method for producing a continuous emulsion in water

专利摘要:
METHOD FOR PRODUCTION OF A CONTINUOUS EMULSION IN WATER The present invention aims to provide a new emulsification method, which can produce continuous concentrated emulsion in water containing lipophilic compounds in a dispersed phase, with a very thin dispersed phase droplet with a smaller size than a micron, and a narrow size distribution of the dispersed phase. This objective was achieved by a method in which the continuous emulsion in water is produced using a Dynamic Controlled Deformation Mixer or a Cavity Transfer Mixer.
公开号:BR112013016302B1
申请号:R112013016302-0
申请日:2011-12-07
公开日:2020-10-27
发明作者:Petrus Martinus Maria Bongers；Henelyta Santos Ribeiro；Graeme Neil Irving；Michael John Egan
申请人:Unilever N.V.；
IPC主号:

专利说明:

Technical Field
The present invention relates to a method for producing emulsions using a Controlled Deformation Dynamic Mixer or Cavity Transfer Mixer. History of the Invention
Mixture can be described as either distributive or dispersive. In a multiphase material comprising discrete domains of each phase, the distributive mixture seeks to change the relative spatial positions of the domains of each phase, while the dispersive mixture seeks to overcome cohesive forces to change 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 change. For example, a machine for mixing peanuts and raisins will be completely distributive so as not to damage the things being mixed, while a mixer / homogenizer will be dispersive.
Many different types of rotor / stator mixers are known. The stirring reactors, such as those described in US2003 / 0139543, comprise a vessel with internally mounted mixing elements and are, in general, of distributive function. Other types of rotor-stator mixer, such as that described in US2007 / 105323, are designed with the intention of forming fine emulsions and are dispersive in character.
EP 194 812 A2 describes a cavity transfer mixer (CTM). Also, WO 96/20270 describes a 'Cavity Transfer Mixer', comprising facing surfaces, each having a series of cavities formed in them, whose surfaces move relatively to each other, in which a liquid material is passed between the surfaces along a path that successively passes through the cavities on each surface. The cavities are arranged on the relevant surfaces so that shear is applied to the liquid as it flows between the surfaces. In a typical embodiment, the mixer comprises an outer casing and an airtight inner drum. The facing surfaces of the casing and the drum are both provided with cavities so that the cavities overlap forming winding and changing flow paths that vary as the drum and the casing rotate relatively with each other. This type of mixer has the stator and rotor elements with opposite cavities that, as the mixer operates, move past each other through the direction of the volumetric flow through the mixer. In such mixers, mainly distributive mixing is obtained. Shear is applied by the relative movement of the surfaces in a direction usually perpendicular to the material flow. In the typical embodiment described above, this is accomplished by the relative rotation of the drum and wrap. In such a device, there is relatively little variation in the cross-sectional area for the flow as the material passes axially downwards in the device. In general, the cross-sectional area for flow varies by a factor of less than 3 across the apparatus.
WO 96/20270 also describes a new mixer, referred to herein as a 'Dynamic Controlled Deformation Mixer' (CDDM). It has characteristics in common with the CTM, that is, it is a type of mixer that has stator and rotor elements with opposite cavities that, as the mixer operates, move past each other through the direction of the volumetric flow along the mixer. It is distinguished from CTM by the fact that the material is also subjected to deformation in the direction of extension. The flow towards the extension and the efficient dispersive mixing are ensured by the existence of surfaces facing cavities arranged in such a way that the cross-sectional area, for the volumetric flow of the liquid through the mixer, successively increases and decreases by a hair factor minus 5 across the device. In comparison to the CTM embodiment described above, the CDDM cavities are generally aligned or slightly displaced in an axial direction so that material flowing axially along the facing surfaces is forced through the narrow gaps, as well as flowing along and between the cavities. CDDM combines CTM's distributive mixing performance with dispersive mixing performance. Thus, CDDM is more suitable for problems, such as reducing the droplet size of an emulsion, where dispersive mixing is essential.
US 6,468,578 B1 describes the use of a cavity transfer mixer to create an emulsion of water droplets in a continuous fat phase.
WO 2010/089320 A1, WO 2010/089322 A1 and WO 2010/091983 A1 describe specific types of a distributive and dispersive mixing apparatus of the type CDDM or type CTM, comprising two facing surfaces having cavities in them. These specific types can be used for the treatment of emulsions.
WO 2010/105922 A1 describes continuous emulsions in water of 5% silicone wax that can be produced in an aqueous solution containing PET-POET polymer as an emulsifier, using a microfluidizer. This microfluidizer operates at high pressures of 120,000 kPa to homogenize emulsions.
WO 96/28045 describes a mixer with distributive and dispersive mixing zones for producing chewing gum.
US 2010/220545 A1 describes a mixer with distributive and dispersive action that can be used for emulsification.
WO 2008/125380 A1 describes continuous edible fat creams comprising phytosterols which are present in the form of elongated crystals, in which the longest dimension is more preferably 2000 microns.
WO 93/05768 and WO 00/67728 describe lipid particles having a diameter between 10 nanometers and 10 micrometers. They are produced by melting a lipid phase into an aqueous phase and subsequent homogenization using a high pressure homogenizer. Brief Description of the Invention
These exposures do not describe the production of concentrated oil-in-water emulsions, having a relatively high amount of dispersed phase. This should be of particular interest for the use of these emulsions as ingredients in consumer products, such as food products (for example, margarines and other spreading creams), personal care products (for example, skin creams), or care products household products (for example, liquid laundry detergents), cosmetic products (for example, makeup like lipstick, eye and lip products), and pharmaceuticals (for example, encapsulation of poorly soluble lipophilic drugs for targeted in vivo release). It should be especially interesting to provide emulsions containing a finely dispersed oil phase that additionally contains phytosterols dispersed in the oil phase. Phytosterols have a very low solubility in both vegetable oils and water, especially at room temperature. These emulsions can be used as a food ingredient to lower LDL cholesterol levels in humans. In order to be effective as an LDL cholesterol lowering agent, the dispersed phase containing phytosterols must be finely dispersed, and in addition the phytosterol is preferably non-crystallized. If phytosterols crystallize, in vivo (in the stomach) bio-accessibility is lower compared to amorphous phytosterols, due to the size and large crystal shape of these crystals.
Similarly, there is a desire for carotenoids that are also very poorly soluble at room temperature, both in vegetable oil and in water. Carotenoids can act as antioxidants in vivo; in addition, beta-carotene is a precursor to vitamin A.
Therefore, one of the objectives of the present invention is to provide a method for the production of oil-in-water emulsions, with a very thin dispersed lipid phase, and to provide emulsions that contain a relatively high concentration of lipophilic compounds, which are poorly soluble at temperature environment in oil and water. These emulsions can be used in food products, home care products, or personal care products, or cosmetic products, or pharmaceutical products.
In addition, it is an object of the present invention to provide a method for preparing the described emulsions with a low energy input and a high yield.
We have now determined that one or more of these objectives can be achieved by a method in which the lipophilic compound is brought to a liquid form and emulsified using a CDDM or CTM mixer to have an average Sauter diameter of at most 1 micrometer. This results in a finely dispersed phase of lipophilic materials, with a high concentration of the lipophilic compound, which can be used in food, home care, personal care, cosmetics or pharmaceutical products.
Furthermore, by using a mixer of the CDDM or CTM type, the required pressure is relatively low and, at the same time, the finely dispersed emulsions that can be produced are stable. In comparison with existing high pressure homogenizers, the concentration of the dispersed phase that can be achieved is high, and the required pressure is up to 20 times lower.
This requires less heavy material specifications for the design of an apparatus (to withstand high pressures), and less energy consumption to apply pressure to the apparatus, and consequently an environmentally friendly process and less carbon dioxide emission.
Consequently, the present invention provides a method for producing a continuous emulsion in water, the dispersed phase of the emulsion comprising a lipophilic compound, and wherein the average Sauter diameter of the dispersed phase is at least 20% of the weight of the emulsion , and the method comprising the steps of: (a) mixing water and an oil-in-water emulsifier to form an aqueous phase; and (b) bringing the lipophilic compound into a liquid form to form the lipophilic phase; and (c) mixing the aqueous phase of step (a) and the lipophilic phase of step (b) in a distributive and dispersive mixing apparatus of the Controlled Deformation Dynamic Mixer or Cavity Transfer Mixer type to create a continuous emulsion in water, and the mixer being suitable to induce flow towards the extension in a liquid composition and the mixer comprising relatively mobile facing surfaces closely spaced, at least one having a series of cavities in it, with the cavities in each surfaces are arranged in such a way that, in use, the cross-sectional area for the flow of the liquid successively increases and decreases by a factor of at least 3 throughout the apparatus.
Brief Description of the Figures - Figure 1: Schematic representation of a Cavity Transfer Mixer (CTM); 1: stator, 2: annular space, 3: rotor; with the cross-sectional views below. - Figure 2: Schematic representation of a Dynamic Controlled Deformation Mixer (CDDM); 1: stator, 2: annular space, 3i rotor; with the cross-sectional views below. - Figure 3: Particle size distribution of 7% phytosterol droplets dispersed in MCT oil, from example 1; at a flow rate of 20 mL / s in CDDM, at various speeds of rotation (0 = 0 rpm, 5 = 5,000 rpm, 12 = 12,000 rpm, 15 = 15,000 rpm). - Figure 4: Scanning electron microscopy images of two colloidal dispersions loaded with 7% phytosterol (containing 70% dispersed phase); from example 1. Image A on the left; flow rate of 22.9 mL / s, speed of 8,250 rpm; image width of about 12 micrometers, bar width of 1 micrometer. Image B on the right: flow rate of 67.6 mL / s, speed of 0 rpm (static); image width about 12 micrometers, bar width 1 micrometer. - Figure 5: Scanning electron microscopy images of colloidal dispersions loaded with phytosterol from example 1; CDDM at a flow rate of 22.9 mL / s, speed of 8,250 rpm. Image A on the left: phase dispersed at 70%, phytosterol at 7% by weight based on the dispersion; image width about 12 micrometers, bar width 1 micrometer. Image B on the right: dispersion of image A diluted to 10% of dispersed phase; phytosterol at 1% by weight based on the dispersion; image width about 60 micrometers, bar width 10 micrometers. - Figure 6: Scanning electron microscopy images of colloidal dispersions loaded with phytosterol (containing 70% dispersed phase) from example 1; CDDM at a flow rate of 22.9 mL / s, speed 0 rpm (static). Image A on the left: phase dispersed at 70%, phytosterol at 7% by weight based on the dispersion; image width about 60 micrometers, bar width 10 micrometers. Image B on the right: dispersion of image A diluted to 10% of dispersed phase; phytosterol at 1% by weight based on the dispersion; image width about 60 micrometers, bar width 10 micrometers. - Figure 7: Droplet size distribution of colloidal dispersions loaded with 7% by weight phytosterol, stabilized with Tween 20 at two different concentrations, produced at a CDDM flow rate of 20 mL / s; static and dynamic processes in example 1; (0 = 0 rpm, 5 = 5,000 rpm, 8 = 8,000 rpm, 12 = 12,000 rpm, 15 = 15,000 rpm); image on the left Tween 20 at 7% by weight, and image on the right Tween 20 at 9% by weight. - Figure 8: Scanning electron microscopy image of colloidal dispersion loaded with 13% phytosterol (containing 65% dispersed phase); produced in CDDM at a flow rate of 80 mL / s and 12,000 rpm of example 1; image width about 6 micrometers (bar width 1 micrometer). - Figure 9: Light microscopy images of dispersions containing: MCT oil at 7% by weight and phytosterol (left) at 3% by weight; or MCT oil at 6% by weight and phytosterol (right) at 4% by weight, bar width 10 micrometers, from example 2. - Figure 10: Schematic representation of a preferred embodiment of the CDDM device, cross-sectional view (direction volumetric flow, preferably from left to right). - Figure 11: Schematic representation of a preferred embodiment of the CTM device, seen in cross section (direction of the volumetric flow preferably from left to right). Detailed Description of the Invention
Unless defined differently, all technical and scientific terms used herein have the same meaning as commonly understood by a person skilled in the art.
All percentages, unless otherwise stated, refer to the percentage by weight. The abbreviation '% by weight' or '% (w / w)' refers to the percentage by weight.
In the context of the present invention, the average particle diameter is generally expressed as the value of, 2, which is Sauter's average diameter, unless otherwise stated. Sauter's average diameter is the diameter of a sphere that has the same volume / surface area ratio as a particle of interest. The value of da.2 is also used here, which is the average diameter of heavy volume. The volume based on particle size is equal to the diameter of the sphere that has the same volume as the given particle.
Polydispersity, that is, the particle size distribution width, is determined by the Amplitude (Span)
Amplitude = [article diameter in cumulative size of 90%] - [article diameter in cumulative size of 10%] / [article diameter in cumulative size of 50%].
Amplitude is a dimensionless number that illustrates whether the spread of the distribution is narrow or wide. A smaller amplitude indicates a narrow size distribution.
In the case where a strip is given, the strip given includes the mentioned ends.
An edible or food product, in the context of the present invention, encompasses, but is not limited to, food products including spreading creams, salad dressings, dairy products, beverages, dietary foods, food supplements, pharmaceutical compositions and the like. Products may contain ingredients common in the art and may be produced by methods common in the art.
In the context of the present invention, a home care product is a product that is normally used in cleaning items such as hard surfaces in the home, or cleaning items such as dishes and kitchen utensils, or can be laundry detergents in the home. liquid or solid form (powders, tablets) or can be conditioners for washing clothes. Examples of such products are liquid or gel cleaning products for the kitchen, bathroom, or toilet and dishwashing liquid. Home care products may contain microcapsules containing perfumes and / or fragrances, or cleaning aids. In the case of laundry detergents or washing conditioners, the microcapsules may contain a perfume or fragrance, and the microcapsules may be deposited on the clothes during the washing process. Subsequently, microcapsules can release perfume and / or fragrance during clothing use, or they can be released, for example, when ironing clothes.
In the context of the present invention, a personal care product is a product that is used by a consumer to clean, sanitize and / or beautify. Cosmetic products, in the context of the present invention, include, but are not limited to, skin creams, body lotions, shampoos, hair conditioners, toothpaste, deodorants, hair styling products, personal soap bars and personal liquid soaps. In the case of these products, the microcapsules may contain perfumes and / or fragrances, or they may, for example, contain one or more compounds that are beneficial to the health and / or beauty of the skin. Cavity Transfer Mixers (CTMs)
Similar to that described in WO 96/20270, MSCs are defined as mixers comprising facing surfaces, at least one of the surfaces, preferably both surfaces, having a series of cavities formed in it, in which the surfaces move relatively to each other and in the which a liquid material is passed between the surfaces and flows along a route successively through the cavities' on each surface. The cavities are arranged on the relevant surfaces so that shear is applied to the liquid as it flows between the surfaces. The cavities are arranged on the respective surfaces so that there is a relatively small variation in the effective cross-sectional flow area as the material passes through the mixer. In such mixers, mainly distributive mixing is obtained. In general, the cross-sectional area for flow varies by a factor of less than 3 across the apparatus. Shearing is applied by the relative movement of the surfaces in a direction generally perpendicular to the flow of the material that lies between them.
Here, we exemplify CTMs by reference to Figure 1 which shows an axial section and four radial cross sections along a CTM configured as a 'concentric cylinder' device and comprises an internal rotor that transits inside an external stator. Briefly, the axial section shows the relative axial positions of the rotor and stator cavities, which are invariant over time, while the cross sections (AA, BB, CC, DD) demonstrate the axial variation in the available cross-sectional area for the material flows axially: ■ AA through the stator cavities in positions where the stator cavities are confronted by 'rotor rings', that is, rings that extend circularly and separate successive rings from the rotor cavities; ■ B-B between the stator cavities and the rotor cavities in positions where the former are confronted by the latter; ■ C-C along the rotor cavities in positions where the rotor cavities are confronted by ‘stator rings’, that is, the rings that extend circularly and separate successive rings from the stator cavities; ■ D-D between the rotor cavities and the stator cavities in positions where the former are confronted by the latter.
The key feature to note is that there is little variation in the cross-sectional area for the flow as the material passes axially in the downward direction along the device. Controlled Strain Dynamic Mixers (CD D Ms)
Similar to that described in WO 96/20270, CDDMs are distinguished from CTMs by their description as mixers: comprising facing surfaces, at least one of the surfaces, preferably both surfaces, having a series of cavities formed on them and whose surfaces move relatively between themselves and in which the liquid material is passed between the surfaces and flows along a route successively through the cavities on each surface, and the material is subjected to deformation in the direction of extension and / or shear deformation and preferably both deformations , in the direction of the extension and by shear. The cavities are arranged on the relevant surfaces so that the shear is applied by the relative movement of the surfaces in a direction generally perpendicular to the flow of the material that passes between said surfaces. In addition to the shear, the following can be ensured: significant flow in the direction of extension and an effective distributive and dispersive mixture by providing a device that has facing surfaces and cavities in them, with cavities arranged in such a way that the cross-sectional area for the flow of the liquid successively increases and decreases by a factor of at least 5 over the device.
Here, we exemplify the CDDMs with reference to Figure 2 which shows an axial section and four radial cross sections along the CDDM configured as a 'concentric cylinder' device comprising an internal rotor that transits inside an external stator. Briefly, the axial section shows the relative axial positions of the rotor and stator cavities, which are invariant over time, while the cross sections (AA, BB, CC, DD) demonstrate the axial variation in the cross section area available for the material flows axially: ■ AA through the stator cavities in positions where those stator cavities are confronted by the 'rotor rings', that is, the rings that extend circularly and which separate the successive rings from the rotor cavities; ■ B-B between the stator cavities and the rotor cavities through the annular space formed in those positions in which the 'rotor rings' are confronted by the 'stator rings'; ■ C-C through the rotor cavities in positions in which those rotor cavities are confronted by 'stator rings', that is, rings that extend circularly and that separate successive rings from the stator cavities; ■ D-D between the rotor cavities and the stator cavities in positions where the former are confronted by the latter.
Clearly, there is a significant variation in the cross-sectional area for the flow as the material passes axially through the annular space formed between the 'rotor rings' and the 'stator rings' (BB), and between the confronting cavities of the rotor and stator cavities (DD).
For the purpose of comparing Figure 1 and Figure 2, it will be understood that CDDMs are distinguished from CTMs by the relative position of the rotor and stator and the consequent incorporation of a flow component in the direction of the extension. Thus, CDDMs combine the performance of the CTMs distributive mix with the performance of the dispersive mix of the multiple expansion-contraction static mixers. Emulsion production method
The present invention provides a method for producing a continuous emulsion in water, the dispersed phase of the emulsion comprising a lipophilic compound, and the average Sauter diameter of the dispersed phase is less than 1 micrometer, and the concentration being the dispersed phase is at least 20% by weight of the emulsion, and the method comprises the steps of: (a) mixing water and an oil-in-water emulsifier to form an aqueous phase; and (b) bringing the lipophilic compound into a liquid form to form a lipophilic phase; and (c) mixing the aqueous phase of step (a) and the lipophilic phase of step (b) in a distributive and dispersive mixing apparatus of the Controlled Deformation Dynamic Mixer or Cavity Transfer Mixer type to create a continuous emulsion in water, and where the mixer is suitable for inducing flow towards the extension in a liquid composition, and where the mixer comprises relatively mobile facing surfaces closely spaced, at least one having a series of cavities in it, whose cavities on each surface they are arranged in such a way that, in use, the cross-sectional area for the liquid flow successively increases and decreases by a factor of at least 3 throughout the apparatus.
In step (a), preferably the temperature of the mixture is at most 110 ° C. An increase in temperature can be used to improve the dispersion of the emulsifier. In addition, at the increased temperature, the subsequent emulsion can be carried out more efficiently than at lower temperatures, when all the compounds to be mixed are in the liquid state. Preferably, this step (a) is carried out at atmospheric pressure. Preferably, the temperature is at most 100 ° C, more preferably at most 95 ° C.
The emulsifier can be any compound that can be used to emulsify oils in water. Preferably, the HLB value of the emulsifier is greater than 7, preferably from 8 to 18. The value of HLB (hydrophilic-lipophilic balance) of an emulsifier is a measure of the degree to which it is hydrophilic or lipophilic, and determines the emulsifying capacity. oil in water emulsifier, or water in oil. Examples of such emulsifiers are: polyoxyethylene (20) sorbitan monolaurate, commercially known as Tween® 20, and the PET-POET polymer (polyethylene terephthalate-co-polyoxyethylene terephthalate, as described in WO 2010/105922 A1). 'PET' is lipophilic, 'POET' is hydrophilic. The chemical structure of PET-POET is:

Other preferred emulsifiers include sugar esters with HLB values greater than 7, or any hydrophilic emulsifier that is not sensitive to temperature.
Preferably, the lipophilic compound of step (b) are lipophilic materials that are often of natural origin, but they can also be synthetic.
In step (b), the lipophilic compound is brought into liquid form, in order to be able to finely disperse the lipophilic phase in the subsequent step (c). When in liquid form, the lipophilic phase that is formed in step (b) will break into droplets in the mixing step (step (c)) and will be dispersed in the aqueous phase of step (a). Preferably, in step (b) the lipophilic compound is brought into liquid form by increasing the temperature to melt the compound. The required temperature will depend on the specific lipophilic compound, preferably the temperature in step (b) is a maximum of 160 ° C, preferably a maximum of 150 ° C, preferably a maximum of 110 ° C, preferably a maximum of 95 ° C.
Preferably, the lipophilic compound comprises lecithin, fatty acid, monoglyceride, diglyceride, triglyceride, phytosterol, phytosteranol, fatty acid ester, phytosanil fatty acid ester, wax, fatty alcohol, carotenoid, oil-soluble dye, vitamin-soluble dye oil, oil-soluble flavoring, oil-soluble fragrance, oil-soluble drugs, mineral oils or derivatives, petroleum jelly or derivatives, or silicon or derivative oils, or combinations of these compounds. Combinations of these compounds are also within the scope of the present invention.
Oils and fats such as dairy fats, vegetable oils or algae oils are a common source of monoglycerides, diglycerides and triglycerides. Examples of fat-soluble vitamins are vitamin A, vitamin D2, vitamin D3, vitamin E and vitamin K. These vitamins include all compounds that function as the respective vitamin. Carotenoids include alpha-carotene, beta-carotene, lycopene, canthaxanthin, astaxanthin, lutein and zeaxanthin, as well as their esterified forms. These compounds can be used as ingredients in food products.
Also materials such as mineral oils, petroleum jelly, silicon oils, and derivatives of these compounds are preferred compounds that can be used in this invention as a lipophilic compound. These compounds can be used as ingredients in personal care products, such as skin creams and body lotions, or home care products, such as laundry detergent compositions, especially liquid laundry compositions.
Lecithin: is a general term for a mixture that can be originated from plant (for example, soybeans) or animal origin (for example, egg yolk) and is used as an emulsifier. The most important compounds in lecithin are phosphatidylcholine, phosphatidylethanolamine and phosphatidylinusitol. In commercially available lecithins, also free of fatty acids, triglycerides and mono- and diglycerides may be present. The nature of the phosphoric group and said fatty acids determine the emulsifying properties of lecithin.
Fatty acid: the appropriate fatty acids in the present invention are C3 fatty acids and longer chains, preferably at least C12, even preferably C26. The aliphatic tail can be saturated or unsaturated. The chain can be unbranched or branched as a hydroxy, methyl or ethyl group. The appropriate fatty acid in the present invention consists of a minimum of 3 carbon atoms and a maximum of 26.
Monoglyceride: an ester of glycerol and a fatty acid, the fatty acid being as described above.
Diglyceride: a glycerol ester and two fatty acids, the fatty acids being as described above.
Triglyceride: a glycerol that is esterified with three fatty acids, as described above. Fatty acids can be saturated, monounsaturated or polyunsaturated. In the context of the present invention, triglycerides are understood to be edible oils and fats. As used herein, the term 'oil' is used as a generic term for oils and fats pure or containing compounds in solution. Oils can also contain suspended particles. As used herein the term 'fats' is used as a generic term for compounds containing more than 80% triglycerides. They can also contain diglycerides, monoglycerides and free fatty acids. In common parlance, liquid fats are often referred to as oils, but here the term fats is also used as a generic term for such liquid fats. Fats include: plant oils (for example, allanblackia oil, apricot oil, arachis oil, arnica oil, argan oil, avocado oil, babassu oil, baobab oil, black seed oil, blackberry seed, black currant seed oil, blueberry seed oil, borage oil, calendula oil, camellia seed oil, castor oil, cherry seed oil, cocoa butter, coconut oil, oil corn, cottonseed oil, oil of onagrace, grapefruit oil, grape seed oil, hazelnut oil, hemp seed oil, ilipod butter, lemon seed oil, lime seed oil, oil flax seed, kukui nut oil, macadamia oil, corn oil (maize), mango butter, Limnanto oil, melon seed oil, Moringa oil, mowrah butter, mustard seed oil, olive oil, orange seed oil, palm oil, palm seed oil, papaya seed oil, seed oil passion fruit, peach seed oil, plum core oil, pomegranate seed oil, poppy seed oil, pumpkin seed oil, rapeseed (or canola) oil, raspberry seed oil, bran oil rice, rosehip berry oil, safflower oil, sea buckthorn oil, sesame oil, shea butter, soybean oil, strawberry seed oil, sunflower oil, sweet almond oil, walnut, wheat germ oil; fish oils (for example, sardine oil, horsetail oil, herring oil, cod liver oil, oyster oil); animal oils (for example, butter or conjugated linoleic acid, bacon or tallow); or any mixture or fraction thereof. Oils or fats may also have been modified by hardening, fractionation, chemical or enzymatic interesterification or by a combination of these steps.
Phytosterol: a group of steroidal alcohols, naturally occurring phytochemicals in plants. At room temperature they are white powders with a characteristic mild odor, insoluble in water and soluble in alcohols. They can be used to reduce the level of LDL cholesterol in plasma in humans.
Phytostanol: similarly to phytosterol, a group of steroidal alcohols, naturally occurring phytochemicals in plants. They can also be obtained by hardening a phytosterol.
Phytosteryl fatty acid ester: a phytosterol that has been modified by esterification with a fatty acid.
Phytostanil fatty acid ester: a phytostanol that has been modified by esterification with a fatty acid.
Waxes: a wax is a non-glyceride lipid substance having the following characteristic properties: plastic (malleable) at normal ambient temperatures; a melting point above approximately 45 ° C; a relatively low viscosity when melted (unlike many plastics); insoluble in water, but soluble in some organic solvents; hygroscopic. Waxes can be natural or artificial, but natural waxes are preferred. Beeswax, candelilla and carnauba wax (vegetable waxes), Chinese wax, epicuticular waxes, Japanese wax, jojoba oil, lanolin or wool wax, Montana wax, Ouricuri wax, paraffin (a mineral wax), petroleum jelly , retamo wax, rice bran wax, lacquer wax, spermaceti, sugar cane wax are commonly found waxes that are naturally occurring. Some artificial materials that have similar properties are also described as wax or waxy. Chemically speaking, a wax can be an ethylene glycol ester (ethane-1,2-diol) and two fatty acids, which are different from fats which are glycerol esters (propane-1,2,3-triol) and three fatty acids. It can also be a combination of fatty alcohols with fatty acids, alkanes, ethers or esters. Preferred waxes are one or more waxes chosen from candelilla wax, carnauba wax, lacquer or beeswax or silicon wax or their synthetic equivalents. Also paraffin-based synthetic waxes are within the scope of the present invention. Also included are polyethylene waxes, polymerized alpha-olefins, chemically modified waxes - usually esterified, or saponified substituted amide waxes.
Most preferred is the lipophilic compound selected from the group of phytosterols, carotenoids and derivatives of these compounds. Mixtures of these compounds are also within the scope of the invention. These compounds are of special interest to be ingredients of food products, as they have a nutritional benefit when consumed. Phytosteroids are known for their LDL cholesterol lowering effect when consumed.
The term phytosterols and plant sterols are considered to be synonymous, and they can also be referred to as 'sterols'. Phytosterols 10 can be classified into three groups, which are the 4-demethylesterisols, 4-monomethylesterols and 4,4'-dimethylsterols. In oils, they mainly exist as free sterols and fatty acid sterol esters, although sterol glucosides and acylated sterol glucosides are also present. There are three major phytosterols, namely beta-sitosterol, 15 stigmasterol and campesterol.
The respective 5-alpha-saturated derivatives (the 'stanols') such as sitoestanol, campestanol and ergostanol and their derivatives are also included by the term phytosterol.
Preferably, phytosterol is selected from the group consisting of: 20 beta-sitosterol, beta-sitoestanol, campesterol, campestanol, stigmasterol, brassicasterol, brassicastenol or a mixture thereof. Appropriate sources of phytosterols are, for example, derived from soy beans or their oil.
Phytosterols are difficult to formulate in food products in their free form due to their poor solubility in fats and immiscibility in water, which can result in food products having poor organoleptic properties, for example, a sandy mouth feeling. This has been partially mitigated in the prior art by esterification of phytosterol with fatty acids, but requires additional processing steps and, thus, an increase in costs. It has also been described in the literature that by using very small particles of phytosterol it may be possible to alleviate, to some extent, the negative impact of phytosterol on organoleptic properties. Typically the size of such particles is in the order of tens of microns, however, particle sizes above one micron are poorly bio-accessible in the gastrointestinal tract. In addition, it has been described in the literature that the negative influence of phytosterols on the organoleptic properties in emulsions can be mitigated to some extent by the emulsification of phytosterols with emulsifiers.
In the context of this invention, the term phytosterol refers to free phytosterol, that is, non-esterified phytosterol, unless otherwise specified.
In step (b), preferably the lipophilic compound is mixed with a non-aqueous phase. Through this mixture, the lipophilic compound is brought to liquid form through dissolution in the non-aqueous phase. Preferably, this step is performed while the temperature of the mixture is increased to a temperature of maximum 160 ° C, preferably maximum 150 ° C, preferably maximum 110 ° C, preferably maximum 95 ° C.
A 'non-aqueous phase' as used in this context can refer to a liquid under ambient conditions (temperature around 20 ° C, atmospheric pressure) and when said liquid has a tendency to flow, as determined by having a loss module G ”greater than the storage module G 'at shear rates y (range) ranging from 1 per second to 500 per second. The non-aqueous phase can also be solid at room temperature, and made liquid by melting. The non-aqueous character is defined as the material that is not being able to dissolve more than 10% by weight in water under ambient conditions, preferably less than 5% by weight, preferably less than 1% by weight, preferably less than 0 , 5% by weight, preferably less than 0.2% by weight.
Preferably, the non-aqueous phase comprises a vegetable oil, for example, sunflower oil, palm oil, olive oil, rapeseed oil, or any other suitable oil or combination of oils, or a wax (for example, candelilla, carnauba wax, or other waxes as described above). The oil can be liquid at room temperature, or alternatively it can be solid at room temperature, in which case the oil must be melted first by increasing the temperature. An animal fat or oil, such as fish oil, dairy fat, bacon, or tallow, can also be used. Such vegetable oil or animal oil or algae oil obtained from step (b) can be used as an ingredient in food products.
The optional non-aqueous phase can also be chosen from materials such as mineral oils, petroleum jelly, silicon oils, and derivatives of these compounds, and combinations thereof. In the case of a structured non-aqueous phase obtained from step (b) it can be used as an ingredient in home care or personal care products.
Preferably the concentration of the lipophilic compound in the non-aqueous phase is at least 5% by weight, preferably at least 10% by weight, preferably at least 20% by weight. Although the lipophilic compound may be poorly soluble in the non-aqueous phase, as in the case of carotenoids and phytosteroids (for example, in vegetable oils at room temperature), such a high concentration of lipophilic compound in a non-aqueous phase can be used in the method of the invention. A high concentration has the advantage that the final emulsion will contain a high amount of the lipophilic compound in a non-aqueous phase, and this non-aqueous phase is dispersed as a colloidal dispersion, in that the droplet size is very small after step (c). The lipophilic compound can be in crystalline form when mixed with the non-aqueous phase. Upon dissolution of the lipophilic compound in the liquid, the lipophilic compound will be in amorphous form. The concentration of the lipophilic compound can be so high that after emulsification, and upon cooling of the emulsion, the dispersed phase becomes supersaturated. Due to the small droplet size of the dispersed phase, the hydrophobic compound can remain in an amorphous state, and not, or only to a limited extent, crystallize. It may even happen that the lipophilic compound remains in a liquid or metastable state.
Less crystallization means that the droplets remain stable; as occurs, in a different way, when crystals can grow and form needles that clump and interfere with the interface between the oil droplet and the continuous aqueous phase, breaking the droplets. Therefore, the method according to the invention leads to improved stability of the emulsion, but also to dispersed non-crystalline lipophilic compounds.
In the case of phytosterols, amorphous phytosterol is more easily incorporated into micelles in the intestinal tract than crystallized phytosterol. As part of the micelles, the function of phytosterols is to influence the adsorption and desorption of LDL cholesterol from the plasma, leading to decreased LDL cholesterol levels. Thus, one of the advantages of the method of the invention is that when the sterols are mixed with a non-aqueous phase and subsequently emulsified, the amorphous phase can lead to improved bio-accessibility and / or bio-availability when compared to crystallized sterols.
Step (c) can preferably be carried out at the temperature which is obtained after mixing the aqueous phase of step (a) with the lipophilic phase of step (b). Prior to step (c), a preemulsion can be produced to mix the aqueous phase from the lipophilic phase, in order to improve the emulsification in step (c). This pre-mixing can be carried out under temperature control, to maintain the liquid mixture. The temperature in this optional pre-mixing step is preferably at most 110 ° C, preferably at most 100 ° C (when at atmospheric pressure), preferably at most 95 ° C. The temperature of the emulsification in step (c) can be controlled to ensure that the aqueous phase of step (a) and the lipophilic phase of step (b) remain liquid. Usually, mixing in step (c) will be carried out at the temperature of the pre-mixtures in steps (a) and (b). Usually, during the emulsification stage, the temperature of the mixture will not decrease due to the admission of energy into the mixing process. Thus, the temperature of the emulsion from step (c) can be increased.
The emulsion obtained in step (c) can be used as an ingredient in food products, or personal care products, or home care products, or cosmetic products, or pharmaceutical products. In this case, the emulsion from step (c) can be placed in contact with any of the other ingredients of such a product. Subsequently, the normal process of preparing such a product can be carried out. Before using the emulsion from step (c), the mixture from step (c) can be cooled. This optional cooling can be done using any appropriate method.
Due to the incorporation of lipophilic compounds in the non-aqueous liquid, the droplets of the dispersed phase can become solid after step (c), especially when the emulsion obtained in step (c) is cooled. The method according to the invention can then be seen as an encapsulation method, the lipophilic compound being encapsulated in the non-aqueous phase. Thus, the method according to the invention preferably also provides a method of encapsulating lipophilic compounds. The average Sauter diameter of the dispersed phase obtained after step (c) is less than 1 micrometer. Preferably, Sauter's average diameter of the dispersed phase is less than 500 micrometers. Even more preferred is the Sauter's average diameter of the dispersed phase less than 400 micrometers, more preferred less than 300 micrometers. Preferably the average Sauter diameter of the dispersed phase is at least 100 micrometers, more preferred at least 150 micrometers. When the average size of the scattered phase is as small as these values, the emulsion can become transparent, as the size of the scattered droplets is less than the wavelength of visible light. This property can be used to formulate products of interest to the consumer, with properties that have not been achieved before.
The concentration of the dispersed phase in the emulsion that is obtained in step (c) is at least 20% by weight of the emulsion. One of the advantages according to the method of the invention is that the concentration of the dispersed phase that can be obtained is high. Especially when compared to emulsions produced by high pressure homogenizers. Preferably, the concentration of the dispersed phase is at least 40% by weight of the emulsion, preferably at least 50% of the emulsion. Preferably the dispersed phase comprises at least 60% by weight of the emulsion. Preferably, the emulsion contains a maximum of 95% by weight of the dispersed phase emulsion, preferably a maximum of 85% by weight, preferably a maximum of 75% by weight. Such highly dispersed emulsions have the advantage that when used in food products, or personal care products, or home care products, or cosmetic products, or pharmaceutical products, only a relatively small amount of the emulsion is required to formulate the products.
Another advantage of the production of continuous concentrated emulsions in water (both, high concentration of the dispersed phase, as well as high concentration of the lipophilic compound in the non-aqueous phase), when compared to more diluted emulsions, as processed in, for example, high homogenizers pressure, is the reduction of the energy required to heat the aqueous phase and the lipophilic phase. This is due to the large difference in heat capacity between water and lipophilic compounds and non-aqueous phases. CDDM device and / or CTM device
In step (c), the continuous water emulsion is prepared by mixing the aqueous phase of step (a) with the lipophilic phase of step (b) in a distributive and dispersive mixing apparatus of the Dynamic Controlled Deformation Mixer type or Cavity Transfer Mixer, and the mixer being suitable for inducing flow in the direction of the extension in a liquid composition, and the mixer comprising relatively mobile facing surfaces closely spaced, at least one having a series of cavities in it, in which the cavities on each surface are arranged in such a way that, in use, the cross-sectional area for the flow of the liquid successively increases and decreases by a factor of at least 3 throughout the apparatus.
For the purpose of understanding the operation of the CTM or CDDM in general, the WO 96/20270 description is hereby incorporated by reference. The distributive mixing regions (where the flow path is wide) comprise cavities similar to CTM with movement between them in the direction perpendicular to the volumetric flow of the liquid. Among these distributive mixing regions there are regions in which the flow path is narrower and the flow is more extensive. It is possible, in the case of the mixer used in the method according to the invention, to provide one or more regions in which the juxtaposition is such that the arrangement is similar to the CTM and one or more regions in which the arrangement is similar to the CDDM. Preferably, a CDDM apparatus is used in the method according to the invention.
In a preferred embodiment, the CDDM device or the CTM device can be described as follows. With reference to Figure 10 and Figure 11, preferably the CDDM or CTM apparatus comprises two facing surfaces 1, 2, spaced at a distance 7, where the first surface contains at least three cavities 3, where at least one of the cavities has a depth 9 with respect to surface 1, with the second surface 2 containing at least three cavities 4, at least one of the cavities having a depth 10 with respect to surface 2, with the cross-sectional area for the liquid flow available during the passage along the apparatus successively increases and decreases at least 3 times, and the surface 1 has a length 5 between two cavities, and the surface 2 has a length 6 between two cavities, and the surfaces 1, 2 are positioned in such a way that the corresponding lengths 5, 6 overlap to create a gap having a length 8 or not overlap, creating a length 81, send what the cavities are arranged in such a way that the cross-sectional area for the flow of liquid available during the passage along the apparatus successively increases in the cavities and decreases in the cracks by a factor of at least 3, and the distance being 7 between the two surfaces 1, 2 is between 2 micrometers and 300 micrometers, and either the ratio between the length 8 and the distance 7 between the two surfaces 1,2 varies from 0 to 250, or the ratio between the length 81 and the distance 7 between the two surfaces 1, 2 varies from 0 to 30.
With reference to Figure 10 and Figure 11: as in the case of CTM and CDDM, there are several possible configurations for the mixing device. In a preferred combination, the facing surfaces 1, 2 are cylindrical. In such a configuration, the apparatus will generally comprise a cylindrical drum and a coaxial wrap. Surfaces 1, 2 will be defined by the outer surface of the drum and the inner surface of the wrap. However, there are alternative configurations in which the facing surfaces are circular or disk-shaped. Between these two extremes of configuration are those in which the facing surfaces are conical or frusto-conical. Non-cylindrical embodiments allow for additional shear variation in different parts of the flow along the mixer.
The regions where the facing surfaces 1, 2 are most closely spaced are those where the shear rate within the mixer tends to be the highest. The gap 7 between surfaces between the facing surfaces 1, 2 forms this region, combined with lengths 8 or 81. The high shear contributes to energy consumption and heating. This is especially true where the mixing surfaces of the mixer are spaced less than 50 micrometers apart. Advantageously, the limitation of high shear regions to relatively short regions means that energy consumption and the effect of heating can be reduced, especially where, in regions similar to CTM, the facing surfaces are spaced by a relatively wide span.
Thus, the device can be designed so that good mixing is obtained, while the pressure drop is kept, throughout the device, as small as possible. The design can be modified by adjusting the dimensions of the various parts of the device, as explained below.
The distance 7 between the corresponding surfaces is preferably 2 micrometers to 300 micrometers, which corresponds to the height of the gap. Preferably the distance 7 is between 3 micrometers and 200 micrometers, preferably between 5 micrometers and 150 micrometers, preferably between 5 micrometers and 100 micrometers, preferably between 5 micrometers and 80 micrometers, preferably between 5 micrometers and 60 micrometers, preferably between 5 micrometers and 40 micrometers micrometers. More preferably, the distance 7 is between 8 micrometers and 40 micrometers, more preferably between 8 micrometers and 30 micrometers, more preferably between 10 micrometers and 30 micrometers, more preferably between 10 micrometers and 25 micrometers, more preferably between 15 micrometers and 25 micrometers.
The actual height of the slot 7 depends on the dimensions of the apparatus and the required flow rate, and a person skilled in the art will know how to design the apparatus so that the shear rates within the apparatus remain relatively constant regardless of the size of the apparatus.
Surfaces 1 and 2, each containing at least three cavities 3, 4, create a volume between the surfaces for the flow of the two fluids being 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 surfaces 1 and 2 can be considered to be a gap having a height 7. The distance 5 between two cavities on surface 1 and the distance 6 between two cavities on surface 2 and the relative position of these corresponding parts determines the maximum slot length.
Preferably, surfaces 1, 2 with cavities 3, 4, which together form the volume for mixing the aqueous phase of step (a) and the lipophilic phase of step (b), are positioned in such a way that the corresponding lengths 5, 6 of the surfaces (which create the gap overlap) create a gap length 8 (in the direction of the volumetric flow) that is at most 250 times wider than the distance 7 between the surfaces. Preferably, the ratio between length 8 and distance 7 between the two surfaces 1, 2 ranges from 0 to 100, preferably from 0 to 10, preferably from 0 to 5. Alternatively, length 81 is preferably at most 600 micrometers.
Preferably and alternatively, surfaces 1, 2 are positioned so that no overlap is created, however, in this case, a length 81 is created. The ratio between length 81 and the distance 7 between the two surfaces 1, 2 preferably varies from 0 to 30. In this case there is no overlap between the corresponding parts of the surfaces, and the gap is created with what can be called 'negative overlap'. This 'negative overlap' accommodates the possibility that the distance 7, between the two corresponding surfaces 1 and 2, is close to zero. Preferably length 81 is such that the ratio between length 81 and distance 7 between the two surfaces 1, 2 varies from 0 to 15, more preferably from 0 to 10, more preferably from 0 to 5 and most preferred of all 0 to 2.
An additional benefit of this variation in the normal separation of the facing surfaces in the direction of the volumetric flow, is that because there are relatively small regions of high shear, especially with a low residence time, the pressure drop across the mixer can be reduced without compromising the mixing performance.
The small overlap between the corresponding parts of the surfaces 1, 2 leads to a relatively small pressure that is required in order to create a fine dispersion, when compared to devices that have a greater overlap and consequently also the need for a higher pressure. Usually a longer distance from a slit (or longer capillary) leads to smaller droplets of the dispersed phase. Now we have found that with a short capillary or even no capillary, the droplets of the dispersed phase remain small, while the required pressure is relatively low compared to the longer overlap. For example, high pressure homogenizers can operate at pressures up to 160,000 kPa or even higher. Preferably the mixer of the invention is operated at a pressure of less than 20,000 kPa, preferably less than 8,000 kPa, preferably less than 6,000 kPa, preferably less than 4,000 kPa, most preferred of all less than 3,000 kPa. With these relatively low pressures, a good mixing process is obtained.
An additional advantage of the relatively low pressure is that the energy consumption to apply the pressure is much lower than in conventional devices that use pressures of 100,000 kPa or greater to achieve dispersed phases having a size of less than 1 micrometer. In addition, less restrictive material specifications are required for the design of an apparatus that can withstand high pressures, so that raw materials can be saved.
With reference to Figure 10 and Figure 11, fluids preferably flow from left to right along the apparatus. The cracks create an acceleration of the flow, while at the exit of the crack the fluids slow down due to the increase in the surface area for the flow and due to the expansion that occurs. The acceleration and deceleration lead to the breaking of the large droplets of the dispersed phase, to create finely dispersed droplets in a continuous phase. Droplets that are already smaller 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 the flow of liquid available during the passage through the apparatus successively increases and decreases at least 3 times, and these passages lead to an effective mixing of the two fluids. This means that the cross-sectional area for the flow of liquid in the cavities is at least 3 times greater than the cross-sectional area for the flow of liquid in the cracks. This refers to the ratio between lengths 11 and 7. Preferably the cross-sectional area for the flow is designed in such a way that the cross-sectional area for the flow of liquid available during the passage along the apparatus successively increases and decreases by a factor of at least 5, preferably at least 10, preferably at least 25, preferably at least 50, to the most preferred values from 100 to 400. The cross-sectional surface area for fluid flow is determined by depth 9 of the cavities 3 on the first surface 1 and the depth 10 of the cavities 4 on the second surface 2. The total cross-sectional area is determined by the length 11 between the bottoms of two corresponding cavities on the opposite surfaces.
Each of the surfaces 1, 2 contains at least three cavities 3, 4. In this case, the flow expands at least 3 times during the passage, and the flow passes through at least 3 cracks during the passage. Preferably, the cross-sectional area for the flow of liquid available during passage along the apparatus successively increases and decreases between 4 and 8 times. This means that the flow during the passage experiences the presence of between 4 and 8 cracks and cavities.
The shape of the cavities 3 can take any appropriate shape, for example, the cross section may not be rectangular, but it can take the form of, for example, a trapezoid, or a parallelogram, or a rectangle where the corners are rounded. Any arrangement of the wells, and number of wells, and size of the wells may be within the scope of the present invention.
The device can be operated in static mode (without rotation), as well as in dynamic mode (with rotation). In this case, preferably, one of the surfaces is capable of rotating with respect to the other surface at a frequency between 10 and 40,000 revolutions per minute, preferably between 20 and 35,000 revolutions per minute, more preferably between 1,000 and 25,000 revolutions per minute.
In general, rotation can lead to an improved mixing process and the creation of smaller dispersed phase droplets. Static operation has the advantage that less energy is required for mixing. Operating the device without rotation leads to a very efficient and effective mixing of fluids. Without rotation, similar sizes of dispersed phase can be obtained, without the need for high pressure or the use of energy for rotation. On the other hand, rotation at high frequencies can lead to very finely dispersed droplets of the dispersed phase, in case the two fluids are mixed to create the emulsion.
Additional features of the known CTM and CDDM can be incorporated into the mixer described here. For example, one or both of the facing surfaces can be provided with means to heat or cool them. When cavities in the facing surfaces are provided, they can be of different geometry in different parts of the mixer in order to further vary the shear conditions.
In a preferred example, 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 micrometers, and / or where the length of the slot 8 is at most 2 millimeters, for example 80 micrometers, or 20 micrometers, or even 0 micrometers. The length of the slot 8 plus the length of the cavity 17, 18 combined is a maximum of 10 millimeters, and / or where the length of the cavities 9, 10 is a maximum of 2 millimeters. In this case, preferably the inner diameter of the outer surface is between 20 and 30 millimeters, preferably about 25 millimeters. The total length of the apparatus, in this case, is between 7 and 13 centimeters, preferably about 10 centimeters. 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 most preferably, alternatively, between 5,000 and 25,000 revolutions per minute.
The shape of the area for the flow of liquid can take different forms, and naturally depends on the shape of the facing surfaces. If the surfaces are flat, then the cross-sectional area for the flow can be rectangular. The two facing surfaces can also be in a circular shape, for example, a cylindrical rotor that is positioned in the center of a cylindrical tube, the outside of the cylindrical rotor forming a surface, and the inner surface of the cylindrical tube forming the other surface . The circular annular space between the two facing surfaces is available for the flow of the liquid. Emulsion obtained by the method according to the invention
The present invention also provides a continuous water emulsion obtained by the method according to the invention. Such an emulsion comprises a dispersed phase comprising a lipophilic compound, the average Sauter diameter of the dispersed phase being less than 1 micrometer, and the concentration of the dispersed phase being at least 20% by weight of the emulsion.
Preferred aspects disclosed herein above, in the context of the invention, are also applicable to this additional aspect of the invention, mutatis mutandis.
Preferably, the lipophilic compound comprises lecithin, fatty acid, monoglyceride, diglyceride, triglyceride, phytosterol, phytosteranol, phytosteryl fatty acid ester, fattystannyl fatty acid ester, wax, fatty alcohol, carotenoid, oil-soluble dye, vitamin-soluble dye oil, oil-soluble flavoring, oil-soluble fragrance, mineral oils or derivatives, petroleum jelly or derivatives, or silicon oils or derivatives, or combinations of these compounds. The most preferred lipophilic compound is selected from the group of phytosterols, carotenoids and derivatives of these compounds. Mixtures of these compounds are also within the scope of the invention.
Preferably, the lipophilic compound is mixed with a non-aqueous phase, which together form the dispersed phase of the emulsion. Preferably, the non-aqueous phase comprises vegetable oil, for example, sunflower oil, palm oil, olive oil, rapeseed oil, or any other suitable oil or combination of oils. The oil can be liquid at room temperature, or alternatively it can be solid at room temperature, in which case the oil must be melted first by increasing the temperature. An animal fat or oil, such as fish oil, dairy fat, bacon, or tallow can also be used.
The optional non-aqueous phase can also be chosen from materials such as mineral oils, petroleum jelly, silicon oils, and derivatives of these compounds, and combinations thereof.
Preferably, the concentration of the lipophilic compound in the non-aqueous phase is at least 5% by weight, preferably at least 10% by weight, preferably at least 20% by weight.
Sauter's average diameter of the dispersed phase is less than 1 micrometer, preferably less than 500 nanometers. Even more preferred is Sauter's average diameter of the dispersed phase of less than 400 nanometers, more preferred less than 300 nanometers.
The concentration of the dispersed phase in the emulsion obtained from step (c) is at least 20% by weight of the emulsion. Preferably, the concentration of the dispersed phase is at least 40% by weight of the emulsion, preferably at least 50% of the emulsion. Preferably, the dispersed phase comprises at least 60% by weight of the emulsion.
The mainly preferred continuous emulsion in water, obtained by the method according to the invention, comprises a dispersed phase comprising a phytosterol, the average Sauter diameter of the dispersed phase being less than 1 micrometer, and the concentration of the phase dispersed is at least 20% by weight of the emulsion. Preferably, the phytosterol is dispersed in a non-aqueous phase. Preferably the non-aqueous phase comprises a vegetable oil, for example, sunflower oil, palm oil, olive oil, rapeseed oil, or any other suitable oil or combination of oils. Fat, or animal oil, such as fish oil, dairy fat, bacon, or tallow can also be used.
Preferably, the phytosterol concentration in the non-aqueous phase is at least 5% by weight, preferably at least 10% by weight, preferably at least 20% by weight. Preferably, the average Sauter diameter of the dispersed phase is less than 500 nanometers, preferably less than 400 nanometers, more preferred is less than 300 nanometers. Preferably, the concentration of the dispersed phase is at least 40% by weight of the emulsion, preferably at least 60% of the emulsion. Preferably, the total phytosterol concentration based on the weight of the emulsion is between 5 and 20% by weight of the emulsion.
The present invention also provides a food product, or a personal care product or a home care product or a cosmetic product, or a pharmaceutical product comprising the emulsion according to the first aspect of the invention. The emulsion obtained by the method according to the invention can be used as such or as an ingredient in food products such as water-in-oil emulsions or oil-in-water emulsions, or personal care products, such as skin creams, or as an ingredient in home care products, such as liquid laundry detergents. These personal care products can be oil-in-water emulsions. Also double emulsions and multiple emulsions (such as oil-in-water-in-oil emulsions) are emulsions that are within the scope of the present invention. For example, the continuous water emulsion can be used to create an oil-in-water-in-oil emulsion: the continuous water emulsion obtained from step (c) of the method according to the invention can be emulsified in an oily phase. to be continued.
In the case of food products, the non-aqueous phase can be a lipid phase, for example, droplets of a dairy fat or sunflower oil dispersed in an aqueous phase to form an oil-in-water emulsion. Examples of an oil-in-water emulsion are spices and mayonnaise products, dairy creams, and body lotions and skin creams. Also dairy drinks, drinking yogurt or milk, are oil-in-water emulsions, if they are not fat-free. In the case of water-in-oil emulsion such as margarine, butter and other spreading creams, the lipid phase can be considered a continuous vegetable oily phase or a fatty butter phase, as applicable.
In the case of personal care products or home care products, the non-aqueous phase can be chosen from materials such as mineral oils, petroleum jelly, or silicon oils, and derivatives of these compounds, and combinations thereof.
The amount of non-aqueous phase in such products can vary from 1% by weight to 99% by weight of the product, depending on the product. For example, a butter can contain 99% by weight of edible oil or fat. A margarine contains about 80% edible oils and fats. A water-in-oil cream can contain 20 to 70% by weight of edible oils and fats. A sauce or mayonnaise can contain from about 5% by weight to 80% by weight of a non-aqueous lipid phase. A dairy cream can contain about 20 to 30% by weight of edible oils and fats. A dairy drink or similar can contain up to 5% by weight of edible oils and fats. A skin cream can contain about 5 to 20% by weight of lipophilic compounds.
Additionally and preferably, the present invention provides a food product comprising the emulsion prepared according to the method of the invention. Such a product can be produced using any conventional method of production, by placing the continuous emulsion in water obtained with one or more other ingredients of such product in contact. Subsequently, the normal process of preparing such a product can be carried out.
The food products of the invention can be of all kinds of food products, for example, marinades, sauces, condiments, butter, spray products, spreading creams, shallow frying products, condiments, seasonings, mayonnaise, mayonnaise low fat and ice cream.
Preferably, the food products according to the invention are: spreading creams (water-in-oil emulsions or oil-in-water emulsions), margarines (water-in-oil emulsions), dairy products, such as butter (emulsion) water-in-oil), or liquid water-in-oil emulsions or liquid oil-in-water emulsions designated as shallow frying.
Other preferred food products according to the invention are drinks containing the emulsion obtained from the method according to the invention. An advantage of the emulsions prepared according to the present invention is that transparent drinks can be produced due to the small size of the droplets of the dispersed phase which are preferably shorter than the wavelength of visible light.
In addition, the present invention provides a personal care product comprising the emulsion prepared according to the method of the first aspect of the invention. In this case, the personal care product is, for example, a skin cream, body lotion, liquid soap, hand washing, facial foam, shampoo or hair conditioner.
Additionally and preferably, the present invention provides a home care product comprising the emulsion prepared according to the method of the first aspect of the invention. In this case the home care product is, for example, a laundry detergent composition, preferably a liquid laundry detergent composition, or a laundry conditioner composition.
In addition and preferably, the present invention provides a cosmetic product comprising the emulsion prepared according to the method of the first aspect of the invention. In this case the cosmetic product is, for example, makeup like lipstick, products for the eyes and lips.
In addition and preferably, the present invention provides a pharmaceutical product comprising the emulsion prepared according to the method of the first aspect of the invention. In this case the pharmaceutical product is, for example, a composition in which the drugs have been encapsulated in a non-aqueous phase to direct the in vivo release.
The various features and embodiments of the present invention, referred to in individual sections, apply below, where appropriate, to other sections, mutatis mutandis. Consequently, the features cited in one section can be combined with the features specified in other sections, where appropriate. All publications mentioned in this description are hereby incorporated by reference. The various modifications and variations of the described methods and products of the invention will become apparent to those skilled in the art without departing from the scope of the invention. Although the invention has been described in connection with specific preferred embodiments, it is to be understood that the invention as claimed should not be unduly limited to such specific embodiments. In fact, various modifications of the described modes for carrying out the invention, which are evident to those skilled in the art in relevant fields, are intended to be within the scope of the claims. EXAMPLES
The following non-limiting examples illustrate the present invention. CDDM device
The experiments were carried out in a CDDM device as schematically represented in Figure 2 and Figure 10, with the device comprising a cylindrical drum and a coaxial wrap (the facing surfaces 1, 2 are cylindrical). Confronting surfaces 1, 2 are defined by the outer surface of the drum and the inner surface of the casing, respectively. The CDDM can be described by the following parameters: - slot 7 height is 10 micrometers; - slot 8 length is 120 micrometers; - total length of the device is 10 centimeters (length means the zone where the fluids are mixed) - along the length of the CDDM in the axial direction (in the direction of the flow), the flow experiences six cracks with height 7, the flow is contracted 6 times; - depth of cavities 3, 4 is a maximum of 2 millimeters; - internal diameter of the stator is 25 mm; - rotational speed of the device is up to 25,000 revolutions per minute, and it was operated in these experiments at a maximum of 18,000 revolutions per minute. Particle size distribution
Particle sizes and their distribution were determined using static and dynamic light scattering (SLS and DLS, respectively) with Mastersizer 2000 and Zetasizer series Nano ZS instruments (Malvern Instruments, UK). The dispersions produced were first diluted using deionized water (approximately 100 times). The SLS technique was used to compare the measurement made by the DLS technique and also to check for the presence of larger particles that are beyond the DLS detection range. Sauter's mean diameter (ds.a), d4.3 and Amplitude were determined using SLS. Scanning Electron Microscopy (SEM)
A low temperature field emission scanning electron microscope was used. A drop of the dispersion was mounted on a brass rivet of 1 mm internal diameter immersed in an antioxidant nitrogen preparation. After transferring to a Gatan Alto 2500 cryocharger, samples of the preparation at low temperature were fractured at -98 ° C, rubbed for 15 seconds, cooled to -110 ° C and coated with 2 nm Pt / Pd. The examination was performed using a JEOL 6301F scanning electron microscope adjusted with a Gatan cold stage at -150 ° C operated at 5 KV. Example 1 - Preparation of highly concentrated sterol-fed colloidal dispersions using CDDM apparatus
Myritol® 318 (medium chain triglyceride oil (MCT), from Cognis, Monheim am Rhein, Germany) and a mixture of crystalline phytosterol (containing 84% beta-sitosterol, 7% phytostanols, 9% other sterols, from Cognis, Monheim am Rhein, Germany) were used as the material of the dispersed phase. A nonionic emulsifier, polyoxyethylene (20) sorbitan monolaurate, commercially known as Tween® 20, was purchased from Sigma Aldrich (UK). Phospholipon 80 was supplied by Phospholipid GmbH (Cologne, Germany).
The colloidal dispersions fed with phytosterol were prepared in 70:30 and 65:35 continuous dispersaiasis phase ratios (w / w). The dispersed phase was prepared with two different concentrations of phytosterol in MCT oil and phospholipon 80, corresponding to phytosterol concentrations of 7% and 13% (w / w) based on the total colloidal dispersion. The percentage of the Tween 20 emulsifier ranged from 7% to 9%. Phospholipon was added as a 1.7% (w / w) crystallization inhibitor, based on the weight of the total dispersion.
For the production of all colloidal dispersions, the dispersed phase, a solution of phytosterol and phospholipon in MCT oil; and continuous phase, water and Tween 20, were separately heated to 108 ° C and 90 ° C, respectively. The dispersed phase was continuously agitated in a feed hopper using a rotor-stator system (Fluid Division Mixing). The continuous phase was prepared by heating water with Tween 20 to 90 ° C with continuous stirring using a magnetic stirrer.
Colloidal oil-in-water (O / W) dispersions containing sterols were produced on a production line using the CDDM apparatus described above. The experiments were performed by CDDM over a range of flow rates from 20 mL / s to 84 mL / s, and rotational speeds from 0 rpm (static mode) to 18,000 rpm (dynamic mode). In each experiment, 50 g of dispersions were prepared with final temperatures between 55 ° C and 70 ° C. After that, the samples were left on the bench for cooling until they reached room temperature.
After collecting the hot samples, their droplet size and size distributions were measured using static light scattering (SLS). After cooling, its morphology was analyzed by scanning electron microscopy (SEM), in order to determine whether the phytosterols had remained in the dispersed phase or had crystallized at the oil-water interface and, thus, migrated to the continuous phase during the process / after cooling. Colloidal dispersions containing 7% phytosterols
The CDDM device was operated at flow rates in the range of 20 to 80 mL / s and rotor speeds from 0 to 18,000 rpm. The pressure drop was from 4,000 to 8,000 kPa. The droplet size distribution of the phytosterols dispersed in MCT oil was determined by static light scattering (see Figure 3 and Table 1), and this showed that all dynamic processes of rotational speeds provided narrow droplet size distribution, consequently less polydispersion than that static. Higher speeds can have a greater impact on the droplet size distribution, as seen at 15,000 rpm, whose droplets are monodisperse. At higher speeds, the emulsifier molecules can quickly reach an interface and be immediately adsorbed. Table 1: Diameters of the dispersed phase d3,2 and d4,3 (θm micrometers) and Amplitude; 7% dispersion of phytosterol in the emulsion, flow rate of 20 mL / s in CDDM, at various rotational speeds.

The dynamic process proved that smaller droplets and fewer phytosterol crystals can be obtained, as can be seen from the morphology of the colloidal dispersions produced by the dynamic process or the static process (Figure 4). This method allows the production of smaller monodispersed droplets containing phytosterols in amorphous form. This is the most stable physical form of those colloidal dispersions suitable for long shelf-life food products. The amorphous form can be proved by the absence of phytosterol needles, instead of a high concentration of phytosterols in the oil. In the case of nano-dispersions as obtained herein, the droplet size provides an additional positive result in preventing phytosterol crystallization. Figure 5 and Figure 6 show the morphology of colloidal dispersions fed with 7% phytosterol (concentrated 70/30 and diluted 10/90) produced by the dynamic and static processes, respectively. After dilution, the particle morphologies show liquid droplets, which can be characterized as a subcooled emulsion. Figure 7 compares the droplet size distributions of colloidal dispersions fed with 7% phytosterol stabilized with Tween® 20 at concentrations of 7% and 9%. It was observed that the increase in the concentration of emulsifier provides smaller droplets (more surface area) (Table 2) and narrower droplet size distribution, protecting the droplets against Ostwald ripening and coalescence (Ostwald ripening). Table 2: Diameters of the dispersed phase of, 2 θ d4,3 and Amplitude of dispersion with 7% (w / w) phytosterol, flow rate of 20 mL / s in CDDM, at various rotational speeds, and in two concentrations of Tween 20 in the dispersion.

Higher speeds provide more energy dissipation throughout the 5 emulsification process, and smaller monodispersed droplets can be produced, which is shown in Table 3. Table 3: Ds, 2 and d4,3 dispersed phase diameters (in micrometers) and Amplitude: dispersion with 7% phytosterol, in CDDM at 18,000 rpm, various flow rates

The influence of the flow rate in da, 2 was not very great in this experiment, while some effect was shown on d4,3-
The average Sauter diameters (ds, 2) of the dispersions were between 260 and 290 nanometers. After running at 18,000 rpm and 40 mL / s, a semitransparent emulsion was produced.
Colloidal Dispersions Containing 13% Phytosterol 15 A high concentration of phytosterol can be successfully incorporated into fine oil droplets. In this type of formulation, the active molecule is in a supersaturated oil solution, when the volume of each simple droplet is further reduced during processing. The increase in surface area provides a reduction in the number of crystal nuclei per droplet, consequently, the chance that the crystal nuclei reach each other is reduced, and crystallization can rarely occur.
Figure 8 shows a SEM image of a sample prepared at 80 mL / s and 12,000 rpm. The dispersed phase and the continuous phase were 65% w / w and 35% w / w, respectively, with a phytosterol concentration of about 20% in the dispersed phase, leading to a phytosterol concentration of about 13% w / w dispersion. The ds, 2 and d <, 3 were 290 and 500 nanometers, respectively, and the amplitude was 1.44.
A similar sample (dispersed phase and continuous phase were 65% w / w and 35% w / w, respectively, with a phytosterol concentration of about 20% in the dispersed phase, leading to a phytosterol concentration of 13% w / w in the dispersion) was produced at a flow rate of 40 mL / s and 12,000 rpm. The ds, 2 of the dispersed phase was about 320 nanometers.
Figure 3.9 illustrates the SEM image droplet size distribution of two samples prepared at 40 mL / s and different rotational speeds. The dispersed phase and the continuous phase were also 65% and 35%, respectively, with phytosterol concentration of 7% and 13%. Smaller droplets and narrower droplet size distribution were obtained at the highest rate, even at the highest phytosterol concentration.
This example 1 refers to a method for the control of the crystalline habit of species via the manufacture of concentrated sub-micron emulsions. Comparative Example 2 - Preparation of colloidal dispersions fed with sterol using a high pressure homogenizer
The same raw materials as Example 1 were used, and additionally solid glyceryl tridodecanoate (trilaurin, ex Fluka, melting point 46.5 ° C) was purchased from Sigma Aldrich (UK). Colloidal oil-in-water (O / W) dispersions were prepared using a high pressure homogenizer, the Microfluidifier M-110S (Microfluidics Internationational Corporation, MA-Newton, USA). It consists of the following major parts: air motor, intensifier pump, and interaction chamber. It can be operated within a pressure range of about 20,000 to 160,000 kPa and a flow rate range of about 250 to 600 mL / min (about 4 to 10 mL / s). The ratio of the dispersed phase to the continuous phase was 10 to 90 (w / w). In the continuous phase, the percentage of the emulsifier Tween 20 varied from 1% to 4% and water from 86% to 89%. The dispersed phase (10%) was prepared with varying levels of phytosterol, either in MCT oil or trilaurin. Phytosterol ranged from 1% w / w to 4% w / w based on the total colloidal dispersion which is equivalent to 10% w / w to 40% w / w of the dispersed phase.
The dispersions were prepared by heating the MCT oil or trilaurin with phytosterol to about 100 ° C. The continuous phase (90%) was prepared by heating the deionized water with Tween 20 to 90 ° C with continuous stirring using a magnetic stirrer. The continuous phase was placed in the sample unit of the Microfluidizer, which was preheated to 95 ° C using a water bath, and then the dispersed phase was added. A coarse emulsion was prepared using a rotor-stator system (Ultra Turrax IKA T-25 digital; IKA Werke GmbH & Co. KG, Staufen, Germany), adapted with a propeller at a speed of 450 rpm. This was then further processed in the Microfluidizer, applying 4 cycles of homogenization at 116,500 kPa at 90 ° C to prepare a colloidal dispersion fed with phytosterol. This was then allowed to cool to ambient conditions at 20 ° C (about 1 ° C / min). The flow rate was 3 to 4 ml / s.
The results in particle diameter (as measured using DLS) are as follows, as a function of phytosterol concentration and oil phase.

Likewise, dispersions were prepared containing higher concentrations of phytosterol, 3% w / w and 4% w / w based on the weight of the emulsion. Microscopy images revealed that the dispersion contained 7% w / w of MCT oil and 3% w / w of phytosterol or 6% w / w of MCT oil and 4% w / w of phytosterol, respectively, phytosterol being in the form of needles (see Figure 9). The length of these needles was up to dozens of micrometers. This effect was particularly pronounced at higher concentrations of phytosterols.
This Example 2 refers to a method for producing solid micro-encapsulates or vehicles via the manufacture of sub-micron emulsions.
The comparison of the CDDM device with the Microfluidizer shows that the material produced in the CDDM had a final dispersed phase fraction of about 6 to 7 times greater, and even above 30 times the lowest pressure drop compared to the Microfluidifier. In addition, the phytosterol dispersions produced using the CDDM apparatus also maintained a small dispersed particle size, meaning that the sterols did not crystallize and remained in an amorphous state. Example 3 - Preparation of highly concentrated colloidal dispersions fed with silicone wax using the CDDM apparatus
The emulsions were produced using the CDDM, containing silicone wax as a dispersed phase (SilCare 41M65, which is stearyl dimethicone, ex Clariant, UK; melting point 32 ° C). The PET-POET polymer (polyethylene terephthalate-co-polyoxyethylene terephthalate, prepared internally as described in WO 2010/105922 A1) was used as an emulsifier. In addition, the polyoxyethylene (20) sorbitan monolaurate emulsifier (Tween® 20, ex Sigma Aldrich, UK) was used as a standard control emulsifier.
Such particles comprising a waxy solid and a polymeric deposition aid, which is partially embedded in the waxy solid, can be used in laundry washing treatment compositions to improve the fabric softening effect after washing (as described in WO 2010/105922 A1).
The standard method for producing silicone wax emulsions was as described below. First, the silicone wax was melted about 20 ° C above the melting point. An aqueous phase containing PET-POET or Tween 20 was heated to a maximum temperature of 90 ° C. The preheated continuous and dispersed phases were placed and maintained at 90 ° C in feed hoppers for the CDDM device. The homogenization of the continuous and dispersed phases was performed using the CDDM in the production line at different flow rates and rotational speeds. The amount of phase dispersed in the emulsions was 65% by weight, and the amount of aqueous phase was 35% by weight. The percentages of the emulsifier Tween 20 and PET-POET were 13% and 9%, respectively, based on the total emulsion. After using the CDDM, samples were collected at 50 ° C and left on the bench for cooling until they reached room temperature. Tween 20 stabilized silicone wax dispersions
Colloidal dispersions of silicone wax (60% w / w) in water (27% w / w) were produced, stabilized with Tween 20 (13% w / w). The results of d3,2, d4.3, amplitude and pressure drop across the CDDM device are given in the table below
Table 5: Droplet size distributions of silicone wax dispersions stabilized with Tween® 20 and produced using the CDDM device at about 70 mL / s, as a function of rotational speed

With an increase in rotational speed at a constant flow rate (about 70 mL / s), Sauter's mean diameter and d4.3 decreased. On the other hand, Amplitude increased slightly in the same process parameters. The lowest ds, 2 achieved was 280 nanometers. This behavior was observed in all dispersions of silicone wax stabilized with Tween® 20. The increase in speed provides greater efficiency in the transfer of energy, consequently better dispersive and distributive mixture, leading to a more intensive deformation and drop rupture, and faster stabilization of the emulsifier at the wax / water interface. PET-POET stabilized silicone wax dispersions
Colloidal dispersions of silicone wax (60% w / w) in 15 water (31% w / w) were produced, stabilized with PET-POET (9% w / w). The results of ds.2, d4,3, amplitude and pressure drop across the CDDM device are given in the table below.

This experiment shows that the dispersion containing 60% w / w silicone wax can be produced, and in which the average diameter of Sauter is less than 1 micrometer. The comparison of PET-POET with Tween 20 results in the fact that the increase in rotational speed showed a similar behavior up to 10,000 rpm at a constant flow rate of 70 mL / s. At speeds above 10K rpm, particle sizes begin to increase and their size distribution also increases. This phenomenon can be attributed to the so-called “bridged flocculation” of particles, when the long chain polymer molecules are adsorbed on the surfaces of the particles by any bond between electrostatic, hydrophobic, van der Waals, covalent or more likely hydrogen. The polymer binds, via relatively few sites, to the particles leaving long loops and tails that extend into the vicinity of the liquid phase. Increasing the concentration of the emulsifier can prevent this phenomenon and decrease the droplet size when the speed increases.
The results show the influence of the process parameters in the droplet size distribution, da, 2, d4.3, in the Amplitude when silicone wax particles were stabilized by means of the mentioned emulsifiers. Comparative Example 4 - Preparation of colloidal dispersions of silicone wax using high pressure homogenizer
The same raw materials as in Example 3 were used. Emulsions were prepared with deionized water and up to 1% emulsifier as the continuous phase, and 5% silicone wax as the dispersed phase. The silicone wax was melted at about 80 ° C-90 ° C. The continuous phase was also heated to 80 ° C-90 ° C to match the temperature of the dispersed phase. One sample additionally contained perfume. The dispersed phase was then added to the continuous phase and homogenized at 13,500 rpm for 5-20 minutes using a rotor-stator system (Ultra Turrax T25 basic (IKA-WERKE GmbH & Co. KG, Staufen, Germany) to form a coarse emulsion The coarse emulsion homogenization was carried out in a hermetically sealed double beaker and connected to a water bath to ensure that the temperature was maintained above the wax melting points. After coarse emulsion homogenization, it was immediately further homogenized at 120,000 kPa for approximately 2 cycles using a high pressure homogenizer Microfluidifier M-110S (Microfluidics Internationational Corporation, MA-Newton, USA) The samples were collected in sterile containers and left on the bench for cooling until the samples reached temperature (20 ° C) The flow rate was about 4 to 6 mL per second.
Three emulsions were produced, of which the average particle size was determined. The compositions and results are given in the table below.
Table 7: Composition and average diameter of the dispersed particle of emulsions containing silicone wax, produced using the Microfluidizer

Ingredient sample 1 sample 2 sample 3 water [% w / w] 94 94 91.5 SilCare silicone wax 41M65 [% w / w] 5 5 5 Oil-based perfume [% w / w] 0 0 2.5 Tween emulsifier 20 [% w / w] 0 1 0 PET-POET emulsifier [% w / w] 1 0 1 d3.2 [micrometers] 0.12 0.17 0.28
When comparing the dispersions produced using the CDDM apparatus and the Microfluidizer, the material produced in the CDDM had a final dispersed phase fraction 5 of at least 12 times higher, and a pressure drop 20 to 25 times lower.

权利要求:
Claims (13)
[0001]
1. Method for producing a continuous emulsion in water, in which the dispersed phase of the emulsion comprises a lipophilic compound, and in which the average Sauter diameter of the dispersed phase is less than 1 micrometer, and in which the concentration of the dispersed phase is at least 20% by weight of the emulsion, characterized by the fact that the method comprises the steps of: (a) mixing water and an oil-in-water emulsifier to form an aqueous phase; (b) bringing the lipophilic compound into a liquid form to form a lipophilic phase; and (c) mixing the aqueous phase of step (a) and the lipophilic phase of step (b) in a distributive and dispersive mixing apparatus of the Controlled Deformation Dynamic Mixer or Cavity Transfer Mixer type to create a continuous emulsion in water, and the mixer being suitable for inducing an extensible flow in a liquid composition, and the mixer comprising closely spaced and relatively mobile facing surfaces, at least one having a series of cavities in them, whose cavities, on each surface, are arranged in such a way that, in use, the cross-sectional area for the flow of the liquid increases and decreases successively by a factor of at least 3 throughout the apparatus.
[0002]
2. Method, according to claim 1, characterized by the fact that in step (a) the temperature of the mixture is at most 110 ° C.
[0003]
3. Method according to claim 1 or 2, characterized in that in step (b) the lipophilic compound is brought to a liquid form by increasing the temperature to melt the compound.
[0004]
Method according to any one of claims 1 to 3, characterized in that the lipophilic compound comprises lecithin, fatty acid, monoglyceride, diglyceride, triglyceride, phytosterol, phytosteranol, fatty acid ester, phytosteranil ester of fatty acid, wax, fatty alcohol, carotenoid, oil-soluble dye, oil-soluble vitamin, oil-soluble flavoring, oil-soluble fragrance, oil-soluble drugs, mineral or derivative oils, petroleum jelly or derivatives, or silicon or derivative oils , or combinations of these compounds.
[0005]
Method according to any one of claims 1 to 4, characterized by the fact that the lipophilic compound is selected from the group of phytosterols, carotenoids, and derivatives of these compounds.
[0006]
Method according to any one of claims 1 to 5, characterized in that in step (b) the lipophilic compound is mixed with a non-aqueous phase.
[0007]
Method according to claim 6, characterized in that the concentration of the lipophilic compound that is in the non-aqueous phase is at least 5% by weight, preferably at least 10% by weight, preferably at least 20% by weight.
[0008]
Method according to any one of claims 1 to 7, characterized in that, in a subsequent step, the mixture of step (c) is cooled.
[0009]
Method according to any one of claims 1 to 8, characterized in that the average Sauter diameter of the dispersed phase is less than 500 nanometers.
[0010]
Method according to any one of claims 1 to 9, characterized in that the concentration of the dispersed phase is at least 40% by weight of the emulsion, preferably at least 60% of the emulsion.
[0011]
11. Method according to any one of claims 1 to 10, characterized in that, in step (c), the Controlled Deformation Dynamic Mixer or Cavity Transfer Mixer comprises two facing surfaces (1, 2), spaced apart over a distance (7), where the first surface (1) contains at least three cavities (3), with at least one of the cavities having a depth (9) with respect to the surface (1), where the second surface (2) contains at least three cavities (4), at least one of the cavities having a depth (10) with respect to the surface (2), in which the cross-sectional area for the flow of liquid available during the passage through of the apparatus increases and decreases successively at least 3 times, and the surface (1) has a length (5) between two cavities, and the surface (2) has a length (6) between two cavities, and being the surfaces (1, 2) are positioned in such a way that the corresponding lengths (5, 6) overlap to create a gap having a length (8) or do not overlap creating a length (81), the cavities being arranged in such a way that the cross section area for the flow of the available liquid during the passage through the apparatus successively increases in the cavities and decreases in the cracks by a factor of at least 3, and the distance (7) between the two surfaces (1, 2) is between 2 micrometers and 300 micrometers, and where either the radius between the length (8) and the distance (7) between the two surfaces (1, 2) varies from 0 to 250, or the radius between the length (81) and the distance (7) between the two surfaces (1, 2) ranges from 0 to 30.
[0012]
12. Method according to any one of claims 1 to 11, characterized in that the mixer is operated at a pressure of less than 20,000 kPa.
[0013]
13. Method according to any one of claims 1 to 12, characterized in that one of the surfaces rotates with respect to the other surface at a frequency between 1,000 and 25,000 revolutions per minute.

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同族专利:

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公开号 | 公开日

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ES2524120T3|2014-12-04|

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CN103459008A|2013-12-18|

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EA201300772A1|2014-11-28|

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BR112013016302A2|2018-06-26|

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US9352289B2|2016-05-31|

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EP2658638B1|2014-09-03|

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EP2658638A1|2013-11-06|

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JP5940556B2|2016-06-29|

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EA024947B1|2016-11-30|

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US20140113852A1|2014-04-24|

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JP2014507261A|2014-03-27|

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CN103459008B|2015-08-19|

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CA2821061A1|2012-07-05|

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WO2012089474A1|2012-07-05|

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法律状态:
2018-07-10| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|

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2019-07-02| B06T| Formal requirements before examination [chapter 6.20 patent gazette]|

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2020-04-07| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|

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2020-10-27| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 07/12/2011, OBSERVADAS AS CONDICOES LEGAIS. |

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2021-02-23| B25A| Requested transfer of rights approved|Owner name: UNILEVER IP HOLDINGS B.V. (PB) |

优先权:

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申请号 | 申请日 | 专利标题

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EPEP10197187|2010-12-28|

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EP10197187|2010-12-28|

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PCT/EP2011/072112|WO2012089474A1|2010-12-28|2011-12-07|Method for production of an emulsion|

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