Process for Manufacturing Concentrated Surfactant Compositions Konzentrierte Tensidzusammensetzungen Compositions Tensioactives Concentrées
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(19) TZZ Z___ T (11) EP 2 089 111 B2 (12) NEW EUROPEAN PATENT SPECIFICATION After opposition procedure (45) Date of publication and mention (51) Int Cl.: of the opposition decision: A61Q 5/02 (2006.01) A61Q 19/10 (2006.01) 04.09.2013 Bulletin 2013/36 A61K 8/02 (2006.01) A61K 8/46 (2006.01) C11D 1/37 (2006.01) C11D 1/83 (2006.01) (2006.01) (2006.01) (45) Mention of the grant of the patent: C11D 1/94 C11D 17/00 24.02.2010 Bulletin 2010/08 (86) International application number: (21) Application number: 07847667.8 PCT/EP2007/063156 (22) Date of filing: 03.12.2007 (87) International publication number: WO 2008/068222 (12.06.2008 Gazette 2008/24) (54) PROCESS FOR MANUFACTURING CONCENTRATED SURFACTANT COMPOSITIONS KONZENTRIERTE TENSIDZUSAMMENSETZUNGEN COMPOSITIONS TENSIOACTIVES CONCENTRÉES (84) Designated Contracting States: (74) Representative: Bristow, Stephen Robert et al AT BE BG CH CY CZ DE DK EE ES FI FR GB GR Unilever Patent Group HU IE IS IT LI LT LU LV MC MT NL PL PT RO SE Colworth House SI SK TR Sharnbrook Bedford, MK44 1LQ (GB) (30) Priority: 08.12.2006 EP 06125743 (56) References cited: (43) Date of publication of application: EP-A- 0 922 754 EP-A1- 1 696 023 19.08.2009 Bulletin 2009/34 EP-A2- 1 225 214 WO-A-99/09944 WO-A1-94/18946 WO-A2-01/25378 (73) Proprietors: DE-A1- 19 641 280 DE-A1- 19 646 882 • Unilever PLC DE-A1- 19 929 511 DE-A1- 19 944 544 London DE-A1- 19 950 925 FR-A1- 2 398 797 EC4Y 0DY (GB) FR-A1- 2 826 017 GB-A- 2 013 235 Designated Contracting States: GB-A- 2 021 141 GB-A- 2 022 125 CY GB IE MT US-A- 4 898 690 US-A- 5 066 425 • Unilever N.V. US-A1- 2005 143 277 3013 AL Rotterdam (NL) Designated Contracting States: • MCCUTCHEON’S: ’Emulsifiers & detergents AT BE BG CH CZ DE DK EE ES FI FR GR HU IS IT international edition’, vol. 1, 1999, THE LI LT LU LV MC NL PL PT RO SE SI SK TR MANUFACTURING CONFECTIONER PUBLISHING CO., GLEN ROCK page 55 (72) Inventors: • HENKEL KGAA: ’Texapon N70’ COSPHA no. 6, • BASAPPA, Geetha September 1996, Bedford • FARN, RICHARD, J.: ’Chemistry and technology Bedfordshire MK44 1LQ (GB) ofsurfactants’, 2006, BLACKWELL PUBLISHING, • BELMAR, Maria Teresa OXFORD pages 1 - 338 Bedford • PROCTER & GAMBLE: ’Process for Bedfordshire MK44 1LQ (GB) manufacturing concentrated surfactant • TELFORD, Julia Helen compositions’ TECHNICAL REPORT 18 July Bedford 2012, pages 1 - 2 Bedfordshire MK44 1LQ (GB) EP 2 089 111 B2 Printed by Jouve, 75001 PARIS (FR) EP 2 089 111 B2 Description [0001] The present invention relates to a method of manufacture of a composition comprising a high amount of a specific surfactant mixture and water. 5 [0002] Concentrated formulations comprising surfactants as well as mixtures of surfactants are usually provided to reduce the transport costs as well as to reduce storage capacities. Usually the commonly known concentrates comprise all essential ingredients for producing, for example, a personal care composition with the exception of solvent (which is usually water). [0003] The goal of the present invention is to provide a highly concentrated surfactant composition which is stable, 10 whichcan serve asa basecomposition (skeleton composition) and whichcan behandled reasonably easily andcomprises two surfactants and water only. [0004] FR 2 826 017 A1 discloses a mixture of surfactants comprising an alkyl and/or alkenyl oligoglycoside, betaine and an alkyl ether sulphate [0005] EP 1 225 214 A2 discloses a detergent composition which foams well and is not slimy containing an alkali 15 metal taurate salt or an organic alkali taurate salt of N-acylmethyltaurate, N- acyltaurine, alkylsulphuric ester, alkyl ether sulphuric ester or alkylsulphonic acid. [0006] DE 199 44 544 A1 discloses a surfactant mixture comprising an alkyloligoglycoside and an alkyl- and/or alke- nylether sulphate. [0007] FR 2 398 797 A1 discloses concentrated aqueous surfactant compositions comprising mixtures of different 20 surfactants for use in aqueous systems. [0008] WO 99/09944 A1 discloses aqueous nacreous lustre dispersions containing fatty acid polyglycol ester sulphate, emulsifiers, nacreous lustre waxes and polyols. [0009] DE 196 41 280 A1 discloses waterborne pearlescent dispersions comprising monoglyceride (ether)sulphate, emulsifiers and polyols. 25 [0010] EP 0 922 754 A1 discloses pearlescent compositions comprising a fatty acid, an alkylether sulphate or acyli- sethionate, and water. [0011] DE 196 46 882 A1 discloses an aqueous polyol free pearlescing concentrate based on selected surface- active emulsifiers and pearlescent waxes. 30 Description of the Invention [0012] The present invention relates to a process for manufacturing a composition, the composition comprising: (i) 50-95% by weight, based on the total weight of the composition, of 35 (ia) an alkyl ether sulphate and/or salt thereof, and (ib) at least one further surfactant which is an anionic and/or amphoteric surfactant, and (ic) optionally one or more non-ionic surfactants; and 40 (ii) 5 - 50 % by weight, based on the total weight of the composition, of water, wherein the alkyl ether sulphate and/or salt thereof of (ia) and the anionic surfactant of (ib) are not identical surfactants, the process comprising the steps of: 45 (a) providing the alkyl ether sulphate or salt thereof in the form of a mixture with no more than 35% by weight, based on the total weight of the mixture, of water; then (b) adding to and mixing with the mixture the at least one further surfactant chosen from the group consisting of anionic and/or amphoteric surfactants in substantially anhydrous form and the optional one or more non- ionic sur- factants in substantially anhydrous form thereby to form the composition, 50 wherein the alkyl ether sulphate or salt thereof remains in a liquid crystalline lamellar phase or lamellar gel phase throughout the process. [0013] Preferred compositions comprise 50 - 90 %, preferably 60 - 85 % by weight of (i). As a consequence thereof preferred compositions comprise 10 - 50 %, preferably 15 - 40 % by weight, based on the total weight of the composition, 55 of water. [0014] A further embodiment of the present invention is a composition where the ratio of (ia) : [(ib) + (ic)] is 1:2 to 40: 1, preferably 1: 1 to 30:1. [0015] Preferred compositions comprise ≤ 10 % by weight, based on the total amount of the composition, of non- ionic 2 EP 2 089 111 B2 surfactants. [0016] The compositions have the advantage that without using any further additives, the compositions show good stability as well as good handling properties. Without the need to include any further additives (such as, for example, preservatives), it opens a wide field of interesting applications and uses. A user can, for example, choose to add a 5 preservative (or other ingredients) or not. The user can be found in industry as well as in private households. [0017] The composition is preferably used as a base composition for a personal care composition. Preferred personal care compositions are body washes (such as for shower or bath) and/or shampoos. [0018] The compositions preferably have a pH ≥ 5, preferably ≥ 5.5. [0019] The composition preferably excludes added preservative, thus the composition may contain traces of preserv- 10 atives which can be found in the commercially available surfactants and which cannot be removed completely. The amount of preservative in the composition is usually less than 0.1 % by weight of the composition. [0020] The term preservative is to be understood as a natural or synthetic chemical that is added to products to retard spoilage, whether from microbial growth, or undesirable chemical changes. A distinction is sometimes made between anti-microbial preservatives which function by inhibiting the growth of bacteria and fungi, and antioxidants such as oxygen 15 absorbers, which inhibit the oxidation of food constituents. Common anti- microbial preservatives include sodium nitrate, sodium nitrite, sulphites (sulfur dioxide, sodium bisulfite, potassium hydrogen sulfite) and disodium EDTA. Antioxidants include BHA and BHT. Other preservatives include formaldehyde (usually in solution), glutaraldehyde, diatomaceous earth (kills insects), ethanol, dimethyl dicarbonate and methylchloroisothiazolinone. Further preservatives include 2- bromo-2-nitropropane-1,3-diol, phenoxy ethanol citric acid, tartaric acid, phosphoric acid, iminodiacetic acid, nitrilotriace- 20 tic acid, hydroxyethyleneaminodiacetic acid and ethylenediaminetetraacetic acid and salts thereof; para-hydroxyben- zoates such as butyl paraben, methyl paraben and propyl paraben; imidazolines (e.g. imidiazolinylurea), triclosan, hydantoins (e.g. dimethyloldimethylhydantoin), isothiazolidinone compounds; and mixtures thereof. Commercially avail- able preservatives include Kathon® CG, Kathon® CGII and Myacide®. [0021] A further preferred embodiment relates to a composition excluding a pearlescent agent or an opacifying agent. 25 Examples of a pearlescent or an opacifying agent include, but are not limited to: mono- or diesters of (a) fatty acids having 16 to 22 carbon atoms and (b) either ethylene or propylene glycol; mono- or diesters of (a) fatty acids having 16 to 22 carbon atoms (b) a polyalkylene glycol of the formula HO-(JO)a-H, wherein J is an alkylene group having 2 to 3 carbon atoms, and a is 2 or 3, and fatty alcohols containing 16 to 22 carbon atoms; fatty esters of the formula KCOOCH 2L, wherein K and L independently contain 15 to 21 carbon atoms; inorganic solids insoluble in the composition; and mixtures 30 thereof. [0022] The compositions always comprise alkyl ether sulphates or salts thereof. Preferred alkyl ether sulphates salts are those of formula RO-(CH2CH2O)xSO3M, 35 wherein R is an alkyl or alkenyl group of 8 to 24 carbon atoms, x is an integer having a value of 1 to 10, and M is a cation such as ammonium, alkanolamines such as triethanolamine, monovalent metals such as sodium and potassium, and polyvalent metal cations such as magnesium and calcium.