WO2008059828A1 - Poudre perlée noire et son procédé de fabrication - Google Patents

Poudre perlée noire et son procédé de fabrication Download PDF

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Publication number
WO2008059828A1
WO2008059828A1 PCT/JP2007/071998 JP2007071998W WO2008059828A1 WO 2008059828 A1 WO2008059828 A1 WO 2008059828A1 JP 2007071998 W JP2007071998 W JP 2007071998W WO 2008059828 A1 WO2008059828 A1 WO 2008059828A1
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WO
WIPO (PCT)
Prior art keywords
powder
black
present
titanium
composition
Prior art date
Application number
PCT/JP2007/071998
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English (en)
Japanese (ja)
Inventor
Masahiro Hashimoto
Shingo Okubo
Fukuji Suzuki
Asa Kimura
Original Assignee
Nihon Koken Kogyo Co., Ltd.
Shiseido Company Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
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Application filed by Nihon Koken Kogyo Co., Ltd., Shiseido Company Ltd. filed Critical Nihon Koken Kogyo Co., Ltd.
Publication of WO2008059828A1 publication Critical patent/WO2008059828A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
    • C09C1/0021—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a core coated with only one layer having a high or low refractive index

Definitions

  • the present invention relates to a black pearly luster powder and a method for producing the same, and more particularly to an improvement in the color of a black pigment using low-order titanium oxide.
  • black which is an achromatic color
  • black is in great demand due to its high-quality feeling, but is required to exhibit uniform absorption over the entire wavelength range of visible light. For this reason, it was extremely difficult to produce a pigment that can produce “black” and has good strength and usability.
  • carbon black has a high blackness, but it has a matte texture and lacks a high-class feeling, and there is a drawback that it is possible to obtain a black pearl glaze powder with gloss, particularly pearly luster, and high blackness. It was a long-standing development issue.
  • pearlescent pigments such as titanium dioxide-covered mica, which are pigments utilizing the interference phenomenon of light in addition to colored pigments, are provided.
  • This pearlescent pigment is used in various fields such as paints, cosmetics, adhesives, printing inks, resin kneading, etc., but conventional black pearlescent pigments are coated with black iron oxide and are strong. Since it is magnetic, it has poor dispersion in a substrate such as a paint, so that sufficient gloss cannot be obtained, and when kneaded into a resin, black iron oxide is oxidized by the temperature and turns brown.
  • the dark pearl luster pigment has a good color tone and luster that is close to true black and has a problem that it is extremely difficult to manage because it uses a toxic ammonia stream in the manufacturing process.
  • Patent Document 2 discloses a method of obtaining a colored mica titanium pigment by mixing metallic titanium with titanium mica coated with titanium dioxide.
  • Patent Document 3 discloses a method for obtaining a colored mica titanium-based pigment by reducing titanium dioxide with silicon, titanium hydride, calcium hydride, and carbon.
  • titanium dioxide which is a mica titanium-based pigment
  • the present invention relates to a method for producing a colored mica titanium-based pigment that is colored as an appearance color.
  • Patent Document 4 discloses a method for producing a colored mica titanium-based pigment obtained by reducing titanium dioxide with aluminum oxide.
  • Patent Document 5 discloses a method for producing a colored mica titanium pigment obtained by reducing titanium dioxide with metallic aluminum, manganese, iron, cobalt, nickel, and zinc.
  • a method for producing a force black pearlescent pigment which is known as a method for reducing titanium dioxide without using ammonia. This is because when low-order titanium oxide is produced using titanium metal or the like, “black” is bluish or red is strong, and “true black” cannot be obtained.
  • Patent Document 1 JP-A-58-164653
  • Patent Document 2 Patent No. 1732810
  • Patent Document 3 Japanese Patent Laid-Open No. 6-211521
  • Patent Document 4 JP-A-8-67830
  • Patent Document 5 Patent No. 3542388
  • the present invention has been made in view of the above prior art, and the problem to be solved is to easily produce a low-order titanium oxide black pearly luster powder excellent in color and the black powder. It is to provide a method.
  • the present inventors have attempted to produce a powder having a color tone and luster equivalent to or higher than those of the black pearl luster pigment obtained by ammonia reduction without using ammonia gas.
  • low-order titanium oxide has a dark blue or black color, so the power of reduction using metallic titanium has a dark brown or reddish tone, and is "black” as obtained by ammonia reduction. Nearly! /, The color has been obtained! / ,!
  • the black pearly luster powder according to the present invention is a black pearly luster powder having a surface of a thin plate powder coated with low-order titanium oxide,
  • low-order titanium oxide contains at least Ti 2 O 3 and Ti 2
  • the method for producing a black pearly luster powder according to the present invention includes:
  • Metallic titanium is mixed with pearly luster powder coated with titanium dioxide on a thin plate-like base powder, and reduced under low oxygen conditions until TiO (X ⁇ l.5) is obtained.
  • metallic pearl luster powder in which the thin plate-like base powder is coated with titanium dioxide is mixed, reduced at 700 1000 ° C under low oxygen conditions, and then in an oxidizing atmosphere. It is preferable to oxidize and fire at 200 to 500 ° C.
  • the glitter was evaluated as follows. That is, the powder lg was added to 15 g of Nitron Riya Lacquer Lacquer 6341 manufactured by Musashi Paint Co., Ltd., mixed well, and applied to a black and white underlayer concealment rate test paper with a 4 mil applicator. Then, the glossiness of the coating film on the white ground was measured with Daros Checker IG-300 manufactured by Horiba.
  • the black pearly luster powder that is useful in the present invention has a value of 60 ° and 20 ° of 60 or more.
  • the blackness was evaluated as follows. That is, the powder lg was added to 15 g of 2 Toronto Tariya Lacquer 6341 manufactured by Musashi Paint Co., Ltd., mixed well, and applied to a black and white underlayer concealment rate test paper with a 4 mil applicator.
  • the black pearly luster powder according to the present invention in which the color tone of the coating film on the white ground was measured with a spectrocolorimeter CM-2500d manufactured by Minolta and represented by Hunter's L, a, b color values, It is preferable that the L value (lightness) is 25 or less, the a value is 1.5 or less, and the b value is 0.5 2.9.
  • the hiding power was evaluated as follows. That is, the powder lg was added to 15 g of Nitron Riya Lacquer Lacquer 6341 manufactured by Musashi Paint Co., Ltd., mixed well, and applied to a black and white underlayer concealment rate test paper with a 4 mil applicator. The color tone of the paint film on the white ground and the black ground was measured with a spectrocolorimeter CM-2500d manufactured by Minolta.
  • the black pearly luster powder that is suitable for the present invention preferably has a color difference ⁇ E between white ground and black ground of 1.0 or less when expressed by Hunter's L, a, b color values. .
  • TiO was measured as follows. Titanium coated on powder substrate Is dissolved in hot sulfuric acid and reduced with metallic aluminum to quantify the amount of titanium. From the amount of titanium and the weight increase when the reduced oxidized powder is oxidized at 700 ° C in the atmosphere, The amount of oxygen was quantified.
  • the black pearly luster powder that is effective in the present invention has a TiO X of 1.56 to 1.75.
  • the compound of the reduced oxide powder is recognized as Ti 2 O and Ti 2 as a titanium oxide compound when measured with a Rigaku X-ray diffractometer Miniflex.
  • the thin plate-like substrate powder is preferably selected from natural mica, synthetic mica, aluminum oxide, and silicon oxide, and it is preferable to use a material obtained by coating this substrate powder with titanium dioxide.
  • the pearly luster powder in which the raw material base powder is coated with titanium dioxide is preferably silver-glossy.
  • the metal of the colorless metal oxide and / or the colorless metal hydroxide is selected from silica, alumina and zircoure.
  • the present inventor provides a “coloring gloss composition” comprising the above black pearly luster powder and / or coated black pearly luster powder as a coloring component.
  • This “coloring gloss composition” is a composition that can take various specific embodiments, for example, external compositions such as makeup cosmetics, coating compositions, printing ink compositions, adhesive compositions, and the like. .
  • a black pearly luster composition is applied on a coated surface, and light interference and light of a specific titanium oxide compound are formed on the powder layer formed on the coated surface. It is preferable to make it black pearl luster by absorption.
  • the black pearly luster powder according to the present invention does not substantially contain nitrogen because it has not undergone ammonia reduction, and has excellent blackness and brightness by adjusting the reduction degree with metallic titanium.
  • a black pearly luster powder can be provided.
  • the titanium dioxide-coated powder is once reduced to strength with metallic titanium and then re-oxidized to adjust the degree of reduction.
  • the reduction degree can be adjusted in an open atmosphere, facilitating manufacturing. , Blackness and pearl luster are also good.
  • the black pearly luster powder and / or the coated black pearly luster powder according to the present invention and the method for producing the same are obtained by mixing metallic titanium with pearly luster powder obtained by coating a thin plate-like substrate powder with titanium dioxide, and under low oxygen conditions. It is reduced below and then oxidized and fired in an oxidizing atmosphere, and a black pearly powder is obtained by the light interference action and the light absorption action of a specific titanium oxide compound.
  • the black pearly luster powder of the present invention is a black pearly luster powder compared to the colored pearly luster powder in which the color tone of the conventional pearly luster powder is colored from silver to an interference color. New features are recognized.
  • V a so-called thin plate-like powder coated with titanium dioxide
  • a silvery pearlescent powder is a silvery pearlescent powder.
  • this silver pearly luster powder commercially available silvery pearly luster powder, for example, Iriodin series made by Merck, Madana Pearl series made by Engelhard, Reflex series made by CQV, etc.
  • those produced using a generally known method can be used.
  • a synthetic My power manufactured by Toby Industries a silver pearly luster powder coated with titanium dioxide can be produced by a conventional method and used.
  • the base particles, V, and the so-called thin plate-like powder are selected from natural mica, synthetic mica, aluminum oxide, and key oxide.
  • natural mica and synthetic mica are relatively easy to control the shape and surface uniformity, particle size and distribution, and further, the surface of the particles is uniformly coated with titanium dioxide to give a silvery color.
  • titanium dioxide In terms of producing pearly luster powder! /, It is the preferred material to select as a base particle.
  • a pearlescent pigment that has a nacreous appearance by coating natural mica with a metal oxide such as titanium dioxide or iron oxide has been conventionally known. Since this type of pearlescent pigment is a natural mica, it contains impurities in the mica, so that it has the disadvantage that the color of the color is poor and the extra color is cloudy. Therefore, it is used as a nacreous pigment coated with titanium dioxide, iron oxide, etc. based on synthetic mica, plate-like aluminum oxide, and plate-like oxide that have been free of impurities. It was.
  • the particle diameter of the base particles is not particularly specified, the average particle diameter is preferably 30 m or less.
  • the hiding power covering power: power to hide the ground
  • the ground This is not preferable because it is easily affected by the color and a sufficient black gloss cannot be obtained.
  • These base particles are mixed with silver pearly luster powder coated with titanium dioxide, and metallic titanium is mixed and reduced under low oxygen conditions.
  • the mixing amount of titanium metal is somewhat different depending on the size of the base particles.
  • the mixing amount of titanium metal is preferably 5 mass% to 18 mass%. When the amount is less than 5% by mass, the reduction of titanium dioxide is insufficient, so that even when fired in an oxidizing atmosphere, a black pearlescent powder is not obtained. On the other hand, when the content is 18% by mass, the reduction of titanium dioxide proceeds, and at the same time, the aggregation due to the solid solution becomes strong, and the luster as pearl luster is lost, which is not preferable.
  • the reduction temperature varies depending on the amount of metallic titanium mixed, but is preferably 700 ° C to 1000 ° C. Titanium dioxide cannot be reduced sufficiently below 700 ° C, so even if it is oxidized and fired in an oxidizing atmosphere, it does not become a black pearlescent powder. If the temperature is 1000 ° C or higher, reduction is too advanced, and aggregation due to a solid solution with titanium metal becomes strong, and the glitter as pearl luster is lost.
  • Low-order titanium oxide obtained by reducing titanium dioxide under the above-mentioned low-oxygen conditions is oxidized and fired in an oxidizing atmosphere.
  • the firing temperature varies depending on the degree of reduction.
  • the ability to fire at 200 ° C to 500 ° C preferable. Below 200 ° C, oxidation of low-order titanium oxide does not occur and there is no change in color tone. Above 500 ° C, the oxidation of low-order titanium oxide proceeds excessively, and the low-order titanium oxide returns to titanium dioxide and the color tone becomes silvery pearlescent powder, which is not preferable.
  • the black pearly luster powder obtained under the above conditions can be surface treated in the same manner as conventional pearly luster powder.
  • the light resistance and dispersibility improvement treatment with silica, alumina, zirconia and a mixture thereof was used as the coated black pearl luster powder.
  • aluminum Hydrophobic treatment with titanium or titanium coupling agent examples thereof include hydrophobization treatment with a silicone oil, a fatty acid metal salt, an alkyl phosphate, a fluorine compound having a perfluoroalkyl group, and the like.
  • the black pearly luster powder of the present invention having such extremely excellent properties is very useful as a compounding component of a "coloring glossy composition" which is a glossy composition whose primary purpose is coloring of an object. Are better.
  • the coloring composition for coloring according to the present invention (hereinafter referred to as the coloring composition for coloring according to the present invention! /) Is! In addition to coloring by "", it also includes imparting gloss using light interference.
  • This is a composition having the primary meaning, and its specific embodiment is not particularly limited.
  • a composition for external use such as makeup cosmetics, a coating composition, a printing ink composition, an adhesive composition, etc.
  • the colored gloss composition of the present invention is a gloss composition that can be applied on a coated surface and blackened by causing light interference in a composite powder layer formed on the coated surface. is there.
  • the content of the black pearly luster powder in the colored glossy composition of the present invention can be appropriately selected depending on the specific mode and purpose of the composition, and is not particularly limited.
  • the makeup cosmetics have a particularly beautiful role, an “aesthetic role” that keeps the makeup lasting, a “psychological role” that tightens the mood, and The "protective role” that protects the skin is recognized.
  • the powder which is suitable for the present invention is suitably used for such an external composition.
  • a powder component may be mentioned as a component that plays a central role.
  • the pigment component is used for makeup cosmetics and has a good feel.
  • the above-mentioned “protective role” is fulfilled by providing makeup with persistence, coloring, and, depending on the type, providing an ultraviolet shielding effect.
  • the colored gloss composition of the present invention By adding the colored gloss composition of the present invention to the composition for external use of the present invention, an external composition having good black gloss and drastically improved cosmetic durability is provided.
  • the blending amount of the black pearly luster powder of the present invention in the composition for external use can be appropriately selected according to the dosage form and form of the composition and the purpose of blending the colored glossy composition of the present invention, and is particularly limited. Usually, it is blended in the composition in the range of about 0.;! To 80.0% by weight.
  • composition for external use of the present invention other components which are usually blended in cosmetics can be blended as long as the desired effects of the present invention are not impaired.
  • solid or semi-solid oils such as petrolatum, lanolin, ceresin, carnauba wax, candelillaro, higher fatty acids, higher alcohols, fluid oils such as squalane, liquid paraffin, ester oil and triglyceride, oils such as silicone oil, hyaluronic acid Moisturizers such as sodium and daricerine, surfactants such as cationic surfactants and nonionic surfactants, pigments, preservatives, fragrances, activators, UV screening agents and the like can be appropriately blended.
  • fluid oils such as squalane, liquid paraffin, ester oil and triglyceride
  • oils such as silicone oil, hyaluronic acid Moisturizers such as sodium and daricerine
  • surfactants such as cationic surfactants and nonionic surfactants, pigments, preservatives, fragrances, activators, UV screening agents and the like can be appropriately blended.
  • the composition for external use of the present invention can take the form of powder, cake, pencil, stick, liquid, etc.
  • foundation, lipstick, eye shadow, scarlet, eyeliner makeup cosmetics such as nail enamel and mascara, hair cosmetics such as hair treatment, hair liquid, and set lotion can be applied to the composition for external use of the present invention.
  • Makeup cosmetics such as nail enamel and mascara
  • hair cosmetics such as hair treatment, hair liquid, and set lotion can be applied to the composition for external use of the present invention.
  • the composition for external use of the present invention is applied on the skin or hair as the application surface, and in the composite powder layer formed on the skin or hair, light interference and light absorption of a specific titanium oxide compound.
  • black pearl luster is recognized. Its black pearly luster is much stronger than conventional pearlescent pigments.
  • the colored gloss composition of the present invention is a coating composition (hereinafter referred to as the present coating composition)
  • the coating composition is a composition that initially has fluidity, spreads and adheres to the surface of an object, and then forms a continuous film through a drying process.
  • the colored gloss composition of the present invention imparts a black pearl luster to an object by light interference and light absorption of a specific titanium oxide compound, and a gloss that has never been obtained can be obtained. It ’s so good!
  • the present invention also provides a coating composition as the above-described coloring gloss composition.
  • the coating composition of the present invention contains the black pearl luster powder of the present invention as a luster pigment as described above.
  • the blending amount of the black pearly luster powder of the present invention in the coating composition of the present invention can be appropriately selected according to the specific type, purpose, etc. of the coating composition of the present invention, and is not limited at all.
  • the powder that is particularly effective in the present invention is a black pearlescent powder, even if it is added in a larger amount than a conventional pearlescent pigment, it is uniformly applied to the object. It is easy to develop a stronger black color.
  • the paint composition of the present invention usually contains elements that can be blended in the paint composition to the extent that the intended effect of the present invention is not impaired. Specifically, coating film forming elements such as polymer oils, natural or synthetic resins, polymer materials such as cellulose and rubber derivatives, etc .; plasticizers, desiccants, curing agents, skin prevention Film formation aids such as agents, fluidity modifiers (thickeners, leveling agents, etc.), sagging inhibitors, antiseptics, antifungal agents, rust inhibitors, UV absorbers, etc .; the black pearl luster powder of the present invention Facial materials other than these can be blended in the coating composition of the present invention.
  • elements such as polymer oils, natural or synthetic resins, polymer materials such as cellulose and rubber derivatives, etc .
  • plasticizers, desiccants, curing agents skin prevention Film formation aids such as agents, fluidity modifiers (thickeners, leveling agents, etc.), sagging inhibitors, antiseptics, antifungal agents, rust inhibitor
  • a solvent for dissolving the coating film-forming element can also be appropriately selected and used.
  • the composite formed on the coated surface is formed on the coated surface.
  • Black pearl luster is observed in the powder layer due to light interference and light absorption by specific compounds of titanium oxide.
  • This paint composition of the present invention comprises various paints such as architectural paints, stone paints, vehicle paints, ships and ship bottom paints, wood paints, equipment paints, marker paints, electrical insulation paints, conductive and semiconductive paints, It can be applied to a wide range of quality paints, anticorrosion paints, heat resistant paints, fireproof paints, temperature indicating paints, luminescent paints, and insecticidal paints.
  • the printing ink composition of the present invention is an image defined on a manuscript or a plate.
  • the composition is used as an image-forming material that is formed and fixed on the surface of a printing material by a printing method.
  • This printing ink composition is distinguished from the above-described coating composition in that it has "printing color", which is a characteristic necessary for producing a printed material without any trouble in the printing process.
  • the black pearly luster powder of the present invention is excellent as a colorant for a printing ink composition in that it imparts a black luster to an object, and is also a black glossy powder. Therefore, the printed matter provided using the printing ink composition using this as a colorant is also excellent in that a black gloss having a strong hiding power can be effectively obtained.
  • the present invention also provides a printing ink composition as the aforementioned coloring composition.
  • the printing ink composition of the present invention contains the black pearly luster powder of the present invention as a colorant as described above.
  • the amount of the black pearl luster powder of the present invention in the printing ink composition of the present invention can be appropriately selected according to the printability required according to the specific type and purpose of the printing ink composition of the present invention.
  • the black pearly luster powder of the present invention has a black concealing power because it is a black glossy powder, so that the black pearly luster is higher than that of conventional pearly luster pigments. It became easy to obtain.
  • the printing ink composition of the present invention is usually printed. Elements that can be incorporated into the ink composition can be incorporated as long as the initial effects of the present invention are not impaired.
  • pigments and dyes other than the black pearl luster powder of the present invention as a coloring material; as a vehicle, oil (vegetable oil such as flaxseed oil and drill oil, mineral oil such as ink oil and solvent) Etc.), resins (natural resins such as gilsonite and rosin, rosin-modified phenolic resins, maleic resins, petroleum resins, alkyd resins, ester resins, etc.), plasticizers, waxes, solvents, etc .; as auxiliary agents , Drying control agents (dryers, anti-skinning agents, etc.), viscosity control agents (compounds, thickeners, waist-cutting agents, etc.), dispersibility control agents (dispersants, anti-coloring agents, stabilizers, etc.), color Conditioning agents (toners, matting agents, etc.), reactive agents (photopolymerization initiators, catalysts, crosslinking agents, etc.), other ingredients, wetting agents, antifoaming agents,
  • the composite powder layer formed on the coated surface is coated on the coated surface and then subjected to a printing process.
  • Black pearl luster is recognized by light absorption.
  • This printing ink composition of the present invention is widely used as various printing inks, for example, lithographic printing ink, gravure printing ink, relief printing ink, screen printing ink, flexographic printing ink, intaglio printing ink, various special printing inks, etc. It is possible.
  • the colored gloss composition of the present invention has many aspects,
  • the embodiment of the colored gloss composition of the present invention is not limited to the embodiment described above! /.
  • the “colored plastic product” obtained by kneading and mixing the black pearl luster powder of the present invention in plastic as shown in the examples described later is also the colored gloss composition of the present invention.
  • the compounding quantity in a present Example is a weight part.
  • the number of measurement methods shown in the production examples is as follows.
  • This black pearl luster powder lg is converted to 15g of Nitron Riya Lacquer 6341 made by Musashi Paint Co., Ltd.
  • the mixture was thoroughly mixed and dispersed with a lab disperser, and applied to a black and white underlayer concealment rate test paper with a 4 mil (0.101 mm) applicator. And the glossiness of the coating film on the white ground was measured at 60 ° and 20 ° with a daros checker IG-300 manufactured by Horiba.
  • the color difference ⁇ was determined by the following equation.
  • Titanium dioxide (%) was determined from the following formula.
  • the amount of titanium dioxide (assumed to be ag) and the amount of thin base powder.
  • the amount of black titanium oxide (bg) is obtained by subtracting the amount of the thin plate-like substrate powder from the amount of the black pearl luster powder, and the relationship between the weight increase rate of a / b and TiOx is obtained by the following equation. .
  • This black pearly luster powder is measured by an X-ray diffractometer miniflex manufactured by Rigaku Corporation using a Cu counter cathode 30 Kv l 5 mA-K ⁇ filter. Titanium oxide compounds are identified from diffraction lines.
  • 100K silver color 15Kg was weighed, 1 ⁇ 95Kg of titanium metal was added to this, and mixed with Henschel mixer.
  • the mixed powder was filled into a reaction vessel, evacuated with a vacuum apparatus, and when the degree of vacuum reached 10, heating was started and the reaction was carried out at 850 ° C. for 10 hours. After the reaction was completed, argon gas was flowed to speed up the cooling.
  • the reduced powder was taken out from the reaction vessel.
  • the reduced powder was pulverized with a pulverizer and the titanium metal was removed by wind classification.
  • the classified reduced powder was oxidized and fired at 300 ° C. for 3 hours in the atmosphere.
  • the powder produced was 14.5 kg and had a black pearly luster! /.
  • Manufactured black pearl luster powder 14Kg in isopropyl Alconole 0.45 kg and Shin-Etsu Chemical Co., Ltd. Silicone KF-9909 were mixed in a Henschel mixer and silicone-treated at 140 ° C for 5 hours. Silicone-covered black pearl luster powder of 14 kg was obtained.
  • the present inventors prepared black pearly luster powder by various production methods according to Production Example 1, and observed the appearance. The results are shown in Table 1 below.
  • the present inventors decided to adjust the reduction to 1.50 or less and then reoxidize to adjust the black pearl luster powder.
  • the powder produced was 1 lKg and had a black pearly luster!
  • the produced powder had a black pearl luster at 13.5 kg.
  • the powder obtained by oxidizing and baking the classified reduced powder at 290 ° C. for 3 hours in the atmosphere had a black pearly luster at 12.5 kg.
  • a 10% aqueous hydrochloric acid solution was added dropwise to adjust the pH to 4.
  • the mixture was aged for 1 hour with stirring. After filtration and washing with water, it was dried at 150 ° C. for 16 hours to obtain 12 kg of fluorine-coated black pearl luster powder.
  • Table 1 shows the powder characteristic values of the black pearl luster powder produced in the above production example. As can be seen from the table, the powders produced from any of the production examples are glossy, have low lightness, low a and b values, and low concealment ratio (strong concealment power). Black pearl luster powder It was a body.
  • Figure 1 shows the X-ray diffraction measurement results of the black pearl luster powder before the surface treatment. As can be seen from the figure, the black nacreous powder can be confirmed by My strength, Ti O and Ti O.
  • the above 1 2 was mixed with a Henschel mixer, and 3 7 mixed with heating and dissolution was added and kneaded. It was pulverized with a pulverizer, passed through a sieve, and pressed into an intermediate dish. Power and eyebrow cosmetics should be used as an eyeliner when wet with a brush, as an eyebrow when using a dry brush, and as a mascara when using a brush for mascara. I can do it. Further, as Comparative Example 1, the component 1 was a silicone-treated black iron oxide.
  • Compounding ingredients Compounding amount (parts by weight)
  • the component 4 was fluorinated black iron oxide.
  • Compounding ingredients Compounding amount (parts by weight)
  • evaluation was made on wrinkles, the naturalness of the finished color, and the uneven color of the finished product.
  • the evaluator performed a five-step evaluation of 1 to 5 by 10 expert panels, and the average value was displayed in Table 4 with the following symbols. : 4.5 or more, 5.0 or less
  • ⁇ 3.5 or more, less than 4.5
  • ⁇ 2.5 or more, less than 3.5
  • X 1.5 or more, less than 2.5
  • Compounding ingredients Compounding amount (parts by weight)
  • the coated body had a strong black gloss.
  • Compounding ingredients Compounding amount (parts by weight)
  • Ataryl adhesive (Toyo Inkki 1 1 0 9) 8 9. 3
  • the obtained pressure-sensitive adhesive sheet for coating had a strong black color!
  • FIG. 1 The diffraction lines of Production Examples 1 to 5 by the X-ray diffraction method of the powder are shown. This curve is the figure used to identify the compound.

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Abstract

[PROBLÈMES] Proposer une poudre perlée noire d'oxyde de titane, de petite dimension, d'excellente couleur, et proposer un procédé de fabrication aisée de la poudre noire. [MOYENS POUR RÉSOUDRE LES PROBLÈMES] Est proposé une poudre perlée noire ayant une poudre en feuillets minces, revêtue à sa surface par un oxyde de titane de petite dimension, caractérisée par le fait que l'oxyde de titane de petite dimension ne contient sensiblement pas d'azote et est représenté par la formule TiOX (X = 1,56 à 1,75).
PCT/JP2007/071998 2006-11-13 2007-11-13 Poudre perlée noire et son procédé de fabrication WO2008059828A1 (fr)

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JP2006306171A JP2008120914A (ja) 2006-11-13 2006-11-13 黒色真珠光沢粉体およびその製造方法
JP2006-306171 2006-11-13

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JP6229481B2 (ja) * 2012-12-25 2017-11-15 三菱ケミカル株式会社 ポリオレフィン系化粧シート用フィルム
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CN110477522B (zh) * 2019-08-27 2022-04-12 广东溢达纺织有限公司 贝壳材料及其制备方法和贝壳纽扣

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JPS59126468A (ja) * 1983-01-11 1984-07-21 Shiseido Co Ltd 雲母チタン系顔料
JPS6060163A (ja) * 1983-09-14 1985-04-06 Shiseido Co Ltd チタン化合物で被覆された雲母
JPS61225264A (ja) * 1985-03-29 1986-10-07 Shiseido Co Ltd 有色真珠光沢塗料
JPH0543417A (ja) * 1991-08-08 1993-02-23 Shiseido Co Ltd 下地化粧料
JPH0867830A (ja) * 1994-08-26 1996-03-12 Shiseido Co Ltd 低次酸化チタン含有顔料及びその製造方法
JPH08109339A (ja) * 1994-10-11 1996-04-30 Shiseido Co Ltd 低次酸化チタン含有顔料及びその製造方法
JPH11343211A (ja) * 1998-05-28 1999-12-14 Shiseido Co Ltd ボディー用化粧料

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59126468A (ja) * 1983-01-11 1984-07-21 Shiseido Co Ltd 雲母チタン系顔料
JPS6060163A (ja) * 1983-09-14 1985-04-06 Shiseido Co Ltd チタン化合物で被覆された雲母
JPS61225264A (ja) * 1985-03-29 1986-10-07 Shiseido Co Ltd 有色真珠光沢塗料
JPH0543417A (ja) * 1991-08-08 1993-02-23 Shiseido Co Ltd 下地化粧料
JPH0867830A (ja) * 1994-08-26 1996-03-12 Shiseido Co Ltd 低次酸化チタン含有顔料及びその製造方法
JPH08109339A (ja) * 1994-10-11 1996-04-30 Shiseido Co Ltd 低次酸化チタン含有顔料及びその製造方法
JPH11343211A (ja) * 1998-05-28 1999-12-14 Shiseido Co Ltd ボディー用化粧料

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