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EP2064292A2 - Revêtement à action photocatalytique - Google Patents

Revêtement à action photocatalytique

Info

Publication number
EP2064292A2
EP2064292A2 EP07801867A EP07801867A EP2064292A2 EP 2064292 A2 EP2064292 A2 EP 2064292A2 EP 07801867 A EP07801867 A EP 07801867A EP 07801867 A EP07801867 A EP 07801867A EP 2064292 A2 EP2064292 A2 EP 2064292A2
Authority
EP
European Patent Office
Prior art keywords
coating
layer
titanium dioxide
coated
interference pigments
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Withdrawn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
EP07801867A
Other languages
German (de)
English (en)
Inventor
Matthias Kuntz
André SALIE
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 EP2064292A2 publication Critical patent/EP2064292A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0215—Coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • C09C1/0021—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
    • 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
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1606—Antifouling paints; Underwater paints characterised by the anti-fouling agent
    • C09D5/1612—Non-macromolecular compounds
    • C09D5/1618—Non-macromolecular compounds 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1687—Use of special additives
    • 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
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • 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
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • 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
    • 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
    • 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
    • C09C2210/00—Special effects or uses of interference pigments
    • C09C2210/10—Optical properties in the IR-range, e.g. camouflage pigments

Definitions

  • the present invention relates to a photocatalytically active coating for surfaces containing as photocatalytically active material platelet-shaped pigments, preferably commercially available interference pigments, which
  • EP 1 074 525 B1 describes a glass substrate comprising an n-type semiconductor film as a primer layer and a photocatalytically active film thereon, the photocatalytically active film consisting of titanium dioxide or containing titanium dioxide particles.
  • the energy band gaps in the primary layer must be greater than the energy band gaps in the photocatalytically active film. In this way, the recombination of the hole-electron pairs is extended and thus the photocatalytic activity can be improved.
  • Both the primer layer and the photocatalytically active layer are applied by sputtering.
  • Documents WO 2004/005577 and WO 2005/105304 describe substrates having a photocatalytic layer which contains photocatalytically active TiO 2 particles, wherein the TiO 2 distribution forms a gradient and the particles are enriched on the surface of the photocatalytic layer.
  • the used ⁇ O 2 is thereby obtained via a sol-gel process and is preferably nanoscale, ie with an average particle size in the nanometer range. Preference is given to using doped titanium dioxide particles.
  • the photocatalytic layers are applied to the desired substrates and at moderate
  • DE 101 58 433 B4 discloses a photocatalytically active coating which consists of a primer layer made of a porous inorganic or inorganic-organic material on which individual, mutually spaced nanoparticles of a photocatalytically active substance are located.
  • the nanoparticles can consist of titanium dioxide.
  • EP 1 404 793 B1 discloses a liquid photocatalytic composition which may comprise a peroxo-modified titanium dioxide and a sensitizer which is intended to improve the photocatalytic activity of the modified titanium oxide, the sensitizer visible, UV or IR light absorbed.
  • Sensitizing agents used are water-soluble dyes, in particular ruthenium complexes. The effect of the light is intended to decompose the sensitizer and to transfer the resulting free electrons into the conduction band of the photocatalytic material, thereby increasing its photocatalytic activity.
  • surfaces for example in the sanitary area, can be temporarily coated, whereby an extension of the period until the next cleaning is to be achieved.
  • the coatings described above have in common that they must be applied either by costly coating process, that is used as the photocatalytically active material nanoparticulate material and / or that only thin films are applied with short-term durability, which for the long-term protection of frequent and strong Weathering impaired surfaces on structures and the like are not suitable.
  • no coating has been disclosed which can be used with good success on surfaces with very high weather load, for example the comparatively cold and thus particularly susceptible to the north of buildings and the like, for permanently avoiding mossing or other vegetation.
  • particulate titanium dioxide tends to agglomerate independently of its particle size, so that when it is used a uniform distribution of the particles on the surface of the treated substrates and thus their uniform over the entire surface acting photocatalytic activity is hindered.
  • TiO 2 nanoparticles are used as a photocatalytically active material, the associated potential dangers for manufacturers and users should not be underestimated. It is now known that nanoparticulate titanium dioxide can be absorbed by the human via the lungs as well as the skin or the digestive tract, where it can lead to accumulation. When used in particular on the outer surfaces of components of all kinds, the passage of considerable amounts of nanoparticles into the groundwater can not be ruled out. Even if there is no detailed investigation available on the actual hazard potential, avoiding the use of TiO 2 nanoparticles represents a reduction of a possible health risk for manufacturers and users. It would therefore be desirable to be able to provide photocatalytically active coatings which are not based on the Base are made of nanoparticulate material, but have good efficacy.
  • components, facade elements and other objects for outdoor use can be coated with protective layers of paint.
  • These usually contain color pigments of all kinds and can also contain interference pigments to achieve special effects, which can either produce a pearlescent effect or even angle-dependent shimmering color effects.
  • interference pigments as a photocatalytically active material in such
  • the object of the invention was to provide photocatalytically active surfaces.
  • interference pigments which consist of a platelet-shaped carrier material which is coated with a layer of titanium dioxide, are outstandingly suitable as a photocatalytically active material in coatings.
  • the present invention therefore relates to a photocatalytically active coating which contains as the photocatalytically active material interference pigments based on platelet-shaped substrates coated with a layer of titanium dioxide.
  • the invention also provides a process for producing a photocatalytically active coating, wherein a surface is coated with a coating composition, the interference pigments based on titanium dioxide coated platelet-shaped substrates as photocatalytically active material and at least one suitable binder and optionally a solvent and / or other auxiliaries and / or additives, and the resulting coating is allowed to dry and / or cure.
  • Another object of the present invention is a process for the preparation of a photocatalytically active coating in which a surface is coated with a coating composition containing at least one suitable binder and optionally a solvent and / or other auxiliaries and / or additives, and the like obtained
  • the present invention furthermore relates to a photocatalytically active coating composition which comprises at least one binder and, as photocatalytically active material, interference pigments based on platelet-shaped substrates coated with a layer of titanium dioxide, optionally a solvent and optionally further additives and auxiliaries.
  • photocatalytically active surfaces comprising an above-mentioned coating are the subject of the present invention.
  • Interference pigments which are used according to the invention as a photocatalytic material are those interference pigments which are platelet-shaped
  • interference pigments which consist of a platelet-shaped substrate, which is coated on both sides, and in particular by interference pigments, in which the substrate is coated on all sides with a layer of titanium dioxide (coated).
  • Platelet-shaped substrates for the purposes of the invention are, for example, platelet-shaped natural or synthetic mica, kaolin, talc, other phyllosilicates, SiO 2 , glass, borosilicates, Al 2 O 3 , metal oxides, metals, or with one or more layers of metal oxides, metal oxide hydrates, metal suboxides , Metal fluorides, metal nitrides, metal oxynitrides or mixtures of these materials coated platelet-shaped natural or synthetic mica, kaolin, talc, other sheet silicates, SiO 2 , glass, borosilicates, Al 2 O 3 , metal oxides or metals suitable.
  • the size of these substrates is not critical per se.
  • the substrates generally have a thickness between 0.01 and 5 .mu.m, in particular between 0.05 and 4.5 .mu.m.
  • the extension in the length or width is usually between 1 and 250 ⁇ m, preferably between 2 and 200 ⁇ m and in particular between 2 and 100 ⁇ m. They usually have an aspect ratio (ratio of diameter to particle thickness) of 2: 1 to 25000: 1, and in particular from 3: 1 to 2000: 1.
  • Platelet-shaped natural mica for example muscovite mica, synthetic mica, platelet-shaped SiO 2 and glass platelets, have proven to be particularly suitable.
  • platelet-shaped supports of the abovementioned materials as substrates coated with one or more layers of metal oxides, metal oxide hydrides, metal suboxides, metal fluorides, metal nitrides, metal oxynitrides or mixtures of these materials is particularly advantageous if, in addition to the photocatalytic property of the interference pigments mentioned their color properties, ie whose interference colors are to be exploited in order to give the coating compositions added thereto and in particular the coatings produced with the latter additional color effects.
  • metal oxide, metal oxide hydrate, metal suboxide, metal fluoride, metal nitride, metal oxynitride layers or the mixtures of these materials may be low (refractive index ⁇ 1.8) or high refractive index (refractive index> 1.8).
  • Suitable metal oxides and metal oxide hydrates are all conventional layer-applied such compounds, e.g. Alumina, alumina hydrate, silica, silica hydrate, iron oxide, iron oxide hydrate, tin oxide, ceria, zinc oxide, zirconia, chromia,
  • Titanium oxide in particular titanium dioxide, titanium dioxide hydrate and mixed phases thereof, such as ilmenite or pseudobrookite.
  • metal suboxides can
  • the titanium suboxides are used.
  • a metal fluoride for example, magnesium fluoride is suitable.
  • metal nitrides or metal oxynitrides for example, the nitrides or oxynitrides of the metals titanium, zirconium and / or tantalum can be used. Preference is given to applying metal oxide, metal fluoride and / or metal oxide hydrate layers and very particularly preferably metal oxide and metal oxide hydrate layers to the platelet-shaped carrier materials.
  • a preferred high refractive index material is, for example, TiO 2 , while SiO 2 is preferably used as the low refractive index material.
  • interference effects only play a role when, in addition to the photocatalytic effectiveness of the interference pigments, interference color effects are desired. For this reason, the known interference effects of interference pigments should not be discussed in more detail here. In addition, it is possible to use the targeted selection of
  • the interference pigments have a layer of titanium dioxide deposited on a platelet-shaped substrate selected from the substrates described above.
  • both the substrates can be mixed and subsequently coated with T ⁇ O 2 , or different substrates are each coated with Ti ⁇ 2 and then mixed.
  • the titanium dioxide layer envelops the temperature-stable substrate completely or largely completely.
  • the thickness of the titanium dioxide layer is generally 1 to 400 nm, preferably 5 to 250 nm and in particular 10 to 200 nm.
  • the layer of titanium dioxide generally represents the outermost layer of the interference pigments or the outermost inorganic layer of the interference pigments.
  • Titanium dioxide in the context of the present invention is understood as meaning both pure titanium dioxide in crystalline form and titanium dioxide hydrate with different proportions of water. This is due to the fact that in the customary wet-chemical preparation process of the interference pigments titanium oxide hydrate is precipitated by hydrolysis of particular inorganic metal salts on a platelet-shaped substrate and then converted by a calcination process substantially into titanium dioxide. The case of not completely complete conversion into crystalline titanium dioxide should be included here.
  • the titanium dioxide is in the interference pigment in the rutile modification or at least predominantly, ie with a proportion of more than 50 wt.%, Preferably more than 60 wt.% And in particular more than 70 wt.%, Based on the total amount of Ti ⁇ 2 , in the rutile modification.
  • titanium dioxide can also be present in the anatase modification or at least predominantly in the anatase modification.
  • an interference pigment which consists of a
  • Substrate of natural mica and a layer of titanium dioxide in the anatase or rutile modification or a mixture of anatase and rutile modification is coated on at least one side, but preferably on both sides with the titanium dioxide layer, and in particular completely or at least largely completely surrounded by the titanium dioxide layer.
  • Such pigments are commercially available as products of Merck KGaA, for example under the name Iriodin® 100 and Iriodin® 103. They are transparent and give coatings a silvery
  • interference pigments are used which consist of natural mica with a layer of titanium dioxide in the rutile modification located thereon.
  • Rutile modification inevitably in the production of the pigments, since the formation of the rutile modification usually at temperatures of about 700 to 750 0 C sets and the interference pigments by default at more than 800 0 C, in particular more than 900 0 C and preferably more than 950 ° C are annealed.
  • the application of the titanium dioxide layer on the platelet-shaped substrate can be carried out wet-chemically from organic or inorganic metal salts, by means of sol-gel methods, CVD and / or PVD methods.
  • a coating is wet-chemically, and in particular wet-chemically with inorganic starting materials.
  • the said methods can also be used for applying single or multiple layers on the carrier material, which are located below the titanium dioxide layer and together with the carrier material form the platelet-shaped substrate.
  • Their composition has already been described above. Such methods are known per se and have been described in detail in the prior art.
  • the substrate particles are suspended in water and admixed with one or more hydrolyzable, especially inorganic, metal salts (eg inorganic titanium salts such as titanium tetrachloride which are suitable for the application of the titanium dioxide layer) at a pH which is suitable for the hydrolysis and which is selected is that the metal oxides or metal oxide are precipitated directly on the platelets, without causing precipitation.
  • the pH is usually kept constant by simultaneous addition of a base and / or acid.
  • the pigments are separated, washed and dried at 50-150 0 C for 6-18 h and annealed for 0.5-3 h, the annealing temperature can be optimized with respect to the particular coating present.
  • the annealing temperatures are between 500 and 1200 ° C, preferably between 600 and 1000 0 C, and in particular between 750 and 950 0 C.
  • the pigments may be separated, dried and, if necessary, calcined, and then re-suspended to precipitate further layers.
  • SiO 2 layers are applied to the substrate, their precipitation generally takes place by adding a potassium or sodium waterglass solution at a suitable pH. But here are others as well
  • Suitable application method such as the application of organic silicon compounds or the order of a SoI-GeI method.
  • a coating can also be carried out in a fluidized bed reactor
  • an interference pigment is used in which the substrate is coated with the various materials described above in such a way that the layer of titanium dioxide represents the outermost or the outermost inorganic coating of the finished pigment.
  • the interference pigments used should expediently be surface-modified, so that in the not yet dried or cured coating composition the so-called leafing effect of the interference pigments, ie their floating and parallel alignment of the pigment platelets the surface of the coating can take place. It comes through the platelet shape the interference pigments for the formation of smooth, largely flat surfaces of the coating, which leads to a high proportion of the surface covered by interference pigments on the total surface, even at a relatively low concentration of the interference pigments in the coating composition, and thus an almost complete the surface lying photocatalytically active TiO 2 layer has.
  • This leafing effect only occurs when the platelet-shaped interference pigments have a high surface tension in the surrounding medium.
  • This high surface tension can be generated by various surface modifiers.
  • the type of surface modifier will be based on the medium surrounding the pigments (binders, solvents and / or additives and other additives).
  • binder, solvents and / or additives and other additives in a hydrophilic medium rather hydrophobic surface-modifying agents, in a hydrophobic medium rather hydrophilic surface-modifying agents are used.
  • the photocatalytically active coating according to the present invention is preferably to be used in the customary coating methods and media which predominantly have a hydrophilic, ie water-attracting, character, preferably hydrophobic, ie water-repellent, acting materials are used as surface modifiers.
  • These materials have one or more functional groups that bind to or interact with reactive groups present on the surface of the interference pigments (for example, OH groups). Furthermore, they have at least one hydrophobic
  • carboxylic acids particularly preference is given to using carboxylic acids, carboxylic acid halides, carboxylic acid esters and carboxylic anhydrides which contain, as hydrophobic group, long-chain aliphatic hydrocarbon groups which may also contain fluorine atoms.
  • alkyl radicals having 3 to 30 carbon atoms and in particular fatty acid radicals having more than 12
  • Carbon atoms are preferred.
  • stearic acid hepta- decafluorononanoic acid, heptafluorobutyric acid chloride, hexanoyl chloride, hexanoic acid methyl ester, perfluoroheptanoic acid methyl ester, perfluorooctanoic acid anhydride, or hexanoic anhydride should be mentioned here.
  • Stearic acid is particularly preferably used.
  • the hydrolyzable silanes used are those which have at least one nonhydrolyzable hydrophobic group.
  • the hydrophobic group used is preferably, but not exclusively, long-chain aliphatic hydrocarbon groups which may also have fluorine atoms. Examples which may be mentioned are hexadecyltrimethoxysilane, hexadecyltriethoxysilane, methyltriethoxysilane, dodecyltriethoxysilane and also propyltrimethoxysilane, of which methyltriethoxysilane and hexadecyltriethoxysilane are preferred.
  • polymer particles which are chemically bound in the unaggregated state on the surface of the interference pigments.
  • These polymer particles are preferably finely divided particles of colloidal ethylenically unsaturated carboxylic acid type resins. They are generally in a proportion of 0.1 to 20% by weight, based on the interference pigment, before and generally have Sizes of 1000 nm or smaller and molecular weights of 10,000 to 3,000,000.
  • the polymer particles contain as the monomer component at least one component comprising an ethylenically unsaturated carboxylic acid salt, an ethylenically unsaturated carboxylic acid or a carboxylate of this type and are usually homopolymers of these monomers or copolymers of these compounds with other ethylenically unsaturated monomers.
  • suitable monomers are acrylic acid, methacrylic acid, itaconic acid, maleic acid and anhydride, fumaric acid and crotonic acid, but also aromatic carboxylic acids, etc., as well as their salts and esters.
  • the surface-modified interference pigments of this type are particularly suitable for use in organic media, as are frequently used, for example, in printing inks and paints. These include, for example, various types of polyester acrylate resins, polyurethane acrylates, polyether acrylates, acrylic melamine resins and various types of aromatic solvents, natural fats and oils.
  • the surface-modified interference pigments arrange themselves preferably parallel to the surface of the still moist coating, thus showing the leafing effect described above.
  • the photocatalytically active coating additionally contains an infrared-absorbing material.
  • This material is preferably present in particulate form.
  • the average particle size of the particles is variable within wide limits and can be adapted in each case to the layer thickness of the coating or other requirements.
  • the mean particle size of the infrared light absorbing material is 0.001 to 100 .mu.m, preferably 0.01 to 50 .mu.m and in particular 0.01 to 30 microns.
  • the infrared absorbing material is preferably selected from the following compounds: LaB 6 , CeB 6 , SmB 6 , YB 6 , Mo 2 B 5 , SiB 6 , SiB 4 , ZrB 2 , TiB 2 , VB 2 , CrB 2 , antimony doped Tin oxide, carbon black, graphite or B 4 C, or mixtures of two or more of these compounds. Particularly preferred are LaB 6 and antimony-doped tin oxide.
  • lanthanum hexaboride is marketed by Stark, Goslar, and antimony-doped tin oxide can be obtained from Merck KGaA, Darmstadt, under the name Minatec® A-IR 230.
  • the infrared-absorbing material in the coating according to the invention ensures that the absorption of the heat radiation components of the sunlight increases the average temperature of the coating.
  • the inclination of the surfaces for growing / mossing decreases and the photocatalytic activity of the interference pigments used is high enough, even on the comparatively cold north sides of outdoor facilities, to prevent or prevent overgrowth, erosion or persistence of the organic material to severely restrict.
  • the photocatalytically active coating according to the invention is formed as one or more layers.
  • the total layer thickness of the coating can generally vary within a wide range from about 0.1 ⁇ m to about 1000 ⁇ m and is preferably in the range from 0.5 to 100 ⁇ m and in particular in the range from 0.6 to 20 ⁇ m.
  • Range of greater than 1000 microns are also generally suitable, is a such high layer thickness uneconomical, because their effectiveness against the said layer thickness range does not increase.
  • the interference pigments are preferably located on the surface of the coating. To do this with the
  • the interference pigments in this case ideally have one of the organic surface modifications described above. This ensures that the pigments do not disperse homogeneously in the coating composition but, in the still moist state of the coating composition, float on the surface of the applied layer and orient themselves parallel to the surface. In this way, the formation of a smooth surface is achieved, wherein even with a comparatively low pigment concentration, a large part of the surface of the coating is covered by interference pigments.
  • a homogeneous distribution of the interference pigments in the coating composition is generally desirable because of the more uniform color effect.
  • the other solid ingredients of the coating composition ie, for example, the above-mentioned infrared-absorbing materials, if any, or the binder or binders and optionally present auxiliaries and additives in the single-layer coating, however, preferably in a homogeneous distribution.
  • the interference pigments are located at least in the uppermost outermost layer of this multilayer coating.
  • the interference pigments are present on the surface of this outermost layer, as previously described in the single-layer coating.
  • the underlying layer (s) may have the same or different ingredients than the top layer.
  • the interference pigments as such form the uppermost layer.
  • the above-mentioned interference pigments are superficially applied to a binder-containing primer layer which may additionally also contain solvents, infrared-absorbing materials, said photocatalytically active interference pigments and, if appropriate, further auxiliaries and / or additives in the still moist state by means of a so-called bronzing process so that they form their own layer, which consists almost entirely of interference pigments.
  • a two-layer composite is formed whose outermost layer consists essentially of interference pigments. If appropriate, further layers of different composition can be present on the surfaces to be treated below the primer layer.
  • the layer thickness of the uppermost layer which consists almost completely of interference pigments, can be kept within the range of nanometers, depending on the layer thickness of the pigments. In general, the proportion of this layer in the total layer thickness is about 0.1 to about 20 microns.
  • the single-layer coating or at least the uppermost layer of a multi-layer Beschich device contains the interference pigments in an amount of 1 to 80
  • Mass% in particular from 5 to 50 mass%, based on the dry mass of the coating.
  • infrared-absorbing materials are present in the single- or multi-layer coating, these are in the single-layer coating or at least one of the binder-containing layers of the multilayer coating in an amount of 1 to 80% by mass, in particular from 5 to 50 mass -%, based on the dry mass of the respective layer or layers.
  • the present invention also provides processes for the preparation of photocatalytically active coatings.
  • this is a process in which a surface is coated with a coating composition, the interference pigments based on titanium dioxide coated platelet-shaped substrates as photocatalytically active material and at least one suitable binder, optionally a solvent and / or other auxiliaries and additives, and the coating thus applied is allowed to dry and / or cure.
  • both a single-layer and a multilayer coating can be produced. It is advantageous if, at least in the coating composition used to produce the uppermost layer of a multi-layer system or a single coating, the photocatalytically active interference pigments are surface-modified as described above so that they float on the surface of the still moist coating composition accumulate and arrange as far as possible parallel to the surface, before then the coating is allowed to dry and / or allowed to cure.
  • the surface modifier which attaches to the outer surface of the outer photocatalytically active interference pigments can then be removed either by suitable mechanical or chemical means, or the photocatalytic effect of the interference pigments is exploited to the extent that this surface modifier, which is organic, is gradually degraded by the photocatalytic activity of the interference pigments, thereby the photocatalytic activity of the interference pigments can then also unfold over externally acting organic substances. If the surface modifier is previously removed, the photocatalytic activity against external organic substances becomes more effective.
  • the coating composition additionally contains an infrared-absorbing material, in particular the previously described materials.
  • the process for producing a photocatalytically active coating is such a process in which a surface is coated with a coating composition which comprises at least one suitable binder and, if appropriate, a solvent and / or further auxiliary substances.
  • the interference pigments are applied to the binder-containing substrate in a suitable manner, for example, powdered, dusted or brushed.
  • a layer forms on the surface, which consists almost completely of interference pigments, which are arranged on the surface plane-parallel on the binder-containing layer. Stick by the adhesive effect of the binder these interference pigments on the surface of the coating. If the solvent dries and / or hardens the binder, a permanent two-layer coating is obtained in this way.
  • the binder must be adapted to the type of substrate. While for many applications the usual paint binders, oil varnishes or adhesives as
  • Binders can be used for substrates such as glass and glass ceramic water glass solution is a suitable binder.
  • the coating composition may additionally contain interference pigments based on platelet-shaped substrates coated with a layer of titanium dioxide.
  • the coating composition preferably additionally contains an infrared-absorbing material, irrespective of whether the described photocatalytically active interference pigments are likewise present or not.
  • photocatalytically active interference pigments in particular those are used in which the platelet-shaped substrate is coated on both sides, in particular on all sides, with a layer of titanium dioxide.
  • the coating of the surfaces to be treated in the process of the invention is carried out using standard application techniques, ie, for example, by brushing, knife coating, rolling, spraying, spraying, drawing, spinning, flooding or dipping.
  • the resulting layer is at a temperature in the range from 5 ° C to 180 0 C, preferably in the range from 10 ° C to 4O 0 C, dry and / or allowed to cure.
  • the drying or curing of the layer can be accelerated by the usual aids, such as UV or IR irradiation or a self-curing two-component system, etc.
  • the surfaces to be coated according to the invention are those surfaces which are exposed to the influence of light, in particular artificial or natural sunlight containing UV light, and water, and which are sustainable against overgrowth, floury, veraing or other contamination by organic materials should be protected.
  • the material composition of these surfaces plays a subordinate role.
  • it can be surfaces
  • Such surfaces are, for example, on the outer surfaces of structures, means of transportation and means of transport, sports and leisure equipment, gardening equipment or equipment, on paths and lanes and the like, the enumeration of which is merely exemplary here.
  • the coatings applied according to the invention are over an extended period, i. Durable and photocatalytically active for a few months to years, so that the objects to be protected are sustainably protected against organic soiling.
  • the surfaces provided with the coating according to the invention have their own photocatalytic activity.
  • the present invention also provides a photocatalytically active coating composition which contains at least one binder and, as photocatalytically active material, interference pigments based on platelet-shaped substrates coated with a layer of titanium dioxide, optionally with solvents and optionally further auxiliaries and / or additives.
  • the coating composition according to the invention preferably additionally comprises an infrared-absorbing material, which is particularly preferably in particulate form.
  • the interference pigments are expediently used in a surface-modified form, as has already been described above.
  • the photocatalytically active interference pigments are generally present in the coating composition in an amount of from 1 to 80% by weight, in particular from 5 to 50% by weight, based on the solids content of the coating composition.
  • an infrared absorbing material When an infrared absorbing material is contained in the coating composition, it is generally present in an amount of from 1 to 80% by mass, more preferably from 5 to 50% by mass, based on the solid content of the coating composition.
  • Suitable binders, solvents, auxiliaries and additives are the materials commonly used in the various known coating processes.
  • organic polymers preferably transparent organic polymers
  • binders examples include polystyrene, polyvinyl chloride and their copolymers and graft polymers, polyvinylidene chloride and fluoride, polyamides, polyolefins, polyacrylic and vinyl esters, thermoplastic polyurethanes, cellulose esters, the previously mentioned polyester acrylate resins, polyurethane acrylates, polyether acrylates and acrylic Melamine resins, and the like in question. They can be used individually or in suitable mixtures.
  • building materials such as cement, clays or frits can be used as inorganic binders.
  • these are preferably used in the lower layers of a multi-layer system.
  • Another suitable inorganic binder is, as already mentioned above, water glass, which is preferably used on glass and glass ceramic substrates.
  • the solvents used are preferably water and water-miscible solvents, for example ethanol or ethoxypropanol.
  • water-miscible solvents for example ethanol or ethoxypropanol.
  • aromatic solvents, fats, oils and the like are used.
  • auxiliaries and additives are customary materials which are commonly used as fillers, UV stabilizers, inhibitors, flame retardants, lubricants, plasticizers, dispersants, colorants or the like. Their use largely depends on the type of application method or the nature or material of the surfaces to be treated or the additionally desired effects (for example color design). The person skilled in the art is readily able to make a corresponding selection for this purpose.
  • the interference pigments used according to the invention as photocatalytically active material have the advantage that, if required, they can also be prepared in such a way that, in addition to the photocatalytic activity, they also have interference colors. Depending on the coating material used and the thickness of the layers, these can be varied as desired in a wide range. In addition to silvery or golden shimmering pigments, clear colors such as red, blue or green are possible in different shades, so that a large color spectrum can be achieved. Varying with the proportion of interference pigments in the coating composition or the amount of the pure pigment in the outermost pigment layer, a wide variety of color effects can be achieved either only by the interference pigments used or by mixtures of these with otherwise commonly used coloring minerals, metal oxides or other colorants the coatings produced therewith are achieved.
  • interference pigments Iriodin® 100 and Iriodin® 103 from Merck KGaA have a silvery white pearlescent color when used in large quantities in coatings.
  • photocatalytically active coatings especially for weather-affected outer surfaces, are provided which can sustainably prevent the overgrowth, persistence and mottling of such surfaces with sufficient activity, can be produced by a conventional application method, easily and on the market contain ingredients that are available at low cost, and that do not present the health risks that nanomaterials may be expected to cause, as some of the pigments are even suitable for human consumption.
  • the coatings according to the invention which preferably contain commercial interference pigments as a photocatalytic constituent, represent an inexpensive and effective solution for preventing undesired growth on, in particular, external surfaces of all kinds.
  • Screen printing lacquer (Aqua-Jet 093 from Pröll, Weissenburg) incorporated and set the required pressure viscosity.
  • a screen printing machine ne of the company Atmar, equipped with a sieve 77T 1 , the obtained screen printing ink is applied to a facade element made of a wood fiber composite material with a cover layer of acrylic resin over the entire surface.
  • the drying of the printing ink takes place at normal temperature. During the drying phase, the pigment particles arrange themselves on the surface of the printed surface.
  • the printed area has a silvery white color.
  • an interference pigment [Iriodin® 103, TiO 2 (rutile) on mica, product of Merck KGaA, Darmstadt] are coated with 40 g of stearic acid in a 5 liter jacketed stainless steel vessel. 15 g of the thus coated pigment are incorporated in 85 g of a solvent-containing screen printing lacquer (MZ-093 from Pröll, Weissenburg) and the required printing viscosity is set.
  • a screen printing machine from Atmar, equipped with a sieve 77T, the screen printing ink obtained is applied to a facade element made of a wood fiber composite material with a cover layer of acrylic resin over the entire surface. The drying of the printing ink takes place at normal temperature. During the drying phase, the pigment particles arrange themselves on the surface of the printed surface. The printed area has a silvery white color.
  • the facade elements produced in Examples 1 and 2 together with a facade element of the same type as a comparative object, which, however, is not subjected to surface coating and therefore has a brown color, stored outdoors in a shaded area in a moist environment. After 2 months, a visual assessment of the facade elements, in which it can be determined that the uncoated facade element on a not irrelevant area fraction has a green color by incipient "Bemoosung", while the invention coated facade elements according to Examples 1 and 2 have no color change.

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  • Chemical & Material Sciences (AREA)
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  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Laminated Bodies (AREA)

Abstract

La présente invention concerne des revêtements à action photocatalytique pour les surfaces de bâtiments, véhicules, appareils, équipements, chaussées et similaires, qui contiennent des pigments d'interférence comme matériau à action photocatalytique ainsi que le cas échéant un matériau absorbant la lumière infrarouge, des procédés de fabrication de telles surfaces et des objets comportant un tel revêtement.
EP07801867A 2006-09-20 2007-08-24 Revêtement à action photocatalytique Withdrawn EP2064292A2 (fr)

Applications Claiming Priority (2)

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DE102006044076A DE102006044076A1 (de) 2006-09-20 2006-09-20 Photokatalytisch aktive Beschichtung
PCT/EP2007/007439 WO2008034510A2 (fr) 2006-09-20 2007-08-24 Revêtement à action photocatalytique

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EP2064292A2 true EP2064292A2 (fr) 2009-06-03

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US (1) US8324129B2 (fr)
EP (1) EP2064292A2 (fr)
JP (1) JP2010504190A (fr)
CN (1) CN101517010A (fr)
DE (1) DE102006044076A1 (fr)
WO (1) WO2008034510A2 (fr)

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US20100022383A1 (en) 2010-01-28
DE102006044076A1 (de) 2008-03-27
JP2010504190A (ja) 2010-02-12
CN101517010A (zh) 2009-08-26
US8324129B2 (en) 2012-12-04
WO2008034510A2 (fr) 2008-03-27
WO2008034510A3 (fr) 2008-08-21

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