MXPA01005622A - Emulsification systems and emulsions - Google Patents

Emulsification systems and emulsions

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Publication number
MXPA01005622A
MXPA01005622A MXPA/A/2001/005622A MXPA01005622A MXPA01005622A MX PA01005622 A MXPA01005622 A MX PA01005622A MX PA01005622 A MXPA01005622 A MX PA01005622A MX PA01005622 A MXPA01005622 A MX PA01005622A
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Mexico
Prior art keywords
emulsifier
emulsion
oil
polysaccharide
weight
Prior art date
Application number
MXPA/A/2001/005622A
Other languages
Spanish (es)
Inventor
Christian Joseph Dederen
Thierry Wetzel
Guido Serrien
Original Assignee
Christian Joseph Dederen
Imperial Chemical Industries Plc
Guido Serrien
Thierry Wetzel
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Application filed by Christian Joseph Dederen, Imperial Chemical Industries Plc, Guido Serrien, Thierry Wetzel filed Critical Christian Joseph Dederen
Publication of MXPA01005622A publication Critical patent/MXPA01005622A/en

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Abstract

Personal care or cosmetic oil in water emulsions include an oil emulsifier and a combination of a Xanthan polysaccharide and a polyglucomannan polysaccharide to provide enhanced stability even at low emulsifier stabiliser levels. The emulsifier stabiliser system provides stable emulsions without dominating system rheology, particularly viscosity. Thus, the emulsions can have a low viscosity suitable for formulation as milks or thin lotions, or can be thickened, desirably by thickening agents other than the Xanthan and/or polyglucomannan, to provide emulsion creams or gels. This enables the system to be used very flexibly in end use applications. The emulsifier is desirably a non-ionic emulsifier and particularly is a combination of a low HLB and a high HLB emulsifier and can be formulated with conventional alcohol ethoxylate surfactants or from non-EO surfactants e.g. sucrose ester high HLB surfactants and citrate or sorbitan ester low HLB surfactants.

Description

EMULSIONING AND EMULSION SYSTEMS This invention relates to emulsification systems and emulsions, and in particular to emulsification systems which include emulsifiers and combinations of high molecular weight polysaccharides, and to emulsions made using these systems such as emulsifiers and emulsion stabilizers and particularly to emulsification and emulsions in the form of personal care products such as creams and cosmetic milk for the skin. Emulsion personal care products such as creams and milks desirably have several properties in combination: stability in manufacture, formulation, storage and use; a viscosity appropriate to the final use; and preferably a desirable body and a good feeling to the skin. The body and the feeling to the skin are usually assessed subjectively, and although a good body and / or sensation to the skin are commonly associated with a viscosity profile of shear thinning, non-neural, a thinning profile of Shear stress does not guarantee a good body or sensation to the skin. Typical products of emulsion of personal care, conventional use emulsifiers (including emulsion stabilizers) in amounts of about 3 to about 5% by weight of the emulsion. Recently, thickeners have been proposed as emulsion stabilizers and the stabilization mechanism when they are used seems to be that the thickener increases the low shear viscosity of the emulsion in a manner sufficient to provide a barrier to the droplet coalescence of the emulsion , probably by limiting the movement of the drops. The present invention is based on the discovery that certain combinations of high molecular weight polysaccharides can provide good emulsion stabilization at levels that do not give a high shear viscosity, or even significantly increased, low and that using these combinations, the amount of An emulsifier, usually a surfactant and a relatively low molecular weight, often non-ionic, can be much less than what is conventionally used in emulsions, particularly emulsions for personal care products such as creams and cosmetic skin milks. Accordingly, the present invention it provides an oil-in-water, cosmetic or personal care emulsion which includes as an emulsifier stabilizing system, an emulsifier for the oil and a combination of polysaccharides of a xanthan polysaccharide and a polysaccharide of polysuccinic acid. The invention also includes the use of a combination of polysaccharides of a xanthan polysaccharide and a polyglucomannan polysaccharide as an emulsifier stabilizer system in oil-in-water, cosmetic or personal care emulsions. The invention further includes a dry mix emulsifier stabilizer formulation which includes an oil emulsifier and an oil in water emulsion stabilizer which is a combination of polysaccharides of a xanthan polysaccharide and a polyglucomannan polysaccharide. The combination of polysaccharides of a xanthan polysaccharide and an iglumanic poly polysaccharide can briefly be referred to briefly as a polysaccharide stabilizer. The combined amount of emulsifier and stabilizer in the emulsions of the invention may be much lower than the typical 3 to 5% used in conventional care emulsion systems personal. In particular, in many emulsions of this invention, the amount of emulsifier can be less than about 1.5%, particularly up to about 1%, and the amount of polysaccharide stabilizer can be less than about 0.5%, and sometimes so little as about 0.02%, desirably with the combined amount that is less than about 1.5%, particularly up to 1%. The minimum amount of emulsifier is typically about 0.02%, more usually 0.025% by weight of the emulsion (see also below). Accordingly, the invention includes an oil-in-water, cosmetic or personal care emulsion which includes as an emulsifier stabilizer system, an emulsifier for the oil in an amount of not more than about 1% by weight of the emulsion and a stabilizer of polysaccharide in an amount of about 0.02 to about 0.5% by weight of the emulsion. Personal care emulsions can be divided by viscosity into milks and lotions, which typically have a low shear viscosity of up to about 10,000 mPa. s, and creams that typically have a low shear viscosity of no more than 20,000 mPa. s. Typically, milk and Lotions have a low shear viscosity from about 100 to about 10000 mPa. s, more usually from about 500 to about 5000 mPa.s, and typically the creams have a low shear viscosity of at least about 30,000 mPa. s, so pcles from about 30000 to about 80000 mPa. s, although higher viscosities may also be used, for example up to about 106 mPa. s. In this context, the low shear viscosity refers to the viscosity measured at shear rates of about 0.1 to lOs'1 as typically used in Brookfield viscometers. Due to good skin feel, cosmetic and personal care emulsions are usually thinning shear thinners, the low shear viscosity measured is only a general guide if the product is a milk (or lotion) or cream. The present invention includes emulsions in both milk (and lotion) and cream and specifically the invention includes an oil-in-water, cosmetic or personal care emulsion milk or lotion having a low shear viscosity of up to 10000 mPa. s, which includes as a stabilizing system of emulsifier, an emulsifier for the oil and a stabilizer of polysaccharide. The invention further includes an oil-in-water, personal care or cosmetic emulsion having a low shear viscosity of more than about 20,000 mPa. s, which includes as an emulsifier stabilizer system, an emulsifier for the oil and a polysaccharide stabilizer, the emulsion which additionally includes thickener components. Xanthan is a polysaccharide that includes mannose, glucose and glucuronic acid monomer units and typically the polymer backbone is polyglucose with acetylated side chains of 3 units including glucose, glucuronic acid, typically present as a mixed salt of potassium, sodium and calcium, and man-made waste. The xanthan polymers typically have a molecular weight in the range of 1106 to 5106 and usually about 2106 and are typically obtained from bacterial fermentations, pcularly from Xan thomanna campestris and related microorganisms. Xanthan products sold under the Keltrol trademark, pcularly grades "F11 and" T1 1, by Kelco they are pcularly suitable in this invention. The polyglucomannan typically has a random glucose / mannose structure, typically in a molar ratio of glucose to sugar in the range of about 1: 1.5 to about 1: 3, usually about 1: 2 with hydroxyl groups in acetylated pendant methylol groups. randomly, typically such that there are about 6 to 20 sugar monomer residues near an acetyl group. The molecular weight of the useful poriglucomannans can vary within a typical range of about 2,105 to about 2,106. Suitable materials include plant polyglucomannans such as those derived from Konjak. The Konjak polyglucomannan, sometimes referred to simply as Konjak or Konjak gum, is pcularly effective in this invention and its use as a polyglucomannan, and / polyglucomannan forms, is a specific aspect of the invention. The Konjak, Amorphophal l us konj ak, is also known as Konjac and Lengua del Diablo, is a tuber plant grown in Asia as a food plant. The carbohydrate components of the tuber include Konjak polyglucomannan. The Konjak polyglucomannan that occurs naturally has typically a molecular weight of about 1.10 ° to about 2.106, but processing, for example refining and milling can reduce the molecular weight. The emulsions of the invention have continuous phases, aqueous and when manufacturing the emulsions, the polysaccharides will usually be dispersed in the water. The particle size of the polysaccharides, especially the polyglucomannan, may be important in achieving a good dispersion in water, especially in a relatively cold, particularly cold (room temperature) water. The Konjak polyglucomannan is easily dispersed in hot water at concentrations of 0.001 to 0.5% by weight. However, as the tuber is typically derived, the Konjak polyglucomannan has a relatively large particle size and typically has an average particle size of about 100 to about 2000 μm. Material with this particle size tends to have a relatively poor dispersion capacity in cold water. Grinding to decrease the particle size, for example from about 50 to about 200 μm, can make the product much more easily dispersible in cold water. The dispersibility in cold water in xanthan polymers in the form of their powders commercially available usually is not a problem. As indicated above, the xanthan polymers typically have a molecular weight in the order of 2,106. The significant reduction of this molecular weight in general is undesirable since these have an adverse effect on the properties of Xanthan. For polyglucanones, particularly Konjak polyglucomannan, the molecular weight is less important with the proviso that the product is not otherwise degraded in a substantially chemical manner. Materials with molecular weights as low as about 2.105, which correspond to fictitious fragments of about 1/10 of the original polymer, can be effective in the present invention. The combination of xanthan and Konjak polysaccharides as the emulsion stabilizer is particularly advantageous and forms a specific aspect of the invention, including the various embodiments described in the invention therefore includes an oil-in-water, cosmetic or personal care emulsion that includes as an emulsifier stabilizer system, an emulsifier for the oil and a combination of polysaccharides of a xanthan polysaccharide and a polysaccharide of Konjak polyglucomannan.
The xanthan and polyglucomannan polysaccharides are believed to form complexes that yield thermoreversible, synergistic gels in aqueous systems (see for example "Biopolymer Mixtures" published by Nottingham University Press [1995], Chapter 14 by VJ Morris), but the detailed structure of These complexes have not yet been definitely established Similarly, other combinations of polysaccharides can also give aqueous gels These properties do not account for the stabilizing effect of the emulsion obtained in this invention, because the stable emulsions can be obtained Comparatively low viscosities This result is remarkable since the use of other gel forming materials such as Tara, Carragahen, Acacia Seed, guar gums and alginate, alone or in combination with xanthan, have not been able to combine a good emulsion stability with acceptable body properties and sensation to - the skin. obtained suggest that these other gel forming materials provide emulsion stabilization because they provide an increased viscosity of emulsion. Similarly, the literature reports that in an aqueous solution, xanthan typically exists as molecular aggregations sometimes referred to as a dimer This may explain why it was found that the stabilizing effect of xantan? / Polyglucomannan can be promoted by heating and / or vigorously mixing an aqueous dispersion of xanthan and polyglucomannan before emulsifying the oil in the aqueous system (see below). In any case, it is not known why it has been able to make very stable emulsions according to the present invention and it is not desired that any particular theory be restricted to explain it. It has been found that an improvement in the stabilization of emulsions can be obtained at weight ratios of xanthan to polyglucomannan, particularly Konjak polyglucomannan, from about 1:10 to about 10: 1, particularly about 4: 1 to about 1: 4, with more desirable results in the range of from about 2: 1 to about 1: 2 and especially about 1: 1. This maintains the case even when lower molecular weight polyglucomannan is used and the relative consistency of this relationship suggests that when a lower molecular weight polyglucomannan is used, the combination formed can include several molecules of polyglucomannan for each Xanthan molecule. The amount of the polysaccharide stabilizer used will generally be sufficient to provide an improvement in emulsion stability more desirably to give adequate stability to the emulsion. Nevertheless, the inclusion of amounts of polysaccharide stabilizer significantly in excess of that necessary to achieve emulsion stability is undesirable since this can give substantial thickening of the emulsion. Aqueous systems, including emulsions thickened with Xanthan, polyglucomannan or the polysaccharide stabilizer generally have a pseudoplastic rheological profile of shear thinning, but they give slug and / or fibrous products with poor body and / or skin feeling which is undesirable in personal care products. These properties represent a significant discouragement to the use of these polysaccharides alone or in combination in cosmetic and personal care emulsions. The use of still very low concentrations of polysaccharide stabilizer, for example, as low as about 0.01% by weight of the emulsion, can give better emulsion stability utilities. In practice, the amount of the polysaccharide stabilizer used will be chosen to give emulsions with extended stability and will be in general at least about 0.02% by weight of the emulsion. The maximum concentration used in general depends on the emulsion system, but typically it is about 0.5% by weight of the emulsion. Thus, suitable general concentration ranges are from about 0.02% to about 0.5%, more usually from about 0.025 to about 0.25%, particularly to about 0.2% and specifically from 0.025 to 0.15% by weight of the emulsion Relatively high concentrations can be used in these ranges, for example where particularly difficult emulsions are made including those which use very hydrophobic oils, or in particular, in cream formulations, or where the electrolyte may be present (see below), although rheology can not be ideal. The emulsions prepared and stabilized according to the invention can have exceptionally high stability even at elevated temperatures, for example up to about 50 ° C. However, combinations of polysaccharides are sensitive to ionic materials that act to destabilize the emulsions. It is believed that the presence of ionic materials destabilizes the combination xanthan / polyglucomannan so that less effective stabilization of the emulsion is provided. For this reason, ionic materials, for example, acids, bases and salts including neutral salts, such as organic or inorganic salts, are desirably present only at low concentrations in the emulsions of this invention, or are absent. In general, the concentration of ionic materials will not be greater than about 0.05 molar, desirably not more than about 0..02 molar and particularly not more than about 0.01 molar. Similarly, ionic surfactants, including emulsifiers, including anionic, cationic and zwitterionic surfactants, are desirably present at significant concentrations in the emulsions of the invention. Amphoteric surfactants can be used, but usually only under conditions where they do not support charged species and as this tends to be an environment where amphoteric surfactants are not particularly effective, usually they are not desirably included. Accordingly, the emulsifier used in the invention is desirably one or more non-ionic emulsifiers. Suitable emulsifiers include agents conventional, non-ionic oil-in-water emulsifier surfactants such as alkoxylate emulsifiers and surfactants which can be derived from natural materials such as fatty acid esters, ethers, hemi-acetals or acetals of polyhydroxy compounds or an acid amide fatty that is N-substu tuted with the residue of a polyhydroxy compound. The specific nature of the emulsifier surfactant used in any particular case depends on the type of emulsion that is made, particularly if fatty amphiphilic thickeners are being used, the degree of stability required, the nature of the oil to be emulsified and the total desired level of the emulsion. emulsifier / stabilizer system. The term "alkoxylate emulsifier" is used to refer to surfactants in which a hydrophobe, usually a hydrocarbyl group, is connected through the residue of a linking group having a reactive hydrogen atom to an oligomeric or polymeric residue chain of alkylene oxide. The hydrocarbyl group is typically a chain, commonly an alkyl chain, containing from 8 to 24, particularly from 12 to 22 and usually from 14 to 20 carbon atoms. The link group can be an oxygen atom (the hydroxyl group residue); a carboxyl group (ester residue or fatty acid); an amino group (amino group residue); or a carboxyamido (boxyl amide residue). The alkylene oxide residues are typically residues of ethylene oxide (C2H40) or propylene oxide (C3H60) or combinations of ethylene or propylene oxide residues. When combinations are used, the proportion of ethylene oxide residues will usually be at least about 50 mol% and more usually at least 75 mol%, the remainder being propylene oxide residues. In a particular manner and desirably, substantially all of the residues are residues of ethylene oxide. The number of alkylene residues in the emulsifying molecule is desirably from 2 to about 200. At least theoretically, alkyl phenyl ethoxylates could be used, but these are generally not now desired in cosmetic and personal care products. other reasons and thus are not used in the usual manner in this invention. The number of alkylene oxide residues is usually from 2 to 200 per mole of alkoxylate emulsifiers and will vary depending on the balance between the hydrophilic and hydrophobic properties desired in the emulsifier (see later). Examples of emulsifiers and alkoxylate. suitable include alcohol alkoxylates, of Formula (Ia): R ^ O- (AO) n-H; a fatty acid alkoxylate of the Formula (Ib): Rx-COO- (AO) n-R2 (plus co-products); a fatty amine alkoxylate of the Formula (le): RX-NR3- (AO) nH, - or a fatty amide alkoxylate of the Formula (Id): RX-NR3- (AO) nH, wherein each R1 is independently hydrocarbyl of 8 to 24 carbon atoms, particularly of 12 to 22 carbon atoms, particularly alkyl group; R2 is a hydrogen atom or an alkyl group of 1 to 6 carbon atoms; and each R3 is independently an alkyl group of 1 to 6 carbon atoms or a group (A0) nH; each AO is independently a group of ethylene oxide or propylene oxide; and the total of the n-indices in the molecule is from 2 to 200. By using the alkoxylate emulsifiers, the invention includes a cosmetic or personal care oil in water emulsion, particularly an emulsion having a low shear viscosity of up to approximately 10000 mPa. s, which includes as an emulsifier stabilizer system an alkoxylate emulsifier for the oil in an amount of about 0.02 to about 1. 5% by weight of the emulsion and a polysaccharide stabilizer in an amount of about 0.02 to about 0.25% by weight of the emulsion. Additionally, using high HLB alkoxylate emulsifiers (see also below), the emulsifier stabilizing system of the invention can be effective at very low levels, and is particularly applicable to low viscosity systems (due only to some materials used to increase the emulsion viscosity may require the presence of additional emulsifier to disperse it), and accordingly, the invention includes a cosmetic or personal care oil in water emulsion, particularly an emulsion having a low shear viscosity of up to about 10000 mPa . s, which includes as an emulsifier stabilizer system, an alkoxylate emulsifier for the oil in an amount from about 0.02 to about 0.25% by weight of the emulsion of a polysaccharide stabilizer in an amount of about 0.02 to about 0.25% by weight of the emulsion. Creams can be made using alkoxylate emulsifiers, but in general the amount of emulsifier will be greater than the amount minimum to stabilize a milk emulsion. The invention thus includes an oil-in-water, cosmetic or personal care oil emulsion having a low shear viscosity of more than about 20,000 mPa. s, which includes as an emulsifier stabilizing system, an emulsifier, including an alkoxylate emulsifier, for the oil in an amount from about 0.25 to about 1.5%, particularly from about 0.5 to about 1%, by weight of the emulsion and a polysaccharide stabilizer in an amount from about 0.02 to about 0.5%, particularly from about 0.05 to about 0.25, by weight of the emulsion, the emulsion also including thickener components. The emulsifier stabilizer system of the invention is flexible since emulsifiers that are not derived from alkylene oxides can also be used. The possibility of using emulsifier stabilizer systems that are completely derived from biological source materials, particularly vegetables, is likely. This possibility may be attractive to formulators of personal care products. In this regard, the invention, therefore, additionally includes an oil in water emulsion cosmetic or personal care including as an emulsifier stabilizer system, an emulsifier for the oil, which is an ester of fatty acid, ether, hemi-acetal or acetal of a polydihydroxy compound, or a fatty acid amide which is N-substi tuted with the residue of a polyhydroxy compound, especially a fatty acid ester of saccharide, and a polysaccharide stabilizer. Sugar esters (saccharides) can be used with the advantage in this invention since they can provide very stable emulsions that can completely avoid using products made using alkylene oxides can allow the use of emulsifier / stabilizer systems that are completely derived from a biological source "natural", particularly plant source materials Particularly useful polyhydroxy compound esters include saccharide esters particularly monoesters of fatty acids and a sugar, especially sucrose, fluctuous and / or glucose Commercially available sugar esters are usually mixtures that they contain monoester, higher esters and sometimes a free starting material (sugar) In this invention, it is desirable to use sugar esters having a relatively high proportion of mono-ester.
Typically, the sugar ester used will have a mono-ester content of at least 50%, more usually at least 60% and desirably at least 65%. The proportion can be higher, for example, of 70%, 80% or even higher, although products with very high proportions of monoester are significantly more expensive and no particular advantage has been found in the use of products with more than approximately 75% of monoester. The sucrose esters are particularly useful in the invention. These sugar esters are relatively hydrophilic emulsifiers and less hydrophilic variants can be used in which hydroxyl groups (usually only one) are esterified in the saccharide residue (or acetyl), typically with an alkyl group of 1 to 4 carbon atoms , for example, a methyl group. Desirable sugar esters may be of Formula (lia) R'-COO- (G) a, wherein R 1 is as defined above for alkoxylate emulsifiers; each G is independently a saccharide residue, particularly a glucose, mannose or fructose residue and a is from 1 to about 5, particularly about 2, especially the residue (G) a is the sucrose or glucose residue. Other esters of polyhydroxy compounds include esters of fatty acids, particularly fatty acids having from 8 to 24, usually from 12 to 22, more usually from 16 to 20 carbon atoms, and polyols, particularly glycerol, or a polyglycerol; or an anhydrous saccharide such as sorbitan. In general, these materials are also used in a primarily desirable way as the mono-ester. Examples include glycerol mono-laurate, triglycerol monostearate and relatively more hydrophobic emulsifiers, glycerol mono-stearate and sorbitan mono-oleate, stearate or laurate. These suitable esters may be of Formula (11b): R ^ COO-R4, wherein R1 is as defined above for alkoxylate emulsifiers, and R4 is a polyhydroxyl-hydrocarbyl group, particularly an alkyl group or an ether group -alkyl containing 3 to 10 carbon atoms and 2 to 6 hydroxyl groups. These materials can be used in combination with others, for example, ester emulsifiers as in the mixture of "" nominally "'' polyglyceryl stearate and met il-glucoside stearate sold under the trade designation Tego Care 450 by Goldschmidt. Still further, ester emulsifiers include esters of fatty acid acids hydroxycarboxylic acids, in particular the trans-esterification products between fatty glycerides, especially mono- and diglycerides, and polyhydroxycarboxylic acids. These products are usually described as esters, but are typically mixtures of the starting materials and the transesterification products, particularly where the fatty acid residues are esterified to hydroxyl groups in the hydroxycarboxylic acids. In these products, the fatty acid typically has from 8 to 24, usually from 12 to 22, more usually from 16 to 20 carbon atoms and the hydroxycarboxylic acid is desirably citric acid. Another type of emulsifier derived from sugars are the hydrocarbyl esters of saccharide, hemi-acetals or acetals, commonly known as hydrocarbyl, particularly alkyl, polysaccharides (more suitably ol i -saccharides), and in particular materials of the Formula (lie): R1-0- (G) a, wherein R1 is as defined above for the alkoxylate emulsifiers; each G is independently a saccharide residue, particularly a glucose residue and a is from 1 to about 5, particularly from about 1.3 to about 2.5. One type of additional emulsifier is the N-substituted fatty acid amides in which the N-substituent is the residue of a polyhydroxy compound, which is commonly a saccharide residue such as a glucoside group. This type of emulsifier includes materials of the Formula (lid): R ^ CO-NR ^ 6, where R: is as defined above for alkoxylate emulsifiers; R5 is a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, a group of the formula R6; and R6 is a polyhydroxylhydrocarbyl group, particularly a group containing from 3 to 10 carbon atoms and from 2 to 6 hydroxyl groups and is typically a glucosyl residue. In this regard, the invention includes low viscosity milk emulsions and higher viscosity cream emulsions. Specifically, the invention includes an oil-in-water, cosmetic or personal care emulsion milk having a viscosity of up to about 10000 mPa.s, which includes as an emulsifier stabilizing system, an emulsifier for the oil, which is an ester of fatty acid, ether, hemi-acetal or acetal of a polyhydroxy compound, or a fatty acid amide which is N-substituted with the residue of a polyhydroxy compound, in an amount of from about 0.5 to about 1.5% in weight of the emulsion of a polysaccharide stabilizer in an amount of about 0.02 to about 0.5% by weight of the emulsion. The invention additionally specifically includes an oil-in-water, cosmetic or personal care cream emulsion having a viscosity of more than about 20,000 mPa.s, which includes as an emulsifier stabilizer system an emulsifier for the oil which is a fatty acid ester, ether, hemi-acetal, or acetal of a polyhydroxy compound or a fatty acid amide that is N-substituted with the residue of a polyhydroxy compound, in an amount of about 0.5 to about 1.5% by weight of the emulsion and a polysaccharide stabilizer in an amount of about 0.02 to about 0.5% by weight of the emulsion, the emulsion which additionally includes thickener components. It may be useful to use a combination of different types of emulsifier and in particular to combine the hydrophilic emulsifiers, ie having a higher hydrophilic-lipophilic balance (HLB) for example, more than about 12, and hydrophobic emulsifiers, i.e. they have a low HLB, for example, less than about 8, when making the emulsions of the invention. The emulsifiers relatively hydrophilic include alkoxylate emulsifiers with an average of about 10 to about 100 alkylene oxides, particularly ethylene oxide residues; and non-alkoxylate emulsifiers including sugar monoesters and polyglycerol mono-esters, hydrocarbyl, especially alkyl, polysaccharides; fatty acid glycerol esters wherein the fatty acid has from 8 to 12 carbon atoms such as glycerol mono-laurate and N-sugar fatty acid amides such as glucamides. Relatively hydrophilic emulsifiers include alkoxylate emulsifiers with an average of from 2 to about 10 alkylene oxide residues, particularly ethylene oxide residues; glycerol esters wherein the fatty acid has from 14 to 24 carbon atoms such as glycerol mono-stearate, mono-oleate or mono-laurate; and fatty esters of anhydrous saccharide such as mono-stearate, -oleate or sorbitan -laurate. The amount of emulsifier used is typically about 0.02 to about 1.5%, more usually from about 0.025 to about 1.2%, particularly from about 0.025 to about 1%, by weight of the emulsion. Where emulsifiers are used hydrophilic alkoxylate, especially those with HLB greater than about 12, it is possible to obtain satisfactory emulsions with very low levels of emulsifier for example from so little, about 5 0.04 to about 0.1% by weight of the emulsion, and this forms a particular feature of the invention. Larger amounts of emulsifiers may be used, for example, in the entire range of from about 0.04 to about 0.8%, particular way about 0.1 to about 0.6%, by weight. Where less hydrophilic alkoxylate emulsifiers are used, such as the primary emulsifier, the concentration used will typically be higher, for example in the range of about 0.1 to about 1.5%, more usually from about 0.2 to about 1.2, particularly from about 0.5 to about 1%, by weight of the emulsion. Similarly, where emulsifiers are used as the main emulsifier non-alkoxylate such as fatty acid esters, ethers, hemi-acetals or acetals of compounds __,. polyhydroxy, or N-fatty acid amides (substituted with poly-hydroxyl residue), the amount used will typically be from about 0.2 to approximately 1.2, more usually from close to 0. 3 to about 1%, particularly from about 0.4 to 0.8%, by weight of the emulsion. When using a combination of hydrophilic emulsifiers (high HLB, for example, more than about 10) and hydrophobic (under HLB, for example less than about 8), the amount of the hydrophilic emulsifier will typically be in the ranges set forth above and the amount of the relatively hydrophobic emulsifier will typically be from 0.1 to 1%, particularly from near from 0.2 to approximately 0.8%. In these combinations, the total amount of emulsifier is typically from about 0.5 to 1.5%, particularly from 0.1 to 1%, by weight of the emulsion. The use of hydrophilic and hydrophobic emulsifier combinations (sometimes called a co-emulsifier) is particularly useful when the oil phase is highly hydrophobic (non-polar), or when the emulsion is thickened by the inclusion of fatty amphiphiles (see below) . In these combinations, the total HLB of the emulsifier system will typically be from about 8 to about 12. It has been found that the inclusion of more emulsifier, particularly of a relatively hydrophilic emulsifier, is then necessary to provide an emulsion drop size properly small, can have a detrimental effect on the stability of the emulsion. The excess of relatively more hydrophobic emulsifiers appears to be less detrimental to stability and may contribute to a desired rheology of emulsion (relatively hydrophobic emulsifiers are in a chemical manner quite similar to fatty amphiphiles as can be used as thickeners, see below). In general, it is technically possible to freely combine nonionic emulsifiers of the alkoxylate and non-alkoxylate types described above. These combinations may be attractive, where the emulsifier system includes a hydrophilic alkoxylate emulsifier, for example, using a non-HLB low alkoxylate emulsifier, in combination. However, non-alkoxylate hydrophilic emulsifiers, especially sugar monoester emulsifiers, are more expensive than typical alkoxylate emulsifiers and will usually be used only when it is desired to have an emulsifier stabilizer system that does not include alkylene oxide derivatives. The oil phase used will typically be mainly an emollient oil of the type widely used in cosmetic or care products personal. The emollient can and will usually be an oily material that is liquid at room temperature. Alternatively, it can be solid at room temperature, in which case in volume it will usually be a waxy solid, provided that it is liquid at an elevated temperature at which it can be included and emulsified in the composition. As described below, the preparation of the composition usually uses temperatures of up to about 100 ° C, usually about 80 ° C, so that these solid emollients will have melting temperatures of less than 100 ° C and usually less than 70 ° C. . Suitable emollient oils, usually liquids, include non-polar oils, for example, mineral or paraffin oils, especially isoparaffins, such as those sold by ICI Surfactants such as Arlamol HD; or oils of medium polarity, for example vegetable glyceride oils tai-like jojoba oil, animal glyceride oils, such as those sold by ICI Surfactants such as Arlamol M812 (caprylic / capric triglyceride), synthetic oils, e.g. synthetic ester, such as isopropyl palmitate and those sold by ICI Surfactants such as Arlamol IPM and Arlamol DOA, ether oils, particularly of two alkyl fatty residues of 8 to 18 carbon atoms, such as that sold by Henkel as Eutanol G (octyl -dodecanol), or silicone oils, such as dimetizing oil such as those sold by Dow Corning as DC200 , cyclomethane oil, or silicones having polyoxyalkylene side chains to improve their hydrophilicity; or highly polar oils including alkoxylate emollients for example fatty alcohol propoxylates such as those sold by ICI Surfactants such as Arlamol E (15-steredoctic alcohol propoxylate). Suitable emollient materials that can be solid at room temperature but liquid at temperatures typically used to make the compositions of this invention include jojoba wax, bait and coconut wax / oil. When non-polar oils are used it may be desirable to use relatively high concentrations of emulsifier, particularly an emulsifier with a high HLB, in order to achieve suitably satisfactory emulsification, particularly to obtain small oil drops. Mixtures of emollients and will be used frequently, and in some cases solid emollients can be completely or partially dissolved in liquid emollients or in combination, the freezing point of the mixture is suitably low. Where the composition of emollients is a solid at room temperature, the resulting dispersion can not technically be an emulsion (although in some cases the precise phase of the oily phase, dispersed can not be easily determined), but these dispersions behave as if they were true emulsions and the term emulsion is used herein to include these compositions. The concentration of the oil phase can vary widely. In general, the concentration of the oil phase will be at least about 1%, and more usually at least about 5% in pesos and in products such as those used, the oil concentration can be as high as about 30-% . Certainly, stable emulsions have been easily obtained in the content of the oil phase of up to 20% by weight. Even greater concentrations are possible, emulsions have been made up to 80% by weight of oil, and these concentrated emulsions can be used as pre-manufactured concentrates for dilution with other components to make product emulsions. The polysaccharide stabilizers used in this invention can be used in other contexts as thickeners, but when used as thickeners, although they appear to provide shear thinning properties, it has been found that they give emulsion products having a cosmetically poor body and skin feel commonly described as "fibrous" materials and / or "" slobbery ''. These properties are undesirable in cosmetics and personal care products, so that the inclusion of the excess polysaccharide stabilizer or the individual polysaccharides is not usually satisfactory for the thickening of emulsions, for example, to form creams, for cosmetic or cosmetic products. personal care and is not used in general in this invention. The most desirable ways of rheology modification to produce higher viscosity products include the use of materials that will build a network of particles in the aqueous, continuous phase. Particularly suitable materials include fatty amphiphiles such as fatty alcohols, acids and fatty waxes. Suitable materials include fatty alcohols, particularly fatty alcohols of 8 to 24 carbon atoms, especially of 14 to 20 carbon atoms such as stearyl alcohol, for example, as commercial cetearyl alcohol (a mixture mainly of cetyl and steretic alcohols); fatty acids, particularly fatty acids of 8 to 24 carbon atoms, especially of 14 to 20 carbon atoms such as stearic acid), and such as microcrystalline wax such as that sold by Fuller as Lunacera M. The technical limit between surfactants Hydrophobic and fatty amphiphiles are not always clear and the presence of emulsifiers with low HLB may contribute to thickening by fatty amphiphiles. The fatty amphiphiles used as thickeners in this invention will be commonly used as mixtures of materials, for example, from a natural source, a distillation cut during manufacture to deliberately mixed to give a mixture. The precise mechanism by which fatty amphiphiles contribute to thickening is not fully understood, but appears to contribute to the structure in the aqueous phase. Other thickeners that can be used include polymeric thickeners such as starches, particularly modified starches, for example, modified potato starch, such as that sold by National Starch as Structure Solanace, and modified corn starch such as that sold by National Starch as Structure Zea (hydroxypropyl phosphate) dialmidon); cellulose thickeners such as carboxy-alkylcellulose for example carboxymethylcellulose such as that sold by Hercules as Natrosol 250HHR (hydroxy-ethylcellulose), or that sold by FMC as Avidel RC-591 (a mixture of sodium carboxymethylcellulose and microcrystalline cellulose); polysaccharide gums such as Tara, Carragahen, Guar, acacia gum, Xanthan gums and Konjak (although with the amounts used it may be necessary to limit, to avoid unwanted skin feeling and undesirable body properties in the emulsion products) and modified gums such as guar hydroxypropyl ether; and synthetic thickeners such as polyacrylic thickeners such as carbomers including Carbopol resins from Goodrich (although one can be careful with these as they are ionic although they are very effective thickeners by weight and can be used without necessarily making the emulsions unstable). An important advantage of the invention is that the thickened emulsions can be processed in which the emulsion is substantially thickened independently of the stabilization of the emulsion. This gives product formulators much more freedom in the design of cream systems that have a desired rheology compared to the use of thickeners to stabilize emulsions, because the rheology is not restricted by that used in the stabilization of the emulsion. For reasons that are not clear, the use of some thickeners, an additive and possibly the synergistic effect in the thickening emulsions of the invention has indicated the use of the polysaccharide stabilizer. When the components of the oil phase include fatty amphiphiles, for example, including, thickeners, it may be necessary to use higher concentrations of emulsifier, particularly emulsifier with high HLB, and / or the use of combinations of hydrophilic and hydrophobic emulsifiers, in order to adequately disperse the fatty amphiphile. However, satisfactory results have been achieved using total emulsifier levels not exceeding about 1.5% and usually not more than about 1.2% and particularly desirable, so that the total polysaccharide stabilizer concentration of the emulsifier is not more than about 1%. The composition of the emulsions of the invention, with respect to the main components, typically falls within the ranges in the tables below.
* Used in combination with a high HLB emulsifier ** After 'allow minor components and additives The emulsions and formulations of this invention are typically of almost acidic / base neutrality, their sensitivity to ionic materials is mentioned above. Moderate deviation from neutrality is possible without loss of the advantages of stability of the invention. Desirably, the pH is from 4 to 9, more desirably from 4.5 to 8 and particularly useful from 6 to 8. Many other components may be included in the emulsion compositions of the invention to make cosmetic or cosmetic formulations. personal care . These components can be soluble in oil, soluble in water or non-soluble. Among the water-soluble components, care must be taken with materials that provide electrolyte to the composition or cause marked changes in pH (see above). Examples of these materials include: - Preservatives such as those based on parabens (alkyl esters of 4-hydroxybenzoic acid), phenoxyethanol, substituted ureas and hydantoin derivatives, for example, those sold commercially under the trade names Germaben II Nipaguard BPX and Nipaguard DMDMH, when they are usually used in a concentration of 0.5 to 2%, by weight of the emulsion; - Perfumes, when a concentration of 0.1 to 10% is typically used up to about 5% and particularly up to 25%, by weight of the emulsion. - Humectants or solvents such as alcohols, polyols such as glycerol and polyethylene glycols, when typically used at a concentration of 1 to 10%, by weight of the emulsion; - Solar filter or solar block materials including chemical sun block and physical sun block including those based on titanium dioxide or zinc oxide; when they are typically used from 0.1 to 5% by weight (but it is noted that physical sunscreen materials are often dispersed using polyanionic acrylic polymers which may tend to destabilize the emulsions because they supply electrolytes; - alpha hydroxy acids such as glycolic acids , citric, malic, tartaric and their esters; - Self-tanning agents such as dihydroxyacetone; - Antimicrobial components, particularly anti-acne such as salicylic acid; Vitamins and their precursors including: a) Vitamin A for example, as a palmitate retinyl and other tretinoin precursor molecules b) Vitamin B, for example, as panthenol and its derivatives, c) Vitamin C, for example, as ascorbic acid and its derivatives, d) Vitamin E, for example, as tocopheryl acetate, and ) vitamin F, for example, as esters of polyunsaturated fatty acids such as gamma-linolenic acid esters; - skin care agents such as ceramides either as natural materials or functional imitators of natural ceramides; - phospholipids; - formulations containing vesicles; - germanium containing compounds for example that sold by ICI Surfactants as Arlamol GEO; - botanical extracts with beneficial properties of skin care; - skin whiteners such as hydroquinone, kojic acid, arbutin and similar materials; - active skin repair compounds, such as allantoin and similar series; - caffeine and similar compounds; cooling additives such as metal or camphor; insect repellents such as N, N-diethyl-3-methylbenzamide (DEET) and citrus or eucalyptus oils; - essential oils; and - pigments, including microfine pigments, particularly oxides and silicates, for example iron oxide, particularly coated iron oxides, and / or titanium dioxide, and ceramic materials such as boron nitride, or other solid components, as used in makeup and cosmetics, to give their emulsions, typically used in an amount from about 1 to about 15%, but usually at least about 5% and particularly about 10%. < The emulsions of the invention can be formulated either as simple emulsions which can be expressed as described above or can be formulated in more complex systems such as suspoemulsions or multiple emulsions. Suspoemulsions include a dispersed, liquid phase and a dispersed, solid phase. As mentioned above, the solid may be a pigment, for example, titanium dioxide and / or colored iron oxides; or a physical sunblock of a metal oxide such as titanium and / or aluminum and / or zinc oxides, in which case the oxide particles may be sufficiently fine so as not to disperse visible light (although they will be selected to disperse light) UV). Therefore, the invention includes a suspoemulsion which is an emulsion of the invention that additionally includes a dispersed solid material, particularly a pigment. Other forms of the more complex system include multiple emulsions in which the dispersed phase of an emulsion has within its drops a dispersion of drops of another liquid. In this way, there are two emulsions, a primary or external emulsion and a secondary or internal emulsion, and the phases can be described as primary or external and secondary or internal, external or internal phases. In this way, there are two internal phases that are commonly referred to as the external or primary internal phase and the internal or secondary internal phase and two external phases commonly referred to as the external or primary external phase and the internal or secondary external phase.
There are two basic types of multiple emulsion, water in oil in water and oil in water in oil. Both types of multiple emulsion can be made using the emulsification stabilization system of this invention. The invention thus further includes a water-in-oil-in-water multiple emulsion in which the primary oil-in-water emulsion is an emulsion of the invention and an oil-in-water-in-oil emulsion in which the secondary or internal emulsion is an emulsion of the invention. The secondary internal phase of the multiple emulsions can be used to distribute materials that are sensitive to environmental conditions or to materials in the primary external phase. The emulsions of the invention can be used, as described above, as cosmetic or personal care products in themselves or can be manufactured in these products. In particular, they can be used to impregnate particularly woven tissues of paper, for example, to provide cleaning tissues. In this application, the emulsion will typically contain a relatively low proportion of the oil phase typically from 3 to 15, more usually about 5% by weight of the emulsion. The amount of emulsion impregnated in tissues will depend on the desired properties in the final product, but typically it will be from 10 to 100 g.m2 of tissue. The fabrics will typically have a basis weight of 30 to 100 gm "2. The invention thus includes a cleaning fabric that is impregnated with an emulsion of the invention Another use for the emulsions of the invention is to remove makeup or other cosmetics It has been found that the emulsions of the invention are effective in this use and can be broadly efficient as the pure oil in the removal of oily makeup, for example, masks, particularly "waterproof" mask. surprising result since the emulsions in this use typically do not contain very high proportions of oil, typical amounts will be from 25 to 50, more usually 15 to 30%, by weight of the emulsion The emulsions of the invention can be made by conventional methods of conventional emulsification and mixing, typical methods include direct emulsification by first dispersing the emulsifier (s) and the polysubstance stabilizer. Acaride (either added as separate components or together) in the aqueous phase and then mixing and emulsifying the oil in the continuous, aqueous phase. For To ensure the formation of the polysaccharide emulsion stabilizer combination, it is desirable to either heat the aqueous phase containing the xanthan and the polyglucomannan, usually above about 60 °, for example, to about 80 to 85 ° C or subject the aqueous phase to high intensity mixing at a lower temperature, for example, about room temperature. Vigorous mixing and the use of moderately elevated temperatures can be combined, if desired. The high intensity heating and / or mixing can be carried out before, during or after the addition of the oil phase. Emulsions can also be made by inverted emulsification methods, particularly where low HLB emulsifiers are used (typically in combination with high HLB emulsifiers). In these methods, the emulsifier components, which usually include the polysaccharide stabilizer (either added as separate components or together) in the oil phase and the aqueous phase are then added and mixed in the oil phase to form a water in oil emulsion. The addition of the aqueous phase is continued until the system is inverted for an oil-in-water emulsion.
Explicitly, a substantial amount of the aqueous phase will generally be needed to effect the inversion and thus this method is not likely to be used for emulsions with a high oil phase content. As described above, to insure the formation of the polysaccharide emulsion stabilizer combination, it is desirable to either heat the xanthan and polyglucomannan in or in contact with the aqueous phase usually above 60 ° C, for example to about 80 ° C. 85 ° C, and subject them to a high intensity isolate at a lower temperature, for example, close to room temperature. Vigorous mixing and the use of moderately elevated temperatures can be combined, if desired. Heating and / or high intensity mixing can be carried out during or after the addition of the aqueous phase and before, during or after inversion. In general, it has been found that hot dispersion methods give emulsions that are more stable than those made by cold dispersion methods, but cold dispersion is very convenient, particularly for formulators and can give good results. For example, where components that need processing at high If temperatures are used, for example, waxes with a relatively high melting point, hot dispersion may be convenient, for this reason. After making the emulsions, the concentration of the dispersed phase can be easily adjusted by the addition of the additional continuous phase material, usually with gentle mixing. In the context of emulsion processing, vigorous high-intensity mixing refers to mixing at constant stress rates typically used in emulsification and will usually do so at a shear rate of at least about 104 sec "1. emulsions with a relatively high viscosity are prepared, dispersible or water-soluble thickener components can be included in the aqueous phase suitably after dispersing the emulsifier and the emulsion stabilizer and dispersing or oil-soluble thickening components can be added. disperse or dissolve in the oil phase and incorporate in the emulsion with the oil.Therefore, the invention includes a method for making an emulsion which includes the steps of: 1. - Disperse the emulsifier (s) and the polysaccharide stabilizer in the aqueous phase; 2. - optionally include the thickener components in the aqueous phase; and 3. - mixing in and emulsifying the oil in the continuous, aqueous phase; Y in which the aqueous dispersion of the emulsifier (s) and the polysaccharide stabilizer it is heated to a temperature of at least about 60 ° C and / or mixed vigorously before or during emulsification of the oil. The emulsions of the invention can be used in a wide variety of cosmetic and personal care products and the invention includes these products and the use of the emulsions of the invention in these products as specific aspects of the invention. The emulsions of the present invention can be incorporated in both cream and milk products. Examples of these products include milk and cleaning creams; skin moistening creams and milks; milks and creams for removing cosmetics; and sunscreens, such as in sprayable milk or milk emulsion forms. The emulsifier and the components of Emulsion stabilizers used in the invention can be used to provide a dry formulation that can be dispersed in water and then easily processed into emulsions and as noted previously, this forms an aspect of the invention. Typically, these dry formulations include the solid components including the emulsifier and the polysaccharide stabilizer. For these formulations, it is useful to use both high HLB and low HLB emulsifiers and optionally include materials such as grinding aids, for example, sugars, particularly glucose and / or sucrose, which provide relatively hard materials to aid grinding and grinding , if needed, and also act as readily soluble materials by adding the subsequent aqueous dispersion of the formulations. These formulations can be made by dry blending the xanthan and polyglucomannan polysaccharides, emulsifiers and optionally sugar, if desired, by consolidating the mixture, eg, by extrusion, to form granules and then grinding the granules to a desired particle size. Desirably, the materials are processed at a temperature, typically 50 ° C to 100 ° C, sufficient for one or more of the components typically one or more of the emulsifiers are at least partially melted and the powder components can be coated and / or bonded, typically including the polysaccharides. The emulsifier components can be melted desirably and completely and the polysaccharides mixed in this melt. This mixing can be carried out an extruder of batch mixing and the product can be solidified into flakes or granules that if necessary, can be subsequently ground to make more finely divided particles. The composition of the dry formulation with respect to the main components, typically falls within the ranges in the table below: Particularly, where the dry formulation is proposed to be cold dispersible, (the dry mixed product) a powder having an average particle size of about 100 to about 500 μm is desirable. To make handling more direct, for example, to reduce the risk of dust combustion, the powder desirably contains little or no material having a much smaller particle size. In particular, the proportion of particles of size less than 50 μm is less than 10% (by weight), and desirably less than 2%, so particular less than 1%. If cold dispersibility is not an important requirement, the physical form of the dry formulation can be divided even finer, for example, pellets, granules and / or flakes. In these forms, the average particle sizes can be significantly greater than with the powder, for example 0.5 to 5 mm for tablets and / or granules and 0.1 to 1 mm in thickness and 2.5 to 100 mm in length and / or width, corresponding a particle size (measured as the diameter of spheres of equal volume) of about 1 to about 6 mm. These large forms of particle size form a further aspect of the invention. As for the powders, the level of fine particles is desirably low, in particular, the proportion of particles of size less than 50 μm is less than 10% (by weight), desirably less than 2%, particularly less than 1. %. The following examples illustrate the invention. All parts and percentages are by weight unless otherwise indicated. The examples of the invention are indicated by a number of examples followed by a run number of the comparative examples by a number including "" C11. materials Formulation methods Hot dispersion. -Leches The powders of xanthan gum and Konjak were dispersed in water at 80 ° C, the emulsifier system was added to the water and mixed for 20 minutes. The Oil components were mixed and added as an oil phase to the mixture at 80 ° C (with heating, if necessary), the mixture was homogenized for 2 minutes in an Ultra-Turrax mixer at 8000 rpm (approximately 133 Hz) at 80 ° C and the emulsion was allowed to cool to room temperature under gentle stirring.
Cold dispersion.- Milks The xanthan gum and Konjak powders were premixed to form a powder (with Konjak grinding if necessary) and the mixed powder was dispersed in water at room temperature, the emulsifier system was added to the water and mixed for 20 minutes. The oil components were mixed and added as an oil phase to the mixture at room temperature, the mixture was homogenized for 2 minutes in an Ultra-Turrax mixer at 8000 rpm (approximately 133 Hz) at room temperature (in specific heating) and then stirred gently for a few minutes.
Hot dispersion., - creams The powders of xanthan gum and Konjak were dispersed in water at 80 ° C and the high HLB emulsifier was added and mixed for 20 minutes at 80 ° C. The low HLB emulsifier was added to a mixture of the oil components forming the oil phase and heating to 80 ° C. The thickener followed by the oil phase was then added to the water phase with stirring. The mixture was then homogenized for 2 minutes in an Ultra-Turrax mixer at 800 rpm (about 133 Hz) at 80 ° C and the emulsion was then allowed to cool to room temperature under gentle stirring.
Cold dispersion.- Creams The powders of xanthan gum and Konjak were dispersed in water at room temperature and the high HLB emulsifier was added and mixed for 20 minutes at room temperature. The low HLB emulsifier was added to a mixture of the oil components forming the oil phase. The thickener component (s) were added to the aqueous phase and the oil phase was then added with stirring. Mix then it was homogenized for 2 minutes in an Ultra-Turrax mixer at 800 rpm (approximately 133 Hz) at room temperature (with specific heating) and then shaking gently for a few minutes.
Test methods: Viscosity.- It was measured with a Brookfield RVDI + viscometer using an appropriate spindle (RV2, RV3, RV4 or RV6 depending on the viscosity of the emulsion to be tested) at 6 rpm (0.1 Hz), one day after it marks the emulsions and the Results are indicated in mPa. s Stability.- It was evaluated when observing the emulsions after storage at room temperature (Amb), cooled at 5 ° C or under storage at an elevated temperature at 40 ° C and 50 ° C. The measurement of storage stability at 50 ° C is a very severe test. The times at which the stability assessments or viscosity measurements were made are abbreviated with "" D "= day; "" W "'= week and" "M1' = month; a" "0" for stability indicates that the emulsion can not be evaluated satisfactorily or that it was suspended before the first assessment. Appearance (abbreviated "" aparien1 ') was visually assessed by sensation to the skin using the following classifications: 1 Very good.- It has a highly suitable appearance for final use and good skin feeling with good thinning of the shear. 2 Good.- It has a suitable appearance for end use, immoderate skin sensation with some thinning of the cutting effort. 3 Acceptable.- Appearance and sensation to the skin are acceptable for final use. 4 Poor.- Appearance is something fibrous and slug and the sensation to the skin is not particularly good. 5 Very poor.- The appearance is very fibrous and sluggish and poor feeling to the skin. State.- The fluidity of the emulsions of the product was visually assessed and the comments are descriptive in relation to the type of product proposed (milk, cream, etc.) Drop size.- It was visually evaluated with a Zeiss Janalumar microscope under polarized light using colored lambda filters. The results are indicated as an interval for most of the particles in micras (μm). Example 1 Milk, cosmetic, liquid water emulsion formulations were prepared using the hot process described above to make milk emulsions. The emulsion compositions are set forth in Table la and the results of the test in Table Ib below.
Table Ib These formulations show that in the presence of the polysaccharide stabilizer, at 1% emulsifier, the emulsion was not stable against the shake and rapid dissolution (in less than a day). The inclusion of still very low levels of polysaccharide stabilizer gives emulsions with extended stability even at elevated temperatures.
Example 2 A series of emulsions was made using various polysaccharide stabilizers, in combination with an alcohol ethoxylate emulsifier, using the hot process described above to make milk emulsions. The compositions are set forth in Table 2a and the results of the test in Table 2b below.
These results show that the use of a combination of polyglucomannan and xanthan as the stabilizer of polysaccharide gives stable emulsions, while the other combinations give emulsions that have poor stability (at most).
Example 3 In this example, emulsions were made using the hot method incorporating various amounts of Konjak (Konjak PA) and xanthan gum (Keltrol F) as the polysaccharide stabilizer were included in a basic aqueous emulsion including 0.05% EM emulsifier, 20% emollient oil 1, 1% Preservative Pre 1 with 100% water. The amount of Konjak PA, Keltrol F and the weight ratio of the two is included in Table 3 below. From the table, it can be seen that the best stability of the emulsions is obtained when the weight ratio between the Konjak gum and the xanthan gum in the polysaccharide stabilizer is about 50:50. For emulsions containing 0.05% total stabilizer, those that do not contain polysaccharide stabilizer or only one of Konjak and xanthan do not give emulsions that were sufficiently stable to the test. When both polymers were used, the stability improves as the ratio reaches 50:50; those in the range of 30:70 to 70:30 have generally good stability. Similarly, the appearance improves as the ratio approaches 50:50; those in the range of 30:70 to 70:30 that have generally good looks. For emulsions containing 0.5% total stabilizer, the emulsion made using Konjak only has poor stability although its appearance was good; the emulsion made using xanthan has only moderate stability good, but poor appearance; and the emulsion made using equal amounts of Konjak and xanthan gave a very good stability but had poor appearance. This suggests that the use of more Konj ak / Xanthan than necessary provides an emulsion stability that contributes to thickening with a rheological profile that is not particularly attractive for personal care applications.
Table 3 * unprocessed stable emulsion ** too high emulsion viscosity for Brookfield measurement RDVI + Example 4 In this example, several emulsions were made using various amounts of emulsifier using the hot emulsification method described above for milk-type emulsions. The compositions are set forth in Table 4a and the test results in Table 4b below. These data indicate that the use of an emulsifier in excess of what is necessary to emulsify the oil phase can have a detrimental effect on the stability of the emulsion. * stable unprocessed emulsion Example 5 Oil-in-water, milk, cosmetic, liquid emulsion formulations were made using the formulations set forth in Table 5a below using the hot process described above to make milk emulsions using fatty acid esters of polyhydroxylic materials which They occur naturally. A comparison was made not using an emulsifier, 5. C, but a stable emulsion can not be made without the emulsifier. The results, set forth in Table 5b, show below that stable emulsions can be easily made in a remarkable manner with sucrose esters, particularly sucrose esters with a high mono-ester content. The level of emulsifier required is greater than the minimum necessary with alcohol ethoxylate emulsifiers in cosmetic milk formulations with triglyceride oil Arlamol M812 (Oil 1). As with alcohol ethoxylates there is a plateau of emulsion stability, for these emulsifiers at about 0.5 to about 1% by weight of the emulsion. The polyglycerol ester can form an emulsion of moderate stability and thus appears to be a less effective emulsifier than the sucrose esters in this type of system.
Table 5a Example 6 This example compares hot and cold emulsification methods for preparing emulsions of the invention. Examples 6.1 to 6.3 were prepared by the hot emulsification method. Examples 6.4 to 6.6 were made by the cold emulsification method using the same level of polysaccharide stabilizer and Examples 6.7 to 6.9 were made by the cold emulsification route using a higher level of polysaccharide stabilizer. The results indicate that emulsions can be made by any route, but that cold emulsification gives somewhat coarse emulsions that may have less stability unless an increased level of polysaccharide stabilizer is used. t o L? Table 6b ~ Co n n e ng co e nts by mixing Xantaneon to Powder indicates the subdivision status of the mixed powders of Xantane-Konj ak Disp indicates how easily the mixed powders of Xantano-Konj ak are dispersed in High intensity mixed low water Residue indicates when xanthan or Konjak was left as a residue after high intensity mixing.
Example 7 This example illustrates emulsion creams, that is, emulsions of a relatively high viscosity, which are thickened by the inclusion of amphiphilic materials and / or waxes, which are processed by the hot dispersion route and stabilized according to the invention. For this example, the oil phase which includes amphiphilic thickening materials has the following composition: Materials Parts Weight parts by weight of the material Components Oil components thickeners Oil 7 4 TH 2 4 Oil 8 1 TH 3 3 Oil 2 1 TH 10 3 Oil 6 2 Oil 5 1 The formulation 7. C.l was emulsified / stabilized by alcohol ethoxylate surfactants at a conventional level. (5% of the total emulsion) for this type of product. Example 7.1 uses a similar level of emulsifier with Xantano / Konj ak as stabilizer. Examples 7.2 to 7.5 use Xanthan / Konj ak as stabilizer and alcohol ethoxylate emulsifiers having a range of HLB values at more closely optimized levels (1% emulsifier and total stabilizer) for this type of products according to the invention . Using emulsifier EM5, the viscosity of the initially produced cream was relatively low (the product had the consistency of a thick milk) so that the example was re-run as 7.4 including a complementary thickener (TH1). The resulting product has a viscosity similar to that of the reference with a lighter skin feel. In Examples 7.6 and 7.7 and the associated comparative runs, a small amount of alkali (10% aqueous NaOH) was added to raise the pH to about 6.5. This comprised a modest improvement in stability when Brij 78 is used. In terms of stability, the stability of 7.1 is somewhat better than that of the reference, but the improved stability obtained using lower levels of emulsifier indicate that larger amounts of emulsifier, beyond those necessary to provide adequate emulsification, they can interfere with the stabilizing effect of combination of polysaccharide stabilizer. Examples 7.1 to 7.4 also indicate that, for this type of oil phase, the relatively more hydrophilic emulsifiers give better results. Examples 7.5 to 7.7 confirm that the slightly lower HLB emulsifiers can be used although the stability results are not completely good. Examples 7.8 and 7.9, sucrose esters (higher mono-esters) were used, as emulsifiers, the cream products have good stability, appearance and feel to the skin and satisfactory viscosity although somewhat lower than that obtained using the ethoxylate emulsifiers of alcohol. The formulations of the Example are set forth in Table 7a and the results of the test in Table 7b below.
Table 7a 1. Additional amphiphilic thickeners included 2% TH 2 and 3% TH3 2. Approximately 0.05% aqueous solution of 10% NaOH was added to increase the pH.
Table 7b Example 8 This example illustrates creams, ie emulsions of relatively high viscosity, made by the cold dispersion route, which are thickened by the inclusion of polymeric thickeners, stabilized according to the invention.
Table 8b Example 9 This example investigates the effect of pH and electrolyte on the stability of the emulsions made by the hot dispersion route. The basic formulation used was that of Example 3.1 (Example 9.4 and 9.8). In Examples 9.1 to 9.3, the pH was reduced by adding lactic acid and in Examples 9.5 to 9.7, it was increased by adding sodium hydroxide. In Examples 9.8 to 9.10, increasing amounts of salt (NaCl) were added to the composition to test stability. Table 9 possibly exposes the properties and results of the stability test for the obtained emulsions. These data show that the emulsions become progressively less stable as the pH is reduced; the effect is particularly marked when the pH is reduced below 4. At alkaline pHs, the emulsions become less stable, but remain stable even when the pH is above 9 except under extreme storage conditions at 50 ° C , when the emulsion is moderately stable, but becomes discolored (yellow) indicating that the chemical degradation of some of the components has occurred. The emulsions also become less stable as the salt concentration increases, indicating that the stabilization of Xantano / Konj ak is sensitive to electrolyte.
Table 9 In this example, the effect of including perfume and preservative additives of types commonly used in personal care emulsions made by the hot dispersion route is investigated. The compositions used are set forth in Table 10a and the test results in Table 10b below.
Table 10a Table 10b Example 11 This example compares the emulsification and stability of the compositions including a range of emollient oils, of different polarity, and includes a comparison of a combination of Xanthan / Konj ak against a combination of xanthan gum / acacia as emulsion stabilizers. The emulsions are processed by the hot dispersion route. The compositions in the test emulsions are set forth in Table Ia and the results of the test in Table llb below. Examples 11.4 to 11.7 include compositions made using minimal amounts of emulsifier and for particularly non-polar Oil 2 (Arlamol E) in Example 11.5, the amount of emulsifier / stabilizer is better than would be desirable in a practical system for stability. optimum It is also noted that in Example 11.7 using Oil 4 (dimethicone oil) the emulsification was not good with relatively large oil droplets. The droplet size could be reduced by using a higher level of emulsifier.
Tabla lia IS to L? or L? L? Table llb LO Example 12 In this example, the effect of including water-soluble additives, co-solvents, and chemical and physical sunscreens in emulsions made by the hot dispersion route is investigated. The compositions used are set forth in Table 12a and the test results in Table 12b below. As expected, in general the. Inclusion of water-soluble additives and co-solvents reduced the stability of the emulsions. The oil-soluble chemical sunscreens in Examples 12.9 to 12.11 have little, if any, adverse effect on the stability of the emulsion. Water-soluble sunscreens were not included in these tests because they are generally ionic and will thus destabilize the emulsion. In 12.12 a physical sunscreen (titanium dioxide) was used, but as the dispersant for titanium dioxide is a dispersant of sodium polyacrylate, the electrolyte affected the stability of the emulsion. This was confirmed separately by including amounts as small as 0.1% by weight of conventional polyacrylate dispersants in emulsions using the emulsifier stabilizing system of the invention and finding that substantially reduced the stability of the emulsion, Table 12a Table 12b Example 13 In this example, emulsions were made by the hot dispersion route using various grades of Konjak and xanthan in combinations such as the emulsion stabilizer. The compositions are given in Table 13a and the test results in Table 13b below. Table 13a Table 13b Example 14 A milk emulsion was made by the dispersion route using a citrate trans-ester as a low HLB emulsifier. The composition and test results are set forth in Table 14 below.
Table 14 Example 15 In this Example, several creams were made using different types of thickener. The basic emulsion formulation was 20% by weight of oil 1.1% by weight of pre-1, 0.9% by weight of emulsifier / emulsion stabilizer, an amount of several thickeners indicated in Table 15 below and water up to 100% in weigh. The emulsifier stabilizer system was based on a combination of one part by weight of PS1 as emulsion stabilizer, 6 parts in weight of EM 8 as a high HLB emulsifier and two parts by weight of EM 10 as a low HLB emulsifier. In the comparative runs, the polysaccharide stabilizer was omitted, but the emulsifiers were included. The runs 15.1, 15.1.C, 15.3 and 15.3. C used hot dispersion route and runs 15.2 and 15.2. C used the cold dispersion route. Table 15 below gives variable formulation information and test results.
Table 15 * slightly sticky * * fibrous Example 16 A range of emulsion compositions was made using the emulsifier stabilizer composition used in Example 15, the basic emulsion having the following composition: Oil Phase Watery Phase Oil 7 4 PS7 0.1 Oil 8 1 EM8 0.6 Oil 2 1 EM10 0.2 Oil 6 2 Addl 4 Oil 5 1 Pre2 0.7 to Water 100 The viscosity of the compositions was varied by the inclusion of thickening components. In the sequence from 16.1 to 16.4, the viscosity was increased from that of a fluid milk to a cream with all the compositions deriving from the same basic emulsion. Runs 16.1 used the cold dispersion route and runs 16.2, 16.3 and 16.4. C used the hot dispersion route to aid the incorporation of the added thickening components (which are solid at room temperature).
The thickening components in the test results are indicated in Table 16 below. Compositions 16.1 and 16.2 were fluid milks and 16.3 and 16.4 were creams. All the compositions had a light skin feel, very good spreading properties and good stability.
Table 16 Example 17 This example illustrates emulsions with variations in oil concentration, including emulsions with high and low oil concentration, made using variable proportions of emulsifier and polysaccharide stabilizer using the cold dispersion method. The composition (ES 17) of emulsifier / emulsion stabilizer used included two parts by weight of EM1, 13 parts by weight of EM5, 2 parts by weight of EM11 and 2 parts by weight of PS7. The emulsions were made by the cold emulsification route using 5% (Example number 17.1), 20% (Example number 17.2) and 40% (Example number 17.3) by weight of oil 1.1% of Pre1 and 0.25% ( runs "a"), 0.5% (runs "b"), 0.75% (runs "c") and 1% (runs "d") of ES 17 with water at 100% by weight. The results of the viscosity and stability test are reported in Table 17 below. The flexibility of the emulsifier stabilizer system of the invention is clear although no attempts were made to optimize the formulation for the particular oil content or amount of the emulsion stabilizer used.
Table 17 Example 18 This example illustrates emulsions with very high oil concentrations and their dilution at typical concentrations of cosmetic use. A base formulation having the following composition was prepared by the hot dispersion route: Parts Parties Oil 1 80 EM11 0.2 PS7 0.2 Prel 1 EM5 1.3 water 17 EM1 0.2 This emulsion of base formulation had a viscosity of 128500 mPa.s. Several (cold) dilutions were made and tested with water (including additional preservative). These formulations and the test results are set forth in Table 18 below. The diluted emulsions were very dilute milk (near water) showing some signs of separation of an aqueous phase during storage, especially at high temperature, but without signs of emulsion dissolution. This is contracted with Example 17 where emulsions with low oil content made directly did not show this kind of separation.
Table 18 Example 19 Using an emulsifier stabilizer (ES 19) containing 0.1 parts of PS 7, 0.65 parts of EM 5, 0.1 parts of EM 1 and 0.1 parts of EM 11, several high oil emulsions were made, using the Cold dispersion route, and they were tested. The formulations are summarized and the results of the tests are shown in Table 18 below. These data indicate that highly concentrated emulsions can be made within the invention having at least moderate stability.
Table 19 Example 20 This example illustrates the use of emulsions of the invention in makeup removers. The so-called "waterproof mask1" is used as a test material for makeup removal because it is usually based on water-insoluble oils and represents a tough target for make-up removers.Wet oils are effective removers, with non-polar oils that are generally better than polar oils, but in practical use, clean oils tend to leave the skin oily.In general, emulsion formulations are less effective than clean oils and emulsifying oil in water in general, they are less effective than water-in-oil emulsions. because the water-in-oil emulsions have the oil in the external (continuous) phase so that the oil is in direct contact with the makeup. The test comprises coating the artificial skin with the mask and attempting to remove it using a pad impregnated with the stripper composition worked through the artificial skin with a mechanical arm. The degree of removal is measured by the difference in the reflectance (delta) of the skin before and after the removal of the mask. The tests are run in sets of replicas and the results cited below are the mean and standard deviation of the measured deltas. The ability of several compositions to remove the "waterproof mask" was valued. Three types of formulation were tested with two types of oil: Oil 3 is a low polarity oil and Oil 14 is a medium polarity oil. The formulations of clean oil and oil-in-water emulsions emulsified and stabilized with EM 4 (a mixture of high and low HLB alcohol ethoxylates were used for comparison with the oil-in-water emulsions of the invention emulsified and stabilized by the formulation used in example 19.
Table 20 * 0.1 parts of a thickener (Carbopol 2050) was included to increase the viscosity of the emulsion sufficient to test it in the artificial test.
These results show that emulsions using EM 4 are much less effective than clean oils although, because the continuous phase is aqueous, there is a very reduced tendency to a greasy feeling. The emulsions of the invention are comparable in effectiveness of mask removal to clean oils and greatly avoid the greasy feeling.
Example 21 This example illustrates the preparation of suspoemulsions in which an oil-in-water emulsion further includes dispersed pigment. The components of the formulations are set forth in Table 21a below. The suspo-emulsions are made as follows: The pigments are mixed and pre-milled in a laboratory mill. The water was heated to 80 ° C and the sugar surfactant (EM 12) and the polymeric stabilizer (PS 11) were dispersed in the water with stirring. The thickener (TH 4) was added and the mixture was subjected to intensive agitation for 5 minutes. The glycerin and the preservative were then added and mixed followed by the dispersion of the pigments in the water phase under intensive agitation. The oil phase was prepared by heating the oily components to 80 ° C including the oil-soluble emulsifier (if used). The oil phase was added to the water phase with stirring and the formulation was homogenized for 2 minutes using an Ultra-Turrax mixer (a about 10,000 rpm, approximately 170 Hz) and the mixture was allowed to cool to room temperature under stirring.
Table 21a Example 21.1 was a fluid milk that had good pigment dispersion and very good skin feeling. Example 21.2 was a viscous cream that had good pigment dispersion and a very good skin feel. Some properties and the sketch of storage stability data are given in Table 21. b below.
Table 21b Example 22 An emulsion was made for use in fabric impregnation. The components of the formulation are given in Table 22a below. The emulsion was processed by the hot process with the polymeric stabilizer (PS7) and kept in the aqueous phase and the emulsifiers (EM 1 and EM 3) in the oil phase (paraffin liquid).
Table 22a The emulsion was a very fluid white milk that was well suited for impregnation into tissue.
Some properties and the summary of the storage stability data are given in Table 22. b below.
Table 22 Example 23 This example illustrates suspo-emulsions with physical sunblocks such as the suspended solid phase. In Example 23a, Examples 23.1 to 23.4 are sunscreen milk from oil-in-water spray with physical sunscreen and, in Example 23b, Examples 23.5 'to 23.8 are oil-in-water sunscreen milk using pre-dispersed physical sunscreens. The compositions of the formulations and their measured viscosities are set forth in Tables 23a and 23b below. The formulations of Examples 23.1 to 23.4 are made by the cold process except that the oil phase, including EM 1 and EM 2 emulsifiers, were heated only sufficiently to melt the emulsifiers, using the following procedure. The polymeric stabilizer was dispersed in the water and stirred until homogeneous, then added and the thickener (TH 4) and under agitation until homogeneous. Then titanium dioxide (Add 18) was added and stirred to give uniform dispersions and the other additive (Add 9) and the preservative were added under stirring. The oil components (Oil 2 and Oil 3) and emulsifiers EM 1 and EM 2 were mixed and heated to melt the emulsifiers and the oil phase was slowly added to the water phase to give a homogeneous mixture. The mixture was homogenized for 2 minutes and then stirred until the emulsion was uniform.
L? or L? L? Table 23a Lp The formulations of Examples 23.5 to 23.9 were made by the following procedure. The water was heated to 80 ° C and the other components of the water phase (polymeric stabilizer and emulsifier EM 13) were added and the water phase was maintained at 80 ° C for 30 minutes with stirring (to swell the emulsifier). The mixture was then homogenized for 30 seconds (using a PowerGen 720 homogenizer at a rate adjusted to 6.5; 8750 rpm approximately 145 Hz). The oil phase was made separately by heating the mixed components of the oil phase, (Oil 3, oil 9, Add 19 and Add 20) at 80 ° C under agitation. The oil phase is then added to the water phase while stirring gently. The mixture was then emulsified by homogenization, above 65 ° C, for 1 minute (using a PowerGen 720 homogenizer at a set rate of 6; 10,000 rpm at about 170 Hz) and then allowed to cool to room temperature under slow stirring. The compositions used and the viscosity of the emulsions are set forth in Table 23b below: NJ NJ L? or L? Table 23b All emulsions were stable, showing no signs of separation, after one week of storage at 4 ° C, at room temperature, 46 ° C and through the freeze-thaw cycle (three cycles of -5 ° C / 40 ° C ).
Example 24 This example illustrates an emulsion of the invention that includes an insect repellent. The polymeric stabilizer was dispersed in the water with stirring until homogeneous and the remaining components of the water phase (emulsifiers (EM 15 and EM 16) were then added with stirring The components of the oil phase (emulsifier EM 14, Oil 9, Oil 3, Oil 12, Add 21 and Add 22) were mixed and then slowly added to the aqueous phase with stirring.The mixture was then homogenized for 2 minutes and the mixture was stirred gently until the emulsion was homogeneous at The preservative is added The compositions used and the viscosity of the emulsions are set forth in Table 24 below.
NJ NJ? or L? or L? Table 24 < JD All emulsions were stable, showing no signs of separation, after one week of storage at 4 ° C, at room temperature, 46 ° C and through the freeze-thaw cycle (-5 ° C / 40CC, 3 cycles) although after the first freeze-thaw cycle, a slight trace of oil was visible on the top of the emulsion, but this does not tend to worsen in subsequent cycles.
Example 25 This example illustrates an oil-in-water-in-oil multiple emulsion (OWO) made according to the invention. The multiple emulsions were made by first elaborating a primary oil-in-water emulsion stabilized according to the invention and subsequently emulsifying this in an external oil phase. The dispersible or water soluble components, the polymeric stabilizer (PS16) glycerol (Addl) and preservative (Pre 1), were gradually added to the water with stirring (speed 800-1000 rpm) and the stirring was continued for about 10 minutes to disperse completely these components and the aqueous mixture was heated to 80 ° C. The components of the oil phase (Oil 12, Oil 13, Oil 14 and EM 3) were mixed and heated to 70 ° C and this oil phase was added to the aqueous phase with stirring (speed 800-1000 rpm). The mixture was homogenized for 2 minutes at high speed using an Ultra-Turrax (+/- 10000 rpm) and the softest stirring was continued for several minutes, stirring for a few minutes (speed 800-1000 rpm) until the appearance of the emulsion was homogeneous and the emulsion was allowed to cool to room temperature under stirring at room temperature. The multiple emulsion was made by mixing the secondary oil phase (Oil 2, Oil 12 and Oil 3) and dissolving the polymeric emulsifier (EM 17) in the oil mixture by stirring and heating at 40 to 45 ° C. The primary emulsion was slowly added to the secondary phase of oil under moderate agitation and the mixture was homogenized for 1 minute at 9600 rpm with an Ultra-Turrax mixer. The emulsion was then gently stirred until a homogeneous appearance was obtained. The composition of the multiple emulsion is shown in Table 25: NJ NJ L? OR Table 25a Ex. Multiple emulsion components No. Primary oil emulsion in water PS16 Addl Pre2 EM3 Oil Oil Oil Water KJ . 1 12 13 14 0.1 0.7 0.9 10 to 100 Multiple emulsion of oil in water in oil Emulsion External components of primary .a Oil Phase EM18 Oil Oil Oil 2 12 3 75 3.5 10.5 5.5 5.5 NJ NJ L? or s? or L? Table 25a (continued) NJ The viscosities of the emulsion were measured (RV3 spindle) and the storage stability was assessed and the results are shown in Table 25b below.
Table 25b All the emulsions were very liquid emulsions of low viscosity. Microscopic examination with a microscope Jenalumar using a lambda filter and an increase of lOOOx showed that the emulsion contained drops of oil in water and droplets that appear to be water droplets (no oil droplets visible on them.
Example 26 This example illustrates water-in-oil-in-water multiple emulsion (WOW) made according to the invention.
The water-in-oil primary emulsion was made by separately mixing and heating to approximately 75 ° C, the components of the aqueous phase (water and Pre 1) and the components of the oil phase (EM 17, Oil 2, Oil 3 and Oil 12), slowly adding the aqueous phase to the oil phase under gentle agitation, homogenizing for 1 minute and then allowing the water-in-oil emulsion to cool to approximately 40 ° C under gentle agitation, homogenizing again and then leaving. The emulsion is cooled to room temperature under gentle agitation. Multiple emulsions were prepared by adding the surfactant (EM 1, EM 5 and EM 7) to the water with gentle agitation, then adding the EM 18 and continuing the agitation for approximately 10 minutes, adding the polymeric stabilizer (PS 16), the The mixture was heated to 80 ° C and homogenized for 2 minutes. The primary emulsion was then added under moderate agitation, followed by the preservative and a second low energy homogenization was carried out and the emulsion was stirred until homogeneous and allowed to cool to room temperature.
Table 26a The viscosities of the emulsion were measured (spindle RV3) and the storage stability of the emulsions was evaluated and the results are given in the Table 26b later. Microscopic examination of the emulsion (as in Example 25) clearly showed that most of the drops were from water-in-oil emulsion droplets.
Table 26b

Claims (33)

  1. CLAIMS 1. An oil-in-water, personal care or cosmetic emulsion that includes as an emulsifier stabilizer system, an emulsifier for the oil and a polysaccharide combination of a xanthan polysaccharide and polyglucomannan polysaccharide.
  2. 2. An emulsion according to claim 1, wherein the polyglucomannan polysaccharide has a random glucose / mannose structure at a molar ratio of glucose to breadmaker from 1: 1.5 to 1:
  3. 3. An emulsion according to any claim 1 or claim 2, wherein the polyglucomannan polysaccharide is a polyglucomannan derived from Konjak.
  4. 4. An emulsion according to any of claims 1 to 3, wherein the weight ratio of xanthan to polyglucomannan is from 1:10 to 10: 1, particularly 2: 1 to 1: 2.
  5. 5. An emulsion according to any one of claims 1 to 4, wherein the polysaccharide combination of a xanthan polysaccharide and polyglucomannan polysaccharide is present as from 0.02 to 0.5%, particularly from 0.025 to 0.15%, by weight of the emulsion.
  6. 6. An emulsion according to any of claims 1 to 4, wherein the emulsifier is or includes one or more nonionic emulsifiers selected from: a) alkoxylate emulsifiers, particularly fatty acid ester derivatives, ethers, hemi-acetals or acetals of polyhydroxy compounds or a fatty acid amide which is N-substituted with the residue of a polyhydroxy compound; b) fatty acid esters, ethers, hemi-acetals of polyhydroxy compounds, or a fatty acid amide that is N-substituted with the residue of a polyhydroxy compound, particularly a fatty acid ester of saccharide.
  7. 7. An emulsion according to claim 6, wherein the emulsifier is or includes one or more alcohol alkoxylates, particularly ethoxylates.
  8. An emulsion according to claim 6, wherein the emulsifier is or includes one or more fatty acid saccharide esters and a sugar, particularly sucrose, fructose and / or glucose in which the monoester content is at least 60%.
  9. 9. An emulsion according to any of claims 1 to 8, wherein the amount of emulsifiers from 0.02 to 1.5%, particularly from 0.1 to 1.5% by weight of the emulsion.
  10. An emulsion according to claim 9, wherein the emulsifier is or includes at least one alkoxylate emulsifier with an average of 10 to 100 alkylene oxide residues and having an HLB greater than 12 and the amount of emulsifier used is from 0.4 to 0.1% by weight of the emulsion.
  11. 11. An emulsion according to any of claims 1 to 10, wherein the emulsifier includes at least one hydrophilic nonionic emulsifier having an HLB of at least 12 and at least one non-ionic hydrophilic emulsifier an HLB of at least 12 and less a non-ionic hydrophobic emulsifier having an HLB of less than 8.
  12. An emulsion according to claim 11, wherein the hydrophilic emulsifier is or includes at least one of alkoxylate emulsifiers with an average of 10 to 100 residues of alkylene; sugar monoesters; polyglycerol monoesters; hydrocarbyl polysaccharides; glycerol esters of fatty acids where the fatty acid has 8 to 12 carbon atoms; and N-sugar amides of fatty acids such as glucamides, and the hydrophobic emulsifier is or includes at least one of emulsifiers of alkoxylate with an average of 2 to about 10 alkylene oxide residues; glycerol esters where the fatty acid has 14 to 24 carbon atoms; and fatty esters of anhydrous saccharides.
  13. An emulsion according to any of claims 11 or claim 12 wherein the amount of the hydrophilic emulsifier is from 0.04 to 0.05% by weight of the emulsion and the amount of the hydrophobic emulsifier is from 0.1 to 1% by weight of the emulsion.
  14. 14. An emulsion according to any of claims 1 to 13 wherein the oil phase is or includes an emollient oil.
  15. 15. An emulsion according to claim 14, wherein the emollient oil is or includes at least one normally liquid emollient oil selected from mineral oils, paraffin oils, vegetable glyceride oils, animal glyceride oils, synthetic ester oils, synthetic ether oils, silicone oils, propoxylates of fatty alcohol or a fat or liquefiable, solid, emollient wax or a mixture of these emollients.
  16. 16. An emulsion according to any of claims 1 to 15 in which the oil phase is at least 5% by weight of the emulsion.
  17. 17. An emulsion according to any of claims 1 to 16 in the form of a milk having a low shear viscosity from 100 to 10000 mPa. s.
  18. 18. An emulsion according to any of claims 1 to 16 in the form of a cream having a low viscosity of constant stress from 30000 to 80000 mPa.
  19. 19. An emulsion according to claim 18, in the signature of a cream that includes as one thickener one or more fatty amphiphiles and / or one or more polymeric thickeners.
  20. 20. An emulsion according to any of claims 1 to 19, which includes: from 1 to 80% of at least one oil; from 0.02 to 1.2% of at least one alkoxide emulsifier having an HLB of at least 12; optionally from 0.1 to 1.2% by weight of at least one emulsifier having an HLB of less than 8; the total amount of the emulsifier which is from 0.02 to 1.5% by weight; from 0.02 to 0.5% of at least one polysaccharide stabilizer; optionally 0.1 to 10% by weight of at least one thickener; the rest that are minor components and additives and water.
  21. 21. An emulsion according to any of claims 1 to 19, which includes: from 1 to 80% of at least one oil; from 0.02 to 1.2% of at least one alkoxide emulsifier having an HLB of at least 12; optionally from 0.1 to 1.2% by weight of at least one emulsifier having an HLB of less than 8, - the total amount of the emulsifier being from 0.02 to 1.5% by weight; from 0.02 to 0.5% of at least one polysaccharide stabilizer; optionally 0.1 to 10% by weight of at least one thickener; the rest that are minor components and additives and water.
  22. 22. An emulsion according to any of claims 1 to 21, having a pH of from 4 to 9.
  23. 23. An emulsion according to any of claims 1 to 22, further including one or more of: preservatives; perfumes; humectants or solvents; sunscreens or sun block materials; alpha-hydroxy acids; self-tan agents; antimicrobial agents, vitamins and their precursors, - skin care agents; phospholipids; formulations containing vesicle; germanium containing compounds; botanical extracts; skin whiteners; skin repair compounds; caffeine; cooling adhesives; insect repellents; insect repellents; essential oils and pigments.
  24. 24. A method for making an emulsion according to any of claims 1 to 23, by direct emulsification, in which the emulsifier (s) and the polysaccharide stabilizer are incorporated into the aqueous phase, optionally including thickener components in the aqueous phase and then mixing the oil in the aqueous continuous phase to emulsify it.
  25. 25. An emulsion according to claim 24, wherein the polysaccharide stabilizer in the aqueous phase is heated above about 60 ° C and / or is subjected to high intensity mixing.
  26. 26. A method for making an emulsion according to any of claims 1 to 25, by inverted emulsification, in which the emulsifier (s) and the polysaccharide stabilizer are incorporated in the oil phase and the aqueous phase is then Mix in the oil phase until the system reverses to form an oil-in-water emulsion.
  27. 27. A method according to claim 26, wherein the polysaccharide stabilizer in contact with the aqueous phase is heated above about 60 ° C and / or subjected to high intensity mixing.
  28. 28. A dry mix emulsifier stabilizing formulation that includes an oil emulsifier and an oil in water emulsion stabilizer that is a combination of a polysaccharide of a xanthan polysaccharide and a polyglucomannan polysaccharide.
  29. 29. A formulation according to claim 28, which additionally includes a sugar.
  30. 30. A dry blend according to either claim 28 or 29 which includes: from 2 to 10 parts by weight of Xanthan; from 2 to 10 parts by weight of polyglucomannan; the weight ratio of xanthan to polyglucomannan which is from 1: 4 to 4: 1; from 30 to 75 parts by weight of an emulsifier having an HLB of at least 12; optionally from 5 to 40 parts by weight of an emulsifier having an HLB of less than 8; and optionally from 2 to 10 parts by weight and milling activity (sugar).
  31. 31. A dry mixture according to any of claims 28 to 30, having an average particle size of about 100 to about 500 μm.
  32. 32. A dry mix according to the claim 31, wherein the proportion of particles of size less than 50 μm is less than 2% by weight.
  33. 33. The use of a polysaccharide combination of a xanthan polysaccharide and a polyglucomannan polysaccharide as an emulsifier stabilizing system in oil-in-water, cosmetic or personal care emulsions.
MXPA/A/2001/005622A 1998-12-05 2001-06-05 Emulsification systems and emulsions MXPA01005622A (en)

Applications Claiming Priority (2)

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GB9826699.2 1998-12-05
US60/111,440 1998-12-08

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MXPA01005622A true MXPA01005622A (en) 2001-12-04

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