EP1831104A1 - Procede de production de particules contenant du metal - Google Patents

Procede de production de particules contenant du metal

Info

Publication number
EP1831104A1
EP1831104A1 EP04788722A EP04788722A EP1831104A1 EP 1831104 A1 EP1831104 A1 EP 1831104A1 EP 04788722 A EP04788722 A EP 04788722A EP 04788722 A EP04788722 A EP 04788722A EP 1831104 A1 EP1831104 A1 EP 1831104A1
Authority
EP
European Patent Office
Prior art keywords
metal
silver
particles
containing particles
solution
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Withdrawn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
EP04788722A
Other languages
German (de)
English (en)
Inventor
Satish N. Chandra
William F. Mcnally
Vinesh Naik
Joel M. Furey
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.)
Noble Fiber Technologies LLC
Original Assignee
Noble Fiber Technologies LLC
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 Noble Fiber Technologies LLC filed Critical Noble Fiber Technologies LLC
Priority claimed from PCT/US2004/029891 external-priority patent/WO2006031229A1/fr
Publication of EP1831104A1 publication Critical patent/EP1831104A1/fr
Withdrawn legal-status Critical Current

Links

Definitions

  • This invention is directed generally to particles, and more particularly to methods of making micro-particles and/or nano-particles.
  • Silver-containing inorganic microbiocides have recently been developed and utilized as antimicrobial agents on and within a plethora of different substrates and surfaces.
  • microbiocides have been adapted ⁇ for incorporation within melt spun synthetic fibers, as taught within Japanese unexamined Patent Application No. Hl 1-124729, to provide certain fabrics which selectively and inherently exhibit antimicrobial characteristics.
  • attempts have been made to apply such specific microbiocides on the surfaces of fabrics and yarns with little success from a
  • the present invention provides a method of producing metal-containing particles.
  • the metal-containing particles are micro-sized and/or nano-sized particles.
  • the metal is complexed with an alkali agent to form the particles.
  • the metal is silver and the particles include silver hydroxide.
  • the particles have anti ⁇ microbial properties.
  • the particles may also provide anti-fungal properties, anti-static properties, and/or conductive properties.
  • the particles may range in size from about 0.01 to about 300 ⁇ m.
  • the present invention provides a method of preparing metal-based particles, hi one aspect, the method is used to form micro-sized and/or nano-sized
  • ⁇ WP195340.2 ⁇ 3 particles that include a metal.
  • the metal is silver.
  • These micro-sized and/or nano-sized particles have utility in a wide variety of different applications due to their size. Additionally, these particles retain the anti-microbial, anti-fungal, anti-static, and/or conductive properties of the metal used. As a result, micro-sized and/or nano- sized particles including silver offer one or more properties such as anti-microbial, anti ⁇ static and/or conductive.
  • the present invention provides a method of making micro-sized and/or nano-sized metal-containing particles.
  • the metal is silver.
  • the metal may be copper, aluminum, zinc, nickel, or the like.
  • the method makes micro-sized and/or nano-sized particles that contain a metal, such as silver.
  • micro-sized particles are particles that have a diameter of from about 1 to about 300 ⁇ m.
  • nano-sized particles are particles that have a diameter of from about 0.01 to about 1 ⁇ m.
  • the method may be used to form micro-size particles only, nano-sized particles only, or a combination thereof, with the resulting mixture either being used as a mixture, or further including a separation step to sort the particles into different size ranges.
  • a separation step is -a screening step to separate the particles into different sizes.
  • the methods of the present invention form these metal-containing particles using a series of process steps, although not all process steps are necessary for each embodiment.
  • the first step is to take a source of the metal, such as silver nitrate powder for embodiments wherein silver particles are to be formed, and dissolve it in water.
  • the water is de-ionized water.
  • a pre- dissolved silver nitrate solution may be used provided the amount of water in the solution is known.
  • the above mentioned solution may then treated with an alkali solution.
  • the alkali solution is sodium hydroxide.
  • Sodium hydroxide may be used due to its great tendency to complex with the metallic solution.
  • any alkali solution that is able to complex with the metallic solution used in a particular embodiment may be used in the present invention.
  • the metallic solution is silver nitrate dissolved in DI water.
  • Other alkali solutions that may be used include, but are not limited to, ammonium hydroxide.
  • the reaction may take place at room temperature, or at a temperature of from about 15 to about 30° C.
  • the alkali solution complexes with the metal to form a precipitate containing the metal.
  • brown precipitate is formed as the sodium hydroxide is added.
  • the solution may be stirred while the precipitate is forming.
  • the resultant mixture may be allowed to settle down for a period of time to permit settling of any precipitate. The amount of time permitted for settling may vary, but may be from about 5 to about 15 minutes.
  • the precipitate is then removed.
  • the precipitate may be filtered using standard filter paper, such as a Buckner funnel.
  • the solution may be neutralized.
  • an acid may be used to bring the solution to a pH of approximately 7.
  • sulfuric acid may be used, although other acids may also be used including, but not limited to, hydrochloric acid and nitric acid, among others. Bringing the pH of the solution to about 7 is beneficial in that it will facilitate easy processing from waste treatment point of view, although this step is not necessary in the formation of the micro-sized and nano-sized particles of the present invention.
  • the precipitate is then rinsed with water, such as deionized water.
  • water such as deionized water.
  • the ' water is, beneficially ⁇ used to wash the precipitate thoroughly. Washing of the precipitate helps facilitate nano- and micro-sized particles of the complexed metal precipitate to be collected in pure form.
  • the resulting precipitate includes nano- and micro-sized particles of silver hydroxide. The rinsing may be done anywhere, including within the funnel itself.
  • the precipitate may then be dried in a conventional oven or other drying mechanism until the precipitate is substantially dry.
  • the drying temperature is from about 50 to about 90° C.
  • the resulting product includes the micro-sized and/or nano-sized particles of the present invention.
  • the micro-sized and/or nano-sized particles of the present invention include silver, the beneficial properties of silver are retained, even with the smaller size of the particles.
  • the particles of the present invention may be used in any application taking advantage of one or more of the beneficial properties of silver. These properties include, but are not limited to, anti ⁇ microbial, anti-fungal, anti-static, conductive, electromagnetic interference (EMI) shielding, filtration, or a combination thereof.
  • EMI electromagnetic interference
  • the solution was neutralized using 50% sulfuric acid.
  • the precipitate was then rinsed with deionized water using 50 - 100 ml at a time through the buckner funnel.
  • Example 1 The resultant nano powder obtained from Example 1 was then subjected to high heat (i.e. greater than about >100° C) for a few minutes. This heating resulted in the formation of shiny white micro- and nano-sized particles of silver. The resultant powder weighed approximately 43 gm.
  • Example 1 The resultant powder from Example 1 was then incorporated into the outer surface of a hydrogel bandage at the ratio of 10: 1 by weight of the hydrogel to the weight of the silver powder. The surface was dipped to apply the hydrogel mixture to the surface. This sample was then subjected to Dow Corning Corporate Test Method 0923 using Staphylococcus aureus ATCC 6538. After 1 hour the organism count CFU/ml reduced from 1.6 x 10 5 at zero time to ⁇ 10. The percentage reduction was >99.99%. As
  • Example 1 The resultant powder from Example 1 was then incorporated into the outer surface of a hydrogel bandage at the ratio of 10:1 by weight of the hydrogel to the weight of the silver powder and then subjected to the same test as Example 3 over a period of 4 hours.. The reduction was again 99.99%. This clearly suggests the enormous surface area of the nano particles and its effectiveness in small quantities.
  • Example 1 The resultant powder from Example 1 was then incorporated into the outer surface of a hydrogel bandage at the ratio of 100:1 by weight of the hydrogel to the weight of the silver powder and then subjected to the same test as Example 3 over a period of 4 hours.
  • the reduction was an amazing 94%, again indicating the effectiveness of the nano particles as well as the surface area benefits.
  • the test result also indicates a great zone of inhibition of the nano particles.

Landscapes

  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

L'invention concerne un procédé de production de particules contenant du métal. Les particules contenant du métal sont micronisées et/ou nanonisées. Selon le métal utilisé, ces particules peuvent posséder des propriétés antimicrobiennes. Dans les modes de réalisation où l'argent est utilisé, ces particules peuvent conférer les propriétés antifongiques, les propriétés antistatiques, un blindage antiparasites électromagnétiques, et/ou les propriétés conductrices dudit métal. La taille des particules peut varier entre environ 0,01 et environ 300 µm.
EP04788722A 2003-09-09 2004-09-09 Procede de production de particules contenant du metal Withdrawn EP1831104A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US50108403P 2003-09-09 2003-09-09
PCT/US2004/029891 WO2006031229A1 (fr) 2004-09-10 2004-09-10 Procede de production de particules contenant du metal

Publications (1)

Publication Number Publication Date
EP1831104A1 true EP1831104A1 (fr) 2007-09-12

Family

ID=38370507

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04788722A Withdrawn EP1831104A1 (fr) 2003-09-09 2004-09-09 Procede de production de particules contenant du metal

Country Status (1)

Country Link
EP (1) EP1831104A1 (fr)

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2006031229A1 *

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