111111
`
`1111111111111111111111111111111111111111111111111111111111111111111111111111
`US 20130089587Al
`
`(19) United States
`c12) Patent Application Publication
`STAUDIGEL et al.
`
`(10) Pub. No.: US 2013/0089587 A1
`Apr. 11, 2013
`(43) Pub. Date:
`
`(54) PERSONAL CARE COMPOSITIONS AND
`METHODS OF MAKING SAME
`
`(71) Applicant: THE PROCTER & GAMBLE
`COMPANY, Cincinnati, OH (US)
`
`(72)
`
`Inventors: James Anthony STAUDIGEL,
`Loveland, OH (US); Eric Scott
`JOHNSON, Hamilton, OH (US); Sean
`Michael RENOCK, Loveland, OH
`(US); Marjorie Mossman PEFFLY,
`Cincinnati, OH (US); Kelly Rose
`KROGER LYONS, Blanchester, OH
`(US)
`
`(73) Assignee: THE PROCTER & GAMBLE
`COMPANY, Cincinnati, OH (US)
`
`A61K33/30
`A61P 17100
`A61P 31100
`A61K8/891
`A61K31/444
`B82Y 5/00
`B82Y99/00
`(52) U.S. Cl.
`USPC ........ 424/401; 424/70.12; 514/188; 424/642;
`977/773; 977/786; 977/926
`
`(2006.01)
`(2006.01)
`(2006.01)
`(2006.01)
`(2006.01)
`(2011.01)
`(2011.01)
`
`(57)
`ABSTRACT
`The present invention relates to a personal care composition
`and methods of using the same, the composition including an
`anionic surfactant, a cationic conditioning polymer, and a
`silicone emulsion wherein a total content of a cyclic polysi(cid:173)
`loxane having a general formula:
`
`(21) Appl. No.: 13/646,300
`
`(22) Filed:
`
`Oct. 5, 2012
`
`Related U.S. Application Data
`
`(60)
`
`Provisional application No. 61/544,769, filed on Oct.
`7, 2011.
`
`Publication Classification
`
`(51)
`
`Int. Cl.
`A61K 81892
`A61Q5112
`A61K 8106
`
`(2006.01)
`(2006.01)
`(2006.01)
`
`is present in the silicone emulsion in an amount less than 2.5
`wt % based on the total weight of all polysiloxanes, R is a
`substituted orunsubstituted C 1 to C 10 alkyl or aryl, whereinm
`is 4 or 5, wherein the composition forms coacervate particles
`upon dilution with water, and wherein a percentage of the
`coacervate particles with a floc size of greater than about 20
`micron is from about 1% to about 60% upon dilution with
`water.
`
`1
`
`

`

`Patent Application Publication
`
`Apr. 11, 2013 Sheet 1 of 5
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`

`US 2013/0089587 AI
`
`Apr. 11, 2013
`
`1
`
`PERSONAL CARE COMPOSITIONS AND
`METHODS OF MAKING SAME
`
`FIELD OF THE INVENTION
`
`[ 0001] The present invention relates to a personal care com(cid:173)
`position and methods of making same. More specifically, it
`relates to a personal care composition including an anionic
`surfactant, a cationic conditioning polymer, and a silicone
`emulsion.
`
`BACKGROUND OF THE INVENTION
`
`[0002] Conditioning shampoos or "2 in 1" hair products
`comprising a detersive surfactant and hair conditioning
`agents are known. These personal care compositions typi(cid:173)
`cally comprise an anionic detersive surfactant in combination
`with a conditioning agent such as a silicone, hydrocarbon oil,
`fatty esters, etc. These products have become more popular
`among consumers as a means of conveniently obtaining hair
`conditioning and cleansing performance from a single prod(cid:173)
`uct.
`[0003] Many conditioning personal care compositions,
`however, do not provide sufficient deposition of conditioning
`agents onto hair or skin during the application process and if
`deposition is possible, it is only possible in formulations with
`relatively low levels of anionic surfactant. Without adequate
`deposition, large proportions of conditioning agent are rinsed
`away during the application process and therefore provide
`little or no conditioning benefit. Without sufficient deposition
`of the conditioning agent on the hair or skin, relatively high
`levels of conditioning agents may be needed. Such high levels
`of a conditioning agent, however, can increase raw material
`costs, reduce lathering, and present product stability con(cid:173)
`cerns. Additionally, limitations on total anionic surfactant in
`order to form coacervate can limit the lather potential of a
`composition, or result in the need for higher levels ofless cost
`effective amphoteric surfactants in order to achieve good
`lather.
`[0004] One known method for improving deposition of a
`hair conditioning agent onto hair involves the use of specific
`cationic deposition polymers. These polymers may be syn(cid:173)
`thetic, but are most commonly natural cellulosic or guarpoly(cid:173)
`mers that have been modified with cationic substituents.
`[0005] The formation of a coacervate upon dilution of the
`cleansing composition with water is important to improving
`deposition of various conditioning actives, especially those
`that have small droplet sizes (i.e., ~2 microns). In order to
`form a coacervate, cleansing compositions comprising typi(cid:173)
`cal cationic polymers tend to be significantly limited in total
`anionic surfactant concentrations,
`in order to achieve
`adequate levels of coacervate particles upon dilution. How(cid:173)
`ever, lower levels of anionic surfactants tend to limit the
`volume of! ather that can be achieved with a particular cleans(cid:173)
`ing composition. Thus, for cost effective, high lathering,
`coacervate-forming compositions, it is desirable to use a cat(cid:173)
`ionic polymer that can form a coacervate in the presence of
`high levels of anionic surfactant.
`[0006] But another complexity arises when the composi(cid:173)
`tion comprises an active substance, such as an anti-dandruff
`active, which also needs to be deposited on the scalp in an
`efficacious deposition amount and quality. However, excel(cid:173)
`lent deposition amount and quality of active substances, for
`example by utilizing high levels of cationic polymers and
`
`those with higher charge density, is often associated with a
`hair conditioning feel that many consumers find unaccept(cid:173)
`able.
`[0007] Consequently, needs exist for a conditioning com(cid:173)
`position that provides excellent active substance deposition
`performance without a hair conditioning and hair feel trade(cid:173)
`off.
`
`SUMMARY OF THE INVENTION
`
`[0008] These and other features, aspects, and advantages of
`the claimed invention will become evident to those skilled in
`the art from a reading of the present disclosure.
`[0009]
`In accordance with an embodiment of the present
`invention, a personal care composition is provided. The com(cid:173)
`position comprises a) an anionic surfactant; b) a cationic
`conditioning polymer; and a silicone emulsion. The cationic
`conditioning polymer is selected from at least one of i) a
`cationic guar polymer, wherein the cationic guar polymer has
`a weight average molecular weight of less than about 1 mil(cid:173)
`lion g/mol, and wherein the cationic guar polymer has a
`charge density offrom about 0.1 meq/g to about 2.5 meq/g; or
`ii) a cationic copolymer of an acrylamide monomer and a
`cationic monomer, wherein the copolymer has a charge den(cid:173)
`sity offrom about 1.0 meq/g to about 3.0 meq/g. The silicone
`emulsion comprises an insoluble polysiloxane having a gen(cid:173)
`eral formula ofR 1-[0-SiR2Jn -OR 1
`, wherein n is an inte(cid:173)
`ger, R is a substituted or unsubstituted C 1 to C 10 alkyl or aryl,
`and R 1 is a hydrogen or a substituted or unsubstituted C 1 to
`clO alkyl or aryl, wherein the insoluble polysiloxane has an
`average molecular weight within the range from about 50,000
`to about 500,000 g/mol, and an average particle size within
`the range from about 30 nm to about 10 fllll, wherein a total
`content of a cyclic polysiloxane having a general formula:
`
`is present in the silicone emulsion in an amount less than
`about 2.5 wt % based on the total weight of the insoluble
`polysiloxane and the cyclic polysiloxane, wherein R is as
`defined above, wherein m is 4 or 5, and wherein the compo(cid:173)
`sition forms coacervate particles upon dilution with water,
`and wherein a percentage of the coacervate particles with a
`floc size of greater than about 20 micron is from about 1% to
`about 60% upon dilution with water.
`[0010] According to another embodiment of the present
`invention, a method of achieving improved hair feel is pro(cid:173)
`vided. The method comprises applying to hair a composition
`comprising: a) an anionic surfactant; b) a cationic condition(cid:173)
`ing polymer; and c) a silicone emulsion. The cationic condi(cid:173)
`tioning polymer is selected from at least one of i) a cationic
`guar polymer, wherein the cationic guar polymer has a weight
`average molecular weight ofless than about 1 million g/mol,
`and wherein the cationic guar polymer has a charge density of
`from about 0.1 meq/g to about 2.5 meq/g; or ii) a cationic
`copolymer of an acrylamide monomer and a cationic mono(cid:173)
`mer, wherein the copolymer has a charge density of from
`about 1.0 meq/g to about 3.0 meq/g. The silicone emulsion
`comprises an insoluble polysiloxane having a general for(cid:173)
`mula ofR 1-[0-SiR2Jn -OR 1
`, wherein n is an integer, R is
`a substituted orunsubstituted C 1 to C 10 alkyl or aryl, and R 1 is
`
`7
`
`

`

`US 2013/0089587 AI
`
`Apr. 11, 2013
`
`2
`
`a hydrogen or a substituted orunsubstituted C 1 to C 10 alkyl or
`aryl, wherein the insoluble polysiloxane has an average
`molecular weight within the range from about 50,000 to about
`500,000 g/mol, and an average particle size within the range
`from about 30 nm to about 10 flill, and wherein a total content
`of a cyclic polysiloxane having a general formula:
`
`is present in the silicone emulsion in an amount less than 2.5
`wt% based on the total weight of the insoluble polysiloxanes
`and the cyclic polysiloxane, R is as defined above, wherein m
`is 4 or 5, wherein the composition forms coacervate particles
`upon dilution with water, wherein the coacervate particles
`have a squeeze flow viscosity of from about 1 Pa ·s to about
`100 Pa·s, and wherein a percentage of the coacervate particles
`with a floc size of greater than about 20 micron is from about
`1% to about 60%.
`[0011] According to another embodiment of the present
`invention, a method of making a personal care composition
`comprising an anionic surfactant, a cationic conditioning
`polymer, and a silicone emulsion is provided, The method
`comprises (a) combining the anionic surfactant and the cat(cid:173)
`ionic conditioning polymer in water, wherein the cationic
`conditioning polymer is selected from at least one of (i) a
`cationic guar polymer, wherein the cationic guar polymer has
`a weight average molecular weight of less than about 1 mil(cid:173)
`lion g/mol, and wherein the cationic guar polymer has a
`charge density offrom about 0.1 meq/g to about 2.5 meq/g; or
`(b) a cationic copolymer of an acrylamide monomer and a
`cationic monomer, wherein the copolymer has a charge den(cid:173)
`sity of from about 1 meq/g to about 3 meq/g; and (ii) com(cid:173)
`bining a silicone emulsion and an aqueous composition that
`includes a product of step (i) to form the personal care com(cid:173)
`position, the silicone emulsion comprising an insoluble pol(cid:173)
`ysiloxane having a general formula of R 1-[0-SiR2Jn(cid:173)
`OR 1
`, wherein n is an integer, R is a substituted or
`unsubstituted C 1 to C 10 alkyl or aryl, and R 1 is a hydrogen or
`a substituted or unsubstituted C 1 to C 10 alkyl or aryl, wherein
`the insoluble polysiloxane has an average molecular weight
`within the range from about 50,000 to about 500,000 g/mol,
`and an average particle size within the range from about 30
`nm to about 10 flill, and wherein a total content of a cyclic
`polysiloxane having a general formula
`
`is present in the silicone emulsion in an amount less than 2.5
`wt% based on the total weight of the insoluble polysiloxanes
`and the cyclic polysiloxane, wherein R is as defined above,
`wherein m is 4 or 5, and wherein the composition forms
`coacervate particles upon dilution with water, wherein the
`coacervate particles have a squeeze flow viscosity of from
`about 1 Pa·s to about 100 Pa·s, and wherein a percentage of
`the coacervate particles with a floc size of greater than about
`20 micron is from about 1% to about 60%.
`
`BRIEF DESCRIPTION OF THE DRAWINGS
`
`[0012] FIG. 1 is a graphical representation showing the
`effect of salt concentration on a floc size of a coacervate of a
`personal care composition in accordance with one embodi(cid:173)
`ment of the present invention.
`[0013] FIG. 2 is a graphical representation showing the
`effect of salt concentration on a floc size of a coacervate of a
`personal care composition in accordance with another
`embodiment of the present invention.
`[0014] FIG. 3 is a graphical representation showing the
`effect of salt concentration on a floc size of a coacervate of a
`personal care composition in accordance with another
`embodiment of the present invention.
`[0015] FIG. 4 is a graphical representation showing the
`effect of salt concentration on a floc size of a coacervate of a
`personal care composition in accordance with another
`embodiment of the present invention.
`[0016] FIG. 5 is a graphical representation showing the
`effect of salt concentration on a floc size of a coacervate of a
`personal care composition in accordance with another
`embodiment of the present invention.
`
`DETAILED DESCRIPTION OF THE INVENTION
`
`[0017] All percentages are by weight of the total composi(cid:173)
`tion, unless stated otherwise. All ratios are weight ratios,
`unless specifically stated otherwise. All ranges are inclusive
`and combinable. The number of significant digits conveys
`neither a limitation on the indicated amounts nor on the accu(cid:173)
`racy of the measurements. The term "molecular weight" or
`"M.Wt." as used herein refers to the weight average molecu(cid:173)
`lar weight unless otherwise stated. "QS" means sufficient
`quantity for 100%.
`[0018] All numerical amounts are understood to be modi(cid:173)
`fied by the word "about" unless otherwise specifically indi(cid:173)
`cated. Unless otherwise indicated, all measurements are
`understood to be made at 25° C. and at ambient conditions,
`where "ambient conditions" means conditions under about
`one atmosphere of pressure and at about 50% relative humid(cid:173)
`ity. All such weights as they pertain to listed ingredients are
`based on the active level and do not include carriers or by(cid:173)
`products that may be included in commercially available
`materials, unless otherwise specified.
`[0019] Herein, "comprising" means that other steps and
`other ingredients which do not affect the end result can be
`added. This term encompasses the terms "consisting of' and
`"consisting essentially of'. The compositions, methods, uses,
`kits, and processes of the present invention can comprise,
`consist of, and consist essentially of the elements and limita(cid:173)
`tions of the invention described herein, as well as any of the
`additional or optional ingredients, components, steps, or limi(cid:173)
`tations described herein.
`[0020] The term "substantially free from" or "substantially
`free of' as used herein means less than about 1%, or less than
`about 0.8%, or less than about 0.5%, or less than about 0.3%,
`or about 0%, by total weight of the composition.
`[0021]
`"Hair," as used herein, means mammalian hair
`including scalp hair, facial hair and body hair, particularly on
`hair on the human head and scalp.
`[0022]
`"Cosmetically acceptable," as used herein, means
`that the compositions, formulations or components described
`are suitable for use in contact with human keratinous tissue
`without undue toxicity, incompatibility, instability, allergic
`response, and the like. All compositions described herein
`
`8
`
`

`

`US 2013/0089587 AI
`
`Apr. 11, 2013
`
`3
`
`which have the purpose of being directly applied to kerati(cid:173)
`nous tissue are limited to those being cosmetically accept(cid:173)
`able.
`"Derivatives," as used herein, includes but is not
`[0023]
`limited to, amide, ether, ester, amino, carboxyl, acetyl, acid,
`and/or alcohol derivatives of a given compound.
`"Polymer," as used herein, means a chemical
`[0024]
`formed from the polymerisation of two or more monomers.
`The term "polymer" as used herein shall include all materials
`made by the polymerisation of monomers as well as natural
`polymers. Polymers made from only one type of monomer
`are called homopolymers. A polymer comprises at least two
`monomers. Polymers made from two or more different types
`of monomers are called copolymers. The distribution of the
`different monomers can be calculated statistically or block(cid:173)
`wise-both possibilities are suitable for the present inven(cid:173)
`tion. Except if stated otherwise, the term "polymer" used
`herein includes any type of polymer including homopolymers
`and copolymers.
`"Kit," as used herein, means a packaging unit com(cid:173)
`[0025]
`prising a plurality of components. An example of a kit is, for
`example, a first composition and a separately packaged sec(cid:173)
`ond composition. Another kit may comprise a first composi(cid:173)
`tion and an energy delivery device. A different kit may com(cid:173)
`types of separately packaged
`prise
`three different
`composition and a hair styling implement. A further kit may
`comprise application instructions comprising a method and a
`composition/formulation.
`[0026] The term "coacervate" as used herein, means the
`complex which forms between surfactant and polymer that
`may either be soluble or insoluble in the neat personal care
`composition, typically forming an insoluble complex in the
`neat personal care composition, and which may become less
`soluble upon dilution and thus yielding an increase in its level
`of phase separation or precipitate in solution.
`[0027] The term "floc" as used herein, means localized
`clusters of agglomerated, insoluble coacervate, which may
`comprise polymer, surfactant, water and dispersed phases
`present in the composition such as anti -dandruff active and
`silicone emulsion. Any floc size disclosed herein is obtained
`using a Lasentec Focused Beam Reflectance Measurment
`(FBRM) [model S400A available from Mettler Toledo Corp.]
`in accordance with the Lasentec Method, which is described
`below.
`[0028] The term "isotropic" as used herein, means a par(cid:173)
`ticular phase structure of coacervate wherein the structure is
`"identical along any three orthogonal directions in space, and
`is therefore dark or 'nonbirefringent' when viewed between
`crossed polarized light. (One direction is 'orthogonal' to
`another if the vector component of the first, in the direction of
`the second, is zero.)" (Laughlin, R. G. (1994). "The Aqueous
`Phase Behavior of Surfactants," 182, 8.2).
`[0029] The term "charge density" as used herein, means the
`ratio of the number of positive charges on a monomeric unit of
`which a polymer is comprised to the M.Wt. of said mono(cid:173)
`meric unit. The charge density multiplied by the polymer
`M. Wt. determines the number of positively charged sites on a
`given polymer chain. For cationic guars, charge density is
`measured using standard elemental analysis of percentage
`nitrogen known to one skilled in the art. This value of per(cid:173)
`centage nitrogen, corrected for total protein analysis, can then
`be used to calculate the number or equivalence of positive
`charges per gram of polymer. For the cationic copolymers, the
`charge density is a function of the monomers used in the
`
`synthesis. Standard NMR techniques know to one skilled in
`the art would be used to confirm that ratio of cationic and
`non-ionic monomers in the polymer. This would then be used
`to calculate the number or equivalence of positive charges per
`gram of polymer. Once these values are know, the charge
`density is reported in milliequivalence (meq) per gram of
`cationic polymer.
`[0030] The term "(meth)acrylamide" as used herein means
`methylacrylamide or acrylamide. The term "(meth)acrylic
`acid" as used herein means acrylic acid or methacrylic acid.
`In accordance with embodiments of the present
`[0031]
`invention, a personal care composition is provided, the com(cid:173)
`position including an anionic surfactant, a cationic condition(cid:173)
`ing polymer, and a silicone emulsion including an insoluble
`polysiloxane.
`It has been surprisingly found that, by formulating
`[0032]
`personal care composition with a silicone emulsion of an
`insoluble polysiloxane, e.g., poly-dimethylsiloxane, having
`at total content of cyclic polysiloxane of less than 2.5 wt %
`based on the total weight of all polysiloxanes, in combination
`with cationic guar polymers and/or cationic copolymers of
`acrylamide monomers and cationic monomers, improves the
`deposition of the conditioning polymer and the insoluble
`polysiloxane on the skin and hair can be improved with mini(cid:173)
`mal or no consumer unacceptance of hair conditioning and
`hair feel.
`[0033] Without being bound by any particular theory, it is
`believed that insoluble polysiloxanes emulsions having levels
`of cyclic polysiloxanes below the aforementioned threshold,
`provide improved consumer acceptance of hair conditioning
`and hair feel and yet also excellent on-scalp deposition. It is
`believed that cyclic polysiloxanes disrupt higher order sur(cid:173)
`factant micelle formation, which in turn requires increasing
`the amount of salt to be added to the composition in order to
`achieve acceptable rheology parameters of the composition.
`However, the observed increase in viscosity induced by the
`increased salt content may also be associated with an
`increased floc size of the coacervate, as shown in FIGS. 1 and
`2. Increasing floc size can negatively affect the on -scalp depo(cid:173)
`sition, for example, by a larger floc becoming trapped in the
`hair. By blending an anionic surfactant, a cationic condition(cid:173)
`ing polymer, and the silicone emulsion defined herein, it has
`been surprisingly found that both the consumer desirable
`benefits of the lower molecular weight cationic guars and the
`enhanced deposition of the cationic copolymers and silicone
`can be achieved in a single composition while still preserving
`the consumer desirability. Advantageously, this combination
`of surfactant, polymer and silicone is useful for the deposition
`of actives, such as anti-dandruff actives.
`[0034] More specifically, it is believed that an insoluble
`polysiloxane of a desired particle size (<10 micron) in the
`embodiments of the present invention can be delivered to the
`hair and scalp via entrapment in the coacervate microstruc(cid:173)
`ture. Insoluble polysiloxane species entrapped in the coacer(cid:173)
`vate microstructure result in a less tightly bound structure
`which can be characteristic of high deposition systems like
`cationic guar/synthetic co-polymer systems. Less tightly
`bound coacervate microstructures can be characterized by
`reduced complex coacervate rheology (CCR).
`[0035] The impact of the silicone emulsion further dictates
`the achievement of the desired reduction of coacervate floc
`size and rheology. In general, silicone microemulsions and
`nanoemulsions contain various amounts of residual cyclic
`polysiloxanes. For example, dimethiconol may include sig-
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`nificant quantities of cyclic polysiloxanes, such as octameth(cid:173)
`ylcyclotetrasiloxane and decamethylcyclotetrasiloxane. The
`cyclic polysiloxanes can significantly impact anionic surfac(cid:173)
`tant based compositions, such as shampoos, by disrupting
`higher order surfactant micelle formation, which is critical for
`achieving consumer accepted compositional viscosity tar(cid:173)
`gets. As a consequence of the higher order micelle formation
`disruption, higher levels of NaCl are added to the personal
`care composition in order to compensate for the drop in
`viscosity. However, increasing the salt level produces a larger
`coacervate particle size, which has been shown to result in a
`negative cosmetic experience. Accordingly, silicone emul(cid:173)
`sions of polysiloxanes with cyclic polysiloxanes below speci(cid:173)
`fied levels unexpectedly yield excellent deposition and qual(cid:173)
`ity, while providing improved hair feel.
`[0036] The features of the composition according to the
`first aspect, as well as the other aspects and other relevant
`components, are described in detail hereinafter. All compo(cid:173)
`nents of the composition described herein should be physi(cid:173)
`cally and chemically compatible with the essential compo(cid:173)
`nents described herein, and should not otherwise unduly
`impair product stability, aesthetics or performance.
`[0037]
`In accordance with one embodiment of the present
`invention, a personal care composition is provided, compris(cid:173)
`ing: a) an anionic surfactant; b) a cationic conditioning poly(cid:173)
`mer; and c) a silicone emulsion comprising an insoluble pol(cid:173)
`ysiloxane.
`[0038] A. Silicone Emulsion
`[0039] The silicone emulsions suitable for use in the
`embodiments of the present invention include emulsions of
`insoluble polysiloxanes prepared in accordance with the
`descriptions provided in U.S. Pat. No. 4,476,282 and U.S.
`Patent Application Publication No. 2007/0276087. Accord(cid:173)
`ingly, insoluble polysiloxanes referred to herein for the pur(cid:173)
`pose of the invention include polysiloxanes such as alpha,
`omega hydroxy-terminated polysiloxanes or alpha, omega
`alkoxy-terminated polysiloxanes having a molecular weight
`within the range from about 50,000 to about 500,000 g/mol.
`As used herein, "insoluble polysiloxane" means that the
`water solubility of the polysiloxane is less than 0.05 wt %. In
`another embodiment, the water solubility of the polysiloxane
`is less than 0.02 wt %, or less than 0.01 wt %, or less than
`0.001 wt %. According to an embodiment, the insoluble pol(cid:173)
`ysiloxane is present in the personal care composition in an
`amount within the range from about 0.1 wt %to about 3 wt %,
`based on the total weight of the composition. For example, the
`insoluble polysiloxane can be present in an amount within the
`range from about 0.2 wt% to about 2.5 wt %, or from about
`0.4 wt% to about 2.0 wt %, or from about 0.5 wt% to about
`1.5 wt %, based on the total weight of the composition.
`[0040] According to one aspect of the silicone emulsion,
`the insoluble polysiloxane used herein include alpha, omega
`hydroxy- or alkoxy-terminated polysiloxanes having a gen(cid:173)
`eral formula I:
`
`R 1-[0-SiR2Jn--OR1
`
`,
`
`wherein 'n' is an integer, R is a substituted orunsubstituted C 1
`to C 10 alkyl or aryl, and R 1 is a hydrogen or a substituted or
`unsubstituted C 1 to C 10 alkyl or aryl. Non-limiting examples
`ofR and R 1 may be independently selected from alkyl groups
`such as methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl,
`tert-butyl, n-pentyl, isopentyl, neopentyl, tertpentyl, hexyl
`such as n-hexyl, heptyl such as n-heptyl, octyl such as n-octyl
`and isooctyl such as 2,2,4-trimethyl-pentyl, nonyl such as
`
`n-nonyl, decyl such as n-decyl, dodecyl such as n-dodecyl,
`octadecyl such as n-octadecyl; or aryl groups such as phenyl,
`naphthyl, anthryl and phenanthryl. In an embodiment, the
`insoluble polysiloxane has a general formula H-[O-SiR2 ]
`n-OH.
`[0041] According to another aspect of the silicone emul(cid:173)
`sion, the insoluble polysiloxane has an average molecular
`weight within the range from about 50,000 to about 500,000
`g/mol. For example, the insoluble polysiloxane may have an
`average molecular weight within the range from about 60,000
`to about 400,000; from about 75,000 to about 300,000; from
`about 100,000 to about 200,000; or the average molecular
`weight may be about 150,000 g/mol.
`[0042] According to another aspect of the silicon emulsion,
`total content of a cyclic polysiloxane having a general for(cid:173)
`mula:
`
`wherein R is as defined above, and wherein m is 4 or 5, is
`present in the silicone emulsion in an amount less than about
`2.5 wt% based on the total weight of all polysiloxanes. For
`example, dimethiconol may include significant quantities of
`cyclic polysiloxanes, such as octamethylcyclotetrasiloxane
`(D4) and decamethylcyclotetrasiloxane (D5). In an embodi(cid:173)
`ment, the amount ofD4 is less than about 2.0%, or less than
`about 1.5%, or less than about 1.0%, or less than about 0.5%,
`based on the total weight of all polysiloxanes. In an embodi(cid:173)
`ment, the amount ofD5 is less than about 0.5%, or less than
`about 0.4%, or less than about 0.3%, or less than about 0.2%,
`based on the total weight of all polysiloxanes.
`[0043] According to yet another aspect of the silicone
`emulsion, the emulsion has a viscosity up to about 500,000
`cPs. For example, the viscosity may be within the range from
`about 75,000 to about 300,000, from about 100,000 to about
`200,000, or about 150,000 cPs.
`[0044] According to yet another aspect of the silicone
`emulsion, the insoluble polysiloxane has an average particle
`size within the range from about 30 nm to about 10 micron.
`The average particle size may be within the range from about
`40 nm to about 5 micron, from about 50 nm to about 1 micron,
`from about 75 nm to about 500 nm, or about 100 nm, for
`example.
`[0045] The average molecular weight of the insoluble pol(cid:173)
`ysiloxane, the viscosity of the silicone emulsion, and the size
`of the particle comprising the insoluble polysiloxane are
`determined by methods commonly used by those skilled in
`the art, such as the methods disclosed in Smith, A. L. The
`Analytical Chemistry of Silicones, John Wiley & Sons, Inc.:
`New York, 1991. For example, the viscosity of the silicone
`emulsion can be measured at 30° C. with a Brookfield visco(cid:173)
`simeter with spindle 6 at 2.5 rpm.
`[0046] According to another aspect of the silicone emul(cid:173)
`sion, the emulsion further includes an anionic surfactant that
`participates in providing high internal phase viscosity emul(cid:173)
`sions having particle sizes in the range from about 30 nm to
`about 10 micron. The anionic surfactant is selected from
`organic sulfonic acids. Most common sulfonic acids used in
`the present process are alkylaryl sulfonic acid; alkylaryl poly(cid:173)
`oxyethylene sulphonic acid; alkyl sulfonic acid; and alkyl
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`polyoxyethylene sulfonic acid. General formulas of the sul(cid:173)
`fonic acids are as shown below:
`
`(II)
`
`(III)
`
`(N)
`
`(N)
`
`Where R2
`, which may differ, is a monovalent hydrocarbon
`radical having at least 6 carbon atoms. Non-limiting
`examples of R2 include hexyl, octyl, decyl, dodecyl, cetyl,
`stearyl, myristyl, and oleyl. 'm' is an integer from 1 to 25.
`Exemplary anionic surfactants include but are not limited to
`octylbenzene sulfonic acid; dodecylbenzene sulfonic acid;
`cetylbenzene sulfonic acid; alpha-octyl sulfonic acid; alpha(cid:173)
`dodecyl sulfonic acid; alpha-cetyl sulfonic acid; polyoxyeth(cid:173)
`ylene octylbenzene sulfonic acid; polyoxyethylene dodecyl(cid:173)
`benzene sulfonic acid; polyoxyethylene cetylbenzene
`sulfonic acid; polyoxyethylene octyl sulfonic acid; polyoxy(cid:173)
`ethylene dodecyl sulfonic acid; and polyoxyethylene cetyl
`sulfonic acid. Generally, 1 to 15% anionic surfactant is used
`in the emulsion process. For example, 3-10% anionic surfac(cid:173)
`tant can be used to obtain an optimum result.
`[00