WO2008066243A1 - Mica composite powder coated with trimethylsiloxysilicate and the long lash mascara composition containing the same - Google Patents

Mica composite powder coated with trimethylsiloxysilicate and the long lash mascara composition containing the same Download PDF

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Publication number
WO2008066243A1
WO2008066243A1 PCT/KR2007/004657 KR2007004657W WO2008066243A1 WO 2008066243 A1 WO2008066243 A1 WO 2008066243A1 KR 2007004657 W KR2007004657 W KR 2007004657W WO 2008066243 A1 WO2008066243 A1 WO 2008066243A1
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WIPO (PCT)
Prior art keywords
mica
composite powder
resin
trimethylsiloxysilicate
coating
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PCT/KR2007/004657
Other languages
French (fr)
Inventor
Se Jun Park
Sun Sang Kwon
Young Hea Roh
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Amorepacific Corporation
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Publication of WO2008066243A1 publication Critical patent/WO2008066243A1/en

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11Encapsulated compositions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26Aluminium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • A61Q1/10Preparations containing skin colorants, e.g. pigments for eyes, e.g. eyeliner, mascara
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns

Definitions

  • the present invention relates to a mica composite powder and a long lash mascara composition containing the same, more particularly, the present invention relates to a mica composite powder that is prepared by coating the surface of mica particles with MQ resin, which is a film forming agent, with a heat treatment of 300 to 350 "C for increasing water repellency, thus obtaining a long lash effect through smooth application, improved adhesion of the mica powder and durability of formulation when the mica composite powder is applied in the formulation, and a long lash mascara composition containing the same.
  • MQ resin which is a film forming agent
  • Prior powders that are frequently used in cosmetics have inherent characteristics. To improve the shortcomings of such powders, techniques of modifying the surface in accordance with characteristics required in cosmetics are frequently used. Among these techniques, a coating technique is frequently used to convert the surface character of powders from a hydrophilic property into a hydrophobic property or from a hydrophobic property into a hydrophilic property. Powders that are inorganic pigments which are used in cosmetics can be classified as follows.
  • Inorganic pigments in cosmetics can be broadly divided, according to the function, into coloring pigments, white pigments, extender pigments and functional pigments.
  • the coloring pigments serve to adjust the color tone of products, and examples thereof include bengala, iron oxide yellow, iron oxide black, chromium oxide, and carbon black.
  • the white pigments can adjust coverage in addition to color tone, and examples thereof include titanium dioxide and zinc oxide.
  • the extender pigments are diluents that are used to adjust color tone and, at the same time, to adjust the feeling of use (extensibility or adhesion) or gloss of products. Also, the extender pigments are used to maintain the formulation of products.
  • the extender pigments among the inorganic pigments used in cosmetics are talc, kaolin and mica having the following characteristics.
  • Talc used in mascara formulations is magnesium silicate hydrate (Mg 3 Si 4 Oi 0 (OH) 2 ) and is generally composed of a compact of fine crystals or an aggregate of foliar crude crystals. Also, the talc feels very soft, and the talc particles have a thin plate shape and are frequently used in cosmetics to improve extensibility or smoothness .
  • Kaolin also known as "china clay” has its name derived from the name of the Chinese town Kao-Ling, where high-purity white clay used as the raw material of porcelain was produced.
  • Kaolin has a composition of aluminum silicate hydroxide (Al 2 Si 2 O 5 (OH) 4 ) and shows a regular hexagonal plate shape at high crystallinity, but has a fine irregular plate shape at low crystallinity. Furthermore, it has an excellent adhesion to the skin, because a low thickness of the plate shaped particles. Also, it is frequently used in cosmetics, because it has excellent oil absorption and water absorption properties.
  • Mica is typically exemplified by muscovite belonging to potassium mica and is represented by a chemical formula of KAl 2 (AlSi 3 )Oi 0 (OH) 2 .
  • the mica consists of light yellow or green hexagonal plate-shaped crystals belonging to the monoclinic system.
  • Mica may also be exemplified as silk mica (sericite) " because it consists of aggregates of fine crystals similarly to muscovite and because it appears as a silky gloss on the surface of buildings.
  • the extender pigments are easy to apply in a mascara formulation due to a soft feeling of use, application and the like, and are used through various coating techniques depending on the purpose.
  • the talc is applied to realize a soft application because it has the lowest refractive index of the extender pigments and soft property, and the talc coated with alkylsilane is applied to solve the problem of flake-off by improving adhesion.
  • the talc is coated with a silicone compound to prevent smudging of mascara, however the silicone has a poor adhesion.
  • the mica has a thin layer shape and has the highest aspect ratio of the extender pigments. Smoothness of the mica is less than that of the talc, but the mica exhibits an excellent adhesion caused by its wide plate form, and has better gloss and a low refractive index, similar to that of the talc, therefore it is used in many applications.
  • the mica has problems of smudging and poor durability due to a shortage of low oil absorption.
  • surface treatments such as coating have been developed. Silicone coating among the coating methods imparts water repellency and oil repellency to provide smooth touch, but a problem of spreadability caused by a property of formulation becomes prevalent, and the silicone further exhibits a poor adhesion. In the case of alkylsilane coating, the spreadability is relatively- improved in the formulation, but a poor durability still remains .
  • the coating methods of extender pigments have been studied for various purposes .
  • the usual coating methods are conducted by a dry, wet or CVD coating, which are well known in the art.
  • Various studies about the coating methods are proceeding to obtain coating materials and methods providing a desirable property and uniform coating.
  • the mica is usually coated with alkylsilane, dimethicone, methicone and amino acid, which are well known as coating materials.
  • heat treatment temperature is generally between 120 and 180 ° C, and certainly less than 200 ° C. If the temperature exceeds 200 ° C, the inherent property of the coating material is disappears, and water-resistance and oil-resistance significantly decrease, in addition to a feeling of use becoming poor .
  • the inventors of the present invention have studied to develop a new cosmetic that improves the durability and spreadability while maintaining adhesion caused by a high aspect ratio of the mica.
  • the present inventors have developed a mascara composition having a long lash effect caused by improved smooth application, adhesion of mica powder and durability of formulation through spraying MQ resin, which is a film forming agent, as a coating material with a heat treatment of 300 to 350 ° C in a vacuum according to a common dry coating process to disperse uniformly and make a coating layer that is formed by covalent bonds between the coating material and the mica, and between the individual MQ resin molecules.
  • the present invention forms a net structure between the MQ resin coating material and the mica through heating at a temperature of more than 300 ° C, higher than a heat treatment temperature applied in a common coating process, whereby it is confirmed that water resistance, which is an effect caused by the coating, is significantly improved, and a smooth surface property and adhesion property of the solid plate shaped mica are increased.
  • the object of the present invention is to provide a mica composite powder that is prepared by coating the surface of mica particles with MQ resin, which is a film forming agent, with a heat treatment of 300 to 350 ° C for increasing water repellency, thus obtaining a long lash effect through smooth application, improved adhesion of the mica powder and durability of formulation when the mica composite powder is applied in the formulation, and a long lash mascara composition containing the same.
  • MQ resin which is a film forming agent
  • the present invention provides a mica composite powder that is prepared by coating the surface of mica particles with MQ resin and heat treating at 300 to 350 ° C, thus obtaining smooth application, improved effects of adhesion of mica powder and durability of formulation when the mica composite powder is applied in the formulation, and a long lash mascara composition containing the same .
  • a long lash mascara composition containing a mica composite powder coated with MQ resin, which is a film forming agent can be prepared to have an improved effect of makeup durability without flake- off.
  • the composition improves water repellency due to the coating layer, increases makeup durability through an enhanced adhesion, and exhibits a long lash effect influenced by a high aspect ratio of the mica powder.
  • the present invention can improve water- resistance, smooth surface and adhesion property of the solid plate shaped mica through a temperature of more than 300 "C in the coating process.
  • the present invention relates to a mica powder that is prepared by coating the mica surface with MQ resin, preferably trimethylsiloxysilicate, with a heat treatment of 300 ⁇ 350 ° C, and to a long lash mascara composition containing the same .
  • MQ resin preferably trimethylsiloxysilicate
  • a mica used in the present invention has preferably a mean particle size of 3 p to 40 ⁇ and an aspect ratio of 90 to 120.
  • the present invention uses Mica FA450 (Yamaguchi Mica Company, Japan) , but is not limited thereto.
  • the mica used in the present invention has an aspect ratio of 100 to 109 and a mean particle size of 22 ⁇ m, and exhibits an excellent adhesion and spreading property because it has a relatively high aspect ratio.
  • the term "long lash effect" as used herein means an effect making eyelashes artificially longer than an inherent length of the eyelashes and looking longer in a mascara formulation.
  • Mica having an aspect ratio of about 70 is commonly used nowadays, because if the aspect ratio of the mica exceeds 70, its adhesion is low so that flake- off will occur.
  • the present invention treats the mica having an aspect ratio of more than 70 with trimethylsiloxysilicate through coating at high temperature to improve an adhesion and water-resistance property.
  • a resin is an M-form if it has one methyl group attached to a central silicon (Si) , a D-form if it has two methyl groups attached to a central silicon, a T- form if it has three methyl groups attached to a central silicon, and a Q- form if it has four methyl groups attached to a central silicon.
  • the MQ resin as used herein is M-form resin attached to Q-form resin.
  • the MQ resin used in the present invention is a silicone based resin
  • a silicone based resin may show four resin forms: M-resin has one Si-O bond, D-resin has two Si- O bonds, T-resin has three Si-O bonds, and Q-resin has four Si-O bonds.
  • the MQ resin used in the present invention is a resin bonded M-resin and Q-resin according to an MQ ratio, which is the ratio between M-resin and Q-resin.
  • MQ ratio which is the ratio between M-resin and Q-resin.
  • Various materials attached to Si of the M-resin exist, but the MQ resin commonly used is generally organo polysiloxane bonded with Si-CH 3 .
  • the compound represented by the following Chemical Formula 1 is trimethylsiloxysilicate, which is a kind of MQ resin that imparts water repellency as a film forming agent .
  • An MQ resin used in the present invention usually has an MQ ratio of between 0.7 and 1.3.
  • the MQ resin may include, for example, a trimethylsiloxysilicate/cyclotetrasiloxane, a trimethylsiloxysilicate/cyclopentasiloxane, a trimethylsiloxysilicate/dimethicone and a trimethylsiloxysilicate/isododecane, most preferably a trimethylsiloxysilicate/isododecane having an MQ ratio of between 1.0 and 1.1.
  • a process and method for coating the mica with MQ resin are similar to a common dry coating process. More specifically, mica is first dried in a dryer at 105 ° C for more than 4 hours. The dried mica is then introduced into a Henschel Mixer, and a vacuum is created inside the Henschel Mixer. The MQ resin is then dispersed by spraying in an amount of 1.0 to 5.0% by weight, more preferably 2.0 to 4.0% by weight. If the MQ resin content is less than 1.0% by weight, it is difficult to obtain an improvement of durability caused by coating, and if the MQ resin content exceeds 5.0% by weight, flake-off and a hard feeling of use occurs when applied in a mascara formulation.
  • the MQ resin is further dispersed by mixing for 15 to 600seconds, preferably 30 to 300seconds, and then the resultant is heat treated for more than lhour at 300 to 350 ° C, preferably 300 to 310 ° C.
  • the spraying time of the present invention is longer than that of a common coating process due to a difficultly of obtaining a uniform dispersion of the MQ resin through a common process because the MQ resin has a high viscosity as compared to those of common coating materials. If the spraying time is less than 30seconds, the prepared mica composite powder loses a soft property due to an uneven surface, and does not uniformly exhibit water resistance. Therefore, the dispersion time of the present invention is longer than that of a common coating process in order that the coating material can be dispersed uniformly, thus the present invention can obtain a uniform surface property and water resistance.
  • the heat treatment temperature of the present invention is greater than that of a common coating process in order to prevent a decrease of eyelash adhesion due to heat treating the mica having an aspect ratio of more than 70 at less than 300 ° C, thereby resulting in a poor long lash effect and flake-off property and reduced water resistance.
  • the heat treatment temperature is greater than 300 ° C, a very small amount of impurities included in the mica are removed to obtain an excellent gloss and uniform coating layer, thus an uneven surface property of the mica is modified to exhibit a soft surface property that is not shown in a heat treatment temperature of a common coating process. This effect is a result of the coating materials forming a net structure uniformly on the mica surface.
  • the mica composite powder of the present invention maintains an adhesion and smooth application due to a high aspect ratio of the mica and improves a durability and spreadability by a coating layer of MQ resin coated on the mica surface to stabilize the formulation, thereby the mica composite powder can be formulated in a cosmetic composition, such as mascara or eye liner, according to a conventional method.
  • a cosmetic composition such as mascara or eye liner
  • the mica composite powder of the present invention is contained in an amount of 0.1 to 4.0% by weight based on the total weight of the cosmetic composition.
  • Example 1 Preparation of a powder with trimethylsiloxysilicate/isododecane coated on mica FA 450 lOOg of mica FA 450 having an aspect ratio of 100 to 109 were dried at 105 ° C for more than 4hours, then the dried mica was introduced into a Henschel mixer and a vacuum was produced. 5g of trimethylsiloxysilicate/isododecane were sprayed on the mica and mixed, then heat treated at 310 ° C for ⁇ hours . After heat treating, 103g of the mica coated with trimethylsiloxysilicate were obtained.
  • Comparative Example 1 Preparation of a powder with trimethylsiloxysilicate/isododecane coated on mica A 325 lOOg of mica A 325 having an aspect ratio of 70 to 80 were dried at 105 ° C for more than 4hours, then the dried mica was introduced into a Henschel mixer, and a vacuum was produced. 5g of trimethylsiloxysilicate/isododecane were sprayed on the mica and mixed, then heat treated at 310 ° C for ⁇ hours . After heat treating, 103g of the mica coated with trimethylsiloxysilicate were obtained.
  • Comparative Example 2 Preparation of a powder with trimethylsiloxysilicate/isododecane coated on mica NCF 322 lOOg of mica NCF 322 having an aspect ratio of 121 to 127 were dried at 105 ° C for more than 4hours, then the dried mica was introduced into a Henschel mixer, and a vacuum was produced. 5g of trimethylsiloxysilicate/isododecane were sprayed on the mica and mixed, then heat treated at 310 ° C for ⁇ hours.
  • Comparative Example 3 Preparation of a powder with trimethylsiloxysilicate/isododecane coated on mica FA 450 lOOg of mica FA 450 having an aspect ratio of 100 to
  • Formulation Example 1 and Comparative Formulation Examples 1 and 4 were applied on artificial eyelashes according to a conventional makeup method, and then dried for lOmins. After drying, artificial tears were dropped to induce wetting for lOmins. A filter paper was applied to cover the eyelashes and pushed using a roller. The durability of the formulation was evaluated through the area adhered to the filter paper and the results thus obtained are given in Table 2 below. [Table 2] ⁇ : completely absent O: almost absent ⁇ : slightly exists X: exists
  • the mascara formulation of Formulation Example 1 containing the mica composite powder according to the present invention exhibits a perfect durability without smudging, whereas Comparative Formulation Example 1 containing the uncoated mica is slightly adhered to the filter paper. Also, it is confirmed that the water resistance of Comparative Formulation Example 4, which has a low coating temperature, is less than that of Formulation Example 1, but is greater than that of Comparative Formulation Example 1, as only a little smudging is induced.
  • the mascara formulation of Formulation Example 1 containing the mica composite powder of Example 1 according to the present invention exhibits an excellent long lash effect because the adhesion of Formulation Example 1 is greater than that of Comparative Formulation Example 1.
  • the flake-off of Formulation Example 1 and Comparative Formulation Examples 2-4 is reduced as compared to Comparative Formulation Example 1 containing the uncoated mica, because the adhesion of the mica is improved by Si-CH 3 of the MQ resin as a coating material. Therefore, the adhesion of the mica can be improved by the coating to reduce flake-off.
  • Comparative Formulation Example 4 which has a relatively low coating temperature, is less than that of Formulation Example 1 because a polymerization time is insufficient to retain an adhesive property of the resin and decreases a smooth property.
  • Comparative Formulation Example 3 having an aspect ratio of 120 to 127 has a shortage of resistance to flake- off due to the high aspect ratio, and Comparative Formulation Example 2 having an aspect ratio of 70 to 80 does not exhibit a long lash effect due to the low aspect ratio. Therefore, the present invention can provide a long lash mascara composition having a long lash effect without flake-off through preparing a mica composite powder by coating the surface of mica particles with MQ resin, which is a film forming agent, with a heat treatment of 300 to 350 ° C for increasing water repellency, thus increasing durability of makeup and obtaining improved durability of formulation and adhesion of the mica powder when the mica composite powder is applied in the formulation.
  • MQ resin which is a film forming agent

Abstract

The present invention relates to a mica composite powder and a long lash mascara composition containing the same, more particularly, the present invention relates to a mica composite powder that is prepared by coating the surface of mica particles with MQ resin, which is a film forming agent, with a heat treatment of 300 to 350 °C for increasing water repellency, thus obtaining a long lash effect through smooth application, improved adhesion of the mica powder and durability of formulation when the mica composite powder is applied in the formulation, and a long lash mascara composition containing the same.

Description

[DESCRIPTION]
[invention Title]
MICA COMPOSITE POWDER COATED WITH TRIMETHYLSILOXYSILICATE AND THE LONG LASH MASCARA COMPOSITION CONTAINING THE SAME [Technical Field]
The present invention relates to a mica composite powder and a long lash mascara composition containing the same, more particularly, the present invention relates to a mica composite powder that is prepared by coating the surface of mica particles with MQ resin, which is a film forming agent, with a heat treatment of 300 to 350 "C for increasing water repellency, thus obtaining a long lash effect through smooth application, improved adhesion of the mica powder and durability of formulation when the mica composite powder is applied in the formulation, and a long lash mascara composition containing the same. [Background Art]
Prior powders that are frequently used in cosmetics have inherent characteristics. To improve the shortcomings of such powders, techniques of modifying the surface in accordance with characteristics required in cosmetics are frequently used. Among these techniques, a coating technique is frequently used to convert the surface character of powders from a hydrophilic property into a hydrophobic property or from a hydrophobic property into a hydrophilic property. Powders that are inorganic pigments which are used in cosmetics can be classified as follows.
Inorganic pigments in cosmetics can be broadly divided, according to the function, into coloring pigments, white pigments, extender pigments and functional pigments. The coloring pigments serve to adjust the color tone of products, and examples thereof include bengala, iron oxide yellow, iron oxide black, chromium oxide, and carbon black. The white pigments can adjust coverage in addition to color tone, and examples thereof include titanium dioxide and zinc oxide. The extender pigments are diluents that are used to adjust color tone and, at the same time, to adjust the feeling of use (extensibility or adhesion) or gloss of products. Also, the extender pigments are used to maintain the formulation of products. The extender pigments among the inorganic pigments used in cosmetics are talc, kaolin and mica having the following characteristics. Talc used in mascara formulations is magnesium silicate hydrate (Mg3Si4Oi0(OH)2) and is generally composed of a compact of fine crystals or an aggregate of foliar crude crystals. Also, the talc feels very soft, and the talc particles have a thin plate shape and are frequently used in cosmetics to improve extensibility or smoothness . Kaolin, also known as "china clay", has its name derived from the name of the Chinese town Kao-Ling, where high-purity white clay used as the raw material of porcelain was produced. Kaolin has a composition of aluminum silicate hydroxide (Al2Si2O5(OH)4) and shows a regular hexagonal plate shape at high crystallinity, but has a fine irregular plate shape at low crystallinity. Furthermore, it has an excellent adhesion to the skin, because a low thickness of the plate shaped particles. Also, it is frequently used in cosmetics, because it has excellent oil absorption and water absorption properties.
Mica is typically exemplified by muscovite belonging to potassium mica and is represented by a chemical formula of KAl2(AlSi3)Oi0(OH)2. The mica consists of light yellow or green hexagonal plate-shaped crystals belonging to the monoclinic system. Mica may also be exemplified as silk mica (sericite) " because it consists of aggregates of fine crystals similarly to muscovite and because it appears as a silky gloss on the surface of buildings.
The extender pigments are easy to apply in a mascara formulation due to a soft feeling of use, application and the like, and are used through various coating techniques depending on the purpose. For example, the talc is applied to realize a soft application because it has the lowest refractive index of the extender pigments and soft property, and the talc coated with alkylsilane is applied to solve the problem of flake-off by improving adhesion. To improve durability, the talc is coated with a silicone compound to prevent smudging of mascara, however the silicone has a poor adhesion.
The mica has a thin layer shape and has the highest aspect ratio of the extender pigments. Smoothness of the mica is less than that of the talc, but the mica exhibits an excellent adhesion caused by its wide plate form, and has better gloss and a low refractive index, similar to that of the talc, therefore it is used in many applications. However, the mica has problems of smudging and poor durability due to a shortage of low oil absorption. To overcome the problems, surface treatments such as coating have been developed. Silicone coating among the coating methods imparts water repellency and oil repellency to provide smooth touch, but a problem of spreadability caused by a property of formulation becomes prevalent, and the silicone further exhibits a poor adhesion. In the case of alkylsilane coating, the spreadability is relatively- improved in the formulation, but a poor durability still remains .
The coating methods of extender pigments have been studied for various purposes . The usual coating methods are conducted by a dry, wet or CVD coating, which are well known in the art. Various studies about the coating methods are proceeding to obtain coating materials and methods providing a desirable property and uniform coating. The mica is usually coated with alkylsilane, dimethicone, methicone and amino acid, which are well known as coating materials. At the coating process, heat treatment temperature is generally between 120 and 180°C, and certainly less than 200°C. If the temperature exceeds 200°C, the inherent property of the coating material is disappears, and water-resistance and oil-resistance significantly decrease, in addition to a feeling of use becoming poor .
[Disclosure] [Technical Problem]
The inventors of the present invention have studied to develop a new cosmetic that improves the durability and spreadability while maintaining adhesion caused by a high aspect ratio of the mica. As a result, the present inventors have developed a mascara composition having a long lash effect caused by improved smooth application, adhesion of mica powder and durability of formulation through spraying MQ resin, which is a film forming agent, as a coating material with a heat treatment of 300 to 350°C in a vacuum according to a common dry coating process to disperse uniformly and make a coating layer that is formed by covalent bonds between the coating material and the mica, and between the individual MQ resin molecules.
Further, the present invention forms a net structure between the MQ resin coating material and the mica through heating at a temperature of more than 300°C, higher than a heat treatment temperature applied in a common coating process, whereby it is confirmed that water resistance, which is an effect caused by the coating, is significantly improved, and a smooth surface property and adhesion property of the solid plate shaped mica are increased.
Therefore, the object of the present invention is to provide a mica composite powder that is prepared by coating the surface of mica particles with MQ resin, which is a film forming agent, with a heat treatment of 300 to 350°C for increasing water repellency, thus obtaining a long lash effect through smooth application, improved adhesion of the mica powder and durability of formulation when the mica composite powder is applied in the formulation, and a long lash mascara composition containing the same. [Technical Solution]
To achieve the object, the present invention provides a mica composite powder that is prepared by coating the surface of mica particles with MQ resin and heat treating at 300 to 350°C, thus obtaining smooth application, improved effects of adhesion of mica powder and durability of formulation when the mica composite powder is applied in the formulation, and a long lash mascara composition containing the same .
[Advantageous Effects]
According to the invention, a long lash mascara composition containing a mica composite powder coated with MQ resin, which is a film forming agent, can be prepared to have an improved effect of makeup durability without flake- off. The composition improves water repellency due to the coating layer, increases makeup durability through an enhanced adhesion, and exhibits a long lash effect influenced by a high aspect ratio of the mica powder. Further, the present invention can improve water- resistance, smooth surface and adhesion property of the solid plate shaped mica through a temperature of more than 300 "C in the coating process.
[Best Mode]
Hereinafter, the present invention is described in detail.
The present invention relates to a mica powder that is prepared by coating the mica surface with MQ resin, preferably trimethylsiloxysilicate, with a heat treatment of 300~350°C, and to a long lash mascara composition containing the same .
A mica used in the present invention has preferably a mean particle size of 3 p to 40 βϋ\ and an aspect ratio of 90 to 120. The present invention uses Mica FA450 (Yamaguchi Mica Company, Japan) , but is not limited thereto. The mica used in the present invention has an aspect ratio of 100 to 109 and a mean particle size of 22 μm, and exhibits an excellent adhesion and spreading property because it has a relatively high aspect ratio. The term "long lash effect" as used herein means an effect making eyelashes artificially longer than an inherent length of the eyelashes and looking longer in a mascara formulation. Mica having an aspect ratio of about 70 is commonly used nowadays, because if the aspect ratio of the mica exceeds 70, its adhesion is low so that flake- off will occur. However, the present invention treats the mica having an aspect ratio of more than 70 with trimethylsiloxysilicate through coating at high temperature to improve an adhesion and water-resistance property.
Generally, a resin is an M-form if it has one methyl group attached to a central silicon (Si) , a D-form if it has two methyl groups attached to a central silicon, a T- form if it has three methyl groups attached to a central silicon, and a Q- form if it has four methyl groups attached to a central silicon. The MQ resin as used herein is M-form resin attached to Q-form resin.
The MQ resin used in the present invention is a silicone based resin, a silicone based resin may show four resin forms: M-resin has one Si-O bond, D-resin has two Si- O bonds, T-resin has three Si-O bonds, and Q-resin has four Si-O bonds. The MQ resin used in the present invention is a resin bonded M-resin and Q-resin according to an MQ ratio, which is the ratio between M-resin and Q-resin. Various materials attached to Si of the M-resin exist, but the MQ resin commonly used is generally organo polysiloxane bonded with Si-CH3. The compound represented by the following Chemical Formula 1 is trimethylsiloxysilicate, which is a kind of MQ resin that imparts water repellency as a film forming agent .
[Chemical Formula l]
Me Me Me
Me Si O Si O Si OH
Me O O O Si O Si O
Me O
OH
An MQ resin used in the present invention usually has an MQ ratio of between 0.7 and 1.3. The MQ resin may include, for example, a trimethylsiloxysilicate/cyclotetrasiloxane, a trimethylsiloxysilicate/cyclopentasiloxane, a trimethylsiloxysilicate/dimethicone and a trimethylsiloxysilicate/isododecane, most preferably a trimethylsiloxysilicate/isododecane having an MQ ratio of between 1.0 and 1.1.
A process and method for coating the mica with MQ resin are similar to a common dry coating process. More specifically, mica is first dried in a dryer at 105 °C for more than 4 hours. The dried mica is then introduced into a Henschel Mixer, and a vacuum is created inside the Henschel Mixer. The MQ resin is then dispersed by spraying in an amount of 1.0 to 5.0% by weight, more preferably 2.0 to 4.0% by weight. If the MQ resin content is less than 1.0% by weight, it is difficult to obtain an improvement of durability caused by coating, and if the MQ resin content exceeds 5.0% by weight, flake-off and a hard feeling of use occurs when applied in a mascara formulation.
After spraying, the MQ resin is further dispersed by mixing for 15 to 600seconds, preferably 30 to 300seconds, and then the resultant is heat treated for more than lhour at 300 to 350°C, preferably 300 to 310°C.
The spraying time of the present invention is longer than that of a common coating process due to a difficultly of obtaining a uniform dispersion of the MQ resin through a common process because the MQ resin has a high viscosity as compared to those of common coating materials. If the spraying time is less than 30seconds, the prepared mica composite powder loses a soft property due to an uneven surface, and does not uniformly exhibit water resistance. Therefore, the dispersion time of the present invention is longer than that of a common coating process in order that the coating material can be dispersed uniformly, thus the present invention can obtain a uniform surface property and water resistance.
Also, the heat treatment temperature of the present invention is greater than that of a common coating process in order to prevent a decrease of eyelash adhesion due to heat treating the mica having an aspect ratio of more than 70 at less than 300°C, thereby resulting in a poor long lash effect and flake-off property and reduced water resistance.
Further, when the heat treatment temperature is greater than 300°C, a very small amount of impurities included in the mica are removed to obtain an excellent gloss and uniform coating layer, thus an uneven surface property of the mica is modified to exhibit a soft surface property that is not shown in a heat treatment temperature of a common coating process. This effect is a result of the coating materials forming a net structure uniformly on the mica surface.
The mica composite powder of the present invention maintains an adhesion and smooth application due to a high aspect ratio of the mica and improves a durability and spreadability by a coating layer of MQ resin coated on the mica surface to stabilize the formulation, thereby the mica composite powder can be formulated in a cosmetic composition, such as mascara or eye liner, according to a conventional method. In the cosmetic composition, the mica composite powder of the present invention is contained in an amount of 0.1 to 4.0% by weight based on the total weight of the cosmetic composition.
[Mode for Invention] Hereinafter, the present invention is described in detail with examples. It is to be understood, however, that the scope of the present invention is not limited to these examples .
Example 1 : Preparation of a powder with trimethylsiloxysilicate/isododecane coated on mica FA 450 lOOg of mica FA 450 having an aspect ratio of 100 to 109 were dried at 105 °C for more than 4hours, then the dried mica was introduced into a Henschel mixer and a vacuum was produced. 5g of trimethylsiloxysilicate/isododecane were sprayed on the mica and mixed, then heat treated at 310°C for δhours . After heat treating, 103g of the mica coated with trimethylsiloxysilicate were obtained.
Comparative Example 1: Preparation of a powder with trimethylsiloxysilicate/isododecane coated on mica A 325 lOOg of mica A 325 having an aspect ratio of 70 to 80 were dried at 105 °C for more than 4hours, then the dried mica was introduced into a Henschel mixer, and a vacuum was produced. 5g of trimethylsiloxysilicate/isododecane were sprayed on the mica and mixed, then heat treated at 310 °C for δhours . After heat treating, 103g of the mica coated with trimethylsiloxysilicate were obtained.
Comparative Example 2 : Preparation of a powder with trimethylsiloxysilicate/isododecane coated on mica NCF 322 lOOg of mica NCF 322 having an aspect ratio of 121 to 127 were dried at 105 °C for more than 4hours, then the dried mica was introduced into a Henschel mixer, and a vacuum was produced. 5g of trimethylsiloxysilicate/isododecane were sprayed on the mica and mixed, then heat treated at 310°C for δhours.
After heat treating, 103g of the mica coated with trimethylsiloxysilicate were obtained.
Comparative Example 3 : Preparation of a powder with trimethylsiloxysilicate/isododecane coated on mica FA 450 lOOg of mica FA 450 having an aspect ratio of 100 to
109 were dried at 105 °C for more than 4hours, then the dried mica was introduced into a Henschel mixer, and a vacuum was produced. 5g of trimethylsiloxysilicate/isododecane were sprayed on the mica and mixed, then heat treated at 180 °C for δhours.
After heat treating, 103g of the mica coated with trimethylsiloxysilicate were obtained.
Experimental Example 1: Test of Durability
In order to prepare a mascara composition containing the mica composite powder prepared in Example 1, a Formulation Example 1 and Comparative Formulation Examples
1 to 4 having the compositions shown in Table 1 were prepared according to a conventional method (Unit: % by weight) . After preparation, the durability of Formulation Example 1 and Comparative Formulation Examples 1 and 4 was measured. [Table l]
Figure imgf000017_0001
For the durability test, Formulation Example 1 and Comparative Formulation Examples 1 and 4 were applied on artificial eyelashes according to a conventional makeup method, and then dried for lOmins. After drying, artificial tears were dropped to induce wetting for lOmins. A filter paper was applied to cover the eyelashes and pushed using a roller. The durability of the formulation was evaluated through the area adhered to the filter paper and the results thus obtained are given in Table 2 below. [Table 2]
Figure imgf000018_0001
©: completely absent O: almost absent Δ: slightly exists X: exists
As can be seen from Table 2, the mascara formulation of Formulation Example 1 containing the mica composite powder according to the present invention exhibits a perfect durability without smudging, whereas Comparative Formulation Example 1 containing the uncoated mica is slightly adhered to the filter paper. Also, it is confirmed that the water resistance of Comparative Formulation Example 4, which has a low coating temperature, is less than that of Formulation Example 1, but is greater than that of Comparative Formulation Example 1, as only a little smudging is induced.
Experimental Example 2 : Test of Long Lash Effect and Flake-off
Formulation Example 1 and Comparative Formulation Examples 1 to 4 were applied to evaluate the long lash effect and flake-off thereof and compared according to a sense of feeling through a consumer panel test of twenty persons . The results thus obtained are shown in Table 3.
[Table 3]
Figure imgf000019_0001
h Very good O: Good Δ : Moderate X: Poor
As can be seen from Table 3, the mascara formulation of Formulation Example 1 containing the mica composite powder of Example 1 according to the present invention exhibits an excellent long lash effect because the adhesion of Formulation Example 1 is greater than that of Comparative Formulation Example 1. The flake-off of Formulation Example 1 and Comparative Formulation Examples 2-4 is reduced as compared to Comparative Formulation Example 1 containing the uncoated mica, because the adhesion of the mica is improved by Si-CH3 of the MQ resin as a coating material. Therefore, the adhesion of the mica can be improved by the coating to reduce flake-off.
Further, in the coated powders, the smooth application of Comparative Formulation Example 4, which has a relatively low coating temperature, is less than that of Formulation Example 1 because a polymerization time is insufficient to retain an adhesive property of the resin and decreases a smooth property.
Comparative Formulation Example 3 having an aspect ratio of 120 to 127 has a shortage of resistance to flake- off due to the high aspect ratio, and Comparative Formulation Example 2 having an aspect ratio of 70 to 80 does not exhibit a long lash effect due to the low aspect ratio. Therefore, the present invention can provide a long lash mascara composition having a long lash effect without flake-off through preparing a mica composite powder by coating the surface of mica particles with MQ resin, which is a film forming agent, with a heat treatment of 300 to 350 °C for increasing water repellency, thus increasing durability of makeup and obtaining improved durability of formulation and adhesion of the mica powder when the mica composite powder is applied in the formulation.

Claims

[CLAIMS]
[Claim l]
A mica composite powder with MQ resin coated on a mica surface, wherein a heat treatment temperature is 300 to 350 "C in a coating process.
[Claim 2]
The mica composite powder of claim 1, wherein the mica has a mean particle size of 3 ~ 40μm.
[Claim 3] The mica composite powder of claim 1, wherein the mica has an aspect ratio of 90 to 120.
[Claim 4]
The mica composite powder of claim 1, wherein the MQ resin has an MQ ratio of 0.7 to 1.3.
[Claim 5]
The mica composite powder of claim 1, wherein the MQ resin is at least one selected from a group consisting of trimethylsiloxysilicate/cyclotetrasiloxane, trimethylsiloxysilicate/cyclopentasiloxane, atrimethylsiloxysilicate/dimethicone and trimethylsiloxysilicate/isododecane .
[Claim 6]
The mica composite powder of claim 1, wherein a content of the MQ resin coated on the mica surface is 1.0 to 5.0% by weight based on the total weight of the mica composite powder.
[Claim 7] A long lash mascara composition containing the mica composite powder prepared according to any one of claims 1 to 6. [Claim 8]
The long lash mascara composition of claim 7, wherein the mica composite powder is contained in an amount of 0.1 to 4.0% by weight based on the total weight of the composition.
PCT/KR2007/004657 2006-11-30 2007-09-21 Mica composite powder coated with trimethylsiloxysilicate and the long lash mascara composition containing the same WO2008066243A1 (en)

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