Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q19/00—Preparations for care of the skin
• • 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
  • A61K8/066—Multiple emulsions, e.g. water-in-oil-in-water
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
  • B01F23/40—Mixing liquids with liquids; Emulsifying
  • B01F23/41—Emulsifying
  • B01F23/414—Emulsifying characterised by the internal structure of the emulsion
  • B01F23/4144—Multiple emulsions, in particular double emulsions, e.g. water in oil in water; Three-phase emulsions
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
  • C11D17/0017—Multi-phase liquid compositions
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0047—Detergents in the form of bars or tablets
  • C11D17/006—Detergents in the form of bars or tablets containing mainly surfactants, but no builders, e.g. syndet bar
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
  • A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q5/00—Preparations for care of the hair

Definitions

• the present invention relates to three-phase emulsion systems and cosmetic compositions/personal wash preparations containing such emulsions.
• the invention relates to a rinse-off composition based on a three-phase emulsion system.
• the compositions according to the invention are most effective for the delivery and deposition of one or more functional ingredients on skin or hair.
• the invention also relates to a process for preparing the cosmetic/personal wash compositions of the present invention.
• the use of functional ingredients in cosmetic compositions in order to deposit them on skin and/or hair treated therewith, is common.
• the common functional agents include perfumes, germicides, sunscreens and other cosmetic agents to provide specific consumer perceivable benefits.
• Silicone oils usually linear poly(dimethyl siloxane) polymers of varying chain lengths and viscosities, are also employed as benefit agents for skin, hair and fabric.
• the deposition of these cosmetic agents onto the substrates is aimed through leave-on or rinse-off cosmetic formulations.
• the problem of depositing the functional ingredients, particularly the ones which are surfactant soluble such as organic sunscreens onto the substrates especially through rinse-off cosmetic products is very pertinent as these get washed off when the composition is rinsed off.
• European Patent Specification 386 898 discloses aqueous shampoo compositions comprising anionic surfactant, a water- insoluble sunscreen material and a cationic polymer. The cationic polymer improves deposition of the sunscreen material onto treated hair, although not very significantly.
• EP 0281 394 granted to Richardson-Vicks relates to a three phase emulsion of the type oil-in-water-in-silicone oil, where glycol modified silicone is used as the emulsifier for the water-in-silicone oil part of the multiphase emulsion.
• This emulsion is a well-defined multiple emulsion prepared by a two-stage method where a separate high HLB emulsifier is needed to first prepare the oil-in-water emulsion which is subsequently dispersed in the silicone oil by using a glycol modified siloxane.
• the procedure and the well defined character of the emulsion demand that a certain minimum amount of water be present and examples quoted therein show as high as 64% water content .
• EP 0552 024 describes a cosmetic composition for enhanced deposition of Parsol MCX from cleanse-off application.
• This patent relates to an oil-in-water emulsion where the oil phase has Parsol dissolved in it.
• the requirement that Parsol be dissolved in the oil phase puts a restriction on the selection of the oil phase.
• the emulsion described is necessarily oil-in-water emulsion.
• oils oilj + oil 2
• water with high internal phase
• a three-phase emulsion system comprising from 2% to 30% by wt. emulsifier; from 20% to 80% by wt . one or more oil-based functional ingredients, from 2% to 30% by wt. emulsion; from 20% to 80% by wt. one or more oil-based functional ingredients, from 20% to 80% by w . silicone oil and from 0.1 to 30% by wt . water, said emulsion being in a water continuous or oil-continuous form.
• the invention provides a method for preparing the three-phase emulsion as described above, comprising mixing an emulsifier with one or more functional ingredient, adding silicone fluid to the mixture, blending the mixture in a high shear mixer, adding water during the mixing to obtain the emulsion.
• the silicone oil particularly alkyl siloxanes and more particularly polydimethyl siloxanes is compatibilized with organic sunscreens such as Parsol MCX (a registered trade name of Givaudan Roure) and chemically 2-ethyl-hexyl-methoxy cinnamate by way of locking the two in an emulsion.
• organic sunscreens such as Parsol MCX (a registered trade name of Givaudan Roure) and chemically 2-ethyl-hexyl-methoxy cinnamate by way of locking the two in an emulsion.
• Both water-in-oil and oil-in-water emulsions can be prepared. Diversity of application to product form can be achieved by altering the viscosity of the emulsion.
• the efficiency of deposition of the active even after the composition is rinsed off is four or five times superior to that achieved by the invention described in the prior art (EP 0 552 024) .
• the emulsion containing the functional ingredient is incorporated into the
• the invention provides rinse-off cosmetic compositions in particular soap bars and gels including the three-phase emulsions of the invention and method of preparation of such compositions.
• the enhanced deposition is owing to a synergistic effect since silicone oil by itself does not have any UV absorbing character.
• the three phase emulsions containing the functional ingredients are added to the ingredients of the personal wash products.
• the presence of the emulsion containing the functional ingredients results in enhanced deposition of the functional ingredient onto skin and/or hair from wash/rinse-off/cleansing products.
• the cosmetic composition prepared by incorporating the novel emulsion system has a synergistic effect in the enhanced delivery of the functional ingredients.
• the cosmetic compositions referred to may be in the form of gels or plodded soap bars with the emulsion containing the cosmetic agent forming stripes.
• the cosmetic agent may be present as stabilised droplets (50 ⁇ ) prepared by casting the bars or may be present as a homogeneous emulsion in the composition.
• the functional ingredient may be any surfactant-soluble material (liquid or solid) intended to be deposited onto the hair or skin for the purpose of imparting functional benefits thereto.
• the functional ingredient may moisturise, condition and/or protect the skin and/or hair.
• Preferred functional ingredients include:
• waxes such as carnauba, spermaceti, beeswax, lanolin and derivatives thereof; b. hydrophobic plant extracts; c. hydrocarbons such as squalene and squalane; d. higher fatty acids such as those having at least 12 carbon atoms, for example, lauric, myristic, palmitic, stearic, behenic, oleic, linoleic, linolenic, lanolic, isostearic and polyunsaturated fatty acids (PUFA) acids; e.
• PUFA polyunsaturated fatty acids
• higher fatty alcohols such as those having at least 12 carbon atoms, for example, lauryl, cetyl, stearyl, oleyl, behenyl, cholesterol and 2-hexadecanol alcohol; f. esters such as cetyl octanoate, lauryl lactate, myristyl lactate, cetyl lactate, isopropyl myristate, myristyl myristate, isopropyl palmitate, isopropyl adipate, butyl stearate, decyl oleate, cholesterol isostearate, glycerol monostearate, glycerol distearate, glycerol tristearte, alkyl lactate, alkyl citrate and alkyl tartrate; g.
• essential oils such as fish oils, entha, jasmine, camphor, white cedar, bitter orange peel, ryu, turpentine, cinnamon, bergamon , citrus unshiu, calamus, pine, lavender, bay, clove, hiba, eucalyptus, lemon, starflower, thyme, peppermint, rose, sage, menthol, cineole, eugenol, citral, citronelle, borneol , linalool, geraniol, evening primrose, camphor, thymol, spirantol, pinene, limonene and terpenoid oils; h.
• essential oils such as fish oils, entha, jasmine, camphor, white cedar, bitter orange peel, ryu, turpentine, cinnamon, bergamon , citrus unshiu, calamus, pine, lavender, bay, clove, hiba, eucalyptus, lemon, starflower, th
• lipids such as cholesterol, ceramides, sucrose esters and pseudo-ceramides as described in European Patent Specification No. 556 957; i. vitamins such as vitamins A and E, and vitamin alkyl esters, including vitamin C alkyl esters; j. sunscreens such as octyl methoxyl cinnamate (Parsol MCX) and butyl methoxy benzoylmethane (Parsol 1789); k. Phospholipids; and 1. derivatives of alpha hydroxy acids such as materials of formula
• R 2 - O R 1 - [O - CH - C] m OR 3 wherein, R 1 is C p H q N r O ⁇ , where P is 0-20, q is 1-41, r is 0-3, and
• R 2 is C C H U , where t is 0-20 and us is 1-41;
• R 3 is C ⁇ O y , where v is 0-20, w is 1-41, x is 0-3 and y is 0-3 or a metallic, ammonium or alkanolammonium anion; and
• m is 1-10;
• m. perfumes; and n mixtures of any of the foregoing components.
• the functional ingredients are present in the emulsions preferably in amounts of from 20% to 80%, more preferably from 40% to 60%.
• Silicone oils have the following formula
• the silicone oil is present in the emulsion preferably in an amount of from 20% to 80%.
• Water is incorporated as the third phase of the three-phase emulsions and may be incorporated in one or more stages during emulsifications .
• Water is present in the emulsion in amount of between 0.1% to 30%, more preferably from 5 to 15%.
• the relative proportions of the siloxane groups and the polyol groups in the copolymer determines the character of the emulsion that can be obtained.
• DC 190 has a lower glycol content that DC 193 and hence leads to water as the internal phase in the emulsions.
• DC 190 and DC 193 are brand names of Dow Corning in respect of the aforesaid siloxanes.
• the emulsifiers are present in the emulsion preferably in amounts from 2 to 30% by w . , more preferably from 5 to 15% by wt .
• the emulsifiers are first dispersed in one or more functional ingredient and slightly heated, if required. This is followed by addition of silicone oil and mixing in a high shear mixer such as the ones available from Silverson. Water and minor additives are then added slowly while mixing is continued. As water is added, the viscosity starts building up and the required consistency of the emulsion is obtained.
• a simple one-step mixing procedure can be used to prepare a three-phase emulsion (hereinafter referred to as Parsol-Silicone-Emulsions [PSE] ) .
• the character of the emulsion was tested by dispersing a small drop of the emulsion in test tubes containing water and oil phases separately.
• the emulsion can be easily dispersed (and hence diluted) in a medium which constitutes the external phase whereas if forms lumps in the other fluids.
• a typical water continuous PSE formulation is as follows
• a typical oil continuous PSE formulation is as follows
• the minors will include:
• particulates such as ppt. silica, talc and high HLB non-ionics preferably the ones which form liquid crystalline phases at interfaces, such as the ethoxylated stearyl alcohol, e.g., Brij 72/BVrij 721 (registered trade mark of TCI) .
• the emulsions themselves offer synergy by combining the benefits of sunscreen and silicone oil. They may be used as such (without further incorporation into a product) as a pre-wash/cleansing cream which is applied on face and later washed off leaving the sunscreen on the face.
• the three-phase emulsions of the invention containing the functional ingredients may be used in personal washing bars and gels.
• PSE' s may be incorporated into gel type products in the form of stripes, and into soap bars either in the form of stripes (for plodding route) or as big droplets (for casting route) .
• Parasol MCX alone cannot be striped on gels and bars and also runs the risk of getting solubilized by the surfactant micelles during application of the product.
• silicone oil alone cannot be stabilized in the form of large droplets while Parsol alone does not give the desired substantivity. Large drops of PSE' s are easy to stabilize in the soap melt.
• synergistic benefits can be obtained by combining Parsol and silicones in the form of PSE' s not only in terms of depositing Parsol but also in terms of the ease of processing.
• Silicone oils poly dimethyl siloxanes
• Glycol modified siloxane surfactants DC-193 and DC-190
• Dow Corning (USA) and Parsol MCX cosmetic grade sunscreen were used.
• the emulsifier (10 gms) was mixed in Parsol MCX (50 gms) in a 150 ml glass beaker and then silicone fluid (60 gms) was added to the mixture.
• the mixture was heated to about 50°C in a water bath and then subjected to high shear mixing on Silverson mixer. When the mass became somewhat uniform on a macroscopic scale, the required amount of water (typically 10 gms) was added slowly while mixing in the Silverson was continued. As the water was added, a sudden build-up in the viscosity of the mass was observed with the whitening of the mass. This indicated the onset of emulsification. Mixing was continued for another 5 minutes to homogenize the emulsion.
• the emulsion nos. 1 to 6 of Table 1 will lead to an internal phases of ⁇ 100 gms on an external phase of only 10 gms if water forms the continuous phase. Hence they come under the category of high internal phase emulsions (HIPE's) in which the internal phases are no longer in the form of discrete droplets. They are instead deformed and pressed against one another. Since the system has already passed the limit of internal phase that can be accommodated assuming hard sphers ( ⁇ 74%) , the viscosity is extremely high. These emulsions offer excellent materials for striping Parsol-rich material on gel type products.
• HIPE's high internal phase emulsions
• the emulsions are easily dispersed in bulk water indicating that the continuous phase is water. However, since the total amount of water is very small (10%) , their structure will look like the one shown in the schematic of Figure 1 with the oil phase consisting of two components (Parsol and Silicone) . The emulsions being very thick, they cannot be examined under an optical microscope as such. Therefore, they were diluted 20 times before looking at them under the microscope.
• Figure 2 shows a microscope picture at 400 magnification. Two distinct type of oil droplets can be seen in the picture which might be interpreted to correspond to two oil phases.
• Figure 3 shows a typical droplet size distribution for these emulsions obtained by dispersing a small amount of the emulsion in water and counting the droplets on a Coulter Multisizer.
• the average droplet size is seen as ⁇ 15 microns and the distribution is quite broad.
• the character of a high internal phase emulsion gets significantly altered once it is diluted since there is no inter-droplet interaction or dense packing left after dilution. A fast coalescence may lead to over-estimation of the droplet size by this technique.
• Adding cationic polymer Jaguar at 1% level to the water phase helps stabilize the emulsion at room temperature but it worsens the stability at high temperature.
• most of our emulsions have passed the stability criterion by centrifugation method.
• DC 190 has a relatively lower glycol content in the silicone glycol copolymer, and is more suitable for making an oil- continuous emulsion.
• a typical recipe is given below:
• FIG. 4 shows an optical microscope picture of an oil-continuous PSE taken without any dilution.
• the slide was prepared by putting a drop of the emulsion onto the slide, cover it with a cover slip and pressing it hard with thumb.
• the continuous oil phase spreads into irregular domains with the two types of droplets dispersed in them. On the whole, the picture exhibits a very different character than the one in Figure 2.
• a typical transparent soap formulation containing 30% soap, 40% polyols, 20% water and 10% ethyl alcohol was taken.
• a 2 kg batch of melt was prepared, cast into moulds, and tablets were cut out on solification. Later, a few of these were remelted and cooled to a lower temperature around 50°C) while continuously stirring the mass not to allow localized solidification. This was done to achieve a higher viscosity of the melt which facilitates the stabilization of droplets.
• an appropriate amount of PSE was added to the viscous (but still liquid) mass.
• the system was homogenized by gently stirring by hand for about 5 minutes and then cast in pre-cooled moults (kept in refrigerator) . Bars were cut after solidification.
• Samples of emulsion nos. 7 to 10 according to the invention were prepared, as in Example 1 but using the appropriate amounts of ingredients, and these are shown in Table 4.
• Emulsion no. 7 was injected at -1% level to give stripes on a 55 TFM soap formulation.
• the procedure involved prewashing the forearms, applying 20 to-and-fro rubs of the experimental soap on one inner forearm, lathering for -10 seconds, rinsing, and drying by tapping paper towel. Similar application of the control was carried out on the other forearm. This was followed by the extraction of the deposited Parsol MCX using 400 microlitres of ethanol from 9 cm 2 are marked on each forearm, and determining the amount of Parsol using UV. The results are shown in Table 5. The results clearly indicate that the deposition from the striped bar prepared as per the invention is significantly higher than from the control bar at 99% statistical confidence level.
• the control bar has both Parsol and Silicone in the same proportions as in the striped bar but without emulsification. This clearly shows the benefit of the two ingredients being locked together in the form of PSE coupled with the striping. This kind of deposition figures from striped bars have not been obtained earlier.
• Table 6 shows the deposition of Parsol MCX respectively from melt-cast-bars containing 2% Parsol incorporated (i) as neat (sample No. MCB-13) , (ii) via a water-continuous emulsion, being emulsion no. 9 (sample no. MCB-14), and (iii) ia oil- continuous emulsion, being emulsion no. 8 (sample no. MCB- 15) .
• the measurements were made by making a 1% solution of the soap bars in water, applying 100 microlitres of this solution on the forearms of the subjects, and then following similar procedure as described. From the deposition values it follows that:
• the deposition figures are further improved significantly when Parsol is incorporated as PSE, whether water-continuous or oil-continuous, implying the synergistic effects of the Parsol and silicone being present together in the form of an emulsion. It is significant that silicone alone cannot be stabilized at droplets in the melt. Due to its lower density it quickly float on the top.
• Panellist Deposition (micrograms/9 cm 2 )
• Protocol Application of 100 microlitres of 1% solution of the product on prewashed inner forearm, lather for 10 seconds, rinse, tap dry extraction with 400 microlitres of alcohol from 9 cm 2
• MCB-14 2% Parsol MCX added via Water-Continuous PSE.
• Panellist Deposition (micrograms/9 cm 2 )
• Panellist Deposition (micrograms/9 cm 2 )

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Cited By (33)

Citations (5)

• 1995
  • 1995-11-13 GB GBGB9523167.6A patent/GB9523167D0/en active Pending
• 1996
  • 1996-09-20 BR BR9611445A patent/BR9611445A/pt not_active Application Discontinuation
  • 1996-09-20 EP EP96933375A patent/EP0861063A1/en not_active Withdrawn
  • 1996-09-20 AU AU72138/96A patent/AU703204B2/en not_active Ceased
  • 1996-09-20 WO PCT/EP1996/004172 patent/WO1997017938A1/en not_active Application Discontinuation
  • 1996-10-01 ZA ZA9608250A patent/ZA968250B/xx unknown
  • 1996-11-08 AR ARP960105099A patent/AR004550A1/es not_active Application Discontinuation
  • 1996-11-12 MY MYPI96004690A patent/MY132583A/en unknown
• 1998
  • 1998-04-30 MX MX9803431A patent/MX9803431A/es unknown

Patent Citations (5)

Non-Patent Citations (1)

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