EP1326928A1 - Particules composites - Google Patents

Particules composites

Info

Publication number
EP1326928A1
EP1326928A1 EP01969777A EP01969777A EP1326928A1 EP 1326928 A1 EP1326928 A1 EP 1326928A1 EP 01969777 A EP01969777 A EP 01969777A EP 01969777 A EP01969777 A EP 01969777A EP 1326928 A1 EP1326928 A1 EP 1326928A1
Authority
EP
European Patent Office
Prior art keywords
particles
composite
inorganic
pigment
organic
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.)
Ceased
Application number
EP01969777A
Other languages
German (de)
English (en)
Inventor
Daniel-Gordon Duff
Werner Hoheisel
Kai BÜTJE
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.)
Bayer Intellectual Property GmbH
Original Assignee
Bayer AG
Bayer MaterialScience AG
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 Bayer AG, Bayer MaterialScience AG filed Critical Bayer AG
Publication of EP1326928A1 publication Critical patent/EP1326928A1/fr
Ceased 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
    • C09C1/0081—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound
    • 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
    • C09C1/22—Compounds of iron
    • C09C1/24—Oxides of iron
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
    • Y10T428/2996—Glass particles or spheres
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2998—Coated including synthetic resin or polymer

Definitions

  • the present invention relates to composite particles which represent significantly improved modifications of inorganic and organic pigments and which, depending on the pigment material, act as absorbers for visible and / or infrared light and can therefore be used as colorants and or as infrared (IR) light absorbers and cause negligible clouding of the matrix.
  • the composite particles according to the invention can be used in media in which high transparency, that is to say a low turbidity, is important, such as, for. B. in
  • inorganic pigments which are used in transparent systems, may have a size of less than 10 nm or only a few 10 nm in order not to cause additional cloudiness. Because of their generally lower refractive index, this limit is found for organic pigments with somewhat larger particle sizes, but here too too large pigments cause turbidity. In addition, these small particles - they are also called “nanoparticles"
  • a disadvantage of the known technical solutions to this problem is the high time and cost-intensive effort involved in incorporating the nanoparticles into the matrix in the required degree of dispersion.
  • the particles which are usually in the form of powders or pastes, are subjected to intensive shear forces (e.g. by grinding) in order to break up the agglomerates present in such small units that the scattering of light by these units and thus also the clouding of the matrix
  • the distribution of the UV-absorbing inorganic particles in or on approximately 300 nm large dielectric particles is reported, which in turn are then introduced into the matrix as carriers ( WO 95/09895).
  • the material of the large dielectric particles is selected in accordance with the matrix used in such a way that the refractive index of the compound particle consisting of dielectric particles and pigment differs only slightly from the refractive index of the surrounding matrix, thus maximizing transmission in the entire visible part of the light spectrum ,
  • this literature only discloses UV-absorbing particles such.
  • Iron oxide haematite which is applied to silicon dioxide, is also described for use as a heterogeneous catalyst (React. Kinet. Catal. Lett. (1999), 66, 183-18).
  • a possible use as a transparent pigment is not discussed, and the transfer of catalyst properties to optical properties of pigments in a plastic or lacquer matrix is in no way obvious.
  • IR light is understood here to mean light which is in the solar radiation beyond the visibility limit, ie. H. is contained in the wavelength range between approx. 700 nm and approx. 2500 nm.
  • composite particles which contain inorganic and / or organic pigment particles with a primary particle size of 1 nm to 100 nm, preferably between 1 nm and 50 nm, which are based on solid inorganic or organic colorless carrier particles of a primary particle size of 1 nm to 200 nm adhere, wherein either the pigment primary particles are essentially not agglomerated with other pigment primary particles and also generally are at a certain minimum distance from one another or that any agglomerates of these pigment primary particles which are formed are less than 100 nm, preferably less than 50 nm, and these are then at a certain minimum distance from one another. Said minimum distance should generally be at least a quarter of the particle or agglomerate diameter.
  • pigment should be understood to mean those particles which absorb visible and / or infrared light.
  • a matrix is understood to be a dielectric material such as B. a clear coat, paint, plastic, glass or a coating material.
  • the primary particle size is defined so that it corresponds to the diameter of a sphere with the same volume.
  • a matrix is understood to be a dielectric material such as B. a clear coat, paint, plastic, glass or a coating material.
  • the carrier particles or the shells around the pigment particles thus act as spacers for the optically active pigment cores, which are up to a few tens of nanometers in size, in order to decouple them electromagnetically. With such a decoupling, no substantial light scattering is caused by an agglomeration of the carrier particles or the coated particles.
  • a further prerequisite for reducing the light scattering from the supported or coated pigments is that the material of the support or the casing has a refractive index similar to that of the surrounding matrix. In most material combinations between carrier or shell and pigment, the material of the carrier should be an even lower and in a few cases a slightly higher one
  • the invention therefore relates to composite particles which contain inorganic and or organic pigment particles with an average primary particle size of 1 nm to 100 nm, preferably between 1 nm and 50 nm, which are based on solid inorganic or organic colorless carrier particles with an average particle size of 1 nm to 200 nm stick, characterized in that the pigment primary particles are not substantially agglomerated with other pigment primary particles and are generally at a certain minimum distance from one another, this distance should generally be a quarter of the pigment primary particle diameter.
  • the invention further relates to composite particles which contain pigment particles with an average primary particle size of 1 nm to 100 nm, preferably 1 nm to 50 nm, which are coated with other primary particles, also called coating particles, or with a solid inorganic or organic layer, the Layer thickness of the shell should generally be at least one eighth of the pigment primary particle diameter.
  • the invention furthermore relates to composite particles which contain agglomerates of inorganic and / or organic pigment particles with an average primary particle size of 1 nm to 100 nm, preferably between 1 nm and 50 nm.
  • Said agglomerates adhere to solid inorganic or organic colorless carrier particles with an average primary particle size of 1 nm to 200 nm and are characterized in that they are on average less than 100 nm, preferably less than 50 nm, and usually at a certain minimum distance stand to each other, this distance should generally be a quarter of the agglomerate diameter.
  • the invention furthermore relates to composite particles which contain agglomerates of inorganic and / or organic pigment particles with a primary particle size of on average 1 nm to 100 nm, preferably between 1 nm and 50 nm. Said agglomerates are on average less than 100 nm, preferably less than 50 nm, which are coated with a solid or particulate, inorganic or organic layer, the total layer thickness of the shell generally being at least one eighth of the agglomerate diameter.
  • the invention further relates to compostite particles, as described above, but which contain combinations of different types of pigment particles, carrier particles and / or coating particles.
  • objects of the invention are transparent coloring and / or transparent IR-absorbing coating materials consisting of the composite particles, which are coated in a clear lacquer (for example polyester, acrylic, alkyd resin, chlorinated rubber, epoxy resin, acrylic resin, oil -, nitro, polyester, polyurethane and combination paints based on cellulose nitrate and alkyd resin), plastic or glass are incorporated.
  • a clear lacquer for example polyester, acrylic, alkyd resin, chlorinated rubber, epoxy resin, acrylic resin, oil -, nitro, polyester, polyurethane and combination paints based on cellulose nitrate and alkyd resin
  • objects of the invention are transparently colored and / or transparent IR-absorbing materials consisting of a plastic (for example polycarbonate, polyamide, polyethylene, polypropylene, polymethyl acrylate, polymethyl methacrylate, Polyurethane, polyethylene terephthalate, polystyrene, styrene acrylonitrile) or glass, in which the composite particles according to the invention are incorporated.
  • a plastic for example polycarbonate, polyamide, polyethylene, polypropylene, polymethyl acrylate, polymethyl methacrylate, Polyurethane, polyethylene terephthalate, polystyrene, styrene acrylonitrile
  • inorganic pigments includes metals such as B. Cu, Ag, Au, Pt, Pd, Co or alloys of these elements, semiconductors such. B. Si and all oxides,
  • the term inorganic pigments also includes doped materials such as B. tin-doped indium oxide, aluminum-doped zinc oxide, antimony-doped tin oxide, fluorine-doped tin oxide or metal-doped silicon oxide.
  • Materials which are suitable as inorganic pigment in the sense of the invention are also inorganic materials whose crystal lattice (host material) is doped with such foreign ions, so that the material fluoresces.
  • host material such foreign ions
  • These include in particular all materials and material classes that are used as so-called phosphors in fluorescent screens or fluorescent lamps and as described in Ullmann's Encyclopedia of Industrial Chemistry, WILEY-VCH, 6 * edition, 1999 Electronic Release, chapter
  • Luminescent Materials 1. Inorganic Phosphors” are mentioned. Materials suitable for the purposes of the invention as inorganic pigment are therefore materials of the type XY: A, where X is a cation from one or more elements of the main groups la, 2a, 3a, 4a, the subgroups 2b, 3b, 4b, 5b, 6b, 7b or the lanthanides of the periodic table, Y is either a polyatomic anion from one or more element (s) of the main groups 3a, 4a, 5a, the subgroups 3b, 4b , 5b, 6b, 7b and or 8b and element (s) of main groups 6a and / or 7 or a monatomic anion from main group 5a, 6a or 7a of the periodic table and A is the doping material from anions from one or more elements of the lanthanides and / or elements of the main groups la, 2a and or AI, Cr, Tl, Mn,
  • the concentration of the doping material in the host lattice is between 10 "5 mol% and 50 mol%, before increases between 0.01 mol% and 30 mol%, particularly preferably between 0.1 mol% and 20 mol%.
  • sulfides preference is given to sulfides, selenides, sulfoselenides, oxysulfides, borates, aluminates, gallates, silicates,
  • (A Sr, Ca, Ba); (Sr, Mg) 2 P2 ⁇ 7: Eu; (Sr, Mg) 3 (PO) 2 : Sn; SrS: Ce; SrS: Sm, Ce;
  • SrS Sm; SrS: Eu; SrS: Eu, Sm; SrS: Cu, Ag; Sr 2 P2 ⁇ 7: Sn; Sr 2 P2 ⁇ 7: Eu;
  • Ln lanthanide
  • YNO4.-A lanthanide, In
  • Y (PN) O 4 Eu
  • YTaO 4 ⁇ b
  • materials for the carrier or the encapsulation particles come such oxides, fluorides, chlorides of metals and semiconductors and e.g. Aluminosilicates or polymers in question, which are essentially transparent in the visible spectral range.
  • volume concentration refers to the proportion of the pigment volume in the total volume of the solid phase of the composite particles.
  • the total volume is the volume of the pigment plus that of the carrier material but without any empty spaces in the composite.
  • non-metallic pigments are present in a volume concentration of 1% - 60% and metallic pigments at 1% - 40% based on the pigment / carrier composite or pigment / carrier composite. In a particularly preferred embodiment, non-metallic pigments are present in a volume concentration of 10% - 50% and metallic pigments at 5% - 20%, based on the pigment / carrier composite.
  • non-metallic pigments are present in a volume concentration of 1% - 60% and metallic pigments at 1% - 40%, based on the shell pigment composite.
  • non-metallic pigments are present in a volume concentration of 10% - 50%) and metallic pigments are 5% - 20% based on the shell pigment composite.
  • the carrier particles or the shell material have a real refractive index in the visible spectral range, which is between 1.3 and 1.9.
  • the use of silicon dioxide as carrier material or shell material is particularly advantageous.
  • the refractive index of the composite of pigment and carrier particles is equal to that of the matrix in which the composite particles are incorporated for the purpose of coloring.
  • the volume concentration of the pigment is based on the pigment / carrier
  • C v ⁇ is the volume concentration of the pigment based on the pigment / carrier composite
  • N ma the refractive index of the matrix in which the composite is embedded
  • N tr the refractive index of the carrier material
  • N p - the refractive index of the pigment.
  • Refractive index is understood here to mean the real part of the same.
  • the refractive index of the composite may differ slightly, preferably not more than 0.3 units, from that of the surrounding matrix.
  • permissible agglomerates are
  • Carrier-pigment composites or pigment / coating particle composite less than 50 ⁇ m, particularly preferably less than 10 ⁇ m, very particularly preferably less than 2 ⁇ m, in order to avoid specks visible to the naked eye and to ensure a homogeneous color impression or infrared absorption.
  • the composite can be modified on the surface by means of inorganic or organic aftertreatment, so that the dispersibility of the composite in the matrix is improved.
  • iron oxide nanoparticles with a size of approximately 10 nm, which have been applied to silicon dioxide particles, were used. This particle size was determined on the basis of electron microscopic examinations.
  • the predispersion was treated with an ultrasound finger (200 W, 5 min).
  • the iron oxide sol was then added to the silicon dioxide dispersion with stirring, sodium hydroxide solution was added until the pH reached 3.5 and the mixture was stirred for a further 5 minutes.
  • the solid was separated off by centrifugation and then dried at 80 ° C. in a vacuum drying cabinet for several hours.
  • a lacquer layer was produced in the following way.
  • the base paint consisted of a mixture of 3500.0 g of alkyd resin ® Alkydal F 48 (55% dry residue was in 38: 7 Spirit: xylene; Bayer AG, DE), 385.0 g of solvent naphtha 100, 28.8 g
  • Hematite was adjusted to 1% by weight based on the dry paint. The mixture was then dispersed for 3 hours. The drying agents were added immediately before the dispersion.
  • the fully dispersed lacquers were filtered through disposable sieves with a mesh size of approx. 280 ⁇ m.
  • the dispersed varnishes were applied to black and white tiles (opal glass tiles) using a paint bar (gap height depending on requirements). Drying takes place for one day at room temperature and then for 1 h at 65 ° C in a drying cabinet. Diffuse reflection spectra in the ultraviolet and visible spectral range were recorded.
  • Figures 1 and 2 demonstrate the advantageous properties of the paint described above based on the composite particles according to the invention.
  • the illustrations show the diffuse reflection of the paint spreads on the black and white surface as a function of the wavelength.
  • Fig. 3 show that agglomerates in the size range of up to a few micrometers are present.
  • unsupported pigments such agglomerates inevitably lead to an undesirable cloudiness (see comparative example).
  • the advantageous color impression of the supported pigments, even in the case of poor dispersion, is made clear on the basis of CIELAB values, which were measured with the Lambda 900 color measuring device from Perkin Elmer (see table).
  • iron oxide nanoparticles with a size of approximately 10 nm, which have been applied to silicon dioxide particles, were used. This particle size could be confirmed by means of electron microscopic examinations.
  • the iron oxide dispersion was prepared as described in Example 1.
  • the iron oxide sol was then added to the silicon dioxide dispersion with stirring, sodium hydroxide solution was added until the pH reached 3.5 and the mixture was stirred for a further 5 minutes.
  • the solid was separated by centrifugation and then dried at 80 ° C. in a vacuum drying cabinet.
  • the test specimen of the color properties of the pigment was carried out as already described in Example 1.
  • Figures 4 and 5 demonstrate the advantageous properties of the lacquer described above based on the composite particle according to the invention.
  • the images show the diffuse reflection of the paint spreads on the black and white surface as a function of the wavelength.
  • the reflection from this varnish on the black surface (Fig. 4) is independent of the wavelength and is less than 1% in the range between 400 nm and 800 nm.
  • the reflection increases by less than 1% at a wavelength of 400 nm to over 75% at 720 nm. This shows the low scattering and high absorption capacity of the lacquer based on composite particles that contain iron oxide pigment.
  • the composite particles containing the supported pigment are present in this lacquer layer even in a poorly dispersed state. Electron microscope images (Fig. 6) show that agglomerates in the size range of up to a few micrometers are present. In the case of unsupported pigment, such agglomerates inevitably lead to an undesirable cloudiness (see comparative example).
  • the pestle is loaded with the highest pressure by moving the weight on the lever arm.
  • the weight and lever arm are flush.
  • the speed of the friction cup was 70 min "1 (at 50 Hz mains frequency).
  • the friction cup has an inner diameter of 150 mm.
  • the pestle has a diameter of 70 mm
  • Mill manufacturer adjusted so that the ground material was pushed from the wall under the pestle. 2.0 g of pigment were weighed out. The milling time was 30 minutes.
  • the base paint consisted of a mixture of 3500.0 g of alkyd resin ® Alkydal F 48 (55% dry residue in 38: 7 TestbenzimXylol; Bayer AG, DE), 385.0 g of solvent naphtha 100, 28.8 g of 2-butanone oxime, 55% by weight in white spirit, and 96.3 g of l-methoxy-2-propyl acetate.
  • the dispersion was carried out in a ball mill (PM 4 planetary high-speed mill
  • Trok- kenscher (0.94 g-octa-soligen lead with 24% Pb; 0.25 g-octa-soligen cobalt with 6% Co (Borchers GmbH, Monheim, DE) and a lot of composite particles were in the grinding set (250 ml agate grinding container) added so that a concentration of composite particles corresponding to 13% by weight based on the dry paint was set. The whole was then dispersed for 4 hours. The dry substances were added immediately before the dispersion. "The finished dispersed paints were mixed with disposable sieves 400 ⁇ m mesh size filtered.
  • the lacquered cardboard (spread) was then dried for at least 12 h at room temperature.
  • Figures 7 and 8 demonstrate the advantageous properties of the paint described above based on the composite particles according to the invention. It shows the diffuse reflection of the paint spreads on the black and white surface as a function of the wavelength.
  • FeSO 4 solution was converted according to the prior art (DE-A 2 508 932, US-A
  • Levasil 300 silica sol approx. 30% by weight SiO 2 (commercial product from Bayer AG, DE), was diluted to 31.5 g SiO / l with non-ferrous water.
  • the dispersion had a pH of 10.3.
  • the composite was filtered through a membrane filter (0.45 ⁇ m pore size) and washed with demineralized water until the conductivity of the filtrate was ⁇ 100 ⁇ S / cm.
  • Figures 9 and 10 demonstrate the advantageous properties of the paint described above based on the composite particles according to the invention.
  • the images show the diffuse reflection of the paint spreads on the black and white surface as a function of the wavelength.
  • ITO tin-doped indium oxide
  • the solid was separated by centrifugation and then at 80 ° C. in
  • Vacuum drying cabinet dried within several hours.
  • the ITO silicon dioxide composite powder obtained in this way was then subjected to dry grinding.
  • the base paint consisted of a mixture of 3500.0 g of alkyd resin ® Alkydal F 48 (55% dry residue in 38: 7 TestbenzimXylol; Bayer AG, DE), 28.7 g 2-butanone oxime , 55% by weight in white spirit, 47.8 g Octa Solingen Calcium 4 basic (Borchers GmbH, Monheim,
  • a plate paint rubbing machine (Muller), as described in DIN EN ISO 8780-5 (April 1995), was used to incorporate the composite particles into the paint. (JEL 25/53, J. Engelsmann AG, Ludwigshafen, DE). The effective plate diameter was 24 cm. The speed of the lower plate was approximately 75 min "1. By hanging a 2.5 kg load weight on the load bracket, the force between the plates was set to approximately 0.5 kN.
  • Figures 11 and 12 demonstrate the advantageous properties of the paint described above based on the composite particles according to the invention.
  • the illustrations show the diffuse reflection of the paint spreads on the black and white surface as a function of the wavelength.
  • Composite particles consisting of iron oxide-silicon dioxide composite were produced as explained in Example 2. The powder obtained in this way was then subjected to dry grinding. The Pulverisette ® 2 mill described in Example 3 was used under the conditions described there.
  • a plastic plate colored with the composite particles was then produced.
  • 1 g of the composite particles was added to 199 g of granules of the polcarbonate to obtain a 0.5% by weight mixture. This was placed in a kneader (Brabender kneader) and kneaded at 230 ° C. for 10 minutes at a speed of 30 rpm.
  • sample (a) By weight of hematite and approximately 80% by weight of silicon oxide. This ratio of the hematite and silicon oxide proportions is optimized for incorporation into polycarbonate in accordance with the relationship C vo ⁇ ⁇ (Nma - Nt r ) (N P i - N tr ) given in the description. This sample is referred to below as sample (a).
  • the color value (according to CIELAB with illuminant D65, 10 ° observer) and the haze (haze according to ASTM D 1003) of the po- lycarbonate plate measured.
  • the haze value was 9%.
  • composite particles were produced analogously to Example 2, in which the weight ratios between hematite and silicon oxide (b) approx. 50% by weight / 50% by weight, (c) approx. 33% by weight / 67% by weight and (d) approx. 10 These composite particles were then incorporated into polycarbonate according to the method given above in this example.
  • the content of carrier pigment in the polycarbonate was ( b) about 0.2% by weight, (c) about 0.3% by weight and (d) about 1% by weight.
  • ITO tin-doped indium oxide
  • a plastic plate was then produced which contained the composite particles produced in this way.
  • 3.2 g of the composite particles were added to 196.8 g of granules of the polycarbonate to obtain a 1.6% by weight mixture. This was placed in a kneader (Brabender kneader) and at 230 ° C for 10 min with a
  • the solid was dried at 100 ° C for 12 hours and then heated in air for 10 hours at 500 ° C, resulting in decomposition of the iron oxalate and formation of iron oxide particles.
  • the iron oxide-silica composite powder thus obtained was then subjected to dry grinding.
  • the Pulverisette 2 mill described in Example 3 was used under the conditions described there.
  • Figures 14 and 15 demonstrate the advantageous properties of the paint described above based on the composite particles according to the invention.
  • the images show the diffuse reflection of the paint spreads on the black and white surface as a function of the wavelength.
  • the reflection from this varnish on the black surface shows only a slight dependence on the wavelength and is below 14% in the range between 400 nm and 800 nm.
  • the reflection on the white surface increases from less than 2% at a wavelength of 400 nm to over 75% at 720 nm. This shows the low scattering and high absorption capacity of the transparent lacquer based on the iron oxide pigment.
  • an iron oxide / Silicon dioxide-containing solid produced, in the synthesis of which both substances are formed by reaction from precursors.
  • the solid gel thus formed was then successively dried at 60 ° C for two days, at 80 ° C for two days and then at 100 ° C for two days.
  • the sample was then calcined at 800 ° C. overnight (air-annealed).
  • the iron oxide-silicon dioxide composite obtained in this way was then subjected to dry grinding.
  • the Puverisette ® 2 described in Example 3 was used under the conditions described there. Here too, the grinding time was 30 minutes.
  • Figures 16 and 17 demonstrate the advantageous properties of the paint described above based on the composite particles according to the invention.
  • the images show the diffuse reflection of the paint spreads on the black and white surface as a function of the wavelength.
  • the iron oxide dispersion was prepared as described in Example 1.
  • FIGs 18 and 19 show the reflection of such a lacquer layer on a black or white background.
  • the measurement curves shown for comparison show a higher reflection of the paint on the black surface (Fig. 18), which is caused by the increased scattering effect of the agglomerated pigments.
  • the reflection of the varnish from the white surface is significantly lower, which is equivalent to a duller shade (Fig. 19).
  • the measurement curves demonstrate the clear advantage with regard to the color properties for the lacquer which contains the composite particles according to the invention.
  • the following table shows a comparison of the CIELAB values which were measured using the Perkin Elmer Lambda 900 color measuring device.

Abstract

La présente invention concerne des améliorations apportées à des pigments inorganiques et organiques. Ces pigments, selon leur nature, peuvent être utilisés comme absorbeurs de lumière infrarouge ou comme colorants et occasionnent une opacification négligeable de la matrice.
EP01969777A 2000-10-09 2001-09-26 Particules composites Ceased EP1326928A1 (fr)

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DE10049803A DE10049803A1 (de) 2000-10-09 2000-10-09 Kompositpartikel
DE10049803 2000-10-09
PCT/EP2001/011127 WO2002031060A1 (fr) 2000-10-09 2001-09-26 Particules composites

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US (1) US6565973B2 (fr)
EP (1) EP1326928A1 (fr)
JP (1) JP2004511612A (fr)
KR (1) KR100773221B1 (fr)
CN (1) CN1262610C (fr)
AU (1) AU2001289927A1 (fr)
DE (1) DE10049803A1 (fr)
HK (1) HK1061041A1 (fr)
TW (1) TWI316952B (fr)
WO (1) WO2002031060A1 (fr)

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DE10049803A1 (de) 2002-04-18
KR20030041154A (ko) 2003-05-23
CN1468289A (zh) 2004-01-14
JP2004511612A (ja) 2004-04-15
HK1061041A1 (en) 2004-09-03
TWI316952B (en) 2009-11-11
US20020071948A1 (en) 2002-06-13
CN1262610C (zh) 2006-07-05
KR100773221B1 (ko) 2007-11-02
AU2001289927A1 (en) 2002-04-22
US6565973B2 (en) 2003-05-20
WO2002031060A1 (fr) 2002-04-18

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