DE4212119A1 - Platelike pigment with high gloss - Google Patents

Platelike pigment with high gloss

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Publication number
DE4212119A1
DE4212119A1 DE4212119A DE4212119A DE4212119A1 DE 4212119 A1 DE4212119 A1 DE 4212119A1 DE 4212119 A DE4212119 A DE 4212119A DE 4212119 A DE4212119 A DE 4212119A DE 4212119 A1 DE4212119 A1 DE 4212119A1
Authority
DE
Germany
Prior art keywords
film
metal oxide
pigment
dried
coated
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.)
Withdrawn
Application number
DE4212119A
Other languages
German (de)
Inventor
Gerd Dr Bauer
Karl Dr Osterried
Christoph Dr Schmidt
Reiner Dr Vogt
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
Priority to DE4212119A priority Critical patent/DE4212119A1/en
Priority to CA002121490A priority patent/CA2121490A1/en
Priority to ES93908759T priority patent/ES2120497T3/en
Priority to DE59209413T priority patent/DE59209413D1/en
Priority to US08/211,791 priority patent/US6630018B2/en
Priority to JP50741393A priority patent/JP3723571B2/en
Priority to EP93908759A priority patent/EP0608388B1/en
Priority to KR1019940701251A priority patent/KR100253774B1/en
Priority to PCT/EP1992/002351 priority patent/WO1993008237A1/en
Priority to CZ94932A priority patent/CZ283898B6/en
Priority to RU94022470/12A priority patent/RU2146687C1/en
Priority to MX9205959A priority patent/MX9205959A/en
Priority to CN92111675A priority patent/CN1055711C/en
Publication of DE4212119A1 publication Critical patent/DE4212119A1/en
Priority to FI941773A priority patent/FI106560B/en
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A61K8/0254—Platelets; Flakes
    • 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
    • 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
    • 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
    • C09C1/0018—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings uncoated and unlayered plate-like particles
    • 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
    • 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
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3045—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
    • 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
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3045—Treatment with inorganic compounds
    • C09C1/3054—Coating
    • 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
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
    • 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
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other 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
    • 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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/42—Colour properties
    • A61K2800/43—Pigments; Dyes
    • A61K2800/436—Interference pigments, e.g. Iridescent, Pearlescent
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/60—Particulates further characterized by their structure or composition
    • A61K2800/61—Surface treated
    • A61K2800/62—Coated
    • A61K2800/621—Coated by inorganic compounds
    • 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
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • 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
    • C09C2200/50—Interference pigments comprising a layer or a core consisting of or comprising discrete particles, e.g. nanometric or submicrometer-sized particles
    • C09C2200/505—Inorganic particles, e.g. oxides, nitrides or carbides

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Inorganic Chemistry (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

Platelike pigment (I) with high gloss and high covering power or high transparency, consists of a transparent, inorganic platelike matrix (II), that may contain an additional component (III) whereby (III) is a soluble or insol. colouring agent. In order to achieve gloss (II) is coated on at leat one side with one or more thin, transparent or semi-transparent reflective metal oxide or metal layers. The prepn. of (I) is also claimed whereby the precursor of (II) is coated onto an endless band as a thin film, dried and a chemical reaction carried out to convert the solid precursor film to (II). The resulting film is sepd. from the substrate, washed and the particles opt. dried, calcined, ground and graded. The solidified film obtd. by drying is treated with an acid and the resulting film particles are coated with one or more reflective metal oxide or metal layers.

Description

Die Erfindung betrifft ein farbiges, transparentes oder deckendes Pigment in Form dünner Plättchen mit Siliciumdioxid als Hauptbestandteil.The invention relates to a colored, transparent or opaque pigment in the form of thin plates with silicon dioxide as the main ingredient.

Es wurde bereits in der deutschen Patentanmeldung P 41 38 376 ein Verfahren zur Herstellung von plättchenförmigen Silicium­ oxidteilchen mit Hilfe eines endlosen Bandes vorgeschlagen. Dieses Verfahren ist dadurch charakterisiert, daß ein Träger­ medium mit einem dünnen, wasserglashaltigen Film belegt wird, der flüssige, wasserglashaltige Film durch Trocknung ver­ festigt wird, der feste Film anschließend mit einer Säure behandelt, vom Trägermedium getrennt, gewaschen und getrock­ net wird und die getrockneten Filmpartikel ggf. geglüht, gemahlen und klassiert werden.It was already in the German patent application P 41 38 376 a process for the production of platelet-shaped silicon oxide particles proposed using an endless belt. This method is characterized in that a carrier medium is covered with a thin film containing water glass, the liquid film containing water glass by drying ver is solidified, then the solid film with an acid treated, separated from the carrier medium, washed and dried is net and the dried film particles may be annealed, be ground and classified.

Nach diesem Verfahren werden plättchenförmige SiO2-Partikel mit einer Dicke zwischen 50 und 3000 nm und einer Schicht­ dickentoleranz von weniger als 10% erhalten, die eine aus­ gezeichnete Oberflächengüte besitzen.According to this process, platelet-shaped SiO 2 particles with a thickness between 50 and 3000 nm and a layer thickness tolerance of less than 10% are obtained, which have an excellent surface quality.

Als Precursor-Material für die plättchenförmigen SiO2-Partikel wird eine Wasserglaslösung verwendet, die als dünner Film z. B. auf ein endloses Band aus Polyester oder einem säure­ resistenten beschichteten Edelstahlband aufgebracht wird. A water glass solution is used as the precursor material for the platelet-shaped SiO 2 particles. B. is applied to an endless belt made of polyester or an acid-resistant coated stainless steel belt.

Der Film wird anschließend bei erhöhten Temperaturen von 80-150°C getrocknet. Daran schließt sich ein naßchemischer Reaktionsschritt an, bei dem das beschichtete Band durch einen mit einer Mineralsäure befüllten Behälter geführt wird, um die Alkali-Ionen aus der Wasserglasmatrix auszuwaschen:The film is then at elevated temperatures of Dried 80-150 ° C. This is followed by a wet chemical Reaction step in which the coated tape through a container is filled with a mineral acid, to wash out the alkali ions from the water glass matrix:

(M2O)x·(SiO2)y + 2x HCl → (SiO2)y + 2x MCl + 2x H2O,
M = Li, Na, K.(M 2 O) x · (SiO 2 ) y + 2x HCl → (SiO 2 ) y + 2x MCl + 2x H 2 O,
M = Li, Na, K.

Der Wasserglasfilm kann vorzugsweise jedoch auch durch HCl-Gas polymerisiert werden.The water glass film can, however, preferably also be HCl gas can be polymerized.

Die Herstellung der plättchenförmigen SiO2-Partikel erfolgt in einem kontinuierlichen oder quasi-kontinuierlichen Prozeß, bei dem der Wasserglasfilm auf ein umlaufendes endloses Band, auf eine Trommel aufgewickelte Trägerfolie oder auf ein anderes Trägermedium aufgebracht wird.The platelet-shaped SiO 2 particles are produced in a continuous or quasi-continuous process in which the water glass film is applied to a continuous endless belt, to a carrier film wound onto a drum or to another carrier medium.

Es wurde nun gefunden, daß farbige, transparente Pigmente erhalten werden, wenn der Wasserglaslösung Lösungen von farbgebenden Metallverbindungen zugesetzt werden. Geeignete Metallverbindungen sind beispielsweise Verbindungen der Metalle Ti, V, Cr, Mn, Fe, Co, Ni und Cu, wobei Verbindungen von Co, Cu, Fe und Cr bevorzugt werden. Der Zusatz der Metallverbindungen kann auch erst beim Auftragen auf das endlose Band über eine Zweistoffdüse erfolgen.It has now been found that colored, transparent pigments be obtained when the water glass solution from coloring metal compounds are added. Suitable Metal compounds are compounds of the Metals Ti, V, Cr, Mn, Fe, Co, Ni and Cu, being compounds of Co, Cu, Fe and Cr are preferred. The addition of the Metal connections can also only be applied to the endless belt done via a two-fluid nozzle.

Die Metallverbindungen werden als 0,01- bis 20%ige Lösungen der Wasserglaslösung zugesetzt. Der Anteil der Metall­ verbindungen im aufgetragenen Film beträgt dabei 0,1 bis 40 Gew.-%, bezogen auf den SiO2-Gehalt des Films, wobei dieser Anteil je nach Metall stark variieren kann. The metal compounds are added to the water glass solution as 0.01 to 20% solutions. The proportion of metal compounds in the applied film is 0.1 to 40% by weight, based on the SiO 2 content of the film, this proportion being able to vary widely depending on the metal.

Um eine Ausfällung als Hydroxide oder Oxidhydrate in der alkalischen Wasserglaslösung zu verhindern, können die Metalle mit einem Komplexbildner maskiert werden. Geeignete Komplexbildner sind beispielsweise Zitronensäure, Weinsäure und EDTA.In order to precipitate as hydroxides or hydrated oxides in the to prevent alkaline water glass solution Metals are masked with a complexing agent. Suitable Complexing agents are, for example, citric acid, tartaric acid and EDTA.

Der auf das endlose Band aufgetragene Wasserglasfilm wird in einer Trocknungszone nach bekannten Verfahren, z. B. mit heißer Luft, getrocknet. Der getrocknete Film wird anschließend mit Säure behandelt. Diese Säurebehandlung kann beispielsweise in einer Begasung mit Chlorwasserstoff für einen Zeitraum von 10 sec bis 30 min, bevorzugt von 5 bis 10 min bestehen.The water glass film applied to the endless belt is in a drying zone by known methods, e.g. B. with hot air, dried. The dried film will then treated with acid. This acid treatment can for example in a fumigation with hydrogen chloride a period from 10 sec to 30 min, preferably from 5 to Insist for 10 minutes.

Der gefärbte SiO2-Film wird anschließend nach bekannten Verfahren, z. B. mit einem Wasserstrahl vom Band getrennt und die Filmpartikel mit Wasser gewaschen, bei Temperaturen von 80 bis 180°C getrocknet und bei 600 bis 1000°C, vorzugsweise 700 bis 900°C, geglüht. Die Trocknungsdauer liegt dabei zwischen 1 und 24 Stunden und die Glühzeit zwischen 15 Minu­ ten und 6 Stunden.The colored SiO 2 film is then by known methods, for. B. separated from the belt with a water jet and the film particles washed with water, dried at temperatures from 80 to 180 ° C and annealed at 600 to 1000 ° C, preferably 700 to 900 ° C. The drying time is between 1 and 24 hours and the glow time between 15 minutes and 6 hours.

Anschließend wird das erhaltene Pigment schonend vermahlen, klassiert und gegebenenfalls kurz nachgeglüht.The pigment obtained is then gently ground, classified and, if necessary, briefly annealed.

Man erhält ein farbiges, transparentes Pigment mit einer Farbskala, ahnlich derjenigen von farbigem, transparentem Glas. Durch Zusatz von Eisenverbindungen erhält man zum Beispiel rotbraune Farbtöne, durch Zusatz von Chromverbindun­ gen grüne Farbtöne und durch Zusatz von Kobaltverbindungen blaue Farbtöne. A colored, transparent pigment with a Color scale, similar to that of colored, transparent Glass. By adding iron compounds you get to Example red-brown shades, by adding chromium compounds green shades and by adding cobalt compounds blue shades.  

Diese Pigmente können zusätzlich mit beispielsweise TiO2, Fe2O3 oder Gemischen derselben nach bekannten Verfahren gemäß DE 20 09 566, DE 23 13 331, DE 31 51 355 oder DE 32 21 045 beschichtet werden. Bei Einhaltung definierter Schichtdicken ist es möglich, Interferenzfarben zu erhalten. Somit lassen sich Pigmente herstellen, bei denen sich Körperfarbe und Interferenzfarbe voneinander unterscheiden können. Derartige Pigmente sind für den Sicherheitsdruck, zum Beispiel für den Druck von Geldscheinen, sehr interessant.These pigments can additionally be coated with, for example, TiO 2 , Fe 2 O 3 or mixtures thereof by known processes according to DE 20 09 566, DE 23 13 331, DE 31 51 355 or DE 32 21 045. If defined layer thicknesses are observed, it is possible to obtain interference colors. Pigments can thus be produced in which body color and interference color can differ from one another. Pigments of this type are very interesting for security printing, for example for printing banknotes.

Die erhaltenen Pigmente besitzen Plättchenform und lassen sich in Formulierungen, wie z. B. von Lacken oder Kunststoffen gut einarbeiten.The pigments obtained have a platelet shape and leave formulations such as B. of paints or plastics Work in well.

Die nachfolgenden Beispiele sollen die Erfindung erläutern, ohne sie zu begrenzen.The following examples are intended to explain the invention, without limiting it.

Beispiel 1example 1

2,4 g Zitronensäure (Handelsprodukt von E. MERCK, Darmstadt) wurden in 4 ml voll entsalztem Wasser gelöst. Nach der Zugabe von 1 g CrCl3·6 H2O (Handelsprodukt von E. MERCK, Darmstadt) wurde mit Natronlauge ein pH-Wert von 10 eingestellt, 30 ml Wasserglas (Natrium-Wasserglas DAB 6, Handelsprodukt von E. MERCK, Darmstadt) und 1 ml Texapon® (Handelsprodukt von Henkel, Düsseldorf) als Benetzhilfsstoff zugegeben und das Gemisch verrührt. Mit der so erhaltenen Lösung wurde eine Polyesterfolie (Melinex® 329, Handelsprodukt von ICI) beschichtet. Der Film wurde getrocknet, 10 min einer HCl-Atmosphäre ausgesetzt, von der Folie abgelöst und 10 min in Wasser gewaschen. Die gewaschenen Partikel wurden 60 min bei 110°C getrocknet. Es wurde ein plättchenförmiges, olivgrünes Pigment erhalten.2.4 g of citric acid (commercial product from E. MERCK, Darmstadt) were dissolved in 4 ml of completely deionized water. After the addition of 1 g of CrCl 3 .6H 2 O (commercial product from E. MERCK, Darmstadt), a pH of 10 was set with sodium hydroxide solution, 30 ml water glass (sodium water glass DAB 6, commercial product from E. MERCK, Darmstadt ) and 1 ml of Texapon® (commercial product from Henkel, Düsseldorf) added as a wetting aid and the mixture stirred. A polyester film (Melinex® 329, commercial product from ICI) was coated with the solution thus obtained. The film was dried, exposed to an HCl atmosphere for 10 minutes, detached from the film and washed in water for 10 minutes. The washed particles were dried at 110 ° C. for 60 minutes. A platelet-shaped, olive-green pigment was obtained.

Beispiel 2Example 2

In 4 ml voll entsalztem Wasser wurden nacheinander 2,7 g Natriumethylendiamintetraacetat (Handelsprodukt von E. MERCK, Darmstadt) und 1 g CoCl2·6 H2O (Handelsprodukt von E. MERCK, Darmstadt) gelöst. Der pH-Wert wurde mit Natronlauge auf 10 eingestellt, 30 ml Wasserglas und 1 ml Texapon® als Benetz­ hilfsstoff zugegeben und das Gemisch verrührt. Mit der so erhaltenen Lösung wurde eine Polyesterfolie beschichtet. Der Film wurde getrocknet, 5 min einer HCl-Atmosphäre ausgesetzt, von der Folie abgelöst und 10 min in Wasser gewaschen. Die gewaschenen Partikel wurden 60 min bei 110°C getrocknet. Es wurde ein plättchenförmiges, lilafarbenes Pigment erhalten.2.7 g of sodium ethylenediaminetetraacetate (commercial product from E. MERCK, Darmstadt) and 1 g CoCl 2 .6H 2 O (commercial product from E. MERCK, Darmstadt) were dissolved in succession in 4 ml of completely deionized water. The pH was adjusted to 10 with sodium hydroxide solution, 30 ml of water glass and 1 ml of Texapon® were added as a wetting agent, and the mixture was stirred. A polyester film was coated with the solution thus obtained. The film was dried, exposed to an HCl atmosphere for 5 minutes, detached from the film and washed in water for 10 minutes. The washed particles were dried at 110 ° C. for 60 minutes. A platelet-shaped, purple pigment was obtained.

Beispiel 3Example 3

2,1 g Weinsäure (Handelsprodukt von E. MERCK, Darmstadt) und 2 g FeCl3·6 H2O (Handelsprodukt von E. MERCK, Darmstadt) wurden nacheinander in 4 ml voll entsalztem Wasser gelöst. Der pH-Wert wurde mit Natronlauge auf 10 eingestellt, 30 ml Wasserglas und 1 ml Texapon® zugegeben und das Gemisch verrührt. Mit der erhaltenen Lösung wurde eine Polyesterfolie beschichtet. Der Film wurde getrocknet, 5 min einer HCl-Atmosphäre ausgesetzt, von der Folie abgelöst und 10 min in Wasser gewaschen. Die gewaschenen Partikel wurden 60 min bei 110°C getrocknet. Es wurde ein plättchenförmiges, bräunlich-gelbes Pigment erhalten.2.1 g of tartaric acid (commercial product from E. MERCK, Darmstadt) and 2 g FeCl 3 .6H 2 O (commercial product from E. MERCK, Darmstadt) were successively dissolved in 4 ml of completely deionized water. The pH was adjusted to 10 with sodium hydroxide solution, 30 ml of water glass and 1 ml of Texapon® were added and the mixture was stirred. A polyester film was coated with the solution obtained. The film was dried, exposed to an HCl atmosphere for 5 minutes, detached from the film and washed in water for 10 minutes. The washed particles were dried at 110 ° C. for 60 minutes. A platelet-shaped, brownish-yellow pigment was obtained.

Claims (12)

1. Farbiges, transparentes oder deckendes Pigment in Form dünner Plättchen, bestehend aus Siliciumdioxid und minde­ stens einem färbenden Metalloxid.1. Colored, transparent or opaque pigment in the form thin plate, consisting of silicon dioxide and minde least a coloring metal oxide. 2. Pigment nach Anspruch 1, dadurch gekennzeichnet, daß es zusätzlich mit einem Metalloxid beschichtet ist.2. Pigment according to claim 1, characterized in that it is additionally coated with a metal oxide. 3. Pigment nach Anspruch 2, dadurch gekennzeichnet, daß das Metalloxid beispielsweise TiO2, Fe2O3 oder ein Gemisch derselben ist.3. Pigment according to claim 2, characterized in that the metal oxide is for example TiO 2 , Fe 2 O 3 or a mixture thereof. 4. Pigment nach Anspruch 1, dadurch gekennzeichnet, daß das färbende Metalloxid beispielsweise Fe2O3, Cr2O3 oder CoO ist.4. Pigment according to claim 1, characterized in that the coloring metal oxide is, for example, Fe 2 O 3 , Cr 2 O 3 or CoO. 5. Pigment nach den Ansprüchen 1 bis 4, dadurch gekenn­ zeichnet, daß der Anteil des färbenden Metalloxids 0,1 bis 40 Gew.-%, bezogen auf das Pigment, beträgt.5. Pigment according to claims 1 to 4, characterized records that the proportion of the coloring metal oxide 0.1 up to 40% by weight, based on the pigment. 6. Verfahren zur Herstellung der Pigmente nach den Ansprüchen 1 bis 5, dadurch gekennzeichnet, daß
  • - eine Wasserglaslösung zusammen mit der wäßrigen Lösung einer Metallverbindung, die durch einen Komplexbildner maskiert sein kann, auf ein endloses Band aufgebracht wird,
  • - der flüssige Film durch Trocknung verfestigt wird,
  • - der feste Film anschließend mit einer Säure behan­ delt, vom Trägermedium getrennt, gewaschen und getrocknet wird, und
  • - die getrockneten Filmpartikel gegebenenfalls geglüht, gemahlen und klassiert werden.
6. A process for the preparation of the pigments according to claims 1 to 5, characterized in that
  • a water glass solution together with the aqueous solution of a metal compound, which can be masked by a complexing agent, is applied to an endless belt,
  • the liquid film is solidified by drying,
  • - The solid film is then treated with an acid, separated from the carrier medium, washed and dried, and
  • - The dried film particles are optionally annealed, ground and classified.
7. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß die vom Trägermedium getrennten und gewaschenen Film­ partikel zusätzlich mit einem Metalloxid nach bekannten Verfahren beschichtet werden.7. The method according to claim 6, characterized in that the separated and washed film from the carrier medium particles additionally with a metal oxide according to known Process coated. 8. Verfahren nach Anspruch 7, dadurch gekennzeichnet, daß das Metalloxid beispielsweise TiO2, Fe2O3 oder ein Gemisch derselben ist.8. The method according to claim 7, characterized in that the metal oxide is for example TiO 2 , Fe 2 O 3 or a mixture thereof. 9. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß die Metallverbindung beispielsweise eine lösliche Eisen-, Chrom- oder Kobaltverbindung ist.9. The method according to claim 6, characterized in that the metal compound, for example, a soluble iron, Chromium or cobalt compound. 10. Verfahren nach den Ansprüchen 6 und 9, dadurch gekenn­ zeichnet, daß der Anteil der Metallverbindung im aufge­ tragenen Film 0,01 bis 20 Gew.-%, vorzugsweise 0,1 bis 40 Gew.-%, bezogen auf den SiO2-Gehalt des Films beträgt. 10. The method according to claims 6 and 9, characterized in that the proportion of the metal compound in the applied film 0.01 to 20 wt .-%, preferably 0.1 to 40 wt .-%, based on the SiO 2 - Content of the film is. 11. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß der Komplexbildner beispielsweise Zitronensäure, Weinsäure oder EDTA ist.11. The method according to claim 6, characterized in that the complexing agent, for example citric acid, Is tartaric acid or EDTA. 12. Verwendung der Pigmente nach den Ansprüchen 1 bis 5 in Formulierungen wie Lacken, Druckfarben und Kunststoffen.12. Use of the pigments according to claims 1 to 5 in Formulations such as paints, printing inks and plastics.
DE4212119A 1991-10-18 1992-04-10 Platelike pigment with high gloss Withdrawn DE4212119A1 (en)

Priority Applications (14)

Application Number Priority Date Filing Date Title
DE4212119A DE4212119A1 (en) 1992-04-10 1992-04-10 Platelike pigment with high gloss
KR1019940701251A KR100253774B1 (en) 1991-10-18 1992-10-12 Coloured and coated platelike pigments
PCT/EP1992/002351 WO1993008237A1 (en) 1991-10-18 1992-10-12 Coloured and coated platelike pigments
DE59209413T DE59209413D1 (en) 1991-10-18 1992-10-12 COLORED AND COATED PLATE-SHAPED PIGMENTS
US08/211,791 US6630018B2 (en) 1991-10-18 1992-10-12 Colored and coated plateletlike pigments
JP50741393A JP3723571B2 (en) 1991-10-18 1992-10-12 Colored and coated flaky pigment
EP93908759A EP0608388B1 (en) 1991-10-18 1992-10-12 Coloured and coated platelike pigments
CA002121490A CA2121490A1 (en) 1991-10-18 1992-10-12 Colored and coated plateletlike pigments
ES93908759T ES2120497T3 (en) 1991-10-18 1992-10-12 PIGMENTS IN THE FORM OF STAINED AND COATED PLATELETS.
CZ94932A CZ283898B6 (en) 1991-10-18 1992-10-12 Plate-like pigment, process for producing and use thereof
RU94022470/12A RU2146687C1 (en) 1991-10-18 1992-10-12 Coloring laminar coated pigment, and method of preparing laminar pigment
MX9205959A MX9205959A (en) 1991-10-18 1992-10-16 LAMINILLA-LIKE PIGMENT, WHICH HAS INTENSE BRIGHTNESS AND POWER OF HIGH COVERAGE OR HIGH TRANSPARENCY AND PROCESS FOR ITS PREPARATION
CN92111675A CN1055711C (en) 1991-10-18 1992-10-17 Pigments
FI941773A FI106560B (en) 1991-10-18 1994-04-15 Coated flake pigment process for its preparation and its use

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE4212119A DE4212119A1 (en) 1992-04-10 1992-04-10 Platelike pigment with high gloss

Publications (1)

Publication Number Publication Date
DE4212119A1 true DE4212119A1 (en) 1993-10-14

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Family Applications (1)

Application Number Title Priority Date Filing Date
DE4212119A Withdrawn DE4212119A1 (en) 1991-10-18 1992-04-10 Platelike pigment with high gloss

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DE (1) DE4212119A1 (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10004888A1 (en) * 2000-02-04 2001-08-09 Eckart Standard Bronzepulver Luster pigment and process for its manufacture
DE10252693A1 (en) * 2002-11-13 2004-06-03 Trovotech Gmbh Production of plate-like, irregular three-dimensional or regularly formed glass particles used as, e.g., pigments comprises adding expanding agent to molten glass under pressure, reducing the pressure, and crushing to form glass particles
WO2008099008A2 (en) * 2007-02-15 2008-08-21 Epg (Engineered Nanoproducts Germany) Ag Fine interference pigments containing glass layers on metal glass and ceramic surfaces and method for production thereof
WO2018178365A1 (en) * 2017-03-30 2018-10-04 Sensient Cosmetic Technologies Dyed particles with a high pigment content

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10004888A1 (en) * 2000-02-04 2001-08-09 Eckart Standard Bronzepulver Luster pigment and process for its manufacture
US7217318B2 (en) 2000-02-04 2007-05-15 Eckart Gmbh & Co. Kg Nacreous pigment and method for the manufacture thereof
DE10252693A1 (en) * 2002-11-13 2004-06-03 Trovotech Gmbh Production of plate-like, irregular three-dimensional or regularly formed glass particles used as, e.g., pigments comprises adding expanding agent to molten glass under pressure, reducing the pressure, and crushing to form glass particles
DE10252693B4 (en) * 2002-11-13 2007-03-29 Trovotech Gmbh Process for producing platelet-shaped and irregular, 3-dimensionally or regularly shaped glass particles
WO2008099008A2 (en) * 2007-02-15 2008-08-21 Epg (Engineered Nanoproducts Germany) Ag Fine interference pigments containing glass layers on metal glass and ceramic surfaces and method for production thereof
WO2008099008A3 (en) * 2007-02-15 2009-04-30 Epg Eng Nanoprod Germany Gmbh Fine interference pigments containing glass layers on metal glass and ceramic surfaces and method for production thereof
US10161043B2 (en) 2007-02-15 2018-12-25 Epg (Engineered Nanoproducts Germany) Ag Fine interference pigments containing glass layers on metal, glass and ceramic surfaces and method for production thereof
WO2018178365A1 (en) * 2017-03-30 2018-10-04 Sensient Cosmetic Technologies Dyed particles with a high pigment content
FR3064468A1 (en) * 2017-03-30 2018-10-05 Sensient Cosmetic Technologies COLORED PARTICLES WITH HIGH PIGMENT CONTENT

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