WO2019098726A1 - Coating composition for heating cookware comprising spherical graphene powder and heating cookware - Google Patents

Coating composition for heating cookware comprising spherical graphene powder and heating cookware Download PDF

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Publication number
WO2019098726A1
WO2019098726A1 PCT/KR2018/014048 KR2018014048W WO2019098726A1 WO 2019098726 A1 WO2019098726 A1 WO 2019098726A1 KR 2018014048 W KR2018014048 W KR 2018014048W WO 2019098726 A1 WO2019098726 A1 WO 2019098726A1
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composition
salt
graphene oxide
cases
combination
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PCT/KR2018/014048
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English (en)
French (fr)
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Jiyoung Yoon
Hanna BAE
Jeonghan Park
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Hayoon Co., Ltd.
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Publication of WO2019098726A1 publication Critical patent/WO2019098726A1/en

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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
    • 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
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • 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
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
    • A—HUMAN NECESSITIES
    • A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
    • A47J—KITCHEN EQUIPMENT; COFFEE MILLS; SPICE MILLS; APPARATUS FOR MAKING BEVERAGES
    • A47J36/00—Parts, details or accessories of cooking-vessels
    • A47J36/02—Selection of specific materials, e.g. heavy bottoms with copper inlay or with insulating inlay
    • A47J36/025—Vessels with non-stick features, e.g. coatings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides

Definitions

  • the present invention relates to a composition comprising spherical graphene.
  • the composition can be used for coating cookware with superior heat conductivity and durability.
  • the present invention relates to a method of preparing the composition and cookware.
  • Heating cookware with conventional coatings are generally manufactured by coating a body of metal such as aluminum with a fluoroplastic (TEFLON) or ceramic coating.
  • a glaze can be applied to a metal surface for making the coating.
  • a melting ingredient can be melted by using a thermal spray apparatus with an oxygen acetylene flame and spray the same onto a metal surface using compressed air.
  • a composition comprising: a spherical graphene powder comprising a Brunauer, Emmett and Teller (BET) specific surface area of at least about 400 m 2 /g.
  • BET Brunauer, Emmett and Teller
  • the BET specific surface area of the spherical graphene powder can be about 400 m 2 /g to about 800 m 2 /g.
  • the BET specific surface area of the spherical graphene powder can be at least about 400 m 2 /g.
  • the BET specific surface area of the spherical graphene powder can be at most about 800 m 2 /g.
  • the BET specific surface area of the spherical graphene powder can be about 400 m 2 /g to about 500 m 2 /g, about 400 m 2 /g to about 600 m 2 /g, about 400 m 2 /g to about 700 m 2 /g, about 400 m 2 /g to about 800 m 2 /g, about 500 m 2 /g to about 600 m 2 /g, about 500 m 2 /g to about 700 m 2 /g, about 500 m 2 /g to about 800 m 2 /g, about 600 m 2 /g to about 700 m 2 /g, about 600 m 2 /g to about 800 m 2 /g, or about 700 m 2 /g to about 800 m 2 /g.
  • the BET specific surface area of the spherical graphene powder can be about 400 m 2 /g, about 500 m 2 /g, about 600 m 2 /g, about 700 m 2 /g, or about 800 m 2 /g.
  • the BET specific surface area is at least 20% larger than a corresponding carbon nanotube powder. In some cases, the BET specific surface area is at least 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, or 100% larger than a corresponding carbon nanotube powder. In some cases, the BET specific surface area is about 20% to about 40%, about 20% to about 60%, about 20% to about 80%, about 20% to about 100%, about 40% to about 60%, about 40% to about 80%, about 40% to about 100%, about 60% to about 80%, about 60% to about 100%, or about 80% to about 100% larger than a corresponding carbon nanotube powder. In some cases, the corresponding carbon nanotube powder have the same weight as the spherical graphene powder.
  • the spherical graphene powder comprises at least 10% (w/w) of the composition. In some cases, the spherical graphene powder comprises at least 10%, at least 20%, at least 30%, at least 40%, at least 50%, at least 60%, at least 70%, at least 80%, at least 90%, or at least 95% (w/w) of the composition. In some cases, the spherical graphene powder comprises about 20% to about 40%, about 20% to about 60%, about 20% to about 80%, about 20% to about 95%, about 40% to about 60%, about 40% to about 80%, about 40% to about 95%, about 60% to about 80%, about 60% to about 95%, or about 80% to about 95% (w/w) of the composition.
  • the composition further comprises an inorganic binder.
  • the inorganic binder comprises a silane compound, a silica sol, or both.
  • the silane compound comprises methyltrimethoxysilane, ethyltrimethoxysilane, normal propyltrimethoxysilane, phenyltrimethoxysilane, vinyltrimethoxysilane, methyltriethoxysilane, ethyltriethoxysilane, normal propyltriethoxysilane, phenyltriethoxysilane, vinyltriethoxysilane, triple fluoropropyl trimethoxysilane, tridecafluorooctyl trimethoxysilane, tetraethoxysilane, heptadecafluorodecyl trimethoxysilane, or any combination thereof.
  • the silica sol comprises a silica powder with an average particle size of 0.2 to 1.0 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.2 to 0.4 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.2 to 0.6 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.2 to 0.8 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.4 to 0.6 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.4 to 0.8 ⁇ m.
  • the silica sol comprises a silica powder with an average particle size of 0.4 to 1.0 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.6 to 0.8 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.6 to 1.0 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.8 to 1.0 ⁇ m. In some cases, the silica powder is dispersed in water.
  • the composition further comprises a solvent.
  • the solvent comprises water, an alcohol-based solvent, a Cellsolve solvent, an ester-based solvent, an aqueous solvent, a ketone-based solvent, an amine-based solvent, an amide-based solvent, a halogenated hydrocarbon solvent, an ether-based solvent, a furan-based solvent, or any combination thereof.
  • the solvent is water, N-methyl-2-pyrrolidone (NMP), N-ethyl-2-pyrrolidone (NEP), or any combination thereof.
  • the composition further comprising a metal salt.
  • the metal salt comprises a silver salt, an iron salt, a copper salt, an aluminum salt, a nickel salt, or any combination thereof.
  • the metal salt comprises an acetate salt, a carbonate salt, a chloride salt, a citrate salt, a cyanide salt, a fluoride salt, a nitrate salt, a nitrite salt, a phosphate salt, a sulfate salt, or any combination thereof.
  • the metal salt comprises silver acetate, silver carbonate, silver chloride, silver citrate, silver cyanide, silver fluoride, silver nitrate, silver nitrite, silver phosphate, silver sulfate, or any combination thereof.
  • the metal salt comprises iron acetate, iron carbonate, iron chloride, iron citrate, iron cyanide, iron fluoride, iron nitrate, iron nitrite, iron phosphate, iron sulfate, or any combination thereof.
  • the metal salt comprises copper acetate, copper carbonate, copper chloride, copper citrate, copper cyanide, copper fluoride, copper nitrate, copper nitrite, copper phosphate, copper sulfate, or any combination thereof.
  • the metal salt comprises aluminum acetate, aluminum carbonate, aluminum chloride, aluminum citrate, aluminum cyanide, aluminum fluoride, aluminum nitrate, aluminum nitrite, aluminum phosphate, aluminum sulfate, or any combination thereof.
  • the metal salt comprises nickel acetate, nickel carbonate, nickel chloride, nickel citrate, nickel cyanide, nickel fluoride, nickel nitrate, nickel nitrite, nickel phosphate, nickel sulfate, or any combination thereof.
  • the metal salt comprises aluminum nitrate, copper nitrate, or any combination thereof.
  • the composition further comprises graphene oxide.
  • the metal salt and graphene oxide has a weight ratio (metal salt : graphene oxide) of at least about 1:1.
  • the metal salt and graphene oxide has a weight ratio of at least about 1:1, 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, 11:1, 12:1, 13:1, 14:1, 15:1, 16:1, 17:1, 18:1, 19:1, or 20:1.
  • the weight ratio is about 1:1 to about 2:1, about 1:1 to about 4:1, about 1:1 to about 6:1, about 1:1 to about 8:1, about 1:1 to about 10:1, about 1:1 to about 15:1, about 1:1 to about 20:1, about 2:1 to about 4:1, about 2:1 to about 6:1, about 2:1 to about 8:1, about 2:1 to about 10:1, about 2:1 to about 15:1, about 2:1 to about 20:1, about 4:1 to about 6:1, about 4:1 to about 8:1, about 4:1 to about 10:1, about 4:1 to about 15:1, about 4:1 to about 20:1, about 6:1 to about 8:1, about 6:1 to about 10:1, about 6:1 to about 15:1, about 6:1 to about 20:1, about 8:1 to about 10:1, about 8:1 to about 15:1, about 8:1 to about 20:1, about 10:1 to about 15:1, about 10:1 to about 20:1, or about 15:1 to about 20:1. In some cases, the weight ratio is about 1:1, about 2:1, about 4:1, about 6:1, about 8:1, about 10:1, about 15:1,
  • the composition further comprises a linear or sheet carbon material.
  • the linear or sheet carbon material comprises sheet graphene, graphite, carbon nanotubes, or any combination thereof.
  • the spherical graphene powder and the linear or sheet carbon material has a weight ratio (spherical graphene powder : linear or sheet carbon material) of about 1:9 to about 9:1. In some cases, the weight ratio is about 1:9 to about 1:3, about 1:6 to about 1:1, 1:3 to about 3:1, about 1:1 to about 1:6, about 3:1 to about 9:1, about 6:1 to about 9:1. In some cases, the spherical graphene powder and the linear or sheet carbon material has a weight ratio of about 4:6 to about 6:4.
  • the composition further comprises an additive.
  • the additive comprises an antimicrobial agent, an anticorrosive agent, a filler, a pigment, or any combination thereof.
  • the composition is a coating composition.
  • a cookware comprising a heating cookware main body, and a cured product of any composition disclosed herein formed on the heating cookware main body.
  • the cookware comprises a frying pan, a saucepan, a pot, a kettle, or a grill.
  • the heating cookware main body comprises iron, steel, stainless steel, copper, aluminum, ceramic, or any combination thereof.
  • a method for preparing a compositing comprising: (i) dispersing graphene oxide in a solvent to form a graphene oxide dispersion; (ii) drying the graphene oxide dispersion to obtain a spherical graphene oxide powder; and (iii) reducing the spherical graphene oxide powder to form the compositing.
  • the method further comprises oxidizing graphite to form the graphene oxide. In some cases, the method further comprises oxidizing graphite using the Hummers method or the modified Hummers method.
  • the solvent comprises water, an alcohol-based solvent, a Cellsolve solvent, an ester-based solvent, an aqueous solvent, a ketone-based solvent, an amine-based solvent, an amide-based solvent, a halogenated hydrocarbon solvent, an ether-based solvent, a furan-based solvent, or any combination thereof. In some cases, the solvent is water, N-methyl-2-pyrrolidone (NMP), N-ethyl-2-pyrrolidone (NEP), or any combination thereof.
  • NMP N-methyl-2-pyrrolidone
  • NEP N-ethyl-2-pyrrolidone
  • the method further comprises mixing a metal salt with the graphene oxide dispersion.
  • the metal salt comprises a silver salt, an iron salt, a copper salt, an aluminum salt, a nickel salt, or any combination thereof.
  • the metal salt comprises an acetate salt, a carbonate salt, a chloride salt, a citrate salt, a cyanide salt, a fluoride salt, a nitrate salt, a nitrite salt, a phosphate salt, a sulfate salt, or any combination thereof.
  • the metal salt comprises silver acetate, silver carbonate, silver chloride, silver citrate, silver cyanide, silver fluoride, silver nitrate, silver nitrite, silver phosphate, silver sulfate, or any combination thereof.
  • the metal salt comprises iron acetate, iron carbonate, iron chloride, iron citrate, iron cyanide, iron fluoride, iron nitrate, iron nitrite, iron phosphate, iron sulfate, or any combination thereof.
  • the metal salt comprises copper acetate, copper carbonate, copper chloride, copper citrate, copper cyanide, copper fluoride, copper nitrate, copper nitrite, copper phosphate, copper sulfate, or any combination thereof.
  • the metal salt comprises aluminum acetate, aluminum carbonate, aluminum chloride, aluminum citrate, aluminum cyanide, aluminum fluoride, aluminum nitrate, aluminum nitrite, aluminum phosphate, aluminum sulfate, or any combination thereof.
  • the metal salt comprises nickel acetate, nickel carbonate, nickel chloride, nickel citrate, nickel cyanide, nickel fluoride, nickel nitrate, nickel nitrite, nickel phosphate, nickel sulfate, or any combination thereof.
  • the metal salt comprises aluminum nitrate, copper nitrate, or any combination thereof.
  • the metal salt and graphene oxide has a weight ratio (metal salt : graphene oxide) of at least about 1:1.
  • the metal salt and graphene oxide has a weight ratio of at least about 1:1, 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, 11:1, 12:1, 13:1, 14:1, 15:1, 16:1, 17:1, 18:1, 19:1, or 20:1.
  • the weight ratio is about 1:1 to about 2:1, about 1:1 to about 4:1, about 1:1 to about 6:1, about 1:1 to about 8:1, about 1:1 to about 10:1, about 1:1 to about 15:1, about 1:1 to about 20:1, about 2:1 to about 4:1, about 2:1 to about 6:1, about 2:1 to about 8:1, about 2:1 to about 10:1, about 2:1 to about 15:1, about 2:1 to about 20:1, about 4:1 to about 6:1, about 4:1 to about 8:1, about 4:1 to about 10:1, about 4:1 to about 15:1, about 4:1 to about 20:1, about 6:1 to about 8:1, about 6:1 to about 10:1, about 6:1 to about 15:1, about 6:1 to about 20:1, about 8:1 to about 10:1, about 8:1 to about 15:1, about 8:1 to about 20:1, about 10:1 to about 15:1, about 10:1 to about 20:1, or about 15:1 to about 20:1. In some cases, the weight ratio is about 1:1, about 2:1, about 4:1, about 6:1, about 8:1, about 10:1, about 15:1,
  • the method further comprises adding an inorganic binder to the graphene oxide dispersion.
  • the inorganic binder comprises a silane compound, a silica sol, or both.
  • the silane compound comprises methyltrimethoxysilane, ethyltrimethoxysilane, normal propyltrimethoxysilane, phenyltrimethoxysilane, vinyltrimethoxysilane, methyltriethoxysilane, ethyltriethoxysilane, normal propyltriethoxysilane, phenyltriethoxysilane, vinyltriethoxysilane, triple fluoropropyl trimethoxysilane, tridecafluorooctyl trimethoxysilane, tetraethoxysilane, heptadecafluorodecyl trimethoxysilane, or any combination thereof.
  • the silica sol comprises a silica powder with an average particle size of 0.2 to 1.0 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.2 to 0.4 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.2 to 0.6 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.2 to 0.8 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.4 to 0.6 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.4 to 0.8 ⁇ m.
  • the silica sol comprises a silica powder with an average particle size of 0.4 to 1.0 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.6 to 0.8 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.6 to 1.0 ⁇ m. In some cases, the silica sol comprises a silica powder with an average particle size of 0.8 to 1.0 ⁇ m. In some cases, the silica powder is dispersed in water. In some cases, the silica powder is dispersed in water.
  • the drying comprises spray drying.
  • the drying is performed with an inlet temperature at 100 to 150 °C, an outlet temperature at 50 to 70 °C, a feed rate at 25 to 30 Hz, or any combination thereof.
  • the drying is performed with an inlet temperature of about 100 °C to about 150 °C.
  • the drying is performed with an inlet temperature of at least about 100 °C.
  • the drying is performed with an inlet temperature of at most about 150 °C.
  • the drying is performed with an inlet temperature of about 100 °C to about 110 °C, about 100 °C to about 120 °C, about 100 °C to about 130 °C, about 100 °C to about 140 °C, about 100 °C to about 150 °C, about 110 °C to about 120 °C, about 110 °C to about 130 °C, about 110 °C to about 140 °C, about 110 °C to about 150 °C, about 120 °C to about 130 °C, about 120 °C to about 140 °C, about 120 °C to about 150 °C, about 130 °C to about 140 °C, about 130 °C to about 150 °C, or about 140 °C to about 150 °C.
  • the drying is performed with an inlet temperature of about 100 °C, about 110 °C, about 120 °C, about 130 °C, about 140 °C, or about 150 °C. In some cases, the drying is performed with an outlet temperature of about 50 °C to about 70 °C. In some cases, the drying is performed with an outlet temperature of at least about 50 °C. In some cases, the drying is performed with an outlet temperature of at most about 70 °C. In some cases, the drying is performed with an outlet temperature of about 50 °C to about 60 °C, about 50 °C to about 70 °C, or about 60 °C to about 70 °C.
  • the drying is performed with an outlet temperature of about 50 °C, about 60 °C, or about 70 °C. In some cases, the drying is performed with a feed rate of about 25 Hz to about 30 Hz. In some cases, the drying is performed with a feed rate of at least about 25 Hz. In some cases, the drying is performed with a feed rate of at most about 30 Hz.
  • the drying is performed with a feed rate of about 25 Hz to about 26 Hz, about 25 Hz to about 27 Hz, about 25 Hz to about 28 Hz, about 25 Hz to about 29 Hz, about 25 Hz to about 30 Hz, about 26 Hz to about 27 Hz, about 26 Hz to about 28 Hz, about 26 Hz to about 29 Hz, about 26 Hz to about 30 Hz, about 27 Hz to about 28 Hz, about 27 Hz to about 29 Hz, about 27 Hz to about 30 Hz, about 28 Hz to about 29 Hz, about 28 Hz to about 30 Hz, or about 29 Hz to about 30 Hz.
  • the drying is performed with a feed rate of about 25 Hz, about 26 Hz, about 27 Hz, about 28 Hz, about 29 Hz, or about 30 Hz.
  • the reducing the spherical graphene oxide powder comprises irradiating the spherical graphene oxide powder with microwave radiation. In some cases, the irradiating the spherical graphene oxide powder is performed in a reducing atmosphere. In some cases, the irradiating the spherical graphene oxide powder is carried out between 30 seconds and 3 minutes. In some cases, the irradiating the spherical graphene oxide powder is carried out in about 0.5 mins to about 3 mins. In some cases, the irradiating the spherical graphene oxide powder is carried out in at least about 0.5 mins.
  • the irradiating the spherical graphene oxide powder is carried out in at most about 3 mins. In some cases, the irradiating the spherical graphene oxide powder is carried out in about 0.5 mins to about 1 min, about 0.5 mins to about 2 mins, about 0.5 mins to about 3 mins, about 1 min to about 2 mins, about 1 min to about 3 mins, or about 2 mins to about 3 mins. In some cases, the irradiating the spherical graphene oxide powder is carried out in about 0.5 mins, about 1 min, about 2 mins, or about 3 mins. In some cases, the irradiating the spherical graphene oxide powder is carried out at an output of about 300W to 1000W, for example, 700W.
  • the method further comprises heating said spherical graphene oxide powder.
  • the heating the spherical graphene oxide powder is carried out at a temperature of about 300 °C to about 400 °C.
  • the heating the spherical graphene oxide powder is carried out at a temperature of at least about 300 °C.
  • the heating the spherical graphene oxide powder is carried out at a temperature of at most about 400 °C.
  • the heating the spherical graphene oxide powder is carried out at a temperature of about 300 °C to about 350 °C, about 300 °C to about 400 °C, or about 350 °C to about 400 °C.
  • the heating the spherical graphene oxide powder is carried out at a temperature of about 300 °C, about 350 °C, or about 400 °C. In some cases, the heating the spherical graphene oxide powder is carried out in a reducing atmosphere.
  • a method for coating a cookware comprising: (a) applying any composition disclosed herein or a composition prepared by any method disclosed herein on a cookware main body; and (b) heat curing the composition on the cookware main body.
  • the method further comprises applying a thermal conductive layer on the cookware main body.
  • the method further comprises dispersing the composition prior to applying the composition.
  • the dispersing the composition is performed using a microfluidizer.
  • the dispersing the composition is performed for about 10 mins to about 30 mins.
  • the dispersing the composition is performed for at least about 10 mins.
  • the dispersing the composition is performed for at most about 30 mins.
  • the dispersing the composition is performed for about 10 mins to about 20 mins, about 10 mins to about 30 mins, or about 20 mins to about 30 mins.
  • the dispersing the composition is performed for about 10 mins, about 20 mins, or about 30 mins.
  • the applying the composition is spray coating.
  • the method further comprising pre-heating the composition prior to applying the composition.
  • the method comprises pre-heating the composition to about 50 °C to about 70 °C.
  • the method comprises pre-heating the composition to at least about 50 °C.
  • the method comprises pre-heating the composition to at most about 70 °C.
  • the method comprises pre-heating the composition to about 50 °C to about 60 °C, about 50 °C to about 70 °C, or about 60 °C to about 70 °C.
  • the method comprises pre-heating the composition to about 50 °C, about 60 °C, or about 70 °C.In some cases, the method comprises pre-heating the composition to about 50 to 60 °C.
  • the heat curing is carried out using hot air heating, infra-red heating, or induction heating. In some cases, the heat curing is carried out for about 5 mins to about 10 mins. In some cases, the heat curing is carried out for at least about 5 mins. In some cases, the heat curing is carried out for at most about 10 mins.
  • the heat curing is carried out for about 5 mins to about 6 mins, about 5 mins to about 7 mins, about 5 mins to about 8 mins, about 5 mins to about 9 mins, about 5 mins to about 10 mins, about 6 mins to about 7 mins, about 6 mins to about 8 mins, about 6 mins to about 9 mins, about 6 mins to about 10 mins, about 7 mins to about 8 mins, about 7 mins to about 9 mins, about 7 mins to about 10 mins, about 8 mins to about 9 mins, about 8 mins to about 10 mins, or about 9 mins to about 10 mins.
  • the heat curing is carried out for about 5 mins, about 6 mins, about 7 mins, about 8 mins, about 9 mins, or about 10 mins. In some cases, the heat curing is carried out at a temperature of about 200 °C to about 280 °C. In some cases, the heat curing is carried out at a temperature of at least about 200 °C. In some cases, the heat curing is carried out at a temperature of at most about 280 °C.
  • the heat curing is carried out at a temperature of about 200 °C to about 220 °C, about 200 °C to about 240 °C, about 200 °C to about 260 °C, about 200 °C to about 280 °C, about 220 °C to about 240 °C, about 220 °C to about 260 °C, about 220 °C to about 280 °C, about 240 °C to about 260 °C, about 240 °C to about 280 °C, or about 260 °C to about 280 °C.
  • the heat curing is carried out at a temperature of about 200 °C, about 220 °C, about 240 °C, about 260 °C, or about 280 °C.
  • FIG. 1 shows scanning electron microscope (SEM) analysis results for the spherical graphene powder of Preparation Example 2 and the sheet graphene of Preparation Example 4.
  • Fig. 1A and 1B are the 500x and 2,000x magnification SEM images of the sheet graphene of Preparation Example 4, respectively, while Fig. 1C and 1D are the 500x and 2,000x magnification SEM images of the spherical graphene powder of Preparation Example 2, respectively.
  • the term “a” or “an” can refer to one or more of that entity, i.e. can refer to a plural referents. As such, the terms “a” or “an”, “one or more” and “at least one” can be used interchangeably herein.
  • reference to “an element” by the indefinite article “a” or “an” does not exclude the possibility that more than one of the elements is present, unless the context clearly requires that there is one and only one of the elements.
  • compositions comprising spherical graphene and methods for preparing the compositions.
  • the compositions can be used for coating cookware. Also disclosed herein are methods of coating a cookware using the compositions.
  • the method can comprise: (i) dispersing graphene oxide in a solvent to form a graphene oxide dispersion; (ii) drying the graphene oxide dispersion to obtain a spherical graphene oxide powder; and (iii) reducing the spherical graphene oxide powder to form a coating compositing.
  • the graphene oxide can be obtained by oxidizing graphite.
  • the method use for preparing the graphene oxide can be the Hummers method (J. A. Chem. Soc. 1958, 80, 1339) or the modified Hummers method (Chem. Mater. 1999, 11(3), 771).
  • the solvent can be water, N-methyl-2-pyrrolidone (NMP), N-ethyl-2-pyrrolidone (NEP), or any combination thereof.
  • the method can further comprise mixing a metal salt into the graphene oxide dispersion.
  • the metal salt can bind to the ends of the graphene oxide and/or act as a central point that causes the graphene oxide to clump around the metal salt, inducing aggregation in a 3-dimensional spherical shape.
  • the metal salt can be dissolved in the solvent, such as a metal nitrate salt, so that the metal salt is ionized in the solvent to take on a (+) charge and thereby attract graphene oxide having a (-) charge through electrostatic attraction.
  • the metal salt can be a silver salt, an iron salt, a copper salt, an aluminum salt, a nickel salt, or any combination thereof.
  • the metal salt can also be an acetate salt, a carbonate salt, a chloride salt, a citrate salt, a cyanide salt, a fluoride salt, a nitrate salt, a nitrite salt, a phosphate salt, a sulfate salt, or any combination thereof.
  • the metal salt can be silver acetate, silver carbonate, silver chloride, silver citrate, silver cyanide, silver fluoride, silver nitrate, silver nitrite, silver phosphate, silver sulfate, or any combination thereof.
  • the metal salt can be iron acetate, iron carbonate, iron chloride, iron citrate, iron cyanide, iron fluoride, iron nitrate, iron nitrite, iron phosphate, iron sulfate, or any combination thereof.
  • the metal salt can be copper acetate, copper carbonate, copper chloride, copper citrate, copper cyanide, copper fluoride, copper nitrate, copper nitrite, copper phosphate, copper sulfate, or any combination thereof.
  • the metal salt can be aluminum acetate, aluminum carbonate, aluminum chloride, aluminum citrate, aluminum cyanide, aluminum fluoride, aluminum nitrate, aluminum nitrite, aluminum phosphate, aluminum sulfate, or any combination thereof.
  • the metal salt can be nickel acetate, nickel carbonate, nickel chloride, nickel citrate, nickel cyanide, nickel fluoride, nickel nitrate, nickel nitrite, nickel phosphate, nickel sulfate, or any combination thereof.
  • the metal salt can be aluminum nitrate, copper nitrate, or any combination thereof.
  • the metal salt and graphene oxide can be mixed at a weight ratio of 1-20 parts of metal salt to 1 part of graphene oxide.
  • the metal salt and graphene oxide can be mixed at a weight ratio of at least about 1:1.
  • the metal salt and graphene oxide can be mixed at a weight ratio of at most about 20:1.
  • the metal salt and graphene oxide can be mixed at a weight ratio of about 1:1 to about 2:1, about 1:1 to about 4:1, about 1:1 to about 6:1, about 1:1 to about 8:1, about 1:1 to about 10:1, about 1:1 to about 15:1, about 1:1 to about 20:1, about 2:1 to about 4:1, about 2:1 to about 6:1, about 2:1 to about 8:1, about 2:1 to about 10:1, about 2:1 to about 15:1, about 2:1 to about 20:1, about 4:1 to about 6:1, about 4:1 to about 8:1, about 4:1 to about 10:1, about 4:1 to about 15:1, about 4:1 to about 20:1, about 6:1 to about 8:1, about 6:1 to about 10:1, about 6:1 to about 15:1, about 6:1 to about 20:1, about 8:1 to about 10:1, about 8:1 to about 15:1, about 8:1 to about 20:1, about 10:1 to about 15:1, about 10:1 to about 20:1, or about 15:1 to about 20:1.
  • the metal salt and graphene oxide can be mixed at a weight ratio of about 1:1, about
  • the drying can be spray drying.
  • the spray drying can be carried out using an spray drying apparatus, and may be performed with the inlet temperature at 100 to 150 °C, the outlet at 50 to 70 °C, for example 60 °C, and/or the feed rate at 25 to 30 Hz, for example 27 to 28 Hz.
  • the spherical graphene oxide powder can be reduced by irradiating with microwave radiation in a reducing atmosphere.
  • the oxygen inside the graphene oxide framework can be expelled at a fast rate, causing the adjacent carbons to bind and create a graphene structure without defects.
  • the method can form a spherical graphene powder having a high specific surface area.
  • the reducing atmosphere may be formed using hydrogen or a mixed gas of hydrogen and an inert gas.
  • the irradiation with microwaves can be carried out between 30 seconds and 3 minutes at an output of about 700W.
  • the method can further comprise a primary heat treatment process of the spherical graphene oxide powder at 300 to 400 °C.
  • the primary heat may be carried out in a reducing atmosphere.
  • the method can comprise (a) dispersing the coating composition using a microfluidizer; (b) applying the dispersed coating composition on a cookware main body, and; (c) heat curing the applied coating composition for the cookware.
  • Step (a) can further improve the thermal conductivity of a coating layer formed by the heating cookware.
  • the dispersion using a microfluidizer can be performed for about 10 minutes to about 30 minutes.
  • the dispersion using a microfluidizer can be performed for at least about 10 minutes.
  • the dispersion using a microfluidizer can be performed for at most about 30 minutes.
  • the dispersion using a microfluidizer can be performed for about 10 minutes to about 20 minutes, about 10 minutes to about 30 minutes, or about 20 minutes to about 30 minutes.
  • the dispersion using a microfluidizer can be performed for about 10 minutes, about 20 minutes, or about 30 minutes.
  • step (b) spray coating can be used as the method for applying the dispersed coating composition for the cookware.
  • step (b) spray coating can be used as the method for applying the dispersed coating composition for the cookware.
  • an additional step of pre-heating the dispersed coating composition for heating cookware may be included between step (a) and step (b).
  • the pre-heating temperature may be 50 to 60 °C.
  • the heat curing can be carried out using hot air heating, infra-red heating or induction heating methods, and/or can be carried out from 5 to 10 minutes at 200 to 280 °C.
  • compositions for coating cookware can comprise a spherical graphene powder having a Brunauer, Emmett and Teller (BET) specific surface area of at least 400 m 2 /g.
  • BET Brunauer, Emmett and Teller
  • the composition can further comprise an inorganic binder and/or a solvent.
  • BET specific surface area refers to the specific surface area determined by the BET theory.
  • the BET specific surface area can be determined by physical adsorption of a gas on the surface of the solid and by calculating the amount of adsorbate gas corresponding to a monomolecular layer on the surface. Physical adsorption can result from relatively weak forces (van der Waals forces) between the adsorbate gas molecules and the adsorbent surface area of the test powder.
  • the determination can be carried out on a BET instrument (Micromeritics Gemini 2375 and Gemini V). The determination can be performed at the boiling point of liquid nitrogen (-196°C).
  • the amount of gas adsorbed can be correlated to the total surface area of the particles including pores in the surface and can be measured by a volumetric or continuous flow procedure.
  • the BET specific surface area can be determined by nitrogen adsorption according to the ASTMD 3663-78 standard, which is based on the publication [The Journal of the American Chemical Society, 60, 309 (1938)].
  • the methods disclosed here can produce a spherical graphene powder having a specific surface area of 400 m 2 /g or greater.
  • the spherical graphene powder can have a spherical shape.
  • the spherical graphene powder can have superior vertical thermal radiation characteristics, and/or can improve the thermal conductivity of a coating layer. Further, the spherical graphene powder can increase the density of a coating layer, improve the durability (wear resistance) of the coating layer, and/or thereby extend the life of heating cookware.
  • the BET specific surface area of the spherical graphene powder can be about 400 m 2 /g to about 800 m 2 /g.
  • the BET specific surface area of the spherical graphene powder can be at least about 400 m 2 /g.
  • the BET specific surface area of the spherical graphene powder can be at most about 800 m 2 /g.
  • the BET specific surface area of the spherical graphene powder can be about 400 m 2 /g to about 500 m 2 /g, about 400 m 2 /g to about 600 m 2 /g, about 400 m 2 /g to about 700 m 2 /g, about 400 m 2 /g to about 800 m 2 /g, about 500 m 2 /g to about 600 m 2 /g, about 500 m 2 /g to about 700 m 2 /g, about 500 m 2 /g to about 800 m 2 /g, about 600 m 2 /g to about 700 m 2 /g, about 600 m 2 /g to about 800 m 2 /g, or about 700 m 2 /g to about 800 m 2 /g.
  • the BET specific surface area of the spherical graphene powder can be about 400 m 2 /g, about 500 m 2 /g, about 600 m 2 /g, about 700 m 2 /g, or about 800 m 2 /g.
  • the inorganic binder can comprise silane compound and silica sol.
  • Silane compounds can comprise methyltrimethoxysilane, ethyltrimethoxysilane, normal propyltrimethoxysilane, phenyltrimethoxysilane, vinyltrimethoxysilane, methyltriethoxysilane, ethyltriethoxysilane, normal propyltriethoxysilane, phenyltriethoxysilane, vinyltriethoxysilane, triple fluoropropyl trimethoxysilane, tridecafluorooctyl trimethoxysilane, tetraethoxysilane, heptadecafluorodecyl trimethoxysilane, or any combination thereof.
  • the composition can further comprise a metal salt.
  • the metal salt can be a silver salt, an iron salt, a copper salt, an aluminum salt, a nickel salt, or any combination thereof.
  • the metal salt can also be an acetate salt, a carbonate salt, a chloride salt, a citrate salt, a cyanide salt, a fluoride salt, a nitrate salt, a nitrite salt, a phosphate salt, a sulfate salt, or any combination thereof.
  • the metal salt can be silver acetate, silver carbonate, silver chloride, silver citrate, silver cyanide, silver fluoride, silver nitrate, silver nitrite, silver phosphate, silver sulfate, or any combination thereof.
  • the metal salt can be iron acetate, iron carbonate, iron chloride, iron citrate, iron cyanide, iron fluoride, iron nitrate, iron nitrite, iron phosphate, iron sulfate, or any combination thereof.
  • the metal salt can be copper acetate, copper carbonate, copper chloride, copper citrate, copper cyanide, copper fluoride, copper nitrate, copper nitrite, copper phosphate, copper sulfate, or any combination thereof.
  • the metal salt can be aluminum acetate, aluminum carbonate, aluminum chloride, aluminum citrate, aluminum cyanide, aluminum fluoride, aluminum nitrate, aluminum nitrite, aluminum phosphate, aluminum sulfate, or any combination thereof.
  • the metal salt can be nickel acetate, nickel carbonate, nickel chloride, nickel citrate, nickel cyanide, nickel fluoride, nickel nitrate, nickel nitrite, nickel phosphate, nickel sulfate, or any combination thereof.
  • the metal salt can be aluminum nitrate, copper nitrate, or any combination thereof.
  • the silica sol where silica (SiO 2 ) powder forms colloid particles in water, may be obtained by dispersing silica (SiO 2 ) powder with an average particle size of 0.2 to 1.0 ⁇ m in water.
  • the solvent can be, but is not limited to, alcohol-based solvents such as isopropyl alcohol, Cellosolve solvents such as butyl Cellosolve, ester-based solvents such as isopropyl acetate, aqueous solvents such as water, ketone-based solvents, amine-based solvents, amide-based solvents, halogenated hydrocarbon solvents, ether-based solvents, and furan-based solvents.
  • alcohol-based solvents such as isopropyl alcohol
  • Cellosolve solvents such as butyl Cellosolve
  • ester-based solvents such as isopropyl acetate
  • aqueous solvents such as water, ketone-based solvents, amine-based solvents, amide-based solvents, halogenated hydrocarbon solvents, ether-based solvents, and furan-based solvents.
  • the coating composition can further comprise a 1-dimensional or 2-dimensional structure carbon material having superior horizontal heat radiation characteristics, which can be linear or sheet carbon.
  • the linear or sheet carbon material can be, for example, sheet graphene, graphite, carbon nanotubes, or any combination thereof.
  • the mix ratio of the spherical graphene powder and the linear or sheet carbon material can be 10:90 to 90:10 parts by weight, preferably 40:60 to 60:40.
  • the coating composition can further comprise additives such as antimicrobial agents, anticorrosive agents, fillers, and pigments.
  • the cookware can comprise a main body, and a cured product of the coating composition formed on the main body.
  • the cookware can refer to an apparatus used for cooking with heat, specific examples including but not limited to frying pans, saucepans, pots, kettles and grills, etc.
  • the material of the heating cookware main body can be any material known to the art. Specifically, the material can be iron or steel, stainless steel, copper, aluminum, or ceramic, etc.
  • the graphene oxide obtained in Preparation Example 1 was dispersed at 10 g/L in distilled water.
  • aluminum nitrate as a metal salt was added at a ratio of 100 parts by weight per 100 parts by weight graphene oxide, and mixed by stirring for 1 hour.
  • the mixture was spray-dried with an inlet temperature of 125°C, an outlet of 60°C, and a feed rate of 27Hz to spherical graphene oxide powder.
  • the spherical graphene oxide powder was subjected to a primary heat treatment process in a rotary kiln at 350°C for 1 hour with an Ar gas mixture containing 4% H 2 , then reduced by irradiating with microwave radiation for 30 seconds to 1 minute at 700W output in a microwave reactor with an Ar gas mixture containing 4% H 2 to prepare a spherical graphene powder.
  • the graphene oxide obtained in Preparation Example 1 was dispersed at 10 g/L in distilled water.
  • the dispersion was spray-dried with an inlet temperature of 125°C, an outlet of 60°C, and a feed rate of 27 Hz to obtain spherical graphene oxide powder.
  • the spherical graphene oxide powder was subjected to a primary heat treatment process in a rotary kiln at 350°C for 1 hour with an Ar gas mixture containing 4% H 2 , then reduced by irradiating with microwave radiation for 30 seconds to 1 minute at 700W output in a microwave reactor with an Ar gas mixture containing 4% H 2 to prepare a spherical graphene powder.
  • the graphene oxide obtained in Preparation Example 1 was dispersed at 5g/L in distilled water. While stirring the dispersion, 30 parts by weight ascorbic acid was added per 100 parts by weight graphene oxide. The mixture was heated for 1 hour at 90°C. After centrifuging the reaction product for 10 minutes at 7,000 rpm, excess distilled water was used to repeatedly rinse, thereby obtaining sheet graphene.
  • 17 parts by weight isopropyl alcohol and 28 parts by weight distilled water, 22 parts by weight methyl trimethoxysilane, 16 parts by weight tetraethoxysilane, 13 parts by weight silica (SiO 2 ), 13 parts by weight butyl cellosolve and 1 part by weight of the spherical graphene powder of Preparation Example 2 were added.
  • This mixture was stirred at 300 to 600 rpm.
  • 10 parts by weight ZrO 2 and Al 2 O 3 (1:1 mixture) as a filler and 14 parts by weight TiO 2 as a pigment was added. The mixture was stirred using a bead stirrer to prepare the coating composition for the cookware.
  • preparation Embodiment 1 was repeated to prepare a coating composition for the cookware, except that 0.5 parts by weight of the spherical graphene powder of Preparation Example 2 and 0.5 parts by weight carbon nanotube were used instead of 1 part by weight of the spherical graphene powder of Preparation Example 2.
  • preparation Embodiment 1 was repeated to prepare a coating composition for the cookware, except that 0.5 parts by weight of the spherical graphene powder of Preparation Example 2 and 0.5 parts by weight graphite were used instead of 1 part by weight of the spherical graphene powder of Preparation Example 2.
  • preparation Embodiment 1 was repeated to prepare a coating composition for heating cookware, except that the spherical graphene powder of Preparation Example 3 was used instead of the spherical graphene powder of Preparation Example 2.
  • preparation Embodiment 1 was repeated to prepare a coating composition for the cookware, except that the spherical graphene powder of Preparation Example 2 was not added.
  • preparation Embodiment 1 was repeated to prepare a coating composition for heating cookware, except that the sheet graphene of Preparation Example 4 was used instead of the spherical graphene powder of Preparation Example 2.
  • Embodiment 1 Preparation of coated heating cookware
  • coating composition for heating cookware of Preparation Embodiment 1 was continuously dispersed for 30 minutes at room temperature using a microfluidizer (M-110-EH, Microfluidics).
  • the dispersed coating composition for heating cookware to 55°C, it was coated onto the surface of the main body of a frying pan (aluminum). After applying three coats to minimize air pockets in the coating, the coats were thermally cured for 10 minutes at 260°C to prepare a coated cookware.
  • Embodiment 2 Preparation of coated heating cookware
  • Embodiment 1 was repeated to prepare a coated heating cookware, except that the coating composition for heating cookware of Preparation Example 2 was used instead of the coating composition for heating cookware of Preparation Example 1.
  • Embodiment 3 Preparation of coated heating cookware
  • Embodiment 1 was repeated to prepare a coated heating cookware, except that the coating composition for heating cookware of Preparation Example 3 was used instead of the coating composition for heating cookware of Preparation Example 1.
  • Embodiment 4 Preparation of coated heating cookware
  • Embodiment 1 was repeated to prepare a coated heating cookware, except that the coating composition for heating cookware of Preparation Example 4 was used instead of the coating composition for heating cookware of Preparation Example 1.
  • Embodiment 1 was repeated to prepare a coated heating cookware, except that the coating composition for heating cookware of Comparative Preparation Example 1 was used instead of the coating composition for heating cookware of Preparation Embodiment 1.
  • Embodiment 1 was repeated to prepare a coated heating cookware, except that the coating composition for heating cookware of Comparative Preparation Example 2 was used instead of the coating composition for heating cookware of Preparation Embodiment 1.
  • the coating composition for heating cookware of Preparation Embodiment 1 was dispersed through ultrasonic treatment for 1 hour at room temperature using an ultrasonic homogenizer (Power sonic 410, Hwashin Tech).
  • the dispersed coating composition for heating cookware was coated onto the surface of the main body of a frying pan (aluminum). After applying three coats to minimize air pockets in the coating, the coats were thermally cured for 10 minutes at 260°C to prepare a coated heating cookware.
  • the coating composition for heating cookware of Preparation Embodiment 1 was dispersed for 1 hour at room temperature and 5,000 rpm using a homogenizer (L5, Silverson).
  • the dispersed coating composition for heating cookware was coated onto the surface of the main body of a frying pan (aluminum). After applying three coats to minimize air pockets in the coating, the coats were thermally cured for 10 minutes at 260°C to prepare a coated heating cookware.
  • a and b are the 500x and 2,000x magnification SEM images of the sheet graphene of Preparation Example 4, respectively, while c and d are the 500x and 2,000x magnification SEM images of the spherical graphene powder of Preparation Example 2, respectively.
  • Fig. 1 shows that whereas the sheet graphene of Preparation Example 4 has a 2-dimensional sheet shape, the spherical graphene powder of Preparation Example 2 has a 3-dimensional spherical shape.
  • thermo conductivity of the heating cookwares prepared in the above embodiments and comparative examples were measured using the method indicated below, and the results are shown in Table 2 below.
  • the durability of the heating cookwares prepared in Embodiment 1 and Comparative Example 1 was measured using the method indicated below.
  • a scrubber (AL-345, 3M) was mounted on an abrasion tester (fabricated in-house according to ASTM standards; Samyang Gear Max Geared Motor #88), and the surfaces of the coating layers of the heating cookwares were scrubbed at 60 repetitions per minute and a load of 1.8kg. After 1,000 repetitions, the scrubber was replaced with a new product.
  • the durability (wear resistance) of the heating cookware prepared in Embodiment 1 was around twice as good as that of the heating cookware prepared in Comparative Example 1.
  • the present invention has an industrial applicability, because the present invention can be applied to cookware, etc., as discussed above.
PCT/KR2018/014048 2017-11-17 2018-11-16 Coating composition for heating cookware comprising spherical graphene powder and heating cookware WO2019098726A1 (en)

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