Classifications

• • 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
• • 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
  • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
  • C09D183/04—Polysiloxanes
• • 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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B82—NANOTECHNOLOGY
  • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
  • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
• • 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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B82—NANOTECHNOLOGY
  • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
  • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites

Definitions

• the present invention generally relates to nonstick cookware coverings which exhibit improved properties of hydrophobicity and high temperature resistance.
• enamel-based coatings are already known, but these do not guarantee good anti-adhesion, and require high vitrification temperatures (greater than 540 ° C.).
• Sol-gel coatings in particular those obtained by polymerization of silanes, are also known. But these do not allow to deposit a large thickness and usually faience for thicknesses of the order of 10 microns.
• their cohesion is completed only if also high temperatures are applied for long periods, for example temperatures above 400 0 C for at least thirty minutes.
• this type of coating makes it possible to envisage a range of use in temperature greater than that of PTFE-based coatings, which can be up to 600 ° C., instead of 300 ° C. at most for coatings based on PTFE). This is, however, to the detriment of anti-adhesion.
• Such coatings have the drawback of losing their hydrophobic properties after aggression which may degrade the surface of the coating, and in particular a chemical attack such as that caused by dishwashing detergents, or a mechanical aggression such as that caused by a too vigorous scrubbing of the coating with an abrasive pad, or exposure of the order of a few minutes at an extreme temperature.
• a non-stick coating obtained by sol-gel by polymerization of a composition based on at least one metal alkoxide and a colloidal metal oxide.
• the Applicant has surprisingly found that when a very small amount of silicone oil is added to such a composition, the sol-gel-formed coating from this composition is not only resistant to high temperature, but it is also able to withstand a passage of several minutes to the flame of a bunsen burner (whose temperature is above 600 0 C), and then quickly find its hydrophobic character.
• silicone oil to make sol-gel coatings from a composition based on alkoxysilane and colloidal silica.
• US patent application US 2006/0147829 describes a process for producing superhydrophobic coatings for self-cleaning surfaces, having a contact angle with water greater than 130 °.
• This method comprises a step of preparing nanoparticles (in particular silica nanoparticles) preferably having a size ranging from 1 nm to 100 nm, and a step of treating these particles with a hydrophobic agent and an additive, the hydrophobic agent being preferably based on silicon (silicone), and the additive being selected from inorganic and organic bases.
• nanoparticles may be prepared by a process of wet synthesis, and in particular by sol-gel, from precursors comprising water, a solvent, in particular an alcohol, and a metal alkoxide such as, for example, tetramethoxysilane. (TMOS) or tetraethoxysilane
• TEOS TEOS
• the nanoparticles After formation of the nanoparticles, they are mixed directly with the hydrophobic agent and the additive, and allowed to react at a temperature of between 0 and 100 ° C.
• the material thus obtained is applied on a substrate (in particular glass, plastics material, metal, ceramic or polymer or composite material) according to any technique for obtaining a coating from a liquid (by centrifugation, dipping, or by coating by brush or roller). Then, after application to the substrate, the coating is dried at a temperature between room temperature and 200 ° C.
• the coating thus obtained has a hydrophobic surface, forming an angle of contact with water of more than 130 °, or even greater than 150 °.
• US 2006/0147829 does not indicate that the sol-gel coating is in the form of a continuous film having a thickness of at least 10 ⁇ m.
• the subject of the present invention is therefore a non-stick coating having improved hydrophobic properties and resistant to high temperature, characterized in that it is in the form of a film having a thickness of at least 10 ⁇ m and consists of a sol-gel material comprising: - a matrix of at least one metal polyalkoxylate,
• the coating according to the invention is preferably free of PTFE.
• the metal polyalkoxylate has hydrophobic groups which are destroyed at high temperature during a flame.
• this disappearance of the hydrophobic character is momentary, since it is progressively compensated by the silicone oil trapped in the polyalkoxylate and whose surface migration in infinitesimal amounts favors the progressive reconstitution of the hydrophobic groups of the polyalkoxylate at the surface of the film.
• the reconstitution of the hydrophobic character is sufficient at the time of a new firing.
• the value of the static contact angle ⁇ of a drop of water deposited on the coating of the invention is of the order of 20 ° after thermal aggression type flame passage. This static contact angle value rises back to at least 75 ° C. after a process of reconstitution of the hydrophobic properties consisting of a reheating of the ambient temperature to 200 ° C. over a period of at least 5 minutes, ie ie when the utensil is ready for a new cooking.
• the silicone oil is 0.1 to 6% by weight and more preferably 0.3 to 5% by weight of the total weight of the coating (dry state). Below 0.1% by weight of silicone oil, the reconstitution of the hydrophobic groups have disappeared during a flaming (600 0 C) is smaller, the angle obtained being less than 62 °.
• the sol-gel material of the coating according to the invention comprises 0.5 to 2% by weight of silicone oil relative to the total weight of the dry coating.
• the initial static contact angle ⁇ of a drop of water deposited on such a coating is 95 °.
• This coating after a flame-type thermal attack has an angle of 20 °. After a reconstitution process comprising at least one temperature reheating step ambient at 200 0 C over a period of at least 5 minutes, the static contact angle becomes greater than 75 ° when the utensil is ready for a new cooking.
• the coating according to the invention may comprise a silicone oil or a mixture of silicone oils.
• Silicone oils that can be used in the coating according to the invention include phenyl silicones, methyl-phenyl silicones and methyl silicones. If the coating according to the invention is used to be in contact with food, a food grade silicone oil, and in particular an oil chosen from methyl-phenyl silicones and methyl silicones of food grade, will preferably be chosen. Mention may be made, for example of methylphenyl silicone oils, of the non-food oils marketed by the company Wacker under the trade name Wacker Siliconol AP150 and by the company Dow Corning under the trade name DOW CORNING 550 fluid, as well as edible oils. marketed by WACKER AROO.
• methyl silicone oils the oil sold by RHODIA under the trade name RHODIA 47 V 350, the oil from WACKER 200 fluid, or the oil from TEGO ZV 9207. , which are food grade methylsilicone oils.
• a silicone oil chosen from those mentioned above, with a molecular weight of at least 1000 g, which is non-reactive and has a viscosity of between 20 and 2000 mPa.s.
• the matrix of the coating according to the invention comprises, as metal polyalkoxylate, a polyalkoxysilane, and in particular an amorphous polyalkoxysilane, an aluminate, a titanate, a zirconate, a vanadate, or their mixtures.
• the matrix of the coating according to the invention comprises a polyalkoxysilane and / or an aluminate so as to constitute a mixed matrix.
• coating of the matrix according to the invention is grafted with one or more organic groups selected from alkyl Cl-C4 and phenyl groups. These groups are necessary to improve the hydrophobicity of the coating.
• the matrix of the coating according to the invention is grafted with one or more methyl groups, which improve the hydrophobic character of the coating without hindering the formation of the inorganic network.
• the non-stick coating according to the invention comprises at least 5% by weight, and preferably from 5 to 30% by weight relative to the total weight of the coating of at least one metal oxide. colloidal, which is preferably finely dispersed in the matrix. This metal oxide is generally in the form of aggregates, whose size is less than one micron, or even 300 or 400 nm.
• the presence of colloidal metal oxide in the matrix of the coating according to the invention makes it possible to obtain a film of sufficient thickness, namely a thickness of at least 10 ⁇ m. If the thickness of the coating is less than 10 microns, a good cohesion of the formed film is not obtained.
• the film has a thickness of between 10 and 80 ⁇ m, and better still between 30 and 70 ⁇ m so that the film thus formed is continuous, coherent and sufficient to absorb the roughness of the support.
• the preferred colloidal metal oxides are silica and alumina.
• the sol-gel material of the coating according to the invention may further comprise fillers for improving the cohesion of the formed coating film, and / or pigments, to impart color to the coating.
• the presence of fillers and / or pigments also has a beneficial effect on the hardness of the film.
• fillers that may be used in the coating according to the invention, there may be mentioned alumina, zirconia, mica, clays (such as montmorillonite, sepiolite, gypsite, kaolinite) and zirconium phosphate.
• the fillers and / or the pigments are in the form of flakes, which has the advantage of improving the hardness of the non-stick coating.
• the pigment and / or the fillers are of nanometric size, in order to improve their dispersion and their distribution in the coating, conferring on it a great regularity of performance.
• the nonstick coating according to the invention can be used for coating the interior surface of a cooking utensil, but also as: coating of plates, grills or barbecue vats, coating of electric cooking equipment (crepe makers, waffle irons, grills table, raclette, fondue, rice cookers, jammers, breadmaker tanks, blender tanks and mixing blades for this equipment), furnace walls lining (electric, gas, microwave, steam ovens), - cookware coating (spatulas, ladles, forks, spoons), coating of handles or buttons of cookware).
• the present invention also relates to a culinary article comprising a support coated with a coating according to the invention.
• the present invention relates to a culinary article having improved hydrophobic properties, comprising a support having an inner surface that can receive food and an outer face to be disposed towards the heat source, characterized in that the inner face of the support is coated with a non-stick coating according to the invention.
• the support is a hollow cap of a culinary article, having a bottom and a side wall rising from said bottom.
• the support of the culinary article according to the invention is made of a material chosen from metals, wood, glass, ceramics and plastics.
• the present invention also relates to a method of producing a coating according to the invention on a support.
• the subject of the present invention is a method for applying to one of the faces of a support at least one non-stick coating according to the invention, characterized in that it comprises the following steps: a) preparation of a aqueous composition A comprising: i) 5 to 30% by weight relative to the total weight of the aqueous composition A of at least one colloidal metal oxide, ii) 0 to 20% by weight relative to the weight of the composition A of a solvent comprising at least one alcohol, iii) 0.05 to 3% by weight relative to the total weight of said aqueous composition A of at least one silicone oil. b) preparing a solution B comprising at least one metal alkoxide precursor, which is advantageously partially combined with a Bronsted or Lewis acid.
• aqueous composition A With regard to the preparation of the aqueous composition A, it is necessary to incorporate at least 5% by weight of at least one colloidal metal oxide with respect to the total weight of the composition A to form a film having after firing a thickness at least 10 microns. If on the other hand we have more than 30% by weight relative to the weight of the composition A, it is no longer stable.
• the colloidal metal oxide of the aqueous composition A is as defined above, and preferably selected from colloidal silica and / or colloidal alumina.
• the purpose of the presence of an alcohol-based solvent is to improve the compatibility of the aqueous composition A with the solution B of metal alkoxide.
• the solvent used in the aqueous composition A of the invention is preferably an oxygenated alcoholic solvent or an ether alcohol.
• the silicone oil is present in the aqueous composition in a proportion of 0.05 to 3% by weight relative to the total weight of the composition.
• a coating according to the invention is obtained which has reconstitutable hydrophobic properties in the context of a process of culinary use.
• the silicone oil of the composition A is a food grade silicone oil defined above.
• the aqueous composition A of the invention may also comprise fillers and / or pigments, which are as defined above.
• the aqueous composition A of the invention may further comprise fumed silica, whose function is to control the viscosity of the sol-gel composition and / or the gloss of the dry coating. Regarding the preparation of the solution
• B is preferably used as a precursor metal alkoxide selected from the group consisting of:
• Mi M 2 or M 3 denoting a metal selected from Si, Zr, Ti, Sn, Al, Ce, V, Nb, Hf, Mg or Ln.
• the metal alkoxide of solution B is an alkoxysilane.
• alkoxysilanes that may be used in solution B of the process of the invention, mention may especially be made of methyltrimethoxysilane (MTMS), tetraethoxysilane (TEOS), methyltriethoxysilane (MTES) and dimethyldimethoxysilane, and mixtures thereof, the preferred alkoxysilanes being TEOS and MTMS.
• MTMS methyltrimethoxysilane
• TEOS tetraethoxysilane
• MTES methyltriethoxysilane
• dimethyldimethoxysilane and mixtures thereof
• the preferred alkoxysilanes being TEOS and MTMS.
• solution B may comprise a mixture of an alkoxylane as defined above and an aluminum alkoxide.
• the metal alkoxide precursor of the solution B is mixed with a mineral organic Lewis acid which represents 0.01 to 10% by weight of the total weight of the solution B.
• acids usable for mixing with the precursor metal alkoxide there may be mentioned in particular acetic acid, citric acid, ethyl acetoacetate, hydrochloric acid or formic acid.
• the preferred acids according to the invention are organic acids, and more particularly acetic acid and formic acid.
• compositions A and B After the preparation of the aqueous composition A and that of the precursor solution B, they are mixed together to form a sol-gel composition (A + B).
• the respective amounts of each of compositions A and B must be adjusted so that the amount of colloidal silica in the sol-gel composition is 5 to 30% by weight on a dry basis.
• the sol-gel composition (A + B) of the invention may be applied to the support by spraying or by any other method of application, such as by dipping, by pad, by brush, by roller, by spin coating or by by screen printing.
• spraying for example by means of a spray gun, has the advantage of forming a homogeneous and continuous film which, after firing, forms a continuous coating of uniform thickness and waterproof.
• drying is generally carried out, preferably at 80 ° C., for 3 minutes.
• the cooking takes place in a preferred mode at a temperature of between 220 and 280 ° C.
• the process of the invention also comprises, after the step of producing the first non-stick coating: the production of a decoration by application and then drying on at least a part of the first non-stick coating of a decorative composition comprising a thermostable binder resistant to at least 200 ° C. and an optically non-transparent or thermochromic chemical substance, and then the production a second non-stick coating by application, then drying and firing on the decoration of at least one layer of sol-gel composition according to steps a) to c) of the process of the invention.
• the method according to the invention may further comprise a step of depositing an enamel layer on the face opposite to that coated with a non-stick coating according to the invention, this step of depositing the enamel layer being carried out prior to that of the non-stick coating according to the invention.
• the method according to the invention is particularly simple to implement and can easily be envisaged without disruption of conventional manufacturing processes of cookware.
• FIG. 1 represents a schematic sectional view of a culinary article according to FIG. the invention according to a first variant embodiment
• FIG. 2 represents a diagrammatic cross-sectional view of a culinary article holder according to the invention according to a second variant embodiment
• FIG. 3 represents a diagrammatic sectional view of a culinary article holder conforming to FIG. invention according to a third variant embodiment
• FIG. 4 represents a diagrammatic cross-sectional view of a culinary article holder according to the invention according to a fourth variant embodiment
• FIG. 5 represents a schematic sectional view of a culinary article holder conforming to FIG. the invention according to a fifth variant embodiment
• FIG. 6 shows a schematic sectional view of a culinary article holder according to the invention according to a sixth embodiment.
• FIGS. 1 to 6 are identical elements shown in FIGS. 1 to 6 are identified by identical reference numerals.
• FIG. 1 shows, as an example of a culinary article according to the invention, a pan 1 comprising a support 3 in the form of a hollow cap with a bottom 34 and a side wall 35 rising to from the bottom 34, and a gripping handle 6.
• the support 3 comprises an inner face 31 can receive food, and an outer face
• the 32 to be disposed on the side of the heat source, such as a cooking plate or a burner.
• a decorative layer 4 covers the bottom coating 2 and consists of a sol-gel material comprising a matrix of at least one metal polyalkoxylate, at least 5% by weight relative to the total weight of the decoration of at least one colloidal metal oxide and at least one silicone oil. More particularly, in the variant illustrated in Figure 3, a second non-stick coating 5, said surface covers the decorative layer 4. This non-stick surface coating 5 is a non-stick coating 5 according to the invention.
• the variant illustrated in FIG. 4 differs from that illustrated in FIG. 3 in that the decoration 40 consists of a sol-gel material that does not comprise silicone oil. Indeed, the decoration 40 consists of a sol-gel material comprising a matrix of at least one metal polyalkoxylate and at least 5% by weight relative to the total weight of the decoration of at least one colloidal metal oxide.
• the variant illustrated in FIG. 5 differs from that illustrated in FIG. 4 in that the non-stick base coating 20 covering the inner surface 31 of the support 3 also does not include silicone oil. Indeed, it is a bottom coating 20 made of a sol-gel material comprising a matrix of at least one metal polyalkoxylate and at least 5% by weight relative to the total weight of the non-stick surface coating at least one colloidal metal oxide.
• the variant illustrated in FIG. 6 differs from that illustrated in FIG. 5, in that the decoration 4 consists of a sol-gel material comprising silicone oil, that is to say a layer of decoration. 4 according to that of the variant illustrated in FIG.
• the decorative layers 4, 40 may be continuous layers partially covering the base layer 2, 20, or discontinuous layers, for example in the form of dots or elementary patterns.
• the decor 4 comprises a reversible thermochromic chemical substance, said decor partially covering said non-stick coating 2.
• thermochromic chemical substance mentioned above may be chosen from those which lighten with the rise in temperature. This is the case of perylene red linked to a black pigment.
• the chemical substance can also be chosen from those which darken with temperature. This is the case of ferric oxide Fe2O3.
• the decoration may comprise at least two motifs, one of the units containing a chemical substance that clears with temperature, such as, for example, perlylene red bonded to a black pigment, and the other pattern containing a chemical substance. which darkens with the rise in temperature, for example ferric oxide Fe2O3.
• a chemical substance that clears with temperature such as, for example, perlylene red bonded to a black pigment
• the other pattern containing a chemical substance which darkens with the rise in temperature
• ferric oxide Fe2O3 for example ferric oxide
• the contrast achieved between the two pigments makes it possible to better distinguish the temperature change.
• the above chemical compounds are used in each of the patterns of the decoration (a pattern comprising Fe 2 O 3 ferric oxide and the other motif comprising perylene red associated with a black pigment)
• a very marked contrast is observed between the two. patterns from 200 0 C, that is the optimum temperature for frying or red roast.
• the bottom release coating comprises non-optically transparent fillers and / or pigments
• the surface release coating comprises neither fillers nor pigments or comprises fillers and / or pigments.
• optically transparent and the decor includes a thermostable binder resistant to minus 200 ° C and a reversible thermochromic chemical.
• Such an article has the combined advantages of being both hydrophobic, even after passing through the flame, and of being able to inform a user about the temperature of the cooking surface of a culinary article.
• the top layer of non-stick coating according to the invention is transparent, the color change of the thermochromic substance of the decor is visible through the top layer of non-stick coating.
• the color change described above allows the user to be warned both that the culinary article is hot, and therefore presents a risk of burning, and secondly that the surface of the article has reaches the correct temperature for its use.
• the outer face of the culinary article may also be coated with a non-stick coating according to the invention, pigmented or not, or a lacquer based on one or more Silicone polyester resins, or enamel, or any other flame resistant coating.
• colloidal silica in the form of 30% aqueous solution of silica, sold by the company Clariant under the trade name Klebosol,
• colloidal silica in the form of 30% aqueous solution of silica, sold by Grace Davison under the trade name Ludox,
• colloidal alumina in the form of a 5% aqueous solution marketed by DGTec.
• Zirconium phosphate (ZrP) marketed by Rhodia
• MTMS methyltrimethoxysilane
• TEOS tetraethoxysilane
• the coating is subjected to the action of materials of different hardness representing the levels of the Mohs hardness scale.
• the hardness of the coating is expressed by the highest value of the material not scratching it.
• the coating is subjected to the action of the flame of a Bunsen burner for 30 seconds, it is cooled by quenching with cold water, then the contact angle is measured.
• hydrophobicity measurement of the contact angle of a drop of water on the coating with a GBX Digidrop type goniometer.
• a first aqueous composition Al according to the invention was produced, which is shown in Table 1:
• a first aqueous control composition A3 without a silicone oil was produced. This composition is presented in Table 3:
• a first solution B1 according to the invention is produced by mixing 99.6 g of MTMS with 0.4 g of formic acid, giving a solution containing 0.4% by weight of acid in the MTMS.
• EXAMPLE 7 Preparation of a Solution B2 Based on MTMS
• a second B2 solution according to the invention is produced by mixing 59.7 g of MTMS with 0.3 g of acetic acid, giving a solution of 0.5% by weight of acid in the MTMS.
• a third solution B3 according to the invention is produced by mixing 50 g of MTMS, 9.5 g of TEOS and 0.5 g of acetic acid to give a 0.83% by weight solution of acid in the mixture of silanes.
• sol-gel composition SGL One carries out a sol-gel composition SGL according to the invention by adding 100 g of Al aqueous composition according to the invention 100 g of solution Bl. Were mixed in a planetary mixer for one hour maintaining a temperature below 60 0 C, at the end of which is obtained a sol-gel composition according to the invention which is stored at room temperature. The composition SG1 is applied 48 hours after mixing.
• EXAMPLE 10 Preparation of a sol-gel SG2 composition according to the invention
• a sol-gel composition SG2 according to the invention is produced by adding 100 g of aqueous composition A2 according to the invention to 60 g of solution B2. It is mixed in a planetary mixer for one hour while maintaining a temperature below 60 ° C., at the end of which a sol-gel composition according to the invention is obtained which is stored at room temperature. The SG2 composition is applied 48 hours after mixing.
• a sol-gel composition SGO1 according to the invention is produced by adding 100 g of aqueous composition A3 according to the invention to 100 g of solution B1. It is mixed in a planetary mixer for one hour while keeping a temperature below 60 ° C. at the end of which is obtained a sol-gel composition according to the invention which is stored at room temperature. The composition SGO1 is applied 48 hours after mixing.
• a sol-gel SG02 composition according to the invention is produced by adding 100 g of aqueous composition A4 according to the invention to 60 g of solution B2. It is mixed in a planetary mixer for one hour while maintaining a temperature below 60 ° C., at the end of which a sol-gel composition according to the invention is obtained which is stored at room temperature. The SG02 composition is applied 48 hours after mixing.
• EXAMPLE 13 Preparation of an aqueous composition SG3 according to the invention
• a sol-gel composition SG3 according to the invention is produced by adding 100 g of aqueous composition A2 according to the invention to 60 g of solution B3. It is mixed in a planetary mixer for one hour while maintaining a temperature below 60 ° C., at the end of which a sol-gel composition according to the invention is obtained which is stored at room temperature. The SG3 composition is applied 30 hours after mixing.
• Example 14 Preparation of an aqueous composition SG4 according to the invention.
• a sol-gel composition SG4 according to the invention is produced by adding 100 g of aqueous composition A5 according to the invention to 100 g of solution B2. It is mixed in a planetary mixer for one hour while maintaining a temperature below 60 ° C., at the end of which a sol-gel composition according to the invention is obtained which is stored at room temperature. The SG4 composition is applied 24 hours after mixing.
• the SG-SG sol-gel compositions of the invention as well as the control sol-gel compositions SGO1 and SG02 are summarized in Table 5 below.
• the non-stick coatings according to the invention R1 to R4 are the coatings obtained from the sol-gel compositions according to the invention SG1 to SG4 respectively.
• the control non-stick coatings RO1 and R02 are the coatings obtained from the sol-gel compositions evmeneve I oins SGO1 and SG02 respectively.
• the coatings R1 to R4 according to the invention have a hardness of between 3 and 4 Mohs, an excellent anti-adhesion (100 points in the carbonized milk test: standard NF D 21-511), and a good resistance to flame (no change of appearance after 30 seconds in direct contact with the Bunsen burner flame).
• the contact angle of a drop of water on the coatings R1 to R4 is respectively 93 and 96 ° (before passing to the flame).
• a drop in hydrophobicity is observed just after the flame has passed through the film (despite the unchanged appearance): the contact angle becomes less than 30 °. But at the end of the reconstitution process (at least 5 minutes at 200 ° C.), angles greater than 75 ° are observed for the coatings R1 to R4.
• control coatings RO1 and R02 have, for an equivalent hardness (between 3 and 4 Mohs), a low anti-adhesion (25 points in the carbonized milk test).
• the static contact angle of a drop of water on these control coatings is of the order of 73-75 ° before passing to the flame. After passing through the flame, the contact angles are smaller than those obtained with the coatings according to the invention (62-63 ° instead of 75-79 °).

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• 2007
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