JP5535669B2 - Titanate compound powder and cosmetics - Google Patents

Description

  The present invention relates to a powder composed of particles of a titanate compound having a flat shape useful as a constituent material for coating compositions, films, coating compositions, cosmetics, and the like, and compositions such as cosmetics containing the powder.

Conventionally, mica, talc, glass flakes, MIO (mica-like titanium oxide) and the like have been used as inorganic pigments to be blended in various compositions such as paints, films, coating compositions, and cosmetics. Recently, various synthetic inorganic powders have been used as these pigments or fillers. For example, JP-A-4-321517 discloses flaky potassium titanate particles (K ₂ Ti ₆ O ₁₃ ). It is disclosed that the resulting powder is excellent in spreadability, hiding properties, etc., and can be suitably used as a pigment for paints and cosmetics. JP-A 2000-230168 discloses titanic acid having a certain composition and crystal structure. flaky powder salt _{(a x M y □ z Ti} 2- (x + y)) is a resin filler, it is used as a coating material filling agent is disclosed. JP-A-5-163117 discloses a cosmetic material excellent in spreadability, lubricity, adhesion, hiding property, etc. by blending powder composed of flaky potassium titanate particles as a pigment. Is disclosed.

Japanese Patent Laid-Open No. 2000-230168 JP-A-5-163117

The powder composed of flaky particles of a titanic acid compound, which is a synthetic inorganic compound, has excellent dispersibility and good orientation as a flaky morphological effect as compared with mica, talc and the like derived from natural raw materials. However, these titanic acid compounds contain alkali metal ions (potassium ions, sodium ions, etc.) in the crystals, and the alkali ions are easily eluted. When this is blended in an organic composition such as a paint, a coating composition, or a cosmetic, it causes deterioration and deterioration of the composition, and also causes an influence on the environment and the human body.
The present invention, as a pigment for paints, films, coating compositions, cosmetics, etc., is not accompanied by the above problems, has excellent spreadability, lubricity, adhesion, hiding properties, etc., and has antibacterial properties, rust prevention properties, etc. The present invention provides a titanic acid compound powder provided and a cosmetic prepared by blending the same.

The titanic acid compound powder of the present invention comprises titanic acid compounds A, B, C, D, E or F having the following composition and crystal structure, average size: 1 to 30 μm, average thickness: 0.05 to It is a powder of particles having a flat shape of 3 μm.
In the following description, the element groups of R ₁ and R ₂ are as follows.
R ₁ ... Li, Mg, Ca, Zn, Ni, Cu, Fe, Al
R ₂ ... Li, Mg, Ca, Co, Ni, Cu, Zn, Sr, Ag, Sn, Ba

(A) Titanate compound A
TiO ₆ octahedron has anatase-type crystal structure consisting of four-ridge shared chain, and part of Ti seat is one or more metal ions selected from R ₁ (excluding Ca) element group It is a substituted anatase type titanate compound.

(B) Titanate compound B
It has a layered crystal structure formed by a chain of TiO ₆ octahedrons, a part of the Ti seat is substituted with one or more metal ions selected from the R1 element group, and an R2 element is interposed between crystal layers It is a titanic acid intercalation compound in which one or more metal ions selected from the group are present.

(C) Titanate compound C
Formula MTi _n O _{2n + m / 2}
[Wherein, M: one or more metal elements selected from Li, Mg, Ca, Zn, Ni, Cu, Fe, Al, n: 0.5-2, m: valence of M]
It is a titanic acid compound shown by these.

(D) Titanate compound D
Formula MTi _n O _{2n + m / 2}
[Wherein, M: one or more metal elements selected from Li, Mg, Ca, Zn, Ni, Cu, Fe, Al, n: 0.5-2, m: valence of M]
The titania compound titanate compound in which the crystal phase of the titanate compound (the titanate compound C) and the titania crystal phase (anatase type or rutile type) are combined.
The composite amount ratio (titania compound C crystal phase / titania crystal phase) of the titania composite titanate compound D is, for example, about 1/3 (molar ratio).

(E) Titanate compound E
Formula MTi _n O _{2n + m / 2}
[Wherein, M: one or more metal elements selected from Li, Mg, Ca, Zn, Ni, Cu, Fe, Al, n: 0.5-2, m: valence of M]
A composite titanic acid compound in which two or more crystal phases of the titanic acid compound (the titanic acid compound C) are combined.

(F) Titanate compound F
Formula MTi _n O _{2n + m / 2}
[Wherein, M: one or more metal elements selected from Li, Mg, Ca, Zn, Ni, Cu, Fe, Al, n: 0.5-2, m: valence of M]
And a titanic acid compound (anatase type or rutile type) and a composite titanic acid compound in which two or more crystal phases of the titanic acid compound (the titanic acid compound C) are combined. The composite amount ratio (total amount of titanate compound C crystal phase / titania crystal phase) is, for example, 3/1 (molar ratio).

  The powder comprising the flat particles of the titanate compounds A to F of the present invention has good dispersibility and orientation as a pigment for coating compositions, cosmetics and the like due to the crystal structure, chemical stability and morphological characteristics. In addition to having this as a cosmetic pigment, for example, foundation, eye shadow, blusher, lipstick, nail enamel, etc., it has good spreadability, lubricity, gloss, gloss, firmness, adhesion, hiding In addition to the above-mentioned characteristics, when it is blended with other paints, it brings about improvement effects such as heat resistance and wear resistance of the coating film.

In particular, zinc titanate containing zinc as a constituent element, when applied as a cosmetic pigment, has low irritation to the skin and is suitable as a pigment for cosmetics for sensitive skin. In addition, titanic acid compound B (an intercalation compound in which R ₂ element is introduced between layers) has an antibacterial action when it contains, for example, copper ions or silver ions due to metal ions existing between the layers, and when it contains zinc ions. Demonstrates antibacterial and antirust effects.

  The titanic acid compound powder of the present invention has a flat shape with an average size of 1 to 30 μm and an average thickness of 0.05 to 3 μm. “Size” is an arithmetic mean value of the longest diameter and the shortest diameter of each particle, and “average size” means the median (size corresponding to 50% of the integrated distribution curve). “Average thickness” means the median in the same manner as described above for the thickness of each particle. The average size is specified in the range of 1 to 30 μm. If the size is less than this, the reflectance is low and the glossiness is poor. Conversely, if the grain size is larger than this, the dispersibility is low. This is because the adhesion of paints and cosmetics is lowered, and the effect of improving weather resistance is weakened by paints. Preferably, it is 2-10 micrometers. In addition, the average thickness is specified in the range of 0.05 to 3 μm. If the thickness is less than this, the mechanical strength is poor and the composition is easily crushed during preparation of the composition, and the predetermined flat shape is stably maintained. On the other hand, if the thickness exceeds this range, when used in paints and cosmetics, the smoothness and glossiness of the film surface will be poor. Preferably it is 0.05-1 micrometer. This flat shape is adjusted by wet pulverization of the intermediate product in the powder production process as described later.

Next, each manufacturing process of the titanic acid compounds A to F will be described.
In the following description, the terms “titanium oxide”, “alkali metal oxide”, “R ₁ metal oxide”, “R ₂ metal oxide”, and “M metal oxide” used for the preparation of the raw materials are respectively determined by heating. It is used in the meaning including the compound which produces | generates this metal oxide.

(A) powder production in the titanic acid compound A] [material made tone]
Titanium oxide, alkali metal oxide (K ₂ O, Na ₂ O, Li ₂ O, etc.), and R ₁ (excluding Ca) metal oxide are mixed at a predetermined ratio and mixed uniformly to obtain a starting material. .
When the number of moles of titanium oxide is expressed as m _TiO2 , R ₁ (excluding Ca) , the number of moles of metal oxide is expressed as m _R1 , and the number of moles of alkali metal oxide is expressed as m _ALK , the mixing ratio [(m _TiO 2 + m _R1 ) / m _ALK ] is preferably adjusted to a range of about _{4/1 to 8/1} . When deviating from this range, the generation efficiency of the TiO ₆ octahedral structure is deteriorated.
In steel stock preparation, _{R 1} 2 or more oxides as (but excluding Ca) metal oxides, for example, when magnesium oxide and zinc oxide (ZnO) a (MgO) complexed used, as a product powder, TiO ₆ A titanic acid compound A in which a part of the octahedral Ti seat is substituted with zinc ions and magnesium ions is obtained.

[Primary firing process]
By holding the starting material at a temperature of about 950 to 1250 ° C. for an appropriate time (for example, 2 Hr), a potassium titanate R ₁ (excluding Ca) metal compound having a layered structure as a calcination reaction product (alkaline metal between layers ) A solidified product consisting of ion coordination is obtained. The reason why the treatment temperature is defined in the above range is that the firing reaction cannot be efficiently caused in a low temperature range that is less than that range, while the high temperature treatment exceeding this causes melting of the treated product.

[Alkali metal ion elution treatment]
Immerse the primary firing reaction product (solidified product) in a sufficient amount of water (about 100 times the weight of the solidified product), add an appropriate amount of acid solution such as sulfuric acid, hydrochloric acid, acetic acid, etc. The total amount of alkali metal ions between the layers is eluted.

[Wet grinding process]
In parallel with the elution treatment of the alkali metal ions or after the elution treatment, a wet pulverization treatment is performed. The solidified product is pulverized to some extent with the elution of alkali metal ions, but it cannot be pulverized into flat particles necessary as a product powder by itself. The flat shape (average size and thickness) is adjusted by wet grinding. The wet pulverization treatment can be performed using, for example, a home mixer. In addition, an emulsifying and dispersing machine, a wet ball mill, or the like can be used. As the medium in the wet pulverization, water, an aqueous acid solution, an organic solvent, alcohol or the like can be used, and the amount of the medium may be about 20 to 250 times (weight) the solidified material processing amount.

[Drying process]
After the wet pulverization treatment, the pulverized product is recovered from the liquid, dehydrated, and dried (for example, held at about 100 ° C. for about 24 hours) to obtain a powder composed of flat particles of a hydrated titanate compound.

[Secondary firing process]
The crystal structure is converted by holding the hydrated titanic acid compound powder at about 400 to 600 ° C. for an appropriate time (for example, 2 hours). The reason why the processing temperature is about 400 ° C. or higher is to promote the structural transformation efficiently, and the upper limit is about 600 ° C. If the upper limit is exceeded, the crystalline phase other than the anatase phase precipitates and the intended composite This is because the yield of the compound decreases.
By this baking treatment, a powder composed of flat particles of titanate compound A is obtained.

(2) Powder production of [titanic acid compound B (interlayer compound)] [raw material preparation] to [acquisition of hydrated titanic acid compound powder]
In the production process of the titanic acid compound A, the hydrated titanic acid compound (dry powder) is subjected to the same processing steps as the “preparation of raw materials”, “primary firing treatment”, “alkali metal ion elution treatment”, “wet pulverization treatment” and “drying treatment”. )

[R ₂ metal iontophoresis process]
The dry powder (hydrated titanic acid compound) is immersed in an appropriate amount of water (about 100 times the powder weight). An appropriate amount of R ₂ metal salt (sulfate, hydrochloride, nitrate, etc.) solution was added to this, and the R2 metal ion was introduced between the crystal layers of the hydrated titanate compound by maintaining the solution under moderate stirring conditions for an appropriate time. To do.

[Drying process]
The powder is collected from the treatment liquid, dehydrated, and dried (maintained at about 300 ° C. for about 24 hours) to obtain a powder composed of flat particles of titanate compound B, which is a titanate intercalation compound.

(C) Powder production of [titanic acid compound C] [Preparation of raw materials]
Dry powder of hydrated titanic acid compound through the same processing steps as "preparation of raw materials", "primary firing process", "alkali metal ion elution process", "wet grinding process" and "drying process" in the manufacturing process of titanic acid compound A Get. However, one or more of “M metal oxide” is used instead of “R ₁ metal oxide” for preparing the starting material.
M metal oxide powder is added to the hydrated titanic acid compound powder and mixed uniformly to prepare a raw material. The M element of the M metal oxide to be mixed is the same element as the M element of the dry powder (hydrated titanate compound).

The blending ratio of the hydrated titanic acid compound powder and the M metal oxide powder in the preparation of the raw material varies depending on the valence of M metal, the composition of the hydrate, the composition of the target titanate compound, etc. Although it cannot be defined generally, a specific example is shown below. ( _{M HTIO} represents the molar ratio of the hydrated titanate compound, and mm represents the molar ratio of the M metal oxide).
When M is a monovalent metal and the target product is M ₂ TiO ₃ : m _HTIO / m _M = 1 / 1.5 to 1 / 1.75
・ M is a divalent metal.
When the object is M ₂ TiO ₄ : m _HTIO / m _M = 1 / 2.5 to 1 / 3.25
When the target is MTiO ₃ : m _HTIO / m _M = 1 / 1-1 to 1 / 1.5
When the target is MTi2O5: m _HTIO / m _M = 1 / 0.25 to 1 / 0.625
When M is a trivalent metal and the target product is M ₂ TiO ₅ : m _HTIO / m _M = 1 / 0.5 to 1 / 1.25

[Baking treatment]
The powder mixture is held in a temperature range of 900 to 1300 ° C. for an appropriate time (for example, 2 hours). If the treatment temperature is less than this, it is difficult to efficiently proceed the structural transformation reaction, while in the high temperature range exceeding this, the reaction product may be melted depending on the composition.
As a reaction product by the firing process to obtain a powder of _{MTi n O 2n + m / 2} ( titanate M metal compound) titanate compound consists flat particles C.

(D) Production of powder of [titanic acid compound D (titania composite compound)] [Preparation of raw materials] to [Acquisition of hydrated titanic acid compound powder]
Dry powder of hydrated titanic acid compound through the same processing steps as "preparation of raw materials", "primary firing process", "alkali metal ion elution process", "wet grinding process" and "drying process" in the manufacturing process of titanic acid compound A Get. However, one or more of “M metal oxide” is used instead of “R1 metal oxide” for the adjustment of starting materials.

[Baking treatment]
The dry powder (hydrated titanic acid compound) is subjected to a firing treatment to convert the crystal structure. Since the treatment temperature varies depending on the composition of the object to be treated, it cannot be defined unconditionally, but it can be achieved by maintaining the temperature in a temperature range of about 700 to 900 ° C. for an appropriate time (for example, 2 hours).
This firing process to obtain a powder of _{MTi n O 2n + m / 2} ( titanate M metal compound) crystalline phase titania crystalline phase (anatase type or rutile type) and consists of flat particles bound titanate compound D .

(E) Production of [titanic acid compound E (complex titanic acid compound)] [Preparation of raw materials] to [Acquisition of hydrated titanic acid compound powder]
In the production process of the titanic acid compound A, the hydrated titanic acid compound (dry powder) is subjected to the same processing steps as the “preparation of raw materials”, “primary firing treatment”, “alkali metal ion elution treatment”, “wet pulverization treatment” and “drying treatment”. ) However, instead of “R1 metal oxide”, one or more of “M metal oxide” is used for the preparation of the starting material.

[M metal ion introduction treatment]
The dry powder (hydrated titanic acid compound) is immersed in an appropriate amount of water (about 100 times the powder weight). An appropriate amount of a solution of M metal salt (sulfate, hydrochloride, nitrate, etc.) is added to this, and M metal ions are introduced between the crystal layers of the hydrated titanate compound by holding for an appropriate time under mild stirring conditions. . The element type of the M metal ion introduced between the layers is the same or different from the M metal of the hydrated titanate compound, and is selected according to the composition of the titanate compound E to be produced.

[Drying process]
After the treatment, the powder is recovered from the liquid, dehydrated and dried (maintained at about 300 ° C. for about 24 hours) to obtain a titanic acid intercalation compound powder in which M metal ions are introduced between crystal layers.
[Secondary firing process]
The titanic acid intercalation compound is subjected to a baking treatment for converting the crystal structure. Although the treatment temperature varies depending on the composition of the compound and cannot be defined unconditionally, it is achieved by maintaining the treatment temperature at about 900 to 1300 ° C. for an appropriate time (for example, 2 hours).
By this baking treatment, a titanic acid compound E powder composed of flat particles of a composite compound in which crystal phases of two or more kinds of titanic acid compounds are combined is obtained.

(F) Production of [titanic acid compound F (titania composite compound)] [raw material preparation] to [acquisition of hydrated titanic acid compound powder]
In the production process of the titanic acid compound A, the hydrated titanic acid compound (dry powder) is subjected to the same processing steps as the “preparation of raw materials”, “primary firing treatment”, “alkali metal ion elution treatment”, “wet pulverization treatment” and “drying treatment”. ) However, in preparation of the starting material, one or more of “M metal oxide” is used instead of “R1 metal oxide”.

[M metal ion introduction treatment]
The dry powder (hydrated titanate compound) is subjected to M metal ion introduction treatment to obtain a titanate interlayer compound in which M metal ions are introduced between crystal layers. The metal ion introduction treatment may be performed under the same treatment conditions as those in the production process of the titanate compound E.

[Drying process]
The powder is recovered from the treatment liquid, dehydrated and dried (maintained at about 300 ° C. for about 24 hours) to obtain a powder of titanic acid intercalation compound in which M metal ions are introduced between crystal layers.
[Baking treatment]
The titanic acid intercalation compound is subjected to a baking treatment for converting the crystal structure. Although the treatment temperature varies depending on the composition of the compound and cannot be defined unconditionally, it is achieved by maintaining the treatment temperature at about 900 to 1300 ° C. for an appropriate time (for example, 2 hours).
A composite compound in which the crystal phase of two or more kinds of titanate compounds and a titania crystal phase (anatase type or rutile type) are bonded by the baking treatment (the titania crystal phase has an excess of titanium oxide blended in the starting material). A titanic acid compound F powder consisting of flat particles produced by precipitation as a reaction residue is obtained.

  Preparation of compositions such as paints and cosmetics using the titanate compound powder of the present invention can be performed according to a conventional method except that the titanate compound powder is blended. For example, in the preparation of cosmetics, the titanate compound powder of the present invention is used as a pigment, and general ingredients as cosmetic raw materials, for example, hydrocarbons such as petrolatum and microcrystalline wax, esters such as jojoba oil, beef tallow, olive oil Triglycerides such as cetanol, oleyl alcohol, fatty acids such as stearic acid and oleic acid, high alcohols such as glycerin, various surfactants (nonionic, anionic, cationic, etc.), thickeners ( Ethanol, carbopol, etc.), preservatives, ultraviolet absorbers, antioxidants, color pigments and the like are appropriately used.

  The amount of titanate compound in the preparation of the cosmetic is not particularly different from the case where conventional extender pigments and pearlescent pigments are used. For example, the oily foundation has about 2 to 70% by weight, and the pressed powder has about 15 to 90%. % By weight, 0.1-15% by weight for lipstick, about 1-85% by weight for eye shadow, about 0.1-1% by weight for nail enamel. A conventionally employed method such as a V-type blender, a kneader, a three-roller, or an extruder may be applied according to the type of cosmetic.

  In the preparation of coating compositions, for example, resin coatings, extender pigments can be used as optional additives in addition to the titanic acid compound powders of the present invention to resins that are main ingredients, such as epoxy resins, unsaturated polyester resins, and epoxy acrylate resins. (Talc, silica, barium sulfate, perlite), colored pigment (zinc white, bengara, titanium oxide), anticorrosive pigment (zinc powder, aluminum powder, basic chromate, zinc phosphate), anti-settling agent, thickener, An antifoaming agent, surfactant, diluent, solvent (methyl isobutyl ketone), etc., can be prepared by blending appropriate amounts as necessary and mixing and dispersing with a mixer such as a roll mill. A curing agent / curing accelerator according to the species is added and used for painting. The compounding quantity of a titanic acid compound powder can be about 10-70 weight part with respect to 100 weight part of resin solid content, for example.

[Example 1 (Production of Compound A powder)]
(1) Raw material preparation Each powder of titanium oxide (TiO ₂ ), potassium carbonate (K ₂ CO ₂ ), and zinc oxide (ZnO) was mixed into 60/25/15 (weight ratio) (≈4 / 1/1, molar ratio. ) In a proportion (weight ratio).
(2) Firing treatment The powder mixture is put in an alumina crucible and held at 1100 ° C. for 2 hours in an electric furnace to obtain a solidified product of potassium zinc titanate having a layered crystal structure as a firing reaction product.

(3) Depotassium treatment and wet pulverization treatment The above solidified product is immersed in water (100 times the weight of the solidified product), industrial sulfuric acid is added thereto, and 5 Hr is required with propeller stirring, and potassium between the crystal layers. Elute the total amount of ions. Then, it is pulverized by a home mixer for 10 minutes.
(4) Drying treatment The pulverized material is recovered from the liquid and kept at 100 ° C. for 2 hours.
The obtained dried product is a powder composed of particles of a hydrated titanic acid compound represented by H _0.8 Zn _0.4 Ti _1.6 O ₄ .nH ₂ O.

(5) Calcination treatment The titanate compound powder is put in an alumina crucible and held at 500 ° C. for 2 hours.
As a calcination reaction product, a powder composed of particles of a zinc titanate compound having an anatase type crystal phase in which a part of Ti of TiO ₆ octahedron forming anatase crystal was substituted with zinc ions was obtained.
This powder is white particles having a flat shape with an average size of about 5 μm and an average thickness of about 0.5 μm.

[Example 2 (Production of B compound powder)]
(1) Raw material The dry powder (particles of hydrated titanic acid compound H _0.8 Zn _0.4 Ti _1.6 O ₄ .nH ₂ O) obtained in step (4) of Example 1 was used.
(2) Metal ion introduction treatment The above dry powder is immersed in water (100 times the dry powder weight), 2 mol / L of zinc nitrate solution is added thereto, and 1 Hr is required under a gentle stirring flow to generate zinc ions. Introduce.

(3) Drying treatment Powder is recovered from the above liquid, and after dehydration, maintained at 300 ° C. for 24 hours.
The obtained powder is a powder composed of particles of a zinc titanate intercalation compound in which a part of the Ti site of the TiO ₆ octahedron is substituted with zinc ions and zinc ions are present between the crystal layers.
This powder is white particles having a flat shape with an average size of about 5 μm and an average thickness of about 0.5 μm.

[Example 3 (Production of B compound powder)]
(1) Raw material The dry powder ((hydrated titanic acid compound H _0.8 Zn _0.4 Ti _1.6 O ₄ .nH ₂ O particles) obtained in step (4) of Example 1 was used.
(2) Metal ion introduction treatment The above dry powder is immersed in water (100 times amount, weight), a 2 mol / L lithium nitrate solution is added thereto, and lithium ions are introduced by taking 1 Hr under a gentle stirring flow. .

(3) Drying treatment Powder is recovered from the above liquid, and after dehydration, maintained at 300 ° C. for 24 hours.
The obtained powder is a powder composed of particles of a lithium zinc titanate intercalation compound in which a part of the Ti site of the TiO ₆ octahedron is substituted with zinc ions and lithium ions are present between the crystal layers.
This powder is white particles having a flat shape with an average size of about 5 μm and an average thickness of about 0.5 μm.

[Example 4 (Production of B compound powder)]
(1) Raw material preparation Each powder of titanium oxide (TiO ₂ ), potassium carbonate (K ₂ CO ₂ ), and magnesium hydroxide (Mg (OH) ₂ ) was converted into 62/27/11 (weight ratio) (≈4 / 1 / 1, molar ratio).
(2) Firing treatment The above powder mixture is put in an alumina crucible and held at 1100 ° C. for 2 hours in an electric furnace to obtain a solidified product of potassium magnesium titanate having a layered crystal structure as a firing reaction product.

(3) Depotassium treatment and wet pulverization treatment The above solidified product is immersed in water (100 times the weight of the solidified product), industrial sulfuric acid is added thereto, and 5Hr is required under propeller stirring, and it exists between crystal layers. Elute the total amount of potassium ions. Then, it is pulverized by a home mixer for 10 minutes.

(4) Drying treatment The pulverized material is recovered from the liquid and kept at 100 ° C. for 2 hours.
As a dry powder, a powder composed of particles of a hydrated titanate compound represented by H _0.8 Mg _0.4 Ti _1.6 O ₄ .nH ₂ O is obtained.
(5) Metal ion introduction treatment The above dry powder is immersed in water (100-fold amount, weight), 2 mol / L copper nitrate solution is added thereto, and copper ions are introduced by taking 1 Hr under a gentle stirring flow. To do.

(6) Drying treatment Powder is collected from the treatment solution, and after dehydration, maintained at 300 ° C. for 24 hours.
The obtained powder is a powder composed of particles of a copper-magnesium titanate intercalation compound in which a part of the Ti site of the TiO ₆ octahedron is substituted with magnesium ions and copper ions are present between the crystal layers.
This powder is light blue particles having a flat shape with an average size of about 6 μm and an average thickness of about 0.8 μm.

[Example 5 (Production of C compound powder)]
(1) Preparation of raw material Dry powder (particles of hydrated titanic acid compound H _0.8 Zn _0.4 Ti _1.6 O ₄ .nH ₂ O) obtained in step (4) of Example 1 and zinc oxide (ZnO) powder , 48/52 (weight ratio).
(2) Firing treatment The powder mixture is placed in an alumina crucible and held at 1100 ° C. for 2 hours in an electric furnace. As a calcination reaction product, a powder composed of particles of zinc titanate (Zn ₂ TiO ₄ ) was obtained.
This powder is white particles having a flat shape with an average size of about 6 μm and an average thickness of about 0.7 μm.

[Example 6 (Production of D compound powder)]
(1) Raw material The dry powder (particles of hydrated titanic acid compound H _0.8 Zn _0.4 Ti _1.6 O ₄ .nH ₂ O) obtained in step (4) of Example 1 was used.
(2) Firing treatment The dried powder is put in an alumina crucible and held at 800 ° C. for 2 hours in an electric furnace.
As a firing reaction product, a powder composed of particles of a titania composite zinc titanate compound in which a zinc titanate (ZnTiO ₃ ) crystal phase and a titania (TiO ₂ , anatase) crystal phase were combined was obtained.
This powder is white particles having a flat shape with an average size of about 5 μm and an average thickness of about 0.5 μm.

[Example 7 (Production of E compound powder)]
(1) Raw material The powder of the zinc titanate intercalation compound (titanate compound B) obtained in Example 2 was used.

(2) Firing treatment The powder is put in an alumina crucible and held at 900 ° C. for 2 hours in an electric furnace.
As a calcination reaction product, a powder composed of composite titanate compound particles in which a zinc titanate (ZnTiO ₃ ) crystal phase and a zinc titanate (Zn ₂ TiO ₄ ) crystal phase were combined was obtained.
This powder is white particles having a flat shape with an average size of about 6 μm and an average thickness of about 0.7 μm.

[Example 8 (Production of F compound powder)]
(1) Raw material The powder of the zinc titanate intercalation compound (titanate compound B) obtained in Example 3 is used.

(2) Firing treatment The powder is put in an alumina crucible and held at 1100 ° C. for 2 hours in an electric furnace.
Titanium composite titanic acid compound particles in which zinc titanate (Zn ₂ TiO ₄ ) crystal phase, lithium titanate (Li ₂ TiO ₃ ) crystal phase and titania (TiO ₂ , rutile type) crystal phase are combined as a firing reaction product A powder consisting of
This is white particles having a flat shape with an average size of about 7 μm and an average thickness of about 0.8 μm.

[Example 9 (Preparation of cosmetics)]
Cosmetics (powder foundation) <1>, <2> and <3> having the following composition are prepared using powder <1>, <2> or <3> comprising flat particles of titanic acid compound as pigments.
[Pigment]
・ Titanate powder <1>
Agent type: Zinc titanate (Zn ₂ TiO ₄ ) powder (according to Example 5)
Flat shape: average size 5μm, thickness 0.7μm
・ Titanate powder <2>
Agent type: titania composite titanic acid compound (ZnTiO ₃ —TiO ₂ )
Powder (according to Example 6)
Flat shape: average size 5μm, thickness 0.5μm
・ Titanate compound powder <3>
Agent type: Compound titanic acid compound (ZnTiO ₃ —Zn ₂ TiO ₄ )
Powder (according to Example 7)
Flat shape: average size 6μm, thickness 0.7μm

  All of the cosmetics <1> to <3> are excellent in spreadability, lubricity, gloss, adhesion and feel. In addition, it has antibacterial and rustproof properties and has low irritation to sensitive skin and can be used safely.

Specific examples of the embodiment of the present invention are shown below.
(1) (Titanate Compound A)
One or two or more metals selected from the group of R ₁ (excluding Ca), having anatase-type crystal form composed of TiO ₆ octahedron four-ridge shared chain Powder composed of particles of titanate compound substituted with ions. The particles have a flat shape with an average size of 1 to 30 μm and an average thickness of 0.05 to 3 μm.
(2) The powder of item 1 above, comprising flat particles of a zinc titanate compound in which R ₁ element is zinc.
(3) The powder according to item 1 above, comprising flat particles of a copper titanate compound in which the R ₁ element is copper.
(4) The powder of item 1 above, comprising flat particles of a magnesium titanate compound in which R ₁ element is magnesium.
(5) The powder according to item 1 above, comprising flat particles of an iron titanate compound in which R ₁ element is iron.
(6) The powder of item 1 above, comprising flat particles of an aluminum titanate compound in which R ₁ element is aluminum.
(7) The powder according to the above item (1), comprising flat particles of a lithium titanate compound in which R ₁ element is lithium.
(8) The powder according to the above item 1, comprising flat particles of a zinc copper titanate compound in which R ₁ elements are zinc and copper.

(9) (Titanate Compound B)
Having a layered crystal structure by TiO ₆ octahedra chain, to one not part of Ti seat is selected from the R ₁ element group is substituted with two or more metal ions, from the R ₁ group of elements between crystal layers A powder comprising particles of a titanic acid intercalation compound coordinated with one or more selected metal ions. The particles have a flat shape with an average size of 1 to 30 μm and an average thickness of 0.05 to 3 μm.
(10) The powder as described in 9 above, comprising flat particles of a zinc titanate intercalation compound in which the R ₁ element is zinc and the R ₂ element is zinc.
(11) The powder according to item 9 above, comprising flat particles of a copper zinc titanate intercalation compound in which the R ₁ element is zinc and the R ₂ element is copper.
(12) The powder according to item 9 above, comprising flat particles of a zinc titanate-copper intercalation compound in which the R ₁ element is copper and the R ₂ element is zinc.
(13) The powder according to item 9 above, comprising flat particles of a silver zinc titanate intercalation compound in which the R ₁ element is zinc and the R ₂ element is silver.
(14) The powder of the above item 9 comprising flat particles of a lithium zinc titanate intercalation compound in which the R ₁ element is zinc and the R ₂ element is lithium.
(15) The powder according to the above item 9, comprising flat particles of a lithium titanate intercalation compound in which the R ₁ element is lithium and the R ₂ element is lithium.
(16) The powder of the above item 9 comprising flat particles of a zinc-magnesium titanate intercalation compound in which the R ₁ element is magnesium and the R ₂ element is zinc.

(17) (Titanate Compound C)
_{MTi n O 2n + m / 2} [M, n and m are as defined above] is a powder consisting of particles of titanic acid compound represented by the particles average size: 1 to 30 [mu] m, average thickness: 0. It has a flat shape of 05 to 3 μm.
(18) The powder according to item 17 above, comprising flat particles of a zinc titanate compound in which M is zinc.
(19) The powder according to item 17 above, comprising flat particles of a lithium titanate compound in which M is lithium.
(20) The powder according to item 17 above, comprising flat particles of a magnesium titanate compound in which M is magnesium.
(21) The powder as described in 17 above, comprising flat particles of an aluminum titanate compound in which M is aluminum.
(22) The powder according to item 17 above, comprising flat particles of an iron titanate compound in which M is iron.
(23) The powder according to item 17 above, comprising flat particles of a copper titanate compound in which M is copper.

(24) (Titanate Compound D)
_{MTi n O 2n + m / 2} [M, n and m are as defined above] is a powder consisting of particles of titania composite titanic acid compound and the crystalline phase of the titanate compound represented by the titania crystalline phase bound, The particles have a flat shape with an average size of 1 to 30 μm and an average thickness of 0.05 to 3 μm.
(25) The powder as described in 24 above, comprising flat particles of a titania composite zinc titanate compound in which M is zinc.
(26) The powder as described in 24 above, comprising flat particles of a titania composite lithium titanate compound in which M is lithium.
(27) The powder according to item 24 above, comprising flat particles of a titania composite magnesium titanate compound in which M is magnesium.
(28) The powder as described in 24 above, comprising flat particles of a titania composite aluminum titanate compound in which M is aluminum.
(29) The powder as described in 24 above, comprising flat particles of a titania composite iron titanate compound in which M is iron.
(30) The powder as described in 24 above, comprising flat particles of a titania composite copper titanate compound in which M is copper.

(31) (Titanate Compound E)
MTi _n O _{2n + m / 2} [M, n, and m are as defined above] is a powder composed of a composite titanic acid compound particle in which two or more crystal phases of the titanic acid compound are bonded. It has a flat shape with an average size of 1 to 30 μm and an average thickness of 0.05 to 3 μm.
(32) The powder according to item 31 above, comprising flat particles of a composite zinc titanate compound in which two kinds of zinc titanate crystal phases (for example, ZnTiO ₃ and Zn ₂ TiO ₄ ) in which M is zinc are bonded.
(33) The powder according to item 31 above, comprising flat particles of a composite titanate compound in which a zinc titanate crystal phase in which M is zinc and a lithium titanate crystal phase in which M is lithium are combined.
(34) The powder according to item 31 above, comprising flat particles of a composite titanic acid compound in which a magnesium titanate crystal phase in which M is magnesium and a lithium titanate crystal phase in which M is lithium are bonded.
(35) The powder according to item 31 above, comprising flat particles of a composite titanate compound in which a crystal phase of magnesium titanate in which M is magnesium and a crystal phase of zinc titanate in which M is zinc are combined.

(36) (Titanate Compound F)
MTi _n O _{2n + m / 2} [M, n and m are the same as defined above] A powder composed of particles of titania composite titanate compound in which two or more kinds of titanate compounds and a titania crystal are combined, The particles have a flat shape with an average size of 1 to 30 μm and an average thickness of 0.05 to 3 μm.
(37) The crystal phase of zinc titanate in which M is zinc, the crystal phase of copper titanate in which M is copper, and flat particles of a titania composite titanate compound in which a titania crystal is bonded. Powder.
(38) The powder according to the above item 36, comprising flat particles of a titania composite titanate compound in which a crystal phase (for example, ZnTiO ₃ and Zn ₂ TiO ₄ ) of two types of zinc titanate in which M is zinc and a titania crystal phase are combined. .
(39) The powder of the above item 36, comprising a titanic composite titanic acid flat particle in which a zinc titanate crystal phase in which M is zinc, and a lithium titanate crystal phase in which M is lithium and a titania crystal are bonded.
(40) The crystal phase of magnesium titanate in which M is magnesium, the crystal phase of lithium titanate in which M is lithium and the titania complex titanate flat particles of the titania composite titanate compound, Powder.
(41) The crystal phase of magnesium titanate in which M is magnesium, the crystal phase of zinc titanate in which M is zinc, and flat particles of a titania composite titanate compound in which a titania crystal is bonded. Powder.
(42) A cosmetic comprising any one or more of the titanic acid compound powders according to the above items 1 to 41.

(43) A coating composition obtained by blending any one or more of the titanate compound powders according to the above items 1 to 41.

  The powder composed of flat particles of the titanic acid compound of the present invention is useful as a pigment for paint compositions, film / coating compositions, cosmetics and the like due to its chemical composition, crystal structure, and flat particle shape, and is excellent. It has dispersibility and is excellent in improving effects such as spreadability, concealability, lubricity and adhesion. In addition, intercalation compounds carrying metal ions between crystal layers make the paint composition and cosmetics antibacterial and rust-proof by the action of the ions, and cosmetics containing zinc titanate compounds are sensitive. It can be used safely for skin.

Claims (4)

It has anatase-type crystal form consisting of four-ridge shared chain of TiO ₆ octahedron, and part of Ti seat is one or two metal ions selected from Li, Mg, Zn, Ni, Cu, Fe, Al What titanate compound powder der substituted with seed above, by performing the pulverization treatment of the raw material powder which is performed after the parallel or elution treatment with an alkali metal ion elution process a wet grinding process, the average size: 1 to 30 [mu] m , Titanate compound powder characterized by being flat particles having an average thickness of 0.05 to 3 μm.   A cosmetic comprising one or more titanate compound powders according to claim 1 as a pigment. The coating composition formed by mix | blending 1 type (s) or 2 or more types of the titanic acid compound powder of Claim 1 . The raw material powder is subjected to an alkali metal ion elution treatment after being subjected to a primary firing treatment, and subjected to a pulverization treatment in parallel with the alkali metal ion elution treatment or after the elution treatment, and further to a drying treatment and a secondary firing treatment. Form is TiO ₆ Anatase-type crystal form consisting of octahedral four-ridge shared chain, and one or more metal ions selected from Li, Mg, Zn, Ni, Cu, Fe, and Al, part of Ti seat In the method for producing titanic acid compound powder substituted with
A method for producing titanic acid compound powder comprising flat particles having an average size of 1 to 30 μm and an average thickness of 0.05 to 3 μm by performing the pulverization process by a wet pulverization process.