GB2467925A - Membrane emulsification using oscillatory motion - Google Patents
Membrane emulsification using oscillatory motion Download PDFInfo
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- GB2467925A GB2467925A GB0902809A GB0902809A GB2467925A GB 2467925 A GB2467925 A GB 2467925A GB 0902809 A GB0902809 A GB 0902809A GB 0902809 A GB0902809 A GB 0902809A GB 2467925 A GB2467925 A GB 2467925A
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- 239000012528 membrane Substances 0.000 title claims abstract description 139
- 230000003534 oscillatory effect Effects 0.000 title claims abstract description 22
- 238000004945 emulsification Methods 0.000 title description 4
- 238000000034 method Methods 0.000 claims abstract description 23
- 230000010355 oscillation Effects 0.000 claims description 24
- 239000000839 emulsion Substances 0.000 abstract description 18
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- 238000005188 flotation Methods 0.000 description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 description 7
- 229940068984 polyvinyl alcohol Drugs 0.000 description 7
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 7
- 229940110456 cocoa butter Drugs 0.000 description 6
- 235000019868 cocoa butter Nutrition 0.000 description 6
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- 239000001814 pectin Substances 0.000 description 6
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- 238000003756 stirring Methods 0.000 description 4
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- 244000215068 Acacia senegal Species 0.000 description 3
- 229920000084 Gum arabic Polymers 0.000 description 3
- 239000000205 acacia gum Substances 0.000 description 3
- 235000010489 acacia gum Nutrition 0.000 description 3
- 239000002775 capsule Substances 0.000 description 3
- 235000019219 chocolate Nutrition 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
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- 229940127557 pharmaceutical product Drugs 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- DLRVVLDZNNYCBX-UHFFFAOYSA-N Polydextrose Polymers OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(O)O1 DLRVVLDZNNYCBX-UHFFFAOYSA-N 0.000 description 2
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- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 1
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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
-
- B01F11/00—
-
- 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
- B01F23/45—Mixing liquids with liquids; Emulsifying using flow mixing
- B01F23/451—Mixing liquids with liquids; Emulsifying using flow mixing by injecting one liquid into another
-
- B01F3/0819—
-
- 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
-
- 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
- B01F31/44—Mixers with shaking, oscillating, or vibrating mechanisms with stirrers performing an oscillatory, vibratory or shaking movement
- B01F31/441—Mixers with shaking, oscillating, or vibrating mechanisms with stirrers performing an oscillatory, vibratory or shaking movement performing a rectilinear reciprocating movement
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
An apparatus 100 and method for dispersing a first phase 110 in a second phase 111 comprises a membrane 107, defined by a plurality of holes 130, arranged to connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane and enabling a first phase in the first volume to egress into a second phase in the second volume. Relative shear is provided between the membrane and the second phase, formed by relative oscillatory motion 102 of the membrane. The direction of relative oscillatory motion is perpendicular to the direction of egression of the first phase. A buoyancy aid or float is attached to the membrane. An emulsion of the first phase dispersed within the second phase results from the relative oscillatory motion. In other aspects of the invention, the membrane is a filter membrane or sintered membrane.
Description
TITLE
An apparatus and method for assisting vibrating membrane emulsification
FIELD OF THE INVENTION
Embodiments of the present invention relate to an apparatus for assisting in the use of a membrane which is being vibrated within a liquid for the purpose of emulsion generation.
BACKGROUND TO THE INVENTION
Generating emulsions, or dispersions, by means of a membrane is when one, or more, first phase is passed through the membrane into another immiscible phase on the other side of the membrane from the first phase. The resulting emulsions and dispersions may be of two, or more, immiscible phases. For the purpose of generating the drops of the first phase within the second phase shear, dr relative motion, between the second phase and the membrane is employed. Higher shear at the membrane surface generates finer drops. One method for generating the shear is to oscillate the membrane within the otherwise static secondary phase. This requires an oscillator drive system that may have to provide a high force in order to successfully oscillate the membrane at high frequencies and amplitudes. This is due to the weight of the membrane system being moved by the oscillator, where high frequency, or amplitude, requires high acceleration.
Dispersions of oil in water, and dispersions of small sized capsules containing solids, or fluids, are of considerable economic importance and are used, by way of example, for creams and lotions, delayed release pharmaceutical products, pesticides, paints and varnishes, spreads and foods. In several instances it is desirable to encase particles in a covering of another phase (microcapsules), to produce a barrier to the ingredient readily dissolving or reacting too quickly in its application. One such example is a delayed release pharmaceutical product.
In many applications it is desirable to employ a consistent drop, or dispersion, size. For example, in the case of a controlled release pharmaceutical product a consistent microcapsule size would result in a predictable release of the encapsulated product. Conversely, a wide drop size distribution would result in rapid release of the product from the fine capsules, which have a high surface area to volume ratio, and a slow release from the larger capsules.
Another example is a surface finish, such as paint, lacquer or varnish where a size distributed dispersion would result in a bumpy surface finish.
Current emulsion manufacturing techniques use: stirrers and homogenisers. A two phase dispersion with large drops is forced though valves and nozzles to induce turbulence and thereby to break up the drops into smaller ones.
However, it is not possible to control the drop sizes achieved and the size range of drop diameters is usually large. This is a consequence of the fluctuating degree of turbulence found in the systems described and the
exposure of the drops to a variable shear field.
In recent years, there has been much research interest in the generation of emulsions using microfilter membranes. Patent Application Number WO 01/45830 Al describes apparatus for dispersing a first phase in a second phase, comprising a tubular microfilter connecting an interior volume of one liquid phase and an exterior volume of the second immiscible liquid phase.
Typically the first phase is provided under pressure to the interior volume of the tubular microfilter and the second phase is circulated through the exterior volume. The method for generation of shear at the surface of the membrane at which the liquid drops egress is by rotation of the tubular membrane. This device has found some application in laboratory studies, but the principle of operation is not one that is easily used in a multiple tube environment for significant commercial application.
It would be desirable to improve further how emulsions are generated in a commercial environment.
BRIEF DESCRIPTION OF VARIOUS EMBODIMENTS OF THE INVENTION
According to one aspect of the present invention there is provided an apparatus for dispersing a first phase in a second phase, comprising: a membrane defining a plurality of through holes that connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane, and through which the first phase egresses from the first volume into the second phase in the second volume; and means for relative oscillating motion of the second phase, or the membrane, in a direction perpendicular to the direction of egression of the first phase, where the application of a buoyancy assisting flotation chamber reduces the load on the oscillation generation system, enabling more aggressive conditions of shear to be reached by the oscillation system.
According to another aspect of the present invention there is provided an apparatus for dispersing a first phase in a second phase, comprising: a membrane defining a plurality of through holes that connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane, and through which the first phase egresses from the first volume into the second phase in the second volume; and means for developing a consistent oscillatory shear field in the second phase at the membrane over the plurality of through holes.
According to another aspect of the present invention there is provided a method for use in dispersing a first phase in a second phase, comprising: providing relative oscillatory motion in a first direction between a membrane, defining a plurality of through holes, and a second phase, while the first phase egresses through the through holes into the second phase in a direction substantially perpendicular to the first direction, where the application of a buoyancy assisting flotation chamber reduces the load on the oscillation generation system, enabling more aggressive conditions of shear to be reached by the oscillation system.
According to another aspect of the present invention there is provided a method for use in dispersing a first phase in a second phase, comprising: providing a consistent oscillatory shear field in a second phase at a membrane over the membrane's plurality of through holes, while the first phase egresses through the plurality of through holes into the second phase.
According to various, but not necessarily all, embodiments of the invention there is provided an apparatus for dispersing a first phase in a second phase, comprising: a filter membrane arranged to connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane, and configured for enabling a first phase in the first volume to egress into a second phase in the second volume; a buoyancy aid attached to the membrane; and means for providing relative shear in a first direction between the membrane and the second phase formed by relative oscillatory motion of the second phase and the membrane in the first direction, the first direction being perpendicular to the direction of egression of the first phase.
According to various, but not necessarily all, embodiments of the invention there is provided a method for dispersing a first phase in a second phase, comprising: providing a filter membrane arranged to connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane, and configured for enabling a first phase in the first volume to egress into a second phase in the second volume; attaching a buoyancy aid to the membrane; and means for providing relative shear in a first direction between the membrane and the second phase formed by relative oscillatory motion of the second phase and the membrane in the first direction, the first direction being perpendicular to the direction of egression of the first phase.
BRIEF DESCRIPTION OF THE DRAWINGS
For a better understanding of embodiments of the present invention reference will now be made by way of example only to the accompanying drawings in which: Fig. 1 illustrates an apparatus for dispersing a first phase in a second phase employing vibration of the membrane without the application of a buoyancy aiding float chamber; and Fig. 2 illustrates an embodiment of an apparatus for dispersing a first phase in a second phase using a buoyancy aiding float chamber.
DETAILED DESCRIPTION OF VARIOUS EMBODIMENTS OF THE
INVENTION
Figs. 1 and 2 schematically illustrates an apparatus 100 for dispersing a first phase 110 in a second phase 111, comprising a membrane 107 defining a plurality of through holes 130 that connect a first volume on a first side of the membrane 107 to a second volume on a second different side of the membrane 107, and through which the first phase 110 egresses from the first volume into the second phase 111 in the second volume; and vibration means 102 for relatively vibrating the membrane 107 in a direction perpendicular to the direction of egression of the first phase 110.
In Fig. 1, the apparatus 100 disperses a first liquid phase 110 in a second liquid phase 111. The first liquid 110 is immiscible in the second liquid 111 and is contained in a reservoir 112 from where it is transferred into a tubular mem6rane 107 by means of a pump 114. The first liquid 110 is consequently provided to the tubular membrane 107 under pressure. Although in this example the pressure is provided by a pump 114, in other examples it may be provided by other means such as hydrostatic pressure.
The tubular membrane 107 has a plurality of through holes 130, which are completely submerged in the second liquid 111 contained by a vessel 108.
The first liquid 110 egresses through the through holes 130 and enters the second liquid 111, while the membrane 107 is subject to vertical oscillation 102, typically at a frequency of between 10 to 5000 Hz.
The vertical rectilinear oscillation 102 develops a consistent oscillatory shear at the surface of the tubular membrane 107. The oscillatory shear field is consistent over the plurality of through holes 130. Thus, the first phase as it emerges through each of the through holes 130 is subject to the same consistent oscillatory shear field perpendicular to the direction of egress. This enables the formation of drops 115 of the first liquid 110 within the second liquid 111 that are of consistent size.
The tubular membrane 130 has a solid base 125 to prevent passage of the first liquid 110 into the second liquid 111 by any means other than the through holes 120.
The apparatus of Fig. 1 is particularly advantageous in that the membrane does not need to be of a tubular shape or of uniform cross section to ensure a uniform shear at its surface. The membrane 130 may, for example, be formed from rectangular boxes, sheets or discs.
Fig. 2, schematically illustrates the invented apparatus for dispersing a first phase 110 in a second phase 112. The apparatus of Fig. 2 is similar to the apparatus of Figure 1 and like reference numerals are used to denote like features.
The apparatus of Fig. 2 differs from the apparatus of Fig. I in that a buoyancy aiding float chamber 127 is attached to the membrane tube 107 and can be wholly or partially submerged within the second liquid 111, in order for a flotation effect to occur. Embodiments of the present invention employ the flotation chamber/float/buoyancy aid 127, to reduce the effective mass of the membrane system when it is immersed within a liquid, thus reducing the effective weight of the membrane system when immersed in a liquid, and permitting higher shears to be used from the oscillator than without the buoyancy aid.
The membrane 107 may be of any suitable type. It may for example be a ceramic membrane formed by sintering particles together or it may be a micro filter membrane such as described in patent application GB 0202832.2.
Therefore, the membrane may be formed by providing a lamina substrate having a first surface, a substantially parallel second surface and a plurality of apertures extending directly through the substrate between the first and second surfaces. A layer of material (e.g. metallic plating) is then provided on the substrate and which extends over at least a portion of the lamina substrate and into the plurality of apertures to form a plurality of filter holes which may have a filtering dimension of less than 10 microns. The plurality of filter holes may be slot shaped.
Although embodiments of the invention are described in relation to "inside-out" embodiments in which the first phase moves from the inside of a membrane 107 to the outside, embodiments of the invention may also be applied to "outside-in" arrangements in which the first phase moves from the exterior of the membrane into the interior and the dispersion is formed in the interior of the membrane.
It should also be appreciated that the described embodiments may be used in the formation of double emulsions, whereby an emulsion is produced firstly by injecting a dispersed phase into a continuous phase and then the resulting emulsion is injected into another continuous phase through pores of a large diameter. The apparatus may be used with a first type of membrane 107 to inject a first dispersed phase into a continuous phase and then can be used with a different membrane 107 to inject the resulting emulsion into another continuous phase.
Although in the described embodiments, the first and second phases are liquids, it should be appreciated that the first and/or second phase may also contain finely divided solids or gases, for example.
The technological method of generating drops is now described below together with a comparison with existing methods to generate emulsions using membrane systems. In a 1997 publication, W09736674, crossflow of one liquid phase over the surface of a microfilter with varying internal diameter is used, and in the paper preparation of monodisperse microspheres using the Shirasu porous glass emulsification technique' by Sinzo Omi, Colloids and Surfaces A; 109, 1996, pp 97-107, crossflow over a sintered glass tube is used. In both of these cases, great effort is made to maintain uniform shear of the liquid phase flowing over the surface of the microfilter so that the immiscible liquid emerging from the pores of the microfilter experiences a uniform shear field, resulting in a uniform force on the emerging liquid and, therefore, a near uniform drop size. The drop will break away from the surface of the microfilter when the shear is sufficient to overcome the surface tension force holding the emerging liquid together, in the pore of the filter, and any adhesion force between the emerging liquid and the solid surface of the filter.
In the system described by Figs I and 2, a uniform shear field does not exist.
Instead, the shear field is oscillating in a sinusoidal manner; between zero shear and high shear in one direction and then high shear in the reverse direction. However, the shear at the membrane surface is varying in this manner consistently over the full surface of the microfilter. Thus, when moved in accordance with Fig I and 2, the shear varies in a consistent linear oscillation'. Clearly, the consistent linear oscillation does not demand a particular geometry in order to function: the filter could be a flat plate, tube, rectangular box, etc. A consistent oscillation will generate a uniform emulsion, or dispersion, so long as the rate of oscillation is sufficiently high enough such that the emerging liquid drop, from a microfilter pore, experiences a number of oscillations. At the peak shear during an oscillation, where the gradient on the sinusoidal curve is the greatest, the drop will break free from the surface because the shear force is sufficient to overcome the surface tension force and any adhesion force between the emerging liquid and the solid surface of the filter. This surface shear is a function of both the frequency and the amplitude of oscillation. Hence, there are two independent means of controlling the peak shear at the surface, providing a system that has a high degree of control over the surface shear and, hence, the formed drop size.
However, the use of an oscillating membrane tube requires a robust method of oscillating the tube, the driving mechanism has to oscillate the tube rapidly and support the weight of the oscillating tube. The force required to do this at high frequencies and amplitudes of oscillation is substantial. This force can be reduced significantly by reducing the effective weight of the membrane tube assembly to almost zero, by using a buoyancy aiding flotation chamber whereby the upthrust force, from the buoyancy effect of the displaced liquid by the chamber, counteracts the weight force of the membrane tube assembly.
This enables the oscillator to be used primarily to overcome the drag force within the system, providing a much more flexible system by increasing the frequency and amplitude over which the system can operate.
This method of generating emulsions, or drops, is different from the commonly employed technique of vibrating a tube, orifice (see US2002054912 for an example), or plate behind an orifice for two main reasons. Firstly, in the case of emulsions, and dispersions, a membrane with a multitude of pores is used -rather than a single orifice. Secondly, the vibration employed in these other systems is normal to the orifice, or hole, whereas embodiments of the invention here rely on oscillation perpendicular to the membrane pores. It would not be possible to generate a uniform emulsion by providing a system with a multitude of pores using a normal vibratory source, as the shear field would vary in an inconsistent fashion over the surface of all the pores; as the shear would depend on the distance from the normal vibratory source.
Whereas in embodiments of the present invention the shear field varies, but in a highly consistent fashion over all the pores. Thus, in the prior art, it is shown that it is possible to generate uniform drops from a single orifice with normal vibration, but the technique is both different to that described here and generates only single drops at a time, whereas embodiments of the present invention describe a technique whereby a multitude of uniform drops may be generated simultaneously over the surface of the microfilter assisted by the buoyancy assisting flotation chamber. There are many similar patents where vibration normal, or perpendicular, to the membrane surface has been employed, see US 4793714 and FR 2699091 Al for two further examples.
This mode of oscillation is well known and is completely different to the method of linear oscillatory vibration of the membrane surface parallel to that surface, as illustrated in Fig I and Fig 2.
Embodiments of the invention will now be described, by way of example only, with reference to Fig 1 and Fig 2.
A tubular microfilter, as prepared according to patent application GB 0202832.2, was mounted vertically inside a beaker with the lower end blocked off. Poly Vinyl Alcohol (PVA) particles were produced by first dispersing an aqueous solution of 15% PVA into a continuous phase of kerosene containing the surfactant Span 80 through a single tubular membrane containing an array of pores 20 microns in diameter. The tube dimensions were: 14 mm outside diameter and 60 mm length. The arrangement was similar to Fig 1: the membrane was mounted on an electrically driven oscillator and vibrated within the kerosene. The frequency of oscillation was 72 Hz and the limit of the force that the amplifier could provide to power the oscillator was 98 Newtons, for sine wave oscillation. The armature and load mass on the system was 0.32 kg, and in this liquid system the maximum amplitude possible was 1.5 mm (i.e. peak to peak oscillation value of 3 mm). When attempting to operate the oscillator amplifier at higher power values, leading to higher amplitudes, the oscillator amplifier reached its maximum capacity and the safety cut-out stopped any further operation. At this combination of frequency and amplitude the median drop size of the PVA solution was 70 microns. However, when employing a buoyancy aid consisting of a 60 mm diameter cylinder 80 mm long attached to the shaft above the membrane generating section, where this float section was sealed and contained air, the net mass of the armature and load on the oscillator reduced to 0.125 kg, when immersed in the liquid, as measured by a spring scale. It was then possible to run the same power amplifier and oscillator up to an amplitude of 3.5 mm (7 mm peak to peak), before the safety cut-out prevented any further increase in amplitude of oscillation. The resulting PVA drop size reduced to 55 microns, due to the increase in amplitude used during the membrane emulsification.
The total mass of the membrane system, including the float chamber, when weighed in air was 0.34 kg, which is greater than the system without the float chamber, but the presence of the float chamber reduced the effective load on the oscillator when submerged in a liquid.
The PVA drops were then crosslinked by addition of glutaraldehyde to the kerosene liquid and the mixture was left to gently stir for ten hours to form the solidified PVA particles from the aqueous phase drops. By thus controlling the frequency and amplitude of linear oscillation of the membrane it was possible to produce solid particles that had 90% of their size distribution between 40 and 70 microns, as measured by a Coulter Multsizer model II. These beads are of a sufficiently uniform quality for use in chromatography applications for blood diagnostic tests.
In another example a tubular microfilter, with an internal diameter of 14 mm and slot width of 5 micrometres and slot length of 400 micrometres, prepared according to patent application GB 0202832.2, was mounted vertically and connected to a linear oscillator, with the flotation chamber mounted above the membrane section. The membrane tube contained slotted pores which were arranged perpendicular to the direction of the shear field, which was generated by the linear oscillation of the tubular membrane within melted cocoa butter. A pectin solution to be used for the egression was prepared by placing a mass of 494 g of water in a two litre beaker with a suspended magnetic stirrer and heated up to 80°C. The inner bar could rotate freely from the supports and it was stirred at a rate sufficient to provide an air vortex. A mass of 6 g of pectin was weighed out and very slowly added to the stirred water -in the air core, but away from the top of the suspended stirrer. To cool, the solution was left stirring with the heater turned off. The stock pectin solution was left overnight to swell the hydro-colloid. A second solution of: Gum Arabic, sugar and calcium chloride was prepared by placing a mass of 59.5 g water in a beaker and a magnetic stirrer added. The water was heated to no more than 80°C. A mass of 0.4 g of Gum Arabic was added slowly whilst stirring rapidly. When the Gum Arabic had dissolved 10 g of polydextrose and 0.033 g of calcium chloride was added.
The two solutions were to form the aqueous phase to become the egression liquid into a melted liquid of cocoa butter oil. The mass of cocoa butter used was 93 g, to which 7 g of the well-known chocolate surfactant polyglycerol polyricinoleate (PGPR) was added. The mass of pectin solution used was 30 g and the mass of gum, sugar and calcium solution was 70 g. The two aqueous solutions were heated to 80°C in separate containers and agitated by magnetic stirrers. When at temperature, the gum, sugar and calcium solution was poured in to the pectin solution whilst stirring vigorously. Gelling immediately started. After further mixing for 5 minutes the temperature dropped to 45 to 50°C and the gel was of an acceptable consistency for injection into the cocoa butter. Egression of the gel in to the cocoa butter continuous phase, which had been heated to 40°C, was performed. The temperature of the dispersed phase was maintained at 80°C during injection and the temperature of the two-phase mixture was maintained at between 40 and 45°C during the process. A linear oscillation frequency of 60 Hz and 3 mm amplitude was used.
Samples of the dispersion were taken for microscope analysis during the egression. The liquid cocoa oil was mixed with kerosene to dilute the drops sufficiently to observe them under the microscope. The largest aqueous drop size obtained was 12 micrometres and there is a substantial amount of drops with diameters less than 8 micrometres. During the egression process the pressure required to inject the egression liquid was monitored, to check for membrane blockage, and the pressure remained constant at only a few inches of water gauge. Hence, the injection pressure was minimal and stable, a consequence of the use of slotted through holes as the membrane material and the high frequency made possible by using the flotation system. The injection rate was 2 ml per minute per cm length of membrane. In the absence of a flotation system, a maximum frequency of 50 Hz was possible, and 2 mm amplitude, giving rise to drops as large as 15 micrometres, whilst using the lower productivity of 1.5 ml per minute per cm length of membrane. Hence, use of an embodiment of the present invention resulted in more desirable finer drops and a higher productivity. The resulting emulsion of pectin gel in cocoa butter oil was suitable for further processing into a useful product, such as the production of a lower fat chocolate product using conventional, or only slightly modified, chocolate processing technology.
These experiments show that embodiments of the present invention are successful at assisting in the production of closely sized emulsions, or dispersions, and that the system is highly controllable by varying the amplitude of motion. Another possible way to control the size of drop formed is to control the frequency of linear oscillation. Thus, embodiments of the invention provide a system that can be easily tuned to the desired product drop size, by minimising the mechanical effort required by the oscillator system as it reduces the power required to oscillate the membrane. Hence, the power input can be reduced to simply that required to overcome liquid drag, and not liquid drag as well as membrane assembly weight and acceleration.
Although embodiments of the present invention have been described in the preceding paragraphs with reference to various examples, it should be appreciated that modifications to the examples given can be made without departing from the scope of the invention as claimed.
Whilst endeavouring in the foregoing specification to draw attention to those features of the invention believed to be of particular importance it should be understood that the Applicant claims protection in respect of any patentable feature or combination of features hereinbefore referred to and/or shown in the drawings whether or not particular emphasis has been placed thereon.
Claims (15)
- Claims 1. An apparatus for dispersing a first phase in a second phase, comprising: a membrane defining a plurality of through holes that connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane, and configured for enabling a first phase in the first volume to egress into a second phase in the second volume; a float attached to the membrane; and means for providing relative shear in a first direction between the membrane and the second phase formed by relative oscillatory motion of the second phase and the membrane in the first direction, the first direction being perpendicular to the direction of egression of the first phase.
- 2. An apparatus for dispersing a first phase in a second phase, comprising: membrane defining a plurality of inter-connected holes, as provided by a sintered type of membrane, that connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane, and configured for enabling a first phase in the first volume to egress into a second phase in the second volume; a float attached to the membrane; and means for providing relative shear in a first direction between a membrane and a second phase formed by relative oscillatory motion of the second phase and the membrane in a direction perpendicular to the direction of egression of the first phase.
- 3. An apparatus as claimed in claims I or 2, wherein the direction of * oscillation is substantially perpendicular to the direction of egression of the first phase.
- 4. An apparatus as claimed in claims I to 3, wherein the membrane is oscillated perpendicular to the direction of egression of the first phase.
- 5. An apparatus as claimed in any preceding claim wherein the membrane has a vertically extending surface and the relative motion involves substantially oscillatory rectilinear motion in the vertical direction.
- 6. An apparatus as claimed in anyone of claims 1 to 4, wherein the membrane is substantially tubular with an axis, and the relative motion involves substantially oscillatory rotation of the membrane about the axis.
- 7. An apparatus as claimed in any preceding claim, further comprising means for providing the first phase to the first volume under pressure.
- 8. An apparatus for dispersing a first phase in a second phase, comprising: a membrane defining a plurality of through holes that connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane, and configured for enabling a first phase in the first volume to egress into a second phase in the second volume; a float attached to the membrane; and means for developing a consistent oscillatory shear field in the second phase at the membrane over the plurality of through holes.
- 9. An apparatus as claimed in claim 8, wherein the shear field is in a direction substantially perpendicular to the direction of egression of the first phase.
- 10. A method for use in dispersing a first phase in a second phase, comprising: providing a membrane defining a plurality of through holes that connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane, and configured for enabling a first phase in the first volume to egress into a second phase in the second volume; attaching a float to the membrane; and providing relative shear in a first direction between the membrane and the second phase formed by providing relative oscillatory motion in a first direction, wherein the direction of egression of the first phase is substantially perpendicular to the first direction.
- 11. A method for use in dispersing a first phase in a second phase, comprising: providing a membrane defining a plurality of through holes that connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane, and configured for enabling a first phase in the first volume to egress into a second phase in the second volume; attaching a float to the membrane; and providing a consistent oscillatory shear field in the second phase at the membrane over the membrane's plurality of through holes, while the first phase egresses through the plurality of through holes into the second phase.
- 12. An apparatus for dispersing a first phase in a second phase, comprising: a filter membrane arranged to connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane, and configured for enabling a first phase in the first volume to egress into a second phase in the second volume; a buoyancy aid attached to the membrane; and means for providing relative shear in a first direction between the membrane and the second phase formed by relative oscillatory motion of the second phase and the membrane in the first direction, the first direction being perpendicular to the direction of egression of the first phase:
- 13. A method for dispersing a first phase in a second phase, comprising: providing a filter membrane arranged to connect a first volume on a first side of the membrane to a second volume on a second different side of the membrane, and configured for enabling a first phase in the first volume to egress into a second phase in the second volume; attaching a buoyancy aid to the membrane; and means for providing relative shear in a first direction between the membrane and the second phase formed by relative oscillatory motion of the second phase and the membrane in the first direction, the first direction being perpendicular to the direction of egression of the first phase.
- 14. An apparatus or method substantially as hereinbefore described with reference to and/or as shown in the drawings.
- 15. Any novel subject matter or combination including novel subject matter disclosed, whether or not within the scope of or relating to the same invention as the preceding claims.
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GB0902809A GB2467925A (en) | 2009-02-19 | 2009-02-19 | Membrane emulsification using oscillatory motion |
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GB0902809A GB2467925A (en) | 2009-02-19 | 2009-02-19 | Membrane emulsification using oscillatory motion |
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EP2661456A4 (en) * | 2011-01-07 | 2014-08-27 | Purolite Corp | Method of producing uniform polymer beads of various sizes |
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EP4234588A3 (en) * | 2013-03-15 | 2023-09-27 | Purolite Corporation | Method of producing uniform, fine polymer beads by vibration jetting |
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