WO2020175003A1 - Pigment blanc ayant une performance de masquage élevée pour une utilisation dans des milieux de dispersion de faible viscosité, et son procédé de production - Google Patents

Pigment blanc ayant une performance de masquage élevée pour une utilisation dans des milieux de dispersion de faible viscosité, et son procédé de production Download PDF

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WO2020175003A1
WO2020175003A1 PCT/JP2020/003550 JP2020003550W WO2020175003A1 WO 2020175003 A1 WO2020175003 A1 WO 2020175003A1 JP 2020003550 W JP2020003550 W JP 2020003550W WO 2020175003 A1 WO2020175003 A1 WO 2020175003A1
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Prior art keywords
titanium oxide
pigment
shape
coated
pigment according
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PCT/JP2020/003550
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English (en)
Japanese (ja)
Inventor
智祐 勝山
昭夫 那須
正育 森下
直敬 下村
珠美 下村
Original Assignee
株式会社 資生堂
チタン工業株式会社
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Application filed by 株式会社 資生堂, チタン工業株式会社 filed Critical 株式会社 資生堂
Priority to JP2021501793A priority Critical patent/JPWO2020175003A1/ja
Priority to CN202080014633.1A priority patent/CN113474292A/zh
Publication of WO2020175003A1 publication Critical patent/WO2020175003A1/fr

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29—Titanium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02—Preparations containing skin colorants, e.g. pigments
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • 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
    • C09C1/36—Compounds of titanium
    • 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00—Pigment pastes, e.g. for mixing in paints

Definitions

  • the present disclosure relates to a surface-coated calcined pigment containing titanium oxide as a main component, which is suitable for use in a low-viscosity dispersion medium, and a method for producing the same.
  • Patent Document 1 the sides of the magnitude 0. 05 ⁇ 0. 2 M m, the thickness direction from 0.02 to 0.1 bar-like particle collection and / or coupling having dimensions of Mm
  • the fan-shaped rutile-type titanium oxide particles are further aggregated, and the aggregated particles have a particle size of 0.1 to 5.O ⁇ m and an average friction coefficient (Ml U value) of 0.2 or more and 0.7 or more. It is disclosed that unsintered unburned rutile type titanium oxide agglomerated particles having a hiding property are used for a high viscosity type cosmetic.
  • Patent Documents 2 to 4 disclose the use of titanium oxide having a particle shape of straw bundles, strips or the like in a high-viscosity type cosmetic.
  • Titanium oxide is widely used mainly in cosmetics, but since it has a large Hammer Kerr constant (Hamak erconn stn t ), which is an indicator of the strength of interaction, it is generally prone to aggregation and sedimentation.
  • Hammer Kerr constant Hamak erconn stn t
  • Equation 1 As an indicator of the sedimentation property of particles in a liquid medium, the Stokes equation shown in the following Equation 1 can be used:
  • the average particle size of pigment-grade titanium oxide is about 0.3.
  • the crystal system of pigment-grade titanium oxide has a high refractive index, and rutile is used because of its hiding power. ..
  • the density of the rutile system is 4.2 7 9 / 1_ (Mr. Seino, Titanium oxide, 1 991).
  • the sedimentation velocity is proportional to the square of the particle diameter and the difference in density, and is inversely proportional to the medium viscosity.For example, in a medium having a low viscosity such as an aqueous dispersion medium, high density pigment-grade titanium oxide particles are sedimented. It's easy to do.
  • pigment-grade titanium oxide may be added to a medium used for cosmetics having a relatively high viscosity, but physical dispersion means such as stirring and shaking should be applied. Therefore, it cannot be blended in a medium of low viscosity such as an aqueous dispersion medium.
  • reducing the particle size of titanium oxide is an effective means for improving the sedimentation resistance.
  • the hiding property decreases, so that the performance required as a cosmetic material may not be satisfied. It was required to have both anti-sedimentation property and hiding property in a low-viscosity dispersion medium.
  • Patent document 1 Patent No. 4 6 8 4 9 7 0
  • Patent Document 2 Patent No. 6 2 5 8 4 6 2 Publication
  • Patent Document 3 Patent No. 5 0 9 6 3 8 3 Publication
  • Patent Document 4 JP 2 0 1 4 _ 8 4 2 5 1 gazette Summary of the invention
  • the subject matter of the present disclosure is to provide a surface-coated calcined pigment containing titanium oxide as a main component, which is hard to settle in a low-viscosity dispersion medium such as an aqueous dispersion medium, and has excellent hiding properties. is there.
  • the inventors of the present invention have conducted extensive studies on the dispersion of titanium oxide, and as a result, treated titanium oxide having a protruding shape as shown in FIG. 1 with an aqueous solution of an inorganic salt as a raw material of the coating agent and calcined. As a result, it was found that a surface-coated calcined pigment containing titanium oxide as a main component, which has excellent sedimentation resistance in a low-viscosity dispersion medium and excellent hiding power, can be obtained.
  • the surface-coated baked pigment containing titanium oxide as a main component of the present disclosure can be used as a composition mixed with a dispersion medium.
  • the secondary structure particles are composed of a plurality of linked primary structures, and the surface of the secondary structure particles is made of an inorganic material other than titanium oxide.
  • the material is coated and the area equivalent circle particle size is 1
  • the inorganic material is one or more oxides of elements selected from aluminum, silicon, zinc, titanium, zirconium, iron, cerium and tin.
  • the pigment according to embodiment 1, wherein the inorganic material is at least one selected from silicon oxide and aluminum oxide.
  • the shape of the primary structure is at least one selected from a needle shape, a granular shape, a spindle shape, a strip shape, a straw bundle shape, a rod shape, and a cocoon shape, Any one of Aspect 1 to Aspect 3 Pigments. 20/175003 4 ⁇ (: 171? 2020 /003550
  • the apparent bulk density of the pigment is 6001 ⁇ or less, Aspect 1 to Aspect
  • the pigment according to any one of 4 to 4.
  • the specific surface area of the pigment is 8 0 2/9 or less, the pigment according to any one of the embodiments 1 to embodiment 5.
  • 3 has at least one selected from the following apparent bulk density and 8 0 2/9 or less specific surface area, and pigments oxide layer of an inorganic material other than titanium oxide on the surface is covered.
  • a composition containing the pigment according to any one of aspects 1 to 10 and a dispersion medium, and having a viscosity at a shear rate of 100 0/3 is 100 00 1 3 3 or less. ..
  • a titanium oxide forming solution is used to prepare a slurry containing secondary structure particles having a surface-projecting shape that is formed by connecting a plurality of primary structures.
  • An inorganic material coating solution consisting of an aqueous solution of an inorganic salt as a raw material of the coating agent is added to the slurry,
  • Aspect 1 A method for producing the pigment according to any one of aspects 1 to 10.
  • a surface-coated fired pigment containing titanium oxide as a main component which hardly precipitates even in a low-viscosity dispersion medium such as an aqueous dispersion medium and has excellent concealing property.
  • FIG. 1 A transmission electron micrograph of titanium oxide that is not coated on the surface and is not fired.
  • FIG. 2 A transmission electron micrograph of the surface-uncoated titanium oxide after firing.
  • FIG. 3 is a transmission electron microscope photograph after firing of the surface-coated fired pigment mainly composed of titanium oxide surface-coated with silicon oxide in an embodiment of the present disclosure.
  • FIG. 4 is a transmission electron microscope photograph after firing of a surface-coated fired pigment mainly composed of titanium oxide surface-coated with silicon oxide and aluminum oxide in another embodiment of the present disclosure.
  • a titanium oxide-based surface-coated baked pigment according to an embodiment of the present disclosure comprises:
  • this secondary structure particle is composed of secondary structure particles having a surface protruding shape as shown in Fig. 3, and this secondary structure particle is composed of a plurality of linked primary structures, and the surface of the secondary structure particles is oxidized. It is coated with an inorganic material other than titanium, and has an area-circular equivalent particle diameter of 150 nm or more and 500 n or less.
  • the secondary structure particles have a large number of surface protrusion shapes.
  • the pigment of the present disclosure has voids due to the protruding shape as shown in FIG. 3, and thus the apparent bulk density becomes small. Therefore, it is considered that even in a low-viscosity dispersion medium such as an aqueous dispersion medium, the sedimentation rate becomes small, and it becomes more difficult to sediment than in general pigment grade titanium oxide. ⁇ 2020/175003 6 ⁇ (:171? 2020/003550
  • Such a pigment has a unique apparent bulk density or specific surface area different from general pigment grade titanium oxide and the like. It is considered that a pigment having such a unique apparent bulk density or specific surface area can exhibit the same action and effect.
  • the surface-coated fired pigment of the present disclosure is It is possible to retain the unique morphology as shown in FIGS. 3 and 4, that is, the morphology of the secondary structure particles constituted by connecting a plurality of secondary structures. It is considered that this is because the sintering of the primary structures was inhibited by the formation of the coating layer made of an inorganic material different from titanium oxide on the surface of the primary structure made of titanium oxide. ..
  • the coating layer on the surface of the pigment is made of an inorganic material other than titanium oxide. Since hydroxyl groups are likely to be arranged on the surface of the coating layer made of an inorganic material, the compatibility between the aqueous dispersion medium and titanium oxide is improved, and it is considered that the coating layer is more easily dispersed in the aqueous dispersion medium.
  • the coating layer on the surface of the pigment is improved in durability as compared with an unsintered coating layer because the binding force with titanium oxide is improved by firing to prevent the coating layer from peeling. ..
  • the pigment of the present disclosure has an area circle equivalent particle diameter of
  • the surface-coated baked pigment containing titanium oxide as a main component (which may be simply referred to as “pigment”) of the present disclosure has a surface coated with an inorganic material other than titanium oxide. ⁇ 2020/175003 7 ⁇ (: 171-1? 2020 /003550
  • the main component is titanium oxide having an area circle equivalent particle diameter of 150 0 n 01 or more and 500 0 n 01 or less and having a surface protrusion shape formed by connecting a plurality of primary structures.
  • Pigment comprising secondary structure particles, and/or 600 Titanium oxide having one at least selected from 9/3 or less of the apparent bulk density and 8 0 2/9 or less specific surface area pigments can be used for the main component.
  • the type of titanium oxide component in the pigment may be any of anatase type, rutile type and brookite type, but rutile type titanium oxide is preferable from the viewpoint of hiding power.
  • the area-equivalent particle diameter of the pigment can be, for example, the particle diameter when converted into a circular particle having the same area as the projected area of the pigment observed with a transmission electron microscope.
  • the particle diameter corresponding to the area circle can be defined as the average value of 10 or more particles.
  • the area circle equivalent particle size of the titanium oxide particles is, for example, preferably a size in the vicinity of 1/2 wavelength of visible light in order to enhance the scattering effect of visible light and enhance the hiding property. More preferably at least 450 n,
  • an apparent bulk density is desirably 6 0 0 9/3 or less.
  • the apparent bulk density can be obtained, for example, by using a specific volume tester as described later.
  • the pigment of the present disclosure has a specific surface area of 80 from the viewpoint of hiding power, sedimentation resistance and the like. The following is desirable.
  • the specific surface area of titanium oxide can be obtained, for example, by the Mitsumi method.
  • the pigment of the present disclosure has a color difference ( ⁇ M), which is an index of the hiding property, in the hiding test described below, for example, 30.0 or less, 27.0 or less, 25.0 or less, 24.0.
  • ⁇ M is an index of the hiding property, in the hiding test described below, for example, 30.0 or less, 27.0 or less, 25.0 or less, 24.0.
  • It can be 0 or less, or 23.0 or less. There is no particular limitation on the lower limit of the color difference, but it can be specified, for example, as 10.0 or more, 12.0 or more, or 15.0 or more.
  • the pigment of the present disclosure is based on the color difference of the titanium oxide that has not been subjected to surface coating and baking treatment in the hiding test described below, and the difference from the color difference of other titanium oxides (hiding power difference).
  • the hiding property can be evaluated.
  • This hiding power difference can be specified to be 2.0 or more.
  • the upper limit of the hiding power difference is not particularly limited, but can be specified to be, for example, 20.0 or less.
  • the pigment of the present disclosure desirably has a crystallite size of 8.0 n or more, and also desirably has a crystallite size of 25.0 n or less.
  • the crystallite diameter of titanium oxide can be measured by a general X-ray diffraction method.
  • the pigment of the present disclosure it is possible to use a secondary particle having a surface protruding shape formed by connecting a plurality of primary structures.
  • the shape of the _ secondary structure may be any shape as long as sedimentation resistance and concealing performance can be obtained, and is not limited to the following, for example, needle-like, granular, spindle-like, rectangular, It can be at least one selected from straw bundle, rod shape, and cocoon shape. Of these, needle-like or rod-like shapes as shown in FIGS. 3 and 4 are preferable.
  • the secondary structure may be linked so as to have a shape protruding on the surface of the secondary structure particle, and the linked structure is not particularly limited, but the primary structure is, for example, a fan-shaped structure. It may be connected radially or randomly, and in particular, it is preferably connected radially from the viewpoint of sedimentation resistance and concealing property.
  • the surface of the pigment of the present disclosure is coated with one or more inorganic materials other than titanium oxide.
  • the inorganic material is not limited to the following, but includes, for example, a component containing an element selected from aluminum, silicon, zinc, zirconium, iron, cerium, and tin, for example, an oxide of the above element. Among them, silicon oxide and aluminum oxide are preferable, and silicon oxide is more preferable.
  • the pigment having the surface coating layer is mainly composed of titanium oxide, that is, 800 g/kg or more is the titanium oxide component, from the viewpoint of hiding property.
  • the ratio of the surface coating layer in the titanium oxide can be 200 g/kg or less, and can be 10 g/kg or more, based on the mass of the pigment.
  • the pigment containing titanium oxide as a main component of the present disclosure can form a composition with a low-viscosity dispersion medium, particularly an aqueous dispersion medium.
  • compositions comprising the pigments of the present disclosure can have viscosities at a shear rate of 1000/s or less than 1 O Om P a -s.
  • the viscosity can be measured using, for example, a rheometer such as MCR-302 (manufactured by Anton-Paar), and the shear rate of the object to be measured when measured at 32°C and 1 atm is 1 000.
  • the viscosity at the time of / s can be specified as 100 mP as or less, 50 mP as or less, or 10 mP as or less, and 1 mP as or more, 2 mP as or more, or It can be defined as 3 m P as or more.
  • the static viscosity of the composition of the present disclosure that is, the shear rate is as close as possible to 0 s- i , for example, the viscosity at a shear rate of 1 /s is defined as 1 OO Om P as or less. And can be defined as 1 Om P as or more. ⁇ 2020/175003 10 boxes (:171? 2020 /003550
  • the static viscosity can also be measured using the above-described rheometer under the conditions of 32 ° and 1 atm.
  • composition of the present disclosure can achieve 90.0% or more, 93.0% or more, or 95.0% or more after 24 hours in the sedimentation resistance test described below, and 100% or less. , Less than 100%, or less than 99.0% can be achieved.
  • composition of the present disclosure can achieve 90.0% or more after 24 hours and can achieve 85.0% or more after 90 hours in the sedimentation resistance test described below.
  • the blending amount of the pigment in the composition can be appropriately adjusted according to the intended use, etc., and is not limited to the following, for example, 509/9 or more in the composition
  • the dispersion medium is not particularly limited as long as it can disperse the pigment, and one or more known dispersion media such as an organic dispersion medium and an aqueous dispersion medium can be used. Above all, it is preferable to use an aqueous dispersion medium.
  • the aqueous dispersion medium include water, various alcohols such as lower alcohols and polyhydric alcohols, and mixtures thereof.
  • lower alcohol e.g., ethanol, propanol, isopropanol, isobutyl alcohol, 1; - butyl alcohol _ le, and the like.
  • polyhydric alcohols examples include dihydric alcohols (eg, ethylene glycol, propylene glycol, trimethylene glycol, 1,2-butylene glycol, 1,3-butylene glycol, tetramethylene glycol 20/175003 1 1 ⁇ (: 171-1? 2020 /003550
  • 2,3-butylene glycol pentamethylene glycol, 2-butene-1,4-diol, hexylene glycol, octylene glycol, etc.
  • trivalent alcohols eg, glycerin, trimethylolpropane, etc.
  • tetravalent Alcohol eg, pentaerythritol such as 1,2,6-hexanetriol
  • pentavalent alcohol eg, xylitol etc.
  • hexavalent alcohol eg, sorbitol, mannitol etc.
  • polyhydric alcohol Coalescence eg, propylene glycol, dipropylene glycol, trimethylene glycol, polypropylene glycol, tetraethylene glycol, diglycerin, polyethylene glycol, triglycerin, tetraglycerin, polyglycerin, etc.
  • divalent alcohol alkyl Teres for example, ethylene glycol monomethyl ether, ethylene glyco
  • compositions of the present disclosure to the extent not impairing the effect of the present disclosure, other ingredients, such as pigments other than titanium oxide, dyes, esters, humectants, water-soluble polymers, oil, higher alcohol _ le, binder _ , Dispersants, various salt components, thickeners, surface tension reducing agents such as various surfactants, film forming agents, UV absorbers, UV scattering agents, metal ion sequestering agents, amino acids, organic amines, polymer emulsions, 1 to 1 regulator, skin nutrition agent, vitamin agent, antioxidant, antioxidant aid, fragrance, preservative, anti-inflammatory agent, anti-inflammatory agent, whitening agent, activator, antiseborrheic agent, various herbal extracts
  • the drug and the like can be appropriately blended as necessary.
  • the pigment of the present disclosure has excellent sedimentation resistance, it is not necessary to use a dispersant, but a dispersant such as a polyelectrolyte was used. ⁇ 2020/175003 13 ⁇ (:171? 2020/003550
  • the surface-coated baked pigment containing titanium oxide as a main component of the present disclosure and the composition containing the pigment of the present disclosure can be suitably used in a wide range of applications such as cosmetics, paints, and inks.
  • the method for producing the surface-coated baked pigment containing titanium oxide as the main component of the present disclosure is not particularly limited.
  • the description in Patent Document 1 can be referred to.
  • ortho titanate titanyl sulfate solution obtained by alkaline neutralization of at 1 0 ° ⁇ temperatures below, 1 0 ° ⁇ less Hydrochloric acid was added at the temperature of 1 to completely dissolve orthotitanic acid, and then heated and hydrolyzed to form secondary structure particles in which needle-like primary structures as shown in Fig. 1 were linked.
  • unfired titanium oxide which is not surface-coated. Ding ⁇ 2 concentration at that time, 5_Rei 9 /! _ Least 1 409 /! _ Or less, preferably 60 9 /! _ Least 1 20 9 /! _ Less, hydrochloric acid concentration, 70 9 /! _ Or more and 1 709 9 /!_ or less, preferably 80 9 /!_ or more and 1 60 9 /!_ or less.
  • the hydrolysis temperature is 25° ⁇ or more and 60° ⁇ or less, preferably 30° ⁇ or more and 55° ⁇ or less.
  • unsintered titanium oxide which is not surface-coated is, in addition to orthotitanic acid, a titanium tetrachloride solution, or metatitanic acid treated with an alkali. It can also be obtained by carrying out hydrolysis using a solution that has been dissolved.
  • unburned titanium oxide having a secondary structure particle in which secondary structures such as straw bundles, strips and the like are connected to each other and whose surface is not coated is described in, for example, Patent Documents 3 and 4. It can be obtained by appropriately using such a method as described above and heating or baking as required.
  • the method for coating the surface of unfired titanium oxide that has not been surface-coated is also particularly limited. ⁇ 2020/175003 14 ⁇ (:171? 2020/003550
  • titanium oxide prepared as described above is added to ion-exchanged water to prepare a slurry.
  • an inorganic material coating solution consisting of an aqueous solution of sodium silicate was added to the slurry while maintaining the slurry at 70 ° C and stirred slowly, and after stirring for a predetermined time, dilute hydrochloric acid, dilute sulfuric acid, or other acid was added.
  • dilute hydrochloric acid, dilute sulfuric acid, or other acid was added.
  • 1 to 1 from 5.0 to 8.0.
  • the coating amount of the surface coating layer can also be adjusted by adjusting the composition, concentration and blending amount of the organic material coating liquid.
  • the obtained slurry is filtered, washed with water, dried, and then calcined in a general calcining furnace such as a muffle furnace or a rotary kiln to obtain titanium oxide having a shape as shown in Figs. 3 and 4. It is possible to obtain a surface-coated fired pigment containing as a main component.
  • the firing temperature for example, be a 5 0 0 ° ⁇ As 8 0 0 ° ⁇ less, more preferably be a 5 5 0 ° ⁇ As 7 5 0 ° ⁇ below, firing
  • the time can be set to 0.5 hours to 2.0 hours, and more preferably 1.0 hours to 1.5 hours.
  • the morphology When unfired titanium oxide that is not surface-coated is fired, the morphology generally changes from the shape of FIG. 1 to the shape of FIG. However, when titanium oxide whose surface is coated with an inorganic material is fired, the particle shape of titanium oxide can substantially maintain the shape of FIG. 1 as shown in FIGS. 3 and 4.
  • the properties such as the retention of the surface protruding shape, the anti-sedimentation property, and the hiding property are controlled by, for example, appropriately adjusting the material of the surface coating layer, the firing temperature, the firing time, and the like. be able to.
  • the area-equivalent particle diameter, specific surface area, apparent bulk density, crystallite diameter, and hiding property of the pigment were evaluated. Further, the composition and the composition obtained by the manufacturing method shown in Table 1 below were evaluated for viscosity and sedimentation resistance.
  • coverage the amount of 3 ⁇ 2 coated on titanium dioxide of unfired not surface-coated is referred to as "coverage”, also "present” a material obtained by calcination treatment, those not calcined Is described as “none”.
  • ⁇ I 7 100 type manufactured by Hiritsu High Technology Co., Ltd. was used to magnify 100,000 times and evaluated as the average value of 10 titanium dioxide particles did.
  • the crystallite diameter of titanium dioxide was measured by an X-ray diffractometer (06 6 "Hiroku 6 X, manufactured by Rigaku Denki Co., Ltd.”, and the average crystallite diameter was calculated by applying the Scherrer formula. [0064] (Evaluation of concealment)
  • a slurry was prepared by mixing and stirring titanium dioxide in a ditrocellulose rattle so that the ratio of the pigment was 50 g/kg. Then, the slurry was applied and dried with a 0.101 mm applicator on the black and white hiding power test paper described in JISK5400 to obtain a test sample. The obtained test sample was subjected to color measurement on each of the coating film surfaces on white and black paper with a spectrophotometer CM-2600 d (manufactured by Konica Minolta).
  • the color difference (AE) in the H under Lab color space was calculated from the following formula 2, and based on the color difference of titanium dioxide that was not surface-coated or calcined, the difference with other pigments
  • the (hiding power difference) was calculated from the following formula 3, and the hiding property was evaluated according to the following criteria:
  • Hiding power difference (color difference of unburned titanium dioxide that has not been surface-coated or baked)-(color difference of other pigments) Equation 3
  • the viscosity was evaluated using 1 ⁇ /1 ⁇ [3 ⁇ 4-302 (manufactured by Anton-Paa "manufactured by.")
  • the viscosity is the shear rate of the object to be measured when measured at 32 ° ⁇ and 1 atm. It is the viscosity of 1 000/3 hours. ⁇ 2020/175003 17 ⁇ (: 171-1?2020/003550
  • Pigment 0.19 is added to the test tube for colorimetry of 50!_, and then ion-exchanged water is injected to make 30!_, and it is shaken vigorously to disperse titanium dioxide. A liquid was prepared. The ratio of the height of the sedimentation interface to the height of the water surface of the dispersion was calculated as a percentage of the sedimentation state of the pigment after a predetermined time, and the results are summarized in Table 1. It can be said that the larger the value, the more excellent is the sedimentation resistance, particularly when it is 90% or more after 24 hours and 85.0% or more after 90 hours.
  • the surface-coated unfired titanium dioxide thus obtained was dispersed in ion-exchanged water to prepare a dispersion liquid. Then, 0 5 with the dispersion to. 3 I ⁇ 2 terms containing titanium dioxide
  • the sodium silicate aqueous solution of 9 was added with stirring, the mixture was stirred for 1 hour, and then diluted hydrochloric acid was slowly added to adjust 1 to 1 to 5.0.
  • the amount of the sodium silicate solution was used in an amount of 3 3 9 3 2 2 coating based on the mass of titanium dioxide 8 before coating.
  • the dispersion thus obtained is filtered, washed with water and dried in a conventional manner to obtain a surface-coated unburned dioxide. ⁇ 2020/175003 18 ⁇ (: 171-1? 2020 /003550
  • composition was prepared by adding the obtained calcined titanium dioxide 0 to ion-exchanged water in a blending ratio shown in Table 1 below and shaking it vigorously.
  • a surface-coated calcined titanium dioxide was prepared in the same manner as in Example 1, except that the amount of 3 I 0 2 coating was changed from 3 30/1 ⁇ 9 to 29/10/1 ⁇ 9. Then, the composition of Example 2 was prepared in the same manner as in Example 1 except that the surface-coated baked titanium dioxide was used.
  • Example 3 A surface-coated rutile-type calcined titanium dioxide was prepared in the same manner as in Example 1, except that the amount of 3 I 0 2 coating was changed from 3 3 9/1 ⁇ 9 to 4 7 9 X kg. At the same time, the composition of Example 3 was prepared in the same manner as in Example 1 using this titanium dioxide.
  • the surface-coated and non-calcined titanium dioxide 8 prepared by the same method as in the step of forming untreated surface-treated and calcined titanium dioxide in Example 1 was calcined at 550° ⁇ for 1 hour in a matsufur furnace. Then, calcined titanium dioxide having no surface coating was prepared. Then, the compounding ratio shown in Table 1 below ⁇ 2020/175003 19 ⁇ (: 171-1? 2020/003550
  • a surface-treated and non-calcined surface-treated titanium dioxide layer was prepared by the same method as the step of forming surface-untreated and non-calcined titanium dioxide and the step of forming surface-coated titanium dioxide in Example 1. did. Then, the obtained titanium dioxide was added to the ion-exchanged water at a blending ratio shown in Table 1 below and shaken vigorously to prepare a composition of Comparative Example 3.
  • titanium dioxide By coating titanium dioxide with an inorganic material and further baking it, titanium dioxide having excellent sedimentation resistance and a hiding power difference of 2.0 or more could be obtained.

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  • Epidemiology (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Cosmetics (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

L'invention concerne un pigment de calcination revêtu en surface qui est moins susceptible de précipiter dans un milieu de dispersion à faible viscosité tel qu'un milieu de dispersion à base d'eau, et qui contient, comme composant principal, de l'oxyde de titane qui a d'excellentes performances de masquage.　Selon la présente invention, le pigment de calcination revêtu en surface contenant de l'oxyde de titane comme composant principal est composé de particules structurelles secondaires, chacun ayant une forme saillante en surface, chacune des particules structurelles secondaires étant composée d'une pluralité de structures primaires reliées l'une à l'autre, la surface de chacune des particules structurelles secondaires est revêtue d'un matériau inorganique autre que l'oxyde de titane, et chacune des particules structurales secondaires ayant un diamètre de particule de surface circulaire équivalent de 150 à 500 nm inclus.
PCT/JP2020/003550 2019-02-28 2020-01-30 Pigment blanc ayant une performance de masquage élevée pour une utilisation dans des milieux de dispersion de faible viscosité, et son procédé de production WO2020175003A1 (fr)

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CN202080014633.1A CN113474292A (zh) 2019-02-28 2020-01-30 低粘度分散介质用高隐蔽性白色颜料及其制造方法

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Citations (8)

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JPH07165423A (ja) * 1993-10-22 1995-06-27 Ishihara Sangyo Kaisha Ltd 樹枝状又はヒトデ状微粒子二酸化チタン及びその製造方法
JPH09202620A (ja) * 1996-01-22 1997-08-05 Titan Kogyo Kk ルチル型二酸化チタン粒子およびその製造法
JPH10245228A (ja) * 1997-02-28 1998-09-14 Titan Kogyo Kk 扇状又は盤状酸化チタン及びその製造方法、並びにその用途
JP2003192349A (ja) * 2001-09-28 2003-07-09 Shiseido Co Ltd 毬栗状酸化チタン粉体及びその製造方法
JP2005298316A (ja) * 2004-03-15 2005-10-27 Sumitomo Osaka Cement Co Ltd 酸化チタン粒子、及び酸化チタン粒子の作製方法
JP2010163369A (ja) * 2009-01-13 2010-07-29 Kao Corp 粉体化粧料
JP2017105967A (ja) * 2015-11-26 2017-06-15 株式会社リコー 白色インク、画像形成方法、画像形成装置及び画像形成物
JP2019157058A (ja) * 2018-03-16 2019-09-19 株式会社リコー 白色顔料分散体、インク組成物、画像形成方法および画像形成装置

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU675000B2 (en) * 1993-10-22 1997-01-16 Ishihara Sangyo Kaisha Ltd. Dendrite or asteroidal titanium dioxide micro-particles and process for producing the same

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07165423A (ja) * 1993-10-22 1995-06-27 Ishihara Sangyo Kaisha Ltd 樹枝状又はヒトデ状微粒子二酸化チタン及びその製造方法
JPH09202620A (ja) * 1996-01-22 1997-08-05 Titan Kogyo Kk ルチル型二酸化チタン粒子およびその製造法
JPH10245228A (ja) * 1997-02-28 1998-09-14 Titan Kogyo Kk 扇状又は盤状酸化チタン及びその製造方法、並びにその用途
JP2003192349A (ja) * 2001-09-28 2003-07-09 Shiseido Co Ltd 毬栗状酸化チタン粉体及びその製造方法
JP2005298316A (ja) * 2004-03-15 2005-10-27 Sumitomo Osaka Cement Co Ltd 酸化チタン粒子、及び酸化チタン粒子の作製方法
JP2010163369A (ja) * 2009-01-13 2010-07-29 Kao Corp 粉体化粧料
JP2017105967A (ja) * 2015-11-26 2017-06-15 株式会社リコー 白色インク、画像形成方法、画像形成装置及び画像形成物
JP2019157058A (ja) * 2018-03-16 2019-09-19 株式会社リコー 白色顔料分散体、インク組成物、画像形成方法および画像形成装置

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JPWO2020175003A1 (fr) 2020-09-03
CN113474292A (zh) 2021-10-01

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