EP3963009A1 - Effektpigmente - Google Patents

Effektpigmente

Info

Publication number
EP3963009A1
EP3963009A1 EP20723320.6A EP20723320A EP3963009A1 EP 3963009 A1 EP3963009 A1 EP 3963009A1 EP 20723320 A EP20723320 A EP 20723320A EP 3963009 A1 EP3963009 A1 EP 3963009A1
Authority
EP
European Patent Office
Prior art keywords
sno
pseudobrookite
tio
sio
layer
Prior art date
Legal status (The legal status 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 status listed.)
Pending
Application number
EP20723320.6A
Other languages
German (de)
English (en)
French (fr)
Inventor
Lukas Hamm
Carsten Griessmann
Nicole Nelischer
Marita Jekel
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Merck Patent GmbH
Original Assignee
Merck Patent GmbH
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
Publication date
Application filed by Merck Patent GmbH filed Critical Merck Patent GmbH
Publication of EP3963009A1 publication Critical patent/EP3963009A1/de
Pending legal-status Critical Current

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Classifications

    • 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
    • C09C1/0024—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index
    • C09C1/003—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index comprising at least one light-absorbing layer
    • C09C1/0039—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index comprising at least one light-absorbing layer consisting of at least one coloured inorganic material
    • C09C1/0042—Sub-stoichiometric inorganic materials
    • 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
    • C09C1/0024—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index
    • C09C1/003—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index comprising at least one light-absorbing layer
    • C09C1/0039—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index comprising at least one light-absorbing layer consisting of at least one coloured inorganic material
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • 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
    • C09C1/0024—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index
    • C09C1/0027—One layer consisting of at least one sub-stoichiometric inorganic compound
    • 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
    • C09C1/0024—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index
    • C09C1/003—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index comprising at least one light-absorbing layer
    • 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/36—Pearl essence, e.g. coatings containing platelet-like pigments for pearl lustre
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C01P2002/54—Solid solutions containing elements as dopants one element only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/10—Interference pigments characterized by the core material
    • C09C2200/1004—Interference pigments characterized by the core material the core comprising at least one inorganic oxide, e.g. Al2O3, TiO2 or SiO2
    • 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
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/10—Interference pigments characterized by the core material
    • C09C2200/102—Interference pigments characterized by the core material the core consisting of glass or silicate material like mica or clays, e.g. kaolin
    • 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
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/10—Interference pigments characterized by the core material
    • C09C2200/1054—Interference pigments characterized by the core material the core consisting of a metal
    • 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
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/10—Interference pigments characterized by the core material
    • C09C2200/1087—Interference pigments characterized by the core material the core consisting of bismuth oxychloride, magnesium fluoride, nitrides, carbides, borides, lead carbonate, barium or calcium sulfate, zinc sulphide, molybdenum disulphide or graphite
    • 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
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
    • C09C2200/301—Thickness of the core
    • 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
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
    • C09C2200/302—Thickness of a layer with high refractive material
    • 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
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
    • C09C2200/303—Thickness of a layer with low refractive material
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    • 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
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
    • C09C2200/305—Thickness of intermediate layers within the stack
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    • 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
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
    • C09C2200/307—Thickness of an outermost protective layer
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    • 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
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
    • C09C2200/308—Total thickness of the pigment particle
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    • 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
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/40—Interference pigments comprising an outermost surface coating
    • C09C2200/401—Inorganic protective coating
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C09C2210/00—Special effects or uses of interference pigments
    • 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
    • C09C2220/00—Methods of preparing the interference pigments
    • C09C2220/10—Wet methods, e.g. co-precipitation
    • C09C2220/106—Wet methods, e.g. co-precipitation comprising only a drying or calcination step of the finally coated pigment

Definitions

  • the present invention relates to temperature-stable effect pigments based on multi-coated platelet-shaped substrates and their use in paints, varnishes, printing inks, plastics and in particular in glazes, enamels, ceramic or vitreous
  • ceramic frits used. Especially when used for ceramic glazes in the high temperature range above 900 ° C, especially above 1000 ° C, as it is used for decorating tiles,
  • Porcelain, fine china, bone china, sanitary ware or cast ceramics are used, the problem arises that the effect pigments the aggressive conditions consisting of oxidic melt
  • the oxides are here in a certain
  • golden effect pigments can only be used to a limited extent, as they partially or completely lose color and effect in the combination of the high temperature and the aggressive melt.
  • the golden multilayer pigments known from the prior art such as those known from EP 0 839 167 B1, US 6,692,561 B1, US 6,599355 B1, US 6,579,355 B, US 2015/0259538 A1, US 5,958,125 A, WO 98/53011 , WO 99/20695 have the disadvantage that they are not temperature stable at temperatures of> 900 ° C.
  • CN101289580 A discloses a gold pigment based on mica platelets, which, however, has the disadvantage that it has a relatively low color intensity C * for a multilayer pigment.
  • the object of the present invention is to find a temperature-stable and strongly colored multilayer pigment, in particular a strongly colored golden effect pigment, based on a platelet-shaped substrate with a layer sequence which is characterized in that at
  • Multi-layer pigment takes place.
  • the layer package thus remains largely unchanged during the burning process.
  • effect pigments based on platelet-shaped substrates containing two pseudobrookit layers which are separated from one another by a sufficiently thick separation layer, are stable at temperatures of> 800 ° C., since no or largely no phase reactions take place between the individual layers of the multilayer system.
  • Substrate at least one layer sequence (A) a high index coating with a refractive index of n 3 1.8
  • Oxides can be doped in amounts of £ 10% by weight based on layer (B),
  • n 3 1, 8 consisting of at least two colorless
  • Oxides can be doped in amounts of £ 10% by weight based on layer (E), and optionally
  • (F) have an outer protective layer.
  • the effect pigments according to the invention are characterized by a very high temperature stability, high color strength, high covering power and high gloss and are therefore particularly suitable for high-temperature applications, e.g. suitable for use in glazes and ceramics.
  • the invention also relates to the use of the
  • pigments according to the invention in paints, varnishes, printing inks,
  • Formulations and especially for high temperature applications e.g. for pigmenting glazes and ceramics.
  • the pigments according to the invention are also used for the production of
  • Pigment preparations as well as for the production of dry preparations such as ceramic paints, granulates, chips, pellets, briquettes, etc., suitable.
  • the dry preparations are particularly suitable for printing inks and paints.
  • Suitable base substrates for the effect pigments of the invention are semitransparent and transparent platelet-shaped substrates.
  • Preferred substrates are sheet silicate flakes, SiC, TiC, WC, B4C, BN, graphite, TiO 2 and Fe 2 O 3 flakes, doped or undoped Al 2 O 3 flakes, doped or undoped glass flakes, doped or undoped SiO 2 flakes, TiO 2 flakes, BiOCI and mixtures thereof.
  • natural and synthetic mica flakes, muscovite, talc and kaolin are particularly preferred.
  • the synthetic mica used is preferably fluorophlogopite or Zn phlogopite as substrate
  • the glass platelets can consist of all types of glass known to those skilled in the art, provided they are temperature-stable in the firing range used. Suitable glasses are, for example, quartz glass, A-glass, E-glass, C-glass, ECR-glass, waste glass, alkali borate glass, alkali silicate glass, borosilicate glass, Duran® glass, laboratory glass or optical glass.
  • the refractive index of the glass flakes is preferably 1.45-1.80, in particular 1.50-1.70. Particularly preferred are the
  • Glass substrates made of C glass, ECR glass or borosilicate glass.
  • Synthetic substrate flakes such as glass flakes, SiO 2 flakes, Al 2 O 3 flakes, can be doped or undoped. If they are doped, the doping is preferably Al, N, B, Ti, Zr, Si, In, Sn, or Zn or mixtures thereof. Furthermore, other ions from the group of transition metals (V, Cr, Mn, Fe, Co, Ni, Cu, Y, Nb, Mo, Hf,
  • the substrate is preferably undoped or doped with TiO 2 , ZrO 2 or ZnO.
  • the Al 2 O 3 platelets are
  • Suitable Al 2 O 3 platelets are preferred doped or undoped a-Al 2 O 3 flakes, in particular a-Al 2 O 3 flakes doped with TiO 2 or ZrO 2 .
  • the proportion of doping is the proportion of doping
  • the size of the base substrates is not critical per se and can be tailored to the particular application.
  • the platelet-shaped substrates have a thickness between 0.05 and 5 mm, in particular between 0.1 and 4.5 mm.
  • Substrates of different particle sizes can also be used.
  • a mixture of mica fractions of N-mica (10-60 mm), F-mica (5-20 mm) and / or M-mica ( ⁇ 15 mm) is particularly preferred.
  • N and S fractions (10-130 mm) and F and S fractions (5-130 mm) are also preferred.
  • D 10 1-50 mm, in particular 2-45 mm, very particularly preferably 5-40 mm
  • D 50 7-275 mm, in particular 10-200 mm, very particularly preferably 15-150 mm
  • D 90 15-500 mm, in particular 25-400 mm, very particularly preferably 50-200 mm.
  • high refractive index means a refractive index of 3 1.8
  • low refractive index means a refractive index of ⁇ 1.8
  • the layer (A) is a high-refractive-index layer with a refractive index of n 3 18, preferably n 3 2.0.
  • the layer (A) can be colorless or absorbent in visible light.
  • the layer (A) preferably consists of metal oxides or
  • the metal oxide is preferably selected from the group TiO 2 , ZrO 2 , ZnO, SnO 2 , Cr 2 O 3 , Ce 2 O 3 , BiOCI, Fe 2 O 3 , Fe 3 O 4 , FeO (OH), Ti suboxides ( TiO 2 partially reduced with oxidation numbers of ⁇ 4 to 2 and lower oxides such as Ti 3 O 5 , Ti 2 O 3 up to TiO), titanium oxynitride and titanium nitride, CoO, Co 2 O 3 , Co 3 O 4 , VO 2 , V 2 O 3 , NiO, WO 3 , MnO, Mn 2 O 3 or mixtures of the oxides mentioned.
  • Layer (A) preferably consists of TiO 2 , Fe 2 O 3 , Cr 2 O 3 or SnO 2 .
  • the layer (A) preferably has a layer thickness of 1-15 nm
  • the pseudobrookit layers (B) and (E) can be the same or different.
  • the layers are preferably identical in composition.
  • the pseudobrookite layers preferably consist entirely of Fe 2 TiO 5 .
  • the Fe 2 TiO 5 can be slightly over or under stoichiometric due to slight variations in the Fe / Ti ratio and the resulting lattice vacancies.
  • the layers can be produced by simultaneous addition and precipitation of an Fe-containing and a Ti-containing salt solution or by co-precipitation from a single solution containing Fe and Ti salts.
  • the pseudobrookit layers should preferably be 100% off
  • the oxides are preferably selected from the group Al 2 O 3 , Ce 2 O 3 , B 2 O 3 , ZrO 2 , SnO 2 , Cr 2 O 3 , CoO, Co 2 O 3 , Co 3 O 4 , Mn 2 O 3 .
  • Oxide mixture in the pseudobrookite layer is preferably not more than 5% by weight and is in particular in the range of 1 -5% by weight, very particularly preferably 1-3% by weight, based on layer (B) or layer (E).
  • the layers (B) and (E) each have, independently of one another, layer thicknesses preferably in the range from 60-120 nm, in particular 70-110 nm, and very particularly preferably from 80-100 nm.
  • Separation layer (C) and a separation layer (D) are separated from one another.
  • the distance between layers (B) and (E) should preferably be 40-100 nm, in particular 45-90 nm and very particularly preferably 50-80 nm.
  • the silicate layer can be doped with further alkaline earth or alkali ions.
  • Layer (C) is preferably a “silicate” layer.
  • Layer (C) very particularly preferably consists of doped or undoped SiO 2.
  • Layer (C) preferably has a layer thickness of 40-90 nm, in particular 40-70 nm and very particularly preferably 50-60 nm.
  • Refractive index of n 3 1.8, preferably n 3 2.0, consists of at least two colorless metal oxide layers.
  • Layer (D) preferably consists of 2 or 3 colorless metal oxide layers.
  • the metal oxides are
  • the coating of the layer (D) preferably consists of the
  • the coating of layer (D) preferably has layer thicknesses of 10-25 nm, in particular 11-21 nm and very particularly preferably 12-17 nm. The sum of all layer thicknesses of the individual
  • Metal oxide layers (D1), (D2), (D3) and possibly further layers of the coating of layer (D) should not exceed 25 nm.
  • Total layer thickness of layers (C) and (D) do not exceed the thickness range of 120 nm and preferably in the range 50-115 nm,
  • the TiO 2 can be in the rutile or anatase modification.
  • Particularly preferred effect pigments have the following structure: - substrate + TiO 2 + pseudobrookite + SiO 2 + SnO 2 + TiO 2 + SnO 2 + pseudobrookite
  • the Al 2 O 3 platelets are preferably doped.
  • the SiO 2 platelets are preferably undoped.
  • the metal oxide layer (s) are preferably applied wet-chemically, with those developed for the production of pearlescent pigments
  • wet chemical coating processes can be used; Such methods are e.g. B. described in US 3087828, US 3087829, US 3553001, DE 14 67 468, DE 19 59 988, DE 20 09 566, DE 22 14 545, DE 22 15 191, DE 22 44 298, DE 23 13 331, DE 25 22 572, DE 31 37 808, DE 31 37 809, DE 31 51 343, DE 31 51 354, DE 31 51 355, DE 32 11 602, DE 32 35 017, DE 196 18 568, EP 0 659 843, or also in further patent documents and other publications known to the person skilled in the art.
  • the substrate platelets are suspended in water and one or more hydrolyzable metal salts are added at a pH value suitable for hydrolysis, which is chosen so that the metal oxides or metal oxide hydrates are precipitated directly on the platelets without it comes to secondary precipitation.
  • the pH is usually kept constant by adding a base and / or acid at the same time.
  • the effect pigments are then separated off, washed and dried and, if necessary, calcined, the calcination temperature being optimized with regard to the coating present in each case can be.
  • the annealing temperatures are between 250 and 1000 ° C, preferably between 350 and 900 ° C. If desired, after the application of individual coatings, the pigment can be separated off, dried and, if necessary, calcined in order then to be resuspended again for the precipitation of the further layers.
  • Sodium or potassium waterglass solution is preferably used to fill the SiO 2 layer.
  • the coating can also be carried out in a fluidized bed reactor by gas phase coating, e.g. the methods proposed in EP 0 045 851 and EP 0 106 235 for producing pearlescent pigments can be used accordingly.
  • the hue of the pigments can be varied within wide limits by different choices of the amounts of coating or the resulting layer thicknesses.
  • the fine-tuning for a certain color shade can be achieved beyond the pure choice of quantity by approaching the desired color with a visual or measurement technique.
  • Post-coatings or post-treatments are, for example, the methods described in DE-PS 22 15 191, DE-OS 31 51 354, DE-OS 32 35 017 or DE-OS 33 34 598 in question.
  • the chemical and photochemical stability is further increased or the handling of the effect pigment, in particular its incorporation into different media, is made easier.
  • the handling of the effect pigment, in particular its incorporation into different media is made easier.
  • Functional coatings made of SnO 2 , Al 2 O 3 or ZrO 2 or mixtures thereof can be applied to the pigment surface for user media.
  • Organic after-coatings are also possible, for example with Silanes, as described, for example, in EP 0090259, EP 0 634 459, WO 99/57204, WO 96/32446, WO 99/57204, US 5,759,255, US
  • the layer (F) is preferably a layer made of SnO 2 .
  • Coating (s) in this patent application are understood to mean the complete covering / covering of the platelet-shaped substrates.
  • the effect pigments of the invention have increased temperature and heat stability compared to the unstabilized effect pigments.
  • the stabilized effect pigments can be easily incorporated into engobes and glazes.
  • the glazes can be matt to glossy or transparent to opaque, depending on the desired effect.
  • the effect pigments of the invention are also suitable for
  • the printing inks can be water-based or solvent-based.
  • the effect pigment according to the invention is preferably used in concentrations of 0.5-25% by weight, in particular 1-20% by weight, and very particularly preferably 1-10% by weight, based on the formulation.
  • the effect pigment according to the invention is preferably used in concentrations of 0.1-5% by weight, and very particularly preferably 0.5-4% by weight, based on the formulation.
  • Multi-layer pigments preferably containing 2, 3, 4, 5 or 7
  • - inorganic pigments e.g. transparent and opaque
  • White, colored and black pigments in particular temperature-stable ceramic pigments;
  • - functional pigments eg IR-reflecting or electrically conductive pigments can be used.
  • the effect pigment according to the invention can be mixed in any ratio with commercially available pigments and / or other commercially available fillers.
  • effect pigment according to the invention can also be combined in the formulations with any type of cosmetic raw materials and auxiliaries.
  • these include Oils, fats, waxes, film formers, preservatives and auxiliary substances that determine application properties in general, such as Thickeners and Theological Additives, e.g. Bentonites, hectorites, silicon dioxide, calcium silicates, gelatins, high-molecular carbohydrates and / or surface-active auxiliaries, etc.
  • the formulation containing the effect pigment according to the invention can be of the lipophilic, hydrophilic or hydrophobic type.
  • the effect pigment according to the invention can be contained in only one of the two phases or can also be distributed over both phases.
  • the pH values of the formulations can be between 1 and 14, preferably between 2 and 11 and particularly preferably between 4 and 10.
  • Active ingredients are, for example, insect repellents, inorganic UV filters such as TiO 2 , UV A / BC protective filters (e.g. OMC, B3, MBC), also in encapsulated form, anti-aging agents, vitamins and their derivatives (e.g. vitamin A , C, E, etc.), self-tanners (eg DFIA, erytrolose, etc.) and other cosmetic active ingredients such as bisabolol, LPO, ectoin, emblica, allantoin, bioflavanoids and their derivatives.
  • inorganic UV filters such as TiO 2
  • UV A / BC protective filters e.g. OMC, B3, MBC
  • anti-aging agents e.g. vitamin A , C, E, etc.
  • vitamins and their derivatives e.g. vitamin A , C, E, etc.
  • self-tanners eg DFIA, erytrolose, etc.
  • other cosmetic active ingredients such as bisabolo
  • Organic UV filters are generally used in an amount of 0.5-10% by weight, preferably 1-8% by weight, and inorganic UV filters 0.1-30% by weight, based on the formulation.
  • the formulations can also contain other customary skin-friendly or skin-care active ingredients, such as e.g. Aloe Vera, Avocado Oil, Coenzyme Q10, Green Tea Extract and also active ingredient complexes.
  • the present invention also relates to formulations, in particular formulations, in addition to the
  • Effect pigment at least one component selected from the group of absorbents, astringents, antimicrobial substances,
  • Chelating agents deodorants, emollients, emulsifiers,
  • Emulsion stabilizers dyes, humectants, film formers,
  • Buffer substances reducing agents, surfactants, propellants, opacifiers, UV filters and UV absorbers, denaturants, aloe vera, avocado oil, coenzyme Q10, green tea extract, viscosity regulators, perfume,
  • inorganic pigments e.g. transparent or opaque white, colored and black pigments, metal pigments, temperature-stable
  • the invention furthermore relates to the use of the effect pigments according to the invention in paints, varnishes, printing inks,
  • the pigments according to the invention are also used for the production of pigment preparations and for the production of dry preparations, e.g.
  • Granules, chips, pellets, briquettes, etc. are suitable.
  • the dry preparations are particularly suitable for paints and printing inks.
  • the invention also relates to formulations such as e.g. ceramic paints, coatings, tiles, cast ceramics,
  • the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution.
  • the pH is raised to 7.5 and at this pH 650 ml of sodium water glass solution (13% by weight SiO 2 ) are slowly metered in, the pH being constant with 10% hydrochloric acid is held.
  • the pH is lowered to 1.8 with 10% hydrochloric acid and a solution of 5 g of SnCl 4 ⁇ 5 H 2 O and 41 ml of hydrochloric acid (20%) is metered in.
  • 105 ml of TiCl 4 solution 400 g / l TiCl 4
  • a solution consisting of 5 g SnCl 4 ⁇ 5 H 2 O and 41 ml hydrochloric acid (20%) is then added again.
  • the pH is kept constant at 1.8 with 32% sodium hydroxide solution.
  • the pH is then adjusted to 2.8 again using sodium hydroxide solution.
  • the coated mica substrate is filtered off, washed and dried at 110 ° C. for 16 h.
  • the effect pigment obtained is calcined at 850 ° C. for 0.5 h and sieved.
  • a temperature-stable golden multilayer pigment with high brilliance is obtained.
  • the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution. After stirring for 0.5 h, the pH is raised to 7.5 and at this pH 650 ml of sodium water glass solution (13% by weight SiO 2 ) are slowly metered in, the pH being constant with 10% hydrochloric acid is held. After another
  • a temperature-stable golden multilayer pigment with high brilliance and good hiding power is obtained.
  • the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution. After stirring for 0.5 h, the pH is raised to 7.5 and at this pH 650 ml of sodium water glass solution (13% by weight SiO 2 ) are slowly metered in, the pH being constant with 10% hydrochloric acid is held. After another
  • Hydrochloric acid (20%).
  • the pH is kept constant at 1.8 with 32% sodium hydroxide solution.
  • the pH is then adjusted to 2.8 again using sodium hydroxide solution.
  • the coated mica substrate is filtered off, washed and dried at 110 ° C. for 16 h.
  • the effect pigment is calcined at 850 ° C. for 0.5 h and sieved.
  • a temperature-stable golden multilayer pigment with a strong glitter effect is obtained.
  • Soda waterglass solution (13% by weight SiO 2 ) is slowly metered in, the pH being kept constant with 10% hydrochloric acid. After a further stirring time of 0.5 h, the pH is lowered to 1.8 with 10% hydrochloric acid and a solution of 5 g SnCl 4 ⁇ 5 H 2 O and 41 ml hydrochloric acid (20%) is metered in. At the same pH value, 105 ml of TiCl 4 solution (400 g / l TiCl 4 ) are then slowly metered in. Another solution consisting of 5 g SnCl 4 ⁇ 5 H 2 O and 41 ml now follows
  • Hydrochloric acid (20%).
  • the pH value is in each case with 32% sodium hydroxide solution held constant at 1.8.
  • the pH is then adjusted to 2.8 again using sodium hydroxide solution.
  • the coated mica substrate is filtered off, washed and dried at 110 ° C. for 16 h.
  • the effect pigment obtained in this way is calcined at 850 ° C. for 0.5 h and then sieved.
  • a temperature-stable golden multilayer pigment with high hiding power is obtained.
  • Demineralized water heated to 80 ° C with stirring. After this temperature has been reached, 44 g of TiCl 4 solution (400 g / l TiCl 4 ) are metered in at pH 1.8, the pH being kept constant with 32% sodium hydroxide solution. The pH value is then adjusted to 2.8 using sodium hydroxide solution and at this pH value and 75 ° C, 600 ml of an aqueous FeCl 3 solution (w (Fe) 7%) and 462 ml of an aqueous TiCl 4 - Solution (200 g TiCl 4 / l) added. During the entire addition time, the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution.
  • a temperature-stable golden multilayer pigment with a strong glitter effect is obtained.
  • Soda waterglass solution (13% by weight SiO 2 ) is slowly metered in, the pH being kept constant with 10% hydrochloric acid. After a further stirring time of 0.5 h, the pH is lowered to 1.8 with 10% hydrochloric acid and a solution of 5 g SnCl 4 ⁇ 5 H 2 O and 41 ml hydrochloric acid (20%) is metered in. At the same pH value, 105 ml of TiCl 4 solution (400 g / l TiCl 4 ) are now slowly metered in. Another addition of a solution consisting of 5 g SnCl 4 ⁇ 5 H 2 O and 41 ml now follows
  • a temperature-stable golden multilayer pigment with a very strong glitter effect is obtained.
  • Demineralized water heated to 80 ° C with stirring. After this temperature has been reached, 44 g of TiCl 4 solution (400 g / l TiCl 4 ) are metered in at pH 1.8, the pH being kept constant with 32% sodium hydroxide solution. The pH value is then adjusted to 2.8 using sodium hydroxide solution and at this pH value and 75 ° C, 600 ml of an aqueous FeCl 3 solution (w (Fe) 7%) and 462 ml of an aqueous TiCl 4 - Solution (200 g TiCl 4 / l) added. During the entire addition time, the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution. After stirring for 0.5 h, the pH is raised to 7.5 and at this pH 650 ml of sodium water glass solution (13% by weight SiO 2 ) are slowly metered in, the pH being constant with 10% hydrochloric acid is held. After another
  • a temperature-stable golden multilayer pigment with high brilliance and good hiding power is obtained.
  • the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution.
  • the pH is raised to 7.5 and at this pH 650 ml sodium water glass solution (13% by weight SiO 2 ) are slowly metered in, the pH being kept constant with 10% hydrochloric acid becomes.
  • the pH is lowered to 1.8 with 10% hydrochloric acid and a solution of 5 g SnCl 4 ⁇ 5 H 2 O and 41 ml hydrochloric acid (20%) is metered in.
  • 105 ml of TiCl 4 solution 400 g / l TiCl 4
  • a solution consisting of 5 g SnCl 4 ⁇ 5 H 2 O and 41 ml hydrochloric acid (20%) is then added again.
  • the pH is kept constant at 1.8 with 32% sodium hydroxide solution.
  • the pH value is then adjusted to 2.8 again using sodium hydroxide solution.
  • the coated mica substrate is filtered off, washed and dried at 110 ° C. for 16 h.
  • the effect pigment obtained in this way is calcined at 850 ° C. for 0.5 h and sieved.
  • a temperature-stable golden multilayer pigment with high brilliance and moderate hiding power is obtained.
  • Demineralized water heated to 80 C with stirring. After this temperature has been reached, 44 g of TiCl 4 solution (400 g / l TiCl 4 ) are metered in at pH 1.8, the pH being kept constant with 32% sodium hydroxide solution. The pH value is then adjusted to 2.8 using sodium hydroxide solution and at this pH value and 75 ° C 1040 ml of an aqueous solution containing FeCl 3 (w (Fe) 4%) and TiCl 4 (95 g TiCl 4 / l) admitted. During the entire addition time, the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution.
  • Example 10 A temperature-stable golden multilayer pigment with high brilliance is obtained.
  • the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution. After stirring for 0.5 h, the pH is raised to 7.5 and at this pH 650 ml of sodium water glass solution (13% by weight SiO 2 ) are slowly metered in, the pH being constant with 10% hydrochloric acid is held. After another
  • the pH is then adjusted to 2.8 again using sodium hydroxide solution.
  • Example 1 A temperature-stable golden multilayer pigment with high brilliance and fine texture is obtained.
  • Example 1 1 A temperature-stable golden multilayer pigment with high brilliance and fine texture is obtained.
  • the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution.
  • the pH is raised to 7.5 and at this pH 650 ml of sodium waterglass solution (13% by weight SiO 2 ) are slowly metered in, the pH being kept constant with 10% hydrochloric acid .
  • the pH is lowered to 1.8 with 10% hydrochloric acid and a solution of 5 g SnCl 4 ⁇ 5 H 2 O and 41 ml hydrochloric acid (20%) is metered in.
  • 105 ml of TiCl 4 solution 400 g / l TiCl 4
  • Another addition of a solution consisting of 5 g of SnCl 4 ⁇ 5 H 2 O and 41 ml of hydrochloric acid (20%) now follows.
  • the pH value is 32% in each case
  • the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution. After stirring for 0.5 h, the pH is raised to 7.5 and at this pH 650 ml of sodium water glass solution (13% by weight SiO 2 ) are slowly metered in, the pH being constant with 10% hydrochloric acid is held. After another
  • the pH value is then adjusted to 2.8 again using sodium hydroxide solution.
  • Example 14 A temperature-stable greenish, golden multilayer pigment with high brilliance is obtained.
  • the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution. After stirring for a further 0.5 h, the pH is raised to 7.5 and at this pH 650 ml of sodium water glass solution (13% by weight SiO 2 ) are slowly metered in, the pH being adjusted to 10% hydrochloric acid is kept constant. After another
  • Example 15 A temperature-stable golden multilayer pigment with a strong glitter effect is obtained.
  • the pH is kept constant by simultaneous dropwise addition of a 32% sodium hydroxide solution. After stirring for a further 0.5 h, the pH is raised to 7.5 and at this pH 650 ml of sodium water glass solution (13% by weight SiO 2 ) are slowly metered in, the pH being adjusted to 10% hydrochloric acid is kept constant. After another
  • a temperature-stable golden multilayer pigment with a strong glitter effect is obtained.
  • the golden multilayer pigments of Examples 1 to 15 are all stable at temperatures of 3 1000 ° C. and show no loss of optical properties at these temperatures.

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CN113767151B (zh) 2023-07-04
JP2022531226A (ja) 2022-07-06
KR20220003010A (ko) 2022-01-07
WO2020221715A1 (de) 2020-11-05
CN113767151A (zh) 2021-12-07
US20220220315A1 (en) 2022-07-14

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