method for transmitting antimicrobial activity to a composite structural solid material

专利摘要:
SOLID SURFACES AND ANTIMICROBIAL TREATMENTS AND PROCESSES TO PREPARE THE SAME It is a semi-flexible or rigid surface based on a non-isostatic antimicrobial polymer in a thermoset and / or thermoplastic resin matrix in which the active antimicrobial ingredient is copper oxide. Processes for preparing the same and applications of it are also described.
公开号:BR112015002704B1
申请号:R112015002704-0
申请日:2013-08-08
公开日:2021-03-02
发明作者:Vik Kamukula；Kenneth Gauthier Trinder Ii
申请人:Eos Surfaces Llc；Cupron, Inc；
IPC主号:

专利说明:

FIELD OF THE INVENTION
[001] The invention relates to solid polymeric panels and sheet possession and polymer resin treatments that grant antibacterial, antifungal, antiviral and sporicidal properties. BACKGROUND OF THE INVENTION
[002] Microbes (bacteria, fungi, viruses and spores) are a part of our everyday life and are located on virtually all hard surfaces. Since bacteria, fungi, viruses and spores can persist on most rigid surfaces, especially if there is even a small amount of moisture, for varying periods of time, these surfaces become a reservoir of infection and transmission to a host in contact with the surface can occur. Unless a surface is specifically treated with an antimicrobial agent, bacteria, fungi and viruses, especially if the surface is moist, have the possibility of establishing a presence on the hard surface. Such surfaces provide an entry into the host by pathogenic microorganisms, which can negatively impact morbidity and mortality.
[003] One way to eradicate or decrease contact with microbes present on solid surfaces is to incorporate an antimicrobial compound inside or on the solid surface. Copper ion-releasing compounds, such as copper oxide, are highly effective microcidal agents, which have been shown to be highly effective against bacteria, fungi and viruses [Gabbay, et al. (2002) The FASEB Journal express article 10.1096 / jf.04-2029fje. Published online on September 2, 2004].
[004] In most cases, the amount of metal oxides that can be incorporated into a polymer is limited (documentonoU.S. 2004/0247653) due to the interfering nature of metal oxides in the disruption of crosslinking and chemical agglutination mechanisms, necessary for the creation of polymeric panels of solid surface and sheet material. Since the antimicrobial activity is proportionally related to the loading of copper oxide, this limitation has impacted the practical development of antimicrobial rigid surface materials that contain copper oxide.
[005] Counters made of copper and its alloys are effective in controlling microbial load on a rigid counter surface as evidenced in "Sustained Reduction of Microbial Burden on Common Hospital Surfaces through Introduction of Copper" [Michael G Schmidt, Hubert H Attaway, Peter A Sharpe, Joseph John Jr, Kent A Sepkowitz, Andrew Morgan, Sarah E Fairey, Susan Singh, Lisa L Steed, J Robert Cantey, Katherine D Freeman, Harold T Michels and Cassandra D Salgado.J Clin- Microbiol July 2012 vol . 50 no 7, 2217 to 2223. Published before printing on May 2, 2012, doi: 10.1128 / JCM.01032-12].
[006] However, copper and its alloys are expensive and the practical aspect of their incorporation is both technically challenging and expensive. In addition, in many cases a rigid metal surface can often be unattractive due to oxidation staining as well as difficult to maintain aesthetically.
[007] The effect of ionic extermination mechanisms is well documented. Copper oxide has been shown to be an effective antimicrobial agent [Current Medicinal Chemistry, 2005, 12, 2163 to 2175 2163 0929-8673 / 05 2005 Bentham Science Publishers Ltd. "Copper as a Biocidal Tool" Gadi Borkow * and Jeffrey Gabbay].
[008] Although it was previously known that the incorporation of copper in composite structural solid materials provides antimicrobial activity to them and, in particular, although copper oxide was known to be an effective antimicrobial agent, composite structural solid materials have so far been limited wherein the loading of more than 10% w / w of particles containing copper in such materials was not achievable. SUMMARY OF THE INVENTION
[009] This invention provides composite structural solid materials with a high copper oxide load that are biocidal.
[010] The present invention, in some embodiments, provides high copper compound loads as well as a system for their incorporation to provide highly effective antimicrobial performance on a rigidly created surface, while maintaining an aesthetic appearance for the product and maintaining product strength with workability to manufacture products that benefit from biocidal properties. Since there is a direct relationship between microcidal efficacy and load levels but since high load levels can negatively affect the qualities of the product, surprisingly these contradictory findings have been overcome and a product and process are presented, which incorporate high loading levels. of copper particles, in a product that has structural integrity and an appropriately satisfactory appearance.
[011] In some embodiments, this invention provides a solid structural composite material characterized by the fact that it comprises a polymeric resin and copper oxide particles substantially uniformly dispersed therein which additionally optionally comprise a filler material, wherein said copper oxide is present in a concentration in the range of 10% to 50% w / w in which a portion of said copper oxide particles has the exposed surface.
[012] In some embodiments, this invention provides a finished product that comprises a composite structural solid material as described herein.
[013] In some embodiments, this invention provides a finished product comprising a structural liquid composite binder material described herein that can be incorporated into structural laminations, sprayed or painted on a surface and will harden to provide an antimicrobial surface.
[014] In some embodiments, this invention provides a batch mixing process for the manufacture of a composite structural solid material comprising a polymeric resin and copper oxide particles dispersed substantially uniformly in the same characterized by the fact that the process it comprises the steps of: ♦ mixing a polymeric resin, a filler and optionally a pigment; ♦ mixing a catalyst with a mixture of said polymeric resin, filler and optionally pigment; ♦ simultaneously mix copper oxide or a composition containing copper oxide with said catalyst for said mixture of said polymeric resin, filler and optionally said pigment or mix the copper oxide or a composition containing copper oxide in stages with said mixture of said polymeric resin, filler and optionally said pigment and said catalyst to form a polymerizable composite structural material; ♦ distribute the said polymeric composite structural material in a mold; and ♦ provide conditions for the polymerization of said structural material with polymeric composite, thus preparing a solid structural composite material.
[015] In some embodiments, this invention provides a continuous pouring process for the manufacture of a composite structural solid material comprising a polymeric resin and copper oxide particles dispersed substantially uniformly in the same characterized by the fact that the process comprises the steps of: ♦ mixing a polymeric resin or a filler with copper oxide until they are well mixed to form a paste of copper oxide and resin or a mixture of copper oxide and resin; ♦ in stages, subsequently mix said copper oxide and resin paste or mixture of copper oxide and resin with a filler or resin, respectively and optionally a pigment to form a mixed composition containing copper oxide; ♦ in stages, subsequently mixing a catalyst with said mixed composition containing copper oxide to form a polymerizable composite structural material; ♦ distribute the said polymeric composite structural material in a mold; and ♦ provide conditions for polymerization of said polymerizable composite structural material, thus preparing a solid composite structural material.
[016] In some embodiments, this invention provides a composite structural solid material prepared by a process as described in this document.
[017] In some embodiments, the invention provides a method for imparting antimicrobial activity to a composite structural solid material, characterized by the fact that said method comprises preparing a composite structural solid material containing copper oxide dispersed therein, in which the said copper oxide is present in a concentration in the range of 10 to 50% w / w in which a portion of said copper oxide particles has the exposed surface. BRIEF DESCRIPTION OF THE DRAWINGS
[018] Figure 1 shows a photograph of two embedded composite structural solid materials that contain copper oxide and a polyester and mix of acrylic resin and two different pigments.
[019] Figure 2 shows the biocidal activity of an embedded composite structural solid material of this invention. Figure 2 A demonstrates the antimicrobial activity of a composite composite structural solid material of this invention against gram-positive bacteria; activity of gram-negative bacteria and fungus. Figure 2B demonstrates the sporicidal activity of a composite composite structural solid material of this invention against C. difficile spores. Figure 2 C demonstrates the antibacterial activity of another composite composite structural solid material of this invention.
[020] Figure 3 shows a block diagram of an embedded process for producing an embedded composite structural solid material of this invention. According to the aspect described in that figure, a main batch containing polymeric resin, cuprous oxide, cupric oxide or a combination of them and pigments is prepared. The materials are mixed and extruded at a high temperature to produce main batch pellets, whose copper oxide concentration is verified. Polymeric resin pellets that contain copper oxide are then sized and classified before being added to the polymeric resin with catalyst and more organic and inorganic pigments. At this stage, copper oxide can be included as a powder or the main batch pellets or a combination of both for the polymeric resin and catalyst. These materials are optionally mixed under pressure in a vacuum and the mixture is then extruded and molded and melted on a rigid surface, before curing between 20 and 90 ° C. The rigid surface is then tested for composition and color before being finished and polished using a 40 to 220 grain wet sanding process and a solid polymeric panel was produced.
[021] Figures 4A, 4B, 4C and 4D represent a series of scanning electron micrographs, showing the substantially uniform distribution of copper particles throughout an embedded composite solid material of this invention. Figures 4A and 4B show representative images of a top surface of the solid composite material of this invention and Figures 4C and 4D show representative images of a bottom surface of a solid composite material of this invention. Figure 4E provides EDS results, which confirm that the particles seen in the micrographs are copper particles.
[022] Figure 5 is a block diagram depicting a built-in continuous pouring process of this invention. DETAILED DESCRIPTION OF THE INVENTION
[023] Surprisingly, as demonstrated in this document, a method by which a solid structural composite material is produced, such a method comprises: 1. Polymeric mixture of epigments; 2.Add catalyst; 3.Add loads to a main batch of PET that contains copper oxide; 4.or add copper powder; 5.or add as much as a main batch of PET that contains copper oxide as much as copper oxide powder; and 5.Fuse the resulting mixture into a mold
[024] The methods of this invention, which produce a solid composite structural material, are characterized by the fact that the material exhibits an improved copper oxide loading of over 10% w / w even higher, without compromising its structural integrity, for example. example, stiffness or uniformity or texture.
[025] As demonstrated in this document, according to some methods and composite materials incorporated in this invention, such materials or materials produced in this way, exhibited fast and effective microbiocidal activity, which will find application against a multiplicity of microbes, including bacteria and fungi , including spores and viruses. In fact, as demonstrated in this document, when a solid material prepared according to the Examples described in this document below was brought into contact with Gram-positive bacteria, Gram-negative bacteria and fungal species as shown in Figure 2, a reduction in 99.9% in microbial count was found within 2 hours and a 90% reduction in spore count was found within 24 hours.
[026] Thus, this invention provides a method and product for high loading of copper within a solid material. Accordingly, it is an object of this invention to provide composite structural solid materials with high loads of copper compound and copper oxide, as described herein.
[027] In some embodiments, this invention provides a composite structural solid material, characterized by the fact that it comprises a polymeric resin and copper oxide particles dispersed substantially uniformly in it, which additionally optionally comprise a filler material, in that said copper oxide is present in a concentration in the range of 10% to 50% w / w in which a portion of said copper oxide particles has the exposed surface.
[028] In some embodiments, this invention provides a solid structural composite material comprising a polymeric resin and a compound containing copper particle dispersed substantially uniformly therein which additionally optionally comprises a filler material, wherein said compound containing copper particle is present in a concentration in the range of 10% to 50% w / w in which a portion of said copper particles has the exposed surface.
[029] In some embodiments, such a compound containing a copper particle may include copper iodide, copper thiocyanate and, in some embodiments, such processes and materials produced may therefore make use of a main batch containing copper as described in this document. In some embodiments, the main batch is prepared / composed of materials as described in the PCT International Order Publication in WO 2006/100665, which is incorporated herein entirely by reference. In some embodiments, copper-containing compounds include copper salt, for example, copper chloride, copper fluoride, copper sulfate and others as will be verified by the skilled worker.
[030] In some embodiments, this invention provides a finished product that comprises a composite structural solid material as described herein.
[031] In some embodiments, this invention provides a finished product comprising a structural liquid composite binder material described herein that can be incorporated into structural laminations, sprayed or painted on a surface and will harden to provide an antimicrobial surface.
[032] In some embodiments, the composite structural solid material is an artificial or synthetic marble. In some embodiments, the terms "artificial or synthetic marble" refer to a material used in the construction of products, which can replace surfaces normally made of extracted, cut and polished marble stone. The term should be understood to include, among others, any solid surface for application in an environment where a rigid surface is desirable.
[033] In some embodiments, the composite structural solid materials of this invention, including artificial marbles as described in this document, comprise marble, onyx and other agglomerated stone and quartz cladding of solid surface materials, which are present as part of a matrix resin, which in some embodiments may additionally comprise a charge.
[034] In some embodiments, the use of cultured marble as envisioned in this document includes the use of an unloaded unsaturated polyester gel coating on a loaded unsaturated polyester substrate. The cargo, in some modalities, may comprise calcium carbonate or similar materials, as will be verified by the skilled worker.
[035] In some embodiments, the use of onyx as envisioned in this document includes the use of an unloaded unsaturated polyester gel coating on a loaded unsaturated polyester substrate. The filler, in some embodiments, may comprise alumina trihydrate.
[036] In some embodiments, the composite structural solid materials of this invention may comprise loaded resin material and, in some embodiments, unlike cultured marble or onyx, may not comprise a gel coating.
[037] In some embodiments, the composite structural solid materials of this invention may make use of a solid surface Corian® material (EI du Pont de Nemours and Company, Wilmington, Del.), Which comprises an acrylic matrix loaded with trihydrate of alumina, which is further modified as described herein to incorporate copper oxide particles dispersed substantially uniformly therein in a concentration in the range of> 10% to 50% w / w in which a portion of said oxide particles copper has the exposed surface.
[038] In some embodiments, the composite structural solid materials of this invention may make use of a quartz surface material such as Silestone, Ceasarstone, or Zodiaq® material, (EI du Pont de Nemours and Company, Wilmington, Del.) , which comprises unsaturated polyester matrix loaded with quartz or other similar charges, which is further modified as described in this document to incorporate copper oxide particles dispersed substantially uniformly therein in a concentration in the range of 10% to 50% in w / w in which a portion of said copper oxide particles has the surface exposed.
[039] The composite structural solid materials of this invention will, in some embodiments, comprise a polymeric resin.
[040] In some embodiments, the resin is made of a grout that comprises an acrylic group polymer dissolved in a material selected from the group of an acrylic group monomer solution and a mixed monomer solution that contains a vinyl monomer for copolymerization with an acrylic group monomer as a major component; the charge is alumina trihydrate; and the antimicrobial agent comprises copper oxide.
[041] In some embodiments, composite structural solid materials may be referred to herein as a synonym as a "resin matrix" or "matrix". The term "matrix" as used herein will be understood to include reference to a polymeric resin component in which fillers and other additives can be dispersed.
[042] In some embodiments, the polymeric resins of this invention by which glimpsed resin matrices will be composed include thermoplastic resins, thermoset resins and combinations thereof.
[043] In some embodiments, thermoplastic resins may comprise any thermoplastic resin known in the art and suitable for the intended application, for example, but without limitation such thermoplastic resins may include olefins (such as low and high density polyethylene and polypropylene), dienes (such as polybutadiene and Neoprene elastomer), vinyl polymers (such as polystyrene, acrylics and polyvinyl chloride), fluoropolymers (such as polytetrafluoroethylene) and heterogeneous polymers (such as polyamides, polyesters, polyurethanes, polyethers, polyacetates and polyacetates). Thermosetting resins include phenolic resins, amino resins, unsaturated polyester resins, epoxy resins, polyurethanes and silicone polymers. ABS, SAN, ASA.
[044] In some embodiments, epoxy resins may comprise any epoxy resin known in the art and suitable for the intended application, for example, but without limitation, such epoxy resins may include bisphenol type A, bisphenol type F, phenol type novolak, epoxy alicyclic, halogenated epoxy and cycloaliphatic epoxy resins.
[045] In some embodiments, polymeric resins may include unsaturated polyester resins, which in turn may include unsaturated polyester resins characterized in that their reactivity is based on the presence of double or triple bonds in carbon atoms. The acrylic component added to the polyester resin at a rate of approximately 5% by weight in the current blend that would also include polystyrene, methyl methacrylate (MMA), or poly (styrene) / MMA combinations.
[046] In some embodiments, polymeric resins can include any resin as described in this document for which an additive has been supplied, for example, an additive that contributes to the curing / crosslinking of monomeric resin units and catalysts can be incorporated to affect the same.
[047] In some embodiments, the invention contemplates the use of zero length catalysts, or in some embodiments, the catalyst is not zero length and should be considered part of the polymeric matrices of this invention.
[048] In some embodiments, polymeric resins may include acrylic resins, which in turn may comprise any known acrylic resin, with non-limiting examples that include various types of conventional acrylic group monomers, partial acrylic group polymers, vinyl monomers for copolymerization other than acrylic group monomers, or partial polymers. In some embodiments, such acrylic polymers may be (meth) acrylic esters. As used herein, "(meth) acrylic" is understood to mean "acrylic and / or methacrylic". Examples of (meth) acrylic esters include methyl (meth) acrylic esters, ethyl (meth) acrylic ester, benzyl (meth) acrylic ester, glycidyl (meth) acrylic ester.
[049] In some embodiments, acrylic resins may comprise a solid surface such as Corian®, which includes a poly (methyl methacrylate) resin (PMMA) with ATH charge, as described earlier in this document and in some embodiments, the polymeric resins of this invention may comprise a quartz surface such as Zodiaq® material, which comprises an unsaturated polyester resin (UPE) with a quartz or other silica filler. In some embodiments, the composite structural solid material comprising polymeric resins according to this aspect may additionally contain pigments, own material rectified in particulate form and other additives as disclosed in Patents No. 3,847,865 and 4,085,246, both of which are incorporated herein. as a reference.
[050] In some embodiments, the composite structural solid materials of this invention may additionally comprise a filler, which in turn may comprise any suitable filler material known as will be verified by the skilled worker. Unlimited examples of such filler material may include quartz, quartz powder, silica powder, stone powder, broken glass shards, calcium carbonate, talc, aluminum trihydrate and thixotropic agent additives such as smoked silica and organo-clay and others as will be verified by the skilled worker. In some embodiments, the amount of filler versus polymeric resin incorporated within the composite structural solid materials of this invention will be proportionally appropriate for the particular applications for the material that is produced, as will be verified by the skilled worker.
[051] In some embodiments, the polymeric resin comprises epoxy, acrylic or polyester resins and in some embodiments the polymeric resin comprises thermoplastic resins, thermoset resins or a combination thereof. In some embodiments, the composite structural solid material additionally comprises calcium carbonate, marble, granite, quartz, feldspar, marble and quartzite and mixtures thereof.
[052] In some embodiments, the composite structural solid material additionally comprises a filler material, as described in this document, such filler material comprises smoked silica, sand, clay, fly ash, cement, shards of ceramic, mica, flakes of silicate, broken glass, glass microspheres, glass spheres, mirror fragments, steel grit, aluminum grit, carbides, plastic microspheres, pelleted rubber, crushed polymer composites, wood chips, sawdust, paper laminates, pigments, dyes and mixtures thereof.
[053] In some modalities, the ATH load makes up between 10% and 30% by weight of the local composition.
[054] In some embodiments, ATH and / or quartz (silica) dust for the compaction method (very rigid material) makes up to 20 to 70%.
[055] In some modalities, the thickener (smoked silica) is about 5% to 30% for the application that can be sprayed / painted.
[056] The composite structural solid materials of this invention will comprise copper oxide particles dispersed substantially uniformly in them, present in a concentration in the range of 10% to 50% w / w
[057] According to this aspect, and in some embodiments, a portion of said copper oxide particles has the surface exposed.
[058] In some embodiments, as a function of the process for the preparation of the composite structural solid materials of this invention, copper oxide particles are incorporated in a manner in which copper oxide particles are not subjected to any chemical interaction with the compounds in a slurry preparation used in the preparation of the composite structural solid materials of this invention due to a pretreatment of the powder of a silicate, PMMA, polyester wax or other encapsulating material.
[059] According to this aspect, and in some embodiments, the copper oxide particles are dispersed evenly in the resin matrices as described in this document.
[060] In some embodiments, the uniform dispersion of the antimicrobial copper oxide particles imparts uniform biocidal or biostatic activity throughout the volume of the solid surface polymeric panel material of the invention and not just on the surface of the solid surface polymeric panel material .
[061] In some embodiments, in accordance with this aspect, such uniformly distributed antimicrobial characteristics dispersed throughout the solid material are particularly useful when surface imperfections in part of the solid surface polymeric panel material chosen from the inventions introduced with the use over time they are treated, for example, by scraping one or more higher-layered surfaces, which until now, with other surface-treated materials would result in a surface no longer characterized by antimicrobial activity. According to this aspect of the invention, the fact that the copper oxide particles are evenly distributed to be dispersed throughout the solid material allows removal of one or more surface layers while providing a new, clean and exposed surface characterized by effective antimicrobial activity.
[062] In some embodiments, copper oxide particles are present in an amount that imparts antimicrobial activity to the composite structural solid material, such that such activity is readily determined on an exposed surface of the material when in contact with a species microbial.
[063] In some embodiments, such antimicrobial efficacy can provide microbicidal or microbistatic activity that, for example, can provide a 3 log reduction in microbe count, within 2 hours of exposure to, or, for example, can provide a reduction of more than 90% in spore count, followed by exposure to the composite structural solid materials of this invention, as demonstrated by the results obtained with an "Antimicrobial Rigid Surface Test" and "Antimicrobial Rigid Surface Cleaning Test" as described in this document.
[064] Without being limited to theories, according to this aspect, the antimicrobial efficacy granted by the copper oxide particles incorporated within the materials as described in this document may be due to the release of snake ions in the exposed surroundings. Although the preferred mode of effectiveness is through a bridge of water or steam, it has been surprisingly found that, even on what appears to be a dry surface, there is efficacy that is possibly due to the water in the microbes themselves.
[065] In some embodiments, the copper oxide particles have a size in the range of about 0.1 to about 20 microns and in some embodiments, the copper oxide particles have a size in the range of about 1 to about 20 microns and in some embodiments, the copper oxide particles have a size in the range of about 5 to about 20 microns and in some embodiments, the copper oxide particle has a size in the range of about 5 to about 10 microns and remain the same size after the formation of the solidified material.
[066] In some embodiments, the "composite structural solid materials" of this invention include non-porous composites of finely divided mineral fillers dispersed in an organic polymer matrix. In some embodiments, the term "organic polymer matrix" is synonymous with resin "matrix".
[067] In some embodiments, this invention provides a finished product that comprises a composite structural solid material as described herein.
[068] In some embodiments, such a finished product may comprise a workbench, table, counter and spray plate, architectural faces and moldings, walkways, residential finish, patio furniture, hospital furniture, hospital bed accessories, handles, decorative stone, interior and exterior tile, floor, coverings, wall faces, both cladding sheets and decorative lining (painting), bathroom accessories, molded and cast structures of imitation stone structures and other related materials in which the incorporation of the composite structural solid material is appropriate.
[069] In some modalities, some finished products envisaged may include bathroom counters, sinks, shower cubicles, floors, wall panels and finishing pieces and kitchen counters and tiles, as well as other functional and / or decorative surfaces. In some embodiments, some glimpses of finished products may include furniture, lining materials and small stationary items. In some embodiments, some glimpses of finished products may include any surfaces found in healthcare environments, where the incidence of exposure to pathogenic microorganisms may be higher. According to this aspect, and in some embodiments, some finished products envisioned may include any surfaces found in hospitals, hospices, nursing homes, doctors' offices or other health therapists, as well as in commercial and residential food preparation facilities.
[070] In some embodiments, some glimpses of finished products may include any surfaces that may make contact as part of a regiment to ensure personal hygiene, such as bathrooms.
[071] In some embodiments, the finished products of this invention include materials useful for decorative solid surfaces such as, for example, those used as construction products such as bathroom countertops, sinks, tiles, shower cubicles and kitchen counters. Furniture, sanitary ware, lining materials and various items, such as office supplies and store displays, can also be finished finished materials, as well as laminate or other material that comprises a very thin coating of the composite structural solid material.
[072] In some embodiments, such finished products may also comprise surfaces in home bathrooms, public toilets, pool areas, bedrooms, stadiums and athletic facilities: sinks, counters, shower walls and bases, tiles and other walls that become wet during use. In some embodiments, such finished products may also comprise surfaces in health care facilities, such as hospitals, clinics, medical vans and nursing homes, the current invention providing antimicrobial protection in the form of surfaces for counters, sinks, walls and shower trays. , tiles and backsplash tiles in, for example, patient rooms, laundries, laundry areas, team and visitor areas, intensive care units and coronary care and corridors.
[073] The finished products and / or composite structural solid materials of this invention may also find application in offering antimicrobial protection where there is direct or indirect contact with food. Some examples are: counters, sinks, backsplash plates, floors and tables in kitchens; cold tables, counters and table protectors, food waiting areas, dirty dish areas and dish washing and drying areas in restaurants and fast-food outlets; certain areas in slaughterhouses where the insult of the nutrient is not excessive; table, counter, floors and spray plate areas canning, freezing, red meat packaging and bread and pastry making facilities; and grocery and fresh food counters, exhibitors and other displays in a grocery store.
[074] In some embodiments, the composite structural solid materials of this invention are useful in inhibiting and destroying many common harmful microorganisms found in the home environment, health care and food preparation. Microorganisms commonly found in such environments, for example, when such environments remain wet, humid, or hydrated, include bacteria, yeasts, fungi and viruses. Examples include, but are not limited to, various Gram-positive and Gram-negative bacteria, fungi and viruses, including, but not limited to Escherichia coli, Candida albicans, Staphylococcus aureus, Salmonella choleraesuis, Listeria weshimeri and Klebsiella pneumonia.
[075] In some embodiments, the composite structural solid material is melted into a sheet. In some embodiments, the composite structural solid material is melted using a compression molding process. In some embodiments, the composite structural solid material is melted using an extrusion process. In some embodiments, the composite structural solid material is melted using an injection molding process.
[076] In some embodiments, the composite structural solid material is prepared first as a viscous mixture in which the copper oxide powder is ultimately in suspension, which when sprayed or applied, followed by evaporation of the solvent will provide a film stiffened solid on top of a surface to which the spray / formulation was applied. In some embodiments, such an application results in a multilayer film, which is characterized in that such film comprises a polymeric resin and copper oxide particles dispersed substantially uniformly in it, in which said copper oxide is present in a concentration in the range of 10% to 50% w / w in which a portion of said copper oxide particles has the exposed surface.
[077] It should be understood that the composite structural solid materials of this invention comprise copper oxide particles dispersed substantially uniformly therein, in which the copper oxide is present in a concentration in the range of 10% to 50% in p / p, or in some modalities, in a concentration in the range of 8% to 60% in w / w, or in some modalities, in a concentration in the range of 15% to 40% in w / w, or in some modalities, at a concentration in the range of 15% to 30% w / w.
[078] In some embodiments, this invention provides a continuous pouring process for the manufacture of a composite structural solid material comprising a polymeric resin and copper oxide particles dispersed substantially uniformly in the same characterized by the fact that the process comprises the steps of: ♦ mixing a polymeric resin or a filler with copper oxide until they are well mixed to form a paste of copper oxide and resin or a mixture of copper oxide and resin; ♦ in stages, subsequently mix said copper oxide and resin paste or mixture of copper oxide and resin with a filler or resin, respectively and optionally a pigment to form a mixed composition containing copper oxide; ♦ in stages, subsequently mixing a catalyst with said mixed composition containing copper oxide to form a polymerizable composite structural material; ♦ distribute the said polymeric composite structural material in a mold; and ♦ provide conditions for polymerization of said polymerizable composite structural material, thus preparing a solid composite structural material.
[079] In some respects, the step which provides the subsequent mixing of a catalyst with said merged composition containing copper oxide to form a polymerizable composite structural material, refers to the formation of a material, which may be casually or not casually. made to heal / stiffen.
[080] In some embodiments, this invention provides a mixed batch process for the manufacture of a composite structural solid material comprising a polymeric resin and copper oxide particles dispersed substantially uniformly in the same characterized by the fact that the process comprises the steps of: ♦ mixing a polymeric resin, a filler and optionally a pigment; ♦ mixing a catalyst with a mixture of said polymeric resin, filler and optionally pigment; ♦ simultaneously mix copper oxide or a composition containing copper oxide with said catalyst for said mixture of said polymeric resin, filler and optionally said pigment or mix the copper oxide or a composition containing copper oxide in stages with said mixture of said polymeric resin, filler and optionally said pigment and said catalyst to form a polymerizable composite structural material; ♦ distribute the said polymeric composite structural material in a mold; and ♦ provide conditions for the polymerization of said structural material with polymeric composite, thus preparing a solid structural composite material.
[081] In some embodiments, this invention provides a continuous pouring process for the manufacture of a composite structural solid material comprising a polymeric resin and copper oxide particles dispersed substantially uniformly in the same characterized by the fact that the process comprises the steps of: ♦ mixing a polymeric resin and pigment well; ♦ in stages, add a catalyst to a mixture of said polymeric resin and pigment to form a mixture of polymeric resin containing catalyst; ♦ optionally in stages add a filler to said polymeric resin mixture containing catalyst to form a polymeric resin mixture containing catalyst and filler; ♦ in stages or simultaneously add a copper oxide or composition containing copper oxide to said polymeric resin mixture containing catalyst or said polymeric resin mixture containing catalyst and filler to form a polymeric resin containing copper oxide, pigment and catalyst mixture, ♦ distribute said polymeric resin containing copper oxide, pigment and catalyst mixture in a mold, optionally while applying a vacuum; and ♦ cure said polymeric resin containing copper oxide, pigment and catalyst mixture, optionally with the application of pressure, thus preparing a solid structural composite material.
[082] In some embodiments, the copper oxide powder will comprise Cu2O and in some embodiments, the copper oxide powder will comprise CuO, and in some embodiments, the copper oxide powder will comprise mixtures thereof. In the preferred embodiment size may vary and the process may take particle sizes of up to 20 microns with an embedded size of between 5 and 10 microns envisioned. In some embodiments, particle sizes of 0.1 to 20 microns are envisioned.
[083] Additionally, a system is shown for entry of copper oxide in the material that allows molding and melting of the material, delaying the solidification that is caused by both the compound's catalyst and the copper oxide. Under normal circumstances both the catalyst and the copper oxide alone would cause practically instantaneous solidification of the mixture, but it was surprisingly found that when the catalyst and copper oxide were mixed with each other as a last step or when copper oxide was added as the final ingredient, or when a mixture of copper oxide and filler or when a paste of copper oxide and resin is formed, solidification has been delayed.
[084] It has been surprisingly found that the manipulation of specific steps in the process of preparing composite materials could significantly impact the ability to arrive at a uniform distribution and optimized production of solid composite materials as described in this document.
[085] It was also surprisingly found that the catalyst could be added at the very beginning of the mixing process and copper oxide could be added as the last stage of the mixture and that such an order also delayed solidification.
[086] In one embodiment it was found that copper oxide when added as the last step in the process caused a delay in the solidification of the slurry and that contact that the copper oxide was added in a final stage there was a delay in the solidification that allowed application for end uses such as spray application.
[087] This invention also provides a method for imparting antimicrobial activity to a composite structural solid material, characterized by the fact that said method comprises preparing a composite structural solid material containing copper oxide dispersed therein, wherein said oxide of copper is present in a concentration in the range of 10 to 50% w / w in which a portion of said copper oxide particles has the exposed surface.
[088] In some embodiments, an exposed surface of said composite structural solid material has an antimicrobial reduction activity that represents a 90% reduction in microbial units in the period of 24 hours apart from the sample incubation.
[089] In some modalities, a surface exposed to said solid structural composite material is characterized by its ability to be exposed, repeatedly to organism challenge while maintaining said antimicrobial reduction activity for a period of time within said 24 hours from incubation of sample.
[090] In some modalities, antimicrobial activity represents bactericidal, sporicidal, or bacteriostatic activity and in some modalities, antimicrobial activity represents fungicidal, viricidal, fungistatic or viristatic activity. EXAMPLES EXAMPLE 1 METHODS FOR PRODUCING SOLID STRUCTURAL MATERIALS CONTAINING COPPER: BATHING MIXING PROCESS
[091] For the preparation of a solid polymeric material, the following ingredients can be used: Alumina trihydrate (ATH), Pigments, Reina and Methyl ethyl peroxide ketone catalyst. The process can be as follows: 1. ATH and fillers were mixed in a dry vessel. 2. Resin and pigments were then added and mixed thoroughly. 3. The MEKP catalyst was then mixed into the contents of the 1 e2acimae mixed thoroughly. 4. Mixed fluid paste was added to a mold. 5. The mold was placed in a vacuum chamber, preferably with a vibrating action to remove air bubbles that are trapped in the slurry that started to solidify within minutes. A normal initial solidification time was 15 to 30 minutes. 6. The solid surface plate or product was placed in a curing oven at 80 ° C for 30 to 45 minutes. 7. The solid surface sheet or product has now been removed and prepared for measurement and finishing sanding.
[092] The skilled worker will verify that several changes to the protocol can be made as part of the routine process execution. When the worker wishes to include copper oxide within the polymeric starting material, for example, it is readily apparent to the worker that the typical process would include making use of the following ingredients: ATH, main batch of PET, Copper oxide powder, Pigments, Resin and MEKP catalyst, whereby the process involves mixing all ingredients other than MEKP, that is, ATH, main batch of PET, copper oxide powder, pigments and resins. The worker would then conventionally add MEKP catalyst and mix the combined ingredients completely just before melting the mixture into a mold.
[093] When the above process was performed, however, surprisingly when MEKP was added and mixed into the mixture after the dry ingredients, pigments and resin were mixed, followed by the addition of copper oxide. When the powder was added to the mixture during normal formulation for the preparation of a solid surface, which was at the time of mixing dry materials and then the resin was mixed with the dry materials and finally MEKP would be added as the last step, by means of Addition of MEKP in the final pasty mixture practically instantaneous solidification occurred, that is, the resulting mixture solidified prematurely, so that an uneven semi-rigid preparation that was obtained could not be readily melted. Such premature solidification was not pronounced when the copper oxide powder was supplied in a w / w concentration of as little as 2%. Even a 2% level resulted in an acceleration of the solidification process and the higher the concentration, the faster the solidification process occurred.
[094] As stated above when the powder was added in small quantities at a 3% w / w ratio, this accelerated the solidification prematurely. Reasons have changed as the level of copper dust has risen as this would mean a decrease in main batch according to the increase in the amount of powder in order to maintain sufficient main batch and combined powder to maintain effectiveness. This formulation was carried out at levels of (1) 3.75% powder with 49% main batch (2) 4.75% powder with 45% main batch (3) 6% powder 40% main batch ( 4) 7% powder with 36% main batch (5) 8% powder with 32% main batch (6) 9% powder with 28% main batch (7) 10% powder with 24% batch main. All other parts of the main ingredients maintained the same reasons.
[095] Unexpectedly, when the process was instead carried out in the following order, in which a mixture of resin and pigments was prepared and MEKP was added to the mixture, after that, loads and main batch / treated powder were then mixed in the pre-mix containing MEKP, or copper oxide was then mixed in the pre-mix containing MEKP, surprisingly, such a mixture could easily be melted into a mold and the process could be easily performed, even with high concentrations of powder copper oxide incorporated into it.
[096] As demonstrated in this document, the stiffening of the mixture was delayed profoundly as a function of the order in which MEKP and copper oxide were added to the mixture containing pigment and resin. EXAMPLE 2 METHODS TO PRODUCE COMPOSITE STRUCTURAL SOLID MATERIALS CONTAINING INCORPORATED COPPER:
[097] A built-in process to produce a composite structural material containing copper of this invention makes use of the following ingredients and the relative percentages by weight are provided in the parentheses that follow them: Alumina Trihydrate (ATH) (7% to 20% ), main batch of PET prepared, for example, as described in EU Patent Application 1860949, which contains copper oxide - (up to 40%), copper oxide powder (up to 10%), pigments (up to 3%) , resin (between 28 to 40%) and MEKP catalyst (1%).
[098] An exemplified process can include the steps: 1) Mix all the dry ingredients [Alumina Trihydrate at a ratio of 17% w / w and main batch at a ratio of 40% w / w] except the oxide powder copper in a first vessel (vessel A). 2) Mix all liquid ingredients except MEKP [at a ratio of 1% w / w] in a second vessel (vessel B) [Resin and Pigment at a ratio of 2% w / w]. 3) Add MEKP and mix completely in vessel B. 4) Add the dry ingredients from vessel A to the liquid ingredients in vessel B and mix thoroughly [Add Alumina Trihydrate and Main Batch from vessel A to Resin and Pigment from vessel B]. 5) Add copper oxide [6% w / w ratio] to the combined mixture [listed above in the previous step] in vessel B and mix quickly 6) Place the mixture in an appropriate mold spreading it evenly. 7) Place the mold in a vacuum and vibration pressure chamber 8) Start vibration sequences for 2 to 10 minutes, start vacuum pressure for 5 to 30 minutes. 9) Remove the initially stiffened blade that remains in the vacuum chamber mold to cool and cure at room temperature for 4 to 24 hours. 10) Warm Up / Post Cure Stage: This is another surprising check and major difference from what someone familiar with the technique would expect to do. It was found that heat was an impediment to producing quality blades and was therefore eliminated. 11) The normal post-curing in a plate oven was eliminated as it was found that this stage surprisingly prevented the plates from obtaining the rigidity of a normal plate. 12) Measure and sand and polish the sheet 13) Inspect any defects 14) Pack for shipping and distribution
[099] It was surprisingly found that with the use of a batch of 20% copper oxide PET a post-curing stage could be eliminated. It was also surprisingly found that adding the copper oxide powder as the last step before melting allowed for a surprising delay in solidification.
[100] It was also surprisingly found that adding MEKP to the resin prior to the addition of fillers and dry ingredients also delayed solidification.
[101] Additionally, when the process was conducted in the absence of vibration applied during the vacuum process, the resulting solid material did not contain air pockets / air bubbles, which would normally be present.
[102] The delay of chemical stiffening in the incorporated processes as described in this document, was consistently between 20 and 30 minutes which is sufficient time for the formation of the desired products.
[103] In one embodiment it was found that 10 micron powder treated with a silicate or PMMA powder treatment grind could be used in place of the main batch or in addition to the main batch to achieve the same effect. Those familiar with the main batch synthesis technique know that copper oxide powder can be treated in a mixture of high purity with a coating ratio of approximately 4 grams of a silicate or PMMA or other inert compound for a kilodepod of copper oxide. EXAMPLE 3 COMPOSITE STRUCTURAL SOLID MATERIALS CONTAINING INCORPORATED COPPER EXHIBIT ANTIMICROBIAL ACTIVITY MATERIALS AND METHODS A. Preparation of inocula:
[104] For Bacteria: - Stock culture bacteria were transferred to TSB and incubated at 35 to 37 ° C for 24 + 2 hours. Daily transfers were made for at least three consecutive days (but no more than 10 days). For each transfer, tubes containing 10 ml of TSB were inoculated with the use of two inoculum loops (internal diameter of 4 mm) for each tube. A culture of 48 + 4 hours was used for the inoculants on the day of testing.
[105] For Fungus: Fungi from stock cultures were transferred to Sarbouraud's dextrose broth and incubated at 25 to 30 ° C for 24 + 2 hours. Daily transfers were made for at least three consecutive days (but no more than 10 days). For expensive transfer, tubes containing 10 ml of SDB were inoculated with the use of two inoculum loops (internal diameter of 4 mm) for each tube. A culture of 48 + 4 hours was used for the inoculum on the day of testing.
[106] For both cultures: transfers more than 15 days away from stock cultures were not used for the inoculum for the test.
[107] For each microorganism, each culture was mixed thoroughly in a vortex mixer and allowed to settle for> 15 minutes. The top two thirds of each culture were aspirated and used as the inoculum.
[108] B. Addition of organic filler: For each prepared inoculum, an aliquot of 0.25 ml of FBS plus 0.05 mll% of Triton X-100 solution to 4.70 ml of bacterial suspension to yield a 5% FBS and 0.01% solid load of Triton X-100.
[109] C. Test Preparation and Carrier Control:
[110] The test (three batches, five repetitions per batch per microorganism) and control / carrier surfaces (three pre-microorganism repetitions) plus additional testing and control surfaces as required for remaining controls were cleaned by submersion in 70 to 85% in isopropyl alcohol, rinsed with sterile deionized water and allowed to air dry. After drying completely, the carriers were sterilized for 15 minutes at 121 ° C. Carriers were allowed to cool and remain at room temperature until use. Prior to use, each carrier was transferred aseptically to plastic Petri dishes (one plate for each carrier) added to two pieces of filter paper using sterile forceps.
[111] D. Carrier inoculation:
[112] A 0.02 ml aliquot of the inoculum was transferred to each sterile carrier using a calibrated micro dropper. The inoculum was spread within approximately 3.17 mm (1/8 ") of the carrier's edge. The carriers were allowed to dry with half-open lids for 20 to 40 minutes under ambient conditions. The exposure period (contact time) started immediately after drying.
[113] E. Test:
[114] For each microorganism per batch, five inoculated and dry carriers were maintained for the duration of exposure (contact). The contact time started immediately after drying in accordance with Section D, Carrier Inoculation. At the conclusion of the contact time, each carrier was transferred to a jar containing 20 ml of neutralizer at the appropriate staggered intervals. Each jar was sonicated for five minutes and then manually rotated to mix. Within one hour after sonication, serial dilutions were prepared using PBS (10-1 to 10-4). Duplicate 1 ml aliquots of each jar / dilution (100 to 10-4) were plated using dump plates.
[115] For Bacteria: Plates were incubated for 48 + 4 hours at 35 to 37 ° C, colonies were counted and CFU / carrier calculated.
[116] For Fungus: Plates were incubated for 48 + 4 hours at 25 to 30 ° C, colonies were counted and the CFU / carrier calculated.
[117] SPORE TESTING
[118] Note: All manipulations and incubation of the test culture, unless otherwise stated, will be conducted under strict anaerobic conditions. All media and reagents will be pre-reduced prior to use.
[119] A. Preparation of spore suspension:
[120] Using a defrosted vegetative frozen stock culture, 100 μl was added to an Erlenmeyer flask containing 10 ml of SPC and incubated for 24 + 4 hours at 35 to 37 ° C. CABA plates were spread with the culture overnight (100 μl / plate) and incubated for 7 to 10 days at 35 to 37 ° C. During the incubation period, plaque growth was checked periodically to inspect the culture and to estimate the approximate spore to vegetative cell ratio using phase contrast microscopy. A sample of the growing culture was collected with a sterile inoculation loop on a glass slide containing 10 μl of deionized water and mixed to make a suspension prior to observation by phase contrast microscopy. Under phase contrast, the spores appeared shiny and ovular, white vegetative cells appear dark and stick-shaped.
[121] Once the spores reached a spore to vegetative cell ratio of> 90%, cultures were collected from each plate by adding 5 + 1 ml of ST80 to each plate and gently scraping the surface of each plate with a cell scraper to dislodge growth. The collected material was grouped in a sterile 50 ml centrifugal tube. The tubes containing the suspensions were centrifuged at 4,500 x g for 15 minutes and washed three times with ice-cold ST80 (2 to 5 ° C). The final pellet in each tube was resuspended in approximately 5 ml of ST80.
[122] Each spore suspension was purified using standard internal procedures and included heat shock, washed with the use of ST80 and a 50% (w / v) solution of HistoDenz and centrifugation with resuspension with the use of ST80. The contents of each tube were combined. A culture sample was collected with a sterile inoculation loop on a glass slide containing 10 μl of deionized water and mixed to make a suspension prior to observation by phase contrast microscopy to confirm the presence of spore ratio to vegetative cell > 90%.
[123] An evaluation of inoculum count was performed by serially diluting the suspension prepared using PBS and duplicate aliquots will be plated using BHIY-HT. The plates were incubated for 2 to 4 days at 35 to 37 ° C. The CFU / ml will be documented. The spore suspension was frozen at approximately -70 ° C until use on the day of the test.
[124] On the day of the test, the suspension was defrosted and a sample of the culture was collected with a sterile inoculation loop on a glass slide containing 10 μl of deionized water and mixed to make a suspension prior to observation by contrast microscopy. phase to confirm the presence of spore to vegetative cell ratio of> 90%.
[125] The culture was diluted using PBS to yield approximately 5 x 106 CFU / ml based on pre-test inoculum counts. The culture was mixed thoroughly in a vortex mixer and allowed to set for> 15 minutes. The upper two thirds of the culture as aspirated and used as the inoculum.
[126] B. Addition of organic load:
[127] One 0.25 ml aliquot of FBS plus 0.05 mll% Triton X-100 solution to 4.70 ml of the bacterial spore suspension to yield a 5% FBS and 0.01% load solid of Triton X-100.
[128] C. Test Preparation and Carrier Control:
[129] The test (three repetitions per contact time using two contact times) and control surfaces / carriers (two repetitions per contact time) plus test and additional control surfaces as required for remaining controls were cleaned by submersion in 70 85% in isopropyl alcohol, rinsed with sterile deionized water and allowed to air dry.
[130] After drying completely, the carriers were sterilized for 15 minutes at 121 ° C. Carriers were allowed to cool and remain at room temperature until use. Prior to use, each carrier was transferred aseptically to plastic Petri dishes (one plate for each carrier) added to two pieces of filter paper using sterile forceps.
[131] D. Carrier inoculation:
[132] A 0.02 ml aliquot of the inoculum was transferred to each sterile carrier using a calibrated micro dropper. The inoculum was spread within approximately 3.17 mm (1/8 ") of the carrier's edge. The carriers were allowed to dry with half-open lids for 20 to 40 minutes under ambient conditions. The exposure period (contact time) started immediately after drying.
[133] E. Test:
[134] For each contact time, three inoculated and dry carriers were maintained for the duration of exposure (contact). The contact time started immediately after drying in accordance with Section D, Carrier Inoculation. At the conclusion of the contact time, each carrier was transferred to a jar containing 20 ml of neutralizer at the appropriate staggered intervals. Each jar was sonicated for five minutes and then manually rotated to mix. Within one hour after sonication, serial dilutions were prepared using PBS. Duplicate aliquots of each jar / dilution were plated using BHIY-HT plates. All plates were incubated for 2 to 4 days at 35 to 37 ° C, colonies were counted and the CFU / carrier was calculated.
[135] Test and Results Protocol: For each challenge organism, three tests (for each concentration) and two control surfaces were processed. Using a +/- 48 hour culture containing organic filler, the test and control surfaces were contaminated with 0.02 ml of the inoculum and the inoculum was spread within approximately 3.17 mm (1/8 inch) the edge of the surface. The surfaces were dried with the lids ajar for 40 minutes under ambient conditions (20C). The contact time was initiated with the completion of the drying period.
[136] Upon completion of the contact time (2 hours), each surface was transferred to a jar containing 20 ml of neutralizer and the jar was sonicated for five minutes. The jar was then turned by hand to mix. Within an hour, serial dilutions were performed and selected dilutions were plated. Alistair: the test methods are much more extensive than the description - there is a repeated abrasion test (up to 12 wet and dry cycles) and repeated contamination every 2 hours for 24 hours.
[137] The challenge microorganisms were confirmed by colony morphology and Gram stain to be consistent with Staphylococcus aureus and Enterobacteri aerogenes. All purity control marks were evaluated in the same way and both challenge microorganisms were validated as pure.
[138] The percentage reduction was calculated using the following formula:
EXAMPLE 4 COMPOSITE STRUCTURAL SOLID MATERIALS CONTAINING INCORPORATED COPPER
[139] Using the following materials and description, synthetic marble slabs for application on rigid surfaces were produced.
[140] INGREDIENTS: ATH -7% to 20% Main batch of PET containing copper oxide - up to 40% Copper oxide powder-10% Pigments-up to 3% Resin - between 20 to 38% Catalyst -1%
[141] Process:
[142] In a vase, mix resin and pigments with each other
[143] Add catalyst
[144] Add ATH
[145] Add main batch of PET (as described in the International PCT Application Publication in WO 2006/100665, which is incorporated entirely hereby in this document for reference), which has been ground into a coarse powder or copper oxide that has been encapsulated with a silicate or PMMA or some other inert material.
[146] Mix thoroughly.
[147] Merging name
[148] Place the mold in a vacuum chamber and apply vacuum, pressure and vibration. Allow the blade to fully cure prior to finishing measurement and sanding.
[149] Using the followingmaterials and description, a liquid form of synthetic marble for application to any surface in an application with paint brush or spray is described.
[150] INGREDIENTS: Smoked silica -7% to 20% Main batch of PET containing copper oxide - up to 40% Copper oxide powder - up to 16% Pigments - up to 3% Resin - between 28 to 75% MEKP-1 catalyst % MEK thinner 0 to 10%
[151] PROCESS:
[152] In a vase, mix resin and pigments with each other
[153] Add smoked silica
[154] Add main batch of PET that has been ground into a coarse powder or copper oxide that has been encapsulated with a silicate or PMMA or some other inert material
[155] Mix thoroughly.
[156] Add MEK until the desired viscosity is achieved.
[157] Add MEKP
[158] Immediately spray or paint on the surface
[159] Using the following materials and description, a flexible sheet of synthetic marble was created for application, but without limitation, on easy-to-clean and quiet floors, foldable molds around columns and corners, impact resistant shock absorbers, chair rails, wheelchair tires, escalator handrail straps, food processing conveyor belts and more scratch resistant surface. INGREDIENTS: ATH -7% to 15% Main batch of PET containing copper oxide - up to 40% Copper oxide powder -10% Pigments-up to 3% Resin - between 25 to 33% MEKP catalyst-0.25 to 1%
[160] PROCESS:
[161] In a vase, mix resin and pigments with each other
[162] Add ATH
[163] Add MEKPe and mix thoroughly
[164] Add MEKP catalyst and main batch of PET that was ground into a coarse powder or copper oxide that was encapsulated with a silicate or PMMA or some other inert material
[165] Mix thoroughly.
[166] In this case, the resin content has been reduced to approximately 25% and the ATH load has been increased to 15%, however, these proportions may change depending on variations in the main batch, resins and MEKP catalysts and the desired qualities of the finished product. EXAMPLE 5 CORPORATE ANALYSIS TO ASSESS ACTIVITY ANTIMICROBIAL COMPOSITE STRUCTURAL SOLID MATERIALS CONTAINING COPPER
[167] Inoculum preparation:
[168] For Staphylococcus aureus: Bacteria from stock cultures were transferred to TSB and incubated at 35 to 37 ° C for 24 + 2 hours. Daily transfers were made for at least three consecutive days (but no more than 10 days). For each transfer, tubes containing 10 ml of TSB were inoculated with the use of two inoculum loops (internal diameter of 4 mm) for each tube. A culture of 48 + 4 hours was used for inoculations on the day of testing.
[169] For Enterobacter aerogenes: Bacteria from stock cultures were transferred to TSBe incubated at 25 to 30 ° C for 24 + 2 hours. Daily transfers were made for at least three consecutive days (but no more than 10 days). For each transfer, tubes containing 10 ml of TSB were inoculated with the use of two loops (inner diameter of 4 mm) from inoculum to each tube. A culture of 48 + 4 hours was used for the inoculum on the day of testing.
[170] For each microorganism, each culture was mixed thoroughly in a vortex mixer and allowed to settle for> 15 minutes. The top two thirds of each culture were aspirated and used as the inoculum. Transfers more than 15 days away from stock cultures will not be used for the inoculum for testing.
[171] ORGANIC LOAD ADDITION:
[172] For each prepared inoculum, an aliquot of 0.25 ml of FBS plus 0.05 mll% Triton X-100 solution to 4.70 ml of bacterial suspension to yield an FBS of 5% and 0 , 01% solid load of Triton X100.
[173] TEST PREPARATION AND CARRIER CONTROL:
[174] The test and control surfaces were cleaned by submersion in 70 to 85% isopropyl alcohol, rinsed with sterile deionized water and allowed to air dry. After drying completely, the carriers were sterilized for 15 minutes at 121 ° C. Carriers were allowed to cool and remain at room temperature until use. Prior to use, each carrier was transferred aseptically to plastic Petri dishes (one plate for each carrier) added to two pieces of filter paper using sterile forceps.
[175] For each batch of test material, by microorganism, five sets of with five repeated carriers per set were prepared along with five sets per microorganism of control material with three repeated carriers each for the primary aspects of the test.
[176] Additional surfaces were prepared as required for remaining controls.
[177] TEST:
[178] All test surfaces were inoculated at staggered intervals with 5 µl of the challenge microorganism using a calibrated dropper. The inoculum was spread within approximately 3.17 mm (1/8 ") of the carrier's edge. This initial inoculation was considered" zero time ". These carriers were dried under ambient conditions for the duration of the exposure. exposure period (s) starts with the initial "zero time" inoculation. Applicable sets not removed for quantitative recovery (see below) were reinoculated in the same way at 3,6,9,12,15,18 and 21 hours post "zero time" inoculation.
[179] Applicable sets for quantitative recovery were removed in 2 (single inoculation), 6 (two inoculations), 12 (four inoculations), 18 (six inoculations) and 24 (8 inoculations) hours. At the conclusion of the applicable contact time for each set of surfaces, each carrier was transferred to a jar containing 20 ml of neutralizer at the appropriate staggered intervals. Each jar was sonicated for five minutes and then manually rotated to mix. Within one hour after sonication, serial dilutions were prepared using PBS (10-1 to 10-4). Duplicate 1 ml aliquots from each jar / dilution (100] to 10-4) were plated using TSA dump plates.
[180] For Staphylococcus aureus: Plates were incubated for 48 + 4 hours at 35 to 37 ° C, colonies were counted and CFU / carrier calculated.
[181] For Enterobacter aerogenes: Plates were incubated for 48 + 4 hours at 25 to 30 ° C, colonies were counted and the CFU / carrier was calculated.
[182] CONTROLS:
[183] CARTER QUANTIFICATION CONTROL:
[184] For each challenge microorganism, a parallel control was performed using the control carriers (surfaces) in the same way as the test (inoculation and quantitative recovery) with the exception that three replicates were evaluated instead of five. All plates were incubated appropriately in the same manner as the test plates as applicable for each challenge microorganism.
[185] CULTURE PURITY CONTROL:
[186] Each prepared culture was marked for isolation using TSA. All plates were incubated appropriately in the same manner as the test plates as applicable for each challenge microorganism. Isolated cultures were observed for purity.
[187] ORGANIC SOIL STERILITY CONTROL:
[188] Duplicate 1 ml aliquots of the prepared organic soil were plated on TSA dump plates. The plates were incubated for 48 + 4 hours at 35 to 37 ° C and observed for growth or non-growth.
[189] INOCULATION CONFIRMATION COUNTS CONTROL:
[190] Each prepared inoculum was serially diluted using PBS and selected dilutions were plated in duplicate using TSA dump plates. All plates were incubated appropriately in the same manner as the test plates as applicable for each challenge microorganism.
[191] NEUTRALIZER STERILITY CONTROL:
[192] A single jar containing the neutralizer was incubated for 48 + 4 hours at 35 to 37 ° C. The neutralizer was observed for growth or non-growth.
[193] CARRIER STERILITY CONTROL:
[194] An uninoculated test (per batch) and control carrier were subcultured in independent jars containing the neutralizer and incubated for 48 + 4 hours at 35 to 37 ° C. The neutralizer was observed for growth or non-growth.
[195] CARRIER FEASIBILITY CONTROL:
[196] For each challenge microorganism, a single inoculated control carrier was subcultured in a jar containing the neutralizer and incubated in the same manner as test plates as applicable for each challenge microorganism.
[197] Neutralizer jars have been observed for growth or non-growth.
[198] NEUTRALIZER EFFICIENCY CONTROL:
[199] For each challenge microorganism, per batch of the test article, a single sterile test holder was neutralized in the same way as the test (transferred to individual jars containing 20 ml of neutralizer). For each jar, a 1 ml aliquot of the diluted inoculum was added to yield 100 CFU / ml in the neutralizer. The jar was mixed and a 1 ml aliquot was removed and plated in duplicate.
[200] A number control was performed in the same way with the exception that a sterile control wearer was used.
[201] All plates were incubated appropriately in the same manner as the test plates as applicable for each challenge microorganism.
[202] MICRO-ORGANISM CONFIRMATION PROCEDURES:
[203] A colony randomly selected from the carrier quantitation control plates and, if applicable, a colony randomly selected from a test plate was confirmed by colony morphology and Gram stain according to existing SOPs. The same procedures were performed with the use of culture purity control plates and the result in relation to purity was also documented.
[204] Preparation of inoculum:
[205] Bacteria from stock cultures were transferred to TSB and incubated at 35 to 37 ° C for 24 + 2 hours. Daily transfers were made for at least three consecutive days (but no more than 10 days). For each transfer, tubes containing 10 ml of TSB were inoculated with the use of two inoculum loops (internal diameter of 4 mm) for each tube.
[206] The film formed in the culture of Pseudomonas aeruginosa was aspirated before use.
[207] For all cultures: transfers more than 15 days away from stock cultures will not be used for the inoculum for testing.
[208] FOR INITIAL AND FINAL DISINFECTANT TEST INOCULUS:
[209] For each challenge microorganism, a culture of 48 to 54 hours was mixed in a vortex and allowed to remain for 15 + 1 minutes. Addition of organic load: a 0.25 ml aliquot of FBS plus 0.05 mll% Triton X-100 solution to 4.70 ml of bacterial suspension to yield a 5% FBS and 0.01% solid TritonX load - 100. The top two thirds of each culture were aspirated and used as the inoculum.
[210] For the inoculations / reinoculations of the carriers used in the simulated wear tests: For each challenge microorganism, a culture of 18 to 24 hours was mixed in a vortex and allowed to stay for 15 + 1 minutes. The upper two thirds of each culture were aspirated and used as inoculum. Two 1: 100 dilutions of the culture were made using sterile deionized water (two serial dilutions from 0.1 ml to 9.9 ml) and a final dilution of 5 ml of the diluted suspension to 5 ml of sterile deionized water. Addition of organic filler: a 0.25 ml aliquot of FBS plus 0.05 mll% TritonX-100 solution to 4.70 ml of bacteria suspension to yield a 5% FBS and 0.01% Triton X 100 solid load .Note: It was not allowed that any culture remained with organic load for more than eight hours. TEST PREPARATION AND CARRIER CONTROL:
[211] The test and control surfaces (carriers) were cleaned by submersion in 70 to 85% isopropyl alcohol, rinsed with sterile deionized water and allowed to air dry. After drying completely, the carriers were sterilized for 15 minutes at 121 ° C. Carriers were allowed to cool and remain at room temperature until use. Prior to use, each carrier was transferred aseptically to plastic Petri dishes (one plate for each carrier) added to two pieces of filter paper using sterile forceps. For each batch of the test material, by microorganism, two sets of with two repeated carriers per set were prepared together with two sets per microorganism of the control material with four repeated carriers each for the primary aspects of the test. Additional surfaces were prepared as required for remaining controls. INITIAL DISINFECTANT ASSESSMENT TEST:
[212] For each batch of the test surface, by microorganism, four carriers and four control surface carriers (by microorganism) were inoculated at staggered intervals with 10 μl (0.01 ml) of the initial disinfectant inoculum prepared with the use of a calibrated dropper. The inoculum was spread within approximately 3.17 mm (1/8 ") of the carrier's edge and carriers were allowed to dry for 30 to 40 minutes at 35 to 37 ° C, at a relative hydration rate of 38 to 42% (RH) Immediately after drying, the contact time of 120 minutes (exposure period) was at room temperature. Upon completion of the contact time of 120 minutes, each carrier was transferred to a jar containing 30 ml of neutralizer in the appropriate staggered intervals Each jar was sonicated for 20 + 2 seconds Samples were mixed on an orbital shaker for 3 to 4 minutes at 250 rpm. Within one hour after sonication, serial dilutions were prepared using deionized water sterile (10-1 to 10-4). Duplicate 1 ml aliquots of each jar / dilution (100 to 10-2) were plated using TSA dump plates. Duplicate 1 ml aliquots of each jar / dilution (101 to 10-4) for the control patients were plated using d and TSA eviction.
[213] Note: All dilutions and plating for each repeated carrier were performed within one hour of transfer to the neutralizer. All test plates were incubated for 48 + 4 hours at 35 to 37 ° C, colonies were counted and CFU / carrier calculated. SIMULATED WEAR AND REINOCULATION:
[214] Prior to inoculation, the abrasion tester was set to a speed of 2.25 to 2.50 for a total surface contact time of approximately 4 to 5 seconds for a complete cycle. Speed was measured with a calibrated stopwatch. The machine cycle was calibrated by setting the number counter to 1, 5, 10 and 20 and checking the cycle time. It was defined so that a pass through the abrasion tester with the surfaces is equal to a contact time of approximately 2 seconds. A wear cycle will be equal to a pass to the left and a return pass to the right on the Gardner scrubber with an abrasion container equipped with a foam lining and dry cotton fabric. The fully assembled abrasion container will be equipped with two weights, a foam lining and a cotton fabric. It was assembled in an aseptic manner. The weight of the fully assembled weighing container was found to be 1,084 + lg prior to use. For each batch of the test surface, by microorganism, four carriers were inoculated at staggered intervals with 10 μl (0.01 ml) of the simulated wear inoculum prepared using a calibrated dropper. The inoculum was spread within approximately 3.17 mm (1/8 ") of the carrier's edge and carriers were allowed to dry for 30 to 40 minutes at 35 to 37 ° C. These inoculation and drying procedures were designated" reinoculated and drying ". To start the wear cycles, each wearer was subjected to a dry wear cycle using the Gardco Washable and Wear Tester and the weighing container fully assembled. At least 15 minutes after the initial wear cycle each carrier was reinoculated and dried as previously described Each carrier was subjected to a wet wear cycle using the Gardco Washable and Wear Tester and the fully assembled weighing container The fully assembled weighing container was sprayed by a second with sterile deionized water using a Preval sprinkler (or equivalent) from a distance of 75 + 1 cm for no more than one second. At least 15 minutes after these wear cycles Secondary, each carrier was reinoculated and dried and subjected to alternating dry and wet wear until a total of 11 reinoculations and 12 wear cycles were performed according to the procedures and timeline outlined in Table 1 on the next page.
[215] Note: The surface support of the Gardner device has been decontaminated with 70% IPA between each set of surface wear to prevent transfer contamination. The IPA was allowed to evaporate completely before proceeding. The foam lining and cotton fabric have been replaced between each set of surface wear.
[216] WEAR AND REINOCULATION PROCEDURE 1.Inoculation and initial drying 2.Wear cycle with dry fabric (wear # 1) 3.Rinoculation and drying 4.Wear cycle with wet fabric (wear 2) 5.Reinoculation and drying 6.Wear cycle with dry fabric (wear no. 3)
[217] End of the first day 8. Wear cycle with damp fabric (wear 4) 9.Rinoculation and dry wear 10. Wear cycle with dry fabric (wear 5) 11.Rinoculation and dry 12. Wear cycle with wet fabric (wear 6) 13. Reinoculation and drying 14.Wear cycle with dry fabric (wear 7) 15.Reinoculation and dry 16.Wear cycle with wet fabric (wear 8) 17.Reinoculation and drying 18.Wear cycle with dry fabric (wear 9) 19.Reinoculation drying. wear with damp fabric (wear 10) 21.Repost and dry 22.Wear cycle with dry fabric (wear no11) 23.Rinoculation and drying 24.Wear cycle with wet fabric (wear12)
[218] Evaluation of Final Disinfectant is performed after the 12th wear cycle and two days after the initial inoculation
[219] Final Disinfectant Evaluation: (Performed at least two days after the initial inoculation for the Simulated Wear and Reinoculation procedures) For each batch of the test surface, by microorganism, four carriers and four control surface carriers (by microorganism ) were inoculated at staggered intervals with 10 μl • (0.01 ml) of the final disinfectant inoculum prepared using a calibrated dropper. The inoculum was spread within approximately 3.17 mm (1/8 ") of the carrier's edge and carriers were allowed to dry for 30 to 40 minutes at 35 to 37 ° C, at a relative hydration rate of 38 to 42% (RH) Immediately after drying, the contact time of 120 minutes (exposure period) was at room temperature At the conclusion of the contact time, each carrier was transferred to a jar containing 30 ml of neutralizer at the appropriate step intervals Each jar was sonicated for 20 + 2 seconds. The samples will then be mixed on an orbital shaker for 3 to 4 minutes at 250 rpm. Within one hour after sonication, serial dilutions were prepared using sterile deionized water ( 10-1 to 10-4). Duplicate 1 ml aliquots from each jar / dilution (100] to 10-2) for test holders were plated using TSA dump plates. each jar / dilution (l0-1 to 10-4) for the control holders were plated using TSA dump plates.
[220] Note: All dilutions and plating for each repeated carrier were performed within one hour of transfer to the neutralizer. All test plates were incubated for 48 + 4 hours at 35 to 37 ° C, colonies were counted and CFU / carrier calculated. For Enterobacter aerogenes: Plates were incubated for 48 + 4 hours at 25 to 30 ° C, colonies were counted and the CFU / carrier was calculated. CONTROLS: 1.CULTURE PURITY CONTROL:
[221] Each prepared culture was marked for isolation with the use of TSA (initial and final disinfectant preparations as well as each Simulated Wear and Reinoculation inoculum (two, one for each day of the two-day regiment)). All plates were incubated with the test plates. Isolated cultures were observed for purity. 2. ORGANIC SOIL STERILITY CONTROL:
[222] Duplicate 1 ml aliquots of the prepared organic soil were plated on TSA dump plates. This was performed on each of the following days of the analysis: the initial and final disinfectant days according to each of the two-day Simulated Wear and Reinoculation procedures. The plates were incubated with the test plates and observed for growth and non-growth. 3. INOCULATION CONFIRMATION COUNTS CONTROL:
[223] Each prepared inoculum was serially diluted using PBS and selected dilutions were plated in duplicate using TSA dump plates. This was performed on each of the following days of the analysis: the initial and final disinfectant days and each of the two-day Simulated Wear and Reinoculation procedures. All plates were incubated with the test plates. 4. NEUTRALIZER STERILITY CONTROL:
[224] A single jar containing the neutralizer was incubated for 48 + 4 hours at 35 to 37 ° C. The neutralizer was observed for growth or non-growth. 5. CARRIER STERILITY CONTROL:
[225] An uninoculated test (per batch) and control carrier were subcultured in independent jars containing the neutralizer and incubated for 48 + 4 hours at 35 to 37 ° C. The neutralizer was observed for growth or non-growth. 6. CARRIER FEASIBILITY CONTROL:
[226] For each challenge microorganism, a single inoculated control carrier was subcultured in a jar containing the neutralizer and incubated in it with the test plates (this control was done for both initial and final disinfectant test days) . The neutralizer jars were observed for growth or non-growth. 7. NEUTRALIZER EFFECTIVENESS CONTROL:
[227] The neutralization efficacy was assessed for each challenge microorganism concurrently with testing. Using sterile forceps, sterile carriers (one repeated for each of the three test lots and one repeated on the control surface) were transferred to jars containing 30 ml of neutralizer. At intervals of time after each surface addition, an aliquot of the bacterial suspension (to yield approximately 1,000 CFU) has been added and the jars will be mixed. In 5 + 1 minutes, a 1 ml aliquot was removed from each jar and plated using TSA dump plates. These procedures were repeated using additional dilutions (to yield approximately 500 CFU and 250 CFU). All plates were incubated with the initial disinfectant test plates. 8. MRSA ANTIMICROBIAL SUSCEPTIBILITY TEST:
[228] The prepared MRSA culture was subcultured on a TSA + plate and the plate was incubated for approximately 24 hours at 35 to 37 ° C. Following incubation, a suspension was prepared by suspending TSA + culture growth in SS to yield turbidity equivalent to a McFarland Standard of 0.5. This prepared suspension was marked on the MHA plate in a cross-hatch pattern and a 1 μg Oxacillin disc was placed in the center of the plate. The plate was inverted and incubated for> 24 hours at 35 to 37 ° C. The same procedures were carried out concurrently with the use of the control microorganism, Staphylococcus aureus, ATCC 25923 to confirm the validity of the analysis. The interpretation of the zone of inhibitions (COI) was based on the National Committee established for performance standards of Clinical Laboratory Standards (NCCLS). As currently published, (M100-S21 NCCLS standard) ZOI discontinuity points need to be <10 mm (rounded to the nearest whole mm) confirms resistance, 11 to 12 mm is considered intermediate resistance and> 13 mm confirms susceptibility. 9. MICRO-ORGANISM CONFIRMATION PROCEDURES:
[229] A colony randomly selected from the carrier quantitation control plates and, if applicable, a colony randomly selected from a test plate was confirmed by colony morphology and Gram stain according to existing SOPs. The same procedures were performed with the use of culture purity control plates and the result in relation to purity was also documented. EXAMPLE 6 METHODS FOR PRODUCING SOLID STRUCTURAL MATERIALS CONTAINING COPPER: CONTINUOUS EVICTION PROCESS
[230] It was also of interest to establish as to whether another methodology could be used to arrive at the composite structural / solid materials of this invention. For this purpose, a casting machine based on continuous auger with integrated vacuum for a void-free dumping was built, such a machine allowed the product ingredients to be mixed.
[231] The machine was built with a catalyst injection system, designed to enable the introduction of catalyst at the last moment of mixing of the materials noted in order to decrease the risk of premature oxidation due to the mixture of oxide and peroxide, which can accelerate catalysis and limit or prohibit curing of material. appropriate.
[232] Since the casting machine uses a central auger to mix all the ingredients, it uses smaller augers to retrieve the ingredients from separate feeders attached to the machine through smaller augers. Figure 5 provides a block diagram that describes a built-in protocol for a continuous dumping process of this invention. Step 1 of the incorporated process shows the mixture of copper oxide (cuprous oxide and / or cupric oxide) and alumina trihydrate (CuO / ATH) to obtain a uniform mixture. Step 2 of the incorporated process describes the use of small augers, which lead CuO / ATH, main batch of PET and resin to the central auger. According to this aspect, the main batch of PET contains polymeric resin, cuprous oxide, cupric oxide or a combination of the same is prepared as described in the PCTnoWO International Order Publication 2006/100665 (incorporated entirely in this document for reference) and pigment can be added to it. Materials are mixed and extruded at a high temperature to produce main batch pellets, from which the concentration of copper oxide is checked. Step 3 of the embedded process describes the mixture of all materials transmitted to the central auger. Such mixing may, in some embodiments, be conducted under a vacuum and / or under pressure. Step 4 of the embedded process describes the extrusion / pouring of the blended composition and molding / casting in appropriate solid forms. In some embodied aspects, such dumping may include casting, hard surface curing, for example, in a batch process, cutting, finishing and polishing the materials produced in this way, etc. Quality control checks for composition and color can be conducted as well.
[233] In some respects, the built-in protocol may make use of three smaller augers that feed the larger central mix auger. A small auger for Alumina Trihydrate, a small auger for mixed PET oxide batch pellets with a size range of 100 microns to 600 microns and a small auger for cuprous oxide.
[234] As a result of the fine micron size of the cuprous oxide and its self-agglutinating nature, when the cuprous oxide powder was placed in the auger system without taking into account the mixing order of the added components, the powder did not flow uniformly within of the auger system and even when it ran, it was brought unevenly in the auger that produces an uneven inhomogeneous mixture. In addition, color distribution problems were identified, as the oxide did not mix evenly and instead aggregated with itself, which resulted in lumpy areas of oxide and marking on the finished product and uneven distribution of the active components of the technology. In summary, it was found that the oxide would not disperse again on its own and resulted in a defective product.
[235] When cuprous oxide at a micron size of between 0.1 micron to 20 microns was mixed with Alumina Trihydrate with a micron size of 12 to 20 microns, the resulting mixture was stabilized not only in terms of Oxide delivery Cuprous through the augers, but the resulting product showed a uniform dispersion of the cuprous oxide material in the mold and in the final product. The pre-mixing method of Alumina Trihydrate (ATH) / Copper Oxide (OXIDE) used horizontal drum mixing, blade mixing or ribbon mixing for thirty to forty minutes. When less than thirty minutes of mixing was conducted, uniform mixing did not occur.
[236] The mixed ATH / OXIDE allowed an ideal uniform distribution both in terms of aesthetics (for example, in terms of coloring) and the antimicrobial efficacy throughout the dumped slide. (This merged ratio can be anywhere from 20: 1 ATH to OXIDE and up to 1: 2 ATH to OXIDE).
[237] Consequently, a blending process was used to mix the copper oxide and ATH to produce a uniform and stable mixture in which the copper oxide bound to the ATH, such a mixture then traveled through a auger from a smaller designated feeder to a central mixing auger inside a continuous casting machine.
[238] The small auger successfully moved the blended mixture on top of the loaded ATH / OXIDE feeder to the main mixing feeder of the casting machine where it was combined with the main batch of PET as described above in this document, polyester MMA with a range of 10% to 50% by weight and catalyst with a range of 0.02 to 4% under vacuum. The mixture was then subjected to casting molding. The resulting product yielded a uniform composite sheet with a homogeneous distribution of the active copper oxide component, which exhibited antimicrobial efficacy.
[239] Figures 4A, 4B, 4C and 4D represent a series of scanning electron micrographs, showing the substantially uniform distribution of copper particles throughout a solid composite material incorporated into this invention. Figures 4A and 4B show representative images of a top surface of the solid composite material of this invention and Figures 4C and 4D show representative images of a bottom surface of a solid composite material of this invention.
[240] EDS or energy dispersive spectroscopy, is a procedure coupled with scanning electron microscopy (SEM), in which the scattered electrons of the SEM are collected and analyzed by means of a detector, which facilitates the determination of the composition of the analyzed sample by SEM.
[241] Figure 4E provides EDS results, which confirm that the particles in the micrographs are copper particles, in examples prepared through the continuous dumping process.
[242] Mixing cuprous oxide with a polyester paste in a ratio of 100: 1 to 4: 1 (oxide paste) facilitated the mixing of cuprous oxide into a stable and uniform paste that could be pumped into the main auger of the machine continuous casting from a separate small mixer.

权利要求:
Claims (3)
[0001]
1. Method for imparting antimicrobial activity to a composite structural solid material, said method comprising a continuous pouring process for the manufacture of a structural solid composite material characterized by comprising a thermoset resin and copper oxide particles substantially uniformly dispersed in the process comprising the steps of: -mixing a charge of trihydrated alumina with copper oxide until well mixed to form a charge-copper oxide mixture; subsequently mixing said charge-copper oxide mixture with a thermosetting resin and optionally a pigment to form a combined composition containing copper oxide; - subsequently mixing a methyl ethyl ketone peroxide catalyst with said mixed composition containing copper oxide to form a polymerizable composite structural material; -distributing said structural composite material polymerizable in a mold; and -providing conditions for the polymerization of said polymerizable composite structural material, thus preparing a solid composite structural material in which copper oxide is present in a concentration ranging from 15% to 50% w / w in which a portion of said oxide particles copper is exposed to the surface.
[0002]
2. Method according to claim 1, characterized by the fact that said copper oxide particle has a size ranging from 5 to 20 microns.
[0003]
Method according to claim 1, characterized in that it further comprises the step of melting said mixture of polymeric resin containing copper oxide powder and catalyst in a slide, or additionally comprising the step of melting said mixture of polymeric resin containing copper oxide powder and catalyst using a compression molding process, or additionally comprises the step of melting said polymer resin mixture containing copper oxide powder and catalyst using an extrusion process, or additionally comprises the melting step said polymeric resin mixture containing copper oxide powder and catalyst using an injection molding process.

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JP2015525840A|2015-09-07|

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US20150320035A1|2015-11-12|

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CL2015000292A1|2015-10-23|

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US20200154701A1|2020-05-21|

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AU2013299616B2|2016-09-15|

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JP2020097885A|2020-06-25|

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IL269797D0|2019-11-28|

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IL237134A|2019-10-31|

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WO2014025949A2|2014-02-13|

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CA2881094C|2019-01-22|

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US11252958B2|2022-02-22|

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ES2894756T3|2022-02-15|

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IL237134D0|2015-03-31|

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JP6800583B2|2020-12-16|

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CA2881094A1|2014-02-13|

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CN104797137A|2015-07-22|

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EP2882295A4|2016-04-13|

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CN110915814A|2020-03-27|

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WO2014025949A3|2014-06-19|

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IN2015DN01799A|2015-05-29|

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BR112015002704A2|2018-05-22|

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EP2882295A2|2015-06-17|

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KR102183853B1|2020-11-27|

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AU2013299616A1|2015-03-26|

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法律状态:
2018-06-05| B11A| Dismissal acc. art.33 of ipl - examination not requested within 36 months of filing|

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2018-06-19| B25A| Requested transfer of rights approved|Owner name: CUPRON, INC. (US) ; KENNETH GAUTHIER TRINDER II (U |

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2018-07-03| B25A| Requested transfer of rights approved|Owner name: EOS SURFACES LLC (US) ; CUPRON, INC. (US) |

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2018-10-02| B04C| Request for examination: application reinstated [chapter 4.3 patent gazette]|

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2018-10-09| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|

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2019-07-23| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|

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2020-03-31| B07A| Application suspended after technical examination (opinion) [chapter 7.1 patent gazette]|

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2020-08-25| B07A| Application suspended after technical examination (opinion) [chapter 7.1 patent gazette]|

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2020-12-08| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|

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2021-03-02| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 08/08/2013, OBSERVADAS AS CONDICOES LEGAIS. |

优先权:

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申请号 | 申请日 | 专利标题

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US201261681158P| true| 2012-08-09|2012-08-09|

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US61/681,158|2012-08-09|

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PCT/US2013/054040|WO2014025949A2|2012-08-09|2013-08-08|Antimicrobial solid surfaces and treatments and processes for preparing the same|

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