(19)
(11)EP 2 392 311 B1

(12)EUROPEAN PATENT SPECIFICATION

(45)Mention of the grant of the patent:
01.11.2017 Bulletin 2017/44

(21)Application number: 10180572.9

(22)Date of filing:  28.09.2010
(51)International Patent Classification (IPC): 
A61Q 1/02(2006.01)
A61Q 1/10(2006.01)
A61K 8/73(2006.01)
A45D 40/16(2006.01)
A61Q 1/08(2006.01)
A61Q 1/12(2006.01)
A61K 8/02(2006.01)

(54)

Process for obtaining a solid, compact powder cosmetic product.

Verfahren zur Herstellung eines festen kosmetischen Kompaktpuderproduktes.

Procédé pour obtention d'un produit cosmétique solide en poudre compacté.


(84)Designated Contracting States:
AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO SE SI SK SM TR

(30)Priority: 01.06.2010 IT MI20100993

(43)Date of publication of application:
07.12.2011 Bulletin 2011/49

(73)Proprietor: Intercos S.p.A.
20123 Milano (IT)

(72)Inventors:
  • Caprarotta, Grazia Anna
    24049, VERDELLO (BG) (IT)
  • Guanziroli, M Marina
    26010, CHIEVE (CR) (IT)

(74)Representative: Mittler, Enrico et al
Mittler & C. S.r.l. Viale Lombardia, 20
20131 Milano
20131 Milano (IT)


(56)References cited: : 
EP-A1- 1 226 811
JP-A- 9 175 939
JP-A- 2007 186 471
US-A1- 2009 304 609
WO-A1-02/17875
JP-A- 62 209 011
US-A- 4 291 025
  
  • DATABASE GNPD [Online] Mintel; 1 March 2009 (2009-03-01), NN: "Mineral Air Pact Powder", XP002617375, Database accession no. 1066658
  • DATABASE GNPD [Online] Mintel; 1 December 2008 (2008-12-01), NN: "D-Blush Blush Trios", XP002617376, Database accession no. 1012525
  • DAWYDOFF W ET AL: "Thermoreversible Gele auf Polysaccharidbasis", NAHRUNG - FOOD, VCH VERLAGSGESELLSCHAFT, WEINHEIM, XX, vol. 28, no. 3, 1 January 1984 (1984-01-01), pages 241-260, XP007916772, ISSN: 0027-769X
  
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).


Description


[0001] The present invention relates to a process for obtaining a solid, compact powder cosmetic product.

[0002] In EP-B-0803245 a solid, compact cosmetic gel containing water, thennoreversible polysaccharides, humectants and a powder phase is described and claimed.

[0003] JP 2007 186471 disclose a water-containing phytoplankton (microalgae) hydrated with alcohols such as 1,3-butylene glycol or, a mixture of acetone and water to obtain an agent capable of activating the production of type I collagen in the extracellular matrix.

[0004] Database GNPD "Mineral Air Pact Powder" of 1 March 2009 and database GNPD "D-Blush Blush Trios" of 1 December 2008 disclose substantially anhydrous cosmetic products.

[0005] US 2009/0304609 discloses make-up products which may contain a thermoreversible polysaccharide (xantan gum), a humectant (butyleneglycol), an emollient (esters) and a powder phase (mica), made free of water by lyophilizing at a temperature of -10°C, preferably between - 20°C and -80°C.

[0006] This solid, compact cosmetic gel is a satisfactory cosmetic product but contains a high percentage of water, whereby it needs a sealed container or packaging to avoid volatile components from being lost.

[0007] Moreover, obtaining this solid cosmetic gel product with a relatively high volume is difficult, because it is prepared by heating and then poured into a special mould or container, in which cooling at room temperature causes a progressive shift in the gel internal bond (cross-linking) and the consequent solidification thereof without a clear solid-liquid transition.

[0008] The cosmetic product volume is thus determined from the mould or container volume, and in particular, when a product with a relief is required, this further limit the product volume.

[0009] It is the object of the present invention to provide a process for obtaining a new solid cosmetic product which may have high volumes and possibly various types of reliefs.

[0010] In accordance with the present invention, such an object is achieved by a process for obtaining a solid, compact powder cosmetic product as disclosed in claim 1.

[0011] By "substantially anhydrous" is meant that the water content in the final cosmetic product is 2% by weight or less.

[0012] The product contains one or more thermoreversible polysaccharides generally in an amount between 0.05 and 20% by weight of the final product, and preferably between 0.1 and 15% by weight of the final product.

[0013] Thermoreversible polysaccharides are carrageenan, agar, gellan gum, xanthan gum, biosaccharide Gum-1, alginic acid and alkaline metal or alkaline earth metal salts thereof. Further suitable examples may be found in the book "Biodegradable hydrogels for drug delivery", (1993), edited by K. Park et al., page 105, chapter 5.2, published by Technomic Publishing Co., Inc. Mixtures of various thermoreversible polysaccharides may also be used.

[0014] The product contains one or more humectants generally in an amount between 0.1 and 20% by weight of the final product, and preferably between 0.5 and 10% by weight of the final product.

[0015] Humectants are glycerine, sorbitol, mannitol, xilytol, glycols such as butylene glycol, pentylene glycol, hexylene glycol, dipropylene glycol, propylene glycol and polyethylene glycol. Others suitable examples may be found in C.T.F.A. Cosmetic Ingredient Handbook, First Edition, (1988). Mixtures of various humectants may also be used.

[0016] The product contains one or more emollients generally in an amount between 0.1 and 45% by weight of the final product, and preferably between 0.5 and 30% by weight of the final product.

[0017] Emollients are silicones, mineral oils, lanoline and derivatives thereof, vegetable oils, cetearyl alcohol esters, sorbitol esters, branch chain saturated hydrocarbons obtained by hydrogenation of the shark liver oil (squalane) or other natural oils, polyethylene glycol esters, potassium stearoyl, hydrolyzed rice proteins, esters with C12-20 fatty acids of polyethylene glycol (8EO), cetearyl ethylhexanoate, polysorbate 80.

[0018] Further examples of suitable humectants may be found in the aforementioned C.T.F.A. Cosmetic Ingredient Handbook, First Edition, (1988). Mixtures of various emollients may also be used.

[0019] The product contains a powder phase generally in an amount between 0.1 and 90% by weight of the final product, and preferably between 5 and 80% by weight of the final product. Typical examples of a suitable powder phase are various common powder excipients used in make-up cosmetic products such as mica, kaolin, talc, fluorphlogopite, nylon 12, starch, zinc oxide, calcium sodium aluminium silicate, acrylate (co)polymers, polyethylene (co)polymers, silica, spherical silica, spherical silicones, pigments such as iron oxides, chromium oxides and hydroxides, ultramarine blue, ultramarine pink, manganese violet, titania, mica and titania or bismuth oxychloride-based pearlescent materials, carmine, organic colorant-based lacquers and others synthetic powder colorants. Mixtures of the various powder excipients and colorants may also be used.

[0020] In addition to the essential ingredients of the above-mentioned product, it may optionally contain conventional cosmetic ingredients such as preservatives, surfactants, emulsifiers, sunscreens, perfumes and flavourings, waxes, soaps, proteins, anti-caking agents, etc.

[0021] The solid, compact powder cosmetic product may be used as a make-up product such as foundation, blush, eye shadow, mascara, concealer, and so on.

[0022] The present invention overcomes the limitations of the previous solid, compact gel cosmetic product to a high extent and allows to obtain a solid, compact powder cosmetic product with a soft creaminess texture having extraordinary colour expressions and high volumes.

[0023] The product is manufactured by means of a process as disclosed in claim 1 by heating the various mixed ingredients to form a pourable paste or liquid followed by pouring the paste or liquid into a suitable mould or container and eventually let it solidify into the mould or container.

[0024] The present invention provides a process for obtaining such a product in high volumes as disclosed in claim 1, thus particularly allowing the preparation thereof in particular shapes and patterns and geometries, with particular reliefs which are very difficult, if not impossible, to be obtained by means of conventional technologies.

[0025] The process according to the present invention substantially involves making an aqueous paste from the various ingredients of the product, which is then let solidify (jellify) into a suitable mould or container, and then the solidified or jellified paste is subjected to a heat treatment to remove the water from the paste itself.

[0026] The process according to the invention is exemplarily described with reference to the accompanying drawings, which show the various steps of the process.

[0027] First, a cosmetic product is prepared by a process as disclosed in claim 1, in a pasty form comprising thermoreversible polysaccharides, humectants, emollients, phase powders and containing also water or other solvents..

[0028] The solvent may entirely consist of water or proper mixtures of water and volatile or non-volatile organic solvents, such as for example aliphatic alcohols like ethanol, isopropanol, butanol, etc., in varying percentages.

[0029] The percentage of the above-indicated solvent or solvents in the paste may highly vary according to the viscosity degree required, and is preferably between 30% and 60%.

[0030] A container which has an internal cavity with a shape complementary to the one desired for the final cosmetic product is also arranged. A container example is shown in figure 1, where the container is indicated as a whole by reference numeral 1, its internal cavity is indicated by 2, and the shaped bottom of said cavity is indicated by 3.

[0031] A container made of metal, silicone or other plastic material, e.g. polyurethane resin, polycarbonate, methacrylate and many others, may be used.

[0032] The use of these materials is justified in that the plastics may be moulded both by injection into a mould and by polymerization in a bicomponent liquid form around a metal template, and in both cases, the shapes may be highly various and very well defined, with very marked, sharp reliefs even with very acute angles.

[0033] The cosmetic paste product is then heated at an average temperature of 90°C, or in any case between 70°C and 90°C, to make it so fluid to be pourable into the container.

[0034] The dosing step may be carried out by a volumetric piston doser, as shown in figure 2, where reference numeral 4 indicates the doser as a whole, 5 indicates a loading hopper, 6 indicates a stirrer, 7 indicates a piston doser, and 8 in the end indicates the fluid paste being dosed.

[0035] Alternatively, a common dosage system with a gear pump or other may also be employed.

[0036] Once the product has been heat-dosed into container 1, it is allowed to cool so as to conform to the inner shape of the mould. The cosmetic product cools down and jellifies very quickly until adopting a semisolid consistence.

[0037] The jellified cosmetic product, indicated by 8', may then be quickly drawn from the mould, if this is made of flexible materials, such as silicone, and then allowed to dry without the container, or allowed to dry directly within the mould itself, if this is made of rigid plastic materials, for example polycarbonate, polyurethane resin, etc.

[0038] The heat treatment is carried out at temperatures between 20°C and 90°C, preferably between 35°C and 80°C. This heat treatment may be carried out by any suitable heating method, such as for example in an air-recycle, humidity-controlled vented oven, a micro-wave oven or other. The heating should be performed over a sufficient period to make the product substantially anhydrous and this depends on the amount of water in the paste and on the temperature at which the heating is carried out.

[0039] In the case of humidity-controlled, forced ventilation ovens, the heating may last 12-24 hrs.

[0040] Once the cosmetic product has been dried, it should be stuck within the final container for sale, and for this purpose, the product may directly be placed within the final container or a shaped strap 9 may be placed on the liquid paste 8, immediately after the dosing step, in contact with the upper surface of the cosmetic product, as shown in figure 3.

[0041] Thereby, by adhering to the product during the jellifying and cooking steps, strap 9 will form a single body with the product itself.

[0042] The thickness of such a strap may range between 3 mm and more, and its shaping will correspond to that of the base of the intended shape.

[0043] Without distinctions, the material employed for strap 9 may be a natural product, such as baked clay, porcelain, chalk, paper or cellulose agglomerates, etc., but also compacted synthetic materials, e.g. plastics such as polycarbonate, polyethylene, Plexiglas, etc. or expanded materials, such as expanded polyurethane, expanded polyethylene, expanded phenolic resins, etc.

[0044] The strap may be employed as such or coated with a proper adhesive, to enhance the gripping abilities thereof.

[0045] As already mentioned, the drying operation may be carried out upon extraction of the jellified cosmetic product from container 1. In such a case, the product-strap assembly may also be overturned so that strap 9 serves the function as a support for the cosmetic product, as shown in figure 4.

[0046] Once the cosmetic product has been dried, in association with its corresponding strap, it is ready to be inserted and stuck into the final container intended to sale.

[0047] It is another advantage obtained by this technique to provide plug powder cosmetic products. In the known art, the final product consisting of different plugs of product is generally obtained through various steps: every single plug is pre-compacted into a single mould, then drawn from said mould and placed in the final cup where, once all the plugs have been placed, the final compacting step is carried out, and the final product is obtained. The limit of this technique is the large amount of steps to be carried out, the high cost for manufacturing several moulds, the shape limitations due to the metal cups, and the long manufacturing times.

[0048] By means of the new method according to the present invention plug powder cosmetic products may be obtained in only two steps, that is by simultaneously dosing the various products of the single plugs 11, 12, 13 into a single mould 14 (Fig. 5), and once the mould has been filled, the water or solvents may be drained off by means of a heat treatment, as mentioned above. The advantages of this new technique are the decrease in manufacturing costs and the possibility of obtaining whichever shapes and volumes.

[0049] Furthermore, the method according to the invention suppresses employing clothes as a gap between the cosmetic product and the mould, and thus also suppresses the weft and haze left by the clothes on the surface of the compacted cosmetic product.

[0050] Another important aspect is the consistency of the obtained product, i.e. very compact and soft, more impact-resistant than other powder products. This is just due to the presence of the compact solid gel formed from the dried paste, which confers a porous and aerated texture to the product.

[0051] The following is an example not exhaustive and not limiting of the composition of the product prepared according to the above-described process of the invention.

Example



[0052] 
Ingredients% WT/WT 
MICA 27.521  
TITANIA CI 7789 16.813  
ALUMINIUM CALCIUM SODIUM SILICATE 16.627  
IRON OXIDES CI 77491 9.099  
CETEARYL ETHYLHEXSANOATE 6.873  
IRON OXIDES CI 77499 5.010 A
C12-20 ACID PEGs-8 ESTER 4.205  
RAFFINOSE ISOSTEARATE 4.124  
HDI/TRIMETHYLOL HEXILLATONE XPOLYMER 3.276  
GLYCERINE 2.491  
FERRIC FERROCYANIDE CI 77510 0.795  
     
GLYCERINE 0.500 B
GELLAN GUM 0.180  
     
CAPRYLYL GLYCOL 0.500  
POTASSIUM CETYL PHOSPHATE 0.438  
POLISORBATE 20 0.404  
1,2-HEXANEDIOL 0.250  
TIN OXIDE 0.087 C
SILICA 0.067  
SYNTETIC FLUORPHLOGOPITE 0.040  
STEAROYL POTASSIUM    
HYDROLYZED RICE PROTEIN 0.200  
SQUALANE 0.500  
Total 100.000  


[0053] This product was prepared as follows.

[0054] The ingredients mentioned above as A were mixed to form a powder phase (a). The ingredients mentioned above as B were then mixed with water to form a phase (b). The ingredients mentioned above as C were then mixed to form a phase (c). Phase (b) was then put into a turbo-emulsifier and heated at 75° C, and phase (c) was then added under stirring and thus the mixture was homogenized. The resulting emulsion was lastly cooled down at 25 °C.

[0055] Phase (a) was then mixed with the emulsion, together with ethanol to obtain a paste. Water and calcium chloride as a catalyst were added to this paste to obtain a gel, and the resulting liquid paste was then poured into a mould, where it was then heated at 80°C and kept at this temperature for more than 6 hrs. Finally, a compact solid powder was obtained with a very creamy texture and high volume.


Claims

1. Process for making a solid compact powder cosmetic product, characterized by comprising the following steps:

a) preparing an aqueous paste by mixing as essential ingredients, one or more thermoreversible polysaccharides, one or more humectants, one or more emollients and a powder phase, wherein said thermoreversible polysaccharides is selected from a group consisting of carrageenan, agar, gellan gum, xanthan gum, biosaccharide Gum-1, alginic acid and alkaline metal or alkaline earth metal salts thereof, said humectant is selected from a group consisting of glycerine, sorbitol, mannitol, xylitol, butyleneglycol, pentyleneglycol, hexyleneglycol, dipropyleneglycol, propyleneglycol, polyethyleneglycol and mixtures thereof, said emollient is selected from a group consisting of silicones, mineral oils, lanoline and derivatives thereof, vegetable oils, cetearyl alcohol esters, sorbitol esters, branch chain saturated hydrocarbons obtained by hydrogenation of the shark liver oil (squalane) or other natural oils, polyethylene glycol esters, potassium stearoyl, hydrolyzed rice proteins, esters with C12-20 fatty acids of polyethylene glycol (8EO), cetearyl ethylhexanoate, polysorbate 80;

b) a first heating of the aqueous paste product at a temperature between 70°C and 90°C, to make it so fluid to be pourable into a container as a liquid paste (8);

c) dosing said liquid paste (8) after said first heating into a container (1) which has an internal cavity (2) with a shape complementary to the one desired for a final product cosmetic;

d) allowing to cool said liquid paste (8) so as to conform to the inner shape of the mould;

e) a second heating of the jellified cosmetic product into said internal cavity (2), at a temperature between 20°C and 90°C, obtaining a final cosmetic product having a content of water of 2% by weight or less;

f) placing the final cosmetic product, after said second heating, into a final container for sale.


 
2. Process according to claim 1, characterized by placing a shaped strap (9) on the liquid paste (8) after the dosing step (c).
 
3. Process according to claim 1, characterized in that said second heating is provided at a temperature between 35°C and 80°C.
 


Ansprüche

1. Verfahren zur Herstellung eines festen kompakten Pulverkosmetikprodukts, dadurch gekennzeichnet, dass es die folgenden Schritte umfasst:

a) Herstellen einer wässrigen Paste durch Mischen, als wesentliche Bestandteile ein oder mehrerer thermoreversibler Polysaccharide, ein oder mehrerer Feuchthaltemittel, ein oder mehrerer Weichmacher und einer Pulverphase, wobei die thermoreversiblen Polysaccharide ausgewählt sind aus einer Gruppe bestehend aus Carrageenan, Agar, Gellangummi, Xanthangummi, Biosaccharid Gum-1, Alginsäure und Alkalimetall- oder Erdalkalimetallsalzen davon, wobei das Feuchthaltemittel aus einer Gruppe ausgewählt ist, die aus Glycerin, Sorbitol, Mannol, Xylitol, Butylenglykol, Pentylenglykol, Hexylenglykol, Dipropylenglykol, Propylenglykol, Polyethylenglykol und Mischungen davon besteht, wobei der Weichmacher aus einer Gruppe ausgewählt ist, die aus Silikonen, Mineralölen, Lanolin und Derivaten davon, pflanzlichen Ölen, Cetearylalkoholestern, Sorbitolestern, gesättigten Kohlenwasserstoffen mit verzweigten Ketten die durch Hydrierung des Haifischleberöls (Squalan) oder anderer natürlicher Öle erhalten wurden, Polyethylenglykolester, Kaliumstearoyl, hydrolysierte Reisproteine, Polyethylenglykol (8EO) Ester mit C12-20 -Fettsäuren, Cetearylethylhexanoat, Polysorbat 80 besteht;

b) ein erstes Erwärmen des wässrigen Pastenprodukts bei einer Temperatur zwischen 70 °C und 90 °C, um es so flüssig zu machen, dass es in einen Behälter als flüssige Paste (8) gießbar ist;

c) Dosieren der flüssigen Paste (8) nach dem ersten Erwärmen in einen Behälter (1), der einen inneren Hohlraum (2) mit einer Form aufweist, die komplementär zu der für ein kosmetisches Endprodukt gewünschten ist;

d) Kühlen lassen der flüssigen Paste (8) so dass sie sich an die Form der Gießform anpasst;

e) ein zweites Erwärmen des gelierten kosmetischen Produkts in den inneren Hohlraum (2) bei einer Temperatur zwischen 20 °C und 90 °C, wobei ein kosmetisches Endprodukt mit einem Gehalt an Wasser von 2 Gew.-% oder weniger erhalten wird;

f) Platzieren des kosmetischen Endprodukts nach dem zweiten Erwärmen in einen endgültigen Behälter zum Verkauf.


 
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass nach dem Dosierschritt (c) ein geformter Riemen (9) auf die flüssige Paste (8) aufgebracht wird.
 
3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass das zweite Erwärmen bei einer Temperatur zwischen 35 °C und 80 °C vorgesehen ist.
 


Revendications

1. Procédé de fabrication d'un produit cosmétique en poudre compact solide, caractérisé en ce qu'il comprend les étapes suivantes :

a) la préparation d'une pâte aqueuse par mélange, en tant que composants essentiels, d'un ou plusieurs polysaccharides thermoréversibles, un ou plusieurs humectants, un ou plusieurs émollients et une phase de poudre, lesdits polysaccharides thermoréversibles étant choisis dans un groupe constitué de la carraghénine, la gélose, la gomme gellane, la gomme xanthane, le biosaccharide Gum-1, l'acide alginique et des sels de métal alcalin ou de métal alcalino-terreux de celui-ci, ledit humectant étant choisi dans un groupe constitué de la glycérine, le sorbitol, le mannitol, le xylitol, le butylèneglycol, le pentylèneglycol, l'hexylèneglycol, le dipropylèneglycol, le propylèneglycol, le polyéthylèneglycol et des mélanges de ceux-ci, ledit émollient étant choisi dans un groupe constitué de silicones, d'huiles minérales, de la lanoline et des dérivés de celle-ci, d'huiles végétales, d'esters d'alcool cétéarylique, d'esters de sorbitol, d'hydrocarbures saturés à chaîne ramifiée obtenus par hydrogénation de l'huile de foie de requin (squalane) ou d'autres huiles naturelles, d'esters de polyéthylène glycol, du stéaroyle de potassium, de protéines de riz hydrolysées, d'esters avec des acides gras en Cl2-20 de polyéthylène glycol (8EO), d'éthylhexanoate de cétéaryle, de polysorbate 80 ;

b) un premier chauffage du produit de pâte aqueuse à une température comprise entre 70 °C et 90 °C, de façon à le rendre suffisamment fluide pour être versé dans un récipient sous la forme d'une pâte liquide (8) ;

c) le dosage de ladite pâte liquide (8) après ledit premier chauffage dans un récipient (1) qui comporte une cavité interne (2) ayant une forme complémentaire de celle souhaitée pour un produit cosmétique final ;

d) le refroidissement de ladite pâte liquide (8) de façon à se conformer à la forme interne du moule ;

e) un deuxième chauffage du produit cosmétique gélifié dans ladite cavité interne (2), à une température comprise entre 20 °C et 90 °C, de façon à obtenir un produit final ayant une teneur en eau de 2 % en poids ou moins ;

f) le placement du produit cosmétique final, après ledit deuxième chauffage, dans un récipient final pour la vente.


 
2. Procédé selon la revendication 1, caractérisé par le placement d'une sangle formée (9) sur la pâte liquide (8) après l'étape de dosage (c).
 
3. Procédé selon la revendication 1, caractérisé en ce que ledit deuxième chauffage est conduit à une température comprise entre 35 °C et 80 °C.
 




Drawing








Cited references

REFERENCES CITED IN THE DESCRIPTION



This list of references cited by the applicant is for the reader's convenience only. It does not form part of the European patent document. Even though great care has been taken in compiling the references, errors or omissions cannot be excluded and the EPO disclaims all liability in this regard.

Patent documents cited in the description




Non-patent literature cited in the description