EP2021114A2 - Production de nanoparticules, notamment de matériaux composites en forme de nanoparticules, à partir d'agglomérats de poudre - Google Patents

Production de nanoparticules, notamment de matériaux composites en forme de nanoparticules, à partir d'agglomérats de poudre

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Publication number
EP2021114A2
EP2021114A2 EP07703457A EP07703457A EP2021114A2 EP 2021114 A2 EP2021114 A2 EP 2021114A2 EP 07703457 A EP07703457 A EP 07703457A EP 07703457 A EP07703457 A EP 07703457A EP 2021114 A2 EP2021114 A2 EP 2021114A2
Authority
EP
European Patent Office
Prior art keywords
particles
organic
matrix particles
aggregates
based matrix
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Withdrawn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
EP07703457A
Other languages
German (de)
English (en)
Inventor
Thomas Launag
Thomas Sawitowski
Bärbel Gertzen
Ulrich Nolte
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.)
BYK Chemie GmbH
Original Assignee
BYK Chemie 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 BYK Chemie GmbH filed Critical BYK Chemie GmbH
Publication of EP2021114A2 publication Critical patent/EP2021114A2/fr
Withdrawn legal-status Critical Current

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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
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/10—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in stationary drums or troughs, provided with kneading or mixing appliances
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C13/00—Disintegrating by mills having rotary beater elements ; Hammer mills
    • B02C13/10—Disintegrating by mills having rotary beater elements ; Hammer mills with horizontal rotor shaft and axial flow
    • B02C13/12—Disintegrating by mills having rotary beater elements ; Hammer mills with horizontal rotor shaft and axial flow with vortex chamber
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C7/00—Crushing or disintegrating by disc mills
    • B02C7/02—Crushing or disintegrating by disc mills with coaxial discs
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • 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
    • C08K9/08—Ingredients agglomerated by treatment with a binding agent
    • 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
    • C09D5/03—Powdery paints
    • 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
    • C09D5/03—Powdery paints
    • C09D5/033—Powdery paints characterised by the 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/67—Particle size smaller than 100 nm
    • 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
    • C09D7/66—Additives characterised by particle size
    • C09D7/68—Particle size between 100-1000 nm
    • 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
    • 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
    • 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
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/70—Nanostructure
    • Y10S977/773—Nanoparticle, i.e. structure having three dimensions of 100 nm or less
    • 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
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/70—Nanostructure
    • Y10S977/778—Nanostructure within specified host or matrix material, e.g. nanocomposite films
    • Y10S977/783—Organic host/matrix, e.g. lipid

Definitions

  • nanoparticles in particular nanoparticle composites, starting from powder agglomerates
  • the present invention relates to the preparation of nanoparticles, in particular nanoparticle composites, starting from powder agglomerates or powder aggregates.
  • the present invention relates to a process for the preparation of preferably particulate composite materials, in particular of generally inorganic and organic constituents, as well as the composite materials produced in this way and their use.
  • organically modified particles eg., Organo harshsilikate
  • z. B. using chemical modifications, etc.
  • the modification leads to a compatibilization with the matrix and thus facilitates the incorporation into the polymer.
  • the synthesis of the particles is such that, due to their surface chemistry and charge, they easily melt into polymer melts can be dispersed.
  • the particles are generated in situ (eg, by chemical precipitation of, for example, inorganic particles in organic media).
  • methods are known from the prior art, with which micro- or millimeter-sized particles can be dispersed in polymers, wherein z. B.
  • US 5 474 803 A describes the use of this process to produce polymer composites of two or more materials wherein a first component of larger particle diameter and lower softening point is modified with a second component of higher softening point on its surface.
  • No. 6,403,219 B1 describes the production of polymer composites by a growth reaction of acicular particles on the surface of a support material.
  • US 6 090 440 A describes the production of composites by the action of impact forces and subsequent chemical reaction of the shell particles.
  • the object of the present invention is to provide an efficient process for the production or production of preferably particulate composite materials.
  • the process should enable a problem-free dispersion of a discontinuous, organically or inorganically based phase in a continuous phase, in particular of at least one organic polymer or oligomer or another fusible organic compound, and advantageously at least largely avoid the previously described problems of the prior art or but at least mitigate it.
  • the present invention proposes a method according to claim 1; Further, advantageous embodiments are Subject of the method claims.
  • the present invention furthermore relates to the composite materials obtainable by the process according to the invention as defined in claims 21 to 23 and to the use thereof as claimed in claims 24 to 26.
  • the subject of the present invention is also a process for comminuting particle agglomerates or Aggregates or for the preparation of stable nanoparticles according to claim 27.
  • the present invention - according to a first aspect of the present invention - is thus a process for the production of particulate composite materials, wherein initially solid, in the dry state, in particular in powder form, present inorganic or organic based particle agglomerates or aggregates in the Gas phase (ie, in a gaseous carrier or reaction medium) and in the presence of organically-based matrix particles comminuted with energy input and subsequently dispersed the resulting comminuted particles in situ in the organically based matrix particles, in particular attached thereto and / or embedded therein.
  • gas phase in the context of the present invention means that the solid (ie present in the solid state) particle agglomerates or aggregates in a preferably inert, gaseous carrier or reaction medium (eg., Air, nitrogen-enriched air, nitrogen, etc.) be transferred (eg in the form of a fluidized bed or a fluidized bed, as described below), in particular by "atomizing” or “Eindüs” the solid particle agglomerates or aggregates, after which they then - as described above - in the gaseous carrier medium (“gas phase”) are comminuted with energy input, followed by in situ dispersion of the resulting comminuted particles in the likewise present, equally solid (ie present in the solid state) organically based matrix particles, so that a total of Dispersion takes place in the solid phase;
  • gas phase as used in the present invention thus does not refer to the state of aggregation of the particle agglomerates or aggregates or of the matrix particles (which both are present in the solid state of matter), but
  • the inorganic or organic based particle agglomerates or aggregates used as starting materials are deagglomerated or deaggregated to smaller, stable nanoparticles or nanopowders and subsequently in situ - before re-agglomeration or aggregation can occur the equally present organic-based matrix particles dispersed, both an addition and storage takes place.
  • the method according to the invention likewise encompasses an embedding and coating process: the comminuted, inorganic or organic-based particles are attached to the surface of the matrix particles by the introduced energy and embedded therein. Subsequent further introduction of energy results in further deformation, so that the particles to be stored are partly completely enclosed by the matrix particles and incorporated therein.
  • the introduction of energy causes deformation, in particular plastic deformation, of the organically based matrix particles and of the resulting composite materials; In particular, irregularly shaped particles are rounded off by plastic deformation, which is advantageous for subsequent use in the corresponding end products.
  • nanoparticulate, inorganic or organically based particles homogeneously and / or very finely divided-in the context of dry or solid dispersion in solid phase-into organically based matrix particles.
  • the method according to the invention can be carried out at any desired printing. According to the invention, it is preferable to proceed at normal or ambient pressure. Nevertheless, according to the invention, it is generally not excluded to proceed at reduced pressure ("vacuum” or “negative pressure”) or at elevated pressure (“overpressure”).
  • the energy input is selected such that the starting particle agglomerates or aggregates are comminuted with respect to their size by at least a factor of 10, preferably at least a factor of 50, preferably at least a factor of 100, particularly preferably at least a factor of 1,000 or deagglomerated or disaggregated.
  • the energy input takes place by introducing impact and / or shear forces, preferably impact and shear forces.
  • the total energy input can vary widely over the duration of the process.
  • the total energy input over the duration of the process is 10 to 10 6 kJ, in particular 10 2 to 10 6 kJ, preferably 10 2 to 10 5 kJ.
  • the process according to the invention is carried out in a fluidized bed or as a fluidized bed process.
  • a dry dispersion in particular powder dispersion, takes place in the solid phase ("solid-phase dispersing process” or “powder dispersing process”).
  • the gas phase or the gaseous carrier medium is formed as a fluidized bed or fluidized bed.
  • the subject matter of the present invention is thus a process for the production of particulate composite materials in which first solid, in dry state, in particular in powder form, present inorganic or organic based particle agglomerates or aggregates in a fluidized bed or in a fluidized bed and crushed in the presence of organically based matrix particles with energy input and subsequently the resulting comminuted particles are dispersed in situ in the organically based matrix particles, in particular attached thereto and / or incorporated herein, are.
  • the method according to the invention can be carried out in a device of the stator / rotor type.
  • Devices suitable according to the invention are marketed, for example, by Nara Machinery Co. Ltd., Zweigniedermik Europa, Frechen, Germany, under the name "Hybridizer” or 11 NHS ".
  • the single FIGURE shows a schematic section through an inventively usable device of the stator / rotor type.
  • the device 1 in addition to a stator 2 and a rotor 3 at least one baffle plate 4, preferably a plurality of baffles 4, for crushing the agglomerates or aggregates on their impact on the baffles 4.
  • an inlet 5, in particular powder inlet is generally provided.
  • a return line 6 is provided.
  • the device 1 may have a double-walled housing 7, which may be equipped to be cooled and / or heated.
  • the device 1 generally still has a closable outlet 8 for withdrawing or removing the manufactured products.
  • the dashed line in the figure in the interior of the device 1 shows an example of the course of a single particle in the device 1 at its impact.
  • the device used according to the invention is operated with a peripheral rotor speed of 50 to 120 m / s, in particular 70 to 100 m / s, preferably at a rotor diameter of 100 to 1000 mm.
  • the duration of the procedure can vary over wide limits.
  • the process time varies in the range of 0.01 to 20 minutes, in particular 0.1 to 10 minutes, preferably 0.5 to 5 minutes, particularly preferably 1 to 3 minutes.
  • the mean particle sizes of the starting agglomerates or aggregates are above 0.1 ⁇ m, in particular above 0.2 ⁇ m, preferably above 0.5 ⁇ m.
  • the starting agglomerates or aggregates have average particle sizes in the range from 0.1 to 2000 .mu.m, in particular 0.2 to 1500 .mu.m, more preferably 0.5 to 1250 .mu.m, most preferably 1 to 1000 .mu.m.
  • average particle size refers, in the case of spherical or nearly spherical particles, to the mean diameter thereof. In the case of other particle shapes (eg rods or tubes) it refers to the mean size in one dimension (eg in the case of elongated rods or tubes, for example, along their length or width).
  • the resulting comminuted particles generally have mean particle sizes below 500 nm, in particular below 200 nm, preferably below 100 nm.
  • the particles obtained by comminution of the starting agglomerates or aggregates have average particle sizes in the range of 1 to 500 nm, in particular 10 to 200 nm, preferably 20 to 100 nm, on. Because of these dimensions, the comminuted particles are sometimes also referred to in the context of the present invention as nanoparticles or nanopowders, which are subsequently dispersed in situ into the organically based matrix particles.
  • the organically based matrix particles have mean particle sizes in the range from 0.1 to 500 .mu.m, in particular from 0.5 to 100 .mu.m, particularly preferably from 1 to 50 .mu.m.
  • V D50 (Mat ⁇ xpiety) / D50 (comminuted particles) ⁇ 10: 1, in particular> 15: 1, preferably> 20: 1
  • the proportion of organically based matrix particles on the one hand to comminuted particles to be stored or embedded in the matrix particles on the other hand can equally vary within wide ranges.
  • the ratio of organic-based matrix particles, on the one hand, to comminuted particles dispersed therein, on the other hand varies in the range of 99.9: 0.1 to 30: 70, more preferably 90:10 to 40:60, preferably 80:20 to 50:50
  • the organically based matrix particles may be selected from fusible organic compounds.
  • the organically based matrix particles may comprise or consist of at least one organic oligomer or polymer.
  • the organically based matrix particles may comprise or consist of mixtures of different, in particular compatible, oligomers and / or polymers.
  • suitable matrix materials for the organically based matrix particles are, for.
  • thermoplastic polymers waxes, resins and mixtures thereof.
  • Equally suitable according to the invention are also other fusible organic compounds (eg fusible organic monomers such as ⁇ -caprolactone or its lactam, carboxylic esters and diesters such as dimethyl terephthalate, phenol-based esters and diesters, etc.).
  • Non-limiting examples of polymers useful for the organic matrix or carrier particles are e.g. B. thermoplastic polymers, in particular poly (meth) acrylates, polyacrylonitrile, polystyrene, styrenic plastics (eg., ABS, SEBS, SBS), polyesters, polycarbonates, polyethylene terephthalate (PET), polybutyl terephthalate, polyamides, thermoplastic polyurethanes (TPU) , Polyvinyl chloride, polyoxymethylene, polyolefins, such as polyethylenes or polypropylene, etc.
  • the thermoplastics may be filled and / or pigmented.
  • thermoplastics are also understood as meaning mixtures (blends) of different types of thermoplastics.
  • polyolefins such as polyethylene (eg LDPE, HDPE etc.) and polypropylene (PP), polyvinyl chloride (PVC), polystyrene (PS), polycarbonate (PC), polymethylmethacrylate (PMMA), acrylonitrile / butadiene / styrene - Graft copolymer (ABS), polyamide (PA), polyoxymethylene (POM) and ethylene / propylene / diene elastomer (EPDM) and blends of the listed thermoplastics can be used.
  • polyolefins such as polyethylene (eg LDPE, HDPE etc.) and polypropylene (PP), polyvinyl chloride (PVC), polystyrene (PS), polycarbonate (PC), polymethylmethacrylate (PMMA), acrylonitrile / butadiene / styren
  • Thermoplastics such as polyethylene (eg LDPE, HDPE etc.), polypropylene (PP), polyvinyl chloride (PVC), polystyrene (PS), polycarbonate (PC), polymethyl acrylate (PMMA), acrylonitrile / butadiene / styrene graft copolymer ( ABS), polyamide (PA), polyoxymethacrylate (POM), ethylene / propylene / diene elastomer (EPDM) and polyvinyl acetate (PVAc) as well as mixtures (blends) of the listed thermoplastics are particularly preferred.
  • polyethylene eg LDPE, HDPE etc.
  • PP polypropylene
  • PVC polyvinyl chloride
  • PS polystyrene
  • PC polycarbonate
  • PMMA polymethyl acrylate
  • PMMA acrylonitrile / butadiene / styrene graft copolymer
  • ABS polyamide
  • Organic resins such as epoxy resins, COOH polyester resins (e.g., saturated or unsaturated), OH polyester resins (e.g., saturated and unsaturated), OH acrylic resins, polyester polyols, polyether polyols, glycidyl acrylate resins, ethylene / vinyl alcohol copoly - mers, polyamides (for example polyamide 11 or 12), tetrahydroxyalkyl bisamides, triglycidyl diisocyanurate, dicyandiamides, isocyanate adducts, dodecanedicarboxylic acid, etc.
  • Organic resins such as epoxy resins, COOH polyester resins (e.g., saturated or unsaturated), OH polyester resins (e.g., saturated and unsaturated), OH acrylic resins, polyester polyols, polyether polyols, glycidyl acrylate resins, ethylene / vinyl alcohol copoly - mers, polyamides (for example poly
  • Organic waxes such as natural waxes (eg animal, vegetable and fossil waxes). se), such as bee (lanolin), carnauba, candelilla, paraffin, microcrystalline and montan waxes, semi-synthetic waxes, such as montan wax esters (fatty acid + alcohol) and amide waxes (fatty acid + amide), as well as synthetic waxes, in particular homopolymers, such as Polyethylene (PE), polypropylene (PP), polyamide (PA), polytetrafluoroethylene (PTFE), Fischer-Tropsch waxes and waxes based on polyvinyl acetate (PVAc), or copolymers such as ethylene vinyl acetate (EVA) or ethylene acrylic acid (EAA), as well as Mixtures (blends) from the listed waxes.
  • natural waxes eg animal, vegetable and fossil waxes. se
  • bee lanolin
  • carnauba candelilla
  • paraffin fatty acid + alcohol
  • the organic matrix or carrier particles include other fusible organic compounds, such as e.g. B. fusible organic monomers (for example, the aforementioned compounds).
  • the organically based matrix particles generally have a melting point or melting range of above 0 0 C. In general, the melting point or melting range of the organic-based matrix particles in the temperature range from 30 to 350 0 C, especially 40-330 0 C, preferably 70 to 160 0 C. ,
  • the organic-based matrix particles have a glass transition temperature Tg above -60 0 C.
  • the glass transition temperature of the organic-based matrix particles in the range from -60 to 200 0 C, in particular -40 to 150 0 C, preferably from -30 to 60 0 C.
  • the organic-based matrix particles i.e., the polymers or oligomers of which they are composed
  • the average molecular weight of the organic-based matrix particles is in the range of 300 to 30,000 g / mol, in particular 500 to 10,000 g / mol.
  • the organic-based matrix particles are plastically deformable under process conditions at least on their surface and preferably formed under process conditions plastically deformable.
  • the process according to the invention is carried out below the melting temperature or the melting range of the organically based matrix particles.
  • the process according to the invention can generally generally be carried out below or above the glass transition temperature of the organically based matrix particles; However, preference is given to above the glass transition temperature of the organically based matrix particles (at the same time, however, below the melting temperature or the melting range), because then the particles to be dispersed can penetrate the surface of the matrix particles better or more easily.
  • the process is carried out below the melting temperature of the inorganic or organic based particle agglomerates or aggregates.
  • solid phase dispersion (solid / solid dispersion” or “solid phase dispersion”) takes place, ie both the particles to be dispersed and the matrix particles are present under process conditions as solids or in the solid state .
  • the temperatures at which the process according to the invention is carried out can vary within wide limits. In general, the inventive method at temperatures ranging from 0 to 80 0 C, especially 5 to 50 0 C, preferably 10 to 40 ° C, particularly preferably 15 to 35 0 C is performed.
  • the nature of the particle agglomerates or aggregates used may in principle be inorganic or organic in nature. According to the invention, however, preference is given to using inorganic-based particle agglomerates or aggregates; In this case, so-called hybrid materials are obtained from inorganic and organic constituents, since in this case inorganic nanoparticles or nanopowders are incorporated into organically based matrix particles.
  • metals and / or semimetals and mixtures or alloys of different metals and / or semimetals can be used as particle agglomerates or aggregates.
  • oxides, hydroxides, carbides, nitrides, sulfides, tellurides, selenides, halides, carbonates, phosphates, sulfates, silicates, borates and / or aluminates of MeOH. to use metals and / or semi-metals.
  • inorganic oxides and mixed oxides such as.
  • alumina for example, for the modification of mechanical properties, such as scratch / abrasion resistance, etc.
  • titanium dioxide eg for UV protection
  • zinc oxide eg., For UV protection, for a bactericidal or fungicidal action, etc.
  • cerium dioxide eg for UV protection, etc.
  • Examples of materials which can be used according to the invention for the starting agglomerates or aggregates are, for example, Silicates, boehmites, talc, CNT, carbon nanofibers, Alosil, ZnO, titanium dioxide, iron oxides, magnetite, iron, cobalt, nickel, silver, phyllosilicates, magnesium hydroxide, ATH, pigments, ATO, ITO, fluorescent materials, for example and nonlimitingly , Alumina, zirconia, diamond, ceria, UV phosphors, up-converters, IR pigments, silsesquioxanes, POSS, calcium carbonate, ZnS, barium sulfate, boron nitride (BN), tungsten carbide (WC) etc.
  • a material for the discontinuous phase, d. H. for the starting agglomerates or aggregates for example, carbon, z. B. in the form of graphite, diamond, fullerenes, etc., for example in grain or fiber form, in rod or tubular form, etc., such. B. as single or multi-walled tubes.
  • Examples of basically equally usable organic starting agglomerates or aggregates are, for. Melamine particles, although less preferred than the inorganic based materials for the discontinuous phase to be dispersed in the matrix particles.
  • the shape or external shape of the starting particle agglomerates or aggregates used is not critical.
  • granular or granular or else spherical to ellipsoidal particle agglomerates or aggregates can be used.
  • rod or tubular agglomerates can also be used.
  • Another object of the present invention - according to a second aspect of the present invention - are the particulate Kompositma- materials which are obtainable by the process according to the invention described above.
  • particulate composite materials which are preferably in the form of a powder and have inorganic or organic-based particles with average particle sizes of 1 to 500 nm, which are preferably homogeneously or finely divided into organic-based matrix particles having mean particle sizes of 0, 1 to 500 microns dispersed, in particular attached thereto and / or incorporated herein are.
  • the mean particle size of the organic-based matrix particles D is 50 (M at ⁇ xpa r Tikei) generally is at least the tenfold, in particular at least 15-fold, preferably at least 20 times, the average particle diameter of the crushed particles D 50 (Z erklei n e r te T EILCs h e n) • for more details regarding the invention teilchenförmi- gen composite materials may be made to avoid unnecessary repetition of the above VERSIONS to the inventive process, which apply correspondingly in regard to the inventive particulate shaped composite materials.
  • the present invention thus serves in particular for the production of polymer particle composites having particle sizes in the stated range on the basis of a dry dispersing process using a stator / rotor-type device, in particular a mechanical hybridizer (eg from Nara Machinery Co. Ltd., Zweigniedermik Europa, Frechen, Germany), as described above.
  • a mechanical hybridizer eg from Nara Machinery Co. Ltd., Zweigniedermik Europa, Frechen, Germany
  • the process of the invention allows, for example, the production of polymer composites by the dry grinding of two or more powders utilizing mechanical impact and shear forces.
  • it is quite unexpectedly possible to break up the high particle interactions in the particle agglomerates, to disperse the particles, and thus to arrive at virtually agglomerate-free composites with filler contents of up to more than 50% in a very efficient manner.
  • the present invention thus relates to a process for producing nanoparticle composites by dispersing, for example, two or more powder components in a fluidized bed process.
  • the resulting powders are nanocomposites in which the nanoparticles The degree of agglomeration in or on an organic carrier is finely divided.
  • the process according to the invention can solve the problem of producing composite materials in which the continuous phase consists of a polymer (such as, for example, a polyolefin, polyester, polyamide, PVC, polystyrene, polysiloxane, polyacrylate, etc.) or an oligomer (such as polyethers, waxes, etc.) or other support material having a melting point above typically 0 ° C.
  • a polymer such as, for example, a polyolefin, polyester, polyamide, PVC, polystyrene, polysiloxane, polyacrylate, etc.
  • an oligomer such as polyethers, waxes, etc.
  • inorganic or organic particles eg, metals or Semi-metals, metal or semimetal oxides, nitrides, carbides, carbonates, hydroxides, sulfides, etc.
  • inorganic or organic particles eg, metals or Semi-metals, metal or semimetal oxides, nitrides, carbides, carbonates, hydroxides, sulfides, etc.
  • agglomerates or aggregates in which, owing to the large surface of mesoscopic particles, these particles adhere to one another with electrostatic and / or van der Waals forces can be efficiently separated from one another by the relatively high energy input and then deposited in the deagglomerated or de-segregated state to the matrix particles and / or incorporated therein, so that the production of homogeneous, agglomerate-free or at least agglomeratarmermer particulate composite is made possible.
  • the agglomerates are first broken up into stable nanoparticles, which are subsequently dispersed in situ into the matrix particles. It is surprising that, according to the invention, the nanoparticles can be prepared stably from the agglomerates or aggregates and subsequently dispersed in the matrix. Because it is essential that the surface of particles in the millimeter range, as used in the prior art, by a factor of 1,000 4 to 1,000 3 are smaller than that of nanoparticles with a diameter smaller than 100 nm; Even micrometer-sized particles have a surface which is smaller by a factor of 1.00O 2 to 1,000 than that of the mesoscopic particles mentioned here.
  • the surface energy and thus the adhesion forces are in turn a function of the specific surface area. These are therefore also many times larger with particles smaller as 100 nm compared to milli or micrometer sized particles. In this way, the dispersion, in particular of particles smaller than 100 nm, places particular demands on the surface chemistry of the particles and the apparatus performance.
  • the present invention now makes it possible to homogeneously disperse particles of said size in fusible organic carriers in amounts of up to more than 50%.
  • the result is a composite material consisting of a deagglomerated particle powder and an organic carrier, in which the particles are homogeneously distributed in and on the polymer particles and are dispersed in an almost agglomerate-free manner.
  • the particulate composite materials according to the invention can be used, for example, in coating compositions, paints and coatings of all kinds (for example in powder coatings, printing inks, leather and textile dyes and paper coatings), in molding compositions, in cosmetic preparations and in plastics (such as, for example, US Pat.
  • thermoplastics, Du- mereren or elastomers use.
  • the particulate composite materials can be used as a masterbatch or masterbatch for incorporation into products, especially for property change in products.
  • the particulate composite materials of the invention may be used for this purpose in amounts of from 0.1 to 10% by weight, in particular from 0.5 to 5% by weight, preferably from 1 to 3% by weight, based on the end products become.
  • the composites according to the invention can in turn be incorporated in known processes into organic matrices using low shear forces and thus act as a so-called masterbatch.
  • the composite materials themselves can be used directly in a wide variety of applications without necessarily being further mixed with organic materials.
  • organic matrices can be significantly changed in their properties: So the incorporation of materials such. For example, ZnO, titanium dioxide, iron oxide or ceria for improved resistance to UV radiation.
  • biocidal materials such as silver, silver compounds, copper oxides, etc.
  • biocidal materials such as silver, silver compounds, copper oxides, etc.
  • carbon tubes eg single-wall or multi-wall
  • carbon fibers eg single-wall or multi-wall
  • conductive oxides or metals e.g single-wall or multi-wall
  • conductive composites with good antistatic or truly conductive equipment can be produced.
  • materials such as alumina, silica, phyllosilicates, talc, boehmite, carbon dust, calcium carbonate, barium sulfate, etc.
  • mechanical properties such as toughness, stiffness, Young's modulus, impact resistance, etc. can be improved.
  • the composite materials produced by the process according to the invention enable a large number of different applications in a wide variety of fields.
  • the composite materials produced by the process according to the invention are suitable for use in thermoplastics, thermosets, elastomers, such as.
  • Polyolefins such as polyethylene (eg LDPE, HDPE etc.) or polypropylene (PP), polyvinyl chloride (PVC), polystyrenes (PS), polycarbonates (PC), polymethyl methacrylate (PMMA), acrylonitrile / styrene graft copolymers (ABS), polyamides (PA), polyoxymethylene (POM), unsaturated polyesters (UP), epoxy resins (EP), melamine resins (MF), phenolic resins (PF), polyurethanes (PUR), ethylene / propylene / diene elastomers
  • Polyolefins such as polyethylene (eg LDPE, HDPE etc.) or polypropylene (PP), polyvinyl chloride (PVC), polystyrenes (PS), polycarbonates (PC), polymethyl me
  • the composite materials produced by the process according to the invention are suitable for use in powder coatings, such as polyester, hybrid (polyester / EP) and acrylate powders, in aqueous, organic solvent or solvent-free paints, printing inks, paper coating, leather and textile dyes, Molding compounds, cosmetic preparations and the like.
  • powder coatings such as polyester, hybrid (polyester / EP) and acrylate powders
  • the composite materials produced by the process according to the invention are suitable for changing the properties of their use in with regard to the products to which they are added, e.g.
  • flame retardance UV protection, magnetism, IR adsorption, product protection, (gas) barrier effect, surface polarity, coatability, mechanics, sliding properties, bacteriocidal effect, algicidal action, fungicidal action, anti-yeast effect, tribological properties , Scratch resistance / abrasion resistance, antistatic, rheological properties, flow behavior, dispersibility, stabilization of non-nanoscale fillers, etc.
  • a further subject matter of the present invention is, according to a fourth aspect of the present invention, a method for comminuting particle agglomerates or aggregates or for producing stable nanoparticles, in which solid, in the dry state, in particular in powder form, is present inorganically or organically Particle agglomerates or aggregates having average particle sizes above 0.1 .mu.m, in particular in the range from 0.1 to 2000 .mu.m, in the gas phase or in a gaseous carrier medium with introduction of energy into nanoparticles with average particle sizes of below 500 nm, in particular in the range of 1 to 500 nm, be crushed.
  • a polyester powder is dispersed with the aforementioned stator / rotor device of the company Nara type NHS-I with 30% zinc oxide of the type NanoTec ZH for one minute at 6,000 U / min.
  • 2% by weight of these nanocomposites are used in the preparation of a pigmented powder coating, and coatings are produced therewith.
  • CERA-Wachs Ceraflour 988 is dispersed with the aforementioned stator / rotor device from Nara type NHS-I with 50% Nanodur alumina for 1 minute at 6,000 U / min. Subsequently, 4% by weight of these nanocomposites according to the invention (hereinafter referred to as "T-23") are used. characterized in a 100% UV system (solvent-free) based on an aromatic epoxy acrylate used.
  • the binder is weighed in with the reactive diluents and the photoinitiator, and the components are mixed for five minutes by stirring with a dissolver.

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Abstract

La présente invention concerne un procédé de production de matériaux composites en forme de particules. Ce procédé consiste d'abord à broyer avec un apport d'énergie des agglomérats ou des agrégats de particules solides à base inorganique ou organique, à l'état sec, se présentant notamment sous forme de poudre, en phase gazeuse ou dans un support gazeux et en présence de particules matricielles à base organique, puis à disperser les particules broyées résultantes dans les particules matricielles à base organique, notamment à les y insérer et/ou à les fixer sur celles-ci. Les matériaux composites ainsi produits peuvent être utilisés de multiples façons et conviennent particulièrement à une utilisation dans des matières plastiques de différents types, dans des substances de revêtement, dans des colorants et dans des peintures, en particulier dans des peintures en poudre, pour modifier les propriétés de ces produits lorsqu'ils sont utilisés dans ceux-ci et dans des produits similaires.
EP07703457A 2006-03-29 2007-02-14 Production de nanoparticules, notamment de matériaux composites en forme de nanoparticules, à partir d'agglomérats de poudre Withdrawn EP2021114A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102006014786 2006-03-29
DE102006025848A DE102006025848A1 (de) 2006-03-29 2006-06-02 Herstellung von Nanopartikeln, insbesondere Nanopartikelkompositen, ausgehend von Pulveragglomeraten
PCT/EP2007/001270 WO2007112805A2 (fr) 2006-03-29 2007-02-14 Production de nanoparticules, notamment de matériaux composites en forme de nanoparticules, à partir d'agglomérats de poudre

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US (1) US8956660B2 (fr)
EP (1) EP2021114A2 (fr)
JP (1) JP5528102B2 (fr)
KR (1) KR100991394B1 (fr)
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CA (1) CA2647178C (fr)
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KR20090005339A (ko) 2009-01-13
US8956660B2 (en) 2015-02-17
DE102006025848A1 (de) 2007-10-04
US20100034857A1 (en) 2010-02-11
KR100991394B1 (ko) 2010-11-02
CN101454074B (zh) 2011-11-16
JP2009531197A (ja) 2009-09-03
WO2007112805A2 (fr) 2007-10-11
JP5528102B2 (ja) 2014-06-25
CN101454074A (zh) 2009-06-10
CA2647178C (fr) 2012-07-03
CA2647178A1 (fr) 2007-10-11
WO2007112805A3 (fr) 2008-02-28

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