Title of Invention

SUBSTANTIALLY ENZYME FREE PERSONAL WASH COMPOSITIONS COMPRISING NON-SILICATES WITH BASAL LAYER CATIONIC CHARGE

Abstract The present invention relates to personal wash compositions comprising, non-silicate particles, wherein the basal layer(s) carries a net cationic charge. The use of these specific particles results in enhanced properties (e.g., enhanced foaming, hydrotroping) of the personal wash products. The invention further discloses process for decreasing viscosity and/or increasing foam comprising formulating compositions with non-silicate layer compounds as specified.
Full Text FORM - 2
THE PATENTS ACT, 1970
(39 of 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See Section 10 and Rule 13)
SUBSTANTIALLY ENZYME FREE PERSONAL WASH COMPOSITIONS COMPRISING NON-SILICATES WITH BASAL LAYER CATIONIC CHARGE
HINDUSTAN LEVER LIMITED, a company incorporated under the Indian Companies Act, 1913 and having its registered office at Hindustan Lever House, 165/166, Backbay Reclamation, Mumbai -400 020, Maharashtra, India
The following specification particularly describes the invention and the manner in which it is to be performed

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SUBSTANTIALLY ENZYME FREE PERSONAL WASH COMPOSITIONS COMPRISING NON-SILICATES WITH BASAL LAYER CATIONIC CHARGE
The subject invention relates to personal wash compositions,
5 particularly those comprising non-silicate particles having cationic charge on their basal layer. Use of such specific non-silicates results in improved properties as noted below.
It is known to use layered aluminosilicates or magnesium
10 silicates in liquid cleansing and detergent compositions to modify the rheology of the composition. The art discloses, however, that these silicate clays are used to thicken (increase the viscosity) of the liquid composition. Typically, increased viscosity is accomplished by swelling
15 or expanding of the silicates when they are in contact with water to form a "house of cards" structure. It is also commonly accepted (see for example, Luckham et al., Adv. Colloid Interface Sci, 82 (1999), 43-92.) that this house of cards structure arises from various interactions between the
20 edges and faces of the layered clays.
Typically, the silicates (e.g., aluminosilicas) have a net negative charge on the basal plane in aqueous solutions, which arises from an isomorphous substitution of certain
25 atoms in their structure for other atoms of a different
4+ 3 +
valence. Thus, for example, Si may be replaced by Al in
the lattice, leading to a net negative charge on the basal plane. Such clays are called "cationic" clays because the net negative charge on the basal plane is compensated by the
30 presence of cations in the interstitial layer. It is the
hydration and dissolution of these interstitial cations that

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leads to swelling of the clays, and the subsequent thickening effect for which they are commonly known. Figure
1 is a schematic drawing showing typical structure with net anionic charge in the basal layer and cationic charge in the
5 interstitial layer.
By contrast, in the subject invention it is critical that the clay be a non-silicate clay. A typical example of such clays are layered double hydroxides. Typically, these
10 compounds have formula corresponding to the generalformula:
MgxAl(OH)yAznH20
in which A represents an equivalent of a non-silicate
15 anionic and the conditions 1 In such clays, the metal cation in the lattice is often substituted for one of a higher valence, which leads toa
20 positive charge on the basal plane. This is thus the
opposite of the silicates described above. Such clays are often referred to as "anionic clays" because the positive charge on the basal plane is balanced by the presence of

anions like CO32- or NO3- in the interstitial layer.
25
In the present invention, the applicants have found that the •addition of the anionic (non-silicate) clay to personal wash compositions unexpectedly lowers the viscosity of the composition, thus acting as a hydrotrope (e.g., viscosity
30 thinner rather than viscosity thickener) . While not wishing

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to be bound by theory, the anionic clay is believed to help break down the mesostructure of surfactants used in the subject invention, thereby leading to easy dispersibility and ready incorporation of air (hence better foam) .
U.S. Patent No. 5,145,599 to Endres et al. does disclose the type of non-silicate layer compounds (having positive charge on basal layer) used in the subject invention. However, in the patent, the compounds are used in enzyme-containing,
10 fabric-cleansing detergent compositions. Such detergent compositions are not concerned with lather, mildness or
other

attributes which the personal cleansing compositions

of the subject invention relate to.
15 U.S. Patent No. 5,661,189 to Grieveson et al. discloses that hydrotalcites can be used as a thickening agent (column 2, line 67) . They are one of many potential "thickening agents", and there is clearly no teaching or suggestion that, if used at all, they serve to reduce viscosity. The
20 present invention is a selection patent in which hydrotalcite must be used.
Unexpectedly, the applicants have found that when non-silicate clays having a basal layer with cationic charge are
25 used in personal wash compositions (i.e., substantially
enzyme-free personal wash compositions) , the clays interact with surfactants in the personal wash compositions to breakdown the surfactant mesostructure. This in turn resultis in easy dispersibility (i.e., lower viscosity),
30 better; foam (easier incorporation of air) and reduced irritation. It also can improve delivery of actives.

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More particularly, in one embodiment, the present invention provides compositions comprising:
(1) about 5 % to 35 %, preferably 5 % to 30 % by wt. of
a surfactant selected from the group consisting of
5 anionic, nonionic, zwitterionic/amphoteric and
cationic surfactants and mixtures thereof;
(2) about 0.1 % to 15 %, preferably 0.5 % to 10 %, more
preferably 0.2 % to 5 % by wt of a non-silicate
layer compound, wherein a net cationic charge is
10 found in the basal layer;
(3) about 3 % to 40 %, preferably 5 % to 30 % by wt. of an aqueous solvent; and
(4) about 5 % to 40 % by wt. non-aqueous solvent; wherein said composition is substantially enzyme
15 free.
In a second embodiment, the invention provides a process to decrease viscosity and/or enhance foam in substantially . enzyme-free personal wash composition which process
20 comprises formulating non-silicate layer compounds as noted above into the personal wash compositions.
These and other aspects, features and advantages will become apparent to those of ordinary skill in the art from a reading
25 of the following detailed description and the appended claims. For the avoidance of doubt, any feature of one aspect of the present invention may be utilized in any other aspect of the invention. It is noted that the examples given in the description below are intended to clarify the

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invention and are not intended to limit the invention to those examples per se.
Other than in the experimental examples, or where otherwise
5 indicated, all numbers expressing quantities of ingredients or reaction conditions used herein are to be understood as modified in all instances by the term "about" . Similarly, all percentages are weight/weight percentages of the total composition unless otherwise indicated. Numerical ranges
10 expressed in the format "from x to y" are understood to include x and y. When for a specific feature multiple preferred ranges are described in the format "from x to y", it is understood that all ranges combining the different end points are also contemplated. Where the term "comprising" is
15 used in the specification or claims, it is not intended to exclude any terms, steps or features not specifically recited.
All temperatures are in degrees Celsius (°C) unless specified
20 otherwise. All measurements are in SI units unless specified otherwise. All documents cited are - in the relevant part -incorporated herein by reference.
The invention will be described by way of example only with 25 reference to the accompanying drawings, in which:
- Figure 1 is a schematic drawing of a typical silicate layered compound ("cationic" clay) having net anionic charge on basal layer;

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- Figure 2 is schematic of a typical non-silicate layered compound of the invention ("anionic" clay) having net cationic charge on basal layer; and
5 - Figure 3 shows how addition of non-silicate clays of the
invention actually has hydrotroping (thinning effect) rather than a thickening effect normally expected from use of clays.
In one embodiment, the present invention relates to personal
10 wash compositions (substantially enzyme-free) comprising
non-silicate layer compounds having a net cationic charge on the basal layer. Unexpectedly, the applicants have found that surfactants present in such compositions interact with and are broken down by the non-silicate compound (e.g.,
15 mesostructure broken down), resulting in multiple sensory and/or other benefits to the consumer (e.g. more foam, less irritation, etc.).
Specifically, in one embodiment the invention comprises:
20
(1) about 5 % to 35 %, preferably 5 % to 30 % by wt. of
a surfactant selected from the group consisting of
anionic, nonionic, zwitterionic/amphoteric and
cationic surfactants and mixtures thereof;
25
(2) about 0.1 % to 15 %, preferably 0.5 to 10 %, more
preferably 0.2 % to 5 % by wt of a non-silicate
layer compound wherein a net cationic charge is
found on the basal layer;

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(3) about 3 % to 40 %, preferably 5 % to 30 % by wt. of an aqueous solvent; and
(4) 5 % to 40 % by wt. non-aqueous solvent
5
wherein the composition is substantially enzyme free.
In preferred embodiments, at least 50 % of surfactant system should be anionic surfactant. Preferably, the combination
10 comprises 5 % to 25 % by wt. of an anionic or mixture of anionic surfactant and 1 % to 10 % by wt. zwitterionic and/or amphoteric surfactant.
The invention is described with more particularity below.
15
As noted, the surfactant of the invention maybe an anionic, nonionic, zwitterionic/amphoteric or cationic surfactant or mixtures thereof. Typically, the cleanser will be an aqueous cleanser comprising 5 % to 25 % of an anionic
20 surfactant and 1 % to 10 %, preferably 3 % to 10 % of a second anionic and/or amphoteric surfactant. The anionic surfactant may be a synthetic surfactant or fatty acid soap.
The term "soap" is used here in its popular sense, i.e., the
25 alkali metal or alkanol ammonium salts of aliphatic alkane-or alkene monocarboxylic acids. Sodium, potassium, mono-, di and tri-ethanol ammonium cations, or combinations thereof, are suitable for purposes of this invention. In general, sodium soaps- are used in the compositions of this
30 invention, but from about 1 % to about 25 % of the soap may be potassium soaps. The soaps useful herein are the well

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known alkali metal salts of natural or synthetic aliphatic (alkanoic or alkanoic) acids having about 12 to 22 carbon atoms, preferably about 12 to about 18 carbon atoms. They may be described as alkali metal carboxylates of acrylic
5 hydrocarbons having about 12 to about 22 carbon atoms.
Soaps having the fatty acid distribution of coconut oil may provide the lower end of the broad molecular weight range. Those soaps having the fatty acid distribution of peanut or
10 rapeseed oil, or their hydrogenated derivatives may provide the upper end of the broad molecular weight range.
It is preferred to use soaps having the fatty acid distribution of coconut oil or tallow, or mixtures thereof,
15 since these are among the more readily available fats. The proportion of fatty acids having at least 12 carbon atoms in . coconut oil soap is about 85 %. The proportion will be greater when mixtures of coconut oil and fats such as tallow, palm oil or non-tropical nut oils or fats are used,
20 wherein the principle chain lengths are Cis and higher.
Preferred soap for use in the compositions of this invention has at least about 85 % fatty acids having about 12-18 carbon atoms.
25 Coconut oil employed for the soap may be substituted in
whole or in part by other "high-1auric" oils, that is, oils or fats wherein at least 50 % of the total fatty acids are composed of lauric or myristic acids and mixtures thereof. These oils are general exemplified by the tropical nut oils
30 of the coconut oil class. For instance, they include: palm kernel oil, babassu oil, ouricuri oil, tucum oil, cohune nut

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oil, rrruru-muru oil, jaboty kernel oil, khakan kernel oil, dika nut oil, and ucuhuba butter.
A preferred soap is a mixture of about 15 % to about 20 %
5 coconut oil and about 80 % to about 85 % tallow. These mixtures contain about 95 % fatty acids having about 12 to about 18 carbon atoms. The soap may be prepared from coconut oil in which case the fatty acid content is about 85
% of C12-C18 chain length.
10
The soaps may contain unsaturation in accordance with commercially acceptable standards. Excessive unsaturation is normally avoided.
15 The anionic may also be an alkyl sulfate (e.g., C12-C18
alkylsulfate) or alkyl ether sulfate (including alkyl glycerol ether sulfates). Among the alkyl ether sulfates are those having the formula:

herein R is an alkyl or alkenyl having 8 to 18 carbons, preferably 12 to 18 carbons; n has an average value of greater than 1.0, preferably greater than 3; and M is a
25 solubilizing cation such as sodium, potassium ammonium or substituted ammonium. Ammonium and sodium lauryl ether sulfates are preferred.
The anionic may also be alkyl sulfosuccinates (including
30 mono- and dialkyl, e.g., C6-C22 sulfosuccinates); alkyl and

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acyl taurates, alkyl and acyl sarcosinates, sulfoacetates, C8-C22 alkyl phosphates and phosphates, alkyl phosphate esters and alkoxyl alkyl phosphate esters, acyl lactates, C8-C22 tnonoalkyl succinates and maleates, sulphoacetates,
5 alkyl glycosides and acyl isethionates.
Sulfosuccinates may be monoalkyl sulfosuccinates having the formula:



and amide-MEA sulfosuccinates of the formula:

15
4 wherein R ranges from C8-C22 alkyl and M is a solubilizing
cation.
Sarcosinates are generally indicated by the formula: 20

wherein R ranges from C8-C20 alkyl and M is a solubilizing
cation. 25
Taurates are generally identified by formula:


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2 3
wherein R ranges from C8-C20 alkyl, R ranges from C1-C4 alkyl and M is a solubilizing cation.
5 Other anionic groups which may be used include glutamates (e.g., acyl glutamates such as sodium acyl glutamate); lysinates; alaninates; and glycinates.
Particularly preferred are the CB-C1B acyl isethionates.
10 These esters are prepared by reaction between alkali metal isethionate with mixed aliphatic fatty acids having from 6 to 18 carbon atoms and an iodine value of less than 20. At least 75 % of the mixed fatty acids have from 12 to 18 carbon atoms and up to 25 % have from 6 to 10 carbon atoms.
15
Acyl isethionates, when present, will generally range from
about 5 % to about 20 % by weight of the total composition. Preferably, this component is present from about 5 % to
about 10 %. 20
In general the anionic component will comprise from about 1 % to 40 % of the composition, preferably 3 % to 25 % by wt. of the composition.
25 Amphoteric detergents which may be used in this invention include at least one acid group. This may be a carboxylic or a sulphonic acid group. They include quaternary nitrogen and therefore are quaternary amido acids. They should generally include an alkyl or alkenyl group of 7 to 18

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carbon atoms. They will usually comply with an overall structural formula:



1 2
10 wherein R is alkyl or alkenyl of 7 to 18 carbon atoms; R
and R are each independently alkyl, hydroxy alkyl or
carboxyalkyl of 1 to 3 carbon atoms; m is 2 to 4; n is 0 to 1, X is alkylene of to 3 carbon atoms optionally substituted
with hydroxyl; and Y is -C02- or -SO3-15
Suitable amphoteric detergents within the above general formula include simple betaines of formula:

25 and amido betaines of formula:


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where m is 2 or 3; in both formulae R1 , R2 and R3 are as defined previously. R1 may in particular be a mixture of C12; and C14 alkyl groups derived from coconut so that at least
5 half, preferably at least three quarters of the groups R

have 10 to 14 carbon atoms. R2 and R3 are preferably methyl.
A further possibility is that the amphoteric detergent is a
10 sulphobetaine of formula:

where m is 2 or 3 ,,or variants of these in which -(012)3803-20 is replaced by:

In these formula R1 , R2 and R3 are as discussed previously.

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The nonionic which may be used includes in particular the reaction products of compounds having a hydrophobic group and a reactive hydrogen atom, for example aliphatic alcohols, acids, amides or alkyl phenols with alkylene
5 oxides, especially ethylene oxide either alone or with propylene oxide.
Specific nonionic detergent compounds are alkyl (C6-C22) phenols-ethylene oxide condensates, the condensation
10 products of aliphatic (Cs-Cis) primary or secondary linear or branched alcohols with ethylene oxide, and products made by condensation of ethylene oxide with the reaction products of propylene oxide and ethylenediamine. Other so-called nonionic detergent compounds include long chain tertiary
15 amine oxides, long chain tertiary phosphine oxides and dialkyl sulphoxides.
The nonionic may also be a sugar amide, such as a polysaccharide amide. Specifically, the surfactant may be
20 one of the lactobionamides described in U.S. Serial No. 816,419 to Au et al. which is hereby incorporated by reference, or it may be one of the sugar amides described in U.S. Patent No. 5,009,814 to Kelkenberg, hereby incorporated into the subject application by reference.
25
Other surfactants which may be used are described in U.S. Patent No. 3,723,325 to Parran Jr., which is also incorporated into the subject application by reference.

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The present invention relates to the use of non-silicate layer compounds corresponding to general formula (I)
MgxAl(OH)yAznH20
5
in which A represents an equivalent of a non-silicate anionic and the conditions 1 10 hydrotalcite with a lattice distance for the most intensive line in the X-ray diffractogram of from 7.4 to 8 A (angstroms) for the product dried at 110°C.
The basal layer of these compounds carries a net cationic
15 charge.
In the context of the invention, these layer compounds are understood to be solids of which the structure is derived from the layer-form magnesium hydroxide, brucite, by the
20 partial replacement of the divalent metal ions by trivalent metal ions. The resulting positive excess charge of the metal hydroxide layers is compensated by exchangeable anions between the layers. Hydrotalcite may be used as a model substance for this class of solids. A schematic of such
25 compound is shown in Figure 2.
Hydrotalcite is a substance occurring in nature as a mineral having the approximate composition:
30 Mg6Al2(0H)16CO3-4H2O

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the ratio of Mg to Al and, hence, the carbonate content being variable within relatively wide limits. The carbonate may be replaced by other anions. By contrast, the substance is
5 characterized by its layer structure with the layer sequence ABAB, where A is a positively charged triple layer of hydroxyl ions, metal cations and more hydroxyl ions. B is an intermediate layer of anions and water of crystallization.
10 This layer structure is shown up in an X-ray powder diagram which may be used for characterization. Thus, ASTM Card No. 14-191 gives the lines for the lattice plane spacings d = 7.69, 3.88, 2.58, 2.30, 1.96, 1.53 and 1.50 A as the most intensive X-ray interferences. The spacing 7.69 A is the
15 basic repetition period of the layers (= layer spacing) of the substance which normally contains water of crystallization. More rigorous drying at elevated temperature (120°C to 200°C a normal pressure) leads to reduced layer spacings through release of the water of
20 crystallization.
The crystal structure of natural hydrotalcite was determined radiographically by Allmann and Jepsen (N. Jahrb. Mineral. Monatsch. 1969, pages 544-551). The range of variation of
25 the Mg to Al ratio and its influence on the repetition period of the layers was investigated, for example, by Gastuche, Brown and Mortland (Clay Miner. & (1967), pages 177-192). Possible processes for the commercial production of synthetic hydrotalcite and its use as an agent for
30 binding stomach acid were described in 1967 by Kyowa Chemical Indlustryu Co., Tokyo (DE-OS 15 92 126).

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Apart from neutralizing stomach acid, hydrotalcite may generally be used for binding acidic components, for example impurities from catalytic processes (DE-OS 27 19 024) or unwanted dyes (DE-OS 29 29 991). Further potential
5 applications are in the field of corrosion prevention (DE-OS 31 28 716), the stabilization of plastics, particularly PVC (DE-PS 30 19 632), in waste water treatment (JP-PS 79 24 993, JP-PS 58 214 388) and in the production of colored pigments (JP-PS 81 98 265) .
10
The incorporation of carbonate ions as intermediate layer anions is particularly preferred. Hydrotalcite-like solids containing other anions may be obtained by using a soluble salt of another acid instead of sodium carbonate in the
15 production process, or by removing the carbonate from the carbonate-containing product in the form of C02 by reaction with weak acids. The exchange of the anions is shown up in the X-ray diffractogram by a change in the layer spacings (T. Reichle, Chemtech. Jan 1986, pages 58-63).
20
Another embodiment of the present invention is characterized by the use of non-silicate layer compounds in which A in general formula (I) represents an equivalent of a carbonate ion.
25
Another preferred embodiment of the present invention is characterized by the use of cationic non-silicate layer compounds corresponding.to general formula (I) in a quantity
of from 0.1 % to 15 % by weight, based on the detergent 30 composition. The use of 0.5 % to 10 % by weight of the

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cationic non-silicate layer compounds, based by the composition, is particularly preferred.
The compositions of the invention are generally aqueous
5 solvent compositions wherein the aqueous solvent (e.g., water) comprises 3 % to 40 % by wt. of composition.
The non-aqueous solvent comprises about 5 % to 40 % by wt. of composition. This solvent may be oils (e.g., sunflower
10 oil), low MW fatty acids, glycols, polyols, etc. In fact, for purposes of the invention, the non-aqueous solvent may be defined as non-water solvent since it can be any solvent other than water itself.
15 The ratio of non-aqueous to aqueous may range from 0.7:1 to 2:1.
In terms of optional aspects, the liquids of this invention may be isotropic single phase liquids, or they may be
20 structured as defined and using structurants as defined in U.S. Patent No. 5,952,2 86 to Puvvada et al. hereby incorporated by reference into the subject invention.
The compositions may contain oils or emollients as noted 25 below.
Vegetable oils: Arachis oil, castor oil, cocoa butter, coconut oil, corn oil, cotton seed oil, olive oil, palm
kernel oil, rapeseed oil, safflower seed oil, sesame seed 30 oil and soybean oil.

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Esters: Butyl myristate, cetyl palmitate, decyloleate, glyceryl laurate, glyceryl ricinoleate, glyceryl stearate, glyceryl isostearate, hexyl laurate, isobutyl palmitate, isocetyl stearate, isopropyl isostearate, isopropyl laurate,
5 isopropyl linoleate, isopropyl myristate, isopropyl
palmitate, isopropyl stearate, propylene glycol monolaurate, propylene glycol ricinoleate, propylene glycol stearate, and propylene glycol isostearate.
10 Animal Fats: Acytylatelte lanolin alcohols, lanolin, lard, mink oil and tallow.
Fatty acids and alcohols: Behenic acid, palmitic acid, stearic acid, behenyl alcohol, cetyl alcohol, eicosanyl
15 alcohol and isocetyl alcohol.
Other examples of oil/emollients include mineral oil, petrolatum, silicone oil such as dimethyl polysiloxane, lauryl and myristyl lactate.
20
It should be understood that where the emollient may also function as a structurant, it should not be doubly included such that, for example, if the structurant is 15 % oleyl alcohol, no more than 5 % oleyl alcohol as "emollient" would
25 be added since the emollient (whether functioning as
emollient or structurant) never comprises more than 20 %, preferably no more than 15 % of the composition.
The emollient/oil is generally used in an amount from about
30 1 % to 20 I, preferably 1 % to 15 % by wt. of the

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composition. Generally, it should comprise no more than 20 % of the composition.
In addition, the compositions of the invention may include 5 optional ingredients as follows:
Organic solvents, such as ethanol; auxiliary thickeners, such as carboxymethylcellulose, magnesium aluminum silicate, hydroxyethylcellulose, methylcellulose, carbopols,
10 glucamides,or Antil (R) from Rhone Poulenc,- perfumes;
sequestering agents, such as tetrasodium
ethylenediaminetetraacetate (EDTA) , EHDP or mixtures in an amount of 0.01 % to 1 %, preferably 0.01 % to 0.05 %; and coloring agents, opacifiers and pearlizers such as zinc
15 stearate, magnesium stearate, TiCO2, EGMS (ethylene glycol monostearate) or Lytron 621 (Styrene/Acrylate copolymer); all of which.are useful in enhancing the appearance or cosmetic properties of the product.
20 The compositions may further comprise antimicrobials such as 2-hydroxy-4,2'4 ' trichlorodiphenylether (DP300);
preservatives such as dimethyloldimethylhydantoin (Glydant XL1000), parabens, sorbic acid etc.
25 The compositions may also comprise coconut acyl mono- or diethanol amides as suds boosters, and strongly ionizing salts such as sodium chloride and sodium sulfate may also be used to advantage.

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Antioxidants such as, for example, butylated hydroxytoluene (BHT) may be used advantageously in amounts of about 0.01 % or higher if appropriate.
5 Cationic conditioners which may be used include Quatrisoft LM-200 Polyquaternium-24, Merguat Plus 3330 - Polyquaternium
39;and Jaguar (R) type conditioners.
Polyethylene glycols which may be used include: PEG-200 to 10 PEG-8000

Polyox WSR-205 PEG 14M,
Polyox WSR-N-60K PEG 45M, or
Polyox WSR-N-750 PEG 7M.
15
Thickeners which may be used include Amerchol Polymer HM 1500
(Nonoxynyl Hydroethyl Cellulose) ; Glucam DOE 120 (PEG 120
(R) Methyl Glucose Dioleate); Rewoderm (PEG modified glyceryl
(R) cocoate, palmate or tallowate) from Rewo Chemicals; Antil
20 141 (from Goldschmidt).
Another optional ingredient which may be added are the deflocculating polymers such as are taught in U.S. Patent No. 5,147,576 to Montague, hereby incorporated by reference.
25
Another ingredient which may be included are exfoliants such as polyoxyethylene beads, walnut sheets and apricot seeds.
EXAMPLES 30

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Protocols
Viscosity measurements for examples which follow were conducted using two different methods:
5
(1) For model surfactant/particles system (as shown in
Table 1) ; the viscosity of the above model
surfactant/particles samples were measured using Haake RV20 Rotovisco Rheometer in a SV1 cup and bob
10 @ 25°c.
(2) For the facial cleanser formulations (shown in Table
2); viscosity of the above model Prototype samples
as shown in table # 3, were measured using ARES
Rheometer @ 25°C using cone and plate geometry.
15
Foam Volume measurements were conducted as follows:
0.5 g of sample was diluted with 5 g. of DI water. Foam was generated by rubbing both the hands 10 times in a circular
20 motion. All the foam was collected and the weight of the
foam was obtained. Also the specific gravity of the foam is obtained by measuring the weight of the foam in small petri dish of known volume. Total foam volume is calculated by dividing total foam weight by foam specific gravity.
25
Definitions
SLES = Sodium lauryl ether sulfate CAPB = Cocoamidopropyl betaine
30

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EXAMPLE 1 and Comparatives A and B
The following example shows the hydrotroping (thinning) effect of hydrotalcite compared to conventional clay on surfactant
5 mixtures (e.g., SLES-Betaine mixtures). The formulations were made by adding SLES, betaine and water, and mixing the components using an overhead stirrer. The clays were then added and dispersed using a ultrasonic probe (model Sonic Vibracell VC 130 PB using W probe). Viscosity measurements
10 (Graphed in Figure 3) were performed immediately as set forth in the Protocol Section.
Table # 1

Formulation SLES/Betaine (60:40 ratio) Clay (level wt.%) Water
Comparative A (no clays) 20 0 80
Comparative B (basal 20 Bentonite (5 %) 75
layer anionic)
Example 1 (Basal layer 20 Hydrotalcite (5 %) 75
cationic)
15 As seen in Figure 3, relative to use of no clay, the traditional "clay" (bentonite) has a thickening effect, while unexpectedly clays of the invention have thinning effect.
20 Specifically, the above example clearly shows that the addition of hydrotalcite reduces the viscosity of SLES-Betaine solutions by a factor of-3, whereas bentonite at the

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same level increases viscosity by a factor of -2 at shear rates EXAMPLE 2 and Comparative C-H
The following examples show the effect of hydrotalcite and bentonite on the viscosity and lather for two facial cleanser compositions. The samples were prepared as follows:
10
1. Water + glycerine + PEG were added in the jacketed flask and mixed using overhead stirrer while heating;
2. Particles (e.g., clays, if any) were added while
15 mixing until they dispersed uniformly. (Sonicating the mixture if needed);
3. Na-Glycinate was added when the temperature reached
-40°C and was mixed until dissolved;
4. Taurate and CAPB were added while mixing until the
20 sample was uniform;
5. Citric acid was dissolved in water and added slowly and the sample was mixed well until it looked uniform;
6. The pH was checked while mixing and adjusted to 7. 0
25 ± 0..5;
7. Preservative was added when temperature was -40°C.

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Table 3 below sets forth the specific clay used in the formulations as well as measured results for foam and viscosity (measured as described in Protocol of the invention). Viscosity results were tested specifically for
5 one clay wherein basal layers has net anionic charge
(bentonite), for one clay where basal layer has net cationic charge (hydrotalcite); and for formulation with no clay (Comparative G). Foam results were taken for all.

10

Table 3


Formulation Particle-Name Foam Volume (ml) Viscosity @ 0.1 (s-1)
Comparative C Bentonite 20.17 437
Comparative D Kaoline 14.63
Example 2 (Invention) Hydrotilcite-C300 45.0 95
Comparative E Titanium Dioxide 16.0
Comparative F Talc 19.20
Comparative G (control with no particles) No-Particles20 % glycerin is replaced by PEG (FCAT) 13.60 299
Comparative H (Control with no particles) No particles 15.52
As clearly shown from Table 3, the addition of hydrotalcite reduces the viscosity of the formulation by a factor of about 3 whereas bentonite, at the same level, increases
15 viscosity by a factor of about 1.5, when measuring at shear
-l rates of 0.1 S as defined in the Protocol. Also, talc and
bentonite increase foam volume slightly, while hydrotalcite increases the foam volume by a factor of about 3. This is
WO 2006/010469 PCT/EP2005/007539
- 27 -
believed to be related to the reduced viscosity and easy dispersibility of the product.

J6904(C)CT

CLAIMS

Wherein at least 50% of the surfubont system is anionic suefarbant;>

1. Personal waph composition comprising:
5 (1) about 5 % to 35 % by wt, of a surfactant/selected
from anionic, nonionic, zwitterionic/amphoteric and
cat ionic surfactants and mixtures thereof;
(2) about 0.1 % to 15 % by wt Df a non-silicate layer
compound wherein a net cationic charge is found on
10 the basal layer or layers;
'(3) about- 3 % to 40 % by wt, of an-agueous solvent; and (4) 5 % to 40 % by wt. non-aqueous solvent, wherein the composition is substantially enzyme free.
15 2. A composition according to claim l, comprising 5 % to 30 % by wt. surfactant.
3. A composition according to claim l or claim 2,
comprising 5 % to 25 % by wt. anionic or mixture of
20 anionic surfactant and 1 % to 10 % by wt. of surfactant
selected from zwitterionic/anpnoterlc and mixtures thereof.
4. A composition according to any one of. the preceding
25 . claims, comprising 0,5 % to 10 % cationic, non-silicate
compound.
5. A composition according to any one of the preceding
claims, comprising E % to 3 0 % aqueous solvent.

Documents:

104-mumnp-2007-abstract(11-08-2008).doc

104-MUMNP-2007-ABSTRACT(11-8-2008).pdf

104-mumnp-2007-abstract-(11-8-2008).pdf

104-MUMNP-2007-ASSIGNMENT(11-8-2008).pdf

104-MUMNP-2007-CANCELLED PAGES(11-8-2008).pdf

104-MUMNP-2007-CLAIMS(11-8-2008).pdf

104-mumnp-2007-claims(granted)-(11-08-2008).doc

104-mumnp-2007-claims(granted)-(11-8-2008).pdf

104-mumnp-2007-claims.doc

104-mumnp-2007-claims.pdf

104-mumnp-2007-correspondance-others.pdf

104-mumnp-2007-correspondance-received.pdf

104-MUMNP-2007-CORRESPONDENCE(11-8-2008).pdf

104-mumnp-2007-correspondence(ipo)-(24-9-2008).pdf

104-mumnp-2007-correspondence1(23-1-2007).pdf

104-mumnp-2007-correspondence2(11-8-2008).pdf

104-mumnp-2007-description (complete).pdf

104-MUMNP-2007-DESCRIPTION(C0MPLETE)-(11-8-2008).pdf

104-MUMNP-2007-DRAWING(11-8-2008).pdf

104-MUMNP-2007-DRAWING(23-1-2007).pdf

104-mumnp-2007-drawing-(11-8-2008).pdf

104-mumnp-2007-drawings.pdf

104-MUMNP-2007-FORM 1(11-8-2008).pdf

104-mumnp-2007-form 1(23-1-2007).pdf

104-mumnp-2007-form 13(3-10-2007).pdf

104-mumnp-2007-form 18(24-5-2007).pdf

104-mumnp-2007-form 2(11-8-2008).pdf

104-mumnp-2007-form 2(granted)-(11-08-2008).doc

104-mumnp-2007-form 2(granted)-(11-8-2008).pdf

104-MUMNP-2007-FORM 2(TITLE PAGE)-(11-8-2008).pdf

104-MUMNP-2007-FORM 3(11-8-2008).pdf

104-mumnp-2007-form 3(23-1-2007).pdf

104-MUMNP-2007-FORM 5(11-8-2008).pdf

104-mumnp-2007-form-1.pdf

104-mumnp-2007-form-2.pdf

104-mumnp-2007-form-3.pdf

104-mumnp-2007-form-5.pdf

104-mumnp-2007-form-pct-ib-306.pdf

104-mumnp-2007-form-pct-ib-311.pdf

104-mumnp-2007-form-pct-ipea-409.pdf

104-mumnp-2007-form-pct-isa-210(11-8-2008).pdf

104-mumnp-2007-form-pct-separate sheet-409.pdf

104-mumnp-2007-pct-search report.pdf

104-MUMNP-2007-POWER OF ATTONEY(11-8-2008).pdf

104-mumnp-2007-power of attorney(11-8-2008).pdf

abstract1.jpg


Patent Number 225375
Indian Patent Application Number 104/MUMNP/2007
PG Journal Number 07/2009
Publication Date 13-Feb-2009
Grant Date 11-Nov-2008
Date of Filing 23-Jan-2007
Name of Patentee HINDUSTAN UNILEVER LIMITED
Applicant Address HINDUSTAN LEVER HOUSE, 165/166,BACKBAY RECLAMATION, MUMBAI-400 020, MAHARASHTRA,INDIA.
Inventors:
# Inventor's Name Inventor's Address
1 SUBRAMANIAN VIVEK UNILEVER HOME & PERSONAL CARE USA, 40 MERRITT BOULEVARD, TRUMBULL, CONNECTICUT 06611 USA
2 SHAH PRAVIN UNILEVER HOME & PERSONAL CARE USA, 40 MERRITT BOULEVARD, TRUMBULL, CONNECTICUT 06611 USA
3 ANANTHAPADMANABHAN KAVSSERY PARAMESWARAN UNILEVER HOME & PERSONAL CARE USA, 40 MERRITT BOULEVARD, TRUMBULL, CONNECTICUT 06611 USA
PCT International Classification Number A61K8/26
PCT International Application Number PCT/EP2005/007539
PCT International Filing date 2005-07-08
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 10/902202 2004-07-29 U.S.A.