WO2019195361A1 - Traitement d'émulsions de soins personnels par les méthodes de la température d'inversion de phase - Google Patents

Traitement d'émulsions de soins personnels par les méthodes de la température d'inversion de phase Download PDF

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Publication number
WO2019195361A1
WO2019195361A1 PCT/US2019/025495 US2019025495W WO2019195361A1 WO 2019195361 A1 WO2019195361 A1 WO 2019195361A1 US 2019025495 W US2019025495 W US 2019025495W WO 2019195361 A1 WO2019195361 A1 WO 2019195361A1
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temperature
phase inversion
phase
emulsion
personal care
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PCT/US2019/025495
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English (en)
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Kathleen JILLIONS
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Johnson & Johnson Consumer Inc.
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Publication of WO2019195361A1 publication Critical patent/WO2019195361A1/fr

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04—Dispersions; Emulsions
    • A61K8/06—Emulsions
    • A61K8/064—Water-in-oil emulsions, e.g. Water-in-silicone emulsions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q90/00—Cosmetics or similar toiletry preparations for specific uses not provided for in other groups of this subclass
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

Definitions

  • phase inversion temperature methods may be applied to personal care formulations containing a diverse range of raw materials provided there is an ethoxylated nonionic surfactant present.
  • Application of phase inversion temperature methods to personal care formulations can reduce the energy required for manufacture and increase the stability of the formula.
  • Emulsions are a class of dispersions consisting of two immiscible liquids. Emulsions can be found in many areas of practical use including in topical drugs and personal care products in the forms of lotions and cream. These emulsions are most commonly oil-and-water systems (frequently oil-in-water), however silicone-water and silicone-oil systems are also employed. These systems range in droplet size of the dispersed phase from microemulsions at 5 - 50 nm and nanoemulsions of 20 - 100 nm to macroemulsions averaging 1 - 2 mm (Tadros, 2013). Thermodynamic Instability
  • thermodynamics As explained by the second law of thermodynamics (Equation 1), oil-and-water emulsions are neither formed spontaneously nor thermodynamically stable. Due to the immiscibility of the continuous and dispersed phase materials, there exists a surface tension g between droplets of surface area A. For a system to be thermodynamically favorable, the change in free energy G must be negative and the change in configurational entropy S positive.
  • An emulsion may break down by a number of mechanisms as depicted in Figure 1 (Holmberg, Jonsson, Kronberg, & Lindman, 2002). Creaming and sedimentation are mechanisms of destabilization that occur due to density differences between the two phases and are reversible through the application of high shear to the system given that the drops have not yet coalesced. Flocculation, also reversible, is the aggregation of droplets when they remain in close proximity for a much longer time than if there were no attractive forces acting between drops. Flocculation is determined by the magnitude of the attractive forces versus the repulsive forces between the droplets. Coalescence occurs when the
  • Ostwald ripening may also occur. Ostwald ripening is the diffusion of dispersed phase material from smaller to larger droplets due to the chemical potential of the material being higher for a smaller radius of curvature, but will not occur if the solubility of the dispersed phase material in the continuous phase is negligible (Becher, 1996). Thus, Ostwald ripening is determined by the solubility of the disperse droplets in the continuous phase and the particle size distribution as given by equation 2 (Izquierdo P. , et al., 2004).
  • a 0.1 mm oil droplet moves 0.4mm/day
  • a lmm drop moves 40 mm/day
  • a lOmm drop moves 4m/day
  • An emulsion can be stabilized through introduction of a potential energy barrier to slow the rate of the droplet movement through the continuous phase, providing a kinetic stability for the emulsion system.
  • a potential energy barrier to slow the rate of the droplet movement through the continuous phase.
  • Droplets can be made stationary within the emulsion system by reducing the rate of their movement.
  • the rate of movement through the system rate is proportional to the density differences between the phases, the square of the droplet radius, and the inverse of the viscosity of the continuous phase. Therefore, to stabilize the droplet, any of three approaches can be taken; decrease the density differences between the phases, reduce the droplet radius, or increase the viscosity of the continuous phase.
  • the shielding of droplets so that they deflect from one another prior to touching can be achieved through application of the DVLO Theory and through the use of electrostatically and sterically stabilizing ingredients.
  • the DLVO theory explains the competition between the van der Waals attractive forces and the double-layer repulsive forces that determine the stability of a dispersed system.
  • the small and large distances between the particles are dominated by the attractive forces while the repulsive forces may dominate if the surfaces are highly charged and the electrolyte concentration is not too high in the continuous phase.
  • Born repulsive forces cause strong repulsion due to the overlapping electron clouds, thus preventing the particles from touching. Due to the high sensitivity of the electrostatic stabilization to electrolyte concentration, this method does not have many practical applications.
  • the continuous phase must be a
  • a surface-active agent is any compound that reduces the interfacial tension between two liquids, a liquid and vapor, or a liquid and solid (Hawley, 1977).
  • a surfactant is an amphiphilic molecule that, in aqueous solutions, is typically described as having a polar head group and a nonpolar tail ( Figure 3), providing the molecule its dual nature (Sinko, 2011).
  • Surfactant molecules aggregate in solution to form micelles in an effort to remove hydrophobic groups from contact with water.
  • micellization reduces the free energy of the system by exposing the hydrophilic surface to the water present in the system and trapping the hydrophobic group within this hydrophilic micelle (Holmberg, Jonsson, Kronberg, & Lindman, 2002).
  • the surfactant polar group may be ionic or non-ionic and are classified by this polar group.
  • Non-ionic surfactants are the second largest class of surfactants (behind anionics) and are simple to formulate due to their general compatibility to other ingredients. They are typically compatible with all other surfactants, are not sensitive to hard water, and are not noticeably affected by electrolytes.
  • Within this surfactant group are ethoxylated non-ionic surfactants whose physicochemical properties exhibit a distinct temperature dependency. Ethoxylated non ionic surfactants become more hydrophobic with increased temperatures, a property that enables phase inversion as discussed in later sections.
  • Figure 4 provides the structures of some representative and commonly employed ethoxylated non-ionic surfactants (Holmberg, Jonsson, Kronberg, & Lindman, 2002).
  • the Critical Micelle Concentration or CMC Critical Micelle Concentration
  • Amphiphilic molecules in solution have a tendency to collect at an interface where the hydrophobic groups can be at least partially removed from the contact of water and the hydrophilic groups can remain wetted to reduce the system free energy. This drive to reduce system free energy drives the organization of surfactant monomers into organized structures such as micelles once a critical concentration of surfactant in the system has been reached, a point known as the Critical Micelle
  • CMC Concentration
  • the CMC of a system is strongly dependent on the alkyl chain length of the surfactant as this property determines the degree of hydrophobicity of the molecule.
  • the radius of a micelle is approximately the length of the
  • An emulsifier is a surfactant that assists in creating an emulsion.
  • Surfactants aid in the fine dispersion of either oil droplets in water or vice versa. By trapping the drops in the center of the micelles, the free energy of the system is reduced and the drops are electrostatically and sterically stabilized as illustrated in Figure 2.
  • the surfactant In order to create an emulsion, the surfactant must reduce the oil-water interfacial tension to favorably low values and, critically, it must rapidly diffuse to the newly created interface. The emulsion will only be stable against coalescence if the new interface is rapidly covered by a surfactant monolayer, making low molecular weight surfactants superior in emulsion formation. Impact of Surfactants on Emulsions
  • Bancroft s Rule determines the inner phase of the emulsion and may be expanded by the Hydrophilic-Lipophilic Balance Rule.
  • the stability of the emulsion is determined by the surfactant’s ability to diffuse to the droplet interface and the size of the droplets, as discussed above.
  • Bancroft the phase in which the stabilizing agent (i.e ., emulsifier) is more soluble is the continuous phase.
  • an oil and water emulsion system containing a water-soluble emulsifier will be an oil-in-water emulsion, due to the preferential curvature of the oil/water interface (Davies, 1957).
  • determination of the continuous phase also depends upon the relative proportions of the phases, as it is problematic to create an oil-in-water emulsion if the former is greatly in excess of the later even with highly hydrophilic surfactants. This rule follows with the Gibbs-Marangoni effect, as exhibited in Figure 6.
  • Surfactant in the continuous phase absorbs at the droplet surface resulting in a gradient of surfactant and interfacial tension.
  • Bancroft’s rule can be quantitatively expanded by the Hydrophobic-Lipophilic Balance (HLB) concept.
  • HLB Hydrophobic-Lipophilic Balance
  • the HLB concept is used to determine the relationship between surfactant hydrophilicity and function in solution (Holmberg, Jonsson, Kronberg, & Lindman, 2002).
  • the HLB numbers can be determined through simple calculations (Equations 3-7):
  • the HLB number of a surfactant is based on the relative percentage of hydrophilic to hydrophobic groups in the surfactant molecules and provides a scaled rating of how hydrophilic the surfactant is. This number can then be used to apply Bancroft’s rule and determine if the surfactant will partition in the oil or water phase of the emulsion system, ultimately determining the continuous phase.
  • Emulsions in personal care and OTC products are typically employed as lotions, creams, and conditioners delivering a multitude of benefits such as drug delivery (sunscreens, topical steroids, etc) and moisturization (conditioners, moisturizing lotions, etc).
  • These formulas are most often oil-in-water emulsions with the number of ingredients ranging anywhere from ten to over twenty unique ingredient additions.
  • water comprises 60 - 80 w/w% of the formula, 15 - 30 w/w% oil phase ingredients, 1-2 w/w% emulsifier, and the remainder made up of fragrances, claims ingredients, and preservatives.
  • The“standard” emulsification process for personal care products is a two-pot, high energy process: (1) Heat the water and oil phases separately to 70-80°C with mixing until phases are homogeneous, (2) Combine phases with high in-tank mixing, (3) Homogenize at 70-80°C for three theoretical passes, (4) Cool to 25-30°C, (5), Add volatiles such as fragrance and preservative.
  • This standard manufacturing process requires a large amount of energy to maintain system temperatures and to apply the amount of mixing required to reduce the droplet size and produce a kinetically stable emulsion.
  • U.S. Published Application No. 20140371332 to Kao Corp. discloses a method for producing a vesicle composition having an aqueous phase as a continuous phase that includes (1) preparing an oil phase by dissolving oil phase containing components at a temperature of equal to or higher than the melting point of the oil phase; (2) emulsifying the oil phase by adding an aqueous phase to the oil phase while mixing; and (3) cooling the obtained composition after emulsifying.
  • U.S. Patent No. 5,362,418 to Kao Corporation discloses a process for preparing a gel-like emulsion for use in cosmetic applications that comprises adding an oil to a surfactant continuous phase formed of a monoalkyl phosphate salt, polyhydric alcohol and water.
  • phase inversion temperature of an oil-and-water emulsion is the temperature at which there is a spontaneous exchange between the dispersed phase and the continuous phase of the emulsion; ie. an oil-in-water emulsion becomes a water-in-oil emulsion (Tadros, 2013). This inversion is inevitable and inherent to the formulation.
  • phase inversion of an oil-and-water emulsion requires the presence of a non-ionic, ethoxylated emulsifier.
  • the emulsifier partitions at the interface between the dispersed and continuous phases with the poly(ethylene oxide) chain in the aqueous phase and the alkyl chain in the oily phase (Izquierdo P. , et al., 2002).
  • the water-soluble non-ionic surfactant changes to oil-soluble, reversing the micelle formation in a three-phase region where the oil, surfactant, and water phases are at equilibrium (Shinoda & Saito, 1968). With continued increase of temperature, the formula will invert, with the continuous phase becoming the dispersed phase.
  • phase inversion temperature the oil, surfactant, and water phases are at equilibrium, thus, the surface tension between the dispersed and continuous phase is at a minimum. Due to the low surface tension, energy directed at the formula at this temperature has a greater affect on the particle size of the droplets than energy applied at another temperature as it does not have to first be expended on overcoming the surface tension.
  • the HLB concept can be used to determine if an emulsion system will be an oil-in-water emulsion or a water-in-oil system, but this classification only holds true at room temperature for ethoxylated non-ionic surfactants as the properties of this class of surfactants are tremendously temperature dependent. With increasing temperature, the interaction between the oxyethylene groups and the water phase weakens, leading to a decrease in spontaneous droplet curvature with increased temperature, as can be seen in Figure 7. At low temperatures, the spontaneous curvature (Ho) is positive. As the temperature is increased, an intermediate temperature is reached where the spontaneous curvature is zero and the surfactant is said to be‘balanced’. This temperature is identified as the HLB or phase inversion temperature (Holmberg, Jonsson, Kronberg, & Lindman, 2002).
  • the hydrophobicity of the ethoxylated non-ionic surfactant changes with increased temperature, promoting the phase inversion. This change can be observed through the work by Friberg and team in Figure 8. Moving from left to right (A to E), the phase diagrams show the change in solubility of a short-chain ethoxylated non-ionic surfactant with increasing temperature. As the temperature increases from A to E, the surfactant shifts from hydrophilic to
  • amphiphilic to hydrophobic This change facilitates and promotes the phase inversion of the system with increased temperature.
  • phase inversion temperature can be varied by the chain length of the ethoxylated non-ionic surfactant used in the system. Longer chain length surfactants require greater temperature increase to induce phase inversion due to the increase in number of sites that must be hydrophobically modified.
  • phase inversion temperature In the earliest published studies by Shinoda on phase inversion temperature, the effect of hydrophilic chain length of the emulsifier on phase inversion temperature was shown. As can be seen in Figure 9, as the chain length increases, so does the phase inversion temperature. Similarly, the concentration of the surfactant may have an effect on phase inversion temperature dependent on the system. In Figure 9, it can be seen that the phase inversion temperature plateaus after a given concentration in a benzene-water emulsion but for a hexadecane-water emulsion ( Figure 10), the phase inversion temperature increases to a maximum between 1.5 - 2 wt% before decreasing.
  • phase inversion temperature of the emulsions in different oil- water systems. This is due to the large effect that the HLB of the oils and overall system have on the phase inversion temperature.
  • the increased concentration correlates to a decrease in HLB or phase inversion temperature, reinforcing that each system is unique.
  • Shinoda introduced the“Emulsification by PIT Method” in 1969.
  • the process is defined as placing the ingredients in an ampoule and shaking the system at (ideally) 2° - 4°C below the inversion temperature to achieve a fine dispersion.
  • the system is then cooled rapidly through the use of an ice bath to storage temperature to slow the coalescence rate.
  • the system is a three- component system comprised of water, oil, and non-ionic surfactant (Shinoda & Saito, The Stability of O/W Type Emulsions as Functions of Temperature and the HLB of Emulsifiers: The Emulsification by PIT-method, 1969).
  • Processing emulsions through phase inversion temperature methods has the ability to produce emulsions of finely dispersed droplets in a continuous phase with significant energy savings due to the low energy mixing requirement and reduce emulsification temperatures (Preziosi, Perazzo, Caserta, Tomaiuolo, & Guido, 2013).
  • the phase inversion of a water-and-oil emulsion containing a non-ionic ethoxylated surfactant is driven by the change of the surfactant’s hydrophobicity with increased temperature.
  • water-in-oil droplets are first produced. With addition of the full quantity of water, the droplets merge together as the system reaches the HLB point and the surface tension minimum is reached. As the system is cooled the hydrophobicity of the surfactants changes and oil-in-water micelles are formed. In an emulsion formed through mechanical methods, addition of oil to the water- surfactant system simply causes growth of the oil-in-water micelles whose size are modulated by mechanical energy only.
  • the phase inversion temperature of an emulsion may be identified through measurement of surface tension, viscosity, or, most commonly, conductivity as a function of temperature. For each method, it is essential to measure the phase inversion temperature of the emulsion as a whole with all other ingredients, not just the phase inversion temperature of the emulsifier (Tadros, 2013). This is particularly critical in personal care formulations due to the large number of formulary constituents that may affect the inversion temperature.
  • phase inversion temperature was introduced by Shinoda an Arai, who cited conductivity as the method of identification (Shinoda & Arai, The Correlation between Phase
  • phase inversion temperature is identified as the average temperature value between the minimum and maximum conductivity points (Izquierdo P. , et al., 2002).
  • the resulting temperature curve exhibits the temperature dependency of the electrical conductivity of the emulsion ( Figure 14, ). As the inversion is temperature dependent and spontaneous, the emulsion will invert back to the original state as the system is cooled.
  • Identification of the phase inversion temperature may be reinforced through constant viscosity measurement while heating the formula and measuring conductivity.
  • a rheomixer device is used.
  • the rheomixer device consists of a jacketed vessel and an impeller connected to a rheometer.
  • the vessel is placed on a rotating turntable and the impeller and conductivity cell are inserted at a fixed position.
  • the impeller is able to measure the viscosity of the emulsion system through relative motion with respect to the contents of the vessel and the torque-rotational speed data is analyzed to determine the viscosity.
  • Figure 15 depicts this set-up.
  • phase inversion temperature is identified as the viscosity minimum and confirmed by the simultaneous conductivity measurements, as seen in Figure 16 (Allouche, Tyrode, Sadtler, Choplin, & Salager, 2004).
  • Emulsions formulated for personal care products contain a relatively large number of materials that may affect the phase inversion temperature of the formula or the methods required to manufacture the formula at a sufficient size for supply chain planning. As discussed in the testing section, it is essential to test the entire formula, not just the emulsifier, to determine the phase inversion temperature of the system. Due to system interactions, it is likely for two different formulations employing the same emulsifier to have differing phase inversion temperatures due to the HLB values of other raw material ingredients. Additional complications arise when multiple and/or high concentrations of ethoxylated non ionic surfactants are employed in the same formula.
  • the combination of surfactants is capable of shifting the phase inversion temperature, causing a potential lack of continuity in conductivity curves, or cause the formulation to never fully invert.
  • Multiple ethoxylated non-ionic surfactants in the formula shifts the HLB of the
  • surfactant may be attributed to the
  • the expected curve is one similar to Figure 14, where the conductivity plateaus then drops to zero at the phase inversion temperature.
  • the plateau indicates the area of low surface tension while the lack of inversion displays the impact of complex formulations on phase inversion.
  • phase inversion temperature of the daily moisturizing lotion used as example in Figure X above is above l00°C and is the reason we are not seeing the catastrophic inversion of the formula and drop of conductivity to zero.
  • chain length of the emulsifier impacts the phase inversion temperature.
  • phase inversion temperatures that are at or below storage temperature of the product.
  • the phase inversion temperature should be at least 20°C greater than the storage temperature (Tadros, 2013), in order to prevent inversion of the product in the package while being stored. If the product were to be exposed to temperatures above the phase inversion point in storage, the product may invert in the package and, without any mixing while the product is cooled, may separate resulting in product complaints. Further concerns may arise in production
  • phase inversion temperature is near the processing or filling temperature as the product may not form the desired micelle structure prior to packaging.
  • the phase inversion temperature process is, academically, defined as emulsifying at the phase inversion temperature and rapidly cooling to room temperature to achieve a nanoemulsion.
  • this process theory may be applied to personal care emulsions provided they contain an ethoxylated nonionic surfactant.
  • the complications arise when applying this method in manufacturing settings where volumes and equipment impact the ability to apply this method as described for academic studies. In a manufacturing setting, it is simple enough to emulsify at the phase inversion temperature, but it is often incredibly difficult to rapidly change the temperature of the batch due to the large volumes of bulk in each batch process.
  • The“standard” processing method for emulsions is a high energy process due to the heat, shear, and time that are involved. These processes leave much to be desired from a sustainability lens and manufacturing site efficiencies, thus application of processes that may reduce the time and energy required to produce a stable product is highly favorable. Through the application of phase inversion temperature methods, reduced emulsification temperature, reduced mixing requirements, and reduced batch cycle times are possible.
  • emulsification temperature may be reduced.
  • a reduced emulsification temperature results in less time and energy required to heat the batch to the emulsification temperature, less energy to maintain that temperature during the emulsification mixing step, and less time and energy to cool the batch to a safe discharge temperature (typically 25-35°C). While seemingly insignificant for smaller scale batches, the time required to heat a batch over 5,000kg l0°C is significant, often hours.
  • the typical manufacturing vessels for these batches are stainless steel jacketed kettles employing heating fluid in the jacket to control the batch temperature. Reducing the emulsification temperature for processing of the formula to the phase inversion temperature is also favorable as the process has the potential to create a reduced droplet size. As previously discussed, the surface tension at the phase inversion temperature has been reduced to a minimum and therefore the energy input to the system is directed primarily to reducing the emulsion droplet size. If the same amount of shear energy is put in to the system at the phase inversion temperature as when it is processed at the standard emulsification temperature, then the droplet size of the phase inversion method batch will be smaller. A reduced droplet size is favorable to the increased kinetic stability of the emulsion.
  • a concern that may be raised when evaluating formula process improvements is the high melting temperature of commonly used raw materials.
  • Many personal care emulsions include waxes with melting points above 65°C and sunscreens that require both heating and homogenization to reduce particle size and ensure product efficacy.
  • the required raw materials may be melted in their respective phases and the phases cooled to the phase inversion temperature prior to emulsification.
  • phase inversion processing methods are applied as part of a capital improvement project, application of the same amount of shear in processing could change the aesthetics of a commercially available product and impact the product used by the consumer, potentially driving complaints and a decrease in sales. If, however, the phase inversion processing methods are applied during development of the formula, the product produced and commercialized has the potential to be the most stable form of the formula. Alternatively, application of phase inversion processing methods may provide formulators an option for producing a product with drastically different aesthetics with minimal formulation changes, for example, turning a pump lotion into ajar cream.
  • the shear energy applied at the emulsification step should be reduced.
  • an equivalent droplet size to the emulsion produced by standard methods may be achieved.
  • Reducing the shear energy applied to the system not only reduces the cost to produce the batch and increases the environmental sustainability of the product, but could reduce batch cycle time.
  • the reduction of shear energy during manufacturing may be done through reduction of mixing speeds, but more commonly would be done by reducing or removing the homogenization time at emulsification.
  • Standard manufacturing processes include homogenization for three theoretical passes of the batch through the recirculation loop immediately following the emulsification.
  • This homogenization step requires a large amount of energy to keep the batch at high
  • phase inversion temperature processing methods may be applied through a“one-pot” process.
  • One-pot processes reduce the number of manufacturing kettles required and thus the overall cycle time by reducing the number of kettles that must be cleaned.
  • oil and oil soluble ingredients hydrophobic and amphiphilic
  • Water is warmed to a sufficient temperature that, when combined, the system is within the phase inversion temperature range.
  • this may look like heated the oil phase that comprises 30 wt% of the formula to 75-80°C and the water (65 wt% of the formula) to 55- 60°C for a phase inversion temperature range of 60-65°C.
  • the water quench would bring the batch to a temperature near or within the phase inversion temperature range to be further modulated by the temperature control on the manufacturing kettle.
  • the formula minus the volatile ingredients combined, the batch is then mixed until a homogeneous emulsion is formed.
  • the batch is then cooled to near room temperature, volatiles are added, and the batch is discharged. Utilizing this process, energy and cycle time may be further reduced from processing involving two manufacturing kettles.
  • phase inversion temperature method processes to the manufacture of personal care products has the ability to shorten batch cycle times, reduce energy requirements, and, ultimately, increase company profitability. Reduced cycle times through quicker batch times and fewer manufacturing kettles to clean result in manufacturing sites being able to increase capacity and produce more product. This increase in production in turn enables an increase in product sales and profitability.
  • An added bonus, the ability to reduce manufacturing kettles and energy used in batch production increases a company’s sustainability profile. In a market where sustainable practices are highly favored, a company that can show the consumer that they are a “green” company increases customer favorability and, thus, drives sales and profitability.
  • Dispersions of the Ternary system Composed of Water, Cyclohexane, and Nonionic Surfactant. Journal of Colloiud and Interface Science, 70-74.
  • emulsions prepared by the phase inversion composition method Preparation variables and scale up. Journal of Colloid and Interface Science, 417-423.
  • Varvaresou A., Papageogiou, S., Tsirivas, E., Protopapa, E., Kintziou, H., Kefala, V., & Demetzos, C.

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Abstract

L'invention concerne l'utilisation de méthodes d'inversion de phase pendant la production d'émulsion de soins personnels pour produire des émulsions de soins personnels durables.
PCT/US2019/025495 2018-04-03 2019-04-03 Traitement d'émulsions de soins personnels par les méthodes de la température d'inversion de phase WO2019195361A1 (fr)

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