KR20130139830A - Sheet-shaped cerium oxide and petal-shaped cerium oxide powder which is aggregate of the sheet-shaped cerium oxide, process for production of the sheet-shaped cerium oxide and the petal-shaped cerium oxide powder, coated sheet-shaped cerium oxide and petal-shaped cerium oxide powder which is aggregate of the coated sheet-shaped cerium oxide, and cosmetic - Google Patents

Abstract

Disclosed is a cerium oxide cerium powder having an average particle size of less than 20 占 퐉, a petal cerium oxide cerium powder as an aggregate thereof, and a process for producing the cerium oxide cerium powder. Also provided is a process for producing High cosmetic effect, high ultraviolet shielding effect, and excellent feeling.
(Solution) The aqueous solution containing cerium nitrate, cerium nitrate, sodium hydrogencarbonate or sodium carbonate and water is adjusted so that the molar ratio of carbonate ion to sediment ion is in the range of 1.5 to 5, and the temperature of the aqueous solution is adjusted to 0 to 40 Cerium carbonate particles are precipitated from the aqueous solution and further calcined to obtain cerium oxide particles having an average particle size of less than 20 mu m and an average aspect ratio of 2 to 80 and cerium oxide cerium oxide particles as an aggregate thereof.

Description

FIELD OF THE INVENTION [0001] The present invention relates to a cerium oxide powder and a petal-shaped cerium oxide powder which is an aggregate thereof, a production method thereof, a coated cerium oxide cerium and a petal-shaped cerium oxide cerium powder which is an aggregate thereof, POWDER WHICH IS AGGREGATE OF THE SHEET-SHAPED CERIUM OXIDE, PROCESS FOR PRODUCTION OF THE SHEET-SHAPED CERIUM OXIDE AND THE PETAL-SHAPED CERIUM OXIDE POWDER, COATED SHEET-SHAPED CERIUM OXIDE AND PETAL-SHAPED CERIUM OXIDE POWDER WHICH IS AGGREGATE OF THE COATED SHEET-SHAPED CERIUM OXIDE, AND COSMETIC}

The present invention relates to a particulate cerium oxide powder and a petal-shaped cerium oxide powder as an aggregate thereof, a process for producing the same, a particulate cerium oxide powder and a petal-shaped cerium oxide cerium powder aggregate, A cerium powder or a coated cerium oxide cerium and a petal cerium oxide cerium powder as an aggregate thereof.

Conventionally, inorganic ultraviolet shielding agents such as a salicylic acid compound, a benzophenone compound-based organic ultraviolet screening agent, titanium oxide, and metal oxide fine particles such as zinc oxide have been used as an ultraviolet shielding agent for use in ultraviolet shielding cosmetics. Among them, organic UV-ray shielding agents are colorless and have transparency when compounded in cosmetics, so they are generally used, but they are low in molecular weight, and thus they are absorbed into skin.

On the other hand, titanium oxide, which is well used as an inorganic ultraviolet shielding agent, is chemically stable but has a large hiding power (high refractive index), which limits its use to products requiring transparency. In addition, zinc oxide is characterized by high UV shielding ability and high transparency in the visible light region. However, zinc oxide has a property of being dissolved in a trace amount in the original water and zinc ions eluted by sweat etc. may penetrate into the skin, This is a concern when you need more safety for your organization.

For this reason, inorganic ultraviolet shielding agents using a cerium compound having relatively high transparency among inorganic ultraviolet shielding agents have been studied. For example, in Patent Document 1, cerium oxide particles or cerium-containing composite oxide particles having an average primary particle diameter of 1 nm to 500 nm, or an ultraviolet shielding agent obtained by coating the surface of these composite materials with an amorphous or crystalline inorganic compound has been proposed. However, the composite cerium oxide particles described in Patent Document 1 have a problem that the feeling of use is poor because they have cohesion because they have ultraviolet shielding ability but are fine particles.

On the other hand, as an inorganic ultraviolet shielding agent having a good feeling of use, the incorporation of a platelike particle and a cerium oxide powder has been investigated. For example, in Patent Document 2, an ultraviolet absorbing composition comprising barium sulfate, whose surface is coated with a metal oxide such as cerium oxide Has been proposed. However, in the cerium oxide coated barium sulfate barium particles as described in Patent Document 2, the plate-shaped barium sulfate barium particles have insufficient ultraviolet shielding ability, so that there is a problem that the ultraviolet shielding ability that can be satisfied as composite plate particles can not be obtained.

Japanese Patent Laid-Open No. 2001-139926 Japanese Patent Laid-Open No. 10-8028

SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned problems, and it is an object of the present invention to provide a cerium oxide powder having an average particle diameter of less than 20 탆, a petal-shaped cerium oxide powder as an aggregate thereof, and a manufacturing method of the powder . It is another object of the present invention to provide a cosmetic which has high ultraviolet shielding effect and excellent feeling in use by blending this platy cerium oxide and the petal cerium oxide powder as an aggregate into a cosmetic.

In order to achieve the above object, the inventors of the present invention have made intensive research efforts, and as a result, have found that cerium nitrate, cerium chloride, sodium hydrogencarbonate or sodium carbonate and a mixture of cerium and carbonate ions in an aqueous solution of water in a molar ratio of 1: 1.5 to 1: And cerium oxide cerium oxide having an average primary particle diameter of less than 20 占 퐉 or a cerium oxide powder having a petal shape as an aggregate thereof is obtained by firing petal cerium carbonate octahydrate which is a mixture of cerium carbonate and cerium carbonate obtained by precipitation from an aqueous solution It is possible to obtain a sieve. The surface of the resulting cerium oxide or cerium oxide powder, which is an aggregate thereof, is treated with a compound such as polysiloxane, alkylsilane compound, alkyl titanate compound or fluorine compound to obtain a powder having hydrophobicity, , The present inventors have found that a cosmetic composition having a high ultraviolet shielding effect and an excellent feeling of use can be provided, thereby completing the present invention.

That is, the cerium oxide plate according to the first aspect of the present invention and the petal-shaped cerium oxide powder,

(Average primary particle size / average thickness) of from 2 to 80. The average particle size of the toner particles is not particularly limited.

The method for producing the cerium oxide plate of the second invention and the petal-shaped cerium oxide powder which is an aggregate thereof is a production method of the cerium oxide plate of the first invention and the petal-shaped cerium oxide powder which is an aggregate thereof, , An aqueous solution containing sodium hydrogencarbonate or sodium carbonate and water is adjusted so that the molar ratio of carbonate ion to cerium ion is in the range of 1.5 to 5 and the temperature of the aqueous solution is maintained within the range of 10 to 40 ° C, Cerium carbonate particles are precipitated from an aqueous solution and further calcined.

The method for producing the flaked cerium oxide powder according to the third invention and the method for producing the petal-shaped cerium oxide powder as the aggregate according to the third invention is a method for producing the flaked cerium oxide powder and the petal- , An aqueous solution containing sodium hydrogencarbonate or sodium carbonate and water is adjusted so that the molar ratio of carbonate ion to cerium ion is in the range of 1.5 to 5 and the temperature of the aqueous solution is maintained within the range of 0 to 10 ° C, Cerium carbonate particles are precipitated from an aqueous solution and further calcined.

In the second invention or the third invention, it is preferable that an alcohol compound is contained in the aqueous solution (the fourth invention).

The cerium oxide of the fifth invention and the petal cerium oxide powder, which is an aggregate thereof,

The surface of the platelet-shaped cerium oxide powder of the first invention and the petal-shaped cerium oxide powder aggregate as the aggregate of the first invention can be replaced with a polysiloxane represented by the following formula (1), an alkylalkoxysilane compound represented by the following formula (2) (3), a fluorinated compound represented by the following general formula (4), the following general formula (5) and the following general formula (6) .

Wherein m is an integer of 1 or more, and n is an integer of 0 or more. R ₁ to R ₃ may be hydrogen, an alkyl group, an alkoxyl group or a phenyl group and may be the same]

[Wherein R ₁ and R ₂ are a saturated hydrocarbon group having 1 or more carbon atoms]

Wherein R ₁ and R ₂ are a saturated hydrocarbon group having 1 or more carbon atoms. A and b are each an integer of 1 to 3, and have a relationship of a + b = 4. The alkyl group represented herein may be linear or branched, and may be either single or double chain.

Wherein R ₁ is a saturated hydrocarbon group having 1 or more carbon atoms and n is an integer of 1 or more,

Wherein n is an integer of 4 or more, m is 1 or 2, and M is an alkali metal, ammonium group or diethanol ammonium group.

[Wherein n is an integer of 4 or more, and M is an alkali metal, ammonium group or diethanolammonium group]

The cosmetic material according to the sixth invention is obtained by blending the cerium oxide of the first invention and the petal cerium oxide powder as the aggregate or the coated cerium oxide of the fifth invention and the petal cerium oxide cerium powder as the aggregate It is characterized by.

(Effects of the Invention)

According to the present invention, it is possible to provide a cerium oxide powder having an average primary particle diameter of less than 20 占 퐉 and a petal-shaped cerium oxide powder which is an aggregate thereof, and the cerium oxide cerium and the petal cerium oxide powder as an aggregate thereof can be cerium nitrate or cerium chloride By precipitating and growing cerium carbonate octahydrate particles in a solution, a mixture of sodium hydrogencarbonate or sodium carbonate and water, and firing the particles.

The cosmetic composition comprising the cerium oxide plate of the first invention and the petal cerium oxide powder as the aggregate or the cerium oxide cerium coated by the fifth aspect of the present invention and the petal cerium oxide powder as the aggregate thereof has an ultraviolet screening effect In addition, it becomes good cosmetics feeling.

1 is a scanning electron micrograph of a cerium oxide powder prepared in Example 1. Fig.
FIG. 2 is a scanning electron micrograph of petal-shaped cerium oxide powder, which is a plate-like aggregate prepared in Example 2. FIG.
3 is a scanning electron micrograph of the cerium oxide powder prepared in Comparative Example 1. Fig.
4 is a scanning electron micrograph of the cerium oxide powder prepared in Comparative Example 2. Fig.
5 is a scanning electron micrograph of the cerium oxide powder prepared in Comparative Example 3. Fig.

Next, specific embodiments of the platelet-shaped cerium oxide powder and the petal-shaped cerium oxide powder according to the present invention, the production method thereof, the coated platelet-shaped cerium oxide and the aggregated petal-shaped cerium oxide-coated cerium powder, .

The platy cerium oxide of the present invention and the petal cerium oxide cerium powder aggregate thereof are cerium oxide powders having an average primary particle diameter of less than 20 占 퐉. In the present invention, the average thickness of the cerium oxide powder is preferably 0.2 to 4 mu m. When the average thickness is less than 0.2 탆, the thickness of the obtained cerium oxide powder becomes insufficient, so that it is easily broken. On the other hand, if it exceeds 4 mu m, the visible light transparency decreases.

In addition, the average primary particle diameter of the cerium oxide plate of the present invention and the petal-shaped cerium oxide powder as an aggregate thereof was observed with a scanning electron microscope (SEM), and the number of the plate- (Long diameter and short diameter) of the platelet-shaped particles constituting the petal-like particles of the aggregate are measured and the average value is calculated.

The average thickness of the platy cerium oxide of the present invention and the petal-shaped cerium oxide powder as an aggregate thereof was observed with a scanning electron microscope (SEM), and the petal shape particles as the aggregate were observed, and arbitrary 20 plate- Measuring the thickness of the plate-like particles constituting the petal-shaped particles of the aggregate, and calculating the average value thereof.

In the present invention, the aspect ratio (average primary particle diameter / average thickness) of the platy cerium oxide and the petal cerium oxide powder as an aggregate thereof is 2 to 80. When the aspect ratio is less than 2, which is the lower limit value, the obtained cerium oxide powder does not become a plate. On the other hand, if the upper limit of 80 is exceeded, the resulting cerium oxide powder does not have a thickness sufficient to maintain the particle shape.

The process for producing the flaked cerium oxide powder of the present invention and the petal-shaped cerium oxide powder aggregate of the present invention is characterized in that the molar ratio of sodium carbonate or sodium carbonate to cerium ion in the cerium nitrate or cerium chloride solution is 1: 1.5 to 1: 5 And cerium carbonate particles are precipitated and grown by leaving the temperature of the mixed solution in the range of 0 to 40 DEG C for 30 minutes or more to obtain cerium carbonate octahydrate and firing the cerium carbonate octahydrate to obtain a plate- (In the case of 0 to 10 占 폚, the petal-shaped cerium oxide which is an aggregate of the platy cerium oxide and the cerium oxide in the case of 10 to 40 占 폚 are obtained).

The molar ratio of the carbonate ion to the cerium ion is preferably larger than 1.5 and smaller than 5 from the viewpoints of the plate-like and petal-like shape retention and production efficiency. When the molar ratio of carbonate ion to cerium ion is less than 1.5, the yield is decreased and the productivity is lowered and the shape of the plate-like particles becomes irregular. When the molar ratio of carbonate ion to cerium ion exceeds 5, the ionic strength is too high and the particles are aggregated.

As the solvent for dissolving cerium nitrate or cerium chloride, sodium hydrogencarbonate or sodium carbonate, water may be used, but a mixed solvent containing water may be used. As the solvent to be mixed with water, any of water-soluble compounds may be used, but an alcohol compound is preferable. Examples of the alcohol compound include monohydric alcohols such as methanol, ethanol, propanol and butanol, and polyhydric alcohols such as polyethylene glycol, ethylene glycol, polyethylene and glycerin.

When such an alcohol-based mixed solvent is used, the mass ratio of the alcohol-based solvent to the water in the solvent is preferably within a range of less than 50%, more preferably within a range of 30% It is mine. When the mass ratio is 50% or more, sodium hydrogencarbonate or sodium carbonate does not dissolve, and the uniformity of the resulting platelet-like phase and the petal-shaped cerium oxide powder as the aggregate is lowered.

With respect to the temperature of the mixed liquid, when the temperature is less than 0 ° C, the progress of the growth reaction of the cerium carbonate particles in the mixed liquid is slowed, so that the platy cerium oxide powder of the platelets and aggregates thereof can not be obtained in a sufficient yield. On the other hand, when the temperature of the mixed solution exceeds 40 캜, the progress of the growth reaction of the cerium carbonate octahydrate particles is accelerated, so that the particles are elongated and have a needle-like shape. Therefore, Can not be obtained. When the time for growing the cerium carbonate particles is less than 30 minutes, the cerium carbonate octahydrate particles obtained during the growth of the particles deteriorate the crystallinity and the irregularly shaped particles are formed. Therefore, A powder can not be obtained.

The calcining temperature is preferably in the range of 350 ° C to 1000 ° C, more preferably 400 ° C to 700 ° C, as the conditions for firing the petal-shaped cerium carbonate octahydrate particles as the plate and its aggregate. If the calcination temperature is lower than the lower limit of 350 占 폚, it is not completely oxidized and cerium carbonate octahydrate tends to remain. If the calcination temperature exceeds the upper limit of 1000 占 폚, sintering of the particles tends to proceed. The firing time is preferably within a range of 0.5 to 5 hours.

Next, the hydrophobic platy cerium oxide powder according to the present invention and the petal-shaped cerium oxide powder as an aggregate thereof will be described. The hydrophobic platelet-shaped cerium oxide powder of the present invention and the petal-shaped cerium oxide powder as the aggregate of the present invention can be produced by mixing the above-mentioned polysiloxane, alkylsilane compound, alkyl A titanate compound, a fluorine compound, or the like.

In addition to these compounds, various conventional surface treatments can be carried out. It is also possible to use a plurality of these processes in combination.

Further, as a treatment method of coating the surface of a hydrophobic compound, the pigment to be coated is stirred in a suitable mixer, and the surface-coated compound is added by droplet spraying or spraying, Followed by aging at a temperature of 80 to 200 DEG C while continuing the stirring, so that the reaction surface coating treatment is generally performed. Or surface-coated compounds are dissolved in an alcohol such as ethanol, isopropyl alcohol or isobutanol, a hydrocarbon-based organic solvent such as toluene, n-hexane or cyclohexane, or a polar organic solvent such as acetone, ethyl acetate or butyl acetate , A method in which the pigment for cosmetics is added and stirred in the solution while stirring, the organic solvent is completely evaporated and removed, and then the solution is aged at 80 to 200 ° C to effect the reaction surface coating treatment.

The mixed dispersion method may be appropriately selected depending on the concentration and viscosity of the solution. Preferred examples thereof include a method using a mixer such as a dispenser, a Henschel mixer, a redesigner mixer, a kneader, a V-type mixer, a roll mill, a bead mill and a twin-screw kneader or a spray drying method in which water and an aqueous solution and a pigment are sprayed into heated air And the like. In the case of pulverization, a conventional pulverizer such as a hammer mill, a ball mill, a sand mill or a jet mill may be used. And any one of these pulverizers can be obtained with the same quality, so that it is not particularly limited.

In this case, the mass ratio of the component which is a compound used in the surface coating treatment of the pigment is preferably 0.5 to 30 mass% with respect to the pigment to be coated. When the mass ratio is less than 0.5 mass%, the long lasting effect and the uniform adhesion to the skin are not sufficient. If the mass ratio is more than 30 mass%, the texture tends to be very bundled and wet.

Next, the cosmetic composition according to the present invention will be described. The cosmetic of the present invention has an excellent ultraviolet shielding effect by blending the petal-shaped cerium oxide powder of the above-described plate of the present invention and its aggregate. Further, since the petal-shaped cerium oxide powder of the plate and its aggregate of the present invention is cerium oxide having an average primary particle size of less than 20 占 퐉, the cosmetic compounded with this powder is superior to the conventional cosmetics containing cerium oxide The feeling of good texture is good. The formulations of cosmetics can be used for skin care cosmetics such as emulsions and lotions, makeup cosmetics such as foundations and lipsticks, hair cosmetics and the like. The blending amount is not particularly limited, but is preferably 0.1 to 70 mass%.

In the cosmetic preparation according to the present invention, the effect is remarkable by combining the organic ultraviolet screening agent and the fine inorganic ultraviolet screening agent. As the organic ultraviolet shielding agent, one or two or more selected from oxybenzone, octyl methoxycinnamate, 4-tert-4'-methoxybenzoylmethane, and diethylaminohydroxybenzoylbenzoate are preferable. The compounding amount of the organic ultraviolet screening agent is not particularly limited, but is preferably 0.1 to 40% by mass. The inorganic ultraviolet shielding agent of the fine particles is preferably titanium oxide and / or zinc oxide, more preferably fine titanium oxide and / or zinc oxide having an average particle diameter of 0.05 탆 or less. The blending amount of the inorganic ultraviolet screening agent of the fine particles is not particularly limited, but is preferably 0.1 to 50 mass%.

The cosmetics of the present invention may be added to cosmetics usually used in cosmetics such as powders, surfactants, emulsions, gelling agents, polymers, cosmetic ingredients, moisturizers, pigments, preservatives and perfumes in a range that does not impair the effects of the present invention .

As the form of the cosmetic of the present invention, any of formulations such as powder, liquid, cream, stick, solid, spray, multi-layer separation type may be used.

(Example)

Hereinafter, the present invention will be described in more detail with reference to examples and comparative examples, but the present invention is not limited to the following examples.

(Example 1)

And 54.6 parts by mass of sodium hydrogencarbonate were dissolved in 1200 parts by mass of water, and the mixture was stirred for 200 revolutions of a three-one motor. 197.7 parts by mass of cerium chloride aqueous solution (cerium concentration: 18.7% by mass) was added to the solution, and the molar ratio of cerium ion to carbonate ion was 1: 4.3 The mixture was stirred at a temperature of 18 캜 for one hour, The cerium carbonate octahydrate particles were recovered by filtration from the obtained hydrate solution, washed and dried, and then the cerium carbonate cerium octahydrate particles were calcined in the air at a temperature of 400 DEG C for 1 hour to obtain a platelike oxidation Cerium powder was obtained.

The cerium oxide powder obtained in Example 1 was observed with a scanning electron microscope (SEM). An SEM photograph of the obtained cerium oxide powder is shown in Fig. As shown in the figure, it was confirmed that the obtained cerium oxide powder was a plate-like particle. Further, arbitrary 20 pieces of the cerium oxide plate bodies in Fig. 1 were observed to measure the average primary particle diameter and average thickness of the cerium oxide plate powder body. As a result, it was confirmed that the average primary particle size of the cerium oxide powder was 7.1 mu m and the average primary particle size was less than 20 mu m. It was also confirmed that the average thickness of the cerium oxide powder was 0.51 占 퐉 and was within the range of 0.2 to 4 占 퐉. It was also confirmed that the aspect ratio (average primary particle diameter / average thickness) of the cerium oxide powder was 13.9.

(Example 2)

A petal-shaped cerium oxide powder as an aggregate of the platelet-shaped particles was obtained in the same manner as in Example 1 except that the temperature of the mixed solution was changed to 7 캜.

The cerium oxide powder obtained in Example 2 was observed with an SEM. An SEM photograph of the obtained cerium oxide powder is shown in Fig. As shown in the figure, it was confirmed that the obtained cerium oxide powder had a large amount of petal-shaped cerium oxide powder as an aggregate of the platelike particles. In addition, the plate-like cerium oxide constituting any of 20 petal-shaped cerium oxide powders in Fig. 2 was observed to measure the average primary particle diameter and the average thickness of the cerium oxide plate. As a result, it was confirmed that the average primary particle size of the cerium oxide powder was 2.1 탆, the average thickness was 0.41 탆, and the aspect ratio was 5.1. Incidentally, the average particle diameter of the petal-shaped cerium oxide powder as an aggregate of the cerium oxide particles was 5.4 占 퐉.

(Example 3)

A cerium oxide powder was obtained in the same manner as in Example 1 except that 1200 parts by mass of water and 60 parts by mass of polyethylene glycol (average molecular weight: 200) were used instead of 1200 parts by mass of water.

The cerium oxide powder obtained in Example 3 was observed by SEM. The cerium oxide powder was a cerium oxide powder having an average primary particle diameter of 18.7 占 퐉, an average thickness of 1.2 占 퐉 and an aspect ratio of 15.6 .

(Example 4)

A cerium oxide powder was obtained in the same manner as in Example 1 except that the cerium chloride solution was added instead of the three-one-one-round rotation of 200, and the mixture was allowed to stand without stirring.

The cerium oxide powder obtained in Example 4 was observed by SEM. The cerium oxide powder was a cerium oxide powder having an average primary particle diameter of 4.7 mu m, an average thickness of 0.34 mu m, and an aspect ratio of 13.8 .

(Comparative Example 1)

A cerium oxide powder was obtained in the same manner as in Example 1 except that the temperature of the mixed solution was changed to 43 캜.

The cerium oxide powder obtained in Comparative Example 1 was observed with an SEM. The cerium oxide powder thus obtained is shown in Fig. As shown in the figure, it was confirmed that the cerium oxide powder obtained in Comparative Example 1 was an elongated needle-shaped powder.

(Comparative Example 2)

Cerium oxide powder was obtained in the same manner as in Example 1 except that the amount of sodium hydrogencarbonate was changed to 16.8 parts by mass instead of 54.6 parts by mass of sodium hydrogencarbonate. The molar ratio of cerium ion to carbonate ion in the prepared aqueous solution was 1: 1.33.

The cerium oxide powder obtained in Comparative Example 2 was observed with an SEM. The cerium oxide powder thus obtained is shown in Fig. As shown in the figure, it was confirmed that the cerium oxide powder obtained in Comparative Example 2 was a large particle having an average particle diameter of 20 mu m or more.

(Comparative Example 3)

Cerium oxide powder was obtained in the same manner as in Example 1, except that sodium hydrogencarbonate (67.2 parts by mass) was used instead of sodium hydrogencarbonate (54.6 parts by mass). The molar ratio of cerium ion to carbonate ion in the prepared aqueous solution was 1: 5.33.

The cerium oxide powder obtained in Comparative Example 3 was observed with an SEM. The cerium oxide powder thus obtained is shown in Fig. As shown in the figure, the cerium oxide powder obtained in Comparative Example 3 was indefinite particles, and it was confirmed that aggregation was observed.

(Production Example 1: Production Example of Silicon Compound-coated Cerium Oxide)

1000 parts by mass of the platelike cerium oxide obtained in Example 1 was put in a Henschel mixer, and then a solution prepared by dissolving 20.4 parts by mass of methylhydrogenpolysiloxane in 125 parts by mass of isopropyl alcohol was mixed dropwise and mixed well with the plate-like cerium oxide. Thereafter, the Henschel mixer was heated and reduced in pressure to remove isopropyl alcohol. The pigment powder was taken out from the Henschel mixer, pulverized and subjected to a heat treatment to obtain titanium oxide treated with 2 mass% of the silicon compound. Titanium oxide, cericite, talc, mica, red iron oxide, iron oxide black and iron oxide black were subjected to the same surface coating treatment in the same process to obtain respective samples.

(Production Example 2: Production example of alkylsilane compound coated cerium oxide)

A sample was obtained in the same manner as in Production Example 1 except that n-octyltriethoxysilane was used in place of the methylhydrogenpolysiloxane of Production Example.

(Production Example 3: Preparation Example of Alkyl Titanate Compound-coated CeO 2)

A sample was obtained in the same manner as in Production Example 1, except that isopropyltriisostearoyl titanate was used in place of the methylhydrogenpolysiloxane of Production Example.

(Production Example 4: Production Example of fluorine compound coated cerium oxide)

A sample was obtained in the same manner as in Production Example 1 except that tridecafluorooctyltriethoxysilane was used instead of the methylhydrogenpolysiloxane of Production Example.

In order to confirm the water repellency and oil repellency of the pigment powder for cosmetic preparation according to this example, the contact angles of the cerium oxide particles prepared in Production Examples 1 to 4 with water and the contact angle with liquid paraffin were measured with a Goniometer And measured using an expression contact angle measuring apparatus. Table 1 shows the measurement results of the contact angles of Production Examples 1 to 4.

From the results shown in Table 1, it was possible to obtain platelike oxide having good water repellency and oil repellency by coating the water repellent compound on the surface.

(Example 5: preparation of powder foundation)

Powder foundation was obtained according to the prescription shown in Table 2 and the following manufacturing method. In addition, the unit of the amount in the table is mass%.

Preparation Method: Component B, which is uniformly heated and dissolved while mixing well with a mixer, is slowly added to the mixture, which is further mixed and pulverized. After passing through a mesh, the mixture is shaped into a gold plate using a mold ≪ / RTI >

(Comparative Example 4)

A product was obtained in the same manner as in Example 5 except that the silicon-treated particulate titanium oxide was used in place of the silicon-treated platelet-like cerium oxide prepared in Production Example 1.

(Comparative Example 5)

A product was obtained in the same manner as in Example 5, except that the silicon-treated particulate zinc oxide was used in place of the silicon-treated platelet-like cerium oxide prepared in Production Example 1.

(Comparative Example 6)

A product was obtained in the same manner as in Example 5, except that the silicon-treated particulate cerium oxide was used in place of the silicon-treated platy cerium oxide prepared in Production Example 1. The cerium oxide fine particle used in Comparative Example 6 is Sari Guide SC-6832 manufactured by Daito Kasei Co., Ltd.

Each of the cosmetics prepared in Example 5 and Comparative Examples 4 to 6 was subjected to a sensory evaluation test on sensation of use by 10 female panelists. The test was conducted in the form of a questionnaire, and the score between 0 and 5 was assigned to each item. The score was evaluated as 0 for poor evaluation and 5 for excellent evaluation, and the result was expressed as a mean score of the entire panelist. Therefore, the higher the score, the better the evaluation. In addition, the cosmetic material was applied in the form of applying the composition after using a foundation makeup in the form of an emulsion. The results are shown in Table 3.

From the results shown in Table 3, Example 5 was excellent in both feeling of use, transparency, and ultraviolet ray shielding effect (ultraviolet ray shielding effect) when applied. In Comparative Example 4, since the titanium dioxide fine particle with silicon was added, it was excellent in ultraviolet ray shielding effect (ultraviolet ray shielding effect), but was inferior in feeling and transparency when applied. Further, in Comparative Example 5, since the silicone-treated fine particle zinc oxide was blended, the transparent feeling and the ultraviolet ray-shielding effect (ultraviolet ray shielding effect) were excellent, but the application feeling after application was poor. Further, in Comparative Example 6, since the cerium oxide microparticles were compounded, the result was poor in transparency and ultraviolet ray shielding effect (ultraviolet shielding effect), but was poor in feeling when applied. Cerium. ≪ / RTI >

(Example 6)

W / O type liquid foundation was prepared according to the prescription shown in Table 4 and the following manufacturing method. In addition, the unit of the amount in the table is mass%.

Preparation method: Component B was mixed well using a mixer. On the other hand, Component A was heated at 80 DEG C and mixed well to make it uniform. Component B was slowly added thereto with stirring, and the mixture was gradually cooled to 50 占 폚 (slow cooling). Subsequently, Component C was heated at 80 占 폚 to dissolve uniformly, and then slowly cooled to 50 占 폚. Component C was added to Component A under stirring, and the mixture was further stirred and cooled to room temperature. The resulting solution was charged into a container to obtain a product.

The obtained liquid foundation was excellent in both feeling of use, transparency and ultraviolet shielding effect when applied with a liquid foundation.

(Example 7)

The W / O type ultraviolet-shielding cosmetic was started (trial) according to the prescription shown in Table 5 and the following manufacturing method. In addition, the unit of the amount in the table is mass%.

Preparation method: Component A was heated at 80 DEG C and mixed well to make it uniform. Component B was slowly added thereto with stirring, and then slowly cooled to 50 캜. Subsequently, Component C was heated at 80 占 폚 to dissolve uniformly, and then slowly cooled to 50 占 폚. Component C was added to Component A under stirring, and the mixture was further stirred and cooled to room temperature. The resulting solution was charged into a container to obtain a product.

The resulting W / O type ultraviolet barrier cosmetic composition was excellent in both feeling of use, transparency, and ultraviolet shielding effect when applied.

(Example 8)

The O / W type liquid foundation was started according to the prescription shown in Table 6 and the following manufacturing method. In addition, the unit of the amount in the table is mass%.

Preparation method: Components A and C were mixed well at 80 占 폚. Component B was added to Component C with stirring, followed by thorough mixing. Component A was slowly added from above, and after cooling, the mixture was charged into a container to obtain a product.

The obtained O / W type liquid foundation was excellent in both feeling of use, transparency and ultraviolet shielding effect when applied.

The cerium oxide of the present invention and the petal cerium oxide powder as an aggregate of the present invention and the coated powder obtained by coating the powder with the hydrophobic compound are added to cosmetics such as powder foundation and liquid foundation, A cosmetic material having excellent feel, feeling of use, transparency, and ultraviolet shielding effect can be obtained, which is highly likely to be used industrially.

Claims (6)

Wherein the cerium oxide has a mean particle size of less than 20 占 퐉 and an average aspect ratio of 2 to 80, and a petal cerium oxide powder as an aggregate thereof. A process for producing a particulate cerium oxide according to claim 1 and a petal-shaped cerium oxide powder as an aggregate thereof, comprising:
An aqueous solution containing cerium nitrate or cerium chloride, sodium hydrogencarbonate or sodium carbonate and water is prepared so that the molar ratio of carbonate ion to cerium ion is in the range of 1.5 to 5. The temperature of the aqueous solution is adjusted in the range of 10 to 40 ° C And cerium carbonate particles are precipitated from the aqueous solution to further calcine the cerium oxide and a method for producing the petal cerium oxide powder as an aggregate thereof. A process for producing a particulate cerium oxide according to claim 1 and a petal-shaped cerium oxide powder as an aggregate thereof, comprising:
An aqueous solution containing cerium nitrate or cerium chloride, sodium hydrogencarbonate or sodium carbonate and water is prepared so that the molar ratio of carbonate ion to cerium ion is in the range of 1.5 to 5. The temperature of the aqueous solution is adjusted in the range of 0 to 10 ° C And cerium carbonate particles are precipitated from the aqueous solution to further calcine the cerium oxide and a method for producing the petal cerium oxide powder as an aggregate thereof. The method according to claim 2 or 3,
Characterized in that an alcohol compound is contained in the aqueous solution, and a process for producing a petal-shaped cerium oxide powder as an aggregate thereof. The surface of the platy cerium oxide powder and the platelet-like cerium oxide powder as an aggregate of the platelet-like cerium oxide according to claim 1 are replaced by a polysiloxane represented by the following formula (1), an alkylalkoxysilane compound represented by the following formula (2) (3), a fluorinated compound represented by the following general formula (4), the following general formula (5) and the following general formula (6) And cerium oxide powder as an aggregate thereof.

Wherein m is an integer of 1 or more, and n is an integer of 0 or more. R ₁ to R ₃ may be hydrogen, an alkyl group, an alkoxyl group or a phenyl group and may be the same]

[Wherein R ₁ and R ₂ are a saturated hydrocarbon group having 1 or more carbon atoms]

Wherein R ₁ and R ₂ are a saturated hydrocarbon group having 1 or more carbon atoms. A and b are each an integer of 1 to 3, and have a relationship of a + b = 4. The alkyl group represented here may be linear or branched and may be either single or double chain.

Wherein R ₁ is a saturated hydrocarbon group having 1 or more carbon atoms and n is an integer of 1 or more,

Wherein n is an integer of 4 or more, m is 1 or 2, and M is an alkali metal, ammonium group or diethanol ammonium group.

[Wherein n is an integer of 4 or more, and M is an alkali metal, ammonium group or diethanolammonium group] A cosmetic characterized by comprising the cerium oxide plate of claim 1 and a petal cerium oxide powder which is an aggregate thereof, or the coated cerium oxide cerium of claim 5 and a petal cerium oxide cerium powder which is an aggregate thereof.

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