Drug – bio-affecting and body treating compositions – Preparations characterized by special physical form – Cosmetic – antiperspirant – dentifrice
Reexamination Certificate
1998-08-25
2001-05-01
Page, Thurman K. (Department: 1615)
Drug, bio-affecting and body treating compositions
Preparations characterized by special physical form
Cosmetic, antiperspirant, dentifrice
C423S611000, C423S610000, C424S400000, C424S401000, C424S059000, C424S061000, C424S063000, C424S064000, C424S070100, C424S450000, C424S489000
Reexamination Certificate
active
06224884
ABSTRACT:
Applicant references herein the patent application of CHRISTOPHE REMY for USE OF AN IONIC CONDUCTOR IN ORDER TO IMPROVE PHOTOCHROMISM, AND COMPOSITION COMPRISING IT (09/139,280) filed on even date herewith and incorporates the disclosure thereof specifically by reference herein.
The present invention relates to the improvement of the photochromic properties of a titanium oxide, by virtue of a novel synthesis process; the invention also relates to the novel compound which is obtained, and to its application in the field of cosmetic compositions in particular.
Cosmetic compositions, in particular make-up compositions such as free or compact powders, foundations, blushers or eye-shadows, lipsticks or nail varnishes, include a suitable vehicle and various colorants intended to impart some degree of colour to the said compositions before and/or after they are applied to the skin, the mucous membranes, the mucocutaneous tissues and/or parts of the exoskeleton, for example the nails or the hair.
A fairly limited range of colorants is presently used to create colours, in particular lakes, inorganic pigments or pearlescent pigments. Lakes allow vivid colours to be obtained, but are for the most part unstable with respect to light, temperature or pH. Some of them also have the drawback of staining the skin unattractively after they have been applied, as a result of the colorant being leached. Conversely, inorganic pigments, in particular inorganic oxides, are highly stable but give somewhat dull and pale colours. In order to obtain coloured effects, use may also be made of pearlescent pigments whose colours are varied, albeit never intense, which make it possible to obtain iridescent but most often fairly weak effects.
It has therefore been proposed to use photochromic compounds in make-up or haircare compositions, so as to obtain attractive and varied changes in the colour effect of make-up for the skin and/or the hair.
Photochromic compounds are compounds which have the property of changing colour when they are exposed to a light source, then of returning to their initial colour, or a similar colour, when they are no longer being exposed. In particular, compounds of this type have a particularly advantageous application in cosmetic compositions, in particular in make-up compositions such as foundations and blushers or eye-shadows. Indeed, it has been found that the make-up effect of skin which has been made up differs depending on whether the illumination is natural or artificial. Thus, make-up applied under artificial illumination will appear lighter under natural light. Conversely, make-up applied out of doors will appear darker in a place where the illumination is artificial.
The photochromic properties of a compound can be characterized using trichromatic coordinates (L, a and b) in the way described before the examples. These coordinates make it possible, in particular, to determine a parameter &Dgr;E which will be used in the present application to characterize the photochromism of the compounds according to the invention and outside the scope of the invention.
In general, the higher the parameter &Dgr;E is, the more the compound is photochromic.
The prior art has, in particular, proposed the use in cosmetics of organic photochromic compounds, for example compounds of the spiropyran or naphthoxazine families.
These photochromic compounds are particularly advantageous since they enable the support to which they are applied to change colour rapidly when the said support is exposed to UV, for example, with a rapid return to the initial colour when it is no longer being exposed to UV.
Mention may thus be made of French Patent FR1604929, which describes cosmetic compositions, in particular for the hair, in aerosol form which contain phototropic compounds such as nitrobenzylpyridines, thiosemicarbazones or spiropyran derivatives. After these compositions have been sprayed onto the hair and exposed to sunlight, a blue-violet coloration is obtained which returns to pale yellow in darkness.
Cosmetic compositions comprising particular inorganic photochromic compounds, selected from metal oxides, their hydrated forms and their complexes, have also been proposed, for example by European Patent EP359909. In particular, this document mentions the use of titanium oxide, treated so as to make it photochromic, in make-up compositions such as powders and foundations.
Furthermore, document U.S. Pat. No. 5,176,905 discloses a process for obtaining a photochromic titanium oxide by mixing iron hydroxide (FeOOH) and titanium dioxide, and calcining at 750-850° C.
In addition, document EP624553 discloses a process for the preparation of titanium oxide having improved photochromism, involving dissolving an organotitanium and an organic compound comprising at least one metal, in an organic solvent, then in hydrolyzing the mixture, recovering the hydrolysate and calcining it at a temperature of 550-700° C. This gives a photochromic titanium oxide having a colour difference which can be quantified using the parameter &Dgr;E whose value is at least equal to 10. The value &Dgr;E is the measured difference between the chromaticity before exposure and the chromaticity after exposure for 1 hour, under UV at 2 mW/cm
2
.
Also, document JP05/017152 discloses a process for the preparation of a photochromic titanium oxide, including mixing organotitaniums with at least one metal selected from iron, chromium, copper, nickel, vanadium or manganese, then in sintering the said mixture in the presence of sodium compounds. It is in this way possible to obtain a parameter &Dgr;E which is improved in comparison with the prior art, and in particular greater than 10. The parameter &Dgr;E is calculated in the same way as in EP624553.
Also, the article by Fitzpatrick et al., published in the journal “Clays and Clay Minerals” Volume 26, No. 3, pp. 189-201 (1978) discloses a process for the preparation of titanium and iron oxide coprecipitates by hydrolysis; the powder which is obtained can, in particular, be calcined, but only up to a temperature of 250° C.
However, it has been observed that the compounds obtained in this way do not have the desired photochromic properties.
There is still the need to provide photochromic compounds which make it possible to obtain strong photochromism, and in particular make it possible to obtain an appreciable change in the colour of the make-up, that is to say a relatively high &Dgr;E, in particular greater than or equal to 12.
An object of the present invention is to provide a particular process for the preparation of compounds of this type.
The present invention therefore relates to a process for the preparation of a photochromic titanium oxide, in which:
a mixture is prepared comprising titanium chloride and a precursor of a metal selected from iron, chromium, copper, nickel, manganese, cobalt and molybdenum,
the mixture is hydrolysed, then
the mixture obtained is heat-treated at a temperature of at least 300° C. so as to obtain a compound having a parameter &Dgr;E greater than or equal to 12.
The invention also relates to the photochromic compound of the titanium oxide type which can be obtained by the above process, as well as to a composition, in particular a cosmetic composition, comprising the compound.
The process according to the invention therefore involves heat-treating a mixture comprising a titanium chloride and at least one precursor of a metal.
The titanium chloride may, in particular, be TiCl
4
.
The term “precursor of a metal” is intended to mean any compound comprising the said metal and capable of releasing it.
Use may, in particular, be made of a hydrate, an oxide and a salt, such as a sulphate or a chloride, of the said metal. The metal is preferably selected from iron, chromium, copper, nickel, manganese, cobalt and molybdenum, alone or as a mixture.
Use is preferably made of an iron chloride or sulphate.
Preferably, use is made of a metal precursor in liquid form or in pulverulent form.
Generally, the amounts of the compounds are selected so as to obtain a “metal oxide e
Finnegan Henderson Farabow Garrett & Dunner L.L.P.
L'Oreal (S.A.)
McQueeney P. E.
Page Thurman K.
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