WO2013056964A1 - Procédé pour la production d'émulsion d'eau dans l'huile alimentaire - Google Patents

Procédé pour la production d'émulsion d'eau dans l'huile alimentaire Download PDF

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Publication number
WO2013056964A1
WO2013056964A1 PCT/EP2012/069036 EP2012069036W WO2013056964A1 WO 2013056964 A1 WO2013056964 A1 WO 2013056964A1 EP 2012069036 W EP2012069036 W EP 2012069036W WO 2013056964 A1 WO2013056964 A1 WO 2013056964A1
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WO
WIPO (PCT)
Prior art keywords
cavities
fat
oil
mixer
emulsion
Prior art date
Application number
PCT/EP2012/069036
Other languages
English (en)
Inventor
Michael John Egan
Eckhard Flöter
Shailendra Gupta
Graeme Neil Irving
Teunis De Man
Henelyta Santos Ribeiro
Petrus Martinus M. Bongers
Original Assignee
Unilever N.V.
Unilever Plc
Hindustan Unilever Limited
Conopco, Inc., D/B/A Unilever
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Application filed by Unilever N.V., Unilever Plc, Hindustan Unilever Limited, Conopco, Inc., D/B/A Unilever filed Critical Unilever N.V.
Publication of WO2013056964A1 publication Critical patent/WO2013056964A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
    • A23D7/02—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by the production or working-up
    • A23D7/04—Working-up
    • 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
    • B01F23/4105—Methods of emulsifying
    • 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
    • B01F23/70—Pre-treatment of the materials to be mixed
    • B01F23/711—Heating materials, e.g. melting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
    • B01F27/272—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces
    • B01F27/2722—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces provided with ribs, ridges or grooves on one surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0436—Operational information
    • B01F2215/0468—Numerical pressure values
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0436—Operational information
    • B01F2215/0481—Numerical speed values
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0486—Material property information

Definitions

  • the present invention relates to a method for the production of an edible water-in-oil emulsion, by using a Controlled Deformation Dynamic Mixer.
  • Mixing can be described as either distributive or dispersive.
  • distributive mixing seeks to change the relative spatial positions of the domains of each phase
  • dispersive mixing seeks to overcome cohesive forces to alter the size and size distribution of the domains of each phase.
  • Most mixers employ a combination of distributive or dispersive mixing although, depending on the intended application the balance will alter. For example a machine for mixing peanuts and raisins will be wholly distributive so as not to damage the things being mixed, whereas a blender/homogeniser will be dispersive.
  • Fat continuous food products are well known in the art and include for example shortenings comprising a fat phase and water-in-oil emulsions like margarine comprising a fat phase and an aqueous phase.
  • Margarine traditionally contains about 80% of an edible fat phase, and 20% of an aqueous phase, that is dispersed as small droplets in the continuous edible fat phase.
  • Other examples of water-in-oil emulsions are low-fat spreads, in which the proportion of edible fat phase is lower and aqueous phase is higher than margarine, for example about 10 to 40% edible fat phase and about 60 to 90% aqueous phase.
  • Such emulsions as described here are commonly known to the consumer as a food product and can usually be spread on bread or toast or the like, or can be used as a frying medium for cooking.
  • the fat phase of margarine and similar edible fat continuous spreads is often a mixture of liquid oil (i.e. fat that is liquid at ambient temperature) and fat which is solid at ambient temperatures.
  • the solid fat also called structuring fat or hardstock fat, serves to structure the fat phase (for example in a shortening as well as in a water-in-oil emulsion) and helps to stabilize the aqueous phase, if present, by forming a fat crystal network.
  • the structuring fat has such properties that it melts or dissolves at mouth temperature upon consumption. Otherwise the product may have a heavy and/or waxy mouthfeel.
  • a fat continuous spread like margarine and low fat spread, are for example hardness, spreadibility and ability to withstand temperature cycling.
  • Temperature cycling means that the product is subjected to low and high temperatures (e.g. when the consumer takes the product out of the refrigerator and leaves it for some time at the table to use it). This may have a negative influence on the structure of the spread (like for example destabilisation of the emulsion or oil-exudation).
  • the fat phase usually contains a mixture of liquid oil (often containing C16-C18 mono- or polyunsaturated fatty acids) and structuring fat (often containing Ci 6 - Ci 8 saturated fatty acids).
  • the warm emulsion is cooled under high shear to induce crystallization of the structuring fat to create an emulsion.
  • a fat crystal network is formed to stabilize the resulting emulsion and give the product some degree of firmness.
  • Common equipment in this step is a scraped surface heat exchanger, wherein the wall of the heat exchanger is at a temperature lower than -10°C.
  • the saturated fatty acids crystallise on the cold wall, and these solids are scraped from the wall.
  • the water-in-oil emulsion is formed in this step, leading to a fine dispersion of aqueous phase droplets (size usually smaller than 10 micrometer) in the continuous fat phase.
  • the droplets are stabilised by small saturated fat crystals on the interface of the droplets.
  • the crystal network is further modified to produce the desired firmness, confer plasticity and reduce the water droplet size. This step is often done in a tube containing a mixer.
  • the choice of fats that can practically be used as structuring agent is rather limited. If the melting point of the structuring agent is too high the melting properties in the mouth are unsatisfactory. If on the other hand, the melting point is too low, the emulsion stability will be negatively affected.
  • Triacylglycerols are the major constituents of natural fats and oils and are esters of glycerol and fatty acids.
  • the chemical structure of the fatty acid and the distribution of the fatty acids over the glycerol backbone determine (at least partly) the physical properties of a fat.
  • the physical properties of fats like for example the solid fat content (SFC) expressed as N-value, can be modified by altering the chemical structure of the fat.
  • SFC solid fat content
  • EP 194 812 A2 discloses a cavity transfer mixer (CTM). Also WO 96/20270 describes a 'Cavity Transfer Mixer', comprising confronting surfaces, each having a series of cavities formed therein in which the surfaces move relatively to each other and in which a liquid material is passed between the surfaces and flows along a pathway
  • the cross- sectional area for flow varies by a factor of less than 3 through the apparatus.
  • WO 96/20270 also describes a novel mixer, hereinafter referred to as a 'Controlled Deformation Dynamic Mixer' (CDDM).
  • this type of mixer has stator and rotor elements with opposed cavities which, as the mixer operates, move past each other across the direction of bulk flow through the mixer. It is distinguished from the CTM in that material is also subjected to extensional deformation.
  • the extensional flow and efficient dispersive mixing is secured by having confronting surfaces with cavities arranged such that the cross sectional area for bulk flow of the liquid through the mixer successively increases and decreases by a factor of at least 5 through the apparatus.
  • the CDDM combines the distributive mixing performance of the CTM with dispersive mixing performance.
  • EP 199 937 A1 describes a mixing device containing a member with cavities rotating within a cylinder containing cavities as well. A fat phase and an aqueous phase are separately cooled and plasticised in the A-unit and C-unit of a votator. Subsequently the phases are mixed in the mixing device, retaining fat crystal structure.
  • WO 2010/089320 A1 disclose specific types of a distributive and dispersive mixing apparatus of the CDDM type or CTM type, comprising two confronting surfaces having cavities therein. These specific types may be used for the treatment of emulsions.
  • US 2010/220545 A1 discloses a mixer with distributive and dispersive action, that can be used for emulsification.
  • WO 2007/105323 A1 discloses a rotor-stator mixer with the intention of forming a water-in-oil emulsion fuel. This device is dispersive in character.
  • JP 7-194301 describes a mixing apparatus used for making emulsions like cream, dressings, and spreads.
  • US 6,468,578 B1 discloses the use of a cavity transfer mixer for creating an emulsion of water droplets in a continuous fat phase.
  • a cream of oil in an aqueous phase is produced which is pasteurised, followed by cooling.
  • Inversion to a water-in-oil emulsion then is conducted in a cavity transfer mixer.
  • the scraped surface heat exchanger is replaced by a cavity transfer mixer as disclosed in EP 199 398 A1.
  • the amount of fat phase in this product is from 50 to 85% by weight.
  • US 5,837,307 discloses a method for making edible fat-continuous emulsions with less than 30% fat, using a cold process.
  • the temperature at mixing of the aqueous phase and the fat phase should not be higher than the melting temperature of the fat phase.
  • the water-in-oil emulsion is formed in a distributive and dispersive mixing apparatus of the Controlled Deformation Dynamic Mixer type to create a water-in-oil emulsion
  • the mixer is suitable for inducing extensional flow in a liquid composition
  • the mixer comprises closely spaced relatively moveable confronting surfaces at least one having a series of cavities therein in which the cavities on each surface are arranged such that, in use, the cross-sectional area for flow of the liquid successively increases and decreases by a factor of at least 5 through the apparatus.
  • the advantage of this method is that energy can be saved, because not the entire premix needs to be pasteurised.
  • a pre-emulsion of aqueous phase and fat phase does not need to be produced, hence it is sufficient if only the aqueous phase is pasteurised before mixing with the fat phase in the CDDM to produce a fat-continuous emulsion.
  • the fat-continuous emulsion is produced in a single process step, and the right consistency and hardness of the emulsion can be achieved without the need to process it any further in another process step. This process requires less unit operations than conventional processes, which makes the process simpler.
  • the invention provides a method for production of an edible water-in-oil emulsion
  • the emulsion comprises an aqueous phase, a structuring fat and a liquid oil, comprising the steps:
  • step b) introducing the molten structuring fat from step a), a liquid oil and an aqueous phase
  • the mixer is suitable for inducing extensional flow in a liquid composition
  • the mixer comprises closely spaced relatively moveable confronting surfaces at least one having a series of cavities therein in which the cavities on each surface are arranged such that, in use, the cross-sectional area for flow of the liquid successively increases and decreases by a factor of at least 5 through the apparatus.
  • FIG. 1 Schematic representation of a Cavity Transfer Mixer (CTM); 1 : stator, 2: annulus; 3: rotor; with cross-sectional views below.
  • CTM Cavity Transfer Mixer
  • FIG. 2 Schematic representation of a Controlled Deformation Dynamic Mixer (CDDM) ; 1 : stator, 2: annulus; 3: rotor; with cross-sectional views below.
  • CDDM Controlled Deformation Dynamic Mixer
  • FIG. 3 Schematic representation of a preferred embodiment of the CDDM
  • cross-sectional view (direction of bulk flow preferably from left to right).
  • the average particle or droplet diameter is generally expressed as the d3,3 value, which is the volume weighted geometric mean particle or droplet diameter.
  • the normal terminology for nuclear magnetic resonance (NMR) is used to measure the parameters d3,3 and sigma (or alternatively exp(sigma)) of a log-normal oil droplet size distribution.
  • Sigma is the standard deviation of the logarithmic of the droplet diameter d3,3.
  • an edible or a food product in the context of the present invention encompasses, but is not limited to, food products including spreads, salad dressings, dairy products, beverages, dietetic foods, dietary supplements, pharmaceutic compositions, and others.
  • the products may contain ingredients common in the art and may be made by methods common in the art.
  • 'fat' and 'oil' are used interchangeably. Where applicable the prefix 'liquid' or 'solid' is added to indicate if the fat or oil is liquid or solid at ambient temperature as understood by the person skilled in the art.
  • 'structuring fat refers to a fat that is solid at ambient temperature.
  • 'liquid oil' refers to an oil that is liquid at ambient temperature.
  • Edible fats contain a large number of different triacylglycerols (TAGs) with varying physical properties.
  • TAGs triacylglycerols
  • the TAGs in edible fats are composed of fatty acids with an even number of carbon atoms in the chains, generally varying between 4 and 24 in number.
  • Common fatty acids from vegetable origin are C10, C12, C14, C16, C18, C20 and C22, and most common TAGs are composed of these fatty acids.
  • each fatty acid can contain up to three double bonds at certain positions in the chain.
  • fish oil contains a high number of unsaturated fatty acids with more than one unsaturated bond in the chain.
  • the terms 'triacylglycerols', 'TAGs', and 'triglycerides' may be used interchangeably in here.
  • Ambient temperature is considered to be a temperature between about 20°C and about 25°C, preferably between 20°C and 25°C, preferably between 20°C and 23°C.
  • CTMs Cavity Transfer Mixers
  • CTMs are defined as mixers comprising confronting surfaces, at least one of the surfaces, preferably both surfaces, having a series of cavities formed therein in which the surfaces move relatively to each other and in which a liquid material is passed between the surfaces and flows along a pathway
  • the cavities are arranged on the relevant surfaces such that shear is applied to the liquid as it flows between the surfaces.
  • the cavities are arranged on the respective surfaces such that there is a relatively small change in the effective cross sectional flow area as the material passes through the mixer. In such mixers, primarily distributive mixing is obtained.
  • the cross-sectional area for flow varies by a factor of less than 3 through the apparatus. Shear is applied by the relative movement of the surfaces in a generally perpendicular direction to the flow of material there between.
  • FIG. 1 displays an axial section and four transverse radial sections through a CTM configured as a 'concentric cylinder' device and comprising an inner rotor journalled within an outer stator.
  • the axial section shows the relative axial positions of rotor and stator cavities which are time invariant, whereas the transverse sections (A-A, B-B, C-C, D-D) demonstrate the axial variation in the available cross-sectional area for material flow axially:
  • CDDMs Controlled Deformation Dynamic Mixers
  • CDDMs are distinguished from CTMs by their description as mixers: comprising confronting surfaces, at least one of the surfaces, preferably both surfaces, having a series of cavities formed therein in which the surfaces move relatively to each other and in which a liquid material is passed between the surfaces and flows along a pathway successively through the cavities in each surface and is subjected to extensional deformation and/or shear deformation and preferably both extensional and shear deformation.
  • the cavities are arranged on the relevant surfaces such that shear is applied by the relative movement of the surfaces in a generally perpendicular direction to the flow of material there between.
  • significant extensional flow and efficient distributive and dispersive mixing may be secured by providing an apparatus having confronting surfaces and cavities therein in which the cavities are arranged such that the cross sectional area for flow of the liquid successively increases and decreases by a factor of at least 5 through the apparatus.
  • CDDMs by reference to Figure 2 which displays an axial section and four transverse radial sections through a CDDM configured as a 'concentric cylinder' device comprising an inner rotor journalled within an outer stator.
  • the axial section shows the relative axial positions of rotor and stator cavities which are time invariant, whereas the transverse sections (A-A, B-B, C-C, D-D) demonstrate the axial variation in the available cross-sectional area for material flow axially :
  • CDDMs are distinguished from CTMs by the relative position of the rotor and stator and consequent incorporation of an extensional component of flow.
  • CDDMs combine the distributive mixing performance of CTMs with the dispersive mixing performance of multiple expansion-contraction static mixers.
  • the invention provides a method for production of an edible water-in-oil emulsion, wherein the emulsion comprises an aqueous phase, a structuring fat and a liquid oil, comprising the steps:
  • step b) introducing the molten structuring fat from step a), a liquid oil and an aqueous phase
  • the mixer is suitable for inducing extensional flow in a liquid composition
  • the mixer comprises closely spaced relatively moveable confronting surfaces at least one having a series of cavities therein in which the cavities on each surface are arranged such that, in use, the cross-sectional area for flow of the liquid successively increases and decreases by a factor of at least 5 through the apparatus.
  • structuring fat refers to a fat that is solid at ambient temperature.
  • the structuring fat serves to structure the emulsion by providing at least part of the structuring fat for the emulsion.
  • the structuring fat is in the form of an edible fat powder, prior to being molten in step a).
  • the main components of structuring fat are triacylglycerols.
  • the structuring fat may originate from one or more natural fats. Structuring fat as commercially available may comprise minor amounts of other components like for example monoglycerides that are naturally present and may likewise be present in the solid particles.
  • the structuring fat may be a single fat or a mixture of different fats.
  • the structuring fat may be of vegetable, animal (e.g. dairy fat) or marine origin.
  • Preferably at least 50 wt% of the structuring fat (based on total amount of structuring fat) is of vegetable origin, more preferably at least 60 wt%, even more preferably at least 70 wt%, still more preferably at least 80 wt%, even still more preferably at least 90 wt% and even still more further preferably at least 95 wt%.
  • the structuring fat essentially consists of structuring fat of vegetable origin.
  • the natural fat is selected from the group consisting of palm fat, allan blackia, pentadesma, shea butter, coconut oil, soybean oil, rapeseed oil and dairy fat. More preferably the natural fat is selected from the group consisting of palm oil, palm kernel oil, palm oil fraction, palm kernel fraction, coconut oil and dairy fat fraction. Even more preferably the natural fat is selected from the group consisting of palm oil, palm kernel oil, palm oil fraction, palm kernel fraction and coconut oil.
  • the various fat sources may be fully hardened by full hydrogenation, they may be fractionated, intra-esterified, and/or inter-esterified.
  • the structuring fat may comprise minor amounts of other components like for example monoglycerides that are naturally present in the fat.
  • the edible fat powder may comprise additional components like for example emulsifier or liquid oil.
  • additional components like for example emulsifier or liquid oil.
  • care must be taken to prevent the properties of the structuring fat to be detrimentally affected.
  • the presence of liquid oil may affect the ability structure the emsulsion, depending on the natural fats and the liquid oil as well as the amounts thereof. It is within the reach of the skilled person to determine without undue burden how much of the additional components may be present using common general knowledge.
  • the structuring fat comprises not more than 20 wt% of protein and/or carbohydrates, more preferably not more than 15 wt%, even more preferably not more than 10 wt%, and still more preferably not more than 5 wt%. Most preferably no protein and carbohydrates are present. Moreover, preferably the amount of water is not more than 20 wt%, preferably not more than 10 wt% and more preferably not more than 5 wt%. Most preferably no water is present in the structuring fat.
  • the structuring fat as present in the solid particles preferably has a solid fat content N10 from 50 to 100%, N20 from 26 to 95% and N35 from 5 to 60%.
  • the N- value expresses the solid fat content (SFC) at a certain temperature (in °C).
  • the structuring fat preferably has a solid fat content N10 selected from the list consisting of 45 to 100%, 55 to 90% and 65 to 85%;
  • N20 selected from the list consisting of 25 to 80%, 40 to 70% and 45 to 65%;
  • N35 selected from the list consisting of 0.5 to 60%, 0.5 to 20%, 0.5 to 14%, 15 to 50% and 30 to 45%.
  • Preferred solid fat content profiles of the structuring fat are:
  • N10 from 45 to 100%, N20 from 25 to 80% and N35 from 0.5 to 60%;
  • N10 from 55 to 90%, N20 from 40 to 70% and N35 from 0.5 to 20%;
  • N10 from 55 to 90%, N20 from 40 to 70% and N35 from 15 to 50%;
  • N10 from 65 to 85%, N20 from 45 to 65% and N35 from 0.5 to 14%;
  • N10 from 65 to 85%, N20 from 45 to 65% and N35 from 30 to 45%.
  • the melting temperature is at least 50°C, preferably at least 60°C, preferably at least 70°C, and preferably maximally 90°C. At these temperatures all crystals of the triacylglycerols have become liquid, there are no nuclei for solidification any more at these melting temperatures.
  • the temperature of the structuring fat when introduced into the mixer in step b) is maximally 70°C, preferably maximally 60°C.
  • the temperature at which the liquid structuring fat is introduced into the mixing device is a few degrees above the melting temperature, preferably 3 to 5°C above the melting temperature.
  • the temperature of the structuring fat is related to the temperature of the aqueous phase, when the temperature of the aqueous phase is lower, the temperature of the structuring fat can be higher.
  • the structuring fat may be cooled after step a) by mixing with the liquid oil, before being introduced into the mixing device.
  • the temperature of the liquid oil when introduced into the mixer in step b) is lower than 20°C, preferably lower than 15°C, preferably lower than 10°C.
  • the temperature of the liquid oil is between 12 and 18°C. The temperature is chosen such that the liquid oil does not start to crystallise before being introduced into the mixing apparatus.
  • the temperature of the aqueous phase when introduced into the mixer in step b) is lower than 20°C, preferably lower than 15°C, preferably lower than 10°C.
  • the temperature of structuring fat, of liquid oil, and of aqueous phase when introduced into the mixing apparatus is important, as together they determine the crystallisation rate of the structuring fat, when the warm structuring fat is brought into contact with the aqueous phase and the liquid oil in the mixing apparatus. If the temperature of one the phases is not correct, then the viscosity of the mixture inside the mixing apparatus may be too low or too high, because the amount of solid fat crystals may be too low or too high.
  • the temperature of the phases may also influence the stability of the emulsion that is produced in the method of the invention.
  • the wall of the mixing apparatus may be cooled by external means. This is only optional though, if the temperature of the phases is chosen correctly, and the weight ratio of the phases is chosen correctly, then external cooling means are not required. Increasing the cooling capacity may lead to the ability to produce low fat or very low fat water-in-oil emulsions.
  • the weight ratio between structuring fat and liquid oil ranges from 1 :100 to 50:100, preferably from 5:100 to 25:100.
  • the total fat phase of the emulsion preferably comprises from 1 % by weight to 50% by weight of structuring fat, and from 50% by weight to 99% by weight of liquid oil. More preferably the total fat phase of the emulsion preferably comprises from 5% by weight to 25% by weight of structuring fat, and consequently from 75% by weight to 95% by weight of liquid oil.
  • An emulsifier may be comprised in the liquid oil fraction, any numbers referring to the concentration of liquid oil includes a possible emulsifier.
  • the fat phase preferably contains an emulsifier having a HLB value of lower than 7.
  • the HLB value is the hydrophilic-lipophilic balance, and is a measure for the degree of hydrophilicity or lipophilicity.
  • An emulsifier with a HLB value lower than 10 generally is oil soluble, while an emulsifier with a HLB value higher than 10 generally is water-soluble.
  • an emulsifier having a HLB value of 7 or lower is mixed with the liquid oil prior to introducing the liquid oil into the mixer.
  • the concentration of the emulsifier is maximally 5% based on the weight of the mixture of liquid oil and emulsifier, preferably maximally 1 %, preferably maximally 0.1 %, preferably maximally 0.01 %.
  • a relatively high emulsifier content may lead to the ability to produce low fat or very low fat water-in-oil emulsions, although a relatively high emulsifier content is not necessary to produce low-fat water-in-oil emulsions.
  • the emulsifier comprises one ore more of emulsifiers chosen from the group consisting of saturated monoglycerides, unsaturated monoglycerides, and sugar-fatty acid esters (also known as the 'Spans', e.g. sorbitan monostearate).
  • the HLB value of the emulsifier is lower than 5, preferably lower than 3, preferably 1.
  • Another preferred emulsifier is lecithin from soyabean, or egg.
  • the amount of aqueous phase and fat phase in the emulsion that is produced in the method according to the invention may range widely.
  • the fat phase includes the structuring fat and the liquid oil, and preferably an emulsifier as defined before.
  • the concentration of the fat phase ranges from 5% to 95% based on the weight of the emulsion, preferably from 15% to 50%.
  • the emulsion may comprise a fat phase as a majority phase (for example, a margarine containing about 70 to 80% by weight of fat phase), preferably the emulsion comprises from 10% to 80%, preferably from 15% to 60% fat phase based on the weight of the emulsion.
  • the produced emulsion is a low fat emulsion with a fat content ranging from 15% to 50% by weight, preferably ranging from 18% to 45% by weight of fat phase, preferably ranging from 25% to 45% by weight of fat phase, preferably ranging from 30% to 45% by weight of fat phase.
  • An advantage of the method of the present invention is that low fat spreads (maximally 50% by weight of fat phase) can be produced in a single step.
  • the aqueous phase is dispersed in small droplets in the continuous fat phase during the mixing in the mixing apparatus.
  • the d3,3 value of the dispersed aqueous phase droplets is less than 10 micrometer, preferably less than 8 micrometer, preferably less than 6 micrometer.
  • the d3,3 value of the dispersed aqueous phase droplets is less than 3 micrometer, or even less than 2 micrometer.
  • the distribution of the aqueous phase droplets preferably is narrow, meaning that the exp(sigma) is maximally 2.5.
  • the three phases may be added as three separate streams to the mixing apparatus.
  • the molten structuring fat is brought into contact with liquid oil prior to introduction into the mixer.
  • the mixing of the two phases prior to introduction into the mixing apparatus can be done in line in a static mixing operation, or can be actively mixed in batch using any mixing device commonly known.
  • step b) of the method of the invention the fat-continuous emulsion is prepared by introducing the molten structuring fat from step a), a liquid oil and an aqueous phase into a distributive and dispersive mixing apparatus of the Controlled Deformation Dynamic Mixer type to create a water-in-oil emulsion,
  • the mixer is suitable for inducing extensional flow in a liquid composition
  • the mixer comprises closely spaced relatively moveable confronting surfaces at least one having a series of cavities therein in which the cavities on each surface are arranged such that, in use, the cross-sectional area for flow of the liquid successively increases and decreases by a factor of at least 5 through the apparatus.
  • Regions of distributive mixing (where the flow path is wide) comprises CTM-like cavities moving across each other in a direction perpendicular to the bulk flow of liquid. Between these regions of distributive mixing are regions in which the flow path is narrower and the flow is more extensional. It is possible for a mixer used in the method according to the invention to be provided with one on more regions in which the juxtaposition is such that the arrangement is CTM-like and one or more regions in which the arrangement is CDDM- like.
  • the CDDM apparatus can be described by the following.
  • the Controlled Deformation Dynamic Mixer comprises two confronting surfaces (1 , 2), spaced by a distance (7), wherein the first surface (1 ) contains at least three cavities (3), wherein at least one of the cavities has a depth (9) relative to the surface (1 ),
  • the second surface (2) contains at least three cavities (4) wherein at least one of the cavities has a depth (10) relative to the surface (2),
  • cross-sectional area for flow of the liquid available during passage through the apparatus successively increases and decreases at least 3 times
  • cavities are arranged such that the cross-sectional area for flow of the liquid available during passage through the apparatus successively increases in the cavities and decreases in the slits by a factor of at least 5 and
  • the distance (7) between the two surfaces (1 ,2) is between 2 micrometer and 300 micrometer, and wherein
  • either the ratio between the offset distance (8) and the distance (7) between the two surfaces (1 , 2) ranges from 0 to 250,
  • the ratio between the offset distance (81 ) and the distance (7) between the two surfaces (1 , 2) ranges from 0 to 60.
  • the confronting surfaces 1 , 2 are cylindrical.
  • the apparatus will generally comprise a cylindrical drum and co-axial sleeve.
  • the confronting surfaces 1 , 2 will be defined by the outer surface of the drum and the inner surface of the sleeve.
  • the confronting surfaces are circular or disk-shaped. Between these two extremes of configuration are those in which the confronting surfaces are conical or frusto-conical.
  • Non-cylindrical embodiments allow for further variation in the shear in different parts of the flow through the mixer.
  • the regions where the confronting surfaces 1 , 2 are most closely spaced are those where the shear rate within the mixer tends to be the highest.
  • the slit 7 between the surfaces between the confronting surfaces 1 , 2 forms this region, combined with offset distance 8 or offset distance 81 .
  • High shear contributes to power consumption and heating. This is especially true where the confronting surfaces of the mixer are spaced by a gap of less than around 50 micrometer.
  • confining the regions of high shear to relatively short regions means that the power consumption and the heating effect can be reduced, especially where in the CTM-like regions the confronting surfaces are spaced apart relatively widely.
  • the apparatus can be designed such that good mixing is obtained, while keeping the pressure drop over the apparatus as small as possible.
  • the design can be modified by adjusting the dimensions of the various parts of the apparatus, as explained in the following.
  • the distance 7 between the corresponding surfaces preferably is from 2 micrometers to 300 micrometers, which corresponds to the height of the slit.
  • the distance 7 is between 3 micrometer and 200 micrometer, preferably between 5 micrometer and 150 micrometer, preferably between 5 micrometer and 100 micrometer, preferably between 5 micrometer and 80 micrometer, preferably between 5 and 60 micrometer, preferably between 5 micrometer and 40 micrometer.
  • the distance 7 is between 8 micrometer and 40 micrometer, more preferably between 8 micrometer and 30 micrometer, more preferably between 10 micrometer and 30 micrometer, more preferably between 10 micrometer and 25 micrometer, more preferably between 15 micrometer and 25 micrometer.
  • the actual height of the slit 7 depends on the dimensions of the apparatus and the required flow rate, and the skilled person will know how to design the apparatus such that the shear rates within the apparatus remain relatively constant irrespective of the size of the apparatus.
  • the surfaces 1 and 2 that each contain at least three cavities 3, 4 create a volume between the surfaces for flow of the two fluids which are mixed.
  • the cavities in the surface effectively increase the surface area available for flow. Due to the presence of the cavities, the small area for flow between the surfaces 1 and 2 can be considered to be a slit having a height 7.
  • the spacing 5 between two cavities in surface 1 and spacing 6 between two cavities in surface 2 and the relative position of these corresponding parts (the offset) determine the maximum length or offset distance 8 of the slit (in the direction of bulk liquid flow).
  • the maximum length of the slit is equal to the smallest of the spacings 5, 6.
  • the two surfaces 1 , 2 with cavities 3, 4, that together form the volume for the mixing of the three phases (aqueous phase, liquid oil, and structuring fat), are positioned such that the corresponding spacings 5, 6 of the surfaces (that create the length of the slit) create an offset distance 8 of the slit (in the direction of the bulk flow) which is maximally 250 times as large as the distance 7 between the surfaces.
  • the two surfaces 1 , 2 can be positioned such that offset distance 8 can be adjusted.
  • the ratio between the offset distance 8 and the distance 7 between the two surfaces 1 , 2 ranges from 0 to 100, preferably 0 to 10, preferably 0 to 5. Most preferably the ratio between the offset distance 8 and the distance 7 ranges from 0 to 1 . As an example, when the ratio between offset distance 8 and distance 7 is 5, and the distance 7 between the two surfaces 1 , 2 is 15 micrometer, then the offset distance 8 of the slit is 75 micrometer.
  • the surfaces 1 , 2 are positioned such that no overlap is created, however in that case an offset distance 81 is created. In that case there is no overlap between the corresponding parts of the surfaces 1 , 2, and the slit is created with what could be called a 'negative overlap'.
  • the two surfaces 1 , 2 can be positioned such that offset distance 81 can be adjusted.
  • the ratio between the offset distance 81 and the distance 7 between the two surfaces 1 , 2 preferably ranges from 0 to 30. This 'negative overlap' accommodates the possibility of near zero distance 7 between the two corresponding surfaces 1 and 2.
  • the offset distance 81 is such, that the ratio between the offset distance 81 and the distance 7 between the two surfaces 1 , 2 ranges from 0 to 15, more preferred from 0 to 10, preferably from 0 to 5, preferably from 0 to 2 and more preferably from 0 to 1 .
  • the offset distance 81 is maximally 600 micrometer, more preferably maximally 300 micrometer. As an example, when the ratio between length 81 and distance 7 is 2, and the distance 7 between the two surfaces 1 , 2 is 15 micrometer, then length 81 (or what could be called negative overlap) is 30 micrometer.
  • a further benefit of this variation in the normal separation of the confronting surfaces in the direction of bulk flow, is that by having relatively small regions of high shear, especially with a low residence time is that the pressure drop along the mixer can be reduced without a compromise in mixing performance.
  • the mixing apparatus is operated at a pressure less than 200 bar, preferably less than 80 bar, preferably less than 60 bar, preferably less than 40 bar, most preferred less than 30 bar. With these relatively low pressures a good mixing process is obtained.
  • the fluids preferably flow from left to right through the apparatus.
  • the slits create an acceleration of the flow, while at the exit of the slit the fluids decelerate due to the increase of the surface area for flow and the expansion which occurs.
  • the acceleration and deceleration leads to the break up of the large droplets of the dispersed phase, to create finely dispersed droplets in a continuous phase. Droplets that are already small, remain relatively untouched. The flow in the cavities is such that the droplets of the dispersed phase eventually become evenly distributed in the continuous phase.
  • the cross-sectional area for flow of the liquid available during passage through the apparatus successively increases and decreases at least 5 times, and these passages lead to effective mixing of the two fluids.
  • the cross-sectional area for flow of liquid in the cavities is at least 5 times larger than the cross-sectional area for flow of liquid in the slits.
  • This relates to the ratio between distance 1 1 and distance 7.
  • the cross-sectional area for flow is designed such that the cross-sectional area for flow of the liquid available during passage through the apparatus successively increases and decreases by a factor of at least 7, preferably at least 10, preferably at least 25, preferably at least 50, up to preferred values of 100 to 400.
  • the cross- sectional surface area for flow of the fluids is determined by the depth 9 of the cavities
  • the total cross-sectional area is determined by the distance 1 1 between the bottoms of two corresponding cavities in the opposite surfaces.
  • the surfaces 1 , 2 each contain at least three cavities 3, 4. In that case the flow expands at least 3 times during passage, and the flow passes through at least 3 slits during the passage.
  • the cross-sectional area for flow of the liquid available during passage through the apparatus successively increases and decreases between
  • the shape of the cavities 3 may take any suitable form, for example the cross-section may not be rectangular, but may take the shape of for example a trapezoid, or a parallelogram, or a rectangle where the corners are rounded. Seen from above, the cavities may be rectangular, square, or circular, or any other suitable shape. Any arrangement of the cavities and the number of cavities and size of the cavities may be within the scope of the present invention.
  • the mixing apparatus preferably is operated dynamically, meaning that one of the surfaces rotates relative to the other.
  • one of the surfaces is able to rotate relative to the other surface at a frequency between 1 ,000 and 25,000 rotations per minute, preferably between 3,000 and 12,000 rotations per minute.
  • rotation may lead to improved mixing process and creation of smaller dispersed phase droplets.
  • the emulsion contains less fat (amount of fat phase is lower)
  • the required rotation speed may be higher in order to create a finely dispersed aqueous phase in the continuous fat phase.
  • Additional features of the known CTM and CDDM may be incorporated in the mixer described herein.
  • one or both of the confronting surfaces may be provided with means to heat or cool it. Where cavities are provided in the confronting surfaces these may have a different geometry in different parts of the mixer to as to further vary the shear conditions.
  • the dimensions of such a CDDM apparatus used in the invention are such that the distance between the two surfaces 7 is between 10 and 20 micrometer; and/or wherein the length of the slit 8 is maximally 2 millimeter, for example 80 micrometer, or 20 micrometer, or even 0 micrometer.
  • the length of the slit 8 plus the length of the cavity 17, 18 combined is maximally 10 millimeter; and/or wherein the depth of the cavities 9, 10 is maximally 2 millimeter.
  • the internal diameter of the outer surface is between 20 and 30 millimeter, preferably about 25 millimeter.
  • the total length of the apparatus in that case is between 7 and 13 centimeter, preferably about 10 centimeter. The length means that this is the zone where the fluids are mixed.
  • the rotational speed of such a preferred apparatus is preferably 0 (static), or more preferred alternatively between 5,000 and 25,000 rotations per minute.
  • the shape of the area for liquid flow may take different forms, and naturally depends on the shape of the confronting surfaces. If the surfaces are flat, then the cross- sectional area for flow may be rectangular.
  • the two confronting surfaces may also be in a circular shape, for example a cylindrical rotor which is positioned in the centre of a cylindrical pipe, wherein the outside of the cylindrical rotor forms a surface, and the inner surface of the cylindrical pipe forms the other surface.
  • the circular annulus between the two confronting surface is available for liquid flow.
  • slit height (distance 7) is 35-40 micrometer
  • offset distance 8 is 20 micrometer
  • - total length of the apparatus is 10 centimeter (length means the zone where the fluids are mixed);
  • depth 9, 10 of cavities 3, 4 is maximally 2 millimeter
  • stator internal diameter of the stator is 25 millimeter
  • rotational speed of the apparatus is up to 25,000 rotations per minute
  • Droplet size and droplet size distribution are determined using standardised NMR equipment.
  • a Bruker magnet with a field of 0.47 Tesla (20 MHz proton frequency) with an air gap of 25 mm is used (NMR Spectrometer Bruker Minispec MQ20 Grad, ex Bruker Optik GmbH, Germany)
  • the NMR signal (echo height) of the protons of the water in a water -in-oil emulsion are measured using a sequence of 4 radio frequency pulses in the presence (echo height E) and absence (echo height E * ) of two magnetic field gradient pulses as a function of the gradient power.
  • the oil protons are suppressed in the first part of the sequence by a relaxation filter.
  • the droplet size of the spread is measured, according to the above described procedure, of a spread stabilized at 5°C right after production for one week. This gives the d3,3 after stabilization at 5°C.
  • Stevens values give an indication about the hardness (also called firmness) of a product.
  • the Stevens value is determined according to the following protocol. Freshly prepared products are stabilized at 5 degrees Celsius. The hardness of the product is measured with a Stevens penetrometer (Brookfield LFRA Texture Analyser (LFRA 1500), ex Brookfield Engineering Labs, UK) equipped with a stainless steel probe with a diameter of 6.35 mm and operated in "normal" mode. The probe is pushed into the product at a speed of 2 mm/s, a trigger force of 5 gram from a distance of 10 mm. The force required is read from the digital display and is expressed in grams.
  • LFRA 1500 Brookfield Engineering Labs, UK
  • Spreadibility is determined according to the following protocol.
  • a flexible palette knife is used to spread a small amount of the spread onto fat free paper.
  • the spreading screen is evaluated according to standardized scaling.
  • a score of 1 represents a
  • a 2 refers to the same product but then with small remarks as slightly inhomogeneous or some vacuoles
  • a 3 refers to the level where defects become almost unacceptable, like loose moisture or coarseness during spreading.
  • a score of 4 or 5 refers to unacceptable products, where the 4 refers to a product still having some spreading properties, but an unacceptable level of defects.
  • the solid fat content (SFC) in this description and claims is expressed as N-value, as defined in Fette, Seifen Anstrichstoff 80 180-186 (1978).
  • the stabilization profile applied is heating to a temperature of 80 degrees Celsius, keeping the oil for at least 10 minutes at 60 degrees Celsius or higher, keeping the oil for 1 hour at 0 degrees Celsius and then 30 minutes at the measuring temperature.
  • the stability of the emulsion after spreading is determined by using indicator paper (Wator, ref 906 10, ex Machery-Nagel, DE) which develops dark spots where free water is adsorbed. A stable product does not release any water and the paper does not change. Very unstable products release free water easily and this is indicated by dark spots on the paper.
  • indicator paper Wator, ref 906 10, ex Machery-Nagel, DE
  • a six point scale is used to quantify the quality of fat spread (DIN 10 31 1 ):
  • 0 (zero) is a very stable and good product; 1 (one) is showing some loose moisture (one or two spots, or the paper changes a little in color as a total);
  • Emulsifier Dimodan RT (monoglyceride, ex Danisco A S (Copenhagen,
  • Demineralised water was obtained from a Millipore filter system
  • inES48 is an interesterified mixture of 65% dry
  • inES48 contains about 86.2% saturated fatty acids, about 1 1 .5% mono- unsaturated fatty acids, and about 2.3% poly-unsatu rated fatty acids, and is free from trans fatty acids. Obtained from Unimills (Zwijndrecht, Netherlands);
  • Beta-carotene (30% in sunflower oil), ex BASF (Ludwigshafen, Germany);
  • Citric acid (20% solution in water); ex Jungbunzlauer AG (Basel, Switzerland);
  • Structuring fat inES48 is made liquid by bringing it to a temperature of 90°C.
  • the temperature of the structuring fat is reduced to 55°C.
  • Emulsifier Dimodan RT is mixed with sunflower oil, at a concentration varying from aboutO.3% to 1 .2% by weight, based on the weight of sunflower oil and emulsifier. This mixture is kept at a temperature of 8°C.
  • the structuring fat (at a temperature of 55°C) is mixed with the sunflower oil- emulsifier mixture (at a temperature of 8°C) at a weight ratio of 16 to 84, resulting in a temperature of the fat phase of 15°C. This is the fat phase of the emulsion.
  • the aqueous phase is prepared by mixing water and salt, and adjusting the pH to 5.2 using citric acid, and kept at a temperature of 10°C.
  • the fat phase and aqueous phase both are fed into the CDDM apparatus using two separate inlets, opposite each other with the stator as the reference (both at the same distance from the outlet of the CDDM apparatus).
  • the rotor rotated at rate of 5,000 rpm.
  • the pressure was 30 bar, this pressure is the line pressure between the intensifier pump supplying the raw materials and the mixer itself.
  • the resulting product is a water-in-oil emulsion that can be used as a spread.
  • the following spreads were produced, and they had the following production parameters and product properties (shortly after production and after 18 weeks storage at 5°C): Table 2 Production parameters and emulsion properties of emulsions that have been produced (short after production and after 18 weeks storage).

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Edible Oils And Fats (AREA)

Abstract

La présente invention porte sur un procédé pour la production d'émulsions d'eau dans l'huile (en particulier d'émulsions d'eau dans l'huile à faible teneur en matière grasse (< 50 % d'huile)), sans nécessiter la formation d'un prémélange de l'émulsion et sans nécessiter de chauffer un prémélange total, l'émulsion pouvant être formée dans une seule étape de traitement. La présente invention a en particulier pour objet de produire des émulsions d'eau dans l'huile à faible teneur en matière grasse (< 50 % d'huile) dans un procédé à une seule étape. Dans ce procédé, un appareil de mélange distributif et dispersif du type mélangeur dynamique à déformation contrôlée est utilisé pour créer une émulsion d'eau dans l'huile, le mélangeur étant approprié pour provoquer un flux en extension dans une composition liquide et le mélangeur comprenant des surfaces se faisant face déplaçables les unes par rapport aux autres à une petite distance les unes des autres, au moins l'une de celles-ci renfermant une série de cavités, les cavités sur chaque surface étant disposées de façon à ce que, lors de l'utilisation, la surface en coupe transversale pour l'écoulement du liquide augmente et diminue successivement d'un facteur d'au moins 5 dans l'appareil.
PCT/EP2012/069036 2011-10-17 2012-09-27 Procédé pour la production d'émulsion d'eau dans l'huile alimentaire WO2013056964A1 (fr)

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Publication number Priority date Publication date Assignee Title
AU2015263494B2 (en) * 2014-05-20 2017-05-04 Upfield Europe B.V. Process for the manufacture of edible water-in-oil emulsion
US20180325137A1 (en) * 2015-11-20 2018-11-15 Unilever Bcs Us Inc. Process for preparing fat continuous emulsions low in fat
EP3376874B1 (fr) 2015-11-20 2021-06-16 Upfield Europe B.V. Procédé de préparation des émulsions avec une phase grasse continue
US11647763B2 (en) * 2013-01-31 2023-05-16 Upfield Europe B.V. Process for the manufacture of edible water-in-oil emulsions

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11647763B2 (en) * 2013-01-31 2023-05-16 Upfield Europe B.V. Process for the manufacture of edible water-in-oil emulsions
AU2015263494B2 (en) * 2014-05-20 2017-05-04 Upfield Europe B.V. Process for the manufacture of edible water-in-oil emulsion
EP3157348B1 (fr) * 2014-05-20 2019-06-12 Unilever NV Procédé de fabrication d'une émulsion eau dans l'huile comestible
EP3552494A1 (fr) * 2014-05-20 2019-10-16 Upfield Europe B.V. Procédé de fabrication d'une émulsion eau dans huile comestible
US20180325137A1 (en) * 2015-11-20 2018-11-15 Unilever Bcs Us Inc. Process for preparing fat continuous emulsions low in fat
EP3376874B1 (fr) 2015-11-20 2021-06-16 Upfield Europe B.V. Procédé de préparation des émulsions avec une phase grasse continue
US11154070B2 (en) * 2015-11-20 2021-10-26 Upfield Europe B.V. Process for preparing fat continuous emulsions low in fat

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