@ Inventor: Constantlne, Margaret Joan

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J ~ " ' Nil II II II Nil II II Mil II Ml Ml European Patent Office Office europeen des brevets _ ^ Publication number: 0 330 435 B1 EUROPEAN PATENT SPECIFICATION Date of publication of patent specification: 02.02.94 Int. CI.5: A61 K 7/075, C11D 17/00 Application number: 89301683.2 @ Date of filing: 22.02.89 Solid shampoo composition. @ Priority: 23.02.88 GB 8804138 @ Date of publication of application: 30.08.89 Bulletin 89/35 Publication of the grant of the patent: 02.02.94 Bulletin 94/05 Designated Contracting States: AT BE CH DE ES FR GB GR IT LI LU NL SE References cited: EP-A- 0 122 664 US-A- 4 012 341 CHEMICAL ABSTRACTS, vol. 92, no. 18, 5th May 1980, page 390, abstract no. 152886f, Columbus, Ohio, US; & JP-A-79 112 906 (KANEBO LTD) 04-09-1979 Proprietor: CONSTANTINE & WEIR LIMITED 29 High Street Poole Dorset BH15 1AB(GB) @ Inventor: Constantlne, Margaret Joan 29 High Street Poole Dorset BH15 1AB(GB) Inventor: Krysztal, Stanlslaw 136 Richmond Hill Richmond Surrey TW10 6RN(GB) Representative: Bowman, Paul Alan et al LLOYD WISE, TREGEAR & CO. Norman House 105-109 Strand London WC2R OAE (GB) Kirk Othmer, Encyclopedia of Chemical Technology, 3rd Edition, vol. 21, pp. 170, 175 00 00 00 Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid (Art. 99(1) European patent convention). Rank Xerox (UK) Business Services (3. 10/3.09/3.3.3)

Description This invention relates to shampoos. Shampoo is usually made from liquid detergent and water with other ingredients such as gelling agents, 5 cream or lotion, perfume, dye and preservatives being added as required. The process of making liquid shampoo essentially comprises mixing the selected detergent in water to form a homogeneous liquid, after which the dye perfume and preservative may be added. U.S. Patent No. 4012341 discloses a solid all synthetic detergent shampoo bar comprising from about 10 to 60% of a water soluble, solid, polyethoxylated dialkyl phenol wherein each of the alkyl groups contain io more than 8 carbon atoms; from about 30 to 60% of a sodium or potassium higher alkyl sulphates wherein the alkyl group contains between 12 and 20 carbon atoms; and from about 10 to 40% of the monoethanolamide of stearic acid. The bar is made by heating the ethoxylated dialkylphenol and the monoethanolamide of stearic acid to about 100 C and adding the alkyl sulphate thereto using a high speed mixer. When the composition is smooth it is passed several times through a grinder and finally moulded 75 under pressure. A main object of the present invention is to provide an improved form of shampoo having advantages over the liquids or semi-liquids hitherto in general use and the known solid shampoo bars. The invention provides shampoo in the form of a solid bar comprising 70% to 90% detergent in solid needle form and 1% to 10% water. Preferably the detergent is a anionic surfactant such as sodium lauryl 20 sulphate. Small amounts of various other ingredients can be included such as conditioners, essential oils, perfumes and dyes, and additional binding agents for the needles. The invention includes a method of making a solid shampoo bar comprising the steps of mixing 70% to 90% detergent in solid needle form with 1% to 10% water, and such other ingredients as may be required, so as to coat the needles, and compacting predetermined quantities of the coated needles in a mould under 25 pressure. For a small bar, the needles can be compacted at room temperature and 40-60 p.s.i. (2.8 to 4.2 kg/cm2). In the finished bar, the needles are apparent, on the surface and throughout the thickness of the bar, and there may be some internal voids. One composition, designated A, will now be given by way of example, using sodium lauryl sulphate as the main ingredient. This can be conveniently purchased under the trade mark EMPICOL (Albright & 30 Wilson) which comes in various grades, EMPICOL LXV being chosen for this example. The Composition A is as follows: EMPICOL LXV (Sodium Lauryl 92.0% Sulphate) EMPILAN CDE Fatty Acid 2.0% (a hair conditioner) Dialkylolamides Water 3.0% POLYMER JR400 (Union 2.0% Carbide) Polyquaternium 10 (a hair conditioner) D-Panthanol (Roche Chemical 0.3% (a hair conditioner) Division Hoffman La Roche) 1% Solution in water, U.S. Food, 0.2% Drugs & Cosmetics Yellow No 5 Perfume 0.5% EMPICOL LXV is in needle form with the composition: Sodium Lauryl Sulphate 85.0% Unsulphated Matter 1.5% Sodium Sulphate 1.6% Sodium Chloride 1.0% 55 Other suitable grades are EMPICOL LMV/T and EMPICOL LZV, in which the proportion of sodium lauryl sulphate in EMPICOL is 89% and 85% respectively. Four further examples follow: 2

10 15 20 Examples:- 1 2 3 4 EMPICOL LXV (Sodium Lauryl Sulphate) 90.00 95.25 92.00 89.00 Water 5.00 2.00 5.00 (see below) Propylene Glycol (Binding Agent) 1.25 2.00 Almond Oil 2.00 2.00 Ground Almond 2.00 Dead Sea Salt 1.00 Egg Powder 1.00 Lemon Juice (providing required water) 2.00 Lemon Peel Powder 5.00 Crocin (dye) 0.50 0.50 Chlorophyllin (dye) 0.3 Perfume 0.50 0.20 1.00 0.50 25 30 35 40 45 As will be understood from the foregoing, the active ingredient sodium lauryl sulphate forms only 85% of EMPICOL LXV. In Example 1, therefore, the percentage of sodium lauryl sulphate is 0.85 x 90 = 76.5%. In each Example, bars may be made by first mixing the liquids and small quantity ingredients, and then pouring these on to the needles in a planetary mixer. When the needles are coated, which takes little time, predetermined quantities (e.g. 115 gm) are compressed into bars at room temperature and 40-60 p.s.i. (2.8 to 4.2 kg/cm2). Preferably the bars are compacted into the eventual packaging, for example foil. They may be circular (2 \ inches or 5 cm in diameter) in plan and oval in vertical section. Vegetable oils such as henna extract, coconut oil or cocamide (ethanolamides of coconut oil) can be used: various alternative conditioners are available, as used in conventional shampoos. The water acts as a binder, and as in Examples 2 and 4, a glycol, here propylene glycol, can be added as an additional binding agent. In the accompanying drawings, Figure 1 is a photograph of part of the outer surface of a solid detergent bar according to Example 3 above, magnified about 6 times; and Figure 2 is a photograph of a bar broken apart to show the interior, magnified about 12 times. As will be seen from the drawings, the needles are clearly visible both from the outside and on the interior. One advantage of the solid shampoo composition of the present invention, over the usual liquid shampoos, is that there is no waste during use. Liquid shampoos run through the fingers and drip, whereas the solid shampoo of the present invention is very economical, just one wipe over wetted hair being sufficient to provide a substantial lather. Tests have shown that a weight of shampoo in bar form gives more hair washes than the equivalent liquid, in normal use. Furthermore the distinctive appearance and texture of the shampoo tablet makes it readily recognisable and clearly distinguishable from a normal tablet of soap. Claims 50 A shampoo in the form of a solid bar comprising 70% to 90% detergent in solid needle form and 1% to 10% water. 2. A shampoo as in Claim 1 wherein the detergent is sodium lauryl sulphate. 55 3. A shampoo as in Claim 2 including a conditioner, an essential oil, a perfume and a dye. 4. A method of making a solid shampoo bar comprising the steps of mixing 70% to 90% detergent in solid needle form with 1% to 10% water, and such other ingredients as may be required, so as to coat the needles, and compacting predetermined quantities of the coated needles in a mould under 3

pressure. 5 10 15 5. A method as in Claim 4 wherein the needles are compacted at room temperature and 40-60 p.s.i. (2.8 to 4.2 kg/cm2). 6. A shampoo bar according to Claim 1 comprising 75% to 80% sodium lauryl sulphate in needle form compressed with 2% to 5% water as binder. 7. A shampoo bar as claimed in Claim 6, including an additional binder comprising 1% to 2% glycol. 8. A shampoo bar as claimed in Claim 6, comprising further ingredients from: an additional binder, an essential oil, a perfume and a dye. Patentanspruche 1. Shampoo in Form einer festen Stange, das 70% bis 90% Reinigungsmittel in fester Nadelform und 1% bis 10% Wasser enthalt. 2. Shampoo nach Anspruch 1, 20 dadurch gekennzeichnet, dal3 das Reinigungsmittel Natriumlaurylsulfat ist. 25 30 3. Shampoo nach Anspruch 2, dadurch gekennzeichnet, dal3 es einen Conditioner, ein atherisches Ol, einen Duftstoff und einen Farbstoff enthalt. 4. Methode zur Herstellung einer festen Shampoostange durch Mischen von 70% bis 90% Reinigungsmittel in fester Nadelform mit 1% bis 10% Wasser und mit anderen, gegebenenfalls gewunschten Ingredienzien zwecks Beschichtung der Nadeln sowie zur Pressung vorbestimmter Mengen von beschichteten Nadeln in einer unter Druck stehenden Form. 5. Methode nach Anspruch 4, dadurch gekennzeichnet, dal3 die Nadeln bei Zimmertemperatur und mit 40-60 psi (2,8 bis 4,2 kg/cm2) geprebt werden. 35 6. Shampoostange nach Anspruch 1, dadurch gekennzeichnet, dal3 sie 75% bis 80% Natriumlaurylsulfat in Nadelform geprebt mit 2% bis 5% Wasser als Bindemittel enthalt. 7. Shampoostange nach Anspruch 6, 40 dadurch gekennzeichnet, dal3 sie ein zusatzliches Bindemittel aus 1% bis 2% Glykol enthalt. 45 8. Shampoostange nach Anspruch 6, dadurch gekennzeichnet, dal3 sie weitere Ingredienzien enthalt: ein zusatzliches atherisches Ol, einen Duftstoff und einen Farbstoff. Revendicatlons Bindemittel, ein 50 55 1. Shampooing sous forme d'un pain solide comprenant 70 a 90% de detergent sous forme d'aiguilles solides et 1% a 10% d'eau. 2. Shampooing selon la revendication 1 dans lequel le detergent est du laurylsulfate de sodium. 3. Shampooing selon la revendication 2 comprenant un conditionneur, une huille essentielle, un parfum et un colorant. 4. Methode de fabrication d'un pain de shampooing solide comprenant les etapes de melange de 70% a 90% de detergent sous forme d'aiguilles avec 1 a 10% d'eau et avec d'autres ingredients qui peuvent etre necessaires de maniere a enrober les aiguilles, et de compactage de quantites predetermines 4

d'aiguilles enrobees dans un moule sous pression. 5 io 5. Methode selon la revendication 4 dans laquelle les aiguilles sont compactees a temperature ambiante et a 40-60 p.s.i. (2,8 a 4, 2 kg/cm2). 6. Pain de shampooing selon la revendication 1 comprenant 75% a 80% de laurylsulfate de sodium sous forme d'aiguilles comprimees avec 2 a 5% d'eau comme liant. 7. Pain de shampooing selon la revendication 6, incluant un liant supplemental comprenant 1 a 2% de glycol. 8. Pain de shampooing selon la revendication 6, comprenant des ingredients supplementaires qui peuvent etre : un liant additionnel, une huile essentielle, un parfum et un colorant. 15 20 25 30 35 40 45 50 5

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