KR20140036158A - Metal oxide conjugated highly-flat cellulose powder and cosmetic containing same - Google Patents

Abstract

It is an object of the present invention to provide a cosmetic powder having a higher functionality such as better usability and UV blocking ability, and a cosmetic using the powder, compared to the conventionally provided cosmetic powder. This cosmetics mix | blends the metal oxide composite high flat cellulose powder obtained by mechanically grinding | pulverizing a cellulose substance, a grinding aid, and a metal oxide, and this.

Description

Metal Oxide Complexed Highly Flat Cellulose Powder and Cosmetics Containing It {METAL OXIDE CONJUGATED HIGHLY-FLAT CELLULOSE POWDER AND COSMETIC CONTAINING SAME}

The present invention relates to a high flatness cellulose powder complexed with a metal oxide and a powder cosmetic containing the same, and more particularly, to a metal oxide composite high flat surface having a high flatness shape and whose surface is coated with a metal oxide. It relates to a cellulose powder 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, powder powder, blusher and the like.

This powder cosmetics are manufactured by generally filling a dish-shaped container with powder mixtures of powder components such as extender pigments and pigments and oily components, and press molding.

As powder components used in the powder cosmetics, mica pieces, sericite, talc, and the like, and surface-treated products of lamellae, sericite, talc, etc. in the form of natural products have been used as extender pigments because of their good spreadability and adhesion on the skin. In addition, in order to improve the sliding and feel of the extender pigment on the skin, a circular organic powder or the like has been used together with the extender pigment. As the pigment, white pigments such as titanium oxide, colored pigments such as bengala, and bright pigments such as mica titanium have been used.

Moreover, what coat | covered the powder component on metal oxide is also known (patent documents 1-3). For example, all of patent documents 1 and 2 coat | cover a fine metal oxide on the fine powder of a polymer or a circular resin powder, and the thing of patent document 3 is a hydroxyapatite in the gas phase which can be used for powder of cosmetics. And zinc oxide.

By the way, there are various forms of powder components, and although inorganic powders in the form of flakes such as mica, sericite, and talc are widely used, these are all aluminosilicate minerals and their properties differ slightly depending on the place of origin. For example, there has been a problem that oil absorbency is low or that the object having the desired physical properties cannot be obtained. On the other hand, it is not reported much in the form of organic substance in the flat form, for example, and it was the extent to which the flat cellulose particle obtained by mixing a cellulose substance and fatty acid, and then mechanically grinding this is known (patent document 4).

However, in this patent document 4, the specific use form of what the flat cellulose particle is disclosed is not disclosed, and the application to cosmetics is also only very simply disclosed.

On the other hand, the technique of treating the surface of crystalline cellulose with hydrogenated lecithin is also known (patent document 5). However, this crystalline cellulose has a ratio of long diameter to short diameter (L / D) of 3 or less, which is not as flat, and actually differs in the advantages of makeup persistence when compared to untreated. However, it is disclosed that there is not much difference in the feeling of using "drinking", "spreading", and "finish".

MEANS TO SOLVE THE PROBLEM First, the present inventors developed the flat cellulose powder (henceforth "high flatness cellulose powder") and its manufacturing method which were extremely high in flatness (aspect ratio) 20-200, and applied for the patent (patent document 6). This high flatness cellulose powder is obtained by drying the purified cellulose powder derived from the wood pulp under reduced pressure, sufficiently removing the adsorbed moisture, and then pulverizing it with a planetary ball mill together with a grinding aid and a hydrophobization treatment agent if necessary. .

And since the obtained high flatness cellulose powder is a cellulose material, and also has a characteristic called high flatness, when it is compounded as a component of powder cosmetics, even if the compounding quantity of an oil-based component is large, it will not produce the aggregation of powder, but the powder itself The characteristics such as the soft feeling of the film are also maintained, and it is also difficult to cause caking even when the powder is pressed.

JPH3-200721 A JPH8-59433 A JP 2002-20218 A JP 2004-230719 A JP 2003-146829 A WO 2010026925 A

Although many cosmetic powders have already been provided, it is a natural result that consumers demand a better usability or high usability cosmetics, and the present invention provides a cosmetic powder that can provide such cosmetics and a cosmetic using the same. It is a task.

MEANS TO SOLVE THE PROBLEM The present inventors further advanced the high flatness cellulose powder obtained from a cellulose substance, The conventional cosmetic powder by adding a grinding aid and a metal oxide to a cellulose substance by a specific method, and compounding these, In the present invention, a metal oxide composite high flat cellulose powder having a property that cannot be easily obtained is obtained, and by using this, it has been found that the commercial property of cosmetics such as powder cosmetics can be made extremely high, thereby completing the present invention.

That is, this invention is a metal oxide composite high flat cellulose powder obtained by mechanically pulverizing a cellulose substance, a grinding aid, and a metal oxide.

Moreover, this invention is the cosmetics characterized by containing the said metal oxide composite high flat cellulose powder.

In addition, the present invention is a method for producing 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.

The metal oxide composite high flat cellulose powder of the present invention exhibits a new effect in addition to the effect of conventional high flat cellulose powder by compounding a metal oxide on the surface thereof. Specifically, when the complexed metal oxide is 10 to 100 nm on the powder, a very good UV blocking effect and a smooth usability can be obtained. In addition, when the complexed metal oxide is more than 100 nm and 1000 nm or less on the powder, a smooth usability can be obtained with natural concealability and excellent color development.

In addition, the cosmetics blended with the metal oxide composite high flat cellulose powder have a smooth feel with excellent uniformity of the makeup film, and have an excellent UV blocking effect, natural concealment, and color development effect, and furthermore, do not cause color fading. It does not have such a lasting effect of makeup.

Therefore, the cosmetics using the metal oxide composite high flat cellulose powder of this invention can be used suitably as powder foundation, an eye shadow, powder white powder, a blusher, etc.

1 is a photograph of the surface of product 6 obtained in Example 6 using a scanning microscope (10,000 times);
FIG. 2 is a photograph of the surface of a product such as that of FIG. 1 observed with a scanning microscope (50,000 times); FIG.
3 is a photograph of the surface of a product as shown in FIG. 1 under a scanning microscope (200,000 times).

In the metal oxide composite high flat cellulose powder of the present invention, fine metal oxide powder is firmly adhered on the surface of the high flat cellulose powder, and is composited.

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

The cellulosic material used as a starting material for the metal oxide complexed high flat cellulose powder is not particularly limited, but for example, woody materials such as wood powder or wood pulp or wood pulp or cotton in the form of wood, It is preferable to use a fibrous or powdered cellulosic material obtained by refining a cotton-based material such as fiber or powder in the form of origin, or a cotton or linter fiber, a wood material, or a cotton-based material. You may use the refined cellulose substance obtained by the above. Moreover, as a cellulose substance originating in cotton, you may originate in cotton certified by organic.

The cellulose-based substance used as this raw material easily adsorbs or absorbs moisture, and has adsorption moisture of about 3 to 10% by mass (hereinafter only referred to as "%") in a normal state. In order to effectively obtain flat cellulose powder from this cellulose substance, it is preferable to dry it by hot air drying, vacuum drying, reduced pressure drying, etc. before grinding | pulverizing this, and to remove adsorption water.

On the other hand, the grinding aid used in the production of the metal oxide composite high flat cellulose powder of the present invention is used to high flatten the cellulose-based material, and examples thereof include amphiphiles, amino acids, fatty acids, and the like. Can be. You may mix these 1 type or 2 or more types.

Among these, 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 lipids in or close to a living body, that is, having a long chain alkyl structure and a hydrophilic group.

Among the amphiphiles, phospholipids are generic terms of lipids having a phosphate ester site in the structure. Specific phospholipids include those derived from natural hydrogenated natural lecithins such as egg yolk lecithin and soybean lecithin, hydrogenated risolicithin, phosphatidylcholine, phosphatidylethanolamine, phosphatidylserine, phosphatidylglycerol, phosphatidyl inositol, sphingomyelin and the like. And the like. Among these phospholipids, hydrogenated lecithin, phosphatidylcholine, phosphatidylethanolamine, and hydrogenated phosphatidyl glycerol are preferable.

In addition, ceramide is a generic term for nonionic amphiphiles having at least one long chain and / or branched alkyl or alkenyl group in the molecule, as well as at least two hydroxyl groups and one or more amide groups (and / or amino groups). to be. Specific ceramides include natural ceramides such as spingosine and phytosphingosine long-chain fatty acid amides such as ceramide 1, ceramide 2, ceramide 3, ceramide 3B, ceramide 4, ceramide 5, ceramide 6, ceramide 6I, ceramide 6II, and the like. Can be. Among these ceramides, ceramide 2 and ceramide 3 are preferable. In addition, these ceramides may be derived from natural products, or may be synthesized.

Cholesterol is a white or pale yellow solid which is purified by extracting, crystallizing and drying an oil obtained from saponified animal fat or fish oil. The molecular formula is C ₂₇ H ₄₆ O. In addition, derivatives of cholesterol are saturated fatty acids or unsaturated fatty acids, such as oleic acid, palmitoleic acid, palmitic acid, stearic acid, 2-ethylhexanoic acid, capric acid, and lauric acid. With a mixture of fatty acids obtained by hydrolyzing fats and oils such as natural vegetable fats and oils such as olive oil, avocado oil, sesame oil, rice germ oil, and macadamia nut oil, and animal fats and oils such as fish oil and butter. Esterified derivatives; Specific examples of preferred cholesterol derivatives include hydroxy stearic acid cholesterol and polyoxyethylene cholesteryl ether. Among these cholesterols or derivatives thereof, cholesterol is preferred.

In addition, phytosterol is a general term for a sterol compound obtained from a plant. Specific phytosterols include cytosterol, stigmasterol, fucosterol, spinasterol, brassicasterol and the like. In addition, the phytosterol derivatives are ester derivatives of saturated fatty acids or unsaturated fatty acids such as oleic acid, palmitoleic acid, palmitic acid, stearic acid, 2-ethylhexanoic acid, capric acid and lauric acid, olive oil and avocado. Esterified derivatives with a mixture of fatty acids obtained by hydrolyzing natural vegetable fats and oils such as oil, sesame oil, rice germ oil, and macadamia nut oil. As a specific example of a preferable phytosterol derivative, hydroxy stearate phytosteryl, polyoxyethylene phytosterol, polyoxyethylene phytostanol, etc. are mentioned. Among these phytosterols or derivatives thereof, phytosterols are preferred.

Moreover, amino acids, such as N-acylamino acid, such as N-lauroyl-L-lysine, theanine, are mentioned as amino acids among grinding aids.

Moreover, as fatty acids, saturated fatty acids, such as lauric acid, myristic acid, palmitic acid, stearic acid, its salt, unsaturated fatty acids, such as oleic acid, and its salt are mentioned.

On the other hand, as a metal oxide used in manufacture of the metal oxide composite high flat cellulose powder of this invention, if it is mix | blended as powder components, such as an extender pigment and a coloring pigment, in general cosmetics, it can use without restriction | limiting. Iron oxide, titanium oxide, zinc oxide, cerium oxide, etc. are mentioned as an example of this metal oxide. This metal oxide can also be used by 1 type (s) or 2 or more types.

Although the particle diameter of this metal oxide is 10-10000 nm is preferable, since some of the effects acquired as mentioned later differ according to the average particle diameter on the metal oxide composite high flat cellulose powder obtained, in view of this point, a raw metal It is preferable to select the particle diameter of the oxide.

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

The timing for adding these grinding aids and metal oxides to the cellulose-based substance may be any time before the grinding treatment, and the addition method may be added simultaneously or separately. Moreover, as a addition method of a grinding aid, after melt | dissolving this in a suitable solvent, you may add to a cellulose substance. 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, and aromatic hydrocarbons such as toluene.

In the process of mechanically grinding the mixture of the cellulosic material, the grinding aid, and the metal oxide described above, the pressure or shear force due to the grinding needs to be applied continuously for a predetermined time. For this reason, it is preferable to use a grinding device such as a vibrating ball mill, a rotary ball mill, a planetary ball mill, a roll mill, a medium ball mill, a disk mill, a high speed mixer with a high speed rotary blade, a homomixer, and the like. This is particularly preferred. As for the grinding | pulverization processing method, the dry grinding | pulverization process which does not use a solvent is preferable. In addition, the grinding energy applied in the case of performing the grinding treatment (gravity acceleration applied in the planetary ball mill in the case of the planetary ball mill) is preferably 3 to 20G, preferably 5 to 15G.

In addition, in the metal oxide composite high flat cellulose powder, the particle diameter, thickness, and flatness (aspect ratio) are important, but also the particle diameter of the metal oxide powder that is firmly adhered to and complexed, is also important depending on its use. Therefore, it is necessary to determine the grinding time while considering these. Since this relationship also relates to the target flat cellulose itself and the particle diameter of the metal oxide which is a raw material, etc., it is preferable to determine grinding | polishing conditions, grinding | pulverization time, etc. experimentally beforehand.

Next, the preferable aspect for obtaining the metal oxide composite high flat cellulose powder of this invention is shown. First, the cellulose powder derived from the refined wood pulp is dried under reduced pressure at 30-50 degreeC, and adsorption water is fully removed to 0.1% or less. This cellulose powder is thrown into a sealable alumina or zirconia grinding vessel together with alumina or zirconia grinding balls, and a grinding aid and a metal oxide powder are added so as to be in the above amount relative to the cellulose powder. Thereafter, the grinding vessel is installed in a planetary ball mill, and grinding is performed at a rotational speed of 100 to 250 rpm. The pulverizing treatment may be repeatedly performed for about 2 to 72 cycles in a continuous cycle, with 5 to 15 minutes of pulverization being stopped for 5 to 15 minutes, or may be continuously performed for about 5 to 120 minutes without stopping.

Moreover, after grinding | pulverization process, you may remove the water etc. which adhered to the metal oxide composite high flat cellulose powder by well-known drying means, such as air drying, hot air drying, vacuum drying, and vacuum drying.

The metal oxide composite high flat 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 0.2 to It is in the form of flakes having a thickness of 2 μm, and the flatness is 4 to 200, preferably 10 to 100. In addition, an average particle diameter is an average value on the apparatus of the width and length of the flat cellulose particle measured in the disperse state in ethanol using particle size distribution measuring apparatuses, such as a laser diffraction and scattering particle size distribution measuring apparatus (integrated volume 50 here). Particle diameter value of%). In addition, an average thickness means the value which selected a plurality of particle | grains of the size equivalent to the average particle diameter calculated | required by electron microscopes, such as a scanning electron microscope, and measured the thickness, and averaged them. In addition, flatness is the average particle diameter / average thickness calculated | required as mentioned above. In addition, the particle diameter of the complexed metal oxide can also be measured by a scanning electron microscope.

The metal oxide composite high flat cellulose powder thus obtained is firmly attached as described above, and the particle diameter of the complexed metal oxide is more than 100 nm and 1000 nm or less (pigment grade size), and this is from 10 to 10. In the case of 100 nm (particulate size), the property is slightly different, and the use also differs. That is, when the complexed metal oxide is a fine particle grade, very excellent UV blocking effect and uniformity of a makeup film can be obtained. In addition, when the complexed metal oxide is pigment grade, excellent color development can be obtained. In addition, since the particle diameter of the metal oxide hardly changes before and after the compounding, the particle diameter of the metal oxide after the compounding is almost equal to the particle diameter of the metal oxide added before the compounding.

And since this metal oxide composite high flat cellulose powder is equipped with the smooth feeling which the high flat cellulose powder originally possessed, the cosmetics which mix | blended this have the outstanding uniformity of the makeup film, the smooth feeling, and the outstanding UV blocking effect. It has a color development effect and has no lasting effect such as no color fading.

The obtained metal oxide composite high flat cellulose powder is thin in thin sheet form compared to talc and sericite of conventional extender pigments, and has excellent properties such as transparency, softness, spreadability, and natural gloss. Since it is excellent in chemical property, and also excellent in UV blocking effect and color development effect, the cosmetics which can use this specifically include many cosmetics which use powder, for example, a base (skin care) cosmetics, a makeup cosmetics, and an ultraviolet-ray cosmetics And various cosmetics such as hair cosmetics. In particular, the use in powder cosmetics, such as powder foundation, liquid foundation, eye shadow, blusher, and powdered powder, and cosmetics which require UV-blocking effects, such as a sunscreen and a makeup base, is effective and preferable.

Preparation of the cosmetics which mix | blends the metal oxide composite high flat cellulose powder of this invention is performed by combining this with a suitable cosmetic base, and formulating it. For example, when cosmetics are powder cosmetics, in the manufacturing method similar to the conventional powder cosmetics, the metal oxide composite high flat cellulose powder of this invention may be used instead of a part or all of the conventional powder components. Moreover, the compounding quantity of the metal oxide composite high flat cellulose powder in the said cosmetics is 1 to 90%, Preferably it is 5 to 90%, Especially preferably, it is 5 to 70%.

In the said cosmetics, it is preferable to mix | blend an oil-based component as a cosmetic base. There is no restriction | limiting in particular as an oil-based component mix | blended with this cosmetics, For example, a paraffin wax, a ceresin wax, an ozokerite, a microbinding wax, a montan wax, a Fischer-Tropsch wax, a polyethylene wax, a liquid paraffin, a squawalan Hydrocarbons such as, petrolatum, polyisobutyrene and polybutene, natural waxes such as carnauba wax, beeswax, lanolin wax, candelilla, tribehenic acid glycerol, rosin acid pentaerythritol ester, jojoba oil Esters such as cetyl isooctanate, isopropyl myristic acid, trioctanoic acid glyceryl, triisostearic acid diglyryl, and dipentaerythritol fatty acid esters, stearic acid, behenic acid, and 12-hydroxystearate Fatty acids such as acids, higher alcohols such as cetanol, stearyl alcohol and behenyl alcohol, oils such as olive oil, castor oil, mink oil and wax; Lanolin derivatives such as lean fatty acid isopropyl and lanolin alcohols, amino acid derivatives such as N-lauroyl L-glutamic acid di (cholesteryl behenyl octyldodecyl), perfluoropolyether and perfluoro And fluorine emulsions such as decane and perfluorooctane. One type or two types or more of these oil-based components can be used, The compounding quantity at the time of mix | blending an oil-based component with the cosmetics of this invention is although it does not specifically limit, 0.1-25% is preferable.

Moreover, in the said cosmetics, conventional powder components, for example, inorganic powders, such as talc, and organic powders, such as nylon, can be mix | blended. In this case, it is good to add and disperse | distribute an inorganic powder and an organic powder with the metal oxide composite high flat cellulose powder of this invention, and to produce it by adding an oil component as needed.

Moreover, as needed, the said cosmetics can see the components used for normal cosmetics, for example, water-soluble components, such as surfactant, an oil gelling agent, polyhydric alcohol, and a moisturizer, a ultraviolet absorber, a preservative, a cosmetic component, a fragrance, etc. It can mix | blend suitably in the range which does not impair the effect of this invention.

The properties and the formulation of the cosmetics are not particularly limited and can be selected according to the purpose. The cosmetic composition of the present invention may be any of liquid, powder, solid, emulsion, cream, gel, and the like, and the formulation may be aqueous, oily, solubilized, aqueous in oil, oil in water or the like. The formulation of the side may be sufficient.

The reason why the metal oxide composite high flat cellulose powder of the present invention described above is particularly superior to the conventional metal oxide composite particles is that the metal oxide is complexed to the high flat cellulose powder in the form of primary particles which are extremely fine. It is presumed to be due to what is there. That is, although the surface of the product 6 obtained in Example 6 was observed with the scanning electron microscope, FIGS. 1-3, the particle | grain zinc oxide cannot be observed at all in FIG. However, when the magnification is increased to 50,000 times, the particulate zinc oxide starts to appear white on the surface, and at 200,000 times the magnification, fine particle zinc oxide of about 20 nm is observed on the mother powder. Since the original particle diameter of the fine particle zinc oxide is about 20 nm, the result is that the fine particle zinc oxide does not agglomerate on the surface of the metal oxide complexed high cellulose powder of the present invention and is composited in a relatively primary particle state. Can be interpreted. That is, on the metal oxide composite high flat cellulose powder, it is thought that the metal oxide exists in the state of the primary particle which can exhibit the effect to the maximum, and is the reason which shows the outstanding outstanding performance.

As described above, the reason why the metal oxide is complexed in the state of the primary particles in the metal oxide composite high flat cellulose powder of the present invention is not yet clear, but it is fine in place where the high flat cellulose particles are formed from the cellulosic material. Since the metal oxide powder is present and is stirred at a high share, it is interpreted as if it is preferentially attached on the freshly produced cellulose surface and thus has a strong bond.

[Example]

Hereinafter, although an Example is given and this invention is demonstrated in detail, this invention is not limited to these Examples at all.

Example 1

Preparation of laurolysine treated fine particle titanium oxide composite high flat cellulose powder (1):

(1) As a raw material, cellulose powder (Nippon Seishi Chemical Co., Ltd .: W-400G) derived from purified wood pulp was used. First, the cellulose powder (55.3 g) from which adsorption water was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding ball. , 0.7 g of lauroyl lysine (Amihope LL Ajinomoto Co., Ltd.), particulate titanium oxide (manufactured by TTO-S-4 Ishihara Sangyo Co., Ltd.) (reduced particle diameter: 10 To 20 nm, long axis: 50 to 100 nm) was added 14 g. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was carried out for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and laurolysine. The treated fine particle 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, the average particle diameter (average value on the apparatus of the width and length) of the powder obtained by dispersing in ethanol of the powder obtained by the flow cell using the laser diffraction scattering type particle size distribution measuring apparatus (Horiba Co., Ltd. LA-920). Was obtained. As an average particle diameter here, the particle diameter value of 50% of the integrated volume was used. In addition, the particle size distribution measurement was carried out by dropping a suspension obtained by dispersing 50 mg of the obtained powder in 10 ml of ethanol in a sample circulation tank using ethanol of the particle size distribution measuring device as a medium, and then measuring the concentration. As a result, the average particle diameter of powder was 16 micrometers.

In addition, the average thickness of the obtained particle | grains directly observed a particle | grains using the scanning electron microscope (S-2150 by Hitachi Seisakusho), and selected several particle | grains of the size equivalent to the average particle diameter calculated | required above. It measured by measuring the thickness and averaging them. In the observation by a scanning electron microscope, very small amount of the obtained powder was put on the sample stand of a scanning electron microscope, and after drying at reduced pressure, platinum was deposited and it was set as the microscope test sample. From the image obtained by observing this microscopy sample with the magnification of 500 to 10,000 times with the acceleration voltage of 10-25 kV, the thickness in the particle | grains of the size equivalent to the average particle diameter measured above was measured, and the average thickness was calculated from them. . As a result, the average thickness was 1.7 μm.

As a result, product 1 had a flat cellulose particle (laurolysine-treated fine titanium oxide composite high flat cellulose powder) having an average particle diameter of 16 μm, an average thickness of 1.7 μm, and a flatness (average particle diameter / average thickness) of 9.4. It was found to be. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 2

Preparation of laurolysine treated fine particle titanium oxide composite high flat cellulose powder (2):

As a raw material, the cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (41.3 g) from which adsorption moisture was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding balls. And 0.7 g of lauroyl lysine (Amihof LL Ajinomoto Co., Ltd.) and 28 g of fine particle titanium oxide (TTO-S-4 manufactured by Ishihara Sangyo) were added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and the laurolysine-treated fine titanium oxide composite high flat cellulose powder (Product 2) was obtained.

About the obtained product 2, it carried out similarly to Example 1 (2), and measured the average particle diameter, thickness, and flatness, and the average particle diameter was 15 micrometers, the average thickness was 1.0 micrometer, and flatness (average particle diameter / average thickness). Was flat. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 3

Preparation of Hydrogenated Lecithin Treated Titanium Oxide Composite High Flat Cellulose Powder (3):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (55.3 g) from which adsorption water was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding ball. 0.7 g of hydrogenated lecithin (manufactured by Resinol S-10 Nikko Chemicals Co., Ltd.) and 14 g of fine particle titanium oxide (manufactured by TTO-S-4 Ishihara Sangyo) were added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and the hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder ( Product 3) was obtained.

About the obtained product 3, the average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 16 micrometers, the average thickness is 1.9 micrometers, and flatness (average particle diameter / average thickness) Was flat with 8.4. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 4

Preparation of Hydrogenated Lecithin Treated Titanium Oxide Composite High Flat Cellulose Powder (4):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (41.3 g) from which adsorption moisture was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding balls. 0.7 g of hydrogenated lecithin (manufactured by Resinol S-10 Nikko Chemicals Co., Ltd.) and 28 g of fine particle titanium oxide (manufactured by TTO-S-4 Ishihara Sangyo Co., Ltd.) were added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and the hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder ( Product 4) was obtained.

About the obtained product 4, the average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 15 micrometers, the average thickness is 1.2 micrometers, and flatness (average particle diameter / average thickness) Was 12.5 flat. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 5

Preparation of ceramide treated fine particle titanium oxide composite high flat cellulose powder (5):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (41.3 g) from which adsorption moisture was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding balls. , 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) and 28 g of fine particle titanium oxide (TTO-S-4 manufactured by Ishihara Sangyo) were added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and the ceramide-treated fine particle titanium oxide composite high flat cellulose powder (Product 5) )

About the obtained product 5, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 16 micrometers, the average thickness is 1.2 micrometers, and flatness (average particle diameter / average thickness) Was flat with 13.3. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 6

Preparation of laurolysine treated fine particle zinc oxide composite high flat cellulose powder (6):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (55.3 g) from which adsorption water was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding ball. 0.7 g of lauroyl lysine (Amihof LL Ajinomoto Co., Ltd.) and 14 g of fine particle zinc oxide (ZnO-610 Sumitomo Osaka Chemical Co., Ltd.) (average particle diameter 20 nm) were added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and the laurolysine-treated fine particle zinc oxide composite high flat cellulose powder was used. (Product 6) was obtained.

About the obtained product 6, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 16 micrometers, average thickness is 1.7 micrometers, flatness (average particle diameter / average thickness) Was flat with 9.4. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 7

Preparation of laurolysine treated fine particle zinc oxide composite high flat cellulose powder (7):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (41.3 g) from which adsorption moisture was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding balls. And 0.7 g of lauroyl lysine (Amihof LL Ajinomoto Co., Ltd.) and 28 g of fine particle zinc oxide (ZnO-610 Sumitomo Osaka Cement Co., Ltd.) were added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and the laurolysine-treated fine particle zinc oxide composite high flat cellulose powder was used. (Product 7) was obtained.

About the obtained product 7, the average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 15 micrometers, the average thickness is 1.0 micrometer, and flatness (average particle diameter / average thickness) Was flat. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 8

Preparation of Hydrogenated Lecithin Treated Particle Zinc Oxide Composite High Flat Cellulose Powder (8):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (41.3 g) from which adsorption moisture was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding balls. 0.7 g of hydrogenated lecithin (manufactured by Resinol S-10 Nikko Chemicals Co., Ltd.) and 28 g of fine particle zinc oxide (manufactured by ZnO-610 Sumitomo Osaka Corporation) were added. Thereafter, using a planetary ball mill (Sansho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and the hydrogenated lecithin-treated fine particle zinc oxide composite high flat cellulose powder ( Product 8).

About the obtained product 8, as in Example 1 (2), when the average particle diameter, thickness, and flatness were measured, the average particle diameter is 15 micrometers, the average thickness is 1.2 micrometers, and flatness (average particle diameter / average thickness). Was 12.5 flat. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 9

Preparation of Ceramide Treated Particulate Zinc Oxide Composite Highly Flat Cellulose Powder (9):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (41.3 g) from which adsorption moisture was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding balls. And 0.7 g of ceramide (manufactured by Ceramide II Wako Pure Chemical Industries, Ltd.) and 28 g of fine particle zinc oxide (manufactured by ZnO-610 Sumitomo Osaka Corporation) were added. Thereafter, using a planetary ball mill (Sansho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)) to obtain a ceramide-treated fine particle zinc oxide composite high flat cellulose powder (Product 9). )

About the obtained product 9, it carried out similarly to Example 1 (2), and measured the average particle diameter, thickness, and flatness, and the average particle diameter was 15 micrometers, the average thickness was 1.2 micrometers, and flatness (average particle diameter / average thickness). Was 12.5 flat. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 10

Preparation of Hydrogenated Lecithin Treated Titanium Oxide Composite High Flat Cellulose Powder (10):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (55.3 g) from which adsorption water was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding ball. 0.7 g of hydrogenated lecithin (manufactured by Resinol S-10 Nikko Chemicals Co., Ltd.) and 14 g of titanium oxide (manufactured by TIPAQUE CR-50 Ishihara Sangyo Co., Ltd.) (average particle diameter 250 nm) were added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and a hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder (product 10) was obtained.

About the obtained product 10, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 18 micrometers, the average thickness is 2.2 micrometers, and flatness (average particle diameter / average thickness) Was flat with 8.2. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 11

Preparation of Hydrogenated Lecithin Titanium Oxide Composite Highly Flat Cellulose Powder (11):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (41.3 g) from which adsorption moisture was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding balls. 0.7 g of hydrogenated lecithin (manufactured by Resinol S-10 Nikko Chemicals Co., Ltd.) and 28 g of titanium oxide (manufactured by TIPAQUE CR-50 Ishihara Sangyo Co., Ltd.) were added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and a hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder (product 11) was obtained.

About the obtained product 11, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 17 micrometers, the average thickness is 1.5 micrometers, and flatness (average particle diameter / average thickness) Was flat with 11.3. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 12

Preparation of Ceramide Treated Titanium Oxide Composite High Flat Cellulose Powder (12):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (55.3 g) from which adsorption water was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding ball. , 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) and 14 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo) were added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotation speed of 200 rpm (about 10 G (gravity acceleration)), and the ceramide-treated titanium oxide composite high flat cellulose powder (Product 12) Got.

About the obtained product 12, in the same manner as in Example 1 (2), the average particle diameter, the thickness, and the flatness were measured, and the average particle diameter was 18 µm, the average thickness was 2.2 µm, and the flatness (average particle diameter / average thickness). Was flat with 8.2. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 13

Preparation of Ceramide Treated Titanium Oxide Composite High Flat Cellulose Powder (13):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (41.3 g) from which adsorption moisture was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding balls. , 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) and 28 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo) were added. Thereafter, using a planetary ball mill (Sansho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and the ceramide-treated titanium oxide composite high flat cellulose powder (Product 13) Got.

About the obtained product 13, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 17 micrometers, the average thickness is 1.5 micrometers, and flatness (average particle diameter / average thickness) Was flat with 11.3. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 14

Preparation of Ceramide Treated Titanium Oxide and Iron Oxide Composite Highly Flat Cellulose Powder (14):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, 41.3 g (59%) of cellulose powder having sufficiently removed the adsorbed moisture by 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a hermetic alumina grinding vessel (volume 500 ml) together with the alumina grinding ball. In addition, 0.7 g (1%) of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.), 21 g (30%) of titanium oxide (TITANIX JR-800 Teika Corporation) (average particle diameter 270 nm), and red iron oxide (Tarox) (TAROX) R-516P Titanium Co., Ltd.) (average particle diameter shortening: 80 nm, major axis: 800 nm) 0.875 g (1.25%), iron sulfate (Tarox synthetic iron oxide YP1200P Titanium Co., Ltd.) ) (Average particle diameter shortening: 90 nm, long axis: 900 nm) was added 6.125 g (8.75%). Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and the ceramide-treated titanium oxide / iron oxide composite high flat cellulose powder (product 14) was obtained.

About the obtained product 14, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 17 micrometers, the average thickness is 1.5 micrometers, and flatness (average particle diameter / average thickness) Was flat with 11.3. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 15

Preparation of ceramide-treated titanium oxide and iron oxide composite high flat cellulose powder (15):

By the same method as in Example 14, 59% of refined wood pulp-derived cellulose powder (W-400G), 1% of ceramide (Ceramide II), 38.2% of titanium oxide (TITANIX JR-800), and red iron oxide (tarox R) -516P) and 0.435% of iron sulfate (tarox synthetic iron oxide YP1200P) were used to obtain ceramide-treated titanium oxide and iron oxide composite high flat cellulose powder (Product 15).

About the obtained product 15, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 17 micrometers, the average thickness is 1.5 micrometers, and flatness (average particle diameter / average thickness) Was flat with 11.3. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 16

Preparation of Stearic Acid Treated Titanium Oxide and Iron Oxide Composite Highly Flat Cellulose Powder (16):

57% refined wood pulp-derived cellulose powder (W-400G), 3% stearic acid, 38.2% titanium oxide (TITANIX JR-800), and red iron oxide (Tarox R) by the same method as in Example 14. -516P) using 0.45% and iron sulfate (Tarox synthetic iron oxide YP1200P) to obtain stearic acid-treated titanium oxide / iron oxide composite high flat cellulose powder (Product 16).

About the obtained product 16, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 17 micrometers, the average thickness is 1.1 micrometers, and flatness (average particle diameter / average thickness) Was flat with 15.5. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 17

Preparation of ceramide-treated titanium oxide and iron oxide composite high flat cellulose powder (17):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (41.3 g) from which adsorption moisture was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding balls. 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.), 25.9 g of titanium oxide (TITANIX JR-800 Teika Co., Ltd.), 0.525 g of red iron oxide (Tarox R-516P Titanium Co., Ltd.), 1.575 g of iron sulfate (produced by Tarox synthetic iron oxide YP1200P Titanium Co., Ltd.) was added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and the ceramide-treated titanium oxide / iron oxide composite high flat cellulose powder (product 17).

About the obtained product 17, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 17 micrometers, the average thickness is 1.5 micrometers, and flatness (average particle diameter / average thickness) Was flat with 11.3. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Comparative Example 1

Preparation of ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (1):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (63.3 g) from which adsorption water was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding ball. And 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) was added. Thereafter, using a planetary ball mill (Sansho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)) to obtain a ceramide-treated flat cellulose powder. Next, the obtained ceramide-treated high flat cellulose powder (60 g), 30 g of titanium oxide (manufactured by TITANIX JR-800 Teika Co., Ltd.), 1.25 g of red iron oxide (manufactured by Tarox R-516P Titanium Co., Ltd.), iron sulfide (Tarox synthesis) 8.75 g of iron oxide YP1200P Titanium Co., Ltd.) was mixed for 10 minutes in a Henschel mixer (manufactured by Mitsui Miike Co., Ltd.) to obtain a ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (comparative product 1).

About the obtained comparative product 1, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), and when average particle diameter is 19 micrometers, average thickness is 1.4 micrometers, flatness (average particle diameter / average thickness), ) Was flat with 13.6.

Comparative Example 2

Preparation of Ceramide Treated High Flat Cellulose Powder / Titanium Oxide / Iron Oxide Mixture (2):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (63.3 g) from which adsorption water was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding ball. And 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) was added. Thereafter, using a planetary ball mill (Sansho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)) to obtain a ceramide-treated high flat cellulose powder. 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 Co., Ltd.), iron sulfate (tarox synthetic iron oxide) 2.25 g of YP1200P Titanium Co., Ltd.) was mixed for 10 minutes in a Henschel mixer (manufactured by Mitsui Miike Co., Ltd.) to obtain a ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (comparative product 2).

About the obtained comparative product 2, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 19 micrometers, average thickness is 1.4 micrometers, and flatness (average particle diameter / average thickness) ) Was flat with 13.6.

Comparative Example 3

Preparation of laurolysine treated high flat cellulose powder / particulate titanium oxide mixture (3):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (63.3 g) from which adsorption water was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding ball. And 0.7 g of lauroyl lysine (Amihof LL Ajinomoto Co., Ltd.) were added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)) to obtain a laurolysine-treated high flat cellulose powder. Next, the obtained laurolysine-treated flat cellulose powder (60 g) and fine particle titanium oxide (manufactured by TTO-S-4 Ishihara Sangyo Co., Ltd.) (12 g) were mixed with a Henschel mixer (manufactured by Mitsui Miike Co., Ltd.) for 10 minutes. A lysine-treated high flat cellulose powder / particulate titanium oxide mixture (comparative product 3) was obtained.

About the obtained comparative product 3, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), and when average particle diameter is 19 micrometers, average thickness is 1.4 micrometers, flatness (average particle diameter / average thickness), ) Was flat with 13.6.

Comparative Example 4

Preparation of laurolysine treated high flat cellulose powder / particulate zinc oxide mixture (4):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (63.3 g) from which adsorption water was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding ball. And 0.7 g of lauroyl lysine (Amihof LL Ajinomoto Co., Ltd.) were added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)) to obtain a laurolysine-treated high flat cellulose powder. Subsequently, the obtained laurolysine-treated flat cellulose powder (60 g) and fine particle zinc oxide (ZnO-610 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 lysine-treated high flat cellulose powder and particulate zinc oxide was obtained.

About the obtained comparative product 4, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), and when average particle diameter is 19 micrometers, average thickness is 1.4 micrometers, flatness (average particle diameter / average thickness), ) Was flat with 13.6.

Comparative Example 5

Preparation of Hydrogenated Lecithin Treated High Flat Cellulose (5):

As a raw material, the cellulose powder (Nippon Paper Chemicals company: W-400G) derived from the refined wood pulp was used. First, the cellulose powder (63.3 g) from which adsorption water was sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C was introduced into a sealable alumina grinding vessel (volume 500 ml) together with the alumina grinding ball. And 0.7 g of hydrogenated lecithin (resinol S-10 manufactured by Nikko Chemicals Co., Ltd.) was added. Thereafter, using a planetary ball mill (Sansho Industries Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and hydrogenated lecithin-treated high flat cellulose powder (comparative product 5). Got.

About the obtained comparative product 5, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 19 micrometers, average thickness is 1.4 micrometers, flatness (average particle diameter / average thickness), ) Was flat with 13.6.

Comparative Example 6

Titanium oxide / iron oxide composite cellulose powder (6):

60 mass% of refined wood pulp-derived cellulose powder (W-400G) is put into a planetary ball mill (Sansho Industries Co., Ltd.), and 38.2% of titanium oxide (TITANIX JR-800) is added to the red iron oxide (Tarox R- 516P) was added 0.45% and iron sulfide (Tarox synthetic iron oxide YP1200P), and pulverized for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)) to obtain titanium oxide / iron oxide composite cellulose powder ( Comparative product 6) was obtained.

About the obtained comparative product 6, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 18 micrometers, the average thickness is 2.0 micrometers, and flatness (average particle diameter / average thickness) ) Was flat with 9.0. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Comparative Example 7

Polysiloxane Treated Titanium Oxide And Iron Oxide Composite Sericite (7):

60% by mass of dimethylpolysiloxane 3% treated sericite (SA sericite FSE; manufactured by Miyoshi Kasei Co., Ltd.) was placed in a planetary ball mill (Sansho Industries Co., Ltd.), and titanium oxide (TITANIX JR-800) was added thereto. ) 38.2%, red iron oxide (Tarox R-516P) 0.45% and iron sulfate (Tarox synthetic iron oxide YP1200P) were added, and at 40 rpm for 40 minutes at a rotation speed of 200 rpm (gravity acceleration of about 10 G). It pulverized and the polysiloxane-treated titanium oxide and iron oxide composite sericite (comparative product 7) was obtained.

About the obtained comparative product 7, it carried out similarly to Example 1 (2), and measured the average particle diameter, thickness, and flatness, and average particle diameter was 7.0 micrometers, average thickness was 1.0 micrometer, and flatness (average particle diameter / average thickness). ) Was flat with 7.0. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Comparative Example 8

Polysiloxane-treated titanium oxide and iron oxide composite talc (8):

60% by mass of dimethylpolysiloxane 2% treated talc (SA talc JA-68R; manufactured by Miyoshi Kasei Co., Ltd.) was placed in a planetary ball mill (Sansho Industries Co., Ltd.), and 38.2% titanium oxide (TITANIX JR-800) was added thereto. 0.45% of red iron oxide (Tarox R-516P) and 1.35% of iron sulfate (Tarox synthetic iron oxide YP1200P) were added, and pulverized for 40 minutes at a rotational speed of 200 rpm (about 10 G (gravity acceleration)), and polysiloxane Treated titanium oxide and iron oxide composite talc (comparative product 8) was obtained.

About the obtained comparative product 8, average particle diameter, thickness, and flatness were measured similarly to Example 1 (2), When the average particle diameter is 7.0 micrometers, the average thickness is 0.7 micrometer, and flatness (average particle diameter / average thickness), ) Was flat with 10.0. In addition, the particle diameter of the metal oxide after compounding was almost equal to the particle diameter before compounding.

Example 18

UV barrier test (1):

About the fine particle titanium oxide composite high flat cellulose powder (product 1, product 2) manufactured in Examples 1 and 2, the UV blocking ability was investigated. In experiment, 0.04 g of each powder was apply | coated uniformly to a trans pore tape (5 cm x 8 cm) so that it might become 1 mg / cm <2>, and UV blocking ability of the 300-450 nm area | region was carried out by SPF analyzer ( Sanyo Trading Co., Ltd.) was used. In addition, the comparative product 3 was used as a comparison. The results are shown in Table 1.

As shown in Table 1, the product 1 and the product 2 of the present invention had a high SPF value of about 5 times or more, and excellent in UV blocking ability, compared to the high flat cellulose powder (comparative product 3) in which fine particle titanium oxide was mixed. .

Example 19

UV barrier test (2):

The UV blocking ability was investigated in the same manner as in Example 18 for the fine particle zinc oxide composited high flat cellulose powder (Products 6 to 9) prepared in Examples 6 to 9. In addition, the comparative product 4 was used as a comparison. The results are shown in Table 2.

As shown in Table 2, the product 6 of the present invention has a SPF value of about 2 times or more higher than that of the high flat cellulose powder (comparative product 4) in which fine particulate zinc oxide is mixed, and the products 7 to 9 are about 3 More than twice as high, the powder of the present invention was a powder having excellent UV blocking ability.

Example 20

Color change test:

The color changeability was tested about the powder prepared in Examples 15 and 16 and Comparative Examples 6-8.

First, each powder was mixed with an oil component of the same weight (tri 2-ethylhexanoic acid glycerol) and a spatula sufficiently, and the test sample was prepared. After filling the sample under test and the produced powder itself in a glass cell, the color value (a value; red / b value; yellow) was measured by a spectrophotometer SE-2000 (manufactured by Nippon Denshoku Kogyo Co., Ltd.). ), Respectively.

Among these color values, the differences (Δa and Δb) of a value (a1) and b value (b1) of the pigment itself and a value (a2) and b value (b2) of the pigment mixed with the oil component are obtained, Moreover, from this value, the color change property of the whole was calculated | required by the following formula. Based on this color changeability, color changeability was evaluated by the following reference | standard. The results are shown in Table 3.

Color Change = √ ((Δa) ² + (Δb) ² )

However, Δa represents the difference between a1 and a2, and Δb represents the difference between b1 and b2.

(Evaluation standard)

Color Variability: Evaluation

0 or more and 1.5 or less: ◎

1.5 or more and 2.0 or less: ○

2.0 or more and 2.5 or less: △

Over 2.5 ~: ×

As shown in Table 3, the product 15 and the product 16 of the present invention were excellent in small change in color even when mixed with the oil component. On the other hand, even if the mixed amount of titanium oxide and iron oxide is the same, the comparative product 6 which does not use the grinding aid, the comparative product whose dimethyl polysiloxane-treated sericite is the parent powder, and the comparative product 8 whose dimethylpolysiloxane-treated talc is the parent powder When it mixed with the oil component, the color change was inferior.

Example 21

Powder Foundation (1):

The powder foundation of the cosmetics 1-5 of this invention was prepared by the prescription of Table 4 and the following method using the microparticles | fine-particles titanium oxide composite high flat cellulose powder (products 1-5) manufactured in Examples 1-5. About this powder foundation, UV blocking ability, SPF value, the uniformity of the makeup film, natural finish (without turbid phenomenon), makeup persistence, stability (with or without agglomerate), and usability (smoothness at the time of application) were investigated by the following method. As a comparison, using fine particle titanium oxide coated mica (58.5% mica, 40% titanium oxide, iron oxide 1.5%) (Comparative cosmetics 1) and high flat cellulose powder and fine particle titanium oxide A mixture (comparative product 3) was used (comparative cosmetic product 2). This result is also shown in Table 4.

(Manufacturing method)

After mixing components 1-18 in a Henschel mixer for 10 minutes, components 19-23 are added and stirred for 5 minutes. Thereafter, it is pulverized in an atomizer (1 HP screen diameter 1.5 mm phi), and filled into a resin dish to obtain a powder foundation.

(Test Methods)

UV protection and SPF value:

About the powder foundation manufactured by the cosmetics 1-5 and the comparative cosmetics 1 and 2 of this invention, the UV blocking ability was investigated. In the experiment, 0.04 g of each powder was uniformly coated on a transpore tape (5 cm x 8 cm) so as to be 1 mg / cm 2, and the UV-blocking ability of a 300 to 450 nm region was obtained by using an SPF analyzer (manufactured by Sanyo Corporation). Measured using. In addition, evaluation was performed by the following determination.

Evaluation contents

(Double-circle): SPF is 25 or more.

(Circle): SPF is 20 or more and less than 25.

(Triangle | delta): SPF is 15 or more and less than 20.

X: SPF is less than 15.

`` Cosmetic uniformity '', `` Natural finish (no haze) '', `` Cosmetic persistence (no adhesion and color change) '' and `` feeling '':

20 cosmetic evaluation panel used powder foundations of cosmetics 1 to 5 and comparative cosmetics 1 and 2 of the present invention, "uniformity of the cosmetic film", "natural finish (no cloudy appearance)", "cosmetic persistence (adhesion) No grade and color change) ”and“ usability ”were evaluated by each of seven levels according to the following evaluation criteria, and each sample was given a rating. Next, each product was determined from the average point of the rating of all panels according to the following criteria. Moreover, "usability" evaluated the smoothness at the time of application | coating.

Evaluation standard;

(Evaluation): (Content)

6: very good

5: good

4: somewhat good

3: normal

2: somewhat poor

1: bad

0: very bad

Criteria;

(Average score of the rating): (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 bad)

Less than 1.5: × (bad)

Stability (with or without agglomerates):

Stability was evaluated by the presence or absence of aggregates. About the powder foundation of the cosmetics 1-5 and comparative cosmetics 1 and 2 of this invention shape | molded by the resin dish, the surface state after rubbing the surface 20 times using the cosmetic sponge was visually observed. In addition, evaluation was performed by the following determination.

Evaluation contents

(Double-circle): Aggregate is not observed.

(Circle): Although an aggregate is observed, the quantity is small.

(Triangle | delta): Aggregate is observed and the quantity is large.

X: A large aggregate is observed and the quantity is large.

As shown in Table 4, the powder foundation of the cosmetics 1 to 5 of the present invention has a high SPF value, excellent UV blocking ability, uniformity of the makeup film, natural finish (no cloudiness), makeup persistence (adhesiveness and color change). None), stability (with or without agglomerates), usability (smoothness during application) were excellent powder foundations.

On the other hand, the powder foundation of the comparative cosmetics 1 which replaced the product 1 of the cosmetics 1 of this invention with the conventional fine particle titanium oxide composite mica showed the aggregation of powder, and was inferior to the uniformity of a makeup film, natural finish, etc. Moreover, the powder foundation of the comparative cosmetics 2 which replaced the product 1 of the cosmetics 1 of the present invention with the comparative product 3 had a low SPF value, was inferior to UV blocking ability, and was inferior to all items, such as a feeling of use (smoothness at the time of application). .

Example 22

Powder Foundation (2):

The powder foundation of the cosmetics 6-9 of this invention was prepared by the prescription | regulation of Table 5, and the following method using the particulate zinc oxide composite high flat cellulose powder prepared in Examples 6-9. In the same manner as in Example 21, UV powder, SPF value, uniformity of the makeup film, natural finish (without turbidity), makeup sustainability, usability and stability were examined for this powder foundation. As a comparison, a fine particle zinc oxide coated mica / barium sulfate composite (40% mica, 50% zinc oxide, barium sulfate 10%) (Comparative cosmetics 3) and a highly flat cellulose powder were used (RONAFLAIR SHADELEAF A Merck Co., Ltd.). A mixture (comparative cosmetic 4) using a mixture of zinc oxide and particulates (comparative product 4) was used. This result is also shown in Table 5.

(Manufacturing method)

After mixing components 1 to 17 for 10 minutes in a Henschel mixer, components 18 to 22 are added and stirred for 5 minutes. Then, it grind | pulverizes in an atomizer (1HP screen diameter 1.5mm (phi)), it fills in a resin plate, 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 makeup film, natural finish (without cloudy phenomenon), makeup persistence, and stability (with or without agglomerates). ), All the items of usability (smoothness during application) were excellent powder foundations.

On the other hand, the powder foundation of Comparative Cosmetic 3 which replaced the product 6 of the cosmetics 6 of the present invention with the fine particle zinc oxide coated mica / barium sulfate composite powder showed cohesion of powder, and was inferior to uniformity, natural finish, etc. of a makeup film. Moreover, the powder foundation of the comparative cosmetics 4 which replaced the product 6 of the cosmetics 6 of this invention with the comparative product 4 had a low SPF value, was inferior to UV blocking ability, and was inferior to all items, such as a usability (smoothness at the time of application).

Example 23

Powder Foundation (3):

The powder foundation of the cosmetics 10-13 of this invention was prepared by the prescription of Table 6 and the following method using the titanium oxide complex high flat cellulose powder (products 10-13) manufactured in Examples 10-13. About this powder foundation, the concealability was performed by the following method, and the uniformity, makeup persistence, and usability of a makeup film were investigated similarly to Example 21. In addition, as a comparison, a mixture of high flat cellulose powder and titanium oxide (comparative cosmetics 5 and 6) was used. This result is also shown in Table 6.

(Manufacturing method)

After mixing components 1-16 for 10 minutes in a Henschel mixer, components 17-19 are added and stirred for 2 minutes. Then, it grind | pulverizes in an atomizer (1HP screen diameter 1.5mm (phi)), it fills in a resin plate, and obtains a powder foundation.

(Test Methods)

Concealability:

20 panelists specializing in cosmetic evaluation use powder foundations of cosmetics 10 to 13 and comparative cosmetics 5 and 6 of the present invention, and each of the seven levels of "cloaking" is evaluated according to the following evaluation criteria. Was given. Next, each product was determined from the average point of the rating of all panels according to the following criteria.

Evaluation standard;

(Evaluation): (Content)

6: very good

5: good

4: somewhat good

3: normal

2: somewhat poor

1: bad

0: very bad

Criteria;

(Average score of the rating): (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 bad)

Less than 1.5: × (bad)

As shown in Table 6, the powder foundation of the cosmetics 10-13 of this invention was the powder foundation which was excellent in all the items of the uniformity, concealability, makeup persistence, and usability (smoothness at the time of application) of a makeup film.

On the other hand, Comparative Cosmetic 5 in which titanium oxide of about the same mass as that of Cosmetics 10 of the present invention is mixed and mixed with other components without treatment, has a poor dispersion of titanium oxide, poor makeup sustainability, concealability and feeling of use (when coating (Smoothness) was also inferior. Moreover, although the concealment property was shown by the comparative cosmetics 6 which double-blended titanium oxide, the usability (smooth at the time of application), the uniformity of a makeup film, and the makeup lasting property were bad.

Example 24

Powder Foundation (4):

The powder foundation of the cosmetics 14 and 15 of this invention was prepared by the prescription of Table 7 and the following method using the titanium oxide and iron oxide composite high flat cellulose powder (products 14 and 15) manufactured in Examples 14-15. About this powder foundation, the color development property and the uniformity, makeup persistence, and usability of the makeup film were investigated similarly to Example 21 in the following method.

(Manufacturing method)

After mixing components 1 to 13 for 10 minutes in a Henschel mixer, components 14 to 16 are added and stirred for 3 minutes. Then, it grind | pulverizes in an atomizer (1HP screen diameter 1.5mm (phi)), it fills in a resin plate, and obtains a powder foundation.

(Test Methods)

Chromaticity:

20 cosmetic evaluation panels were made to use powder foundations of cosmetics 14 to 15 and comparative cosmetics 7, 8 of the present invention, and each of the "coloring properties" was evaluated in seven steps according to the following evaluation criteria. Was given. Next, each product was determined from the average point of the rating of all panels according to the following criteria.

Evaluation standard;

(Evaluation): (Content)

6: very good

5: good

4: somewhat good

3: normal

2: somewhat poor

1: bad

0: very bad

Criteria;

(Average score of the rating): (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 bad)

Less than 1.5: × (bad)

As shown in Table 7, the powder foundation of the cosmetics 14 and 15 of this invention was the powder foundation which was excellent in all the items of the uniformity, concealability, makeup persistence, and usability (smoothness at the time of application) of a makeup film.

On the other hand, Comparative Cosmetics 7 and 8 which mix | blended the mixture which mixed and mixed titanium oxide and iron oxide with cellulose powder were especially bad in color development and makeup persistence.

Example 25

Powder Foundation (5):

Using the fine particle zinc oxide composite high flat cellulose powder (product 7) prepared in Example 7, the powder foundation of the cosmetics 16 of this invention was prepared by the prescription of Table 8, and the following method. For this powder foundation, the SPF value was determined in the same manner as in Example 21, and the UV blocking ability, the uniformity of the makeup film, the natural finish (no turbidity), the makeup persistence, the stability (with or without agglomerates), the feeling of use (coating Poem smoothness). In addition, as a comparison, the cosmetics (comparative cosmetic 9) which used the flat cellulose powder and the fine particle zinc oxide mixture of the comparative example 4 were used. The results are shown in Table 8.

(Manufacturing method)

A: The components 1-12 are mixed for 10 minutes in a Henschel mixer.

B: The components 13-18 are added to said A, and it mixes for 4 minutes.

C: The B is pulverized in an atomizer (1HP screen diameter 1.5mmφ).

D: 60 parts of hard-flowing paraffin and C100 part are mixed, it is filled in a resin dish, it shape | molds, it is dried at 70 degreeC, and a powder foundation is obtained.

(Measured SPF Value)

Evaluation was made by the following method based on the "SPF Measurement Standard (2007 revised edition)" set by the Japan Cosmetics Industry Association.

First, 10 subjects were selected from healthy men and women 18 to 60 years of age corresponding to Fitzpatrick's skin types I, II, and III. Except for those taking drugs (such as anti-inflammatory drugs, hypertensives, etc.) involved in photosensitivity). As the test site, a site having a substantially uniform skin color without pigmentation, birthmarks, or the like was selected as the back of the test subject. The test sample was apply | coated to 50 cm <2> of this test part. The coating amount was 2.00 mg / cm 2 ± 2.5% / cm 2.

The test sample application part 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 solar simulator has a continuous spectrum close to sunlight in the UV-B and UV-A regions having a wavelength of 290 to 400 nm. In addition, the ultraviolet-ray with a wavelength of 290 nm or less was removed as much as possible using a filter.

16 to 24 hours after irradiating the ultraviolet rays, the occurrence of red spots on the ultraviolet irradiated portion was examined in a sufficiently bright room. At least 2/3 of the irradiated site, the minimum amount of ultraviolet irradiation that initially causes some red spots with clear boundaries was defined as the minimum red spot amount (MED). Using MED in a test sample application part and a non-coating part, respectively, the SPF value of each subject was calculated | required by the following formula, it was arithmetic-averaged, and it was set as actual SPF value.

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

As shown in Table 8, the powder foundation of the cosmetics 16 of the present invention has a higher SPF measurement value than the comparative cosmetics 9, and has excellent UV blocking ability, uniformity of the makeup film, natural finish (no cloudy appearance), and makeup sustainability ( All items of adhesion and no color change), stability (with or without agglomerates), and usability (smoothness during application) were excellent powder foundations.

On the other hand, the powder foundation of the comparative cosmetics 9 which replaced the product 7 of the cosmetics 16 of this invention with the laurolysine treatment high flat cellulose powder / particulate zinc oxide mixture has a somewhat low SPF measurement value and UV blocking ability, All items 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, a powder foundation was prepared in the following manner by the composition shown in Table 9 below (prescriptions 1 to 3). As a comparison, the thing which used the iron oxide which did not give special treatment was used (comparative prescription). In addition, the total amount of iron oxide in each prescription in a present Example is that composition 1 is the same amount (100%) as a comparative prescription, and compositions 2 and 3 are 80% of a comparative prescription.

<Manufacturing Method>

A: The components 1-13 are mixed for 10 minutes by Henschel mixer.

B: The components 14-20 are added to A, and it mixes for 5 minutes.

C: B is pulverized with an atomizer (1 HP screen diameter 1.5 mmφ).

D: 60 parts of hard-flowing paraffins and C100 parts are mixed, and it is made to dry at 70 degreeC after filling molding in a resin dish, and a powder foundation is obtained.

About each obtained composition, "color development property", "cosmetic persistence (no color fading)", and "cosmetic persistence (adhesiveness)" were investigated. Makeup persistence (adhesiveness) was investigated in the same manner as in Example 21. In addition, about "chromic property", what apply | coated each powder foundation of the state shape | molded by the said manufacturing method to each cosmetic foundation on the upper arm inner part about "cosmetic persistence (no color fading)" was applied to each exterior color. The a and b or L, a and b were measured using a spectrophotometer SE-2000 (Nihon Denshoku Kogyo Co., Ltd.) and evaluated as follows. The results are shown in Table 10.

Chromaticity:

About each prescription, the value of each measured a and b was compared with the values (as and bs) of a and b of the comparative prescription, and the difference (Δa and Δb) was obtained. After this Δa and Δb were squared and added, the value was developed in a square root, and the value was taken as an evaluation value of "color development". About this evaluation value, 1 or more evaluated (circle) and 0.5 or more and less than 1, (circle) and 0.25 or more and less than 0.5 evaluated (triangle | delta) and less than 0.25 as x.

Makeup persistence (no fading):

Immediately after application and 2 hours after application, the values of L, a and b of the appearance of the present invention and the comparative prescription were determined. The square immediately after coating and the difference between the measured value is applied after 2 hours _(0-2 ΔL, Δa Δb _0-2 and _0-2) in each regimen, respectively, and then combined them together, was developed as a square root. This value was made into the evaluation value of "cosmetic persistence (no fading)." About this evaluation value, 0 or more and 1 or less evaluated (circle) and 1 or more and 1.5 or less that 0, 1.5 or more and 2 or more and (triangle | delta) and 2 or more as x.

As shown in Table 10, using the product 14 of Example 14, Formulation 1 in which the comparative prescription and the same mass of iron oxide were blended in the entire prescription, the color development was higher than that of the comparative prescription, and the color faded two hours after application. This was small and was excellent in adhesiveness. In addition, Formula 2, which reduced the compounding amount of iron oxide from Formula 1 and made the compounding amount of iron oxide 80% of the comparative prescription, is superior in color development and superior in other items, even though the compounding amount of iron oxide is smaller than that of the comparative prescription. It was. Using the product 15 of Example 15, similarly to the prescription 2, the formulation 3 in which the compounded amount of iron oxide was 80% of the comparative formulation was also excellent in color development and excellent in other items.

Example 27

2nd floor lotion:

The two-layer lotion of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-3 are mixed.

The components 4-9 were added to (2) and (1), it stirred uniformly, and the two-layer lotion was obtained.

The obtained two-layer lotion was a two-layer lotion which was excellent in powder dispersibility and excellent in the smooth usability and the uniformity of a makeup film.

Example 28

latex:

The emulsion of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-7 are mixed uniformly at 80 degreeC.

(2) The components 8-14 are uniformly mixed at 80 degreeC.

(3) To (1), (2) is added and emulsified.

(4) and (3) were cooled, stirring, homogeneous mixing was carried out after addition of the component 15, and the emulsion was obtained.

The obtained milky lotion was the milky lotion which was excellent in emulsion stability, and was excellent in the smooth usability, the uniformity of a makeup film, and UV blocking ability.

Example 29

cream:

The cream of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-7 are mixed uniformly at 80 degreeC.

(2) The components 8-13 are mixed uniformly at 80 degreeC.

(3) To (1), (2) is added and emulsified.

(4) and (3) were cooled and stirred, and cream was obtained.

The obtained cream was excellent in emulsion stability, and was a cream excellent in the smooth usability, the uniformity of a makeup coat, and UV blocking ability.

Example 30

Serum:

The cosmetic liquid of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-10 were mixed-dissolved at normal temperature, and the cosmetic liquid was obtained, stirring.

The obtained cosmetic liquid was excellent in stability, and was a cosmetic liquid excellent in the smooth usability, the uniformity of a makeup coat, and UV blocking ability.

Example 31

pack:

The pack of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-4 are mixed uniformly at 80 degreeC.

(2) The components 5-12 are mixed uniformly at 80 degreeC.

(3) To (1), (2) is added and emulsified.

It cooled by stirring (4) and (3), and the pack was obtained.

The obtained pack was excellent in emulsion stability, and was a pack which was excellent in the smooth usability and the uniformity of a makeup coat.

Example 32

Face wash:

The face wash of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-7 are mixed uniformly at 80 degreeC.

(2) The components 8-11 are mixed uniformly at 80 degreeC.

(3) To (1), (2) is added and neutralized.

The component 12 is added to (4) and (3), and it mixes uniformly.

It cooled by stirring (5) (4) and obtained the face wash.

The obtained face wash was a face wash excellent in the smooth usability.

Example 33

cleansing cream:

The cleansing cream of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-8 are mixed uniformly at 80 degreeC.

(2) The components 9-14 are mixed uniformly at 80 degreeC.

(3) To (2), (1) is added and emulsified.

It cooled by stirring (4) and (3), and cleansing cream was obtained.

The obtained cleansing cream was excellent in emulsion stability and was a cleansing cream excellent in the smooth usability.

Example 34

Hair wax:

The hair wax of the composition shown below was manufactured by the following method.

(quite)

(1) Components 1 to 3 are uniformly mixed at 80 占 폚.

(2) The components 4-8 are mixed uniformly at 80 degreeC.

(3) To (1), (2) is added and emulsified.

After component 9-16 was added to (4) and (3), it cooled with stirring, and hair wax was obtained.

The obtained hair wax was excellent in emulsion stability and hairstyling property, and was a hair wax excellent in the smooth usability and UV blocking ability.

Example 35

Oily eyeliner:

The oily eyeliner of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-4 are warmed at 100 degreeC, and are mixed uniformly.

(2) The components 5-9 are warmed to 80 degreeC, and uniformly mixed.

(3) The above-mentioned (2) is added to the above (1), and the mixture is homogeneously mixed.

(4) and (3) were processed with the roller and oily eyeliner was obtained.

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

Example 36

Water based eyeliner:

An aqueous eyeliner of the composition shown below was produced by the following method.

(quite)

(1) Components 1 to 5 are uniformly dispersed in a roller.

(2) The components 6-10 are mixed uniformly.

(3) Said (1) was added to said (2), it mixed uniformly, and the aqueous eyeliner was obtained.

The obtained aqueous eyeliner was an aqueous eyeliner excellent in the smooth usability, the uniformity of a makeup coat, and the makeup lasting effect.

Example 37

Eye Brow:

The eye brow of the composition shown below was manufactured by the following method.

(quite)

(1) Components 1 to 4 are uniformly mixed.

(2) The components 5-10 are processed by a roller.

(3) After adding (2) and components 11 and 12 to said (1), it mixed uniformly and obtained the eye brow.

The obtained eye brow was an eye brow excellent in the smooth usability, the uniformity of a makeup film, and the makeup lasting effect.

Example 38

O / W type mascara:

O / W type mascara of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-8 are mixed uniformly at 80 degreeC, and a roller process is carried out.

(2) The components 9-14 are mixed uniformly at 80 degreeC.

(3) To (1), (2) is added and emulsified.

(4) and (3) were cooled and mascara (O / W) was obtained.

The obtained O / W type mascara was O / W type mascara which was excellent in powder dispersibility, and was excellent in the smooth usability, the uniformity of a makeup film, and the makeup lasting effect.

Example 39

Non-aqueous mascara:

The non-aqueous mascara of the composition shown below was manufactured by the following method.

(quite)

(1) Components 1 to 5 are heated to 110 占 폚.

The components 6-9 are added and mixed with (2) and (1).

The components 10-13 are added and mixed with (3) and (2).

(4) and (3) were processed with the roller and the non-aqueous mascara was obtained.

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

Example 40

Stick form lipstick:

Stick-type lipsticks having the composition shown below were prepared by the following method.

(quite)

(1) The components 1-7 are uniformly melt-mixed at 100 degreeC.

The components 8-13 are added to (2) and (1), and it mixes uniformly.

(3) and (2) were put into the container, and it cooled, and obtained the stick form lipstick.

The obtained stick type lipstick was a lipstick which was excellent in the smooth usability, the uniformity of a makeup film, and the makeup lasting effect.

Example 41

Liquid Rouge:

Liquid loose of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-5 are melt-mixed uniformly at 100 degreeC.

The components 6-12 are added to (2) and (1), and it mixes uniformly.

(3) and (2) were poured into the container, and it cooled, and obtained liquid loose.

The obtained liquid rouge was a liquid rouge which was excellent in the smooth usability, the uniformity of a makeup coat, and the makeup lasting effect.

Example 42

O / W Foundation:

The O / W type foundation of the composition shown below was manufactured by the following method.

(quite)

(1) Components 1 to 8 are uniformly dispersed in the roller.

(2) Components 9 to 12 are uniformly mixed.

(3) The above-mentioned (1) is added to the above (2), and the mixture is homogeneously mixed.

(4) Components 13 to 19 are mixed and dissolved at 80 占 폚.

(5) The above-mentioned (4) is added to the above-mentioned (3) at 80 캜 and emulsified.

(6) and (5) were cooled, and component 20 was added and the O / W type foundation was obtained.

The obtained O / W type foundation was O / W type foundation which was excellent in powder dispersibility, and was excellent in the smooth usability, the uniformity of a makeup film, hiding property, UV blocking ability, and the makeup lasting effect.

Example 43

W / O Foundation:

The W / O type foundation of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-3 are mixed uniformly.

(2) The components 4-11 are uniformly dispersed by a roller.

(3) To (1), (2) is added and uniformly mixed.

The components 12-15 were added and emulsified in (4) and (3), and the W / O type foundation was obtained.

The obtained W / O-type foundation was W / O-type foundation which was excellent in powder dispersibility, and was excellent in the smooth usability, the uniformity of a makeup film, hiding property, UV blocking ability, and makeup lasting effect.

Example 44

O / W Eye Color:

The O / W type eye color of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-5 are mixed uniformly at 80 degreeC.

The components 6-8 are added to (2) and (1), and it emulsifies.

(3) The components 9-14 are disperse | distributed uniformly in a roller.

(3) and (15) were added to (4) and (2), and O / W type eye color was obtained.

The obtained O / W eye color was excellent in powder dispersibility, and was O / W eye color excellent in the smooth usability, the uniformity of a makeup film, color development, and a makeup lasting effect.

Example 45

Oily Solid Form Foundation:

The oil-based solid form foundation of the composition shown below was manufactured by the following method.

(quite)

(1) Components 7 to 13 are dissolved by heating at 90 占 폚.

(2) Components 1 to 6 are added to the above (1) and dispersed uniformly on the roller.

The component 14 was added to (3) and (2), and after melt | dissolving at 80 degreeC, it filled into the metal dish and obtained the oil-based solid foundation.

The obtained oil-based solid form foundation was an oil-based solid form foundation which was excellent in powder dispersibility, and was smooth also with the uniformity, UV blocking ability, and makeup lasting effect of a makeup coat.

Example 46

Stick form concealer:

The stick form concealer of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-5 are dissolved by heating at 90 degreeC.

The components 6-12 are added to (2) and (1), and it disperse | distributes uniformly by a roller.

The component 13 was added to (3) and (2), and after melt | dissolving at 80 degreeC, it filled into the container and obtained the stick form concealer.

The obtained stick form concealer was the stick form concealer which was excellent in powder dispersibility, and was excellent in the smooth usability, the uniformity of a makeup film, hiding property, UV blocking ability, and makeup lasting effect.

Example 47

Body milk:

The body milk of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-7 are melt | dissolved uniformly at 80 degreeC.

(2) The components 8-16 are melt | dissolved uniformly at 80 degreeC.

(3) To (2), (1) is added and emulsified.

After component 17 was added and uniformly mixed to (4) and (3), it stirred and cooled, and body milk was obtained.

The obtained body milk was excellent in emulsion stability, and was a body milk which was excellent in the smooth usability, the uniformity of a makeup film, UV blocking ability, and the makeup lasting effect.

Example 48

conditioner for hair:

The conditioner of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-5 are mixed uniformly at 80 degreeC.

(2) The components 6-9 are mixed uniformly at 80 degreeC.

(3) To (1), (2) is added and emulsified.

The component 10 was added to (4) and (3), and it stirred and cooled after homogeneous mixing, and obtained the conditioner.

The conditioner obtained was excellent in emulsion stability, and was a conditioner excellent in the smooth usability.

Example 49

Hair pack:

The hair pack of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-6 are mixed uniformly at 80 degreeC.

(2) The components 7-9 are mixed uniformly at 80 degree | times.

(3) To (1), (2) is added and emulsified.

The component 10 was added to (4) and (3), and it stirred and cooled after homogeneous mixing, and obtained the hair pack.

The obtained hair pack was excellent in emulsion stability, and was a hair pack excellent in the smooth usability.

Example 50

W / O sunscreen:

The sunscreen of the composition shown below was manufactured by the following method.

(quite)

(1) Components 1 to 5 are uniformly dispersed in a roller.

The components 6-9 are added to (2) and (1), and it mixes uniformly.

The components 10-14 were added and emulsified in (3) and (2), and the W / O-type sunscreen agent was obtained.

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

Example 51

manicure:

The nail polish of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-9 were mixed uniformly and the nail polish was obtained.

The obtained nail polish was excellent in powder dispersibility, and was a nail polish excellent in the smooth usability, the uniformity of a makeup coat, and the makeup lasting effect.

Example 52

Makeup base:

The makeup base of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-4 are melt | dissolved uniformly at 80 degreeC.

(2) The components 5-12 are melt | dissolved uniformly at 80 degreeC.

(3) The said (1) is added to said (2), and it emulsifies.

The components 13-14 were added to (4) and (3), it mixed, it cooled, and the make-up base was obtained.

The obtained makeup base was the base which was excellent in emulsion stability, and was excellent in the smooth usability, the uniformity of a makeup film, UV blocking ability, and the makeup lasting effect.

Example 53

Percentage:

The powder of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-5 and 8-10 are mixed uniformly.

The components 6 and 7 are added to (2) and (1), and it mixes uniformly.

(3) The said (2) was grind | pulverized in the grinder, and white powder was obtained.

The obtained white powder was white powder which was excellent in powder dispersibility, and was excellent in the smooth usability, the uniformity of a makeup film, UV blocking ability, and the makeup lasting effect.

Example 54

Solid Powder Foundation:

Solid powder foundation of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-7, 11-13 are mixed uniformly.

The components 8-10 are added to (2) and (1), and it mixes uniformly.

(3) The above (2) is pulverized in a crusher.

(4) and (3) were filled in the metal dish, and the solid powder type foundation was obtained.

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

Example 55

Solid Powder Cheek:

The solid powder type teak of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-4, 7-9 are mixed uniformly.

The components 5 and 6 are added to (2) and (1), and it mixes uniformly.

(3) The above (2) is pulverized in a crusher.

(4) and (3) were filled in the metal dish, and the solid powder type teak was obtained.

The obtained solid powder type | mold teak was excellent in powder dispersibility, and was the teak which was excellent in the smooth usability, the uniformity of a makeup film, UV blocking ability, and the makeup lasting effect.

Example 56

Solid Powder Eyeshadow:

Solid powder eye shadow of the composition shown below was manufactured by the following method.

(quite)

(1) The components 1-6 and 10-12 are mixed uniformly.

The components 7-9 are added to (2) and (1), and it mixes uniformly.

(3) The above (2) is pulverized in a crusher.

(4) and (3) were filled in the metal dish, and the solid powder type foundation was obtained.

The obtained solid powder eye shadow was a foundation which was excellent in powder dispersibility and was excellent in the smooth usability, the uniformity of a makeup film, the coloring property, and the makeup lasting effect.

The metal oxide composite high flat cellulose powder of the present invention is a metal oxide of talc or sericite, which is a conventional flat inorganic material, because cellulose itself, which is a base material, is organic and is flat, and its surface is complexed with extremely fine metal oxide particles. Compared with the powder composited with, the adhesiveness is high, there is an excellent usability, and the UV blocking ability and the coloring property by a metal oxide are also excellent.

Therefore, although the metal oxide composite high flat cellulose powder of this invention can be used for many cosmetics, especially the cosmetics which the effect is easy to express include powder components, such as powder foundation, eye shadow, a blusher, powdered powder, and an oily component. Cosmetics to be mentioned. Of these cosmetics, press-filled cosmetics are preferable, and powder foundation and eye shadow are particularly preferable. When the cosmetic composition of the present invention is used as a powder foundation and eye shadow, there is no powder blowing, and the wetness and adhesion to the skin are good, and as a result, it is naturally familiar with the skin, so that stains, dullness, dullness of color, lifting, etc. No makeup persistence is good.

Claims (20)

A metal oxide composite high flat cellulose powder obtained by mechanically pulverizing a cellulose substance, a grinding aid, and a metal oxide. The metal oxide composite high flat cellulose powder according to claim 1, wherein the average particle diameter is 1 to 50 µm, the average thickness is 0.1 to 10 µm, and the flatness is 4 to 200. The metal oxide composite high flat cellulose powder according to claim 1 or 2, wherein the amount of the metal oxide in the total is 5 to 50% by mass. The metal oxide composite high flat cellulose powder according to any one of claims 1 to 3, 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 mechanical grinding is performed by a planetary ball mill. The method according to any one of claims 1 to 5, wherein the cellulosic material is wood or wood pulp in the form of fiber or powder of wood origin, or cotton or linter in the form of fiber or powder of cotton origin. linter) a metal oxide composite high flat cellulose powder, which is a cellulose-based material selected from the group consisting of fibers and fiber or powder form thereof. The metal oxide complexed flat cellulose powder according to any one of claims 1 to 6, wherein the grinding aid is selected from the group consisting of amphiphiles, amino acids and fatty acids. 8. The metal oxide complexed flat cellulose powder according to claim 7, wherein the amphipathic substance is selected from the group consisting of phospholipids, ceramides, cholesterol or derivatives thereof and phytosterol or derivatives thereof. 8. The metal oxide complexed flat cellulose powder according to claim 7, wherein the amino acids are selected from the group consisting of N-acylamino acid and theanine. 8. The metal oxide complexed flat 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. The metal oxide composite high flat cellulose powder according to any one of claims 1 to 11, wherein the average particle diameter of the composite metal oxide is 10 to 100 nm. The metal oxide composite high flat cellulose powder according to any one of claims 1 to 11, wherein the average particle diameter of the complexed metal oxide is more than 100 nm and 1000 nm or less. Cosmetics containing the metal oxide composite high flat cellulose powder in any one of Claims 1-13. 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, blusher, powdered powder, sunscreen or makeup base. A method for producing 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. 18. The method for producing a metal oxide composite high flat cellulose powder according to claim 17, wherein the amount of the metal oxide added is 5 to 50 mass% in total. The method for producing a metal oxide composite high flat cellulose powder according to claim 17 or 18, wherein the amount of the grinding aid added is 0.5 to 5 mass% in total. 20. The method for producing a metal oxide composite high flat cellulose powder according to any one of claims 17 to 19, wherein mechanical grinding is performed by a planetary ball mill.

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