix, beat multiple through holes, obtain the perforated membrane for emulsification.
Preferably, the method for described machining is boring or laser boring.
Preferably, describedly also comprise beat multiple through holes on described matrix after:
Matrix after air exercise through hole carries out surface hydrophilic modification processing.
Preferably, described surface hydrophilic modification is treated to the processing of naphthalene Sodium chemistry, the processing of ammonia sodium method, the processing of biphenyl sodium method, and high-temperature melting method processing, radiation method are processed or Cement Composite Treated by Plasma.
The invention provides the application in film emulsification of preparation method obtains described in perforated membrane described in technique scheme or technique scheme perforated membrane.
Preferably, described film emulsification is:
Decentralized photo and continuous phase are placed in to the both sides of described perforated membrane, the relatively described perforated membrane uniform motion of described continuous phase, described decentralized photo enters described continuous water by the hole on described perforated membrane, completes emulsification.
The material of perforated membrane provided by the invention is perfluor plastics, the perforated membrane preparing taking perfluor plastics as matrix, and aperture adjustability, and can obtain larger aperture, thus obtain the microballoon of greater particle size.Embodiment of the present invention result shows, taking circular perforated membrane as emulsifying film, obtains the polylactic acid microsphere that average grain diameter is 75 μ m; Taking tubulose perforated membrane as emulsifying film, obtaining average grain diameter is 115 μ m, the uniform microballoon of particle diameter.The present invention, taking perfluor plastics as matrix, adopts the method for machining to stamp through hole on described matrix, obtains the perforated membrane for emulsification.The preparation method of perforated membrane provided by the invention is simple, easy to operate, is conducive to large-scale industrial production.
And it is matrix that the present invention adopts perfluor plastics, shape is adjustable, and those skilled in the art can prepare difform perforated membrane as required, as the perforated membrane of tabular, tubulose or other given shapes, is beneficial to industrial needs.
Brief description of the drawings
Fig. 1 is the hydrophilic circular flat porous membrane structure schematic diagram that the embodiment of the present invention 1 obtains;
Fig. 2 is the tubulose porous membrane structure schematic diagram that the embodiment of the present invention 3 obtains;
Fig. 3 is the circular perforated membrane emulsifier unit structural representation that the embodiment of the present invention 2 adopts;
Fig. 4 is the tubulose perforated membrane emulsifier unit structural representation that the embodiment of the present invention 4 adopts.
Detailed description of the invention
The invention provides a kind of perforated membrane for emulsification, the material of described perforated membrane is perfluor plastics.
The material of perforated membrane provided by the invention is perfluor plastics, the perforated membrane preparing taking perfluor plastics as matrix, and aperture adjustability, can obtain the perfluor plastics of larger aperture, thereby obtains the microballoon of greater particle size; And it is matrix that the present invention adopts perfluor plastics, shape is adjustable, and those skilled in the art can prepare difform perforated membrane as required, as the perforated membrane of tabular, tubulose or other given shapes, is beneficial to industrial needs; Moreover compared with traditional cellular glass (SPG) film, the perforated membrane for emulsification provided by the invention has lower manufacturing cost.
The material of perforated membrane provided by the invention is perfluor plastics, is preferably polytetrafluoroethylene (PTFE), perfluor (ethylene, propylene) copolymer, poly-perfluoroalkoxy resin, more preferably polytetrafluoroethylene (PTFE).The present invention does not have special restriction to the source of described perfluor plastics, adopts the commercial goods of above-mentioned perfluor plastics well known to those skilled in the art;
The present invention does not have special restriction to the thickness of described perforated membrane, and those skilled in the art can be according to the thickness of the perforated membrane that in prior art, film emulsifying technology is used, and sets the thickness of the perforated membrane for emulsification provided by the invention.As in the present invention, the thickness of described perforated membrane is preferably 0.1mm～3mm, more preferably 0.5mm～2.5mm; In specific embodiment, the thickness of described perforated membrane can be specially 0.5mm, 1.0mm, 1.5mm or 2mm;
The present invention does not have special restriction to the shape of described perforated membrane, and those skilled in the art can be cut to different shapes by perfluor plastic substrate as required, thereby obtains having difform perforated membrane.As in the present invention, the shape of described perforated membrane can be planar rondure, can be also tubulose; Concrete, in the time that described perforated membrane is tubulose perforated membrane, described pore size distribution is in a side in tubulose perfluor plastics vertical section.
The present invention does not have special restriction to the aperture of described perforated membrane mesopore, and those skilled in the art can set the perforated membrane in suitable aperture as required, as described in the aperture of perforated membrane can be less than 100 μ m, also can be more than or equal to 100 μ m; In an embodiment of the present invention, the aperture of described perforated membrane can be 100 μ m, can be also 150 μ m, thereby obtains the microballoon of greater particle size;
In the present invention, the hole in described perforated membrane can be random distribution, can be also regular distribution, and as being array distribution, the present invention does not have special restriction to the distribution mode in described hole, can realize in film emulsification.In the present invention, described hole is preferably circular array distribution or rectangular array distribution in perforated membrane.Concrete, when described perforated membrane be shaped as planar rondure time, the hole on described perforated membrane can rounded matrix distribution; When described perforated membrane be shaped as tubulose time, the hole on described perforated membrane can rectangular array distribution.
Those skilled in the art can also as required, adjust aperture and adjacent holes spacing, thereby obtain the microballoon of suitable dimension, if aperture is that 100 μ m, adjacent holes spacing are the perforated membrane of 800 μ m, can obtain the microballoon that average grain diameter is 75 μ m; For another example, aperture is the perforated membrane that 150 μ m, adjacent holes spacing are 1mm, can obtain the microballoon that average grain diameter is 115 μ m.
In the present invention, perfluor plastics are hydrophobic type, and the porous film surface that directly punching obtains is hydrophobic type, and the perforated membrane of described hydrophobic type can be directly used in the preparation of Water-In-Oil system; The method that the present invention prepares Water-In-Oil system to described hydrophobic type perforated membrane does not have special restriction, the technical scheme that adopts film emulsification well known to those skilled in the art field Water-In-Oil system to prepare.In order to obtain oil-in-water system, the present invention preferably provides a kind of perforated membrane of surface hydrophilic type.In the present invention, the perforated membrane of described surface hydrophilic type preferably carries out surface hydrophilic modification processing by perfluor plastics perforated membrane and makes.The present invention does not have special restriction to the method for described surface hydrophilic modification processing, adopts the technical scheme of surface hydrophilic modification well known to those skilled in the art.In the present invention, described surface hydrophilic modification processing is preferably the processing of naphthalene Sodium chemistry, the processing of ammonia sodium method, the processing of biphenyl sodium method, and high-temperature melting method processing, radiation method are processed or Cement Composite Treated by Plasma, the more preferably processing of naphthalene Sodium chemistry.
The present invention is preferably immersed the perfluor plastics perforated membrane after described punching in sodium naphthalene solution, leaves standstill, and obtains the perforated membrane of surface hydrophilic type.In the present invention, the molar concentration of described sodium naphthalene solution is preferably 0.1mol/L～2mol/L, and more preferably 0.4mol/L～0.7mol/L, most preferably is 0.5mol/L～0.6mol/L; In the present invention, those skilled in the art can, according to the needs of surface hydrophilic modification processing, set suitable time of repose, can hold over night, also can leave standstill a few minutes; In the specific embodiment of the present invention, the described standing time is preferably 2min～15min, and more preferably 3min～5min, most preferably is 3min～4min; The present invention does not have special restriction to described standing temperature, without standing system being heated or cooling, at room temperature.
Complete after described leaving standstill, the present invention preferably cleans the perfluor plastics perforated membrane after described leaving standstill, and obtains surface hydrophilic type perforated membrane.The present invention does not have special restriction to the method for described cleaning, adopts the technical scheme of the cleaning after well known to those skilled in the art, above-mentioned hydrophilic treated.The present invention preferably the perfluor plastics perforated membrane after described leaving standstill is carried out to acetone cleaning successively and absolute ethyl alcohol cleans, and obtains hydrophile type porous film.
The preparation method who the invention provides a kind of perforated membrane for emulsification, comprising:
Taking perfluor plastics as matrix, adopt the method for machining, on described matrix, beat multiple through holes, obtain the perforated membrane for emulsification.
Method provided by the invention, taking perfluor plastics as matrix, adopts the method for machining, beats multiple through holes on described matrix, obtains the perforated membrane for emulsification.Method provided by the invention is simple, and easy operating is beneficial to large-scale industrial production.In the present invention, the method for described machining is preferably boring or laser boring, and the aperture that this area machinery personnel can be as required adopts the method for boring or mechanical punching, beats multiple through holes on perfluor plastic substrate.The present invention does not have special restriction to the method for described boring or laser boring, adopts the technical scheme of boring well known to those skilled in the art or laser boring.
In the present invention, the parameter such as the source of described perfluor plastics, thickness, shape is consistent for parameters such as source, kind and the shapes of the perforated membrane scheme perfluor plastics of emulsification with described in technique scheme; The parameters such as the distribution of through hole on described perforated membrane, aperture, adjacent holes spacing are consistent for parameters such as pore size distribution, aperture and adjacent holes spacing on the perforated membrane scheme perforated membrane of emulsification with described in technique scheme, do not repeat them here.
Complete after described punching, the porous film surface for emulsification obtaining is hydrophobic type, can adopt film emulsifying technology, is directly used for preparing Water-In-Oil system.In order to prepare oil-in-water system, the perforated membrane obtaining after punching need to be carried out to surface hydrophilic and process modification, obtain surface hydrophilic type perforated membrane.In the present invention, the preparation method of described surface hydrophilic type perforated membrane is preferably consistent with the preparation method of surface hydrophilic type perforated membrane described in technique scheme, does not repeat them here.
The perforated membrane that preparation method described in perforated membrane or technique scheme described in technique scheme of the present invention obtains, can be used in film emulsifying technology field, prepares emulsification system, as emulsion, microballoon or micro-capsule etc.The present invention also provides the application in film emulsification of perforated membrane that the preparation method described in perforated membrane described in a kind of technique scheme or technique scheme obtains.In the present invention, described film emulsification is preferably specially:
Decentralized photo and continuous phase are placed in to the both sides of described perforated membrane, the relatively described perforated membrane uniform motion of described continuous phase, described decentralized photo enters described continuous water by the hole on described perforated membrane, completes emulsification.
The film emulsifier unit that the present invention adopts described film emulsification does not have special restriction, adopts film emulsifier unit well known to those skilled in the art, and those skilled in the art can be according to the shape of perforated membrane, selects suitable film emulsifier unit.As when as described in perforated membrane while being planar rondure, the present invention can adopt circular perforated membrane emulsifier unit as shown in Figure 3, in Fig. 3,1 is perforated membrane, 2 be syringe pump, 3 for magnetic stir bar, 4 be liquid container.In described liquid container 4, be contained with continuous phase, under the stirring of magnetic stir bar 3, described continuous phase moves with uniform velocity in described beaker; Decentralized photo is placed in to syringe pump 2, decentralized photo in syringe pump 2 is pushed into by perforated membrane in the continuous phase of uniform motion, decentralized photo forms drop and constantly grows up at the opening part in hole, when drop grows to certain degree, under the pulling of continuous phase, depart from described perforated membrane and enter continuous water, complete described emulsion process.
For another example, in the time that described perforated membrane is tubulose, the present invention can adopt tubulose perforated membrane emulsifier unit as shown in Figure 4 to carry out emulsification, and in Fig. 4,1 is tubulose perforated membrane, 2 is circulating pump, 3 is syringe pump, and 4 is liquid container, described liquid container sidewall opening, described liquid container lower end has choana, and opening, choana and the circulating pump of described sidewall are connected by pipeline; Described choana is connected with the outlet of described tubulose perforated membrane, and described syringe pump is connected with the hole on described tubulose perforated membrane.In syringe pump, fill decentralized photo, fill continuous water in liquid container, ON cycle pump and syringe pump, clamp-on decentralized photo in continuous water by perforated membrane, stops circulating pump and syringe pump after having pushed, and obtains emulsion; In order to obtain microballoon, the present invention can also transfer to described emulsion in another container, stirs until solvent evaporates is complete, obtains the uniform microballoon of particle diameter.
In the present invention, the particle diameter of described microballoon is subject to the impact of aperture, adjacent holes spacing and the speed of the relative perforated membrane of continuous phase of perforated membrane, generally speaking, large-sized micropore is applicable to the larger microballoon of preparation size, and undersized micropore is applicable to the less microballoon of preparation size; And for the spacing of micropore, excessive spacing can cause microballoon preparation efficiency slack-off, and the too intensive drop forming on film surface that may cause in hole is in contact with one another or collides and assembles, and it is inhomogeneous that drop becomes.Those skilled in the art can be according in film emulsifying technology in prior art, relation between the speed of membrane aperture, adjacent holes spacing and the relative perforated membrane of continuous phase, to the aperture of perforated membrane in the present invention and the pitch of holes that is connected, and the speed of the relative perforated membrane of continuous phase adjusts, thereby obtain the effect of required optimum.
The material of perforated membrane provided by the invention is perfluor plastics, the perforated membrane preparing taking perfluor plastics as matrix, and aperture adjustability, can obtain the perfluor plastics of larger aperture, thereby obtains the microballoon of greater particle size.Embodiment of the present invention result shows, taking circular perforated membrane as emulsifying film, obtains the polylactic acid microsphere that average grain diameter is 75 μ m; Taking tubulose perforated membrane as emulsifying film, obtaining average grain diameter is 115 μ m, the uniform microballoon of particle diameter.The present invention, taking perfluor plastics as matrix, adopts the method for machining to stamp through hole on described matrix, obtains the perforated membrane for emulsification.The preparation method of perforated membrane provided by the invention is simple, easy to operate, is conducive to large-scale industrial production.
And it is matrix that the present invention adopts perfluor plastics, shape is adjustable, and those skilled in the art can prepare difform perforated membrane as required, as the perforated membrane of tabular, tubulose or other given shapes, is beneficial to industrial needs.
In order to further illustrate the present invention, below in conjunction with embodiment, the perforated membrane for emulsification provided by the invention, its preparation method and application thereof are described in detail, but they can not be interpreted as to limiting the scope of the present invention.
Embodiment 1
Adopting diameter is that the circular polytetrafluoroethylene film of 25mm is matrix, and the thickness of this flat sheet membrane is 0.5mm, bores the boring of through hole employing diameter 0.1mm, adjacent spacing of wells 0.8mm on described matrix.Arrange around center annular in hole, and the porous disk obtaining after Drilling operation is used in the sodium naphthalene solution that immerses 0.5M and processed 4 minutes under room temperature, uses successively acetone, and absolute ethyl alcohol cleans up, and obtains surface hydrophilic type circular flat perforated membrane.
The structure of the hydrophilic circular flat perforated membrane that the present embodiment obtains as shown in Figure 1, Fig. 1 is the structural representation of the hydrophilic circular flat perforated membrane for preparing of the embodiment of the present invention 1, aperture, hole on the hydrophilic circular flat perforated membrane that the present embodiment obtains is consistent, adjacent holes spacing is consistent, rounded array distribution.
Embodiment 2
1g PLA is dissolved in the chloroform of 10mL, obtains disperseing oil phase, 4g polyvinyl alcohol is dissolved in to 200mL deionized water, obtain continuous water.Adopt embodiment 1 to prepare surperficial hydrophilic circular flat perforated membrane, adopt the device of Fig. 3 to carry out film emulsion process, continuous water is placed in to liquid container 4, bottom of liquid container is placed with magnetic stir bar 3, and mixing speed is set as 400rpm; Dispersion oil phase is placed in to syringe pump 2, passes through perforated membrane by syringe pump according to the oil phase in the speed pushing syringe of 1mL/min, after having advanced, reduce mixing speed to 100rpm, continue to stir the polylactic acid microsphere that obtains 75 microns of average grain diameters after being dried.
Embodiment 3
Employing external diameter is that the polyfluortetraethylene pipe that 8mm, internal diameter are 6mm is matrix, and the footpath of punching on the tube wall of polyfluortetraethylene pipe vertical section one side is 0.15mm micropore, and adjacent micropore spacing is 1mm, 504 of quantity, rectangular matrix distribution.Process 3 minutes under room temperature obtaining in the sodium naphthalene solution that antipriming pipe immersion molar concentration is 0.5mol/L, use successively acetone, absolute ethyl alcohol to clean up, obtain surface hydrophilic type tubulose perforated membrane.
The structure of the hydrophilic circular flat perforated membrane that the present embodiment obtains as shown in Figure 2, Fig. 2 is the structural representation of the surface hydrophilic type tubulose perforated membrane for preparing of the embodiment of the present invention 3, aperture, hole on the surface hydrophilic type tubulose perforated membrane that the present embodiment obtains is consistent, adjacent holes spacing is consistent, rectangular array distribution.
Embodiment 4
1g PLA, 5mg rhodamine are dissolved in the chloroform of 10mL, obtain disperseing oil phase, 4g polyvinyl alcohol is dissolved in 200mL deionized water, obtain continuous water.The surface hydrophilic type tubulose perforated membrane that adopts embodiment 3 to prepare, adopt the film emulsifier unit shown in Fig. 4 to carry out film emulsion process, continuous water is placed in to liquid container, dispersion oil phase is placed in to syringe pump, ON cycle pump, oil phase is clamp-oned in continuous water by tubulose perforated membrane with the speed of 1.6mL/min, extruding completes, and stops circulating pump, and acquisition emulsion is transferred in another one beaker, regulate mixing speed to 100rpm, until solvent evaporates is complete.Obtain average grain diameter at the uniform microsphere of 115 microns.
As seen from the above embodiment, the material of perforated membrane provided by the invention is perfluor plastics, the perforated membrane preparing taking perfluor plastics as matrix, and aperture adjustability, can obtain the perfluor plastics of larger aperture, thereby obtains the microballoon of greater particle size.Embodiment of the present invention result shows, taking circular perforated membrane as emulsifying film, obtains the polylactic acid microsphere that average grain diameter is 75 μ m; Taking tubulose perforated membrane as emulsifying film, obtaining average grain diameter is 115 μ m, the uniform microballoon of particle diameter.The present invention, taking perfluor plastics as matrix, adopts the method for machining to stamp through hole on described matrix, obtains the perforated membrane for emulsification.The preparation method of perforated membrane provided by the invention is simple, easy to operate, is conducive to large-scale industrial production.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; 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. for a perforated membrane for emulsification, the material of described perforated membrane is perfluor plastics.
2. perforated membrane according to claim 1, is characterized in that, the material of described perforated membrane is polytetrafluoroethylene (PTFE), perfluor (ethylene, propylene) copolymer, poly-perfluoroalkoxy resin.
3. perforated membrane according to claim 1, is characterized in that, the thickness of described perforated membrane is 0.1mm～3mm.
4. perforated membrane according to claim 1, is characterized in that, the surface of described perforated membrane is hydrophilic.
5. for a preparation method for the perforated membrane of emulsification, comprising:
Taking perfluor plastics as matrix, adopt the method for machining, on described matrix, beat multiple through holes, obtain the perforated membrane for emulsification.
6. preparation method according to claim 5, is characterized in that, the method for described machining is boring or laser boring.
7. preparation method according to claim 5, is characterized in that, describedly also comprises beat multiple through holes on described matrix after:
Matrix after air exercise through hole carries out surface hydrophilic modification processing.
8. preparation method according to claim 7, is characterized in that, described surface hydrophilic modification is treated to the processing of naphthalene Sodium chemistry, the processing of ammonia sodium method, the processing of biphenyl sodium method, and high-temperature melting method processing, radiation method are processed or Cement Composite Treated by Plasma.
9. the application of the perforated membrane that described in claim 1～4 any one, described in perforated membrane or claim 5～8 any one, preparation method obtains in film emulsification.
10. application according to claim 9, is characterized in that, described film emulsification is:
Decentralized photo and continuous phase are placed in to the both sides of described perforated membrane, the relatively described perforated membrane uniform motion of described continuous phase, described decentralized photo enters described continuous water by the hole on described perforated membrane, completes emulsification.
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| CN110624428B (en) * | 2019-10-21 | 2021-11-19 | 天津工业大学 | Membrane emulsification system |
| CN114073920A (en) * | 2020-08-12 | 2022-02-22 | 财团法人食品工业发展研究所 | Preparation method of oily component microcapsule |
| CN114073920B (en) * | 2020-08-12 | 2024-01-30 | 财团法人食品工业发展研究所 | Preparation method of microcapsule containing oily component |
| JP7033232B1 (en) | 2021-10-05 | 2022-03-09 | 小川香料株式会社 | Method for producing an emulsified composition |
| JP2023054928A (en) * | 2021-10-05 | 2023-04-17 | 小川香料株式会社 | Method for producing emulsion composition |
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