DE102007022457A1 - Plasma-modified natural minerals with nanoscale properties, process for their preparation and their use - Google Patents
Plasma-modified natural minerals with nanoscale properties, process for their preparation and their use Download PDFInfo
- Publication number
- DE102007022457A1 DE102007022457A1 DE200710022457 DE102007022457A DE102007022457A1 DE 102007022457 A1 DE102007022457 A1 DE 102007022457A1 DE 200710022457 DE200710022457 DE 200710022457 DE 102007022457 A DE102007022457 A DE 102007022457A DE 102007022457 A1 DE102007022457 A1 DE 102007022457A1
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- Germany
- Prior art keywords
- plasma
- products according
- mineral products
- nanoparticles
- treated mineral
- 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.)
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Classifications
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- 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
- C09C1/40—Compounds of aluminium
- C09C1/42—Clays
-
- 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
- C01P2006/16—Pore diameter
-
- 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
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Abstract
Die vorliegende Erfindung betrifft plasmabehandelte natürliche Minerale mit nanoskaligen Eigenschaften, hergestellt aus Nanopartikeln, die aus natürlichen geologischen Vorkommen gewonnen werden. Mögliche Anwendungsgebiete sind Kosmetika, Pharmazeutika oder Nano-Kompositwerkstoffe. Vorzugsweise wird ein Niederdruckplasma oder ein Atmospharendruckplasma verwendet. Die Herstellung der plasmabehandelten natürlichen Minerale erfolgt durch Beschichtung von trocknem Mineralpulver in einem Plasmareaktor mit einer kohlenstoffhaltigen Schicht und anschließender Abscheidung von stickstoffhaltigen funktionellen Gruppen auf der Oberfläche der Mineralpulver.The present invention relates to plasma-treated natural minerals having nanoscale properties prepared from nanoparticles derived from natural geological occurrences. Possible applications are cosmetics, pharmaceuticals or nano-composite materials. Preferably, a low pressure plasma or an atmospheric pressure plasma is used. The plasma-treated natural minerals are produced by coating dry mineral powder in a plasma reactor with a carbon-containing layer and then depositing nitrogen-containing functional groups on the surface of the mineral powder.
Description
Die vorliegende Erfindung betrifft plasmabehandelte natürliche Minerale mit nanoskaligen Eigenschaften, hergestellt aus Nanopartikeln, die aus natürlichen geologischen Vorkommen gewonnen werden. Mögliche Anwendungsgebiete sind Kosmetika, Pharmazeutika oder Nano-Kompositwerkstoffe.The The present invention relates to plasma-treated natural Minerals with nanoscale properties, made from nanoparticles, obtained from natural geological resources. Possible applications are cosmetics, pharmaceuticals or nano composite materials.
Stand der TechnikState of the art
Die Verwendung von natürlichen Nanopartikeln als funktionelle Füllstoffe und deren Herstellungsverfahren sind für folgende Applikationen beschrieben:
- • Herstellung
von Thermo- und Duroplastwerkstoffen (
DE 60114538 T2 EP 1195775 A1 EP 0813955 A2 - • Herstellung von Farben und Tinten (
EP 1426422 A1 - • Herstellung von Flammverzögerungsharzen
(
JP 2006089534 A KR 1020030021620 A - • Herstellung von Polymer-Nanokompositen (
US 20040097630 A1 WO 2000034180 A1 WO 2000034378 A1 WO 2000034380 A1 WO 2002024750 A2 WO 2000024760 A1 WO 9801346 A2 - • Herstellung von transparenten Kunststoffen mit elektrisch
leitfähigen Bahnen (
WO 2004098254 A1 WO 2004099836 A1 - • Herstellung von beschichteten Verpackungsmaterialien
(
WO 2001066653 A1 - • Herstellung von Zwei-Komponenten-Klebstoff (
US 20050019510 A1 - • Herstellung von Oberflächenbeschichtungen
(
WO 2001096511 A2
- • Production of thermo and thermoset materials (
DE 60114538 T2 EP 1195775 A1 EP 0813955 A2 - • Production of inks and inks (
EP 1426422 A1 - Preparation of flame retardant resins (
JP 2006089534 A KR 1020030021620 A - • production of polymer nanocomposites (
US 20040097630 A1 WO 2000034180 A1 WO 2000034378 A1 WO 2000034380 A1 WO 2002024750 A2 WO 2000024760 A1 WO 9801346 A2 - Production of transparent plastics with electrically conductive webs
WO 2004098254 A1 WO 2004099836 A1 - • production of coated packaging materials (
WO 2001066653 A1 - • production of two-component adhesive (
US 20050019510 A1 - • production of surface coatings (
WO 2001096511 A2
Gewöhnlich werden als natürliche Minerale Smektite, Talk, Karbonate, Glimmer, Silica oder Kaolinit/Halloysit eingesetzt, wobei durch diverse Aufbereitungsverfahren die Kornverfeinerung (bis ca. 100 nm) erreicht bzw. durch Desagglomeration/Exfoliation, insbesondere ausgewählter Tonminerale, die Nanoskalierung erzielt wird.Usually are natural minerals smectites, talc, carbonates, Mica, silica or kaolinite / halloysite are used, passing through various processing methods grain refinement (up to approx. 100 nm) achieved or by deagglomeration / exfoliation, in particular selected Clay minerals, the nanoscale is achieved.
Diese natürlichen Nanopartikel stehen als preisgünstige funktionelle Fülleralternativen zu synthetischen Nanopartikeln (Kohlenstoff-Nanotubes-CNT, Nano-Metallpartikel – wie Silber oder Titanoxid) für diverse Anwendungen zur Verfügung.These Natural nanoparticles are considered cheap functional filler alternatives to synthetic nanoparticles (Carbon nanotube CNT, nano-metal particles - like silver or titanium oxide) for various applications.
Neben der äußeren nanoskalierten Morphologie weisen einige der natürlichen Minerale nanoskalierte innere Porenräume aus, die für diverse Anwendungen (z. B. drug delivery) von Interesse sind. Dies betrifft Diatomite, Zeolithe und Halloysite, wobei die Durchmesser der Nanoporen zwischen 0,3 und ca. 20 nm schwanken.Next the outer nanoscale morphology point some of the natural minerals have nano-scaled internal pore spaces out for various applications (eg drug delivery) are of interest. This concerns diatomites, zeolites and halloysites, wherein the diameters of the nanopores fluctuate between 0.3 and about 20 nm.
Nachteile der bisher verwendeten Nanopartikel sind die hohen Herstellungskosten, insbesondere bei synthetischen Nanopartikeln und die z. T. ungenügende Dispergierbarkeit in organischen Matrixsystemen von mineralischen Nanopartikeln.disadvantage The nanoparticles used hitherto are the high production costs, especially with synthetic nanoparticles and the z. T. insufficient Dispersibility in organic matrix systems of mineral Nanoparticles.
Aufgabe der ErfindungObject of the invention
Die Aufgabe der Erfindung bestand darin die im Stand der Technik genannten Nachteile der Nanopartikel zu beseitigen und damit neue Anwendungsmöglichkeiten bereitzustellen.The The object of the invention was that mentioned in the prior art Disadvantages of nanoparticles eliminate and thus new applications provide.
Lösung der AufgabeSolution of the task
Die Aufgabe wurde gemäß den Merkmalen der Patentansprüche gelöst. Erfindungsgemäß wurden ausgewählte natürliche Mineralprodukte mit nanoskaligen Eigenschaften (Primärmorphologie und Nanoporen) hergestellt, die durch Behandlung mit Plasmen, vorzugsweise Niedertemperaturplasmen, erhalten wurden.The Task has been in accordance with the features of the claims solved. Selected according to the invention natural mineral products with nanoscale properties (Primary morphology and nanopores) produced by Treatment with plasmas, preferably low temperature plasmas were.
Überraschenderweise hat sich herausgestellt, dass dabei eine Zerstörung der Kristallstruktur und eingelagerter Wassermoleküle nicht eintritt, die natürliche mikrobiologische Keimbelastung reduziert wird und die Dispergierbarkeit in diversen Matrixsystemen durch Hydrophilierung, Hydrophobierung oder Beschichtung verbessert wird.Surprisingly has been found to be a destruction of the Crystal structure and embedded water molecules not occurs, the natural microbial germ load is reduced and the dispersibility in various matrix systems improved by hydrophilization, hydrophobing or coating becomes.
Damit ist einerseits eine optimale Anpassung an die Matrix in Verbund- und Schichtsystemen möglich, was mit höherem Füllungsgrad und besserer Haftung und Dispergierbarkeit verbunden ist und andererseits kann eine verbesserte Spurenelementdotierung (z. B. In, Se) oder Wirkstoffdotierung erfolgen, was für spezielle Life-Science-Produkte (Kosmetik, Medizinprodukte, Pharmaka, Tierarzneimittel und Medizinalfutter) bedeutsam ist.In order to On the one hand, optimal adaptation to the matrix in composite and layer systems possible, what with higher degree of filling and better adhesion and dispersibility, and on the other hand can be an improved trace element doping (eg In, Se) or Drug doping done, which is special for life science products (Cosmetics, medical devices, pharmaceuticals, veterinary drugs and medicated feed) is significant.
Die erfindungsgemäßen plasmamodifizierten natürlichen Minerale mit nanoskaligen Eigenschaften, wie Halloysit, eignen sich für den Einbau in Verbund- und Schichtsysteme. Halloysit besitzt ein hohes Aspektverhältnis und ist damit für den Aufbau von netzartigen Strukturen geeignet. Weiterhin besitzen die Halloysit-Partikel eine röhrenförmige Morphologie. Damit können im Nanoporenraum, z. B. pharmazeutische Wirkstoffe oder Spurenelemente angelagert werden, die dann nach der Aufnahme in den menschlichen oder tierischen Körper verzögert wieder freigesetzt werden. Voraussetzung für die Verwendung des Halloysits in diesen Anwendungen ist eine Plasmabehandlung, die einerseits eine vollständige und homogene Oberflächenmodifizierung (Sauerstoff- oder Stickstoff-Funktionalisierung und Beschichtung mit kohlenstoffhaltigen Schichten) realisiert und andererseits zu keinen Veränderungen in der Struktur und der Form der Partikel fuhrt. Erst durch einen derartig oberflächenbehandelten Halloysit kann optimal in einer Matrix dispergiert werden bzw. es können Wirkstoffe oder Spurenelemente angelagert werden. Für eine derartige Oberflächenbehandlung wurde ein Plasmaverfahren bereitgestellt, bei dem Halloysitpulver z. B. als Haufwerk mit einer Schichtdicke von mindestens 5 mm auf einer Schale oder in einer Trommel liegt und durch mechanische Aktivierung ständig bewegt wird, so dass die einzelnen Teilchen nur zeitweise mit dem Plasma in Berührung kommen. Dadurch wird gewährleistet, dass der Energieeintrag auf die einzelnen Teilchen nicht kontinuierlich, sondern diskontinuierlich erfolgt und somit eine Schädigung vermieden werden kann. Zusätzlich kann hierfür auch ein gepulstes Plasma eingesetzt werden.The plasma-modified natural minerals according to the invention with nanoscale properties, such as halloysite, are suitable for incorporation in composite and layer systems. Halloysite has a high aspect ratio and is therefore suitable for the construction of net-like structures. Furthermore, the halloysite particles have a tubular morphology. This can be in the nanopore space, z. As pharmaceutical agents or trace elements are attached, which are then released after being absorbed into the human or animal body delayed. A prerequisite for the use of the halloysite in these applications is a plasma treatment, which realizes on the one hand a complete and homogeneous surface modification (oxygen or nitrogen functionalization and coating with carbonaceous layers) and on the other hand leads to no changes in the structure and shape of the particles. Only by such a surface-treated Halloysit can be optimally dispersed in a matrix or it can be added active ingredients or trace elements. For such a surface treatment, a plasma process was provided in which Halloysitpulver z. B. as a debris with a layer thickness of at least 5 mm on a dish or in a drum and is constantly moved by mechanical activation, so that the individual particles come into contact only temporarily with the plasma. This ensures that the energy input to the individual particles is not continuous, but discontinuous and thus damage can be avoided. In addition, a pulsed plasma can also be used for this purpose.
Die Erfindung soll anhand eines Beispiels näher beschrieben werden, ohne sie auf dieses Beispiel zu begrenzen.The Invention will be described in more detail by way of example without limiting it to this example.
Ausführungsbeispielembodiment
Mittels
Luftstrahlmühle trocken aufbereiteter oder durch Nassaufbereitung
mit anschließender Trocknung und Klassierung gewonnener
Halloysit wird als Ausgangsstoff für die Plasmabehandlung eingesetzt.
Das Nanomineralpulver wird in einem Niederdruck-Plasmareaktor in
einem vibrierenden Substrathalter mit einer kohlenstoffhaltigen
Schicht beschichtet.
Bedingungen: Pulvermenge 0,5 kg, Druck
p = 0,1 mbar, Plasmaleistung P = 100 W, Mikrowellenanregung f =
2,45 GHz, Gaszusammensetzung Ar:CH4 = 1:1,
Behandlungszeit 1 h.Halloysite dry-processed or obtained by wet treatment with subsequent drying and classification by means of an air jet mill is used as starting material for the plasma treatment. The nanomineral powder is coated with a carbon-containing layer in a low-pressure plasma reactor in a vibrating substrate holder.
Conditions: Powder quantity 0.5 kg, pressure p = 0.1 mbar, plasma power P = 100 W, microwave excitation f = 2.45 GHz, gas composition Ar: CH 4 = 1: 1, treatment time 1 h.
Das behandelte Material wird nun durch ein weiteres Plasmaverfahren funktionalisiert, d. h. es werden stickstoffhaltige funktionelle Gruppen auf der Oberfläche abgeschieden. Bedingungen: Pulvermenge 0,5 kg, Druck p = 1 mbar, Plasmaleistung P = 50 W, Mikrowellenanregung f = 2,45 GHz. Prozessgas NH3, Behandlungszeit 1 h.The treated material is now functionalized by another plasma process, ie, nitrogen-containing functional groups are deposited on the surface. Conditions: Powder quantity 0.5 kg, pressure p = 1 mbar, plasma power P = 50 W, microwave excitation f = 2.45 GHz. Process gas NH 3 , treatment time 1 h.
Anschließend
werden das beschichtete und funktionalisierte Material mit einer
Werkstofflösung imprägniert. Wie aus elektronenoptischen
Untersuchungen belegbar ist, bleibt im Ergebnis der Plasmabehandlung
der Nanoröhrchenhohlraum erhalten (
ZITATE ENTHALTEN IN DER BESCHREIBUNGQUOTES INCLUDE IN THE DESCRIPTION
Diese Liste der vom Anmelder aufgeführten Dokumente wurde automatisiert erzeugt und ist ausschließlich zur besseren Information des Lesers aufgenommen. Die Liste ist nicht Bestandteil der deutschen Patent- bzw. Gebrauchsmusteranmeldung. Das DPMA übernimmt keinerlei Haftung für etwaige Fehler oder Auslassungen.This list The documents listed by the applicant have been automated generated and is solely for better information recorded by the reader. The list is not part of the German Patent or utility model application. The DPMA takes over no liability for any errors or omissions.
Zitierte PatentliteraturCited patent literature
- - DE 60114538 T2 [0002] - DE 60114538 T2 [0002]
- - EP 1195775 A1 [0002] EP 1195775 A1 [0002]
- - EP 0813955 A2 [0002] - EP 0813955 A2 [0002]
- - EP 1426422 A1 [0002] - EP 1426422 A1 [0002]
- - JP 2006089534 A [0002] - JP 2006089534 A [0002]
- - KR 1020030021620 A [0002] - KR 1020030021620 A [0002]
- - US 20040097630 A1 [0002] US 20040097630 A1 [0002]
- - WO 2000034180 A [0002] - WO 2000034180 A [0002]
- - WO 2000034378 A1 [0002] - WO 2000034378 A1 [0002]
- - WO 2000034380 A1 [0002] - WO 2000034380 A1 [0002]
- - WO 2002024750 A2 [0002] - WO 2002024750 A2 [0002]
- - WO 2000024760 A1 [0002] - WO 2000024760 A1 [0002]
- - WO 9801346 A2 [0002] WO 9801346 A2 [0002]
- - WO 2004098254 A1 [0002] - WO 2004098254 A1 [0002]
- - WO 2004099836 A1 [0002] - WO 2004099836 A1 [0002]
- - WO 2001066653 A1 [0002] - WO 2001066653 A1 [0002]
- - US 20050019510 A1 [0002] US 20050019510 A1 [0002]
- - WO 2001096511 A2 [0002] - WO 2001096511 A2 [0002]
Claims (15)
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE200710022457 DE102007022457A1 (en) | 2007-05-09 | 2007-05-09 | Plasma-modified natural minerals with nanoscale properties, process for their preparation and their use |
PCT/EP2008/055744 WO2008138883A1 (en) | 2007-05-09 | 2008-05-09 | Plasma-modified natural minerals with nanoscale properties, method for the production and use thereof |
EP08750230A EP2150229A1 (en) | 2007-05-09 | 2008-05-09 | Plasma-modified natural minerals with nanoscale properties, method for the production and use thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE200710022457 DE102007022457A1 (en) | 2007-05-09 | 2007-05-09 | Plasma-modified natural minerals with nanoscale properties, process for their preparation and their use |
Publications (1)
Publication Number | Publication Date |
---|---|
DE102007022457A1 true DE102007022457A1 (en) | 2008-11-13 |
Family
ID=39615761
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE200710022457 Withdrawn DE102007022457A1 (en) | 2007-05-09 | 2007-05-09 | Plasma-modified natural minerals with nanoscale properties, process for their preparation and their use |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP2150229A1 (en) |
DE (1) | DE102007022457A1 (en) |
WO (1) | WO2008138883A1 (en) |
Citations (17)
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EP0813955A2 (en) | 1996-06-20 | 1997-12-29 | Oji-Yuka Synthetic Paper Co., Ltd. | Laminate with excellent printability |
WO1998001346A2 (en) | 1996-07-09 | 1998-01-15 | Tetra Laval Holdings & Finance S.A. | Nanocomposite polymer container |
WO2000024760A1 (en) | 1998-10-26 | 2000-05-04 | Ventana Medical Systems, Inc. | DETECTION OF HUMAN PAPILLOMA VIRUS IN PAPANICOLAOU (Pap) SMEARS |
WO2000034180A1 (en) | 1998-12-07 | 2000-06-15 | Eastman Chemical Company | A polymer/clay nanocomposite having improved gas barrier comprising a clay material with a mixture of two or more organic cations and a process for preparing same |
WO2000034380A1 (en) | 1998-12-07 | 2000-06-15 | Eastman Chemical Company | A polymer/clay nanocomposite having improved gas barrier comprising a clay material with a mixture of two or more organic cations and a process for preparing same |
WO2000034378A1 (en) | 1998-12-07 | 2000-06-15 | Eastman Chemical Company | Polymer/clay nanocomposite and process for making same |
WO2001066653A1 (en) | 2000-03-03 | 2001-09-13 | Dow Corning Corporation | Barrier coatings having bis-silanes |
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-
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- 2007-05-09 DE DE200710022457 patent/DE102007022457A1/en not_active Withdrawn
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- 2008-05-09 WO PCT/EP2008/055744 patent/WO2008138883A1/en active Application Filing
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EP0813955A2 (en) | 1996-06-20 | 1997-12-29 | Oji-Yuka Synthetic Paper Co., Ltd. | Laminate with excellent printability |
WO1998001346A2 (en) | 1996-07-09 | 1998-01-15 | Tetra Laval Holdings & Finance S.A. | Nanocomposite polymer container |
WO2000024760A1 (en) | 1998-10-26 | 2000-05-04 | Ventana Medical Systems, Inc. | DETECTION OF HUMAN PAPILLOMA VIRUS IN PAPANICOLAOU (Pap) SMEARS |
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WO2000034380A1 (en) | 1998-12-07 | 2000-06-15 | Eastman Chemical Company | A polymer/clay nanocomposite having improved gas barrier comprising a clay material with a mixture of two or more organic cations and a process for preparing same |
WO2000034378A1 (en) | 1998-12-07 | 2000-06-15 | Eastman Chemical Company | Polymer/clay nanocomposite and process for making same |
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EP1426422A1 (en) | 2002-12-06 | 2004-06-09 | Eastman Kodak Company | Aqueous pigmented ink formulation containing polymer-encapsulated pigments binder and smectite clay particles |
WO2004098254A1 (en) | 2003-04-28 | 2004-11-11 | Eastman Kodak Company | Article comprising conductive conduit channels |
WO2004099836A1 (en) | 2003-04-28 | 2004-11-18 | Eastman Kodak Company | Conductive patterned sheet utilizing multilayered conductive channels |
US20050019510A1 (en) | 2003-07-23 | 2005-01-27 | Gibson Lawrence E. | Fluid ejection cartridge utilizing a two-part epoxy adhesive |
JP2006089534A (en) | 2004-09-21 | 2006-04-06 | Fuji Electric Holdings Co Ltd | Flame-retardant resin processed product |
Also Published As
Publication number | Publication date |
---|---|
EP2150229A1 (en) | 2010-02-10 |
WO2008138883A1 (en) | 2008-11-20 |
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