WO2020101515A2 - Composition de résine polymère de revêtement, son procédé de production et procédé d'activation de la composition polymère - Google Patents

Composition de résine polymère de revêtement, son procédé de production et procédé d'activation de la composition polymère Download PDF

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WO2020101515A2
WO2020101515A2 PCT/RO2019/060001 RO2019060001W WO2020101515A2 WO 2020101515 A2 WO2020101515 A2 WO 2020101515A2 RO 2019060001 W RO2019060001 W RO 2019060001W WO 2020101515 A2 WO2020101515 A2 WO 2020101515A2
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photocatalytic
composition
resin composition
polymeric resin
zno
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WO2020101515A3 (fr
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Razvan-Catalin BUCURESTEANU
Gheorghe-Mihai STĂRUŞ
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Bucuresteanu Razvan Catalin
Starus Gheorghe Mihai
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Publication of WO2020101515A2 publication Critical patent/WO2020101515A2/fr
Publication of WO2020101515A3 publication Critical patent/WO2020101515A3/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/16—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
    • A61L2/23—Solid substances, e.g. granules, powders, blocks, tablets
    • A61L2/232—Solid substances, e.g. granules, powders, blocks, tablets layered or coated
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L9/00—Disinfection, sterilisation or deodorisation of air
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D21/00—Separation of suspended solid particles from liquids by sedimentation
    • B01D21/02—Settling tanks with single outlets for the separated liquid
    • B01D21/04—Settling tanks with single outlets for the separated liquid with moving scrapers
    • B01D21/06—Settling tanks with single outlets for the separated liquid with moving scrapers with rotating scrapers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/015—Biocides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances

Definitions

  • the present invention refers to a coating polymeric resin composition with biocidal photocatalytic properties and to a process for producing thereof, and to a method of activating the polymeric composition.
  • Fagan shows that Ti0 2 singly or doped with Ag, or Au, Cu, Ni has excellent photocatalytic bactericidal properties and explains the biocidal photocatalytic action mechanism of Ti0 2 [Fagan, R. et al., (2015) A review of solar and visible light active Ti0 2 photocatalysis for treating bacteria, cyanotoxins and contaminants of emerging concern, Materials Science in Semiconductor Processing, vol.42, pp. 2-14].
  • DE202015000762U it is described a model of universal panel for lamps covered with T1O2 and having a function of odour neutralization and a function of hygiene.
  • the disadvantage of this invention is given by the dopant that fails to reduce the energy of the forbidden band sufficiently enough for the metal oxide to be excited by light radiation from the visible spectral range.
  • the patent US2006/0116279 discloses a method of preparing a composite based on semiconductor metal oxides such as titanium dioxide which is mixed with an inorganic material such as silica or a Bronsted acid salt, preferably phosphate.
  • the composite particles are produced by dry mixing under specific conditions determined by selecting suitable parameters.
  • the major disadvantage of this technique is that, in order to activate the photosensitizer, it is necessary to radiate with light from the UV-A domain, which exists in small quantities in the light radiation.
  • the pigment in the process of processing the resins, the pigment must not influence the chemical reaction or the physico-chemical properties of the finished product.
  • the pigments proposed in the state of art have a strong polar character and may block the polymerization reaction or lead the reaction to other undesirable products.
  • the biocidal photocatalytic polymeric resin composition in which a photosensitizing agent based on doped Ti0 2 or doped ZnO type metallic oxide is firstly dispersed, and the biocidal photocatalytic polymeric resin, thus prepared, is used for the protection of Floor surfaces, walls, ceilings from precincts with high requirements for microbial hygiene and disinfection, or for protecting and covering the surfaces of products and accesories made of metal, solid or laminated wood, plastics, glass or carbon fibers used in areas susceptible to microbial contamination; protection and coating which is carried out either by direct deposition of polymeric resin on the surface of the objects to be protected, or the resin is incorporated in the polymeric solutions used to make the coatings for hygienic protection of the spaces with special hygienic requirements.
  • this biocidal photocatalytic polymeric resin composition is made of either polymeric resin of the epoxy resin type, or polyurethane, vinyl, polyester, acrylic or hybrid epoxy-ester resin or epoxy vinyl, or resins for thermosetting plastic wares such as methyl polymeth acrylate, acryl-butadiene-styrene, polyethylene, polypropylene, vinyl polychloride, polyamide, polycarbonates, polytetrafluoroethylene, whereat it is added, in mass ratio based to the total mass of the composition, between 3 and 20 parts of biocidal photocatalytic agent made of semiconductor metallic oxides particles of the Ti0 2 or ZnO type, and whereat there are added, in the crystalline structure, by means of different impurification chemical processes, transition metal ions such as Ag, or Cu, Au, Ni, Fe, Cr, Co, Mn, or combinations thereof, used as dopants in proportions between 0.7 and 4.5 parts by weight, based to the total weight of the semiconductor metal oxide mass, the
  • the invention also describes a photocatalytic method of activating the doped semiconductor metallic oxide photosensitizer which is dispersed in the biocidal photocatalytic polymeric resin composition described above, an activation method that uses LED interior lighting lamps, which also emit visible spectral ranges with a wavelength of between 452 nm and 550 nm and by means of which the biocidal photocatalytic polymer resin used in areas susceptible to microbial contamination is irradiated.
  • the photocatalytic activation of the semiconductor metallic oxide doped and dispersed in the composition of the polymer biocidal photocatalytic resin is achieved.
  • the light that radiates the biocidal photocatalytic polymeric resin initiates the chemical process of photocatalysis that is generated at the level of the dispersed semiconductor metal oxide.
  • Carrying out the chemical process of photocatalysis by the method described in the present invention has disinfectant biocidal action against the microorganisms that come into contact with the biocidal photocatalytic polymeric resin.
  • composition described in the present invention provides an antimicrobial and antifungal protection and disinfection of the surfaces of floors, walls, ceilings in the precincts with high hygienic requirements, as well as a disinfecting protection when covering surfaces of metallic, plastic or fiberglass products and accesories used in areas susceptible to microbial contamination.
  • Semiconductor metal oxides act as a photosensitizer in photocatalytic reactions.
  • the photocatalytic effect is determined by the forbidden band energy.
  • the band energy is of 3.2 eV - 3.3 eV, and it corresponds to the near ultraviolet spectral domain, with wavelengths of 360 nm - 380 nm.
  • the generation of photocatalytic chemical reactions is obtained when the semiconductor metal oxide of Ti0 2 or ZnO type is excited by the light energy equal to or greater than the bandwidth of the forbidden band.
  • the effect and mode of action in the photodynamic therapy of photosensitizers based on photochemical reactions are known. These reactions are triggered by the interaction of a photosensitive substance with light at a certain wavelength, and form reactive species of the singlet oxygen of the ROS type (type O2 1 D 9 1 +
  • the disinfectant action of the semiconductor metallic oxide photosensitizers of T1O2 or ZnO type is achieved by the occurence of this photocatalytic mechanism, triggered by the interaction of the photosensitizing agent, which contains the semiconductor metallic oxides of T1O2 or ZnO type, with a light of a certain wavelength wherefrom the reactive oxygen species - oxygen singlet ROS appear, reactive species with a decisive role in the destruction of microorganisms, and conferring these reactive species a bactericidal and antifungal role.
  • ROS reactive oxygen species
  • reactive oxygen species species of reactive oxygen radicals that arise as a result of the electron transfer from the semiconductor substrate to the oxygen free molecules, which are much more reactive to the organic molecules in the cell wall structure of the microorganisms, than the molecular oxygen itself.
  • the forbidden band energy can be modified by a chemical process of impurification with metal ions, a process called chemical doping of semiconductor metallic oxide crystals.
  • chemical doping process into the crystal structure of semiconductor metallic oxide of Ti0 2 or ZnO type, transition metal ions of Ag, or Cu, Au, Ni, Fe, Cr, Co, Mn type, or combinations thereof, are introduced.
  • impurities, in the form of metal ions, introduced into the structure of metallic oxide crystal by chemical doping modify the energy of the forbidden band and shift to the visible spectrum the wavelength of the electromagnetic radiation required for the photocatalytic activation of the doped semiconductor metal oxides.
  • the electromagnetic radiation in the visible spectral domain with wavelengths of between 450 and 550 nm triggers photocatalytic chemical processes at the level of semiconductor metallic oxides of T1O2 or ZnO type, which have been chemically doped with transition metal ions such as Ag, or Cu, Au, Ni, Fe, Cr, Co, Mn type, or combinations thereof.
  • a first technical problem to be solved by the present invention is to obtain a biocidal photocatalytic polymeric resin composition based on polymeric resin of the epoxy resin type, or polyurethane, vinyl, polyester, acryl or hybrid epoxy-ester resin or epoxy vinyl, or resins for thermosetting plastic wares such as methyl poly methacrylate, acryl-butadiene- styrene, polyethylene, polypropylene, vinyl polychloride, polyamide, polycarbonates, polytetrafluoroethylene, and wherein it is dispersed, in mass ratio, based to the total mass of the composition, between 3 and 20 parts by weight, based on the total weight of a biocidal photocatalytic agent made up of semiconductor metal oxide particles of Ti02 or ZnO type, and in the crystalline structure of these metallic oxides, transitional metal ions such as Ag are introduced by means different impurification chemical processes; transition metal ions such as Ag or Cu, Au, Ni, Fe, Cr, Co, Mn, or combinations thereof, used as dopants
  • the doped semiconductor metal oxides are incorporated into the resin mass by mixing. After homogenization, the polymeric resin composition is either applied by direct deposition of the protective polymeric resin layer on the surface of the objects to be protected, or the polymeric resin is incorporated into the polymeric solutions used to make the coatings for the hygienic protection of the surfaces from spaces with special hygienic demands. In photocatalytic reactions, the semiconductor metal oxides of the T1O2 or ZnO type act as photosensitizers.
  • the polymeric resin described in the present invention has a photocatalytic function due to the fact that the semiconductor metal oxide of doped T1O2 or doped ZnO was dispersed in its mass.
  • the wavelength of the electromagnetic radiation which triggers photocatalytic chemical reactions upon irradiation of the semiconductor metal oxides in the biocidal photocatalytic resin composition, is given by the forbidden band energy.
  • the forbidden band energy is equivalent to the irradiation of these oxides with the electromagnetic radiation emitted in the ultraviolet spectral domain with lengths of 360nm - 380nm.
  • Modification of the forbidden band energy of semiconductor oxides is obtained by introducing into the crystal structure of Ti0 2 or ZnO type semiconductor metallic oxide some transition metal atoms of the Ag, or Cu, Au, Ni, Fe, Cr, Co, Mn type, or combinations thereof. The process is known as chemical doping with metal impurities of semiconductor metal oxides.
  • the chemical doping procedure performs the shift to the spectral domain between 450nm and 550 nm of the electromagnetic radiation wavelength used to activate the photocatalytic chemical process generated by the semiconductor metallic oxides of the doped T1O2 or doped ZnO type.
  • the biocidal photocatalytic polymeric resin acquires photocatalytic properties. More exactly, when irradiating the biocidal photocatalytic polymeric resin with visible radiation in the wavelength range of between 450 nm and 550 nm, a series of photocatalytic chemical processes with biocidal disinfectant action are initiated by the photosensitizers from the resin composition on the surface of the coatings that the prepared polymeric resin has been deposited on.
  • the semiconductor metal oxides of the doped Ti0 2 or doped ZnO type are excited with an energy equal to or greater than the forbidden band energy, and photocatalytic chemical reactions occur at the photosensitizer level.
  • ROS reactive oxygen species
  • Species of reactive oxygen radicals 0 2 1 D 9 or 0 2 appear as a result of electron transfer from the semiconductor metallic oxide substrate to free molecules of the atmospheric oxygen, an energy transfer process triggered by irradiation with visible light.
  • the photochemical excitation of neutral oxygen molecules results in their transformation into ROS (Reactive oxygen species of the 0 2 1 D 9 or 0 2 type).
  • the protection and the coating is made either by direct deposition of biocidal photocatalytic polymeric resin on the surface of the objects to be protected, or the biocidal photocatalytic resin is incorporated into the polymeric solutions used to achieve the hygienic protection of the spaces with special hygienic requirements.
  • Another technical problem solved by the present invention is carrying out a photocatalytic method for the disinfection of surfaces coated with polymeric resins, method that uses light radiation in the spectral range of between 450 nm and 550 nm to activate the photosensitizer dispersed in the biocide photocatalytic polymeric resin composition, photosensitizer made from Ti0 2 doped or ZnO type doped semiconductor metal oxides. These Ti0 2 or ZnO semiconductor metal oxides were doped into their crystalline structure with transition metals such as Ag, or Cu, Au, Ni, Fe, Cr, Co, Mn, or combinations thereof, as described in the present invention.
  • the lamps used for carrying out this method provide the normal lighting of interior spaces, yet they also contain irradiation sources that emit continuous, pulsating or intermittent light in the spectral range between 450 nm and 550 nm. Electromagnetic radiation emitted by these lamps for carrying out the method has the role to excite the photocatalytic semiconductor metallic oxides dispersed in the polymeric resin composition applied to the surfaces of the objects to be protected.
  • the described method - The photocatalytic method for disinfection of surfaces coated with polymeric resins, - activates and initiates the disinfection function of the biocidal photocatalytic polymeric resin, a polymeric resin made according to the description of this invention.
  • This function is generated by the irradiation of this biocidal photocatalytic polymeric resin with photons emitted by the interior lamps, photons having wavelengths in the spectral range of between 450 nm and 550 nm.
  • a photocatalytic excitation of the semiconductor metal oxides is performed, and there are triggered photochemical processes of formation the reactive singlet oxygen species having a disinfectant role on the surface of the polymeric resin.
  • the lamps used to achieve the photocatalytic activation method of the present invention can be fixed to the ceiling of the rooms or to the side walls of the rooms, or as LED strips applied to the walls of the rooms, or as mobile lamps that illuminate according to the disinfection requirements, and they have different shapes, depending on these requirments.
  • An object of the present invention is to provide a coating polymeric resin composition with biocidal photocatalytic properties comprising: 80-97 parts by weight, given the total weight of the composition, the resin; 3-20 parts by weight, based on the total weight of the composition, a photosensitizing agent based on Ti0 2 or ZnO doped with transition metal ions selected from Ag, Cu, Au, Ni, Fe, Cr, Co, Mn, or combinations thereof, wherein the transition metal ions represent 0,7-4, 5 of the semiconductor oxide mass.
  • the resin is selected from epoxy resin, polyurethane, vinyl, polyester, acryl, hybrid epoxy-ester or epoxy vinyl, or resins for thermosetting plastic wares, preferably metal polymethacrylate, acryl-butadiene-styrene, polyethylene, polypropylene, vinyl polychloride, polyamide, polycarbonates, polytetrafluoroethylene, and the particle grain size of Ti0 2 or ZnO is between 1 and 100 micrometers, more preferably of between 10 to 50 micrometers.
  • This composition can be used to cover the surfaces of floors, walls, ceilings, metallic accesories, of products of solid or laminated wood, plastics, glass fiber or carbon fiber.
  • Activation of the biocidal photocatalytic polymeric resin composition is done by exposing the surface covered with the resin composition to a light source emitting at wavelengths of 450-550 nm.
  • the light source can be a LED source with permanent or intermittent lighting.
  • photosensitizers based on metal oxides of Ti0 2 or ZnO doped with transition metals such as Ag, or Cu, Au, Ni, Fe, Cr, Co, Mn, or combinations thereof, having particle sizes of micrometers does not require special working conditions, they are easy to handle and store, do not require protective measures to avoid possible toxic effects as in the case of using metal oxide particles of the order of nanometers.
  • the photosensitizer activation spectrum made of Ti0 2 or ZnO semiconductor metal oxides is shifted towards light waves emitted in the visible spectral domain, and the photochemical processes with disinfectant role are obtained by irradiation in the visible domain;
  • Example 1 thermoplastic and thermostable biocidal photocatalytic polymeric resin composition
  • Ti0 2 or ZnO semiconductor metal oxide with transitional metal ions is firstly performed by a wet or a sol-gel process. There may be used Ag, or Cu, Au, Ni, Fe, Cr, Co, Mn ions, or combinations thereof. Due to the electrochemical potentials of Zn and Cu ions, however, the use of doping ZnO semiconductor metal oxide with Cu (I) - Cu 2 0 monovalent oxide is preferred. To a reactor provided with a stirrer there are added 500 liters of 1 M NaOH solution wherein 200 kg of ZnO are dissolved. The solution is stirred for 15-30 minutes.
  • Ccopper oxide (I) - Cu 2 0- is added slowly, so that the mass of copper (I) - Cu + - be at a ratio of between 0,7-4, 5 parts by weight, given the total weight of the ZnO mass.
  • the pH of the final solution is adjusted to minimum 8,5-9 by the addition of 1 M NaOH solution.
  • the stirring is continued for 1 hour.
  • the excess water is decanted, dried and then burnt at a temperature of 450° C. It is then cooled slowly and the burnt mass is brought to the correponding granulation by grinding into ball mills.
  • doping agent for semiconductor metal oxide there may also be used other transitional metals in the form of salts or oxides of AgN03, FeO, Mn0 2 or Fe(N03)3.
  • the photocatalytic pigment is brought to the corresponding granulation, it is stored in storage tanks wherefrom it will be introduced into the manufacturing process.
  • a powder paint is then prepared by mixing polymers in powder form, in a mass ratio of 60-70% polymers based on epoxy, polyurethane or polyester resins or using an epoxy-polyester hybrid resin, and whereat 10-20% hardening agents, 15-20% filling agents, stabilizers and rheological agents and catalyst are added, and then the photosensitizing agent is added up to 10%, previously prepared, in the form of Ti0 2 doped or ZnO doped semiconductor metal oxide. It is homogenized and the granulation is checked.
  • the powder paint composition thus produced is applied to metal surfaces using conventional electrostatic painting technologies.
  • thermoplastic or thermosetting layer with photocatalytic properties is formed, due to the presence of pigment in the form of Ti0 2 or ZnO doped semiconductor metal oxide.
  • an embodiment of the invention in the form of an epoxy or polyester polymer resin composition as a gel coat to be applied to the outer surface of composite material objects such as glass fiber, carbon fiber etc., and forming a photocatalytic hygienic biocidal outer layer.
  • the composite objects whereon this photocatalytic gel coat was applied can be used in areas with special hygienic requirements.
  • T1O2 type semiconductor metal oxide doped with Cu (I) - CU2O monovalent copper oxide One can also use T1O2 type semiconductor metal oxide doped with Cu (I) - CU2O monovalent copper oxide.
  • a reactor provided with a stirrer there are added 500 liters of 1 M NaOH solution wherein 200 kg of Ti0 2 are dissolved. The solution is stirred for 15-30 minutes. Copper (I) - Cu 2 0 - oxide is added slowly, so that the mass of copper (I) - Cu + - be at a ratio of between 0.7 and 4.5 parts by weight, based on the total weight of the Ti0 2 mass.
  • the pH of the final solution is adjusted to a minimum of 8.5-9 by the addition of 1 M NaOH solution. It is stirred continuously for 1 hour.
  • the excess water is decanted, dried and then burnt at a temperature of 200° C. It is then cooled slowly and the burnt mass is brought to the corresponding granulation by grinding into ball mills.
  • doping agent for semiconductor metal oxide there may also be used other transitional metals in the form of salts or oxides of AgN03, FeO, Mn0 2 or Fe (N0 3 ) 3 .
  • the photocatalytic pigment is brought to the corresponding granulation, it is stored in the storage tank, wherefrom it will be introduced into the manufacturing process. It is then proceeded to the preparation of the polymer resin based composition.
  • a gel-coat composition using a base of epoxy resin or polyester resin or a mixture of epoxy-ester hybrid resin, in which a catalyst and a thixotropic agent are added to improve the flow conditions.
  • a catalyst and a thixotropic agent are added to improve the flow conditions.
  • this mass of resin there are introduced up to 10 parts by weight, based on the total weight, the photosensitized pigment based on doped T1O2 semiconductor metal oxide or doped ZnO, pigment which was prepared as above.
  • the gel coat thus prepared is used in the manufacture of composite objects based on glass fiber or carbon fiber, and forms their outer surface which provides the shine of the objects.
  • the gel coat is applied directly to the surface of the molds wherein the objects are made, from composite materials made of glass fiber, or carbon fiber, and then the layers of composite materials are added, according to the known techniques of composite material manufacturing. After drying, the molds are removed. On the surface of the composite objects a hardened resin layer is thus formed, having photocatalytic properties generated by the presence of the doped semiconductor metal oxides in the gel coat composition. When irradiating this layer with light from the visible spectrum, photochemical reactions with hygienic protection role are generated at the level of semiconductor metallic oxides.
  • an embodiment of the invention in the form of a liquid polymer resin composition of the type ENAMEL, which is applied by rolling or with a brush, and used to protect wooden surfaces (doors, windows, shutters, railings, walls, garden wooden furniture, cottages, etc.), to protect the primed metallic surfaces, the masonry surfaces used both on the outside and inside, as well as application for protection purposes on PVC surfaces, or glass fiber or carbon fiber surfaces.
  • wooden surfaces doors, windows, shutters, railings, walls, garden wooden furniture, cottages, etc.
  • PVC surfaces primed metallic surfaces
  • glass fiber or carbon fiber surfaces glass fiber or carbon fiber surfaces
  • Objects covered with this layer of enamel from biocidal photocatalytic polymer resin can be used in areas with special hygiene requirements.
  • the doping procedure of the T1O2 or ZnO semiconductor metal oxide with transitional metal ions by a wet or a sol-gel process.
  • Copper oxide (I) - CU2O - is added slowly, so that the mass of copper (I) - Cu + - be at a ratio of between 0.7 and 4.5 parts by weight, based on the total weight of the ZnO mass.
  • the pH of the final solution is adjusted to a minimum of 8.5-9 by the addition of 1 M NaOH solution.
  • the stirring is continued for 1 hour.
  • the excess water is decanted, dried and then burnt at a temperature of 450° C. It is then cooled slowly and the burnt mass is brought to the corresponding granulation by grinding into ball mills.
  • To a reactor provided with a stirrer there are added 500 liters of 1 M NaOH solution wherein 200 kg of Ti0 2 are dissolved. The solution is stirred for 15-30 minutes.
  • Copper oxide (I) - Cu 2 0 - is added slowly, so that the mass of copper (I) - Cu + - be at a ratio of between 0.7 and 4.5% by weight, based on the total weight of the Ti0 2 mass.
  • the pH of the final solution is adjusted to a minimum of 8.5-9 by the addition of 1 M NaOH solution. It is continuously stirred for 1 hour. The excess water is decanted, dried and then burnt at a temperature of 200° C. It is then cooled slowly and the burnt mass is brought to the corresponding granulation by grinding into ball mills.
  • doping agent for semiconductor metal oxide there may be used other transitional metals in the form of salts or oxides of AgN0 3 , FeO, Mn0 2 or Fe(N0 3 ) 3 .
  • the photocatalytic pigment is brought to the corresponding granulation, it is stored in storage tanks wherefrom it will be introduced into the manufacturing process. It is then proceeded to the prepararation of the polymer resin based composition.
  • an enamel liquid polymer resin composition by mixing some liquid polymers, at a mass ratio of 60-70% - based on the epoxy, polyurethane or polyester resin or using an epoxy-polyester hybrid resin, and whereat 10-20% hardeners, 15-20% fillers, a catalyst, are added and then up to 10% the photosensitized agent prepared previously as doped Ti0 2 or ZnO doped semiconductor metal oxide. Then there are added stabilizers, emulsifiers, and a thixotropic agent to improve the flow conditions and to obtain a viscous enamel liquid composition. It is homogenized and packaged. The resin composition is then applied to the pre-prepared substrate.
  • Surfaces intended to be protected wood in the form of doors, windows, shutters, railings, walls, garden furniture, cottages, etc., or metal surfaces, or masonry surfaces, or PVC, or fiberglass, or wallpaper surfaces based on fiberglass etc.
  • a polymer resin composition prepared in the form of an enamel is applied.
  • To apply the fiberglass wallpaper first the walls are cleaned and then the wallpaper is applied using an adhesive. After the adhesive has been dried, a layer of enamel in the form of a polymer resin composition, prepared as in this example, is applied to the fiberglass wallpaper.
  • a hygienic protective layer with photocatalytic properties is formed on the surface of the objects, generated by the presence of the photocatalytic pigment of T1O2 or ZnO doped semiconductor metal oxide.
  • an embodiment of the invention in the form of a biocidal photocatalytic polymeric resin composition which is applied to the upper surface of a vinyl resin flooring system used for hygienic protection in the medical field, educational field, or heavy traffic areas, presenting a risk of bacterial contamination. It is recommended to be used especially in rooms with very high humidity such as bathrooms or kitchens or in other rooms with high humidity. Vinyl coating systems provide adhesion, are waterproof and there can be mounted on both floors and walls. In order to manufacture them, it is proceeded first to carrying out the doping procedure of the semiconductor metal oxide of T1O2 or ZnO type with transitional metal ions using either a wet, or a sol-gel process.
  • the pH of the final solution is adjusted to a minimum of 8.5-9 by the addition of 1 M NaOH solution.
  • the stirring is continued for 1 hour.
  • the excess water is decanted, dried and then burnt at a temperature of 200° C. It is then cooled slowly and the burnt mass is brought to the corresponding granulation by grinding into ball mills.
  • doping agent for semiconductor metal oxide there may be used other transitional metals in the form of salts or oxides of AgN0 3 , FeO, MnC>2 or Fe (N0 3 ) 3 .
  • the photocatalytic pigment is brought to the corresponding granulation, it is stored in storage tanks wherefrom it will be introduced into the manufacturing process. Thereafter the manufacture the vinyl coating systems by means of the existing technologies proceeds.
  • Vinyl resin flooring systems are mainly made up of different multiple layers: the base layer, which adheres to the screed, is made of a compact layer of woven glass fiber impregnated with vinyl resin, a layer that provides the strength of the product and over which another layer of polyurethane foam can be casted, providing the thermal and sound insulation of the system. There follows another third compact layer made of woven glass fiber impregnated with vinyl resin, a layer that prevents changes in the dimensions and appearance of the floor, then a top layer of printing and providing a floor design.
  • the final wear layer which is made of an epoxy varnish or epoxy varnish mixture and vinyl resin in equal ratios, wherein it is added, by dispersion, a metallic oxide semiconductor pigment of T1O2 or ZnO doped type of between 5 and 15 parts by weight, based on the total weight of the varnish mass, and prepared according to the above recipe. Catalysts and hardeners are also added to this layer. It is very well homogenized and then applied by stretching or extrusion as the last layer of wear and protection.
  • This layer has photocatalytic properties that are due to the presence, in its structure, of T1O2 doped or ZnO doped semiconductor metal oxides. When irradiating this layer with light from the visible spectrum, photochemical reactions with hygienic protection role are generated.
  • a vinyl coating system with excellent adhesion having a hygienic, disinfectant and biocidal role.
  • This vinyl coating system manufactured as described above, can be used in the medical field, in education field, or in areas with heavy traffic and at risk of bacterial contamination. It is recommended to be used in rooms with very high humidity such as bathrooms, kitchens, because these vinyl systems are impermeable.
  • the final layer of varnish on these vinyl systems forms, on their surface, a photocatalytic protective layer with hygienic role, generated by the presence of the photocatalytic pigment of doped semiconductor metal oxide of the Ti0 2 or ZnO type.
  • an embodiment of the invention in the form of a two-component biocidal photocatalytic polymeric resin composite that is applied to the surface of floors in the medical industry, food industry, refrigeration or high-traffic areas and special requirements for maintaining hygiene, areas at risk of bacterial contamination.
  • Epoxy coating systems provide adhesion, are waterproof and provide protection against the spread of microbial germs.
  • the combined epoxy resin matrix forms a temporary barrier against rising moisture and provides a very strong and lasting support. This uniform and homogeneous intermediate layer allows overlaying with resin layers or solid resin-based system structures.
  • the procedure of doping the Ti0 2 or ZnO semiconductor metal oxide with transitional metal ions is performed by using a wet or a sol-gel process.
  • Ti0 2 type semiconductor metal oxide which is doped with Cu (I) - Cu 2 0 monovalent copper oxide.
  • the pH of the final solution is adjusted to a minimum of 8.5-9 by the addition of 1 M NaOH solution.
  • epoxy resin coatings for floor protection For some floors it is recommended to apply a self-leveling primer beforehand. After applying and drying the primer, it is proceeded to the preparation of epoxy resin coatings for floor protection.
  • the epoxy resin is mixed by homogenisation with the hardener and added up to 15% by mass the photocatalytic pigment made from doped semiconductor metal oxides of T1O2 or ZnO type, prepared as described above. It is very well homogenized, for about 30 minutes, and then it is applied on the primer by rolling or with a brush, or by spraying.
  • an industrial coating system of epoxy coating is formed, very resistant to mechanical stresses, with excellent adhesion, having a hygienic, disinfectant and biocidal role, coating system that can be used to protect the floor surfaces of the medical industry, food industry, in refrigerated spaces or in areas with heavy traffic and special requirements for maintaining hygiene, areas being at risk of bacterial contamination.
  • the coating systems of epoxy type offer adhesion, are waterproof and provide protection against the spread of microbial germs.
  • the combined epoxy resin matrix forms a temporary barrier against rising moisture.
  • the presence of photocatalytic semiconductor metallic oxide forms, on the surface of these coatings, a photocatalytic hygienic protective layer that is generated by photoexcitation of the pigment with the light radiation from the visible spectrum.
  • thermosetting or composite plastic objects prepared according to this composition can be used in areas with special hygiene requirements.
  • the doping procedure of the T1 ⁇ 2 or ZnO semiconductor metal oxide with transitional metal ions is performed by a wet or a sol-gel process. There may be used Ag, or Cu, Au, Ni, Fe, Cr, Co, Mn ions, or combinations thereof.
  • Copper oxide (I) - Cu 2 0 - is added slowly, so that the mass of copper (I) - Cu + - be at a ratio of between 0.7 and 4.5 parts by weight, based on the total weight of the ZnO mass.
  • the pH of the final solution is adjusted to a minimum of 8.5-9 by the addition of 1 M NaOH solution.
  • the stirring is continued for 1 hour.
  • the excess water is decanted, dried and then burnt at a temperature of 450° C. It is then cooled slowly and the burnt mass is brought to the corresponding granulation by grinding into ball mills.
  • the pH of the final solution is adjusted to a minimum of 8.5-9 by the addition of 1 M NaOH solution.
  • the stirring is continued for 1 hour.
  • the excess water is decanted, dried and then burnt at a temperature of 200 ° C. It is then cooled slowly and the burnt mass is brought to the corresponding granulation by grinding into ball mills.
  • doping agent for semiconductor metal oxide there may be used other transitional metals in the form of salts or oxides of AgNC>3, FeO, Mn0 2 or Fe (N0 3 ) 3 .
  • a composition is prepared, using as raw material a resin for the manufacture of polymer-based thermosetting plastics such as methyl polymethacrylate, acryl-butadiene-styrene, polyethylene, polypropylene, vinyl polychloride, polyamide, polycarbonates, polytetrafluoroethylene, and whereat there are added catalysts, fillers, or coloured or support pigments.
  • a resin for the manufacture of polymer-based thermosetting plastics such as methyl polymethacrylate, acryl-butadiene-styrene, polyethylene, polypropylene, vinyl polychloride, polyamide, polycarbonates, polytetrafluoroethylene, and whereat there are added catalysts, fillers, or coloured or support pigments.
  • this resin mass there is introduced up to 10% by mass a photosensitized pigment, based on doped Ti0 2 semiconductor metal or doped ZnO, prepared as above.
  • the resin composition for the thermosetting plastic mass thus prepared is homogenized and granulated
  • thermosetting or composite objects manufactured according to this recipe On the surface of thermosetting or composite objects manufactured according to this recipe, a contact layer is formed, which has photocatalytic properties generated by the presence, on the surface, of the composition of doped semiconductor metal oxides. When irradiating this layer with light from the visible spectrum, photochemical reactions with hygienic protection role are generated at the level of doped semiconductor metallic oxides.
  • one or more types of photocatalytic polymeric resin composition that covers the surface of the floors, walls, ceilings is /are prepared according to the methods described above, the surface of metal, plastic or fiberglass objects and accesories used in areas susceptible to microbial contamination is also covered.
  • These biocidal photocatalytic polymeric resin compositions contain in the surface layer a photocatalytic pigment prepared from Ti0 2 or ZnO semiconductor metallic oxide, which has been doped with transitional metal ions such as Ag, or Cu, Au, Ni, Fe, Cr, Co, Mn, or combinations thereof.
  • LED lighting lamps are installed on the ceilings or on the side walls.
  • the lamps also contain sources also emitting electromagnetic radiation in the form of light quanta in the spectral range of from 450 nm to 550 nm.
  • LED lighting lamps have the function of providing the lighting requirements of the respective precincts, and also performs the irradiation with a wavelength of from 450 nm to 550 nm of the interior walls and floors of the precincts, and of the objects in said precincts, which are coated with a photocatalytic polymer resin composition prepared according to the above examples.
  • the electromagnetic radiation emitted by these lamps falls incidentally on the polymer resin composition and photocatalytically excites the pigment of Ti0 2 or ZnO doped semiconductor metal oxide, pigment which was dispersed into the resin composition.
  • photocatalytic chemical processes are triggered at the level of doped Ti0 2 or ZnO semiconductor metallic oxide pigments, and the disinfectant, bactericidal and antifungal function at the surface of this composition is initiated.
  • the generation of photocatalytic chemical processes by applying this method of photocatalytic activation, activates the occurrence of reactive oxygen species of single oxygen type ROS on the surface of the photocatalytic polymeric resin composition, reactive chemical species that destroy microorganisms.
  • a photocatalytic function o biocidal and antifungal disinfection by continuous irradition, pulsation or intermittent with light from the visible spectral wavelength of netween 450 nm to 550 nm is carried out.
  • the method of photocatalytic activation of the photocatalytic polymeric resin composition, described in the present invention is applied for the protection of surfaces exposed to microbiological risk and provides the disinfection of said surfaces, eliminating the risk of occurrence and spread of nosocomial infections.
  • the lamps used to achieve the photocatalytic activation method of the present invention can be fixed to the ceiling of the rooms or to the side walls of the precincts, or are in the form of LED strips applied to the walls of the rooms, or are mobile lamps that illuminate according to the disinfection requirements, and have different shapes, depending on the needs.

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Abstract

L'invention concerne une composition de résine polymère de revêtement ayant des propriétés photocatalytiques biocides, à base de résines en un rapport de 80 à 97 parties en poids, compte tenu du poids total de la composition, et de 3 à 20 parties en poids, compte tenu du poids total de la composition, un agent photosensibilisant à base d'oxyde de TiO 2 ou de ZnO dopé avec des ions métal de transition choisis entre Ag, Cu, Au , Ni, Fe, Cr, Co, Mn, ou des combinaisons de ceux-ci, les ions métal de transition représentant 0,7-4,5 de la masse d'oxyde semi-conducteur. L'invention concerne également un procédé photocatalytique d'activation de la composition de résine polymère, dans lequel la surface revêtue de la composition de résine est exposée à une source de lumière émettant à des longueurs d'onde de 450 à 550 nm. L'invention concerne également l'utilisation de la composition de résines polymères à propriétés photocatalytiques biocides pour revêtir les surfaces de sols, de murs, de plafonds, de produits d'accessoires métalliques, de bois massif ou stratifié, de plastiques, de fibres de verre ou de fibres de carbone.
PCT/RO2019/060001 2018-10-24 2019-10-23 Composition de résine polymère de revêtement, son procédé de production et procédé d'activation de la composition polymère WO2020101515A2 (fr)

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ROA201800828A RO134027A2 (ro) 2018-10-24 2018-10-24 Compoziţie de răşini polimerice de acoperire, cu proprietăţi fotocatalitice biocide, şi metodă fotocatalitică pentru dezinfecţia suprafeţelor acoperite cu răşini polimerice
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