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WO1995016022A1 - Procede de fabrication de savonnettes et produits obtenus par ce procede - Google Patents

Procede de fabrication de savonnettes et produits obtenus par ce procede Download PDF

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Publication number
WO1995016022A1
WO1995016022A1 PCT/US1993/011743 US9311743W WO9516022A1 WO 1995016022 A1 WO1995016022 A1 WO 1995016022A1 US 9311743 W US9311743 W US 9311743W WO 9516022 A1 WO9516022 A1 WO 9516022A1
Authority
WO
WIPO (PCT)
Prior art keywords
soap
mixture
isethionate
fatty acids
weight
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US1993/011743
Other languages
English (en)
Inventor
Ravi Subramanyam
Liem D. Vu
Ben Gu
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Colgate Palmolive Co
Original Assignee
Colgate Palmolive Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority to US07/802,160 priority Critical patent/US5284598A/en
Priority claimed from US07/802,160 external-priority patent/US5284598A/en
Application filed by Colgate Palmolive Co filed Critical Colgate Palmolive Co
Priority to PCT/US1993/011743 priority patent/WO1995016022A1/fr
Priority to AU57381/94A priority patent/AU5738194A/en
Publication of WO1995016022A1 publication Critical patent/WO1995016022A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2075—Carboxylic acids-salts thereof
    • C11D3/2079—Monocarboxylic acids-salts thereof
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D10/00—Compositions of detergents, not provided for by one single preceding group
    • C11D10/04—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap
    • C11D10/042—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap based on anionic surface-active compounds and soap
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D13/00—Making of soap or soap solutions in general; Apparatus therefor
    • C11D13/14—Shaping
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/006—Detergents in the form of bars or tablets containing mainly surfactants, but no builders, e.g. syndet bar
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/126—Acylisethionates

Definitions

  • the invention relates to an improved process for making a mild, detergent-soap, toilet bar containing, by weight, about 45% to 70% of sodium or potassium C6 - C18 acyl isethionate, about 10% to 40% of C12 - C20 fatty acids as a plasticizer and superfatting agent, about 3% to 25% of a water-soluble sodium or potassium soap and 2% to 10% of water which comprises the step of forming a liquid mixture of said isethionate, said fatty acids and said soap in the presence of from 0.5% to 2.5% by weight based upon the toilet bar of a vegetable oil at a temperature of from about 85° C. to 105°C.
  • the liquid mixture formed in the presence of the vegetable oil has a reduced viscosity as compared with an identical mixture made without said vegetable oil and yields bars with improved slip, low isethionate degradation and low grit.
  • the bars were prepared from a liquid mixture of acyl isethionate, fatty acids, anionic syndet and soap mixed at a temperature of about 110°C. to 113°C. for about fifteen minutes.
  • the latter bars contained at least about 4% by weight of sodium isethionate as a processing aid.
  • U.S. 4,696,767 discloses a process for making mild toilet bars wherein a slurry of acyl isethionate, water and a polyol such as sorbitol is formed into a stable solution by heating at a temperature of from 100°C. to 120°C. at 4 - 10 p.s.i.g. and said slurry is mixed with neat soap and this mixt ⁇ re is heated to about 150°C. under a pressure of 4 atmospheres before being spread on a chill roll to provide flakes which yield a toilet bar without grit.
  • the presence of the polyol leads to increased water penetration in the soap dish as well as bar of increased cost.
  • This patent further teaches that use of acyl isethionate in particulate form causes problems-fine particles function as a lacrimatory agent and larger particles yield bars with grit.
  • U.S. 4,663,070 a toilet bar composition in which soap is the principal surfactant is described. Liquid mixtures containing a major proportion of soap plus acyl isethionate, fatty acids, water and sodium isethionate were formed at temperatures of 96°C. to 103°C.
  • U.S. 5,030,376 a similar mixture containing a major proportion of soap is processed under conditions of high shear in a special cavity transfer mixer at temperatures maintained below 40°C. to form a mixture with some of the soap in the delta phase.
  • U.S. 5,041,233 also relates to a similar mixture wherein a mixture of acyl isethionate, fatty acids and soap is prepared at a temperature of 82°C. to 94°C., with the soap being formed in situ. This patent indicates that high viscosity mixtures and hydrolysis of acyl isethionate can be problems in such mixtures.
  • the present invention relates to another process for preparing mild, detergent-soap, toilet bars containing, by weight, from 45% to 70% of sodium or potassium C6 - C18 acyl isethionate, about 10% to 40% of C12 - C20 fatty acids as a plasticizer and superfatting agent, about 3% to 25% of a water soluble C8 - C20 soap and about 2% to 10% water which comprises the step of forming a liquid mixture of said acyl isethionate, fatty acids and soap at a temperature in the range of about 85 C C. to 105 C C. in the presence of about 0.5% to 2.5% by weight
  • SUBSTITUTE SHEET (RULE 9fi ⁇ of a vegetable oil, said weight being based upon the toilet bar, prior to processing said liquid mixture on a chill roll to form particles, e.g., flakes which are further processed to yield said toilet bars, said liquid mixture having a reduced viscosity and being readily pumpable as compared to a liquid mixture prepared in the absence of said vegetable oil. Also included in the invention are the improved toilet bars produced by the foregoing process.
  • the inventive process yields substantially homogeneous, thin chips which result in bars with minimal grit.
  • the process is carried out at temperatures below 110°C. so as to minimize hydrolysis of the acyl isethionate and the process utilizes standard bar processing equipment. Further, the process conserves energy as compared with the prior art processes which employ temperatures above about 110°C. Additionally, the toilet bars resulting from the improved process have the desired hardness, water permeability, low grit and enhanced slip.
  • the improved process comprises the steps of forming a liquid mixture of said isethionate, said fatty acids and at least about 50% by weight of the soap at a temperature of about 85°C. to 88°C. forming a liquid mixture of said vegetable oil and the balance of the soap, admixing said vegetable oil-soap mixture with said isethionate-fatty acids mixture with agitation while maintaining the temperature at 85°C. to 88°C. and continuing the agitation for from 5 to 15 minutes prior to processing the resultant mixture on the chill roll.
  • the improved process comprises the steps of forming a liquid mixture of said isethionate and said fatty acids, forming a liquid mixture of said vegetable oil and said soap at a temperature above about 80°C., admixing the vegetable oil-soap mixture with the isethionate-fatty acids mixture with agitation at a temperature of about 99°C. to 105°C. and continuing said agitation while maintaining said temperature for up to twenty minutes prior to processing the resultant mixture on the chill roll.
  • the resultant bars exhibit the desired properties and are characterized by improved slip due to the presence of the vegetable oil which desirably is a mixture of palm oil and olive oil.
  • the instant invention relates to an improved process of making mild, detergent-soap, toilet bars containing, by weight, about 45% to 70% of sodium or potassium C6 to C18 acyl isethionate, about 10% to 40% of C12 - C20 fatty acids as a plasticizer and superfatting agent, about 3% to 25% of a water-soluble or potassium C8 - C 20 soap and about 2% to 10% of water.
  • Preferred toilet bars contain, by weight, about 45% to 60% of said acyl isethionate, about 15% to 30% of said fatty acids, about 10% to 20% of said soap and about 3% to 9% of water.
  • the improved process which is the subject of this invention is based upon the discovery that the incorporation of about 0.5% to about 2.5% of a vegetable oil into a mixture of alkali metal C6 - C18 acyl isethionate, C12 - C20 fatty acid, a water soluble sodium or potassium C8 - C20 soap and water maintained at a temperature of from 85°C. to about 105°C. reduces the viscosity of the mixture and renders the mixture readily pumpable. Furthermore, the resultant bars made using the reduced viscosity mixture exhibit improved slip and post- washing skin feel.
  • the mixture into which the vegetable oil is incorporated is prepared by melting the fatty acids and the acyl isethionate salt in flake form at a temperature in the range of 85°C. and 105 C C. to form a substantially homogeneous liquid mixture which is mixed with neat soap thereafter.
  • the proportions of each of the three components is chosen to result in the desired mild, detergent- soap, toilet bar.
  • the molten mixture of the acyl isethionate and fatty acids is maintained at a temperature of from 85°C. to 88°C. and the water soluble soap is admixed therewith in two increments-about 75% by weight of soap being added initially and the remaining soap being added about 5 to 15 minutes later after it is mixed with the vegetable oil.
  • the temperature of the molten mixture of acyl isethionate and fatty acids is maintained in the range of about 99°C. to 105°C. prior to being admixed with a mixture of the neat soap and vegetable oil.
  • Suitable acyl isethionate salts contain 6 to 20, preferably 8 to 18, carbon atoms in the acyl group and the salt forming cation is sodium or potassium. These salts are prepared in a known manner by reacting a fatty acid with sodium or potassium isethionate or by reacting. an acyl chloride such as cocoyl chloride or palmitoyl chloride with sodium or potassium isethionate.
  • an acyl chloride such as cocoyl chloride or palmitoyl chloride with sodium or potassium isethionate.
  • the fatty acyl isethionate should have an acyl group in which about 75% of the carbon atoms are in the range of 12 to 18.
  • a particularly preferred salt is sodium cocoyl isethionate.
  • the acyl isethionate is available in particulate form, e.g., flakes, and the content of acyl isethionate is about 50% to 75% by weight.
  • This particulate material contains minor amounts of unmodified reactants such as fatty acids and sodium or potassium isethionate.
  • the concentration of fatty acids ranges from 20% to 45% by weight and the concentration of isethionate salt ranges from 1% to 4% by weight. Water also is usually present in the range of 0.5% to 1.5% by weight.
  • the included quantity of isethionate salt does not adversely affect the resultant toilet bars and, in fact, may provide some desirable properties.
  • the C8 - C20 aliphatic carboxylic acids serve as satisfactory binders and plasticizers in the mild, detergent-soap, toilet bars. Such acids may be saturated or unsaturated and have either straight or branched chains. Suitable acids include lauric acid, myristic acid, palmitic acid, stearic acid and mixtures thereof. A preferred binder plasticizer is a mixture of lauric acid and stearic and palmitic acid wherein about 60% to 80% by weight is the stearic and palmitic acid mixture.
  • the aliphatic carboxylic acids are usually derived from naturally occurring oils and fats.
  • the water soluble soaps employed in the toilet bars are sodium or potassium salts of natural or synthetic aliphatic (alkanoic or alkenoic) acids having a carbon chain length of about 8 to 20 carbon atoms.
  • trigyceride sources providing soaps with carbon chain lengths in this range include coconut oil, palm kernel oil, babassu oil, ouricuri oil, tallow, palm oil, rice bran oil, groundnut oil and rapeseed oil.
  • Preferred soap mixtures are prepared from coconut oil and tallow and comprise about 50% to 90% by weight of tallow fatty acids and about 10% to 50% by weight of coconut oil fatty acids. Such mixtures contain more than 90% by weight of fatty acids having carbon chain lengths in the C12 to C18 range.
  • the preferred mixtures contain some unsaturated soaps, but excessive unsaturation is typically avoided.
  • Soaps may be made by the classic kettle boiling process or fatty acid neutralization process or by more modern continuous soap manufacturing processes. These processes typically produce a neat soap containing from about 65% to 70% by weight of sodium soap, up to about 1.5% by weight of glycerine, up to about 1% by weight of salt, e.g., sodium chloride, and the balance water.
  • neat soap is employed in the described inventive process.
  • Neat soap required in the formula also can be made in the process by mixing soap chips containing 14 - 20% by weight of moisture and the necessary amount of water.
  • the oils utilized in the inventive process may be broadly classed as vegetable oils.
  • Satisfactory oils include tropical nut oils such as palm oil, coconut oil and olive oil as well as non-tropical nut oils such as groundnut oil and rapeseed oil.
  • Preferred oils are palm oil, olive oil and mixtures thereof. Such oils are used in proportion in the range of 0.5% to 2.5%, preferably 1.0% to 2.0%, by weight based upon the final detergent-soap bar.
  • the mild, detergent-soap, toilet bars can contain a variety of other ingredients. These include up to 10% by weight of other anionic detergents such as alkylbenzene sulfonates, alkyl sulfates and alkane sulfonates, up to 5% by weight of fillers such as starch and up to 5% by weight of salts such as sodium chloride and sodium isethionate. Further, up to 2.0% by weight of each of bactericidal agents, fluorescers, dyes or pigments, polymers and perfumes may be included where desired.
  • anionic detergents such as alkylbenzene sulfonates, alkyl sulfates and alkane sulfonates
  • fillers such as starch
  • salts such as sodium chloride and sodium isethionate.
  • salts such as sodium chloride and sodium isethionate.
  • the resultant mild, detergent-soap, toilet bars are prepared by transferring the acyl isethionate, fatty acid, soap and oil homogeneous, pumpable slurry to a chilling roll where some of the moisture is flashed off and the mixture solidifies and is removed by a knife or scraper and pelletized or ground before being transferred to the amalgamator wherein the other ingredients such as the perfume, germicide, dye, etc., is incorporated. Thereafter the mixture is spread on a three or five roll mill from which it is removed in ribbons or flakes. The milled ribbons are compressed and extruded in a plodder to form a log of detergent-soap that is cut, optionally cooled and stamped to form bars or cakes.
  • the inventive process is characterized by the step of forming a liquid mixture of the acyl isethionate, fatty acids and soap at a temperature in the range of 85°C. to 105°C. in the presence of about 0.5% to 2.5% by weight, based upon the finished toilet bar composition, of a vegetable oil.
  • the vegetable oil will be a mixture of palm oil and olive oil, most preferably in a 1:1 weight ratio.
  • the vegetable oil will be mixed with part or all of the added water- soluble soap prior to the admixture of said soap with the liquid mixture of acyl isethionate and fatty acids.
  • the vegetable oil may be admixed with the mixture of acyl isethionate and fatty acids prior to admixture with the water soluble soap which normally is added as neat soap.
  • the acyl isethionate will be added in the form of flakes which include some fatty acids and sodium or potassium isethionate salt in addition to said acyl isethionate.
  • the inventive process comprises the steps of forming a liquid mixture of said acyl isethionate and fatty acids at a temperature of about 85°C. to 88°C., admixing said isethionate-fatty acid mixture with more than 50% by weight of the added water soluble soap in the presence of agitation.
  • the vegetable oil is admixed with the balance of the soap and said mixture is admixed with the foregoing mixture while maintaining the temperature in the range of 85°C. to 88°C.
  • a Paterson mixer is preheated to a temperature of about 85°C. to 88°C. and the sodium cocoyl isethionate in the form of flakes and the stearic acid are charged into the mixer and melted therein in the presence of agitation. Thereafter, 75% of the formula weight of neat soap-an aqueous mixture containing about 70% by weight of the sodium salt of a mixture of about 82% by weight of tallow fatty acids and 18% by weight of coconut oil fatty acids, about 1.5% by weight of glycerine, about 1% by weight of sodium chloride and the balance water— is mixed with the liquid mixture of stearic acid and sodium cocoyl isethionate with agitation.
  • the balance of the neat soap amounting to 25% of the bar formula weight is added with agitation which is continued for from five to fifteen minutes while maintaining the temperature in the range of about 85 C C. to 88 C C.
  • the resultant mixture is processed through a chill-roll mill to form flakes which are admixed with the miscellaneous ingredients in an amalgamator.
  • the mixture from the amalgamator is homogenized on a roll mill and processed through a plodder to form an extrusion which is cut and stamped into bars in a well known manner.
  • EXAMPLE 2 In order to further define the reduction in viscosity achieved by addition of the 1:1 mixture of palm oil and olive oil, a ten pound batch of the mixture of sodium cocoyl isethionate, fatty acids and neat soap of Formulation A above is prepared in a pilot plant Sigma mixer at a temperature in the range of 85°C. to 88°C. The dough-like mass is placed in a covered container and transferred into an oven where the temperature is increased to 106°C. Samples of the mixture are taken and incubated in water baths maintained at 88°C. and 99°C. respectively. A 1:1 mixture of palm oil and olive oil is added to some samples in concentrations of 1% by weight and 2% by weight respectively, said weight being based upon the final bar.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Detergent Compositions (AREA)

Abstract

L'invention concerne un procédé amélioré de fabrication de savonnettes qui contiennent du tensioactif et du savon et qui sont douces pour la peau. Ces savonnettes contiennent un C6 - C18 acyle iséthionate en tant que tensioactif principal, en combinaison avec des proportions mineures d'acides gras en C12 - C20, un savon hydrosoluble et de l'eau. Ce procédé consiste à former un mélange liquide dudit acyle iséthionate, des acides gras et du savon, à une température d'environ 85 °C - 105 °C, en présence d'environ 0,5 % à 2,5 % en poids de la savonnette, d'une huile végétale, puis de passer ce mélange sur un cylindre refroidisseur, pour former des particules qui sont ensuite transformées en savonnettes. Le mélange liquide en question a une viscosité moindre que des mélanges liquides préparés en absence de ladite huile végétale et il est plus facile à pomper. Les savonnettes produites par le procédé décrit font également partie de l'invention.
PCT/US1993/011743 1991-12-04 1993-12-09 Procede de fabrication de savonnettes et produits obtenus par ce procede Ceased WO1995016022A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US07/802,160 US5284598A (en) 1991-12-04 1991-12-04 Process for making mild, detergent-soap, toilet bars and the bar resulting therefrom
PCT/US1993/011743 WO1995016022A1 (fr) 1991-12-04 1993-12-09 Procede de fabrication de savonnettes et produits obtenus par ce procede
AU57381/94A AU5738194A (en) 1991-12-04 1993-12-09 Process for toilet bars and resulting bar

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US07/802,160 US5284598A (en) 1991-12-04 1991-12-04 Process for making mild, detergent-soap, toilet bars and the bar resulting therefrom
PCT/US1993/011743 WO1995016022A1 (fr) 1991-12-04 1993-12-09 Procede de fabrication de savonnettes et produits obtenus par ce procede

Publications (1)

Publication Number Publication Date
WO1995016022A1 true WO1995016022A1 (fr) 1995-06-15

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US1993/011743 Ceased WO1995016022A1 (fr) 1991-12-04 1993-12-09 Procede de fabrication de savonnettes et produits obtenus par ce procede

Country Status (1)

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WO (1) WO1995016022A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006002890A1 (fr) * 2004-07-01 2006-01-12 Unilever Plc Composition de pain de savon de toilette detergent synthetique doux

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH479695A (de) * 1964-12-11 1969-10-15 Unilever Nv Reinigungsmittelstück
FR2273865A1 (fr) * 1974-06-03 1976-01-02 Ferrara Peter Composition pour savon et le procede de preparation correspondant
GB1477897A (en) * 1974-09-06 1977-06-29 Unilever Ltd Synthetic detergent bar
DE2813324A1 (de) * 1977-03-30 1978-10-05 Unilever Nv Herstellung eines reinigungsstuecks
US5041233A (en) * 1988-05-03 1991-08-20 Lever Brothers Company, Division Of Conopco, Inc. Process for preparing soap-acyl isethionate compositions

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH479695A (de) * 1964-12-11 1969-10-15 Unilever Nv Reinigungsmittelstück
FR2273865A1 (fr) * 1974-06-03 1976-01-02 Ferrara Peter Composition pour savon et le procede de preparation correspondant
GB1477897A (en) * 1974-09-06 1977-06-29 Unilever Ltd Synthetic detergent bar
DE2813324A1 (de) * 1977-03-30 1978-10-05 Unilever Nv Herstellung eines reinigungsstuecks
US5041233A (en) * 1988-05-03 1991-08-20 Lever Brothers Company, Division Of Conopco, Inc. Process for preparing soap-acyl isethionate compositions

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006002890A1 (fr) * 2004-07-01 2006-01-12 Unilever Plc Composition de pain de savon de toilette detergent synthetique doux

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