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Neutral Ph Floating Bathing Bar

Abstract: In the present invention there is provided a neutral pH floating bathing bar with very high amount of free fatty acids (FFA) (i.e. greater than 25% w/w) and protic acid greater than 0.5 % wt. the soap bar of the present invention maintains a neutral pH ranging from 6.8 to 8.3.

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Patent Information

Application #
Filing Date
10 February 2014
Publication Number
35/2016
Publication Type
INA
Invention Field
PHARMACEUTICALS
Status
Email
cal@patentindia.com
Parent Application
Patent Number
Legal Status
Grant Date
2019-10-22
Renewal Date

Applicants

ITC LIMITED
37, J.L. Nehru Road, Kolkata-700071,State of West Bengal, India.

Inventors

1. DAS, Subir, Kumar
ITC Limited, ITC R&D Centre, # 3, 1st Main, Peenya Industrial Area, Phase 1, Bengaluru – 560 058, India
2. SACHAN, Payal
ITC Limited, ITC R&D Centre, # 3, 1st Main, Peenya Industrial Area, Phase 1, Bengaluru – 560 058, India
3. SODANKURU, Satyanarayana, Sharma
ITC Limited, ITC R&D Centre, # 3, 1st Main, Peenya Industrial Area, Phase 1, Bengaluru – 560 058, India
4. RAMAMURTHI, Suresh
ITC Limited, ITC R&D Centre, # 3, 1st Main, Peenya Industrial Area, Phase 1, Bengaluru – 560 058, India

Specification

CLIAMS:1. A neutral pH bathing bar comprising:
(i) a first portion which is floating soap;
(ii) a second portion which is syndet bathing bar;
wherein the ratio of combination of floating soap and syndet bathing bar ranges from 10:90 to 30:70; and

wherein said syndet bathing bar has free fatty acid greater than 25% w/w and protic acid greater than 0.5 % w/w.

2. The neutral pH bathing bar as claimed in claim 1, wherein said first portion comprises In-situ soap, Surfactants, polymer, salt, Aqua, Solvents, Preservative, Color / Fragrance / Emotive.
3. The neutral pH bathing bar as claimed in claim 1, wherein said second portion comprises Surfactant, Free fatty acid, Emulsifier, polymer, soap, binders, oil, emollient, preservatives, color / fragrance / emotive, protic acid and aqua.
4. The neutral pH bathing bar as claimed in claim 1, wherein the best working ratio of floating soap and syndet bathing bar is 20:80.
5. The neutral pH bathing bar as claimed in claim 1, wherein the pH of the neutral pH bathing bar ranges from 6.8 to 8.3.
6. The neutral pH bathing bar as claimed in claim 3, wherein said free fatty acids are chosen from a group comprising fatty acids with alkyl chain lengths of from C8 – C18 like linear chained fatty acids, branched chain fatty acids, saturated and unsaturated fatty acids such as Caprylic, Capric, Lauric, Myristic, Palmitic, Stearic, Oleic, and mixtures thereof.

7. The neutral pH bathing bar as claimed in claim 3, wherein amount of said free fatty acid ranges from 25 to 40% wt., preferably from 26 to 37% wt.

8. The neutral pH bathing bar as claimed in claim 3, wherein said Protic acid is selected from but is not limited to, citric acid, lactic acid, oxalic acid.

9. The neutral pH bathing bar as claimed in claim 3, wherein amount of said protic acids ranges from 0.5 to 2% wt., preferably from 0.5 to 1.5% wt. ,TagSPECI:Field of the invention
The present invention relates to soap bar, more particularly the present invention relates to neutral pH floating bathing bar with very high amount of free fatty acids (FFA) (i.e. greater than 25% w/w) and protic acid.
Background and prior art of the invention
Floating soap with is widely accepted among the customers, preparation of opaque floating soap is well known state of the art. However it is difficult to formulate a neutral pH floating bathing bar. Soap formulations which are close to neutral pH are highly desirous among the consumers. It becomes a challenge to develop a neutral pH floating bathing bar. The mild syndet bar with neutral pH available have density equivalent to other toilet bars (i.e. =1 g/ml).

US 4504433 disclose dried shapes of soap embedded within transparent soap. The dried soap which are embedded inside the transparent soap are coloured for improved aesthetic. US ‘433 also provide a process for the preparation of the transparent soap which contains dried shapes of coloured soap. The dried shape according to US’433 can be a bird or flower which floats within the transparent soap.

Further US ‘433 also discloses that a soap base is prepared, comprising 5 to 15% by weight of sugar, 25 to 35% by weight of alcoholic compounds, 12 to 25% by weight of an aqueous matter and 58 to 25% by weight of a soap component obtained by saponification of oils and fats or higher fatty acids, etc. The alcoholic compounds may comprise 10% by weight or higher of glycerine, 60% by weight or higher of ethanol and 30% by weight or lower of one or more selected from the group consisting of ethylene glycol, polyethylene glycol, propylene glycol, polypropylene glycol, maltitol, sorbitol and a higher aliphatic alcohol. Suitable amounts of perfumes and coloring agents and, optionally, pearl pigment, are added to, and dispersed in, the soap base heated to 60 degree to 75.degree C and fused, thereby to obtain a colored soap base to be formed into various shapes.

Inserting an embedded material into the soap mass is a cumbersome process from formulation point of view. It is always advantageous to have a full soap formulation as it provide uniform in-use profile till the end.

US 20090253601 relates to a mixture for producing a combi-bar floating in water at 20.degree. C. (and other temperatures), i.e. having a density below 0.99821 g/mL at 20.degree. C. Such combi-bar herein after are also designated as "floating combi-bar". The present invention also relates to a method for producing a floating combi-bar and a combi-bar itself. The composition further comprises of 20-50 wt. %, preferably 25-40 wt. %, of one or more non-soap surfactants, preferably solid non-soap surfactants, vi) 25-60 wt. %, preferably 35-55 wt. %, of one or more free C.sub.14-C.sub.18 fatty acids, vii) 2-40 wt. %, preferably 5-25 wt. %, of one or more metal C.sub.8-C.sub.24 fatty acid soaps, and viii) 0-20 wt. %, preferably 2-20 wt. %, of further ingredients, said mixture containing less than 10 wt. % of water as a further ingredient.

EP1377658 teaches aerated, ultra low-density cast-dehydrated syndet detergent bars for use in personal wash, fabric wash and hard surface cleaning. A process for preparing aerated, ultra low-density cast-dehydrated detergent bars wherein the air is entrained in the bars after rigidification and shaping the product is also provided. The low density soap bar of EP ‘658 is a syndet bar which floats. EP ‘658 teaches entrainment of air in the range 1-90% by volume in order to enable the soap composition to float.

It is desired to have a mild floating soap mass in which the entire soap is floating and not the inside soap that is floating. It is always advantageous to have a full floating formulation as it provide uniform in-use profile till the end.
Hence there is a need to formulate a neutral pH floating bathing bar having similar or milder benefit on skin with low density. It is further also very challenging to introduce very high amount of free fatty acids (i.e. greater than 25% w/w) together with protic acid to maintain the neutral pH in floating bathing bar. The introduction of high amount of FFA will not maintain the viscosity profile which is very much desired to entrap the air in the floating mass. Processing of floating soap mass with high amount of FFA is difficult as the air retention ability is less and it makes it difficult to formulate low density soap.
Objective of the invention
An object of the present invention is to overcome the drawbacks of the prior art.
Another object of the present invention is to provide a floating bathing bar with neutral pH.
Another object of the present invention is to provide a floating bathing bar with high amount of FFA (i.e. greater than 25% w/w) and protic acid.
Yet another object of the present invention is to provide a floating bathing bar with high amount of FFA (i.e. greater than 25% w/w) and protic acid which has neutral pH.
Summary of the present invention
An aspect of the present invention is to provide a neutral pH bathing bar comprising:
(i) a first portion which is floating soap;
(ii) a second portion which is syndet bathing bar;
wherein the ratio of combination of floating soap and syndet bathing bar ranges from 10:90 to 30:70;

wherein said syndet bathing bar has free fatty acid greater than 25% w/w and protic acid greater than 0.5 % w/w.
Brief description of the accompanying drawings
Figure 1 illustrates the surface finish for Neutral pH bathing bar comparing the neutral pH floating bathing bar of the present invention and Floating soap bar of the prior art.
Detailed description of the invention
The present invention aims at providing a neutral pH floating bathing bar with high amount of free fatty acid and protic acid. Incorporation of free fatty acids in low density soap is a challenge as its air retention ability is very less. The present invention describes a formulation approach to develop a neutral pH floating bathing bar with high amount of free fatty acids and protic acid.
The unique formulation approach helps in maintaining the high amount of FFA (i.e. greater than 25% w/w) and protic acid in order to achieve a neutral pH floating bathing bar. The unique formulation of two phases also has excellent compatibility amongst each other so that the final soap mass appears as single phase and deliver the benefit of formulation in each use.
An embodiment of the present invention provides a formulation a neutral pH floating bathing bar with high amount of FFA which comprises of:
(i) A first portion that is floating soap.
(ii) A second portion that is syndet bathing bar.
The ratio of combination of floating soap and syndet bathing bar is from 10:90 to 30:70.

The neutral pH floating bathing bar of the present invention has high level of FFA (greater than 25% w/w) and protic acid greater than 0.5 % w/w. The pH ranges from 6.8 to 8.3.
Since both the phase is opaque and as they have very good compatibility among each other they appear to be one phase. Both the phases uniformly get mixed such that it appears as one single opaque floating soap. The significance of providing the two phases is that floating soap can be made with high amount of free fatty acids (FFA) and the composition will provide the neutral pH as a whole.
In floating bathing bar, it is very difficult to incorporate high amount of free fatty acids. It may lead to destabilization of the entrapped air which is essential to maintain the floating behavior.
The composition for the first portion floating soap bar comprises of In-situ soap ((FFA+ NaOH solution), Surfactants, polymer, salt, Aqua, Solvents, Preservative and Color / Fragrance / Emotive.
In-situ soap (FFA+ NaOH solution) according to the present invention includes alkali metal salts of fatty acids such as sodium palmitate and sodium oleate (i.e. anionic surfactants). Among the soaps that are used herein may be saponified glycerides from plant or animal sources such as sodium palmate, sodium palm kernelate, sodium cocoate, sodium tallowate, potassium tallowate, sodium lardate and other alkali metal salt of C8-C22 single chained and branched carboxylic acids
The amount of in-situ soap (FFA+ NaOH solution) required ranges from 15 to 60% wt., preferably from 30 to 50% wt.
Surfactants used in the present invention may be selected from a group comprising anionic surfactants, amphoteric surfactants, nonionic surfactants, and any combinations thereof. As it is well known in the art that surfactant materials can also be an emulsifier, the term “surfactant” does not exclude materials which also have emulsification properties.
The anionic surfactants that may be used in the present invention include but are not limited to alkyl sulfates, anionic acyl sarcosinates, anionic alkyl sarcosinates, methyl acyl taurates, N-acyl glutamates, acyl isethionates, alkyl ether sulfates, alkyl sulfosuccinates, alkyl phosphate esters, ethoxylated alkyl phosphate esters, trideceth sulfates, protein condensates, mixtures of ethoxylated alkyl sulfates and the like. Alkyl chains for these surfactants are C8-22, preferably C10-18 and, more preferably, C12-14 alkyls.
The amphoteric surfactants which can be used in the compositions of the present invention are those which can be broadly described as derivatives of aliphatic secondary and tertiary amines in which the aliphatic radical can be straight chain or branched and wherein one of the aliphatic substituents contains from about 8 to about 18 carbon atoms and one contains an anionic water solubilizing group, e.g., carboxy, sulfonate, sulfate, phosphate, or phosphonate. Examples of compounds falling within this definition are sodium 3-dodecylaminopropionate, sodium 3-dodecylaminopropane sulfonate. Other amphoterics such as betaines are also useful in the present composition. Examples of betaines useful herein include the high alkyl betaines such as coco betaine, coco dimethyl carboxymethyl betaine, lauryl dimethyl carboxy-methyl betaine, lauryl dimethyl alpha-carboxyethyl betaine, cetyl dimethyl carboxymethyl betaine, lauryl bis-(2-hydroxyethyl)carboxy methyl betaine, stearyl bis-(2-hydroxypropyl)carboxymethyl betaine, oleyl dimethyl gamma-carboxypropyl betaine, lauryl bis-(2-hydro-xypropyl)alpha-carboxyet-hyl betaine, etc. The sulfobetaines may be represented by coco dimethyl sulfopropyl betaine, stearyl dimethyl sulfopropyl betaine, amido betaines, amidosulfobetaines, and the like.
The nonionic surfactants useful in this invention can be broadly defined as compounds produced by the condensation of alkylene oxide groups (hydrophilic in nature) with an organic hydrophobic compound, which may be aliphatic or alkyl aromatic in nature. Non-limiting examples of preferred nonionic surfactants for use herein are those selected form the group consisting of glucose amides, alkyl polyglucosides, sucrose cocoate, sucrose laurate, alkanolamides, ethoxylated alcohols and mixtures thereof. In a preferred embodiment the nonionic surfactant is selected from the group consisting of glyceryl monohydroxystearate, isosteareth-2, trideceth-3, hydroxystearic acid, propylene glycol stearate, PEG-2 stearate, sorbitan monostearate, glyceryl laurate, laureth-2, cocamide monoethanolamine, lauramide monoethanolamine, decyl glucoside and mixtures thereof. The composition of the present invention may also comprise one or more sugar based surfactants selected from but not limited to condensation products of long chain alcohols with sugar or starch polymers (e.g. decyl polyglucoside and lauryl polyglucoside), amides (e.g. cocoamide diethanolamine and cocoamide monoethanolamine), alkylene oxide derived surfactants (e.g. ceteth-6, ceteareth6, steareth-6, PEG-12 stearate, and PEG-200 glyceryl tallowate), Maltooligosyl Glucoside/Hydrogenated Starch Hydrolysate and mixtures thereof. Preferred sugar based surfactants include Maltooligosyl Glucoside/Hydrogenated Starch Hydrolysate and Alkyl polyglucoside.
The amount of surfactants ranges from 15 to 40% wt., preferably from 20 to 30% wt.
According to the present invention polymers are starches such as corn starch, silicone polymers; water soluble polymers such as polyurethanes, polyacrylates, polyalkylene glycol with molecular weight between 200 and 20,000, preferably between 400 and 10,000 such as PEG 200, PEG 400, PEG600, PEG 1500, PEG 4000, PEG 6000, PEG 8000 and the like; anionic, zwitterionic, amphoteric and nonionic polymers that can be used are, for example, vinylacetate/crotonic acid-copolymers, vinylpyrrolidone/vinylacrylate-copolymers, vinylacetate/butylmaleate/ isobornylacrylate-copolymers, methylvinylether/maleic acid anhydride-copolymers and their esters, which are not cross-linked and with polyoles linked polyacrylacids which are cross-linked, acrylamidopropyltrimethylammonium chloride/ acrylate-copolymers, octylacrylamide/ methylmethacrylate/tert.butylaminoethylmethacrylate/2-hydroxypropylmethacrylate-copolymers, polyvinylpyrrolidone, vinylpyrrolidone/vinylacetate-copolymers, vinylpyrrolidone/ dimethylaminoethylmethacrylate/vinyl caprolactam-terpolymers as well as optionally derivatized cellulose ethers and silicones. The amount of polymers ranges from 0.1 to 3% wt., preferably from 0.5 to 2% wt.
Salts in accordance with the present invention is selected from group comprising sodium chloride, sodium sulfate, sodium lactate, sodium glycolate, sodium citrate, potassium chloride, potassium sulfate, magnesium chloride, calcium chloride and combinations thereof .The amount of salt ranges from 0.1 to 0.8% wt., preferably from 0.3 to 0.5% wt.
The required amount of aqua ranges from 5 to 15% wt., preferably from 7 to 13% wt.
Solvent that may be used in the present invention include glycerin , propylene glycol, sorbitol.
The amount of solvents required ranges from 15 to 35% wt., preferably from 17 to 25% wt.
Preservatives according to the present invention include BHT, EDTA, and phenoxy ethanol. The required amount of preservatives ranges from 0.01 to 0.1% wt., preferably from 0.02 to 0.06% wt.
The colours can be selected from a group comprising C.I. Pigment Black 7 (C.I. 77266), C.I. Pigment Blue 15 (C.I. 74160), C.I. Pigment Blue 15:1 (C.I. 74160), C.I. Pigment Red 4 (C.I. 12085), C.I. Pigment Red 5 (C.I. 12490), C.I. Pigment Red 112 (C.I. 12370), C.I. Pigment Red 181 (C.I. 73360), C.I. Vat Red 1 , C.I. Pigment Green 7 (C.I. 74260), C.I. Pigment Violet 23 (C.I. 51319), C.I. Pigment Yellow 1 (C.I. 11680), C.I. Pigment Yellow 3 and the likeThe required amount of color ranges from 0.0001 to 0.1% wt., preferably from 0.005 to 0.05% wt.
The fragrance may be selected from a group comprising musk oil, civet, castreum, ambergris, plant perfumes such as sandalwood oil, bergamot oil, lemon oil, lavender oil, sage oil, rosemary oil, peppermint oil, eucalyptus oil, menthol, camphor, verbena oil, citroneUa oil, cauout oil, salvia oil, clove oil, chamomiUe oil, sandalwood oil, costus oil, labdanum oil, broom extract, carrot seed extract, jasmine extract, minmosa extract, narcissus extract, oUbanum extract, rose extract and the like, and chemical substances such as acetophenonene, dimethyUnadane derivatives, naphthaline derivatives, aUyl caprate, a-amylcinnamic aldehyde, anethole, anisaldehyde, benzyl acetate, benzyl alcohol, benzyl propionate, borneol, cinnamyl acetate, cinnamyl alcohol, citral citronneUal, cumin aldehyde, cyclamen aldehyde, decanol, ethyl butyrate, ethyl caprate, ethyl cinnamate, ethyl vanillin, eugenol, geraniol, hexenol, a-hexylcinnamic aldehyde, hydroxycitrolneUal, indole, iso-amyl acetate, iso-amyl iso-valeratek iso-eugenol, nalol, linalyl acetate, p-methylacetophenone, methyl anthranilate, methyl dihydroasmonate, methyl eugenol, methyl-ß-naphthol ketone, methylphenhlcarbinyl acetate, musk ketol, musk xylol, 2,5,6-nanodinol, ?-nanolactone, phenylacetoaldehydodimethyl acetate, ß-phenylethyl alcohol, 3,3,5-trimethylcyclohexanol, ?- undecalactone, undecenal, vanillin and mixtures thereof.The required amount of fragrance ranges from 0.1 to 3% wt., preferably from 0.8 to 1.5% wt.
The emotive may be selected from a group comprising , Houttuynia cordata extract, Phellodendron bark extract, melilot extract, dead nettle extract, licorice extract, peony root extract, soapwort extract, luffa extract, cinchona extract, strawberry geranium extract, sophora root extract, nuphar extract, fennel extract, primrose extract, rose extract, rehmannia root extract, lemon extract, lithospermum root extract, aloe extract, calamus root extract, eucalyptus extract, field horsetail extract, sage extract, thyme extract, tea extract, seaweed extract, cucumber extract, clove extract, bramble extract, lemon balm extract, carrot extract, horse chestnut extract, peach extract, peach leaf extract, mulberry extract, knapweed extract, hamamelis extract, placenta extract, thymic extract, silk extract, and licorice extract, blue lotus extract, sea mineral extract, blueberry extract, black currant extract and the like. The required amount of emotive ranges from 0.001 to 0.5% wt., preferably from 0.005 to 0.05% wt.
The composition for the second portion syndet bathing bar comprises of Surfactant, Free fatty acid, Emulsifier, polymer, soap, binders, oil, emollient, preservatives, color / fragrance / emotive, protic acid and aqua.
Surfactants used in the present invention may be selected from a group comprising anionic surfactants, amphoteric surfactants, nonionic surfactants, and any combinations thereof. As it is well known in the art that surfactant materials can also be an emulsifier, the term “surfactant” does not exclude materials which also have emulsification properties.
The anionic surfactants that may be used in the present invention include but are not limited to alkyl sulfates, anionic acyl sarcosinates, anionic alkyl sarcosinates, methyl acyl taurates, N-acyl glutamates, acyl isethionates, alkyl ether sulfates, alkyl sulfosuccinates, alkyl phosphate esters, ethoxylated alkyl phosphate esters, trideceth sulfates, protein condensates, mixtures of ethoxylated alkyl sulfates and the like. Alkyl chains for these surfactants are C8-22, preferably C10-18 and, more preferably, C12-14 alkyls.
The amphoteric surfactants which can be used in the compositions of the present invention are those which can be broadly described as derivatives of aliphatic secondary and tertiary amines in which the aliphatic radical can be straight chain or branched and wherein one of the aliphatic substituents contains from about 8 to about 18 carbon atoms and one contains an anionic water solubilizing group, e.g., carboxy, sulfonate, sulfate, phosphate, or phosphonate. Examples of compounds falling within this definition are sodium 3-dodecylaminopropionate, sodium 3-dodecylaminopropane sulfonate. Other amphoterics such as betaines are also useful in the present composition. Examples of betaines useful herein include the high alkyl betaines such as coco betaine, coco dimethyl carboxymethyl betaine, lauryl dimethyl carboxy-methyl betaine, lauryl dimethyl alpha-carboxyethyl betaine, cetyl dimethyl carboxymethyl betaine, lauryl bis-(2-hydroxyethyl)carboxy methyl betaine, stearyl bis-(2-hydroxypropyl)carboxymethyl betaine, oleyl dimethyl gamma-carboxypropyl betaine, lauryl bis-(2-hydro-xypropyl)alpha-carboxyet-hyl betaine, etc. The sulfobetaines may be represented by coco dimethyl sulfopropyl betaine, stearyl dimethyl sulfopropyl betaine, amido betaines, amidosulfobetaines, and the like.
The nonionic surfactants useful in this invention can be broadly defined as compounds produced by the condensation of alkylene oxide groups (hydrophilic in nature) with an organic hydrophobic compound, which may be aliphatic or alkyl aromatic in nature. Non-limiting examples of preferred nonionic surfactants for use herein are those selected form the group consisting of glucose amides, alkyl polyglucosides, sucrose cocoate, sucrose laurate, alkanolamides, ethoxylated alcohols and mixtures thereof. In a preferred embodiment the nonionic surfactant is selected from the group consisting of glyceryl monohydroxystearate, isosteareth-2, trideceth-3, hydroxystearic acid, propylene glycol stearate, PEG-2 stearate, sorbitan monostearate, glyceryl laurate, laureth-2, cocamide monoethanolamine, lauramide monoethanolamine, decyl glucoside and mixtures thereof. The composition of the present invention may also comprise one or more sugar based surfactants selected from but not limited to condensation products of long chain alcohols with sugar or starch polymers (e.g. decyl polyglucoside and lauryl polyglucoside), amides (e.g. cocoamide diethanolamine and cocoamide monoethanolamine), alkylene oxide derived surfactants (e.g. ceteth-6, ceteareth6, steareth-6, PEG-12 stearate, and PEG-200 glyceryl tallowate), Maltooligosyl Glucoside/Hydrogenated Starch Hydrolysate and mixtures thereof. Preferred sugar based surfactants include Maltooligosyl Glucoside/Hydrogenated Starch Hydrolysate and Alkyl polyglucoside.
The amount of surfactants ranges from 30 to 55% wt., preferably from 30 to 45% wt.
The “free fatty acids” as used herein are selected from fatty acids with alkyl chain lengths of from C8 – C18. These may be selected from group of linear chained fatty acids, branched chain fatty acids, saturated and unsaturated fatty acids such as Caprylic, Capric, Lauric, Myristic, Palmitic, Stearic, Oleic, etc and mixtures thereofThe amount of free fatty acid required ranges from 25 to 40% wt., preferably from 26 to 37% wt.
Emulsifiers of the present invention can be selected from the list of sodium lauryl ether sulfate (1EO, 2EO, 3EO), Cocomonoethanolamide (CMEA), Cocamidopropyl betaine (CAPB), Alpha Olefin Sulfonate (AOS), decyl glucoside (DG) and the like. Preferred emulsifier is selected from sodium lauryl ether sulfate 1EO, CMEA or CAPB. The amount of emulsifier required ranges from 0.1 to 7 % wt., preferably from 0.5 to 5% wt.
According to the present invention polymers are starches such as corn starch, silicone polymers; water soluble polymers such as polyurethanes, polyacrylates, polyalkylene glycol with molecular weight between 200 and 20,000, preferably between 400 and 10,000 such as PEG 200, PEG 400, PEG600, PEG 1500, PEG 4000, PEG 6000, PEG 8000 and the like; anionic, zwitterionic, amphoteric and nonionic polymers that can be used are, for example, vinylacetate/crotonic acid-copolymers, vinylpyrrolidone/ vinylacrylate-copolymers, vinylacetate/ butylmaleate/ isobornylacrylate-copolymers, methylvinylether/maleic acid anhydride-copolymers and their esters, which are not cross-linked and with polyoles linked polyacrylacids which are cross-linked, acrylamidopropyltrimethylammonium chloride/ acrylate-copolymers, octylacrylamide/ methylmethacrylate/tert.butylaminoethylmethacrylate/2-hydroxypropylmethacrylate-copolymers, polyvinylpyrrolidone, vinylpyrrolidone/ vinylacetate-copolymers, vinylpyrrolidone/ dimethylaminoethylmethacrylate/vinyl caprolactam-terpolymers as well as optionally derivatized cellulose ethers and silicones.The amount of polymer required ranges from 0.5 to 6% wt., preferably from 1 to 3% wt.
Soap according to the present invention includes alkali metal salts of fatty acids such as sodium palmitate and sodium oleate (i.e. anionic surfactants). Among the soaps that are used herein may be saponified glycerides from plant or animal sources such as sodium palmate, sodium palm kernelate, sodium cocoate, sodium tallowate, potassium tallowate, sodium lardate and other alkali metal salt of C8-C22 single chained and branched carboxylic acids. The amount of soap required ranges from 10 to 25% wt., preferably from 12 to 18% wt.
Binders according to the present invention include high molecular weight poly acrylates, high molecular weight poly-ox, silicates, fatty alcohols, lanolin, sugars, tallow alcohol ethoxylates, and mixtures thereof. Other plastic binders are identified in the published literature (J. Amer. Oil Chem. Soc. 1982, 59, 442). The amount of binder required ranges from 0.05 to 5% wt., preferably from 1 to 3% wt.
Preferred oil is selected from propylene glycol, glycerin, sorbitol, paraffin oil and the preferred oil is glycerin. The amount of oil required ranges from 0.01 to 5% wt., preferably from 0.5 to 3% wt.
Emollients are substance which soften or improve the elasticity, appearance, and youthfulness of the skin (stratum corneum) by increasing its water content, and keeps it soft by retarding the decrease of its water content. Emollients that may be used in the present invention include but are not limited to silicone oils and modifications thereof such as linear and cyclic polydimethylsiloxanes; polyols such as glycerol, sorbitol; amino, alkyl, alkylaryl, and aryl silicone oils; fats and oils including natural fats and oils such as jojoba, soybean, sunflower, rice bran, avocado, almond, olive, sesame, persic, castor, coconut, mink oils; cacao fat; beef tallow, lard; hardened oils obtained by hydrogenating the aforementioned oils; and synthetic mono, di and triglycerides such as myristic acid glyceride and 2-ethylhexanoic acid glyceride; waxes such as carnauba, spermaceti, beeswax, lanolin, and derivatives thereof; hydrophobic plant extracts; hydrocarbons such as liquid paraffin, petrolatum, microcrystalline wax, ceresin, squalene, pristan and mineral oil; higher fatty acids such as lauric, myristic, palmitic, stearic, behenic, oleic, linoleic, linolenic, lanolic, isostearic, arachidonic and poly unsaturated fatty acids (PUFA); higher alcohols such as lauryl, cetyl, stearyl, oleyl, behenyl, cholesterol and 2-hexydecanol alcohol; esters such as cetyl octanoate, myristyl lactate, cetyl lactate, isopropyl myristate, myristyl myristate, isopropyl palmitate, isopropyl adipate, butyl stearate, decyl oleate, cholesterol isostearate, glycerol monostearate, glycerol distearate, glycerol tristearate, alkyl lactate, alkyl citrate and alkyl tartrate; essential oils and extracts thereof such as mentha, jasmine, camphor, white cedar, bitter orange peel, ryu, turpentine, cinnamon, bergamot, citrus unshiu, calamus, pine, lavender, bay, clove, hiba, eucalyptus, lemon, starflower, thyme, peppermint, rose, sage, sesame, ginger, basil, juniper, lemon grass, rosemary, rosewood, avocado, grape, grapeseed, myrrh, cucumber, watercress, calendula, elder flower, geranium, linden blossom, amaranth, seaweed, ginko, ginseng, carrot, guarana, tea tree, jojoba, comfrey, oatmeal, cocoa, neroli, vanilla, green tea, penny royal, aloe vera, menthol, cineole, eugenol, citral, citronelle, borneol, linalool, geraniol, evening primrose, camphor, thymol, spirantol, penene, limonene and terpenoid oils; and mixtures of any of the foregoing components, and the likeThe amount of emollient required ranges from 0.01 to 2% wt., preferably from 0.1 to 0.8%n wt.
Preservatives according to the present invention include BHT, EDTA, and phenoxy ethanol. The required amount of preservatives ranges from 0.01 to 0.1% wt., preferably from 0.02 to 0.05% wt.
The colours can be selected from a group comprising C.I. Pigment Black 7 (C.I. 77266), C.I. Pigment Blue 15 (C.I. 74160), C.I. Pigment Blue 15:1 (C.I. 74160), C.I. Pigment Red 4 (C.I. 12085), C.I. Pigment Red 5 (C.I. 12490), C.I. Pigment Red 112 (C.I. 12370), C.I. Pigment Red 181 (C.I. 73360), C.I. Vat Red 1 , C.I. Pigment Green 7 (C.I. 74260), C.I. Pigment Violet 23 (C.I. 51319), C.I. Pigment Yellow 1 (C.I. 11680), C.I. Pigment Yellow 3 and the like. The required amount of color ranges from 0.0001 to 0.1% wt., preferably from 0.005 to 0.05% wt.
The fragrance may be selected from a group comprising musk oil, civet, castreum, ambergris, plant perfumes such as sandalwood oil, bergamot oil, lemon oil, lavender oil, sage oil, rosemary oil, peppermint oil, eucalyptus oil, menthol, camphor, verbena oil, citronea oil, cauout oil, salvia oil, clove oil, chamomie oil, sandalwood oil, costus oil, labdanum oil, broom extract, carrot seed extract, jasmine extract, minmosa extract, narcissus extract, obanum extract, rose extract and the like, and chemical substances such as acetophenonene, dimethynadane derivatives, naphthaline derivatives, ayl caprate, a-amylcinnamic aldehyde, anethole, anisaldehyde, benzyl acetate, benzyl alcohol, benzyl propionate, borneol, cinnamyl acetate, cinnamyl alcohol, citral citronneUal, cumin aldehyde, cyclamen aldehyde, decanol, ethyl butyrate, ethyl caprate, ethyl cinnamate, ethyl vanillin, eugenol, geraniol, hexenol, a-hexylcinnamic aldehyde, hydroxycitrolneal, indole, iso-amyl acetate, iso-amyl iso-valeratek iso-eugenol, nalol, linalyl acetate, p-methylacetophenone, methyl anthranilate, methyl dihydroasmonate, methyl eugenol, methyl-ß-naphthol ketone, methylphenhlcarbinyl acetate, musk ketol, musk xylol, 2,5,6-nanodinol, ?-nanolactone, phenylacetoaldehydodimethyl acetate, ß-phenylethyl alcohol, 3,3,5-trimethylcyclohexanol, ?- undecalactone, undecenal, vanillin and mixtures thereof. The required amount of fragrance ranges from 0.1 to 3% wt., preferably from 0.8 to 1.5% wt.
The emotive may be selected from a group comprising, Houttuynia cordata extract, Phellodendron bark extract, melilot extract, dead nettle extract, licorice extract, peony root extract, soapwort extract, luffa extract, cinchona extract, strawberry geranium extract, sophora root extract, nuphar extract, fennel extract, primrose extract, rose extract, rehmannia root extract, lemon extract, lithospermum root extract, aloe extract, calamus root extract, eucalyptus extract, field horsetail extract, sage extract, thyme extract, tea extract, seaweed extract, cucumber extract, clove extract, bramble extract, lemon balm extract, carrot extract, horse chestnut extract, peach extract, peach leaf extract, mulberry extract, knapweed extract, hamamelis extract, placenta extract, thymic extract, silk extract, and licorice extract, blue lotus extract, sea mineral extract, blueberry extract, black currant extract and the like. The required amount of emotive ranges 0.001 to 0.5% wt., preferably from 0.005 to 0.05% wt.
Protic acid may include, but are not limited to, citric acid, lactic acid, oxalic acid. The amount of protic acids required ranges from 0.5 to 2% wt., preferably from 0.5 to 1.5% wt.
The required amount of aqua ranges from 1 to 5% wt., preferably from 1 to 4% wt.
The neutral pH floating soap bar has properties like:

· Neutral pH
· superior surface finish
· high level of FFA
· improved post wash deposition
· better In-use sensory
· Higher amount of lather
· creamy lather
· employs energy efficient process

Another embodiment of the present invention provides a process for the preparation of the floating bathing bar with high amount of FFA.
The process for making the first portion i.e. the floating bathing bar ( Part A) comprises steps of:
(a) Mixing all the solvents and FFA in the mixer at a specified temperature. The required temperature ranges from 50-75°C, preferably from 60 to 70°C for 5-15 mins, preferably for 7 to 10 mins.
(b) Adding surfactants after step (a) at 70 °C
(c) Generation of in-situ soap after step (b) with the drop wise addition of NaOH solution and carrying out homogenization. The temperature for homogenization ranges from 80 to 95°C, preferably from 80 to 90°C.
(d) Mixing to obtain a homogenous mass.
(e) adding other additives like BHT, EDTA, and fragrance etc once the product of step (d) is obtained.
The process for making the second portion i.e. syndet mass with high amount of FFA (part B) and protic acid comprises steps of:
(a) Melting and mixing fatty acids, polymers, waxes, oil, and emulsifier at a specific temperature. The temperature ranges from 60-75°C, preferably from 60 to 70°C
(b) Adding soap at a specified temperature after step (a) is carried on for a while. Step (a) is carried out for 10-30 mins, preferably for 15 to 25 mins. The specified temperature for which step (b) is carried out ranges from 80-95°C, preferably from 80 to 90°C.
(c) Adding protic acids followed by surfactants after completion of step (b) and maintaining the product at a temperature ranging from 85-95°C, preferably from 85 to 90°C.
(d) Adding of additives like TiO2, EDTA, and fragrance after mixing the soap and surfactants thoroughly.
(e) Adding binders, emollients and emotives at a high mixing speed. The mixing time ranges from 0.5 to 10 minutes, preferably from 4 to 7 minutes. The process is followed by the process of homogenization.
(f) Maintain the final product at a temperature ranging from 80-90°C, preferably from 85 to 90°C. This is done to achieve pouring consistency in mixer.
The first portion is then cast into desired mould and once the mass reaches to semisolid stage, the second portion is added in desired ratio. The desired ratio is 10:90, preferably 30:70. The second portion completely coats the solidified first portion to achieve high FFA floating bar with excellent finish.

The present inventors have found that the best possible ratio of the floating soap bar and the syndet bathing bar of the present invention in order to achieve the desired result is 20:80.

The present invention is now illustrated by way of non limiting examples. Experiments have been conducted to illustrate the floating bathing bar with high amount of FFA.

Example 1: Neutral pH Floating bathing bar
Table 1
Ingredients Range % w/w Exact % w/w
Part-A (floating soap mass)
Surfactant 15-40 23.95
In-situ soap (FFA+ NaOH solution) 15-60 43
Polymer 0.1-3.0 1.5
Salt 0.1-0.8 0.3
Aqua 5-15 12
Solvents (PG, Sorbitol etc) 15-35 18
Preservatives 0.01-0.1 0.05
Additives like color, fragrance etc 0-4 1.2
Part-B (Syndet mass)
Surfactant 35-55 39
Free Fatty Acid 30-40 30*
Emulsifiers 1-7 5
Polymer 1-6 2
Soap 10-25 14
Binders 0.5-5.0 2
Oil 0-5 3
Emollient 0-2 0.5
Preservatives 0.01-0.1 0.05
Color / Fragrance / Emotive 0-1.5 1.25
Protic acid 0.55-2.0 0.7#
Aqua 1-5 3.5

The ratio of combination of combination of floating mass (part A) to Syndet mass (part B) is 10:90.
*Part B used in the formulation is 90%. So the free fatty acid (FFA) in the final composition is 90% of 30 i.e. 27.
#Part B used in the formulation is 90%. So the protic acid in the final composition is 90% of 0.7 i.e. 0.63.
Example 2: Neutral pH floating bathing bar
Table 2
Ingredients Range % w/w Exact % w/w
Part-A (Floating soap mass)
Surfactant 15-40 25
In-situ soap (FFA+ NaOH solution) 15-60 46
Polymer 0.1-3.0 1.5
Salt 0.1-0.8 0.3
Aqua 5-15 10
Solvents (PG, Sorbitol etc) 15-35 16
Preservatives 0.01-0.1 0.05
Additives like color, fragrance etc 0-4 1.15
Part-B (Syndet mass)
Surfactant 35-55 38.5
Free Fatty Acid 33-50 34*
Emulsifiers 1-7 3
Polymer 1-6 2
Soap 10-25 11
Binders 0.5-5.0 2
Oil 0-5 3
Emollient 0-2 0.5
Preservatives 0.01-0.1 0.05
Color / Fragrance / Emotive 0-1.5 1.25
Protic acid 0.5-2.0 0.7*
Aqua 1-5 4

The ratio of combination of combination of floating mass (part A) to Syndet mass (part B) is 20:80.
*Part B used in the formulation is 80%. So the free fatty acid (FFA) in the final composition is 80% of 34 i.e. 27.2.
#Part B used in the formulation is 80%. So the protic acid in the final composition is 80% of 0.7 i.e. 0.56.
Example 3: Non-working example

Table 3:

Ingredients Exact % w/w[Ratio of combination of floating to Syndet mass is 50:50] Exact % w/w[Ratio of combination of floating to Syndet mass is 40:60]
Total free fatty acids in composition The free fatty acid (FFA) in the final composition is 50% of 36 i.e. 18 The free fatty acid (FFA) in the final composition is 60% of 33.3 i.e. 19.9
Total protic acid in composition The protic acid in the final composition is 50% of 0.5 i.e. 0.25 The protic acid in the final composition is 60% of 0.5 i.e. 0.3
Part-A (Floating soap mass)
Surfactant 12 11
In-situ soap (FFA+ NaOH solution) 54.35 51.45
Polymer 1 1
Salt 0.3 0.3
Aqua 8 8
Solvents (PG, Sorbitol etc) 23 27
Preservatives 0.05 0.05
Additives like color, fragrance etc 1.2 1.2
Part-B (Syndet mass)
Surfactant 35.5 35.2
Free Fatty Acid 36 33.3
Emulsifiers 5 7
Polymer 2 2
Soap 10 12
Binders 1.5 1
Oil 4 3
Emollient 0.2 0.5
Preservatives 0.05 0.05
Color / Fragrance / Emotive 1.25 1.45
Protic acid 0.5 0.5
Aqua 4 4
pH of the formulation 8.6 8.5

The pH of the formulation is not in the desired range (i.e. between 6.8 to 8.3) and hence the desired results are not obtained.

Example 4: Table showing the working and the non-working ratio of the low pH floating bathing bar of the present invention.

Table 4

Floating: Syndet ratio FFA % Protic acid pH @ 23-250C Foam Quality (visual assessment) Floating Properties Surface Finish
10:90 30 0.55 6.8-7.2 Very Creamy Floats Very good
20:80 28 0.6 7.1-7.4 Very Creamy Floats Very good
25:75 27 0.7 7.3-7.6 Very Creamy Floats Very good
30:70 25 0.70.12 8.1-8.3 Very Creamy Floats very Good
40:60 20 0.15 8.4-8.5 Very creamy Floats Very Good
50:50 18 0.10 8.5-8.9 Very Creamy Floats very Good
70:30 12 0.10 9.2-9.3 Creamy Floats very Good
60:40 10 0.10 9.3 Creamy Floats very Good
85:15 7-8 0.10 9.3-9.5 Airy Foam Floats Uneven
100:0 (normal floating bar) 5-6 0.10 9.8-10 Airy Foam Floats Uneven

Best working ratio of the present invention is 20:80 (ratio of floating mass (part A) to Syndet mass (part B) )

Example 5: Improved post wash deposition

Table 5

Composition Surface finish (figure 1) Post wash deposition Lather amount (ml) in 30 FH Creamy lather In-use sensory score pH
Neutral pH bathing bar Good High 360 Yes 4 7.5
Neutral pH floating bathing bar Good High 500 Yes 4 7.6
Floating soap bar Not good Low 500 No 2 10.2

Example 6: Process for the preparation of the floating bathing bar with high amount of FFA.

For Making Part-A: floating bathing bar

a) Mix all solvents and FFA in mixer at 70-75°C for (10-15min).
b) Post mixing of solvent, add surfactants
c) Once solvent & surfactant mixed properly, generate in-situ soap by drop wise addition of NaOH solution by mixing followed by homogenization .Maintain the temperature between 85-90°C
d) Mixing for long enough to get homogenous mass
e) Once soap & surfactants are mixed completely, add other additives like BHT, EDTA, and fragrance etc.

For Making Part-B: syndet bathing bar

a) Mix all fatty acids, polymers, waxes, oil, emulsifier in mixer at 65-75°C
b) Post melting and mixing for sufficient time (20-30mins), add soap @ 85-90°C
c) Post soap melting add protic acid followed by surfactants. Maintain temperature between 90-950C
d) Once soap & surfactants are mixed completely, add other additives like TiO2, EDTA, fragrance etc
e) Then binders, emollients, minerals will be added at high mixing speed followed by homogenization.
f) Maintain the final mass in 85-90°C temperature to achieve pouring consistency in mixer.

Now, Take Part A, Cast into desired mould and once the mass reaches to semisolid stage, Add Part B in desired ratio, coat over the solidified part A to achieve High FFA floating bar with excellent finish.

Example 7: data demonstrating the significance of the presence of free fatty acid in an amount greater than 25% w/w and acid in an amount greater than 0.5% w/w.

Table 6:

Ingredients Exact % w/w[Ratio of combination of floating to Syndet mass is from 20:80]
Free fatty acids (FFA) The free fatty acid (FFA) in the final composition is 80% of 30 i.e. 24 (Less than 25 % w/w) The free fatty acid (FFA) in the final composition is 80% of 28.7 i.e. 22.9 (Less than 25 % w/w) The free fatty acid (FFA) in the final composition is 80% of 33.7 i.e. 26.9 (Greater than 25 % w/w) The free fatty acid (FFA) in the final composition is 80% of 35 i.e. 28 (Greater than 25 % w/w)
Protic acid The protic acid in the final composition is 80% of 0.25 i.e. 0.2 (Less than 0.5 % w/w) The protic acid in the final composition is 80% of 0.68 i.e. 0.54 (Greater than 0.5 % w/w) The protic acid in the final composition is 80% of 0.25 i.e. 0.2 (Less than 0.5 % w/w) The protic acid in the final composition is 80% of 0.75 i.e. 0.6 (Greater than 0.5 % w/w)
Part-A (Floating soap mass)
Surfactant 25 25 25 25
In-situ soap (FFA+ NaOH solution) 46 46 46 46
Polymer 1.5 1.5 1.5 1.5
Salt 0.3 0.3 0.3 0.3
Aqua 10 10 10 10
Solvents (PG, Sorbitol etc) 16 16 16 16
Preservatives 0.05 0.05 0.05 0.05
Additives like color, fragrance etc 1.15 1.15 1.15 1.15
Part-B (Syndet mass)
Surfactant 39 41.5 39.5 38.5
Free Fatty Acid 30 28.7 33.7 35
Emulsifiers 4 4 3 3.95
Polymer 2 2 2.75 2
Soap 13 13 12 10
Binders 2 2 2 2
Oil 3 2.32 2 3
Emollient 0.5 0.5 0.5 0.5
Preservatives 1 0.05 0.05 0.05
Color / Fragrance / Emotive 1.25 1.25 1.25 1.25
Protic acid 0.25 0.68 0.25 0.75
Aqua 4 4 3 3
pH of the formulation 9.0 8.7 8.9 7.5
Observation Not within the desired pH range Not within the desired pH range Not within the desired pH range Within the desired PH range

Documents

Application Documents

# Name Date
1 GPA of ITC limited.pdf 2014-02-12
2 FORM 3.pdf 2014-02-12
3 Form 2 with complete specification as filed.pdf 2014-02-12
4 Drawings as filed.pdf 2014-02-12
5 173-KOL-2014-(16-04-2014)-FORM-1.pdf 2014-04-16
6 173-KOL-2014-(16-04-2014)-CORRESPONDENCE.pdf 2014-04-16
7 173-KOL-2014-FER.pdf 2017-11-30
8 173-KOL-2014-OTHERS [29-05-2018(online)].pdf 2018-05-29
9 173-KOL-2014-FER_SER_REPLY [29-05-2018(online)].pdf 2018-05-29
10 173-KOL-2014-CLAIMS [29-05-2018(online)].pdf 2018-05-29
11 173-KOL-2014-HearingNoticeLetter.pdf 2019-05-20
12 173-KOL-2014-Written submissions and relevant documents (MANDATORY) [03-07-2019(online)].pdf 2019-07-03
13 173-KOL-2014-PatentCertificate22-10-2019.pdf 2019-10-22
14 173-KOL-2014-IntimationOfGrant22-10-2019.pdf 2019-10-22
15 173-KOL-2014-RELEVANT DOCUMENTS [25-03-2020(online)].pdf 2020-03-25

Search Strategy

1 Searchstrategy_30-11-2017.pdf

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