EP2879779A1 - Single/pass pulsed membrane emulsification method and apparatus - Google Patents
Single/pass pulsed membrane emulsification method and apparatusInfo
- Publication number
- EP2879779A1 EP2879779A1 EP13762293.2A EP13762293A EP2879779A1 EP 2879779 A1 EP2879779 A1 EP 2879779A1 EP 13762293 A EP13762293 A EP 13762293A EP 2879779 A1 EP2879779 A1 EP 2879779A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- membrane
- continuous phase
- phase
- emulsification
- dispersed phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/41—Emulsifying
- B01F23/411—Emulsifying using electrical or magnetic fields, heat or vibrations
- B01F23/4111—Emulsifying using electrical or magnetic fields, heat or vibrations using vibrations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/30—Injector mixers
- B01F25/31—Injector mixers in conduits or tubes through which the main component flows
- B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
- B01F25/3142—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction
- B01F25/31421—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction the conduit being porous
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
- B01F31/65—Mixers with shaking, oscillating, or vibrating mechanisms the materials to be mixed being directly submitted to a pulsating movement, e.g. by means of an oscillating piston or air column
Definitions
- the present invention concerns a single-pass pulsed membrane emulsification process and apparatus.
- the invention concerns a single pass pulsed cross flow membrane emulsification method and an apparatus for performing such method.
- Membrane emulsification is a technique that permits to produce emulsion droplets through extrusion of one liquid phase (dispersed phase) into a second liquid phase (continuous phase) using a microporous membrane. During droplet formation, dispersed phase droplets grown at the membrane pores opening are detached in the continuous phase thought a drop-by-drop mechanism.
- the principal membrane emulsification technologies developed include:
- moving membranes are used to generate relative motion between the membranes and the continuous phase (rotating or vibrating membrane emulsification) ;
- Cross-flow membrane emulsification is a well- studied technique [A. J. Abrahamse, 2002; S.J. Peng, 1998; G. De Luca 2004] in which the continuous phase is circulated in tangential direction along the membrane lumen side.
- the continuous phase is stirred using a rotator or a paddle stirrer positioned over the membrane [Stillwell M., 2007; Egidi E. , 2008] .
- the main advantages of membrane emulsification process compared to the conventional mechanical emulsification processes are the low energy consumption per unit of product made [H. Schubert, 2006] with high energy efficiency, quality and functionality of delicate used ingredients and the precise manufacture of emulsions with controlled droplets size and size distribution.
- the interaction between the disperse phase and the pore is a significant factor in the productivity enhancement.
- the membrane pore wall having good wettability to the disperse phase allows the oil phase to permeate more quickly in the pores, and hence results in significantly higher productivity.
- the addition of one miscible alcohol to viscous oil was proven to increase oil flux much more than expected based on its viscosity.
- the alcohol is water soluble and can increase the wettability of the oil phase on the pore wall with a consequent increase in the oil flux [Yuan Q. , 2009 a].
- Results suggest that the modification of the pore wall in order to increase hydrophobic properties will permit to increase the dispersed phase flux while the hydrophilic detachment part retained will avoid the spread of oil phase over the membrane for emulsion quality control. This knowledge can be used to design high-productivity membranes .
- a novel approach to decrease the average droplet size while maintaining high disperse phase fluxes is the use of moving membranes .
- the use of high membrane shear rates has long been recognized in filtration process (ultra filtration UF, micro filtration MF, nano filtration NF, reverse osmosis RO) [Jaffrin, 2008] as one of the most efficient factors for increasing permeate flux as it reduces fouling phenomena.
- Dynamic or shear-enhanced filtration consists in creating the shear rate at the membrane by a moving part such as a rotating membrane, or a disk rotating near a fixed circular membrane or by vibrating the membrane either longitudinally or torsionally around a perpendicular axis .
- Zhu and Barrow [Zhu J, 2005] reported the first investigation into the efficacy of transversal excitation in membrane emulsification using a micro machined silicon nitride membrane excited by a piezoactuator system. Zhu and Barrow found a decrease in droplet size for frequencies around 10 Hz and cross- flow velocities on the order of centimeters per second.
- Kelder et al carried out a numerical study intruding the influence of inertia in droplet detachment model [Kelder, 2007] .
- the simulations show that membrane excitation potentially has a strong effect on the average droplet size in membrane emulsification, but that successful exploitation will require careful design of membrane and process.
- First estimates seem to indicate that systems with lower excitation frequency and larger excitation amplitude may perform better, but this will require experimental verification.
- Holdich et al. [Holdich R. , 2010] described the application of vibrating membrane emulsification at low frequency oscillation in order to control the production of droplets larger than 30 ⁇ i .
- a new method and a rationed rotating membrane system using periodical switch-on between the rotating membrane and micro-nozzle were introduced (Y.B. Li, 2011) .
- the dispersed phase is forced to flow through the nozzle to form a fluid stream which later is divided into rationed parts by a rotating membrane.
- the quantitative volume of the dispersed phase will transform into droplets as it flies out of the membrane.
- the droplet size decreases with the increase of the rotation speed and with the decrease of the jetting velocity.
- a general rule in membrane emulsification is the use of high shear rate to generate uniform small droplets.
- High shear rates at the membrane surface are obtained by:
- Static membrane emulsification process in the absence of shear flow at the membrane surface is potentially suitable for the production of less viscous and/or larger droplets with uniform size.
- the simple experimental set-up and the low energy input required makes the static membrane emulsification process interesting from a technology point of view.
- polydispersed droplets were generated [M . Kukizaki, 2009] and the membrane controlled droplets formation is possible only at low dispersed phase flux with low productivity.
- the solution according to the present invention aims to provide a membrane emulsification method using pulsed liquid continuous phase at the lumen level of a microporous membrane.
- the method allows obtaining highly concentrated uniform liquid droplets without any damaging due to mechanical stress.
- the purpose of the present invention is therefore to provide a method which allows to overcome the limits of the solutions according to the prior art and to obtain the previously described technical results.
- Another object of the invention is to provide a method which is substantially simple, safe and reliable.
- a membrane emulsification method wherein a continuous phase is present on a first side of a membrane wall and a dispersed phase is pressed on the other side of the membrane wall, so that the dispersed phase passes through the pores of the membrane, wherein the continuous phase is moved back- and-forward in a direction tangential to the membrane wall, until an emulsion is obtained with the desired concentration of the dispersed phase within the continuous phase.
- said emulsion is removed from the membrane only after the desired concentration of the dispersed phase within the continuous phase is obtained.
- surfactants are added in the continuous phase .
- said back-and-forward movement has an amplitude comprised between 10 and 400 mm and a frequency comprised between 0,1 and 5Hz .
- a membrane emulsification apparatus wherein a membrane module is fed with a continuous phase on a first side of a porous membrane wall and a dispersed phase on the other side of the membrane wall, said dispersed phase being pressed against the membrane wall by pressure means so that the dispersed phase passes through the pores of the membrane wall, further comprising means for moving said continuous phase back- and-forward in a direction tangential to said membrane wall .
- said membrane module comprises at least one tubular membrane, and more preferably said continuous phase is fed tangentially to a lumen of said at least one tubular membrane .
- said means for moving said continuous phase comprise a pump with reverse flow direction function.
- the pulsed membrane emulsification method eliminating the shear stress outside of the membrane related to the recirculation of emulsion droplets along the pump and fitting circuit as it happens in conventional cross-flow membrane emulsification.
- the emulsion is collected within the shaking phase within the lumen (which serves as batch system) and then collected in the reservoir in a single pass without recirculating it.
- the process can be considered a cross-flow batch system operating in a semicontinuous mode.
- Results obtained showed that it was possible obtaining uniform emulsion droplets also when high concentration of dispersed phase was reached with high productivity comparing the traditional cross-flow membrane operation.
- the pulsed membrane emulsification method and apparatus according to the present invention are suitable for the production of particles containing bioactive molecule or viscous dispersed materials or large droplets with uniform size.
- a novel dynamic membrane emulsification method is proposed utilizing a static and fixed tubular membrane.
- the system has been tested in the preparation of an oil-in-water emulsion.
- a fixed volume of continuous phase A is fed tangentially to the membrane lumen 1 and the flow direction 2 is reverted at appropriate frequency in such a way that the volume is kept in the lumen 1.
- the continuous phase A is tangentially agitated by inverting the flow direction 2 back-and-forward within the membrane lumen 1, which contains the "batch" volume.
- the dispersed phase B passes radially through the pores 3 of the porous membrane wall 4 and forms droplets C into the shaking continuous phase A.
- the continuous phase volume is then removed from the membrane lumen 1 once the desired dispersed phase concentration has been obtained.
- the method can be applied in the preparation of simple emulsions such as oil-in-water (O/W) and water- in-oil (W/O) emulsions.
- simple emulsions such as oil-in-water (O/W) and water- in-oil (W/O) emulsions.
- Oil-in-water emulsions can be prepared using as dispersed phase vegetal oil such as (but not limited to) soybean oil, sunflower oil, olive oil and corn oil or other organic compounds such as (but not limited to) squalene or limonene or hydrocarbons such as (but not limited to) isooctane or hexane .
- Different water soluble surfactants can be dissolved in the water continuous phase such as (but not limited to) Tween 20 ® or Tween 80 ® (non-ionic surfactants) or sodium dodecyl sulfate (SDS, ionic surfactant) .
- Biomolecules such as (but not limited to) proteins ( ⁇ -lactoglobuline or bovin serum albumin (BSA) or lipase) can also be used without structural modifications to promote emulsion stability or to give specific functional activities.
- the method according to the present invention is particularly suitable for the preparation of formulation containing labile biomolecules because no strong mechanical stress is applied.
- the present invention allows the generation of new products having properties that could not be achieved using conventional methods. For example (but not limited to), in the production of viscous high concentrated emulsions or polymeric suspensions.
- Water-in-oil emulsions can be prepared using different combination of water and oil phases as indicated for the preparation of oil- in-water emulsions.
- Oil soluble surfactants can be dissolved in the oil continuous phase such as (but not limited to) SpanTM 80, SpanTM 85, SY Glyster PO-5S.
- emulsions can also be prepared using a primary emulsion as dispersed phase.
- the method can also be used to prepare solid particles by polymerization process or by direct chemical precipitation.
- Polymeric solutions such as (but not limited to) polyvynil acetate (PVA) or chitosan can be used to produce solid particles by emulsion droplets polymerization.
- PVA polyvynil acetate
- chitosan can be used to produce solid particles by emulsion droplets polymerization.
- high-melting point solid lipid material such as (but not limited to) cocoa butter, hard wax it is also possible to produce solid particles by direct precipitation by cooling down method.
- the temperature of the membrane emulsification process is kept at a higher temperature than the melting point of the oil phase.
- Emulsion droplets are produced through the temperature-controlled membrane emulsification step while the resultant emulsions are immediately cooled to solidify the oil phase.
- the method is particularly suitable for this specific application because the temperature-controlled emulsification step can be carried out by controlling the temperature operative conditions at the membrane module level where the emulsion is obtained while the solidification cooling step will be obtained outside of the membrane module. This is possible because the emulsion is not recirculated along the circuit.
- solid lipid particles are produced by conventional cross-flow membrane emulsification, it is necessary to keep the equipment, included dispersed phase and continuous phase circuit, under controlled temperature conditions to prevent the solidification of the dispersed phase at the membrane level without production of particles.
- the back-and-forward movement is described by two parameters: amplitude and frequency.
- amplitude comprised between 10 and 400 mm and a frequency comprised between 0,1 and 5 Hz were used in the production of 0/W emulsions.
- a specific range of frequency and amplitude must be chosen for a selected formulation. In general, high frequency and low amplitude permit to generate uniform droplets with size equal to three times the pore diameter.
- the method was proven with membranes having 3 micron as pore size in a range between 10-400 mm as amplitude and 0,1-5 Hz as frequency in the preparation of oil-in-water emulsions.
- the method of the present invention may be adapted to produce particles with membranes having both lower and higher pore size, in principle with no limitations but preferably in the range of 0,2 - 20 micron pore size.
- the range of amplitude and frequency could be adapted on the basis of pore size (especially for the larger size) and physical chemical properties.
- FIG. 1 a schematic figure of the apparatus used for pulsed membrane emulsification according to the present invention is shown, wherein a membrane module 10 is present.
- a dispersed phase B coming from a dispersed phase vessel 11, is fed to the membrane module 10, on a first side of the porous membrane wall 4, having a first and a second side, by a dispersed phase inlet conduit 12.
- the dispersed phase B is pressed through the membrane wall 4 by a pressurized gas, contained in a gas vessel 13.
- the continuous phase A coming from a continuous phase vessel 14, is fed to the membrane module 10, on the second side of the membrane wall 4, by a continuous phase inlet conduit 15 and "shaked" using a programmable pump 16 with reverse flow direction function.
- Pressure gauges 17 and valves 18 are also present in order to control pressure and flow within the membrane module 10.
- valve 19 is open, so the emulsion is removed from the lumen 1 of the membrane module 10 through an emulsion outlet conduit 20 and stored in an emulsion vessel 21.
- a dispersed phase outlet conduit 22 is also present, and provided with a valve 23.
- Oil pressure was ensured by N 2 gas and it was injected from the shell side of the membrane.
- the continuous phase was recirculated or pulsed on the lumen side of the membrane by peristaltic pump (Digi- Staltic double-Y Masterflex ® pump Micropump, model GJ- N23. JF1SAB1) .
- the applied transmembrane pressure (TMP) was 0,7 bar.
- the axial flow rate velocity along the circuit was 850 ml/min that correspond to an axial velocity of 0,26 m/s.
- Dispersed phase flux, oil %, droplets size and droplets size distribution were evaluated and monitored as a function of time during pulsed membrane emulsification experiments.
- the initial continuous phase volume used was 30 ml. Around 30% of oil was obtained in approximately 2,5 hours. After that 30% oil was obtained, emulsion was removed and 30 ml of fresh continuous phase was replaced. The process was carried out until 30% oil was obtained in 120 ml of emulsion total volume.
- the dispersed phase flux maintained a constant value of 1 ⁇ 0,08 1/hm 2 for the duration of the experiment . Uniform droplets with span values of 0,8 were obtained. No difference in droplet size and droplets size distribution was observed when the oil % in emulsion increased.
- Table 1 shows that when cross-flow membrane emulsification method was used droplets size uniformity was lost when highly concentrated emulsions are produced and span changed from 0,8 to 3,5. The most significant effect on droplets size was observed in the volume-weighted mean particle diameter (D[4,3]) which is more sensitive to the presence of any large particles and D[4,3] changed from 9,8 micron to 16,5 micron.
- This emulsification method guarantees appropriate shear stress at the membrane level while preventing the shear stress effect related to the recirculation of emulsion droplets along the circuit within the pump and fitting in cross-flow membrane emulsification.
- This innovative technique is suitable for the production of bioactive functionalized particles, viscous dispersed materials and large droplets with uniform size .
- Pulsed membrane emulsification technology has many advantages compared to the conventional emulsification methods and the other membrane emulsification mode operations used.
- Pulsed membrane emulsification technology guarantees appropriate shear stress at the membrane level while preventing the shear stress effect related to the recirculation of emulsion droplets along the circuit within the pump and fitting in cross -flow membrane emulsification.
- Pulsed membrane emulsification technology permits to obtain uniform emulsion droplets also using trans-membrane pressure value higher than the critical pressure and with high final dispersed phase concentration .
- Pulsed membrane emulsification technology is suitable for the production of bioactive functionalized particles, viscous dispersed materials and large droplets with uniform size.
- Pulsed membrane emulsification technology permits to operate for hours in continuous mode without decrease of dispersed phase flux and perfect control in terms of droplets size and size distribution.
- Pulsed membrane emulsification technology is related to the development of a new method for collecting droplets in a single pass in the continuous phase along the lumen of the microporous membrane.
- the method allows obtaining highly concentrated uniform liquid droplets without damaging.
- the great advantage of the single pass pulsed membrane emulsification is that it eliminates the shear stress outside of the membrane related to the recirculation of emulsion droplets along the pump and fitting circuit as it happens in conventional cross- flow membrane emulsification.
- Pulsed membrane emulsification technology permits to eliminate the shear stress to which the particles are subjected in the circuit outside of the membrane since emulsion is produced in the membrane with a single pass mode .
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Colloid Chemistry (AREA)
Abstract
Description
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Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IT000378A ITRM20120378A1 (en) | 2012-08-02 | 2012-08-02 | METHOD AND EMULSIFICATION EQUIPMENT WITH SINGLE PULSE PASSAGE MEMBRANE. |
PCT/IT2013/000218 WO2014020631A1 (en) | 2012-08-02 | 2013-08-02 | Single/pass pulsed membrane emulsification method and apparatus |
Publications (2)
Publication Number | Publication Date |
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EP2879779A1 true EP2879779A1 (en) | 2015-06-10 |
EP2879779B1 EP2879779B1 (en) | 2018-05-30 |
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ID=46939848
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP13762293.2A Active EP2879779B1 (en) | 2012-08-02 | 2013-08-02 | Single/pass pulsed membrane emulsification method and apparatus |
Country Status (3)
Country | Link |
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EP (1) | EP2879779B1 (en) |
IT (1) | ITRM20120378A1 (en) |
WO (1) | WO2014020631A1 (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111615379B (en) * | 2018-01-19 | 2023-03-28 | 株式会社Lg生活健康 | Cosmetic composition comprising particles containing high content of ceramide and method for producing same |
CN113631249A (en) * | 2019-04-17 | 2021-11-09 | 宝洁公司 | Device and method for producing an emulsion |
CN114534531A (en) * | 2022-03-08 | 2022-05-27 | 南京工业大学 | Method for preparing W/O and O/W emulsion without using emulsifier |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2885408B2 (en) * | 1988-11-30 | 1999-04-26 | 冷化工業株式会社 | Mixing device |
JPH11333271A (en) * | 1998-05-28 | 1999-12-07 | Reika Kogyo Kk | Membrane emulsifying device |
FR2845619B1 (en) * | 2002-10-15 | 2005-01-21 | Christophe Dominique No Arnaud | DEVICE AND METHOD FOR MANUFACTURING MIXTURE, DISPERSION OR EMULSION OF AT LEAST TWO NON-MISCIBLE REPUTABLE FLUIDS |
JP2008517760A (en) * | 2004-10-29 | 2008-05-29 | コーニンクレッカ フィリップス エレクトロニクス エヌ ヴィ | Apparatus and method for producing ultrasonic contrast agent |
GB2444035A (en) * | 2006-11-25 | 2008-05-28 | Micropore Technologies Ltd | An apparatus and method for generating emulsions |
GB2467925A (en) * | 2009-02-19 | 2010-08-25 | Richard Graham Holdich | Membrane emulsification using oscillatory motion |
-
2012
- 2012-08-02 IT IT000378A patent/ITRM20120378A1/en unknown
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2013
- 2013-08-02 EP EP13762293.2A patent/EP2879779B1/en active Active
- 2013-08-02 WO PCT/IT2013/000218 patent/WO2014020631A1/en active Application Filing
Non-Patent Citations (1)
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Also Published As
Publication number | Publication date |
---|---|
EP2879779B1 (en) | 2018-05-30 |
ITRM20120378A1 (en) | 2014-02-03 |
WO2014020631A1 (en) | 2014-02-06 |
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