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WO2005085339A1 - Procede de preparation d'un composite a base de polymeres et nanoparticules d'argent - Google Patents

Procede de preparation d'un composite a base de polymeres et nanoparticules d'argent Download PDF

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Publication number
WO2005085339A1
WO2005085339A1 PCT/KR2005/000576 KR2005000576W WO2005085339A1 WO 2005085339 A1 WO2005085339 A1 WO 2005085339A1 KR 2005000576 W KR2005000576 W KR 2005000576W WO 2005085339 A1 WO2005085339 A1 WO 2005085339A1
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WO
WIPO (PCT)
Prior art keywords
polymer
silver
silver nanoparticles
nanoparticles
composite
Prior art date
Application number
PCT/KR2005/000576
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English (en)
Inventor
Gil-Bae Choi
Jeong-Hun Lee
Original Assignee
Gil-Bae Choi
Jeong-Hun Lee
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 Gil-Bae Choi, Jeong-Hun Lee filed Critical Gil-Bae Choi
Publication of WO2005085339A1 publication Critical patent/WO2005085339A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04G—SCAFFOLDING; FORMS; SHUTTERING; BUILDING IMPLEMENTS OR AIDS, OR THEIR USE; HANDLING BUILDING MATERIALS ON THE SITE; REPAIRING, BREAKING-UP OR OTHER WORK ON EXISTING BUILDINGS
    • E04G17/00—Connecting or other auxiliary members for forms, falsework structures, or shutterings
    • E04G17/004—Strips for creating a chamfered edge
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04G—SCAFFOLDING; FORMS; SHUTTERING; BUILDING IMPLEMENTS OR AIDS, OR THEIR USE; HANDLING BUILDING MATERIALS ON THE SITE; REPAIRING, BREAKING-UP OR OTHER WORK ON EXISTING BUILDINGS
    • E04G9/00—Forming or shuttering elements for general use
    • E04G9/10—Forming or shuttering elements for general use with additional peculiarities such as surface shaping, insulating or heating, permeability to water or air
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04G—SCAFFOLDING; FORMS; SHUTTERING; BUILDING IMPLEMENTS OR AIDS, OR THEIR USE; HANDLING BUILDING MATERIALS ON THE SITE; REPAIRING, BREAKING-UP OR OTHER WORK ON EXISTING BUILDINGS
    • E04G17/00—Connecting or other auxiliary members for forms, falsework structures, or shutterings
    • E04G2017/008—Pin and hole connection type

Definitions

  • the present invention relates to a method for the preparation of silver nanoparticle-polymer composite. More particularly, the present invention relates to a method for the preparation of a silver nanoparticle-polymer composite by dispersing silver nanoparticle in a polymer without coagulation and a., silver nanoparticle-polymer composite prepared thereby.
  • nanoparticles can give much more physical and chemical effects than bulk material even when used in much less amount than the bulk material, as well as they may show properties significantly different from the bulk material.
  • nanoparticles since nanoparticles are used in an extremely small amount, they shows the equivalent or better effect than micro-particles or bulk material, nanoparticles can be used in an extremely small amount, and thus they shows less toxicity to the human body and the environment. As a result, nanoparticles are considered as being stable to the environment and benefit to human body and the environmental and many studies have been made on nanoparticles.
  • nanoparticles are incorporated in a polymer to prepare composites such as synthetic fiber, plastic molding article, film, paint, ink, etc.
  • a polymer to prepare composites such as synthetic fiber, plastic molding article, film, paint, ink, etc.
  • Silver nanoparticles which have been made into nano-sized particulate are expected to have more excellent properties than bulk silver and there have been made many studies on nanotechnology about methods of preparing silver nanoparticles in the form of powder or solution. Further, several studies using thus prepared silver nanoparticles have reported that silver nanoparticles show extremely improved antibacterial, germicidal, antifungal effects with relative to bulk silver, for example, more than 99 % of germicidal effect even within several seconds against many bacteria. Many documents have proposed to incorporate silver nanoparticles into a polymer to prepare antibacterial articles such as fibers (for example, see Korean Patent Laid-open publication Nos. 2003-0055197 and 2003-0091574), films (for example, see Korean Patent Laid-open publication No.
  • nanoparticles prepared in the form of colloid solution When silver nanoparticles prepared in the form of colloid solution are dried for use, the nanoparticles coagulate and grow to a micro-particles, and it is difficult to divide thus resulted micro-particles into nanoparticles to uniformly incorporate in a polymer. Further, when silver nanoparticles prepared in the form of powder are employed, the nanoparticles have a low compatibility with the polymer and thus coagulate with each other to grow to particles having a micro size. Such coarsening or coagulation of nanoparticles will essentially reduce the excellent effects of nanosized particles, deteriorate the properties of the polymer, and particularly, make it impossible to prepare the composite in the form of fiber or film.
  • Figure 1 is a photograph (magnification lOOO) showing the distribution of silver nanoparticles on a sectioned surface of a silver nanoparticle-polymer composite prepared according the present invention.
  • Figure 2 is a photograph (magnification x2000) showing the distribution of silver nanoparticles on a sectioned surface of a silver nanoparticle-polymer composite prepared according the present invention.
  • the object of the present invention is to provide a method for the preparation of silver nanoparticles-polymer composite comprising: (1) introducing a silver nanoparticle colloid solution to a polymer preheated to a
  • Another object of the present invention is to provide a silver nanoparticle-polymer composite prepared by the above method, in which silver nanoparticles are uniformly dispersed.
  • the still another object of the present invention is to provide a use of a silver nanoparticle-polymer composite thus prepared according to the above method as a master batch or a functional chip.
  • the silver nanoparticle colloid solution means a water solution in which silver particles having a nanometer size exist as a colloid.
  • the silver nanoparticle colloid solution which can be used in the present invention may be prepared according to documents [See, for example, Nature 1985, 317, 344; Material Letters 1993, 17, 314; Korean Patent Laid-open Publication No. 2003-0082065] or any nanoparticles sold in a market may be employed.
  • the silver nanoparticles of the present invention can generally have a mean diameter
  • nm nanometers
  • m microns
  • the silver nanoparticle colloid solution can contain silver nanoparticles in a concentration of more than 10,000 ppm, preferably more than 20,000 ppm, more preferably more than 30,000 ppm, particularly more than 50,000 ppm. If the content of silver nanoparticles is too low, for example not more than 5,000 ppm, the removal of water is difficult and expensive. Although there is no upper limit of the concentration of silver nanoparticles in a colloid solution, it may have a concentration of not more than 500,000 ppm, preferably not more than 300,000 ppm, more preferably not more than 200,000 ppm in the view of economy and process efficiency.
  • Polymers which can be used in the present invention are not particularly restricted and may include, for examples: - Polyethylenes, for example, low density polyethylene (LDPE), very low density polyethylene (VLDPE), linear low density polyethylene (LLDPE), high density polyethylene (HDPE), ethylene-vinyl acetate (EVA), their copolymers; - Polypropylenes, for example, homo polypropylene, random polypropylene, their copolymers; - Polystyrene, for example, HIPS (High Impact Polystyrene), GPPS (General Purpose Polystyrene), SAN (Poly(Styrene Acrylonitrile)), etc.; - Transparent or general ABS (acrylonitrile-butadiene-styrene terpolymer), - Hard PVC, - Engineering plastics, for example, nylon, PBT (Polybutylene terephthalate), PET
  • LDPE low density polyethylene
  • VLDPE very low density polyethylene
  • the preheating temperature of polymer in a first step of the present invention the preheating temperature of polymer in a first step of the present invention
  • mixer is 45 - 85 ° C , preferably 50 - 80 °C, more preferably 55 - 70 °C . If the preheating
  • the preheating of polymers can be earned out for 10 min - 150 min, preferably 20 min - 100 min, more preferably 30 min - 70 min under rotation.
  • the rotation speed is not particularly restricted, but may be generally not more than 1000 rpm, preferably 10 - 700 rpm, more preferably 20 - 500 rpm. It is thought that such rotation will generate static electricity on the surface of polymer, which attracts and adsorbs silver nanoparticles in a static electricity manner on the surface of polymer to prevent the coagulation of silver nanoparticles.
  • the present invention is not limited to the above range.
  • the water evaporating speed and the amount of water to be removed is not strictly limited if silver nanoparticles can uniformly adsorbed on the surface of polymer without coagulation. It is possible to remove more than 80%, preferably more than 90 %, more preferably more than 95% of water present in the mixture of the polymer and the colloid solution before transferring the polymer on which silver nanoparticles are adsorbed to an extrude.
  • the second step of the present invention constitutes an important characteristics and advantage of the process of the present invention. Polymers have an inherent property that, if they are heated, they attract surrounding particles.
  • the second step utilizes such inherent property of polymers to uniformly disperse silver nanoparticles in a polymer without using any dispersant or compatibilizer.
  • the other reason that the present invention would not employs any dispersant or compatibilizer which may help the uniform dispersion of silver nanoparticles is that such dispersant or compatibilizer may deteriorate the properties of polymer or may offset the effect of nano-sized particles.
  • many experiments have been performed by controlling the temperature and rotation speed of polymers in a mixer or extruder. In one experiment, a polymer (LDPE5321) had been treated at a condition of 200
  • the colloid solution had been added.
  • the colloid solution had mixed with the polymer but had not uniformly dispersed in the polymer.
  • silver nanoparticles did not uniformly disperse in the polymer due to phase separation.
  • the suitable ranges of process conditions enabling silver nanoparticles to uniformly disperse in polymers had been determined via many experiments carried out under many combinations of temperature and rotation speed (rpm) of polymer in a mixer.
  • the second step of the present invention it is assumed that the coagulation of silver nanoparticles can be prevented since silver nanoparticles are fixed on the surface of polymers by adsorption and/or sealing.
  • polymers on which silver nanoparticles are adsorbed are transferred into an extruder and then kneaded and extruded.
  • a silver nanoparticle-polymer composite in which silver nanoparticles are uniformly dispersed without coagulation can be obtained.
  • the kneading and extrusion can be made under common conditions known in the pertinent field.
  • the silver nanoparticles-adsorbed polymer obtained at the above second step is directly introduced to an extruder.
  • the temperature of the input portion of an extruder is adjusted to a temperature similar to the above process temperature of the second step.
  • the temperatures of barrel and dies of the extruder are not strictly limited and can be suitable determined by a skilled person in this field according to the type of polymer used. For example, if polymer is polypropylene, the temperatures of the extruder are adjusted to
  • extruder are adjusted to 220 - 260 ° C ( ⁇ 5 ° C ) at cylinder barrel portion and to 220 -
  • mixer or extruder is not strictly limited in the present invention, a mixer and/or extruder sold in the market may be employed.
  • the silver nanoparticle-polymer composite prepared according to the method of the present invention may be used as a master batch or functional chip for the preparation of a molding article, film, sheet, fiber or the like.
  • the silver nanoparticles are uniformly dispersed without coagulation in the silver nanoparticle-polymer composite prepared according to the method of the present invention. Therefore, when the composite is formed in a thin film or microfiber with less than 1 denier, the silver nanoparticles do not deteriorate or lower the physical properties of the resulted articles.
  • the silver nanoparticle-polymer composite prepared according to the method of the present invention has advantages that the uniform dispersion state of the nanoparticles can be maintained without coagulation of the particles for a long time or nearly permanently, that a good or excellent antibacterial effect can be achieved even with relatively small amount of silver due to maximized antibacterial effect of silver nanoparticles, that the friction fastness is permanent because the nanoparticles are incorporated within the polymer matrix, that the one-step process can lower the cost, that very thin or fine articles such as fiber or film can be prepared, and that, when a fiber is formed, it is possible to make a mixed textile with natural fibers with little or no deterioration of their properties.
  • the silver nanoparticle-polymer composite according to the method of the present invention is stable to the human body and the environment since silver nanoparticles are sealed on the surface or inside the polymer to minimize the loss or scattering of the silver nanoparticles into the environment.
  • Example 1 Preparation of silver nanoparticle-LDPE composite 1) To a super mixer (Model: Super Mixer 300L AC 75HP 4P; made by
  • Figures 1 and 2 are the photographs (Magnification of 1000 times and 2000 times, respectively) showing the distribution of silver nanoparticles on the surface of silver nanoparticle-polymer composite thus prepared.
  • Comparative Example 1 The same procedure was repeated as in Example 1 except that the polymer was treated with a colloid solution in a room temperature without preheating of the polymer.
  • the silver nanoparticle colloid solution was introduced at an interval after introducing the polymer.
  • the silver nanoparticle colloid solution could be blended with the polymer.
  • Comparative Example 2 The same procedure was repeated as in Example 1 except that a dispersant was incorporated and the polymer was treated with a colloid solution in a room temperature without preheating of the polymer.
  • a dispersant a wax (trade name : X861; sold by Bayer), which is usually employed as an additive (dispersant) in the preparation of a color master batch (color M/B), was employed to prevent the nanoparticles from coagulating and from not uniformly dispersing.
  • a wax trade name : X861; sold by Bayer
  • color M/B color master batch
  • polypropylene (PP) (Trade name : PPJ700; made by HYOSUNG Corp., Korea) was introduced and then rotated for about 40 minutes in a high speed (about 100 rpm), during
  • Example 3 Preparation of silver nanoparticle-PET composite The same procedure was repeated as in Example 1 except that polyethylene terephthalate (PET) (Trade name: K177Y; made by KOLON Ind. Inc., Korea) was PET (Trade name: K177Y; made by KOLON Ind. Inc., Korea) was PET (Trade name: K177Y; made by KOLON Ind. Inc., Korea) was PET (Trade name: K177Y; made by KOLON Ind. Inc., Korea) was
  • a silver nanoparticle-PET composite in which silver nanoparticles were uniformly dispersed in the PET polymer without coagulation was obtained in the form of pellet.
  • Example 4 Preparation of silver nanoparticle-Nylon composite The same procedure was repeated as in Example 1 except that nylon (Nylon 6 or 66; made by KOLON Ind. Inc., Korea) was employed and preheated to 60 - 70 °C.
  • nylon Nylon 6 or 66; made by KOLON Ind. Inc., Korea
  • a silver nanoparticle-Nylon composite in which silver nanoparticles were uniformly dispersed in Nylon polymer without coagulation was obtained in the form of pellet.
  • Example 5 Preparation of silver nanoparticle-PC composite The same procedure was repeated as in Example 1 except that polycarbonate (PC)
  • the extruder had maintained the temperatures of 70 °C ( ⁇ 5 ° C) at the input
  • a silver nanoparticle-PC composite in which silver nanoparticles were uniformly dispersed in PC polymer without coagulation was obtained in the form of pellet.
  • Example 6 Preparation of silver nanoparticle- ABS composite The same procedure was repeated as in Example 1 except that acrylonitrile-butadien-styren (ABS) terpolymer (Trade name: ABS380; sold by KUMHO
  • Example 7 Preparation of a nonwoven fabric by using a melt blown method
  • nanoparticle-polypropylene composite having a concentration of 2000 ppm/kg prepared in
  • the resulted fiber had a silver concentration of 80 - 100 ppm/kg.
  • thermosetting Before the fiber was hardened, it is subjected to thermosetting to prepare a nonwoven fabric, which has uniform micro-spaces and can filter more than 99.9 % of fine particulate having a size of more than 0.3 micron.
  • a nonwoven fabric of microfiber level has uniform micro-spaces and can filter more than 99.9 % of fine particulate having a size of more than 0.3 micron.
  • the unwoven fabric was cut into a disc (diameter 4.8 cm), inoculated with test
  • the resulted disc is immersed and shaken in a predetermined amount buffer solution (pH 7.0 ⁇ 0.2) of phosphoric acid to extract the incubated bacteria.
  • the number of bacteria in the resulted solution was counted to determine the change of number.
  • the results obtained as a mean value from two tests are shown in the following
  • silver nanoparticle-polymer composite can be used as a master batch or a functional chip for extrusion, injection, spinning and then formed in various articles such as molding article, fiber, sheet, film, etc.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Architecture (AREA)
  • Structural Engineering (AREA)
  • Nanotechnology (AREA)
  • Mechanical Engineering (AREA)
  • Civil Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

L'invention vise un nouveau composite constitué de nanoparticules d'argent et d'un polymère, les nanoparticules d'argent étant incorporées au polymère de façon uniforme, sans coagulation, de manière à porter au maximum l'effet antibactérien de l'argent sans détériorer les propriétés et fonctions du polymère. Selon l'invention, un procédé de préparation du composite constitué de nanoparticules d'argent et d'un polymère consiste à introduire une solution colloïde de nanoparticules d'argent dans un polymère préchauffé, à faire pivoter le mélange ainsi obtenu à la même température pour en évacuer l'eau, à malaxer et à extruder le mélange ainsi obtenu dans une forme acceptable. Le composite constitué de nanoparticules d'argent et d'un polymère préparé selon ce procédé peut s'utiliser en tant que mélange monté ou cristal fonctionnel pour l'extrusion, l'injection ou le filage dans la fabrication d'un article moulé, d'un film, d'une feuille, d'une fibre ou similaire.
PCT/KR2005/000576 2004-03-10 2005-03-02 Procede de preparation d'un composite a base de polymeres et nanoparticules d'argent WO2005085339A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR10-2004-0016124 2004-03-10
KR1020040016124A KR100702848B1 (ko) 2004-03-10 2004-03-10 은나노입자 및 고분자수지의 복합재료의 제조방법

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US9504405B2 (en) 2013-10-23 2016-11-29 Verily Life Sciences Llc Spatial modulation of magnetic particles in vasculature by external magnetic field
WO2017006259A1 (fr) * 2015-07-06 2017-01-12 Universita' Degli Studi Di Roma "Tor Vergata" Procédé pour la production de matériaux plastiques nanocomposites
ITUB20152019A1 (it) * 2015-07-08 2017-01-16 Fabrizio Quadrini Metodo di fabbricazione di additivi per plastiche nanocomposite con proprieta' antimicrobiche e antibatteriche
US9861710B1 (en) 2015-01-16 2018-01-09 Verily Life Sciences Llc Composite particles, methods, and in vivo diagnostic system
IT201700001597A1 (it) * 2017-01-10 2018-07-10 Viganò Carlo Maria Stefano preparazione semplice ed economica di compositi di poliolefine antibatterici con nano particelle di argento puro
US10542918B2 (en) 2013-10-23 2020-01-28 Verily Life Sciences Llc Modulation of a response signal to distinguish between analyte and background signals
FR3085105A1 (fr) * 2018-08-22 2020-02-28 Commissariat A L'energie Atomique Et Aux Energies Alternatives Nouvel agent antimicrobien a base de materiau polymerique particulaire poreux dope
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KR100704316B1 (ko) 2006-05-29 2007-04-09 주식회사 동부한농 은나노 항균 수지 및 그 제조 방법
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KR102167281B1 (ko) 2020-03-12 2020-10-20 한국교통대학교산학협력단 Ｕｖ 경화용 항균성 및 상용성이 우수한 유／무기 하이브리드 수지 및 그 제조방법
KR102718336B1 (ko) * 2022-05-31 2024-10-17 한국광기술원 유연 패치형 항균/살균 필터를 제조하는 장치 및 방법

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KR20020074913A (ko) * 2001-03-22 2002-10-04 광주과학기술원 나노 입자와 고분자 물질을 이용한 나노 복합체 제조 방법
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KR20030038585A (ko) * 2003-03-28 2003-05-16 인교진 은 나노입자를 함유한 폴리우레탄 나노복합체의 합성

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WO2006069696A1 (fr) * 2004-12-24 2006-07-06 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Procede de production de polymeres contenant de fines particules
EP1991365B1 (fr) * 2006-02-08 2014-12-24 Kimberly-Clark Worldwide, Inc. Procedés de fabrication des surfaces traitées avec des nanoparticules d'argent
EP1991365A2 (fr) * 2006-02-08 2008-11-19 Acrymed, Inc. Procedes et compositions destines a des surfaces traitees avec des nanoparticules metalliques
US9096737B2 (en) 2007-12-17 2015-08-04 Inktec Co., Ltd. Method for preparing resin compositions containing nano silver particles
US8709601B2 (en) 2009-01-30 2014-04-29 Hewlett-Packard Development Company, L.P. Block copolymer nanoparticle compositions
US8785004B2 (en) 2009-01-30 2014-07-22 Hewlett-Packard Development Company, L.P. UV light-emissive fluorene-based copolymers
WO2010087842A1 (fr) * 2009-01-30 2010-08-05 Hewlett-Packard Development Company Polymère et compositions polymère-nanoparticule
US20140205642A1 (en) * 2010-10-14 2014-07-24 Zeus Industrial Products, Inc. Antimicrobial substrate
US11464429B2 (en) 2013-10-23 2022-10-11 Verily Life Sciences Llc Modulation of a response signal to distinguish between analyte and background signals
US9504405B2 (en) 2013-10-23 2016-11-29 Verily Life Sciences Llc Spatial modulation of magnetic particles in vasculature by external magnetic field
US10542918B2 (en) 2013-10-23 2020-01-28 Verily Life Sciences Llc Modulation of a response signal to distinguish between analyte and background signals
US9636034B2 (en) 2013-10-23 2017-05-02 Verily Life Sciences Llc Non-invasive analyte detection system with modulation source
US9861710B1 (en) 2015-01-16 2018-01-09 Verily Life Sciences Llc Composite particles, methods, and in vivo diagnostic system
WO2017006259A1 (fr) * 2015-07-06 2017-01-12 Universita' Degli Studi Di Roma "Tor Vergata" Procédé pour la production de matériaux plastiques nanocomposites
ITUB20152019A1 (it) * 2015-07-08 2017-01-16 Fabrizio Quadrini Metodo di fabbricazione di additivi per plastiche nanocomposite con proprieta' antimicrobiche e antibatteriche
US9491947B1 (en) 2015-09-28 2016-11-15 King Saud University Method of synthesizing nanoparticles and a nanoparticle-polymer composite using a plant extract
IT201700001597A1 (it) * 2017-01-10 2018-07-10 Viganò Carlo Maria Stefano preparazione semplice ed economica di compositi di poliolefine antibatterici con nano particelle di argento puro
WO2018131055A1 (fr) * 2017-01-10 2018-07-19 VIGANO' Carlo Maria Stefano Préparation simple et économique d'échantillons de polyoléfines antibactériennes avec des nanoparticules d'argent exposées à nu
FR3085105A1 (fr) * 2018-08-22 2020-02-28 Commissariat A L'energie Atomique Et Aux Energies Alternatives Nouvel agent antimicrobien a base de materiau polymerique particulaire poreux dope
US20240336747A1 (en) * 2022-05-02 2024-10-10 Sabic Global Technologies B.V. Metal-glycerol decorated antimicrobial polymer composite

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