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WO1998016193A1 - Dispersion de dioxyde de titane particulaire dans du silicone - Google Patents

Dispersion de dioxyde de titane particulaire dans du silicone Download PDF

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Publication number
WO1998016193A1
WO1998016193A1 PCT/JP1997/002760 JP9702760W WO9816193A1 WO 1998016193 A1 WO1998016193 A1 WO 1998016193A1 JP 9702760 W JP9702760 W JP 9702760W WO 9816193 A1 WO9816193 A1 WO 9816193A1
Authority
WO
WIPO (PCT)
Prior art keywords
titanium dioxide
silicone
dispersion
dispersion according
fine particle
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP1997/002760
Other languages
English (en)
Japanese (ja)
Inventor
Hideo Futamata
Hideo Takahashi
Masakazu Hattori
Masanori Iida
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ishihara Sangyo Kaisha Ltd
Original Assignee
Ishihara Sangyo Kaisha Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from JP28913296A external-priority patent/JP3224750B2/ja
Application filed by Ishihara Sangyo Kaisha Ltd filed Critical Ishihara Sangyo Kaisha Ltd
Priority to AU37840/97A priority Critical patent/AU3784097A/en
Publication of WO1998016193A1 publication Critical patent/WO1998016193A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89—Polysiloxanes
    • A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • A61K8/894—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by a polyoxyalkylene group, e.g. cetyl dimethicone copolyol
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29—Titanium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/58—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
    • A61K8/585—Organosilicon compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89—Polysiloxanes
    • A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/413—Nanosized, i.e. having sizes below 100 nm

Definitions

  • the present invention relates to a dispersion in which fine particle titanium dioxide is dispersed in silicone and a sunscreen cosmetic using the same.
  • Fine particle titanium dioxide with a single particle size of about 0.15 ⁇ m or less when incorporated into a film or molded product such as a resin, shields ultraviolet rays and protects substances that are altered by ultraviolet rays, while transmitting visible light. It is well known that it exhibits properties different from pigment-grade titanium dioxide having a single particle size of 0.15 to 0.5 ⁇ m, such as high transparency. In addition, since its effect on the human body is extremely low and there is almost no deterioration by ultraviolet light or chemicals, particulate titanium dioxide is a highly safe, stable, and highly transparent ultraviolet shielding agent for paints and cosmetics. It is used for chemical fiber.
  • silicones have come to be widely used in paints and cosmetics as a material having excellent water resistance, water repellency, chemical resistance, and weather resistance.
  • cosmetics have attracted much attention because of their excellent water-resistance, good stretchability when applied to the skin, and a light touch.
  • titanium dioxide is blended with silicone-based cosmetics for the purpose of imparting ultraviolet shielding properties, the surface of titanium dioxide is hydrophilic, while silicone has high hydrophobicity. Titanium dioxide particles were agglomerated without being compatible with silicone, causing a problem that the original transparency and ultraviolet shielding properties were not exhibited.
  • the present invention relates to a fine particle titanium dioxide, which is an ultraviolet ray shielding agent with excellent safety, stability, and transparency, that is formulated into a highly dispersed state by a relatively simple dispersion treatment when blended with silicone-based cosmetics.
  • An object of the present invention is to provide a dispersion capable of imparting an excellent ultraviolet shielding ability.
  • the present inventors have formulated fine particle titanium dioxide into a silicone cosmetic.
  • the dispersant is used and the silicone is used as a solvent and the silicone is used as a medium, the above-mentioned problems can be solved.
  • the feeling of elongation is improved.
  • the present inventors have found that there is an excellent effect not found in the prior art, such as improvement of the conventional technology, and completed the present invention.
  • the fine particle titanium dioxide dispersion of the present invention comprises silicone as a medium, fine particle titanium dioxide, and a dispersant that stably disperses the particles.
  • the dispersion medium is 20 to 70% by weight, preferably 40 to 70% by weight
  • the fine particle titanium dioxide is 30 to 70% by weight
  • the dispersant is 1 to 40% by weight. It is.
  • the shape of the fine particle titanium dioxide in the fine particle titanium dioxide dispersion of the present invention may be any of a spherical shape, a rod shape, a spindle shape, a dendritic shape, and a starfish shape, and the average single particle size is 0.005 to 0.15. ⁇ M, preferably 0.005 to 0.11 ⁇ m.
  • ⁇ M preferably 0.005 to 0.11 ⁇ m.
  • particulate titanium dioxide having a shape other than spherical their volumes were determined and a true sphere equivalent to the volume was assumed, and the diameter was taken as the average single particle diameter of each shape.
  • titanium dioxide having a length of 0.05 to 6 / m and an axial ratio of 3 or more is preferable.
  • the average major axis diameter is 0.
  • the fine particle titanium dioxide used in the present invention can be produced by various methods.
  • the titanium tetrachloride aqueous solution is neutralized and hydrolyzed with an alkali, and the obtained hydrous titanium dioxide is calcined or hydrous titanium dioxide is produced.
  • a hydrous titanium dioxide solution obtained by heating and hydrolyzing an aqueous solution of titanium sulfate or titanium tetrachloride may be peptized with an acid, or may be further baked.
  • the fine particle titanium dioxide is coated with, for example, at least one oxide or hydrated oxide of aluminum, silicon, zirconium, titanium, zinc, and tin in order to improve the affinity with the dispersant and the light resistance.
  • fine particle titanium dioxide is an organic substance such as higher fatty acids such as stearic acid and lauric acid and metal salts thereof; siloxane compounds such as dimethyl polysiloxane and methyl hydrogen polysiloxane; and polyol compounds such as trimethylolethane and trimethylolpropane. It may be coated.
  • the silicone used as a solvent in the present invention may be selected according to the cosmetic to be blended.
  • methylpolysiloxane; octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane Such as methylcyclopolysiloxane; methylfluoropolysiloxane.
  • the dispersant used in the present invention is preferably a silicone compound, for example, dimethylpolysiloxane-methyl (polyoxyalkylene) siloxane copolymer, trimethylsiloxycyanic acid, carboxy-modified silicone oil, amino And modified silicone oil.
  • a good silicone dispersion in terms of dispersibility, viscosity, stability and the like can be obtained.
  • the greater the specific surface area of titanium dioxide and the greater the amount of surface coating the greater the optimal blending of the dispersant.
  • the optimum amount of the dispersant varies depending on the method of producing ultrafine titanium dioxide and the type of surface coating agent. In some cases, it is better to use a combination of two or more dispersants. This is because the use of only one dispersant can suppress the elongation and the emulsification stability of cosmetics, if they are not sufficient.
  • the dispersion of the present invention is obtained by pre-mixing a specific dispersant, a solvent solution, and particulate titanium dioxide using a blade-type stirrer, disperser, homomixer, or the like, and then using a pulverizer such as a sand mill, a pebble mill, or a disk mill. To obtain fine particles of titanium dioxide.
  • the heat treatment may be performed at a temperature of 50 ° C. or more, preferably 80 ° C. or more, before, after, or after such a dispersion operation.
  • the type of mill, the selection of grinding media, and the setting of optimal grinding conditions are important in adjusting advanced dispersions.
  • a vertical or horizontal sand mill with a 0.5 mm diameter zircon It is desirable to pulverize using. Since the fine particle titanium dioxide dispersion thus obtained contains the fine particle titanium dioxide in an extremely dispersed state, when blended in cosmetics, the fine particle titanium dioxide inherently has excellent ultraviolet shielding ability. In addition to fully exerting the effect, it has the effect of improving the stability of the combined cosmetics and improving the feeling of use such as good elongation.
  • the fine particle titanium dioxide silicone dispersion is prepared under conditions that are very suitable for dispersing the fine particle titanium dioxide, it is blended with a desired cosmetic, so that the inherent ultraviolet ray shielding capability inherent in the fine particle titanium dioxide is sufficiently exhibited. You. On the other hand, in general, even if the fine particle titanium dioxide is blended in such a way that the powder is blended into the cosmetic, the fine particle titanium dioxide does not sufficiently exhibit the inherent ultraviolet shielding ability. Problems such as sedimentation and separation from the silicone component often occur.
  • the fine particle titanium dioxide silicone dispersion of the present invention is used as a sunscreen cosmetic, for example, an oily component mainly containing silicone, a humectant, a surfactant, a pigment, a fragrance, a preservative, water, alcohols, It can be used in various forms, such as lotions, creams, pastes, sticks, emulsions, etc., by mixing with a viscous agent.
  • a sunscreen cosmetic for example, an oily component mainly containing silicone, a humectant, a surfactant, a pigment, a fragrance, a preservative, water, alcohols, It can be used in various forms, such as lotions, creams, pastes, sticks, emulsions, etc., by mixing with a viscous agent.
  • the slurry 7 0 sodium aluminate with good stirring was heated to ° C was added 5% T i 0 2 weight as A 1 2 0 -3, subsequently Mature form and hydrated oxides of aluminum was precipitated and coated on the titanium dioxide particles.
  • the solid content is filtered and washed, and the washed cake is dried and then powdered with a hammer type mill. This was ground to obtain ultrafine titanium dioxide powder (average single particle diameter: 0.02 urn).
  • the hydrous titanium oxide obtained by hydrolysis of the titanium tetrachloride aqueous solution was used as an aqueous suspension having a concentration of 100 g / 1 in terms of T i 0.
  • To this aqueous suspension 21 was added 1400 g of a 48% aqueous sodium hydroxide solution with stirring, heated at 95 ° C. for 120 minutes, filtered, and sufficiently washed. .
  • the washed cake was Reparupu with water, and T i 0 2 conversion 1 0 0 g / 1 concentration of the aqueous suspension, placed the aqueous suspension 1.5 1 reflux condenser flask, 35% hydrochloric acid 4 After adding 0 g with stirring, the mixture was heated and aged at 95 ° C for 120 minutes, and the major axis of the rutile crystal was 0.20 // m, the axial ratio was 5.0 (average single particle diameter). When expressed, an aqueous suspension of 0.078 ⁇ m) of rod-shaped fine particle titanium oxide was obtained.
  • the hydrous titanium oxide obtained by hydrolysis of titanium tetrachloride aqueous solution was T i 0 2 conversion 1 0 0 g / 1 concentration of the aqueous suspension.
  • To this aqueous suspension 21 was added 1400 g of a 48% aqueous sodium hydroxide solution with stirring, and after heating at 95 ° C for 120 minutes, filtration was performed. And thoroughly washed.
  • the washed cake was Reparupu with water, T i 0 2 and converted 1 0 0 gZ l aqueous suspension with a concentration of, putting the aqueous suspension 1.5 1 reflux condenser flask, 3 5% hydrochloric acid 5 7 0 g was added instantaneously with stirring, and the mixture was aged by heating at 95 ° C for 120 minutes, and the long axis of the rutile crystal was 0.30 ⁇ m and the short axis was 0.055 ⁇ m (average). An aqueous suspension of dendritic particulate titanium oxide having a particle diameter of 0.11 ⁇ m) was obtained.
  • the suspension was added 5% T i 0 2 weight sodium aluminate as A 1 2 0 3 with good stirring after heating to a 7 0 ° C, hydrated oxides of Aruminiu beam subsequently was aged Was precipitated and coated on the titanium dioxide particles.
  • the solid content was filtered and washed, and the washed cake was dried and then pulverized with a hammer type mill to obtain dendritic fine particles of titanium dioxide powder.
  • the dendritic titanium dioxide powder 40 parts by weight of the dendritic titanium dioxide powder was mixed with a dispersion of 12 parts by weight of a dispersant (trimethylsiloxygayic acid) and 48 parts by weight of a dispersion medium (decamethylcyclopentasiloxane) using a disperser. did. Next, this was pulverized with a sand mill using zircon beads as a medium to obtain a silicone oil dispersion (C) having a viscosity of 130 cP.
  • a dispersant trimethylsiloxygayic acid
  • a dispersion medium decamethylcyclopentasiloxane
  • Example 4 40 parts by weight of the fine particle titanium dioxide powder of Example 1 was dispersed with a dispersant (6 parts by weight of trimethylsiloxy gay acid and 6 parts by weight of dimethylpolysiloxane 'methyl (polyoxyethylene) siloxane copolymer) in a total of 12 parts by weight.
  • the mixture was mixed with a solvent (octamethylcyclotetrasiloxane) 48 parts by weight using a disper.
  • this was pulverized with a sand mill using zircon beads as a medium to obtain a silicone oil dispersion (D) having a viscosity of 90 cP.
  • the fine particle titanium dioxide of Example 1 was used as a powder (E).
  • the rod-shaped fine particle titanium dioxide of Example 2 was used as a powder (F).
  • the dendritic particulate titanium dioxide of Example 3 was used as the powder (G). Test example 1
  • a sunscreen cream (WZO emulsion) is prepared by blending the silicone dispersion (A) to (D) and the powders (E) to (G) of the fine particle titanium dioxide in the following formulation so that the total amount is 100 parts by weight.
  • the components (1) to (5) were mixed and dispersed with a disperser, and the premixed components (6) to (8) were gradually added with stirring to prepare a sunscreen cream.
  • Each of the above creams was applied on a quartz glass plate so as to have a thickness of 25 // m, and the transmittance at 750 to 300 nm was measured with a spectrophotometer.
  • the fine particle titanium dioxide silicone dispersion of the present invention contains finely particulate titanium dioxide, which is an ultraviolet shielding agent excellent in safety, stability, and transparency, in a very well-dispersed state.
  • finely particulate titanium dioxide which is an ultraviolet shielding agent excellent in safety, stability, and transparency, in a very well-dispersed state.

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Pharmacology & Pharmacy (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Dermatology (AREA)
  • Cosmetics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Les tentatives destinées à mélanger une matière cosmétique à base de silicone avec du dioxyde de titane particulaire, pour conférer des propriétés de barrage des ultraviolets à ladite matière, provoquent l'agglomération du dioxyde de titane particulaire et empêchent donc ladite matière de présenter les propriétés de transparence et de barrage des ultraviolets inhérentes au dioxyde de titane, parce que la surface du dioxyde de titane particulaire est hydrophile, tandis que le silicone est fortement hydrophobe, c'est-à-dire que ces deux constituants sont incompatibles l'un avec l'autre. La présente invention concerne donc une dispersion stable préparée par dispersion de dioxyde de titane particulaire dont le diamètre moyen unique des particules va de 0,005 à 0,15 νm dans un milieu de silicone à l'aide d'un dispersant.
PCT/JP1997/002760 1996-10-11 1997-08-07 Dispersion de dioxyde de titane particulaire dans du silicone Ceased WO1998016193A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU37840/97A AU3784097A (en) 1996-10-11 1997-08-07 Dispersion of particulate titanium dioxide in silicone

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP28913296A JP3224750B2 (ja) 1995-11-28 1996-10-11 微粒子二酸化チタンシリコ−ン分散体
JP8/289132 1996-10-11

Publications (1)

Publication Number Publication Date
WO1998016193A1 true WO1998016193A1 (fr) 1998-04-23

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP1997/002760 Ceased WO1998016193A1 (fr) 1996-10-11 1997-08-07 Dispersion de dioxyde de titane particulaire dans du silicone

Country Status (3)

Country Link
AU (1) AU3784097A (fr)
TW (1) TW409127B (fr)
WO (1) WO1998016193A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001037795A1 (fr) * 1999-11-25 2001-05-31 Shiseido Co., Ltd. Procede de production de produits cosmetiques
KR100376089B1 (ko) * 2001-03-14 2003-03-15 주식회사 태평양 자외선 차단용 베이스 조성물 및 이를 포함하는 화장품

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03115211A (ja) * 1990-08-22 1991-05-16 Kao Corp 化粧料
JPH08127514A (ja) * 1994-10-27 1996-05-21 Kanebo Ltd メイクアップ化粧料

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03115211A (ja) * 1990-08-22 1991-05-16 Kao Corp 化粧料
JPH08127514A (ja) * 1994-10-27 1996-05-21 Kanebo Ltd メイクアップ化粧料

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001037795A1 (fr) * 1999-11-25 2001-05-31 Shiseido Co., Ltd. Procede de production de produits cosmetiques
US6972129B1 (en) 1999-11-25 2005-12-06 Shiseido Co., Ltd. Method for producing cosmetics
KR100376089B1 (ko) * 2001-03-14 2003-03-15 주식회사 태평양 자외선 차단용 베이스 조성물 및 이를 포함하는 화장품

Also Published As

Publication number Publication date
AU3784097A (en) 1998-05-11
TW409127B (en) 2000-10-21

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