WO2012133018A1

WO2012133018A1 - Metal oxide conjugated highly-flat cellulose powder and cosmetic containing same

Info

Publication number: WO2012133018A1
Application number: PCT/JP2012/057110
Authority: WO
Inventors: 増渕　祐二; 五十嵐　啓二; 村田　東吾; 村田　哲雄
Original assignee: 株式会社オーケン; 株式会社コーセー
Priority date: 2011-03-28
Filing date: 2012-03-21
Publication date: 2012-10-04
Also published as: TW201302228A; HK1186687A1; TWI595886B; JP6069189B2; JPWO2012133018A1; KR20140036158A; CN103442685B; CN103442685A; KR101600058B1

Abstract

The purpose of the present invention is to provide a powder for a cosmetic having, when compared to conventional powders for cosmetics, a better skin feel, and high functionality such as a UV blocking ability, and also to provide a cosmetic using the same. The cosmetic is a metal oxide conjugated highly-flat cellulose powder obtained by mechanically grinding a cellulosic material, a grinding aid, and a metal oxide, and combines the same.

Description

Metal oxide composite high flat cellulose powder and cosmetics containing the same

The present invention relates to a cellulose powder having high flatness composited with a metal oxide and a powder cosmetic containing the same, and more specifically, has a shape having high flatness and the surface thereof is a metal oxide. The present invention relates to a metal oxide-complexed highly flat cellulose powder coated with a cosmetic and a cosmetic containing the same.

Powder cosmetics containing a powder component, an oily component, and the like are widely used in the field of cosmetics, and examples thereof include powder foundation, eye shadow, powdered white powder, blusher, and the like.

This powder cosmetic is generally produced by filling a powder container of powder components such as extender pigments and pigments and an oil component into a dish-like container and press-molding.

As the powder component used in this powder cosmetic, natural pigment-derived thin mica pieces, sericite, talc, etc. and surface treated products thereof are extender pigments because they have good elongation and stickiness on the skin. Has been used as. Further, spherical organic powders and the like have been used together with the above extender pigments in order to improve the slip and feel of extender pigments on the skin. Furthermore, as pigments, white pigments such as titanium oxide, colored pigments such as Bengala, and glossy pigments such as titanium mica have been used.

Also known are powder components coated with metal oxide (Patent Documents 1 to 3). For example, Patent Documents 1 and 2 both cover polymer fine powder and spherical resin powder with a fine metal oxide, and Patent Document 3 can be used as cosmetic powder. The substrate was treated with hydroxyapatite and zinc oxide.

By the way, the powder component has various shapes, and flaky inorganic powders such as mica pieces, sericite, and talc are widely used, but these are all aluminosilicate minerals. In addition, since the properties are slightly different depending on the production area, for example, there is a problem that the oil absorbability is low or the desired physical properties cannot be obtained. On the other hand, flat organic powders have not been reported so much, for example, to the extent that flat cellulose particles obtained by mixing cellulose-based substances and fatty acids and then mechanically pulverizing them are known. (Patent Document 4).

However, in this Patent Document 4, although flat cellulose particles are disclosed, the specific usage form is not disclosed, and the application to cosmetics is only disclosed very simply.

On the other hand, a technique for treating the surface of crystalline cellulose with hydrogenated lecithin is also known (Patent Document 5). However, this crystalline cellulose has a major axis / minor axis ratio (L / D) of 3 or less, which is not flat. In fact, when compared with untreated ones, there is a difference in the goodness of makeup. However, it is disclosed that there is not much difference between “Take”, “Nobi”, and “Finish” that are the feeling of use.

The present inventors have previously developed a flat cellulose powder having an extremely high flatness (aspect ratio) of 20 to 200 (hereinafter referred to as “high flatness cellulose powder”) and a method for producing the same, and applied for a patent. (Patent Document 6). This high flatness cellulose powder is obtained by drying the purified cellulose pulp-derived cellulose powder under reduced pressure to sufficiently remove the adsorbed moisture, and then grinding it with a planetary ball mill together with a grinding aid and, if necessary, a hydrophobizing agent. It is obtained by.

The resulting high flatness cellulose powder is made of cellulose and has the characteristics of high flatness, so when it is blended as a powder cosmetic ingredient, the amount of oily ingredients is large. However, the agglomeration of the powder is not caused, the characteristics such as the smoothness of the powder itself are maintained, and the caking is difficult to occur even if the powder is pressed.

JP-A-3-2000072 JP-A-8-59433 Japanese Patent Laid-Open No. 2002-20218 JP 2004-230719 A JP 2003-146829 A WO / 2010/026925

Although many cosmetic powders have already been provided, it is natural for consumers to seek cosmetics with a better feeling of use and higher usability, and the present invention provides such cosmetics. An object of the present invention is to provide a cosmetic powder and a cosmetic using the same.

The inventors of the present invention were further researching on the high flatness cellulose powder obtained from the cellulosic material, and added a grinding aid and a metal oxide to the cellulosic material by a specific method. By compounding, a metal oxide composite high flattened cellulose powder with properties that can hardly be obtained with conventional cosmetic powders is obtained, and by using this, commercial properties of cosmetics such as powder cosmetics are obtained. The present invention has been completed.

That is, the present invention is a metal oxide composite high flattened cellulose powder obtained by mechanically grinding a cellulosic material, a grinding aid, and a metal oxide.

The present invention is also a cosmetic comprising the metal oxide composite high flattened cellulose powder.

Furthermore, the present invention provides a metal oxide composite high flat cellulose powder characterized by adding a grinding aid and a metal oxide to a cellulosic material to form a mixture, and mechanically grinding the mixture. Is the method.

The metal oxide composite high flattened cellulose powder of the present invention has a new effect in addition to the effect of the conventional high flattened cellulose powder by combining the metal oxide on the surface thereof. . Specifically, when the composite metal oxide has a thickness of 10 to 100 nm on the powder, an extremely excellent UV blocking effect and a smooth use feeling can be obtained. Further, when the composite metal oxide is more than 100 nm and not more than 1000 nm on the powder, natural concealing properties, excellent color developability and a smooth feeling of use can be obtained.

The cosmetic compounded with this metal oxide composite high flattened cellulose powder has excellent cosmetic film uniformity and smooth use feeling, as well as excellent UV blocking effect, natural hiding property, and coloring effect. In addition, it has an excellent makeup lasting effect such as no color sink.

Therefore, the cosmetics using the metal oxide composite high flat cellulose powder of the present invention can be suitably used as powder foundation, eye shadow, powdered white powder, blusher and the like.

It is the photograph which observed the surface of the product 6 obtained in Example 6 with the scanning microscope (10,000 times). It is the photograph which observed the surface of the same product as FIG. 1 with the scanning microscope (50,000 times). It is the photograph which observed the surface of the same product as FIG. 1 with the scanning microscope (200,000 times).

The metal oxide composite high flat cellulose powder of the present invention is one in which fine metal oxide powder is firmly attached and combined on the surface of the high flat cellulose powder.

This metal oxide composite high flat cellulose powder is produced by adding a grinding aid and a metal oxide to a cellulose-based material to form a mixture, and mechanically grinding the mixture.

The cellulosic material used as a starting material for the metal oxide composite high flattened cellulose powder is not particularly limited, but for example, a woody material such as fibrous or powdery wood powder or wood pulp originating from wood It is preferable to use a cotton-based material such as fibrous or powdered cotton or linter fiber originating from cotton, a woody material, or a fibrous or powdery cellulose material obtained by refining the cotton-based material Alternatively, a purified cellulosic material obtained by acid hydrolysis may be used. In addition, as a cellulosic substance originating in cotton, the thing originating in the cotton which received the organic certification | authentication may be used.

The cellulosic material used as a raw material easily adsorbs or absorbs moisture, and has an adsorbed moisture of about 3 to 10% by mass (hereinafter simply referred to as “%”) in a normal state. In order to effectively obtain a flat cellulose powder from this cellulosic material, it is preferable to dry it beforehand by hot air drying, vacuum drying, reduced pressure drying or the like before removing the adsorbed water before pulverization.

On the other hand, the grinding aid used in the production of the metal oxide-complexed highly flat cellulose powder of the present invention is used for highly flattening the cellulosic material. And other substances, amino acids, fatty acids and the like. These may be used alone or in combination of two or more.

Among these, examples of amphiphilic substances include phospholipids, ceramides, cholesterol or derivatives thereof, phytosterols or derivatives thereof, and the like. These are substances having a common property of being a lipid in vivo or a structure close to that, that is, having a long-chain alkyl structure and a hydrophilic group.

Among the above amphiphiles, phospholipid is a generic term for lipids having a phosphate ester moiety in the structure. Specific phospholipids include those derived from natural products hydrogenated to natural lecithin such as egg yolk lecithin and soybean lecithin, hydrogenated lysolecithin, phosphatidylcholine, phosphatidylethanolamine, phosphatidylserine, phosphatidylglycerol, phosphatidylinositol, sphingomyelin, etc. And the like. Among these phospholipids, hydrogenated lecithin, phosphatidylcholine, phosphatidylethanolamine, and hydrogenated phosphatidylglycerol are preferable.

In addition, the ceramide has a non-linear group having one or more long-chain linear and / or branched alkyl or alkenyl groups, at least two hydroxyl groups, and one or more amide groups (and / or amino groups) in the molecule. A general term for ionic amphiphiles. Specific examples of ceramide include natural ceramides such as ceramide 1, ceramide 2, ceramide 3, ceramide 3B, ceramide 4, ceramide 5, ceramide 6, ceramide 6I, ceramide 6II and the like, which are long-chain fatty acid amides of sphingosine and phytosphingosine. Is mentioned. Among these ceramides, ceramide 2 and ceramide 3 are preferable. These ceramides may be derived from natural products or synthesized.

Furthermore, cholesterol is a white to slightly yellow solid purified by extracting, crystallizing and drying a fraction obtained from saponified animal oil and fat and fish oil, and its molecular formula is C ₂₇ H ₄₆ O. . Further, cholesterose derivatives include ester derivatives of saturated fatty acids such as oleic acid, palmitooleic acid, palmitic acid, stearic acid, 2-ethylhexanoic acid, capric acid, lauric acid, etc. , Esterified derivatives with a mixture of fatty acids obtained by hydrolyzing oils such as natural vegetable oils such as avocado oil, sesame oil, rice germ oil, macadamia nut oil, and animal oils such as fish oil and butter. Specific examples of preferable cholesterol derivatives include cholesteryl hydroxystearate, polyoxyethylene cholesteryl ether, and the like. Among these cholesterol or derivatives thereof, cholesterol is preferable.

Furthermore, phytosterol is a general term for sterol compounds obtained from plants. Specific examples of phytosterols include sitosterol, stigmasterol, fucostosterol, spinasterol, and brush castrol. Further, phytosterol derivatives include ester derivatives of saturated or unsaturated fatty acids such as oleic acid, palmitooleic acid, palmitic acid, stearic acid, 2-ethylhexanoic acid, capric acid, lauric acid, olive oil, avocado, etc. And esterified derivatives with a mixture of fatty acids obtained by hydrolyzing natural vegetable oils such as oil, sesame oil, rice germ oil and macadamia nut oil. Specific examples of preferred phytosterol derivatives include phytosteryl hydroxystearate, polyoxyethylene phytosterol, polyoxyethylene phytostanol and the like. Among these phytosterols or derivatives thereof, phytosterol is preferable.

Among the grinding aids, amino acids include N-acyl amino acids such as N-lauroyl-L-lysine and amino acids such as theanine.

Furthermore, examples of fatty acids include saturated fatty acids such as lauric acid, myristic acid, palmitic acid and stearic acid and salts thereof, and unsaturated fatty acids such as oleic acid and salts thereof.

On the other hand, as the metal oxide used in the production of the metal oxide composite high flat cellulose powder of the present invention, it can be used in general cosmetics as long as it is blended as a powder component such as extender pigment or colored pigment. It can be used without any particular restrictions. Examples of the metal oxide include iron oxide, titanium oxide, zinc oxide, cerium oxide and the like. These metal oxides can also be used singly or in combination of two or more.

The particle diameter of the metal oxide is preferably 10 to 10,000 nm, but some of the effects obtained will differ depending on the average particle diameter on the obtained metal oxide composite high flat cellulose powder. In view of this point, it is desirable to select the particle size of the raw metal oxide.

In the production of the metal oxide composite high flattened cellulose powder of the present invention, the amount of the grinding aid added to the whole of the above components is 0.5 to 5%, preferably 1 to 3%. . The total amount of metal oxide is 5 to 50%, preferably 20 to 40%.

These pulverization aids and metal oxides can be added to the cellulosic material at any time before the pulverization treatment, and the addition method can be added separately even if the pulverization aid and metal oxide are added simultaneously. May be added. Furthermore, as a method for adding the grinding aid, it may be dissolved in a suitable solvent and then added to the cellulosic material. Examples of the solvent used for dissolving the grinding aid include alkanes such as hexane, alcohols such as ethanol, ketones such as acetone, ethers such as tetrahydrofuran, aromatic hydrocarbons such as toluene, and the like.

In the process of mechanically pulverizing the mixture of the cellulose-based substance, the pulverization aid and the metal oxide, it is necessary to continuously apply the pressure and shear force due to the pulverization for a certain period of time. Therefore, it is preferable to use a pulverizing apparatus such as a vibration ball mill, a rotating ball mill, a planetary ball mill, a roll mill, a media mill, a disk mill, a high-speed mixer using high-speed rotating blades, a homomixer, etc., and a planetary ball mill is particularly preferable. The pulverization method is preferably dry pulverization without using a solvent. Note that the crushing energy applied in the crushing process (in the case of a planetary ball mill, the gravitational acceleration applied to the planetary ball mill) is 3 to 20 G, preferably 5 to 15 G.

In addition, the particle size, thickness, and flatness (aspect ratio) of the metal oxide composite high flattened cellulose powder are important. Since the diameter is also important depending on the application, the pulverization time must be determined in consideration of these. This relationship is related to the target flat cellulose itself, the particle size of the metal oxide as a raw material, and the like, so it is desirable to experimentally determine pulverization conditions, pulverization time, and the like in advance.

Next, a preferred embodiment for obtaining the metal oxide composite high flat cellulose powder of the present invention will be shown. First, the purified cellulose pulp-derived cellulose powder is dried under reduced pressure at 30 to 50 ° C. to sufficiently remove the adsorbed moisture to 0.1% or less. This cellulose powder is put into a sealable alumina or zirconia grinding container together with alumina or zirconia grinding balls, and further, a grinding aid and a metal oxide powder are added so as to have the above amount with respect to the cellulose powder. Added. Thereafter, the pulverization container is placed in a planetary ball mill, and pulverization is performed at a rotational speed of 100 to 250 rpm. The pulverization treatment may be repeated for about 2 to 72 cycles continuously, with 5 to 15 minutes of pulverization-5 to 15 minutes of rest, or for about 5 to 120 minutes without interruption. May be.

In addition, after the pulverization treatment, moisture adhering to the metal oxide composite high flattened cellulose powder may be further removed by a known drying means such as air drying, hot air drying, vacuum drying, and reduced pressure drying.

The metal oxide composite high flattened cellulose powder obtained as described above has, for example, an average particle diameter of 1 to 50 μm, preferably 5 to 40 μm, and an average thickness of 0.1 to 10 μm, preferably 0. It has a flake shape of 2 to 2 μm and a flatness of 4 to 200, preferably 10 to 100. Here, the average particle size is the average value of the width and length of the flat cellulose particles measured in a dispersion state in ethanol using a particle size distribution measuring device such as a laser diffraction / scattering type particle size distribution measuring device. (Particle size value of 50% cumulative volume). In addition, the average thickness refers to a value obtained by selecting a plurality of particles having the same size as the average particle size obtained above with an electron microscope such as a scanning electron microscope, measuring the thickness, and averaging the values. Say. Further, the flatness is the average particle diameter / average thickness determined as described above. The particle size of the composite metal oxide can also be measured with a scanning electron microscope.

As described above, the metal oxide composite high flat cellulose powder obtained in this way has a particle size of the metal oxide that is firmly adhered and composited more than 100 nm and not more than 1000 nm (pigment grade size). In some cases, this is a case of 10 to 100 nm (fine particle size), and the properties are slightly different, and the applications are also different. That is, when the composite metal oxide is a fine particle class, an extremely excellent UV blocking effect and uniformity of the decorative film can be obtained. Further, when the composite metal oxide is a pigment grade, excellent color developability can be obtained. Since the particle size of the metal oxide hardly changes before and after the compounding, the particle size of the metal oxide added before the compounding and the particle size of the metal oxide after the compounding are almost the same.

And since this metal oxide composite high flat cellulose powder also has the smooth feeling of use originally possessed by the high flat cellulose powder, the cosmetic compounded with this has an excellent cosmetic film. It has a uniform and smooth use feeling, an excellent UV blocking effect and a color developing effect, and also has an excellent makeup sustaining effect such as no color sink.

The resulting metal oxide composite high flattened cellulose powder has a thin flake shape compared to the conventional extender pigments talc and sericite, and has excellent properties such as transparency, softness, elongation, and natural gloss. In addition, since it has excellent affinity with the oil used, and has excellent UV blocking effect and coloring effect, specifically, as cosmetics that can use this, many cosmetics that use powder Examples thereof include various cosmetics such as basic (skin care) cosmetics, makeup cosmetics, sunscreen cosmetics, hair cosmetics, and the like. Particularly, it is effective and preferable to use in powder cosmetics such as powder foundation, liquid foundation, eye shadow, cheek red, powdered white powder and the like and sunscreens, cosmetics requiring UV blocking effect such as makeup base.

Preparation of a cosmetic compounded with the metal oxide composite high flattened cellulose powder of the present invention is carried out by combining it with a suitable cosmetic base and formulating it. For example, when the cosmetic is a powder cosmetic, the metal oxide composite high flatness of the present invention is used instead of a part or all of the conventional powder component in the same manufacturing method as that of the conventional powder cosmetic. Cellulose powder may be used. The blending amount of the metal oxide composite high flat cellulose powder in the cosmetic is 1 to 90%, preferably 5 to 90%, particularly preferably 5 to 70%.

In the above cosmetics, it is preferable to blend an oil component as a cosmetic base. There are no particular restrictions on the oily ingredients blended in this cosmetic, but for example, paraffin wax, ceresin wax, ozokerite, microcrystalline wax, montan wax, fisher trops wax, polyethylene wax, liquid paraffin, squalane, petrolatum, Hydrocarbons such as polyisobutylene and polybutene, natural waxes such as carnauba wax, beeswax, lanolin wax and candelilla, glyceryl tribehenate, rosin acid pentaerythritol ester, jojoba oil, cetyl isooctanoate, isopropyl myristate, trioctanoic acid Esters such as glyceryl, diglyceryl triisostearate, dipentaerythritol fatty acid esters, fatty acids such as stearic acid, behenic acid, 12-hydroxystearic acid Higher alcohols such as cetanol, stearyl alcohol and behenyl alcohol, oils and fats such as olive oil, castor oil, mink oil and owl, lanolin derivatives such as lanolin fatty acid isopropyl and lanolin alcohol, N-lauroyl L-glutamate di (cholesteryl and behenyl) -Amino acid derivatives such as octyldodecyl), fluorine oils such as perfluoropolyether, perfluorodecane, and perfluorooctane. These oily components can be used alone or in combination of two or more. The amount of the oily component to be blended with the cosmetic of the present invention is not particularly limited, but is preferably 0.1 to 25%.

Further, in the above cosmetics, conventional powder components, for example, inorganic powder such as talc and organic powder such as nylon can be blended. In this case, an inorganic powder or an organic powder may be added and dispersed together with the metal oxide composite high flat cellulose powder of the present invention, and oil may be added as necessary.

Furthermore, the above cosmetics include components used in normal cosmetics, for example, surfactants, oil gelling agents, water-soluble components such as polyhydric alcohols and humectants, and ultraviolet absorbers as necessary. In addition, preservatives, cosmetic ingredients, fragrances, and the like can be appropriately blended within a range not impairing the effects of the present invention.

The properties and dosage forms of the cosmetics are not particularly limited and can be selected according to the purpose. The properties of the cosmetic of the present invention may be any of liquid, powder, solid, emulsion, cream, gel and the like, and the dosage form is aqueous, oily, solubilized, in oil Any dosage form such as a water mold and an oil-in-water mold may be used.

The reason why the metal oxide composite high flattened cellulose powder of the present invention described above has much superior performance compared to conventional metal oxide composite particles is that the metal oxide is very fine, This is presumed to be due to the fact that it is combined with the highly flat cellulose powder in the form. That is, FIGS. 1 to 3 are obtained by observing the surface of the product 6 obtained in Example 6 with a scanning electron microscope. In FIG. 1 where the magnification is about 10,000 times, the fine zinc oxide is completely observed. Can not. However, when the magnification is increased to 50,000 times, fine zinc oxide begins to appear white on the surface, and at a magnification of 200,000, fine zinc oxide of about 20 nm is observed on the mother powder. Since the original particle size of the fine particle zinc oxide is about 20 nm, this result shows that the fine particle zinc oxide does not aggregate on the surface of the metal oxide composite high flat cellulose powder of the present invention, and is relatively primary particles. It can be understood that it is compounded in the state of. That is, on the metal oxide composite high flattened cellulose powder, the presence of the metal oxide in a primary particle state that can exert its action to the maximum is considered to be the reason that the performance is remarkably improved.

As described above, in the metal oxide composite high flat cellulose powder of the present invention, the reason why the metal oxide is composited in a primary particle state is not yet clear. Since the fine metal oxide powder is present on the spot where it is formed and stirred with a high share, it adheres on the cellulose surface just preferentially formed and has a strong bond. It is understood that there is not.

Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited to these examples.

Example 1
Production of Lauroyllysine-treated Fine Titanium Oxide Composite High Flat Cellulose Powder (1):
(1) As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). In addition, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co., Inc.), fine particle titanium oxide (TTO-S-4 Ishihara Sangyo Co., Ltd.) (particle diameter minor axis: 10 to 20 nm, major axis: 50 to 100 nm) 14 g was added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, lauroyllysine-treated fine titanium oxide composite high flat cellulose powder. (Product 1) was obtained.

(2) The average particle diameter, thickness, and flatness of the product 1 were measured as follows. That is, using a laser diffraction / scattering type particle size distribution measuring apparatus (Horiba: LA-920), the average particle diameter (width and length on the apparatus of the width and length) of the obtained powder in a dispersed state in ethanol in a flow cell. The average value was determined. As the average particle size, a particle size value with an integrated volume of 50% was used. In the particle size distribution measurement, a suspension in which 50 mg of the obtained powder was dispersed in 10 mL of ethanol was dropped into a sample circulation tank using ethanol as a medium in the particle size distribution measurement device, and after reaching an appropriate concentration. It was measured. As a result, the average particle size of the powder was 16 μm.

The average thickness of the obtained particles was determined by directly observing the particles using a scanning electron microscope (S-2150, manufactured by Hitachi, Ltd.) and selecting a plurality of particles having a size equivalent to the average particle size obtained above. The thickness was measured and averaged. In observation with a scanning electron microscope, a very small amount of the obtained powder was placed on a sample stage of a scanning electron microscope, dried under reduced pressure, and platinum was deposited to obtain a spectroscopic sample. From the image obtained by observing the microscopic sample at an acceleration voltage of 10 to 25 kV and an enlargement ratio of 500 to 10,000 times, the thickness of particles having a size equivalent to the average particle size measured above was measured, The average thickness was determined from them. As a result, the average thickness was 1.7 μm.

As a result, the product 1 has an average particle diameter of 16 μm, an average thickness of 1.7 μm, and a flat cellulose particle (lauroyllysine-treated fine particle titanium oxide composite) having a flatness (average particle diameter / average thickness) of 9.4. Flat cellulose powder). Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 2
Production of Lauroyllysine-treated Fine Titanium Oxide Composite High Flat Cellulose Powder (2):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co.) and 28 g of fine titanium oxide (TTO-S-4 Ishihara Sangyo Co., Ltd.) were added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, lauroyllysine-treated fine titanium oxide composite high flat cellulose powder. (Product 2) was obtained.

The obtained product 2 was measured for average particle size, thickness and flatness in the same manner as in Example 1 (2). The average particle size was 15 μm, the average thickness was 1.0 μm, and the flatness (average) The particle size / average thickness was 15 flat. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 3
Production of hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder (3):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 14 g of fine particle titanium oxide (TTO-S-4 manufactured by Ishihara Sangyo Co., Ltd.) were added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder A body (product 3) was obtained.

The obtained product 3 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 16 μm, the average thickness was 1.9 μm, and the flatness (average) The particle size / average thickness was 8.4. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 4
Production of hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder (4):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 28 g of fine particle titanium oxide (TTO-S-4 manufactured by Ishihara Sangyo Co., Ltd.) were added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder A body (product 4) was obtained.

The obtained product 4 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 15 μm, the average thickness was 1.2 μm, and the flatness (average) The particle size / average thickness was 12.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 5
Production of Ceramide-treated Fine Titanium Oxide Composite High Flat Cellulose Powder (5):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) and 28 g of fine particle titanium oxide (TTO-S-4 Ishihara Sangyo Co., Ltd.) were added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)), and ceramide-treated fine particle titanium oxide composite high flat cellulose powder ( Product 5) was obtained.

The obtained product 5 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 16 μm, the average thickness was 1.2 μm, and the flatness (average) The particle size / average thickness was 13.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 6
Production of Lauroyllysine-treated Fine Zinc Oxide Composite High Flat Cellulose Powder (6):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). Further, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co., Inc.) and 14 g of fine zinc oxide (ZnO-610, Sumitomo Osaka Cement Co., Ltd.) (average particle size 20 nm) were added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, lauroyllysine-treated fine zinc oxide composite high flat cellulose powder. (Product 6) was obtained.

For the obtained product 6, the average particle diameter, thickness and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 16 μm, the average thickness was 1.7 μm, and the flatness (average) The particle size / average thickness was 9.4. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 7
Production of Lauroyllysine-treated Fine Zinc Oxide Composite High Flat Cellulose Powder (7):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co.) and 28 g of fine zinc oxide (ZnO-610, Sumitomo Osaka Cement Co., Ltd.) were added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, lauroyllysine-treated fine zinc oxide composite high flat cellulose powder. (Product 7) was obtained.

The obtained product 7 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 15 μm, the average thickness was 1.0 μm, and the flatness (average) The particle size / average thickness was 15 flat. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 8
Production of hydrogenated lecithin-treated fine zinc oxide composite high flat cellulose powder (8):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 28 g of fine zinc oxide (ZnO-610 manufactured by Sumitomo Osaka Cement) were added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)), and hydrogenated lecithin-treated fine zinc oxide composite high flat cellulose powder. A body (product 8) was obtained.

The obtained product 8 was measured for average particle size, thickness and flatness in the same manner as in Example 1 (2). The average particle size was 15 μm, the average thickness was 1.2 μm, and the flatness (average) The particle size / average thickness was 12.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 9
Production of Ceramide-treated Fine Zinc Oxide Composite High Flat Cellulose Powder (9):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) and 28 g of fine particle zinc oxide (ZnO-610, Sumitomo Osaka Cement Co., Ltd.) were added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)), and ceramide-treated fine zinc oxide composite high flat cellulose powder ( Product 9) was obtained.

The obtained product 9 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 15 μm, the average thickness was 1.2 μm, and the flatness (average) The particle size / average thickness was 12.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 10
Production of hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder (10):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 14 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) (average particle size 250 nm) were added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (about 10 G (gravity acceleration) grinding energy), and hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder. (Product 10) was obtained.

The obtained product 10 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 18 μm, the average thickness was 2.2 μm, and the flatness (average) The particle size / average thickness was 8.2. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 11
Production of hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder (11):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 28 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) were added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (about 10 G (gravity acceleration) grinding energy), and hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder. (Product 11) was obtained.

The obtained product 11 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 17 μm, the average thickness was 1.5 μm, and the flatness (average) The particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 12
Production of ceramide-treated titanium oxide composite high flat cellulose powder (12):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). Furthermore, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries) and 14 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) were added. After that, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, ceramide-treated titanium oxide composite high flat cellulose powder (product) 12) was obtained.

For the obtained product 12, the average particle diameter, thickness and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 18 μm, the average thickness was 2.2 μm, and the flatness (average) The particle size / average thickness was 8.2. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 13
Production of ceramide-treated titanium oxide composite high flat cellulose powder (13):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries) and 28 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) were added. After that, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, ceramide-treated titanium oxide composite high flat cellulose powder (product) 13) was obtained.

The obtained product 13 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 17 μm, the average thickness was 1.5 μm, and the flatness (average) The particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 14
Production of Ceramide-treated Titanium Oxide / Iron Oxide Composite High Flat Cellulose Powder (14):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, 41.3 g (59%) of cellulose powder from which adsorbed moisture has been sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C. is placed in an alumina crushing container (capacity 500 mL) in an alumina crushing ball. In addition, 0.7 g (1%) of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.), 21 g (30%) of titanium oxide (manufactured by TITANIX JR-800 Teika) (average particle size 270 nm), red 0.875 g (1.25%) of iron oxide (Tarox R-516P made by Titanium Industry Co., Ltd.) (average particle diameter minor axis: 80 nm, major axis: 800 nm), yellow iron oxide (Tarox synthetic iron oxide YP1200P made by Titanium Industry Co., Ltd. ) (Average particle diameter minor axis: 90 nm, major axis: 900 nm) was added in an amount of 6.125 g (8.75%). Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)), and ceramide-treated titanium oxide / iron oxide composite high flat cellulose powder. A body (product 14) was obtained.

The obtained product 14 was measured for average particle size, thickness and flatness in the same manner as in Example 1 (2). The average particle size was 17 μm, the average thickness was 1.5 μm, and the flatness (average) The particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 15
Production of Ceramide-treated Titanium Oxide / Iron Oxide Composite High Flat Cellulose Powder (15):
In the same manner as in Example 14, purified wood pulp-derived cellulose powder (W-400G) 59%, ceramide (Ceramide II) 1%, titanium oxide (TITANIX JR-800) 38.2%, red iron oxide ( A ceramide-treated titanium oxide / iron oxide composite high flat cellulose powder (Product 15) was obtained using 0.45% of Tarox R-516P) and 1.35% of yellow iron oxide (Tarox synthetic iron oxide YP1200P).

The obtained product 15 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 17 μm, the average thickness was 1.5 μm, and the flatness (average) The particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 16
Manufacture of stearic acid-treated titanium oxide / iron oxide composite high flat cellulose powder (16):
In the same manner as in Example 14, 57% of purified wood pulp-derived cellulose powder (W-400G), 3% of stearic acid instead of ceramide, 38.2% of titanium oxide (TITANIX JR-800), red iron oxide (Tarox R-516P) 0.45% and yellow iron oxide (Tarox synthetic iron oxide YP1200P) 1.35% were used to obtain stearic acid-treated titanium oxide / iron oxide composite high flat cellulose powder (Product 16). It was.

The obtained product 16 was measured for the average particle size, thickness and flatness in the same manner as in Example 1 (2). The average particle size was 17 μm, the average thickness was 1.1 μm, and the flatness (average) The particle size / average thickness was 15.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 17
Production of Ceramide-treated Titanium Oxide / Iron Oxide Composite High Flat Cellulose Powder (17):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. In addition, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries), 25.9 g of titanium oxide (TITANIX JR-800 Teika), and 0 of red iron oxide (Tarox R-516P made by Titanium Industry Co., Ltd.) .525 g, 1.575 g of yellow iron oxide (Tarox synthetic iron oxide YP1200P manufactured by Titanium Industry Co., Ltd.) was added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)), and ceramide-treated titanium oxide / iron oxide composite high flat cellulose powder. A body (product 17) was obtained.

The obtained product 17 was measured for the average particle size, thickness and flatness in the same manner as in Example 1 (2). The average particle size was 17 μm, the average thickness was 1.5 μm, and the flatness (average) The particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Comparative Example 1
Manufacture of ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (1):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) was added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) to obtain a ceramide-treated flat cellulose powder. Next, the obtained ceramide-treated high flattened cellulose powder (60 g), 30 g of titanium oxide (manufactured by TITANIX JR-800 Teika), 1.25 g of red iron oxide (Tarox R-516P manufactured by Titanium Industry Co., Ltd.), yellow oxide Iron (Tarox synthetic iron oxide YP1200P manufactured by Titanium Industry Co., Ltd.) 8.75 g was mixed for 10 minutes with a Henschel mixer (Mitsui Miike Co., Ltd.), and ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (Comparative product 1) Got.

About the obtained comparative product 1, the average particle diameter, thickness, and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 19 μm, the average thickness was 1.4 μm, and the flatness ( The average particle diameter / average thickness was 13.6.

Comparative Example 2
Manufacture of ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (2):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) was added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, a ceramide-treated high flat cellulose powder was obtained. Next, the obtained ceramide-treated flat cellulose powder (60 g), 37 g of titanium oxide (manufactured by TITANIX JR-800 Teika Co., Ltd.), 0.75 g of red iron oxide (manufactured by Tarox R-516P Titanium Industry Co., Ltd.), yellow iron oxide 2.25 g (Tarox synthetic iron oxide YP1200P made by Titanium Industry Co., Ltd.) was mixed for 10 minutes with a Henschel mixer (Mitsui Miike Co., Ltd.), and a ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (Comparative product 2) Obtained.

The obtained comparative product 2 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 19 μm, the average thickness was 1.4 μm, and the flatness ( The average particle diameter / average thickness was 13.6.

Comparative Example 3
Production of Lauroyllysine-treated High Flat Cellulose Powder / Fine Particle Titanium Oxide Mixture (3):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co.) was added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) to obtain a lauroyllysine-treated high flat cellulose powder. Next, the obtained lauroyllysine-treated flat cellulose powder (60 g) and fine particle titanium oxide (TTO-S-4 manufactured by Ishihara Sangyo Co., Ltd.) (12 g) were mixed with a Henschel mixer (manufactured by Mitsui Miike Co., Ltd.) for 10 minutes. A lauroyllysine-treated high flat cellulose powder / fine particle titanium oxide mixture (Comparative Product 3) was obtained.

About the obtained comparative product 3, the average particle diameter, thickness, and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 19 μm, the average thickness was 1.4 μm, and the flatness ( The average particle diameter / average thickness was 13.6.

Comparative Example 4
Production of Lauroyllysine-treated High Flat Cellulose Powder / Fine Particle Zinc Oxide Mixture (4):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co.) was added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) to obtain a lauroyllysine-treated high flat cellulose powder. Next, the obtained lauroyllysine-treated flat cellulose powder (60 g) and fine particle zinc oxide (ZnO-610, manufactured by Sumitomo Osaka Cement Co., Ltd.) (12 g) were mixed with a Henschel mixer (manufactured by Mitsui Miike Co., Ltd.) for 10 minutes. A mixture (comparative product 4) of lauroyllysine-treated high flat cellulose powder and fine zinc oxide was obtained.

About the obtained comparative product 4, the average particle diameter, thickness, and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 19 μm, the average thickness was 1.4 μm, and the flatness ( The average particle diameter / average thickness was 13.6.

Comparative Example 5
Production of hydrogenated lecithin-treated high flattened cellulose (5):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) was added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding for 40 minutes at a rotation speed of 200 rpm (about 10 G (gravity acceleration) grinding energy), hydrogenated lecithin treated high flat cellulose powder (comparative product) 5) was obtained.

The obtained comparative product 5 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 19 μm, the average thickness was 1.4 μm, and the flatness ( The average particle diameter / average thickness was 13.6.

Comparative Example 6
Titanium oxide / iron oxide composite cellulose powder (6):
60% by mass of refined wood pulp-derived cellulose powder (W-400G) was put in a planetary ball mill (Misho Industry Co., Ltd.), and 38.2% titanium oxide (TITANIX JR-800), red iron oxide ( Add 0.45% of Tarox R-516P) and 1.35% of yellow iron oxide (Tarox synthetic iron oxide YP1200P), and crush for 40 minutes at a rotation speed of 200 rpm (crushing energy of about 10 G (gravity acceleration)). Then, a titanium oxide / iron oxide composite cellulose powder (Comparative Product 6) was obtained.

The obtained comparative product 6 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 18 μm, the average thickness was 2.0 μm, and the flatness ( The average particle size / average thickness was 9.0. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Comparative Example 7
Polysiloxane-treated titanium oxide / iron oxide composite sericite (7):
60% by mass of dimethylpolysiloxane 3% -treated sericite (SA sericite FSE; manufactured by Miyoshi Kasei Co., Ltd.) is placed in a planetary ball mill (Misho Industry Co., Ltd.), and titanium oxide (TITANIX JR-800) is added to 38 0.2%, 0.45% red iron oxide (Tarox R-516P) and 1.35% yellow iron oxide (Tarox synthetic iron oxide YP1200P) were added, and the grinding energy was 200rpm (about 10G (gravity acceleration)) ) For 40 minutes to obtain polysiloxane-treated titanium oxide / iron oxide composite sericite (Comparative Product 7).

For the obtained comparative product 7, the average particle diameter, thickness and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 7.0 μm, the average thickness was 1.0 μm, and the flatness was measured. The degree (average particle diameter / average thickness) was 7.0. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Comparative Example 8
Polysiloxane-treated titanium oxide / iron oxide composite talc (8):
60% by mass of dimethylpolysiloxane 2% treated talc (SA talc JA-68R; manufactured by Miyoshi Kasei Co., Ltd.) is placed on a planetary ball mill (Misho Industry Co., Ltd.), and titanium oxide (TITANIX JR-800) is added to 38 0.2%, 0.45% red iron oxide (Tarox R-516P) and 1.35% yellow iron oxide (Tarox synthetic iron oxide YP1200P) were added, and the grinding energy was 200rpm (about 10G (gravity acceleration)) ) For 40 minutes to obtain polysiloxane-treated titanium oxide / iron oxide composite talc (Comparative Product 8).

The obtained comparative product 8 was measured for the average particle diameter, thickness, and flatness in the same manner as in Example 1 (2). The average particle diameter was 7.0 μm, the average thickness was 0.7 μm, and the flatness was measured. The degree (average particle diameter / average thickness) was 10.0 flat. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.

Example 18
UV blocking test (1):
The UV blocking ability of the finely divided titanium oxide composite high flat cellulose powder (Product 1 and Product 2) produced in Examples 1 and 2 was examined. In the experiment, 0.04 g of each powder was uniformly applied to a transpore tape (5 cm × 8 cm) so as to be 1 mg / cm ^2, and the UV blocking ability in the region of 300 to 450 nm was measured with an SPF analyzer (manufactured by Sanyo Trading Co., Ltd.). ). For comparison, comparative product 3 was used. The results are shown in Table 1.

As shown in Table 1, the products 1 and 2 of the present invention have an SPF value of about 5 times higher than that of the high flat cellulose powder mixed with fine particle titanium oxide (Comparative Product 3), and have a UV blocking ability. It was an excellent powder.

Example 19
UV blocking test (2):
The UV blocking ability of the fine zinc oxide composite high flat cellulose powder (Products 6 to 9) produced in Examples 6 to 9 was examined in the same manner as in Example 18. For comparison, the comparative product 4 was used. The results are shown in Table 2.

As shown in Table 2, the product 6 of the present invention has an SPF value that is about twice or more higher than that of the highly flat cellulose powder mixed with fine zinc oxide (Comparative Product 4). About 3 times higher, the powder of the present invention was excellent in UV blocking ability.

Example 20
Color change test:
The powders prepared in Examples 15 and 16 and Comparative Examples 6 to 8 were tested for color change.

First, each powder was thoroughly mixed with the same weight of oil (glyceryl tri-2-ethylhexanoate) with a spatula to prepare a test sample. After filling this test sample and the produced powder itself into a glass cell, the color value (a value; redness / b value; yellowness) is measured with a spectral color difference meter SE-2000 (manufactured by Nippon Denshoku Kogyo Co., Ltd.). ) Respectively.

Among these color values, the difference (Δa and Δb) between the a value (a1) and b value (b1) of the pigment itself and the a value (a2) and b value (b2) of the pigment mixed with the oil component, respectively. Further, from this value, the whole color change property was obtained by the following equation. Based on this color change property, the color change property was evaluated according to the following criteria. The results are shown in Table 3.

Color changeability = √ ((Δa) ² + (Δb) ² )
However, Δa means the difference between a1 and a2, and Δb means the difference between b1 and b2.

( Evaluation criteria )
Color change: Evaluation 0 or more and 1.5 or less: ◎
More than 1.5 and less than 2.0: ○
Over 2.0 and under 2.5: △
Over 2.5 ~: ×

As shown in Table 3, the product 15 and the product 16 of the present invention were excellent with little color change even when mixed with oil. In contrast, even if the mixing amount of titanium oxide and iron oxide is the same, comparative product 6 without using a grinding aid, comparative product 7 in which dimethylpolysiloxane-treated sericite is the base powder, dimethylpolysiloxane-treated talc Comparative product 8, which is a mother powder, was greatly inferior in color change when mixed with oil.

Example 21
Powder foundation (1):
Using the finely divided titanium oxide composite high flattened cellulose powders (Products 1 to 5) produced in Examples 1 to 5, powder foundations of the cosmetics 1 to 5 of the present invention were prepared by the formulation shown in Table 4 and the following method. About this powder foundation, UV blocking ability, SPF value, uniformity of makeup film, natural finish (no whitening), makeup lasting, stability (presence of aggregates), and feeling of use (when applying) Smoothness). As a comparison, fine titanium oxide-coated mica (mica 58.5%, titanium oxide 40%, iron oxide 1.5%) (manufactured by SPS-LTF Teica) (comparative cosmetic 1) and high flatness A mixture (comparative cosmetic 2) using a mixture of cellulose powder and fine particle titanium oxide (Comparative Product 3) was used. The results are also shown in Table 4.

( Production method )
Ingredients 1-18 are mixed in a Henschel mixer for 10 minutes, then ingredients 19-23 are added and stirred for 5 minutes. Then, it grind | pulverizes with an atomizer (1HP screen diameter 1.5mmphi), and it fills with a resin dish, and obtains a powder foundation.

( Test method )
UV blocking ability and SPF value:
The UV blocking ability of the powder foundations produced with the cosmetics 1 to 5 of the present invention and the comparative cosmetics 1 and 2 was examined. In the experiment, 0.04 g of each powder was uniformly applied to a transpore tape (5 cm × 8 cm) so as to be 1 mg / cm ^2, and the UV blocking ability in the region of 300 to 450 nm was measured with an SPF analyzer (Sanyo Trading Co., Ltd.). ). In addition, evaluation was implemented by the following determination.

Evaluation content A: SPF is 25 or more.
○: SPF is 20 or more and less than 25.
Δ: SPF is 15 or more and less than 20.
X: SPF is less than 15.

“Makeup uniformity”, “Natural finish (no whitening)”, “Make-up (no adhesion and no color change)” and “Usage”:
Twenty panelists specializing in cosmetics evaluation use the powder foundations of the cosmetics 1 to 5 of the present invention and the comparative cosmetics 1 and 2, and “uniformity of the cosmetic film” and “natural finish (no whitening)” Each of the samples was evaluated on a 7-point scale according to the following evaluation criteria for “make-up holding (no adhesion and no color change)” and “use feeling”, and a score was assigned to each sample. Next, each product was determined from the average score of all panels according to the following criteria. The “use feeling” was evaluated by the smoothness at the time of application.

Evaluation criteria;
(Evaluation): (Contents)
6: Very good 5: Good 4: Somewhat good 3: Normal 2: Somewhat bad 1: Bad 0: Very bad

Judgment criteria;
(Average score): (Judgment)
5.0 or more: ◎ (very good)
3.5 or more and less than 5.0: ○ (good)
1.5 or more and less than 3.5: △ (somewhat poor)
Less than 1.5: × (defect)

Stability (with or without aggregates):
Stability was evaluated by the presence or absence of aggregates. For the powder foundations of the cosmetics 1 to 5 of the present invention and the comparative cosmetics 1 and 2 molded on a resin dish, the surface state after 20 times of surface coating was visually observed using a cosmetic sponge. In addition, evaluation was implemented by the following determination.

Evaluation content A: Aggregates are not observed.
○: Aggregates are observed, but the amount is small.
Δ: Agglomerates are observed and the amount is large.
X: Large aggregates are observed and the amount is large.

As shown in Table 4, the powder foundations of the cosmetics 1 to 5 of the present invention have a high SPF value, excellent UV blocking ability, uniformity of the cosmetic film, natural finish (no whitening), long-lasting makeup ( The powder foundation was excellent in all the items of adhesion and no color change), stability (presence / absence of aggregates), and feeling of use (smoothness during application).

On the other hand, the powder foundation of the comparative cosmetic 1 in which the product 1 of the cosmetic 1 of the present invention is replaced with the conventional fine particle titanium oxide composite mica shows agglomeration of the powder, and the uniformity of the cosmetic film, the natural finish, etc. It was inferior. Moreover, the powder foundation of the comparative cosmetic 2 in which the product 1 of the cosmetic 1 of the present invention is replaced with the comparative product 3 has a low SPF value, inferior UV blocking ability, and a feeling of use (smoothness during application). Was inferior.

Example 22
Powder foundation (2):
Using the fine zinc oxide composite high flat cellulose powder produced in Examples 6 to 9, powder foundations of the cosmetics 6 to 9 of the present invention were prepared according to the formulation shown in Table 5 and the following method. About this powder foundation, it carried out similarly to Example 21, and investigated UV blocking ability, SPF value, the uniformity of a cosmetic film, the natural finish (no powder whiteness), makeup lasting, usability, and stability. For comparison, a product using a zinc oxide-coated mica / barium sulfate composite (mica 40%, zinc oxide 50%, barium sulfate 10%) (manufactured by RONAFAIR SHADELEAF A Merck) (comparative cosmetic 3) and high A product (comparative cosmetic 4) using a mixture of flat cellulose powder and fine zinc oxide (Comparative product 4) was used. The results are also shown in Table 5.

( Production method )
Ingredients 1-17 are mixed in a Henschel mixer for 10 minutes, then ingredients 18-22 are added and stirred for 5 minutes. Then, it grind | pulverizes with an atomizer (1HP screen diameter 1.5mmphi), and it fills with a resin dish, and obtains a powder foundation.

As shown in Table 5, the powder foundation of the cosmetics 6 to 9 of the present invention has a high SPF value, excellent UV blocking ability, uniformity of the cosmetic film, natural finish (no whitening), long-lasting makeup, The powder foundation was excellent in all items of stability (presence / absence of aggregates) and feeling of use (smoothness during application).

On the other hand, the powder foundation of the comparative cosmetic 3 in which the product 6 of the cosmetic 6 of the present invention is replaced with the fine particle zinc oxide-coated mica / barium sulfate composite powder shows agglomeration of the powder, uniformity of the cosmetic film and natural The finish was inferior. In addition, the powder foundation of the comparative cosmetic 4 in which the product 6 of the cosmetic 6 of the present invention is replaced with the comparative product 4 has a low SPF value, inferior UV blocking ability, and a feeling of use (smoothness during application). Was inferior.

Example 23
Powder foundation (3):
Using the titanium oxide composite high flattened cellulose powders (Products 10 to 13) produced in Examples 10 to 13, powder foundations of the cosmetics 10 to 13 of the present invention were prepared by the formulation shown in Table 6 and the following method. The powder foundation was examined for concealment by the following method, and in the same manner as in Example 21, the uniformity of the cosmetic film, the cosmetic durability and the feeling of use were examined. For comparison, high-flat cellulose powder and titanium oxide (comparative cosmetics 5 and 6) were used separately. The results are also shown in Table 6.

( Production method )
Ingredients 1-16 are mixed in a Henschel mixer for 10 minutes, then ingredients 17-19 are added and stirred for 2 minutes. Then, it grind | pulverizes with an atomizer (1HP screen diameter 1.5mmphi), and it fills with a resin dish, and obtains a powder foundation.

( Test method )
Concealment:
20 panelists specializing in cosmetics evaluation use the powder foundations of the present cosmetics 10 to 13 and comparative cosmetics 5 and 6, and each of them evaluates the “concealment” in 7 levels according to the following evaluation criteria. A rating was given. Next, each product was determined from the average score of all panels according to the following criteria.

As shown in Table 6, the powder foundation of the cosmetics 10 to 13 of the present invention is a powder foundation that is excellent in all items of uniformity of the cosmetic film, concealment, makeup lasting, and feeling of use (smoothness during application). It was.

On the other hand, the comparative cosmetic 5 in which the titanium oxide having almost the same mass as that of the cosmetic 10 of the present invention is mixed and mixed with other components without treatment is poor in dispersion of titanium oxide, has poor makeup, and has concealment and use. The feeling (smoothness during application) was also inferior. Moreover, although the comparative cosmetic 6 containing double amount of titanium oxide has a concealing property, the feeling of use (smoothness at the time of application), the uniformity of the cosmetic film, and the longevity of the makeup are poor.

Example 24
Powder foundation (4):
Using the titanium oxide / iron oxide composite high flattened cellulose powder (Products 14 and 15) produced in Examples 14 to 15, the powder foundations of the cosmetics 14 and 15 of the present invention were prepared by the formulation shown in Table 7 and the following method. . The powder foundation was examined for color development by the following method, and in the same manner as in Example 21, the uniformity of the cosmetic film, the cosmetic durability and the feeling of use were examined.

( Production method )
Ingredients 1-13 are mixed in a Henschel mixer for 10 minutes, then ingredients 14-16 are added and stirred for 3 minutes. Then, it grind | pulverizes with an atomizer (1HP screen diameter 1.5mmphi), and it fills with a resin dish, and obtains a powder foundation.

( Test method )
Color development:
20 panelists specializing in cosmetics evaluation use the powder foundations of the present cosmetics 14 to 15 and comparative cosmetics 7 and 8, and each of them evaluates their “color development” in 7 stages according to the following evaluation criteria. Was given a score. Next, each product was determined from the average score of all panels according to the following criteria.

As shown in Table 7, the powder foundations of the cosmetics 14 and 15 of the present invention are powder foundations that are excellent in all items of uniformity of the cosmetic film, concealment, makeup lasting, and feeling of use (smoothness during application). It was.

On the other hand, comparative cosmetics 7 and 8 containing a mixture of titanium oxide or iron oxide mixed with cellulose powder had particularly poor color development and long lasting makeup.

Example 25
Powder foundation (5):
Using the fine zinc oxide composite high flat cellulose powder (Product 7) produced in Example 7, a powder foundation of the cosmetic 16 of the present invention was prepared according to the formulation shown in Table 8 and the following method. For this powder foundation, the SPF value was determined by the following method, and in the same manner as in Example 21, UV blocking ability, uniformity of the cosmetic film, natural finish (no whitening), makeup retention, stability (of aggregates) Existence) and usability (smoothness during application) were examined. For comparison, a cosmetic (comparative cosmetic 9) using the flat cellulose powder of Comparative Example 4 and a fine particle zinc oxide mixture was used. The results are shown in Table 8.

( Production method )
A: Components 1 to 12 are mixed with a Henschel mixer for 10 minutes.
B: Components 13 to 18 are added to A and mixed for 4 minutes.
C: B is pulverized with an atomizer (1HP screen diameter 1.5 mmφ).
D: 60 parts of light liquid paraffin and 100 parts of C are mixed, filled in a resin dish, dried at 70 ° C. to obtain a powder foundation.

(Measured SPF value)
Evaluation was made by the following method based on “SPF measurement method standard (2007 revised version)” established by the Japan Cosmetic Industry Association.

First, 10 subjects were selected from healthy men and women aged 18 to 60 who fall under Fitzpatrick skin types I, II, and III (however, they were interviewed and those with photosensitivity or light on the skin) (Except for those who take drugs related to sensitivity (such as anti-inflammatory drugs, antihypertensive drugs)). Moreover, as a test site | part, the site | part which is a test subject's back, and there is no pigmentation, a nevus, etc. and the skin color was substantially uniform was selected. A test sample was applied to 50 cm ^{2 of} this test site. The coating amount was 2.00 mg / cm ² ± 2.5% / cm ² .

The test sample application site of the subject was irradiated with ultraviolet rays using a xenon arc solar simulator (manufactured by SOLAR LIGHT) as a light source. This xenon arc simulator has a continuous spectrum similar to that of sunlight in the UV-B and UV-A regions with wavelengths of 290 to 400 nm. Further, ultraviolet rays having a wavelength of 290 nm or less were removed as much as possible using a filter.

16 to 24 hours after irradiation with ultraviolet rays, the occurrence of erythema at the site irradiated with ultraviolet rays was examined in a sufficiently bright room. The minimum amount of ultraviolet irradiation that initially causes slight erythema with a clear boundary at 2/3 or more of the irradiated region was defined as the minimum erythema dose (MED). Using the MED at the test sample application part and the non-application part, respectively, the SPF value of each subject was determined by the following formula, and this was arithmetically averaged to obtain the measured SPF value.

SPF value = MED (sample application part) / MED (sample non-application part)

As shown in Table 8, the powder foundation of the cosmetic 16 of the present invention has a higher SPF measured value than the comparative cosmetic 9, excellent UV blocking ability, uniformity of the cosmetic film, natural finish (powder whiteness) No powder), makeup lasting (no adhesion and no color change), stability (presence of agglomerates), and feeling of use (smoothness during application) were excellent powder foundations.

On the other hand, the powder foundation of the comparative cosmetic 9 in which the product 7 of the cosmetic 16 of the present invention is replaced with a lauroyl lysine-treated high flattened cellulose powder / particulate zinc oxide mixture has a slightly low SPF measured value and UV blocking ability, All items, such as a feeling of use (smoothness at the time of application | coating), were inferior.

Example 26
Powder foundation (6)
Using the pigments of the product 14 prepared in Example 14 and the product 15 prepared in Example 15, powder foundations were prepared by the following method according to the composition described in Table 9 below (Formulations 1 to 3). As a comparison, the one using iron oxide not subjected to special treatment was used (comparison prescription). In addition, as for the total amount of iron oxide in each prescription in a present Example, the composition 1 is the same amount (100%) as a comparison prescription, and the compositions 2 and 3 are 80% of a comparison prescription.

<Manufacturing method>
A: Components 1 to 13 are mixed with a Henschel mixer for 10 minutes.
B: Add components 14 to 20 to A and mix for 5 minutes.
C: B is pulverized with an atomizer (1HP screen diameter 1.5 mmφ).
D: 60 parts of light liquid paraffin and 100 parts of C are mixed, filled in a resin dish, molded and dried at 70 ° C. to obtain a powder foundation.

For each of the obtained compositions, “color development”, “long-lasting makeup (no color sink)”, and “long-lasting makeup (adhesion)” were examined. The makeup holding (adhesiveness) was examined in the same manner as in Example 21. In addition, for “color development”, each powder foundation in a state molded by the above manufacturing method, and for “makeup (no color sink)”, each powder foundation applied on the inner side of the upper arm, Each appearance color was evaluated by measuring a and b or L, a and b using a spectral color difference meter SE-2000 (manufactured by Nippon Denshoku Kogyo Co., Ltd.) and calculating as follows. The results are shown in Table 10.

Color development:
For each formulation, the measured a and b values were compared to the comparative formulation a and b values (as and bs) to determine the difference (Δa and Δb). After Δa and Δb were squared and added, the value was opened with a square root, and the value was used as an evaluation value of “color development”. For this evaluation value, 1 or more was evaluated as ◎, 0.5 or more and less than 1 as ◯, 0.25 or more and less than 0.5 as Δ, and less than 0.25 as ×.

Makeup (no color sink):
Immediately after application and 2 hours after application, the values of L, a, and b of the appearances of the present invention and comparative formulations were determined. The difference between the measured values immediately after application in each formulation and 2 hours after application (ΔL _0-2 , Δa _0-2 and Δb _0-2 ) was squared, and after adding them, the square root was opened. This value was used as an evaluation value for “long makeup (no color sinking)”. With respect to this evaluation value, 0 or more and 1 or less were evaluated as ◎, 1 and 1.5 or less were evaluated as ◯, 1.5 or more and 2 or less as Δ, and 2 or more as x.

As shown in Table 10, the formulation 1 in which the same amount of iron oxide as the comparative formulation was blended in the overall formulation using the product 14 of Example 14 was higher in color development than the comparative formulation, and the application 2 The color settling after time was small and the adhesion was excellent. In addition, Formula 2 in which the compounding amount of iron oxide is reduced from Formula 1 and the compounding amount of iron oxide is 80% of the comparative formulation is less than that of the comparative formulation, although the compounding amount of iron oxide is smaller than that of the comparative formulation. Excellent color development and other items were also excellent. The formulation 3 using the product 15 of Example 15 and having the compounding amount of iron oxide 80% of the comparative formulation as in the formulation 2 also had good color development and other items.

Example 27
Double layer lotion:
A two-layer lotion having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 3 are mixed.
(2) Components 4 to 9 were added to (1) and stirred uniformly to obtain a two-layer lotion.

The obtained two-layer lotion was excellent in powder dispersibility, a smooth feeling in use, and a two-layer lotion excellent in the uniformity of the decorative film.

Example 28
Milk liquid:
An emulsion having the composition shown below was produced by the following method.

(Production method)
(1) Components 1 to 7 are uniformly mixed at 80 ° C.
(2) Components 8 to 14 are mixed uniformly at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) Cool (3) while stirring, add component 15 and mix uniformly;
An emulsion was obtained.

The obtained emulsion was excellent in emulsification stability, smooth use feeling, uniformity of decorative film, and excellent UV blocking ability.

Example 29
cream:
A cream having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 7 are uniformly mixed at 80 ° C.
(2) Components 8 to 13 are mixed uniformly at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) (3) was cooled with stirring to obtain a cream.

The obtained cream was excellent in emulsification stability, smooth use feeling, uniformity of cosmetic film, and excellent UV blocking ability.

Example 30
Beauty liquid:
A serum having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 10 were mixed and dissolved at room temperature, and a cosmetic liquid was obtained while stirring.

The obtained essence was excellent in stability, smooth sensation of use, uniformity of cosmetic film, and essence excellent in UV blocking ability.

Example 31
Pack:
A pack having the composition shown below was produced by the following method.

(Production method)
(1) Components 1 to 4 are uniformly mixed at 80 ° C.
(2) Mix components 5 to 12 uniformly at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) (3) was cooled with stirring to obtain a pack.

The obtained pack was excellent in emulsification stability, smooth in feeling of use, and excellent in uniformity of the decorative film.

Example 32
Facial wash :
A face wash having the composition shown below was produced by the following method.

(Production method)
(1) Components 1 to 7 are uniformly mixed at 80 ° C.
(2) Components 8 to 11 are mixed uniformly at 80 ° C.
(3) Add (2) to (1) and neutralize.
(4) Add component 12 to (3) and mix uniformly.
(5) (4) was cooled while stirring to obtain a face wash.

The obtained facial cleanser was an excellent facial cleanser.

Example 33
Cleansing cream:
A cleansing cream having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 8 are uniformly mixed at 80 ° C.
(2) Components 9 to 14 are uniformly mixed at 80 ° C.
(3) Add (1) to (2) and emulsify.
(4) Cooling with stirring (3) gave a cleansing cream.

The obtained cleansing cream was excellent in emulsification stability and excellent in smooth use feeling.

Example 34
Hair wax:
A hair wax having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 3 are uniformly mixed at 80 ° C.
(2) Components 4 to 8 are uniformly mixed at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) After adding components 9 to 16 to (3), cool with stirring,
A hair wax was obtained.

The obtained hair wax was excellent in emulsification stability and hair styling property, and was a hair wax excellent in smooth use feeling and UV blocking ability.

Example 35
Oily eyeliner:
An oily eyeliner having the following composition was produced by the following method.

(Production method)
(1) Ingredients 1 to 4 are heated to 100 ° C. and mixed uniformly.
(2) Ingredients 5 to 9 are heated to 80 ° C. and mixed uniformly.
(3) Add (2) to (1) and mix uniformly.
(4) (3) was processed with a roller to obtain an oily eyeliner.

The obtained oily eyeliner was an oily eyeliner excellent in smooth use feeling, uniformity of the makeup film, and makeup lasting effect.

Example 36
Aqueous eyeliner:
An aqueous eyeliner having the composition shown below was produced by the following method.

(Production method)
(1) Components 1 to 5 are uniformly dispersed with a roller.
(2) Components 6 to 10 are mixed uniformly.
(3) (1) was added to (2) and mixed uniformly to obtain an aqueous eyeliner.

The obtained water-based eyeliner was a water-based eyeliner excellent in smooth use feeling, uniformity of the makeup film, and makeup lasting effect.

Example 37
Eyebrow:
An eyebrow having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 4 are mixed uniformly.
(2) Components 5 to 10 are treated with a roller.
(3) After adding (2), components 11 and 12 to (1), mix uniformly,
I got an eyebrow.

The obtained eyebrow was an eyebrow excellent in smooth use feeling, uniformity of the makeup film, and makeup lasting effect.

Example 38
O / W type mascara:
An O / W type mascara having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 8 are uniformly mixed at 80 ° C. and subjected to a roller treatment.
(2) Components 9 to 14 are uniformly mixed at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) (3) was cooled to obtain mascara (O / W).

The obtained O / W type mascara was excellent in powder dispersibility, and was an O / W type mascara excellent in smooth feeling of use, uniformity of the cosmetic film, and makeup lasting effect.

Example 39
Non-aqueous mascara:
A non-aqueous mascara having the following composition was produced by the following method.

(Production method)
(1) Ingredients 1 to 5 are heated to 110 ° C.
(2) Add components 6 to 9 to (1) and mix.
(3) Add components 10 to 13 to (2) and mix.
(4) (3) was processed with a roller to obtain a non-aqueous mascara.

The obtained non-aqueous mascara was a non-aqueous mascara excellent in smooth use feeling, uniformity of the cosmetic film, and a makeup lasting effect.

Example 40
Sticky lipstick:
A stick-shaped lipstick having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 7 are uniformly dissolved and mixed at 100 ° C.
(2) Add components 8 to 13 to (1) and mix uniformly.
(3) (2) was poured into a container and cooled to obtain a stick-shaped lipstick.

The obtained stick-shaped lipstick was a lipstick with a smooth feeling of use, uniformity of the cosmetic film, and excellent makeup lasting effect.

Example 41
Liquid Rouge:
A liquid rouge having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 5 are uniformly dissolved and mixed at 100 ° C.
(2) Add components 6 to 12 to (1) and mix uniformly.
(3) (2) was poured into a container and cooled to obtain a liquid rouge.

The obtained liquid rouge was a liquid rouge excellent in smooth feeling of use, uniformity of the makeup film, and makeup lasting effect.

Example 42
O / W type foundation:
An O / W type foundation having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 8 are uniformly dispersed with a roller.
(2) Mix components 9 to 12 uniformly.
(3) Add (1) to (2) and mix uniformly.
(4) Components 13 to 19 are mixed and dissolved at 80 ° C.
(5) Add (4) to (3) at 80 ° C. and emulsify.
(6) (5) was cooled, component 20 was added, and an O / W type foundation was obtained.

The obtained O / W type foundation was excellent in powder dispersibility, and was an O / W type foundation excellent in smooth use feeling, uniformity of cosmetic film, hiding property, UV blocking ability, and makeup lasting effect.

Example 43
W / O type foundation:
A W / O type foundation having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 3 are mixed uniformly.
(2) Components 4 to 11 are uniformly dispersed with a roller.
(3) Add (2) to (1) and mix uniformly.
(4) Components 12 to 15 were added to (3) and emulsified to obtain a W / O type foundation.

The obtained W / O-type foundation was excellent in powder dispersibility, and was a W / O-type foundation excellent in smooth feeling of use, cosmetic film uniformity, hiding properties, UV blocking ability, and makeup lasting effect.

Example 44
O / W eye color:
An O / W eye color having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 5 are uniformly mixed at 80 ° C.
(2) Add components 6 to 8 to (1) and emulsify.
(3) Components 9 to 14 are uniformly dispersed with a roller.
(4) (3) and Component 15 were added to (2) to obtain an O / W type eye color.

The obtained O / W type eye color was excellent in powder dispersibility, and was an O / W type eye color excellent in smooth feeling of use, uniformity of the cosmetic film, color developability, and makeup lasting effect.

Example 45
Oil solid foundation:
An oily solid foundation having the following composition was produced by the following method.

(Production method)
(1) Components 7 to 13 are dissolved by heating at 90 ° C.
(2) Add components 1 to 6 to (1) and uniformly disperse with a roller.
(3) Add component 14 to (2) and dissolve at 80 ° C., then fill into a metal pan,
An oily solid foundation was obtained.

The obtained oil-based solid foundation was excellent in powder dispersibility, had a smooth feeling of use, and was excellent in the uniformity of the cosmetic film, UV blocking ability, and makeup lasting effect.

Example 46
Stick concealer:
A stick concealer having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 5 are dissolved by heating at 90 ° C.
(2) Add components 6 to 12 to (1) and uniformly disperse with a roller.
(3) Add component 13 to (2) and dissolve at 80 ° C.
A stick-like concealer was obtained.

The obtained stick-like concealer was excellent in powder dispersibility, and was a stick-like concealer excellent in smooth feeling of use, makeup film uniformity, hiding property, UV blocking ability, and makeup lasting effect.

Example 47
Body milk:
Body milk having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 7 are uniformly dissolved at 80 ° C.
(2) Components 8 to 16 are uniformly dissolved at 80 ° C.
(3) Add (1) to (2) and emulsify.
(4) Add component 17 to (3), stir and cool after uniform mixing,
Got body milk.

The obtained body milk was excellent in emulsification stability, and was excellent in smooth use feeling, uniformity of cosmetic film, UV blocking ability, and makeup lasting effect.

Example 48
conditioner:
A conditioner having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 5 are uniformly mixed at 80 ° C.
(2) Mix components 6 to 9 uniformly at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) Add component 10 to (3), stir and cool after uniform mixing,
I got a conditioner.

The obtained conditioner was excellent in emulsification stability and excellent in smooth use feeling.

Example 49
Hair pack:
A hair pack having the composition shown below was produced by the following method.

(Production method)
(1) Components 1 to 6 are mixed uniformly at 80 ° C.
(2) Mix components 7 to 9 uniformly at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) Add component 10 to (3), stir and cool after uniform mixing,
I got a hair pack.

The obtained hair pack was excellent in emulsification stability and was excellent in smooth usability.

Example 50
W / O sunscreen:
A sunscreen with the composition shown below was produced by the following method.

(Production method)
(1) Components 1 to 5 are uniformly dispersed with a roller.
(2) Add components 6 to 9 to (1) and mix uniformly.
(3) Components 10 to 14 were added to (2) and emulsified to obtain a W / O type sunscreen.

The obtained W / O type sunscreen was excellent in powder dispersibility, and was excellent in smooth use feeling, uniformity of cosmetic film, UV blocking ability, and makeup lasting effect.

Example 51
Manicure:
A nail polish having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 9 were mixed uniformly to obtain nail polish.

The obtained nail polish was excellent in powder dispersibility, smooth maneuverability, uniformity of the cosmetic film, and excellent makeup lasting effect.

Example 52
Makeup base:
A makeup base having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 4 are uniformly dissolved at 80 ° C.
(2) Components 5 to 12 are uniformly dissolved at 80 ° C.
(3) Add (1) to (2) and emulsify.
(4) Components 13 to 14 were added to (3), mixed and cooled to obtain a makeup base.

The obtained makeup base was excellent in emulsification stability, and was excellent in smooth use feeling, uniformity of makeup film, UV blocking ability, and makeup lasting effect.

Example 53
White powder:
White powder having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 5 and components 8 to 10 are mixed uniformly.
(2) Add components 6 and 7 to (1) and mix uniformly.
(3) (2) was pulverized with a pulverizer to obtain white powder.

The obtained white powder was excellent in powder dispersibility, and was excellent in smooth use feeling, uniformity of the cosmetic film, UV blocking ability, and makeup lasting effect.

Example 54
Solid powder foundation:
A solid powder type foundation having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 7 and components 11 to 13 are mixed uniformly.
(2) Add components 8 to 10 to (1) and mix uniformly.
(3) Grind (2) with a pulverizer.
(4) A metal pan was filled with (3) to obtain a solid powder type foundation.

The obtained solid powder type foundation was excellent in powder dispersibility, and had a smooth feeling in use, uniformity of a cosmetic film, UV blocking ability, and a makeup lasting effect.

Example 55
Solid powder type teak:
A solid powder type cheek having the composition shown below was produced by the following method.

(Production method)
(1) Components 1 to 4 and components 7 to 9 are mixed uniformly.
(2) Add components 5 and 6 to (1) and mix uniformly.
(3) Grind (2) with a pulverizer.
(4) (3) was filled in a metal pan to obtain a solid powder type teak.

The obtained solid powder type cheek was excellent in powder dispersibility, excellent in smooth use feeling, uniformity of the cosmetic film, UV blocking ability, and makeup lasting effect.

Example 56
Solid powder eyeshadow:
A solid powder eye shadow having the following composition was produced by the following method.

(Production method)
(1) Components 1 to 6 and components 10 to 12 are mixed uniformly.
(2) Add components 7 to 9 to (1) and mix uniformly.
(3) Grind (2) with a pulverizer.
(4) A metal pan was filled with (3) to obtain a solid powder type foundation.

The obtained solid powder type eye shadow was excellent in powder dispersibility, and had a smooth feeling in use, a makeup film uniformity, color development, and a makeup lasting effect.

In the metal oxide composite high flat cellulose powder of the present invention, since the base cellulose itself is an organic substance and is flat, the surface thereof is composited with extremely fine metal oxide particles. Compared with powders made by combining talc and sericite, which are flat inorganic materials, with metal oxides, they have higher adhesion, excellent usability, and excellent UV blocking ability and coloring ability due to metal oxides It is.

Accordingly, the metal oxide-complexed high flat cellulose powder of the present invention can be used in many cosmetics. Particularly, cosmetics that easily exhibit the effect include powder foundation, eye shadow, blusher, powdered white powder, etc. And cosmetics containing the powder component and the oil component. Among these cosmetics, press-filled cosmetics are preferable, and powder foundations and eye shadows are particularly preferable. When the cosmetic of the present invention is a powder foundation and eye shadow, there is no powderiness, good wet feeling, good adhesion to the skin, and as a result, it blends naturally with the skin, unevenness, twist, color It will have good makeup without dullness or float.

Claims

Metal oxide composite high flat cellulose powder obtained by mechanically pulverizing a cellulosic material, a pulverization aid, and a metal oxide.
2. The metal oxide composite high flat cellulose powder according to claim 1, having an average particle diameter of 1 to 50 μm, an average thickness of 0.1 to 10 μm, and a flatness of 4 to 200.
3. The metal oxide composite high flat cellulose powder according to claim 1, wherein the amount of the metal oxide in the whole is 5 to 50% by mass.
4. The metal oxide composite high flattened cellulose powder according to claim 1, wherein the amount of the grinding aid in the whole is 0.5 to 5% by mass.
The metal oxide composite high flat cellulose powder according to any one of claims 1 to 4, wherein the mechanical pulverization is performed by a planetary ball mill.
Cellulosic material from fibrous or powdered wood flour or wood pulp originating from wood, fibrous or powdered cotton or linter fiber originating from cotton and refined fibers or powders The metal oxide composite high flat cellulose powder according to any one of claims 1 to 5, which is a cellulosic material selected from the group consisting of:
The metal oxide composite high flattened cellulose powder according to any one of claims 1 to 6, wherein the grinding aid is selected from the group consisting of an amphiphile, amino acids and fatty acids.
The metal oxide composite high flat cellulose powder according to claim 7, wherein the amphiphilic substance is selected from the group consisting of phospholipid, ceramide, cholesterol or a derivative thereof and phytosterol or a derivative thereof.
The metal oxide composite high flat cellulose powder according to claim 7, wherein the amino acids are selected from the group consisting of N-acylamino acids and theanine.
The metal oxide composite high flattened cellulose powder according to claim 7, wherein the fatty acids are selected from the group consisting of lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid and salts thereof.
The metal oxide composite high flat cellulose powder according to any one of claims 1 to 10, wherein the metal oxide is a compound selected from the group consisting of iron oxide, titanium oxide and zinc oxide.
12. The metal oxide composite high flat cellulose powder according to claim 1, wherein the composite metal oxide has an average particle size of 10 to 100 nm.
12. The metal oxide composite high flat cellulose powder according to claim 1, wherein the composite metal oxide has an average particle size of more than 100 nm and 1000 nm or less.
Cosmetics containing the metal oxide composite high flattened cellulose powder according to any one of claims 1 to 13.
15. The cosmetic according to claim 14, which is a powder cosmetic.
The cosmetic according to claim 14 or 15, which is a foundation, eye shadow, cheek red, powdered white powder, sunscreen or makeup base.
A method for producing a metal oxide composite high flattened cellulose powder comprising adding a grinding aid and a metal oxide to a cellulosic material to form a mixture, and mechanically grinding the mixture.
The method for producing a metal oxide composite high flat cellulose powder according to claim 17, wherein the addition amount of the metal oxide is 5 to 50% by mass in the whole.
The method for producing a metal oxide composite high flattened cellulose powder according to claim 17 or 18, wherein the addition amount of the grinding aid is 0.5 to 5% by mass in the whole.
The method for producing a metal oxide composite high flat cellulose powder according to any one of claims 17 to 19, wherein the mechanical pulverization is performed by a planetary ball mill.