Curing of intumescent coating compositions by pulsed infrared radiation

Abstract

The present disclosure relates to a method of imparting fire resistance to a substrate by applying an intumescent coating composition onto a surface of the substrate or forming the intumescent coating composition into a self-supporting film or sheet, irradiating with pulsed infrared radiation to form a cured intumescent coating or a cured self-supporting film or sheet, and applying the self-supporting film or sheet to a portion of a surface of the substrate. The present disclosure further relates to the use of the intumescent coating composition and the use of pulsed infrared radiation.

Description

[Technical Field]

[0001] The present disclosure relates to a method of imparting fire resistance to a substrate by applying an intumescent coating composition onto the surface of the substrate or forming the intumescent coating composition into a self-supporting film or sheet, and irradiating with pulsed infrared radiation to form a cured intumescent coating or a cured self-supporting film or sheet. The disclosure further relates to the use of the intumescent coating composition and the use of pulsed infrared radiation. [Background technology]

[0002] Intumescent coatings are widely used in various aspects of daily life and industry. They are generally applied to the surface of a substrate to change the surface's combustion characteristics, slowing the rapid spread of fire. Such coatings provide protection by forming a carbonaceous char when exposed to intense heat. Many substrates can benefit from being coated with intumescent coatings, including batteries, e.g., lithium-ion batteries, or structural building components used in commercial and transportation infrastructure, such as hotels, airports, concert halls, or offshore sites, chemical plants, and oil rigs, that are exposed to extreme heat during a fire. However, the process of curing intumescent coating compositions requires a significant amount of time and energy.

[0003] It is therefore an object of the present disclosure to provide a more efficient process for curing intumescent coatings that impart fire resistance to substrates, reducing energy consumption and processing time while maintaining the fire performance of the cured intumescent coating.

[0004] This object is solved by the subject matter defined in the appended claims. By irradiating the intumescent coating composition with pulsed infrared radiation, the cure time can be significantly reduced while maintaining the fire performance of such intumescent coatings. Summary of the Invention

[0005] The present disclosure relates to a method of imparting fire resistance to a substrate, the method comprising: (I) applying (i) an intumescent coating composition to a portion of a surface of a substrate, or (ii) forming the intumescent coating composition into a self-supporting film or sheet; (II) irradiating the (i) applied intumescent coating composition or (ii) self-supporting film or sheet with pulsed infrared radiation to form a cured intumescent coating or a cured self-supporting film or sheet; and applying the self-supporting film or sheet to a portion of a surface of the substrate.

[0006] The present disclosure also relates to substrates coated according to the methods of the present disclosure. Additionally, the present disclosure is directed to articles comprising substrates according to the present disclosure.

[0007] The present disclosure further relates to the use of an intumescent coating composition in a method of curing the intumescent coating composition by irradiating it with pulsed infrared radiation.

[0008] The present disclosure also relates to the use of pulsed infrared radiation in methods for curing intumescent coating compositions. DETAILED DESCRIPTION OF THE INVENTION

[0009] For purposes of the following detailed description, it is to be understood that the present disclosure may contemplate various alternative modifications and step sequences unless expressly specified to the contrary. Further, other than in any examples or unless otherwise indicated, all numbers expressing quantities of ingredients used in the specification and claims, for example, should be understood as being modified in all instances by the term "about." Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and appended claims are approximations that may vary depending upon the desired properties to be obtained by the present disclosure. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should be construed in light of at least the number of reported significant digits and by applying ordinary rounding techniques.

[0010] Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the disclosure are approximations, the numerical values ​​set forth in the specific examples are reported as precisely as possible. However, any numerical value inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements.

[0011] It should also be understood that any numerical range recited herein is intended to include all subranges subsumed therein. For example, a range of "1 to 10" is intended to have all subranges between (and including) the recited minimum value of 1 and the recited maximum value of 10, i.e., minimum values ​​equal to or greater than 1, and maximum values ​​equal to or less than 10.

[0012] In this application, unless otherwise specified, the use of the singular includes the plural and the plural encompasses the singular. Additionally, in this application, although "and / or" may be expressly used in certain instances, the use of "or" means "and / or" unless otherwise specified. Furthermore, in this application, the use of "a" or "an" means "at least one" unless otherwise specified. For example, "a" polymer, "a" film-forming resin, etc. refers to one or more than one of any of these items.

[0013] The present disclosure relates to a method for imparting fire resistance to a substrate, the method comprising: (I) applying (i) an intumescent coating composition to a portion of a surface of a substrate, or (ii) forming the intumescent coating composition into a self-supporting film or sheet; (II) irradiating the (i) applied intumescent coating composition or (ii) self-supporting film or sheet with pulsed infrared radiation to form a cured intumescent coating or a cured self-supporting film or sheet; and applying the self-supporting film or sheet to a portion of a surface of the substrate.

[0014] As used herein, the term "intumescent coating" refers to a coating that undergoes expansion, thus increasing in volume and decreasing in density, and charring when exposed to heat, e.g., the high temperatures experienced during a fire. As used herein, the term "self-supporting film or sheet" refers to a film or sheet that is capable of supporting itself and holding itself firmly without the support of a substrate.

[0015] According to the present disclosure, a method of imparting fire resistance to a substrate includes the steps of: (I) applying an intumescent coating composition to a portion of a surface of the substrate; and (II) irradiating the applied intumescent coating composition with pulsed infrared radiation to form a cured intumescent coating.

[0016] According to the present disclosure, the expandable coating composition may include a film-forming resin (a). As used herein, the term "film-forming resin" refers to a resin capable of forming a self-supporting, continuous film on a horizontal surface of a substrate upon removal of any diluent or carrier present in the composition, or upon curing at ambient conditions, e.g., temperatures ranging from 20 to 25°C, or at elevated temperatures, e.g., temperatures ranging from 40 to 200°C. Terms such as "resin" and "resinous" are used interchangeably with terms such as "polymer" and "polymeric." Furthermore, the term "polymer" is used herein in the sense commonly used in the art to refer to a macromolecular compound, i.e., a compound having a relatively high molecular weight (e.g., 500 Da or greater), the structure of which actually or conceptually includes multiple repeating units (also referred to as "mers") derived from relatively low molecular weight species. Unless otherwise indicated, molecular weights are given on a weight-average basis ("M w "), as determined by gel permeation chromatography using polystyrene standards.

[0017] By ambient conditions, it is meant that the composition cures without the aid of heat, for example, baking in an oven, use of forced air, or the like.

[0018] Any film-forming composition can be used in accordance with the present invention. The film-forming resin can react with itself, i.e., undergo a self-crosslinking reaction, or can react with a crosslinking agent. Therefore, the expandable coating composition can further comprise a crosslinking agent (b) suitable for crosslinking the film-forming resin (a). The crosslinking agent contains functional groups capable of reacting with the film-forming resin.

[0019] As used herein, the term "crosslinking" refers to the formation of covalent bonds between polymer chains of constituent polymer molecules. The terms "crosslinking agent," "curing agent," and "crosslinker" are used interchangeably herein. The curing or crosslinking reaction can be induced, for example, by exposing the coating composition to heat or radiation, but can also be carried out at ambient conditions to form a cured coating.

[0020] The type of film-forming resin (a) used in the expandable coating composition is not particularly limited, and any known type of resin can be used in principle. For example, the film-forming resin (a) can include an epoxy resin, an acrylic resin, a polyurethane resin, a polyvinyl resin, a urea-formaldehyde resin, a polyimide resin, a melamine resin, a polyester resin, a cyanate resin, a copolymer thereof, or a mixture thereof. According to the present disclosure, the film-forming resin can include an epoxy resin, an acrylic resin, a polyurethane resin, a copolymer thereof, or a mixture thereof. In particular, the film-forming resin can include an epoxy resin.

[0021] The film-forming resins used in accordance with the present disclosure may contain one or more functional groups that react with each other and / or with the functional groups of the crosslinker. Examples of suitable functional groups include, but are not limited to, ketone, hydrazide, carbodiimide, oxazoline, epoxy, amine, vinyl, amide, carbamate, urea, mercaptan, carboxylic acid, (meth)acryloyl, isocyanate, alkoxysilyl, anhydride, hydroxyl, alkoxy, and combinations thereof.

[0022] Suitable functional groups capable of reacting with each other include, for example, n-methylol amide groups; silane groups with silicone-bonded hydrolyzable or condensable groups, such as chloro, hydroxy, alkoxy, acetoxy, and / or ketoximo groups; azomethine groups; azetidine groups; and groups capable of thermally reversible Diels-Alder reactions, such as furan / maleimide. If the film-forming resin contains functional groups capable of reacting with each other, it is considered self-crosslinking, and the presence of a crosslinking agent is not required in the expandable coating composition.

[0023] The film-forming resin may also contain a combination of functional groups capable of self-crosslinking and functional groups reactive with the functional groups of the crosslinker. In such cases, a crosslinker may be present, and upon curing, two crosslinking mechanisms occur: a self-crosslinking reaction of the functional groups of the film-forming resin and a reaction between the functional groups of the crosslinker and the functional groups of the film-forming resin.

[0024] According to the present disclosure, the film-forming resin may include an epoxy resin. Suitable epoxy resins can be prepared in a known manner, for example, by reacting a compound containing an epoxide functional group with a cyclic co-reactant containing at least two hydroxyl groups. Examples of suitable compounds containing one epoxide functional group include, but are not limited to, glycidol, epichlorohydrin, glycidolamine, and mixtures thereof. As used herein, the terms "epoxy" and "epoxide" are used interchangeably. Examples of suitable cyclic co-reactants containing at least two hydroxyl groups include, but are not limited to, bisphenol A, hydrated bisphenol A, bisphenol F, hydrated bisphenol F, novolac resins (e.g., phenol novolac, cresol novolac), and mixtures thereof.

[0025] Epoxy resins suitable for use in the present disclosure may include polyepoxides. Polyepoxides typically have at least two 1,2-epoxy groups. The epoxy equivalent weight of the polyepoxides may range from 80 to 600, e.g., from 100 to 700. The epoxy equivalent weight may be determined by potentiometric titration according to ASTM D1652. The epoxy compounds may be saturated or unsaturated, cyclic, aliphatic, cycloaliphatic, aromatic, or heterocyclic. The epoxy compounds may include substituent(s), e.g., halogen, hydroxy, and ether groups.

[0026] Suitable polyepoxides may include, but are not limited to, polyglycidyl ethers of polyphenols, such as 2,2-bis(4-hydroxyphenyl)propane (bisphenol A), resorcinol, hydroquinone, benzenedimethanol, phloroglucinol, bisphenol F, and catechol, or polyglycidyl ethers of polyols. As used herein, the term "polyol" refers to a compound having more than one hydroxyl group per molecule, for example, two, three, four, five, six, or more than six hydroxyl groups per molecule. Suitable polyols include alicyclic polyols such as 1,2-cyclohexanediol, 1,4-cyclohexanediol, 2,2-bis(4-hydroxycyclohexyl)propane, 1,1-bis(4-hydroxycyclohexyl)ethane, 2-methyl-1,1-bis(4-hydroxycyclohexyl)propane, 2,2-bis(4-hydroxy-3-tert-butylcyclohexyl)propane, 1,3-bis(hydroxymethyl)cyclohexane, and 1,2-bis(hydroxymethyl)cyclohexane, or aliphatic polyols such as trihydroxymethylpentane, ... Examples of suitable olefin glycols include, but are not limited to, ethanediol, ethylene glycol, diethylene glycol, triethylene glycol, 1,2-propylene glycol, 1,4-butylene glycol, 1,5-pentanediol, 1,2,6-hexanetriol, cyclohexanedimethanol, glycerol, trimethylolpropane, hydrogenated bisphenol A, hydrogenated bisphenol F, or polyether glycols such as poly(oxatetramethylene) glycol, poly(oxyethylene) glycol, poly(oxypropylene) glycol, and neopentanediol.

[0027] Further suitable epoxy resins include, but are not limited to, polyglycidyl ethers of polycarboxylic acids. As used herein, the term "polycarboxylic acid" refers to a compound having more than one carboxylic acid group per molecule, for example, two, three, four, five, six, or more than six carboxylic acid groups per molecule, including the corresponding acid anhydrides. Suitable polycarboxylic acids can be formed by reacting an epoxy compound, such as epichlorohydrin, with an aliphatic or aromatic polycarboxylic acid, such as oxalic acid, succinic acid, glutaric acid, terephthalic acid, 2,6-naphthalenedicarboxylic acid, or dimerized linoleic acid. Such resins are commercially available, for example, from Hexion Inc. (USA) under the EPIKOTE and EPON lines.

[0028] Other suitable epoxy resins that can be used in accordance with the present disclosure can include epoxidized olefinically unsaturated alicyclic materials such as epoxy alicyclic ethers and esters, epoxy resins containing oxyalkylene groups, epoxy novolac resins, which are prepared by reacting an epihalohydrin with the condensation product of an aldehyde and a mono- or polyhydric phenol, such as epoxy phenol novolac resins, or epoxy cresol novolac resins.

[0029] It may be advantageous to use a flexible polyepoxide resin as the film-forming resin of the expandable coating composition. Flexible polyepoxide resins are generally essentially linear resins, although a small amount of branching is acceptable. Suitable examples of flexible polyepoxides include, but are not limited to, epoxidized soybean oil, dimer acid-based materials such as EPOL 1010 resin commercially available from BASF (Germany), and rubber-modified polyepoxide resins such as the product of a polyglycidyl ether of bisphenol A and an acid-functional polybutadiene. Other suitable examples of flexible polyepoxides include flexible acid-functional polyesters and epoxy-functional adducts prepared from polyepoxides.

[0030] The acid-functional polyester may have an acid number of at least 10 mg KOH / g, e.g., 140 to 350 mg KOH / g, or 180 to 260 mg KOH / g. The acid number may be determined according to ASTM D974. The acid-functional polyester may be prepared by polyesterification of an organic polycarboxylic acid or anhydride with an organic polyol. The polycarboxylic acid and polyol may be an aliphatic or aromatic dibasic acid and diol. Linear polyesters may be preferred over branched polyesters.

[0031] Suitable polyols that can be used to make the polyester include, but are not limited to, alkylene glycols such as ethylene glycol, diethylene glycol, neopentyl glycol, hydrogenated bisphenol A, cyclohexanediol, cyclohexanedimethanol, carpolactonediol, hydroxyalkylated bisphenols; polyether glycols such as poly(oxytetramethylene) glycol, poly(oxyethylene) glycol, poly(oxypropylene) glycol, and the like; trimethylolpropane; trimethylolethane; pentaerythritol; glycerol; isosorbide; and tetramethylcyclobutenediol. Suitable polycarboxylic acids that can be used to make the polyesters include dicarboxylic acids or anhydrides having 2 to 36 carbon atoms per molecule, such as phthalic acid, isophthalic acid, terephthalic acid, tetrahydrophthalic acid, hexahydrophthalic acid, adipic acid, azelaic acid, sebacic acid, maleic acid, glutaric acid, chlorendic acid, tetrachlorophthalic acid, tetrabromophthalic acid, decanedioic acid, dodecanedioic acid, rosin acid, diphenolic acid, gallic acid, and various types of other dicarboxylic acids (e.g., unsaturated C 18 Examples of epoxy-functional adducts include, but are not limited to, Diels-Alder adducts of fatty acids. In particular, polyesters used to make the epoxy-functional adducts can be prepared from a polycarboxylic acid component comprising a polycarboxylic acid having 7 to 16 carbon atoms and a polyol comprising diethylene glycol.

[0032] Alternatively or additionally, the film-forming resin may comprise an acrylic resin. Suitable acrylic resins may be homopolymers or copolymers, which may be obtained by polymerizing one or more monomers, including substituted or unsubstituted (meth)acrylic acids and (meth)acrylates. As used herein, the terms "(meth)acrylic acid" and "(meth)acrylate" and similar terms refer to both the acrylic acid or acrylate and the corresponding methacrylic acid or methacrylate, respectively. Suitable (meth)acrylates may include, but are not limited to, alkyl (meth)acrylates, cycloalkyl (meth)acrylates, alkylcycloalkyl (meth)acrylates, aralkyl (meth)acrylates, alkylaryl (meth)acrylates, aryl (meth)acrylates, and functional group-containing (meth)acrylates. As used herein, the term "functional group" refers to a group containing hydrogen and sp 3It refers to a group containing one or more atoms other than carbon atoms. Examples of functional groups include, but are not limited to, hydroxyl, carboxylic acid, amide, isocyanate, urethane, thiol, amino, sulfone, sulfoxide, phosphine, phosphite, phosphate, and halide. Non-limiting examples of acrylic resins include methyl (meth)acrylate, ethyl (meth)acrylate, propyl (meth)acrylate, butyl (meth)acrylate, isobutyl (meth)acrylate, 4-methyl-2-pentyl (meth)acrylate, 2-ethylhexyl (meth)acrylate, isooctyl (meth)acrylate, isobornyl (meth)acrylate, isodecyl (meth)acrylate, lauryl (meth)acrylate, tridecyl (meth)acrylate, tetradecyl (meth)acrylate, hexadecyl (meth)acrylate, octadecyl (meth)acrylate, and stearyl (meth)acrylate. and acrylic resins derived from methylphenyl (meth)acrylate, benzyl (meth)acrylate, 2-phenoxyethyl (meth)acrylate, 3,3,5-trimethyl-cyclohexyl (meth)acrylate, 3-methylphenyl (meth)acrylate, 1-naphthyl (meth)acrylate, 3-phenyl-n-propyl (meth)acrylate, 2-phenyl-aminoethyl (meth)acrylate, hydroxyethyl (meth)acrylate, hydroxypropyl (meth)acrylate, 4-hydroxybutyl (meth)acrylate, glycidyl (meth)acrylate, or combinations thereof.

[0033] Suitable acrylic resins may include epoxy-functional acrylic resins, which may be prepared by free radical addition polymerization of (meth)acrylate monomers, optionally in combination with vinyl monomers or other monomers containing carbon-carbon double bonds, wherein the monomer composition includes an epoxy-functional compound having a carbon-carbon double bond.

[0034] Suitable epoxy-functional ethylenically unsaturated monomers include, for example, glycidyl (meth)acrylate, allyl glycidyl ether, vinyl glycidyl ether, vinylcyclohexene oxide, limonene oxide, 2-ethylglycidyl acrylate, 2-ethylglycidyl methacrylate, 2-(n-propyl)glycidyl (meth)acrylate, 2-(n-butyl)glycidyl (meth)acrylate, glycidylmethyl (meth)acrylate, (3',4'-epoxyheptyl)-ethyl (meth)acrylate, 6',7'-epoxyheptyl)(meth)acrylate, p)acrylate, allyl-3,4-epoxyheptyl ether, 6,7-epoxyheptyl allyl ether, vinyl-3,4-epoxyheptyl ether, 3,4-epoxyheptyl vinyl ether, 6,7-epoxyheptyl vinyl ether, o-vinylbenzyl glycidyl ether, m-vinylbenzyl glycidyl ether, p-vinylbenzyl glycidyl ether, 3-vinylcyclohexene oxide, α-methylglycidyl methacrylate, 3,4-epoxycyclohexylmethyl (meth)acrylate, and combinations thereof.

[0035] In preparing the epoxy-functional acrylic resin, additional monomers may be used, such as ethylenically unsaturated nitrile compounds; vinyl aromatic monomers; amides of ethylenically unsaturated acids; ethylenically unsaturated sulfonic acids; ethylenically unsaturated phosphorus-containing acids; vinyl carboxylates; conjugated dienes; monomers having at least two ethylenically unsaturated groups; and combinations thereof.

[0036] Suitable examples of ethylenically unsaturated nitrile monomers include, but are not limited to, aliphatic nitrile monomers containing 2 to 4 carbon atoms in a linear or branched configuration and which may be substituted with an acetyl group, such as acrylonitrile, methacrylonitrile, α-cyanoethyl acrylonitrile, fumaronitrile, and combinations thereof, with acrylonitrile being particularly suitable.

[0037] Suitable vinyl aromatic monomers may include, but are not limited to, styrene, alpha-methylstyrene, p-methylstyrene, t-butylstyrene, and vinyltoluene.

[0038] Suitable amides of ethylenically unsaturated acids can include, but are not limited to, (meth)acrylamide, and diacetone acrylamide.

[0039] Suitable vinyl ester monomers can include, but are not limited to, vinyl acetate, vinyl propionate, vinyl butyrate, vinyl benzoate, vinyl-2-ethylhexanoate, vinyl stearate, and vinyl esters of versatic acid.

[0040] Suitable ethylenically unsaturated carboxylic acid monomers include, but are not limited to, monocarboxylic and dicarboxylic acid monomers and monoesters of dicarboxylic acids. Ethylenically unsaturated aliphatic monocarboxylic or dicarboxylic acids or anhydrides containing 3 to 5 carbon atoms are particularly suitable. Examples of monocarboxylic acid monomers include, but are not limited to, (meth)acrylic acid and crotonic acid, and examples of dicarboxylic acid monomers include, but are not limited to, fumaric acid, itaconic acid, maleic acid, and maleic anhydride. Other suitable ethylenically unsaturated acids include vinyl acetic acid, vinyl lactic acid, vinyl sulfonic acid, 2-methyl-2-propene-1-sulfonic acid, styrene sulfonic acid, acrylamidomethylpropane sulfonic acid, and salts thereof.

[0041] Suitable conjugated diene monomers include 1,3-butadiene, isoprene, 2,3-dimethyl-1,3-butadiene, 2-chloro-1,3-butadiene, 1,3-pentadiene, 1,3-hexadiene, 2,4-hexadiene, 1,3-octadiene, 2-methyl-1,3-pentadiene, 2,3-dimethyl-1,3-pentadiene, 3,4-dimethyl-1,3-hexadiene, 2,3-diethyl-1,3-butadiene, 4,5-diethyl-1,3-octadiene, 3-butyl-1,3-octadiene, 3,7-dimethyl-1,3,6-octatriene, 2-methyl-6-methylene-1,7-octadiene, 7-methyl-3-methylene-1,7-octadiene, and the like. ,6-octadiene, 1,3,7-octatriene, 2-ethyl-1,3-butadiene, 2-amyl-1,3-butadiene, 3,7-dimethyl-1,3,7-octatriene, 3,7-dimethyl-dimethyl-1,3,6-octariene, 3,7,11-trimethyl-1,3,6,10-dodecatetraene, 7,11-dimethyl-3-methylene-1,6,10-dodecatriene, 2,6-dimethyl-2,4,6-octatriene, 2-phenyl-1,3-butadiene, and 2-methyl-3-isopropyl-1,3-butadiene, 1,3-cyclohexadiene, and combinations thereof.

[0042] Alternatively or additionally, the film-forming resin may comprise a polyurethane resin. Suitable polyurethane resins may be prepared in a known manner, for example, by reacting a polyisocyanate with a polyol. As used herein, the term "polyisocyanate" refers to a compound having more than one isocyanate group per molecule, for example, two, three, four, five, six, or more than six isocyanate groups per molecule. Suitable polyisocyanates include aliphatic polyisocyanates, such as 2,2,4-trimethylhexamethylene diisocyanate, 2,4,4-trimethylhexamethylene diisocyanate, and 1,6-hexamethylene diisocyanate; alicyclic polyisocyanates, such as isophorone diisocyanate and 4,4'-methylene-bis(cyclohexylisocyanate); aromatic polyisocyanates, such as 4,4'-diphenylmethane diisocyanate, toluene diisocyanate, 1,2,4-benzene triisocyanate, tetramethylxylylene diisocyanate, and polymethylene polyphenyl isocyanate; and combinations thereof. Non-limiting examples of suitable polyols are those described above. Specifically, polyurethanes prepared by reacting a polyester polyol or an acrylic polyol with a polyisocyanate at an OH / NCO equivalent ratio greater than 1:1, resulting in the presence of free hydroxyl groups in the product, are preferred. A suitable polyurethane resin that can be used in accordance with the present disclosure can be exemplified by the reaction product of Desmodur N 3300, available from Covestro (Germany), with an alkylene glycol, such as ethylene glycol or propylene glycol.

[0043] Alternatively or additionally, the film-forming resin can comprise a polyvinyl resin.Suitable polyvinyl resins can be homopolymers or copolymers, which can be obtained by polymerizing one or more monomers, including vinyl aromatic compounds, such as styrene and vinyltoluene; nitriles, such as (meth)acrylonitrile; vinyl and vinylidene halides, such as vinyl chloride and vinylidene fluoride; and vinyl esters, such as vinyl acetate.Suitable polyvinyl resins that can be used according to the present disclosure can be exemplified by the vinyl resins under the trademark LUMIFLON™, available from AGC Chemicals Europe, Ltd. (Netherlands).

[0044] Alternatively or additionally, the film-forming resin may comprise a urea-formaldehyde resin.Suitable urea-formaldehyde resins can be prepared in a known manner, for example, by condensation of formaldehyde and urea.Suitable examples of urea-formaldehyde resins include, but are not limited to, urea-formaldehyde resins under the trademark Kaurit (registered trademark) available from BASF (Germany) and urea-formaldehyde resins under the trademark Casco (registered trademark) Resin available from Hexion Inc. (USA), such as Casco (registered trademark) Resin CR-5H.

[0045] Alternatively or additionally, the film-forming resin may comprise a polyimide resin. Suitable polyimide resins can be prepared in a known manner, for example, by reacting a polyanhydride with a polyamine or by reacting a polyanhydride with a polyisocyanate. Suitable polyanhydrides and polyisocyanates are those described above. As used herein, the term "polyamine" refers to a compound having more than one amine group per molecule, for example, two, three, four, five, six, or more than six amine groups per molecule.Suitable polyamines include aliphatic diamines, such as 1,2-ethanediamine, 1,2-propanediamine, 1,3-propanediamine, 1,2-butanediamine, 1,3-butanediamine, 1,4-butanediamine, 1,3-pentanediamine, 1,5-pentanediamine, 1,6-hexanediamine, 2-methyl-1,5-pentanediamine, 2,5-dimethylhexane-2,5-diamine, 2,2,4-trimethyl-1,6-hexanediamine, 2,4,4-trimethyl-1,6-hexanediamine, 1,7-heptanediamine, 1,8-octanediamine, 1,9-nonanediamine, 1,10-decanediamine, 3,3-amino-bis-propylamine, triethylenetetramine, and tetraethylenepentamine; alicyclic diamines, such as 2,4'-diaminodicyclohexylmethane, 4,4'-diaminodicyclohexylmethane, 3,3'-dimethyl-4,4'-diaminodicyclohexyl silmethane, isophoronediamine, 1,3-bis(aminoethyl)cyclohexane, bis(4-aminocyclohexyl)methane-aminoethylpiperazine, and 3,3′-diethyl-4,4′-diaminodicyclohexylmethane; and aromatic diamines such as 1,2-benzenediamine, 1,3-benzenediamine, 1,4-benzenediamine, 1,5-naphthalenediamine, 1,8-naphthalenediamine, 2,4-toluenediamine, 2,5-toluenediamine, 2,6-toluenediamine, xylylenediamine, 4,4′-diaminodiphenylmethane, 4,4′-diamino-3,3′-diethyldiphenylmethane, diaminodiphenylsulfone, and 3,3′-dimethyl-4,4′-biphenyldiamine, as well as reaction products of polyamines with aliphatic fatty acids, such as the VERSAMID series of materials commercially available from BASF (Germany). Suitable examples of polyimide resins include, but are not limited to, polyimide resins under the trademark Kerimid®, such as 701 A N-70, Kerimid 8292 N-75, and Kerimid 8292 NPM 60, available from Huntsman Corp. (USA).

[0046] Alternatively or additionally, the film-forming resin may comprise a melamine resin. Suitable melamine resins may be prepared in a known manner, for example, by reacting melamine with formaldehyde. Suitable examples of melamine resins include, but are not limited to, CYMEL 1156, available from Allnex (Germany).

[0047] Alternatively or additionally, the film-forming resin may comprise a polyester resin. Suitable polyester resins may be prepared in a known manner, for example, by condensation of a polyol with a polycarboxylic acid or by ring-opening polymerization of a lactone. Non-limiting examples of suitable polyols are those described above, and non-limiting examples of suitable polycarboxylic acids are those described above. Suitable lactones may include, but are not limited to, β-propiolactone, γ-butyrolactone, δ-valerolactone, ε-caprolactone, α-angelicalactone, and mixtures thereof. Suitable polyester resins that may be used in accordance with the present disclosure may be exemplified by polyester resins under the SETAL® trademark, such as SETAL® 1715 VX-74, SETAL® 91703 SS-53, and SETAL® 91715 SS-55, available commercially from Allnex Germany GmbH (Germany).

[0048] Alternatively or additionally, the film-forming resin may comprise a cyanate resin. Suitable cyanate resins may be exemplified by those cyanate resins under the trademark AroCy®, available from Huntsman Corp. (USA), such as AroCy L-10, AroCy XU 366, AroCy 371, or AroCy XU 378.

[0049] According to the present disclosure, the film-forming resin may include, for example, a combination of an epoxy resin and an acrylic resin, or an epoxy resin and a polyurethane resin, as disclosed in US Pat. No. 5,108,832, or US Pat. No. 5,070,119.

[0050] The intumescent coating composition can include any suitable amount of film-forming resin (a). For example, the intumescent coating composition can include more than 5% by weight, e.g., more than 8% by weight, or more than 10% by weight, or more than 12% by weight, or more than 15% by weight of film-forming resin (a). The intumescent coating composition can include, for example, less than 40% by weight, e.g., less than 35% by weight, or less than 32% by weight, or less than 30% by weight, or less than 28% by weight, or less than 25% by weight of film-forming resin. The intumescent coating composition can include, for example, the film-forming resin (a) in an amount ranging between any of the above-mentioned values, such as 5 to 40 wt. %, or 8 to 35 wt. %, or 10 to 35 wt. %, or 10 to 30 wt. %, or 10 to 28 wt. %, or 12 to 25 wt. %, where the weight percentage is based on the total solids weight of the intumescent coating composition.

[0051] As mentioned above, the expandable coating composition may also include a crosslinker (b). Any suitable crosslinker (b) may be used according to the present disclosure, and it may be selected by one skilled in the art to react with the functional groups of the film-forming resin. According to the present disclosure, the crosslinker (b) may include a polyamine, such as a polyetheramine, a polyamide, a polyepoxide, an aminoplast resin, a phenolic resin, a polyisocyanate, a polythiol, a polyol, a copolymer thereof, or a mixture thereof. The crosslinker (b) may specifically include a polyamine.

[0052] The crosslinker may be a latent or blocked crosslinker, where the functional groups of the crosslinker that react with the functional groups of the film-forming resin are generated or restored by a reaction that unblocks them under curing conditions, such as high temperatures, e.g., temperatures above 120°C. A suitable crosslinker of this type is, for example, a blocked polyisocyanate. As used herein, the term "polyisocyanate" is intended to include both blocked and free polyisocyanates. Latent or blocked crosslinkers are particularly suitable for providing single-component compositions that ensure sufficient storage stability and pot life before application and curing. Examples of suitable blocking agents include materials that unblock at high temperatures, e.g., temperatures above 120°C, such as lower aliphatic alcohols having 1 to 6 carbon atoms, e.g., methanol, ethanol, and n-butanol; alicyclic alcohols, e.g., cyclohexanol; aromatic alkyl alcohols, e.g., phenylcarbinol and methylphenylcarbinol; and phenolic compounds, such as phenol itself and substituted phenols where the substituents do not affect the coating process, e.g., cresol and nitrophenol. Glycol ethers can also be used as blocking agents.Suitable glycol ethers include ethylene glycol butyl ether, diethylene glycol butyl ether, ethylene glycol methyl ether, and propylene glycol methyl ether.Other suitable blocking agents include oximes such as methyl ethyl ketoxime, acetone oxime, and cyclohexanone oxime; lactams such as epsilon-caprolactam; pyrazoles such as dimethylpyrazole; and amines such as dibutylamine.

[0053] The crosslinking agent (b) may include a polyamine. As used herein, the term "polyamine" refers to a compound having more than one amine group per molecule, for example, two, three, four, five, six, or more than six amine groups per molecule. Suitable crosslinking agents may include, for example, aliphatic polyamines, aromatic polyamines, polyamine amides, polyether amines, polysiloxane amines, polysulfide amines, or combinations thereof.

[0054] Suitable polyamines include aliphatic diamines, such as 1,2-ethanediamine, 1,2-propanediamine, 1,3-propanediamine, 1,2-butanediamine, 1,3-butanediamine, 1,4-butanediamine, 1,3-pentanediamine, 1,5-pentanediamine, 1,6-hexanediamine, 2-methyl-1,5-pentanediamine, 2,5-dimethylhexane-2,5-diamine, 2,2,4-trimethyl-1,6-hexanediamine, 2,4,4-trimethyl-1,6-hexanediamine, 1,7-heptanediamine, 1,8-octanediamine, 1,9-nonanediamine, 1,10-decanediamine, 3,3-amino-bis-propylamine, triethylenetetramine, and tetraethylenepentamine; alicyclic diamines, such as 2,4'-diaminodicyclohexylmethane, 4,4'-diaminodicyclohexylmethane, 3,3'-dimethyl-4,4'-diaminodicyclohexyl silmethane, isophoronediamine, 1,3-bis(aminoethyl)cyclohexane, bis(4-aminocyclohexyl)methane-aminoethylpiperazine, and 3,3′-diethyl-4,4′-diaminodicyclohexylmethane; and aromatic diamines such as 1,2-benzenediamine, 1,3-benzenediamine, 1,4-benzenediamine, 1,5-naphthalenediamine, 1,8-naphthalenediamine, 2,4-toluenediamine, 2,5-toluenediamine, 2,6-toluenediamine, xylylenediamine, 4,4′-diaminodiphenylmethane, 4,4′-diamino-3,3′-diethyldiphenylmethane, diaminodiphenylsulfone, and 3,3′-dimethyl-4,4′-biphenyldiamine, as well as reaction products of polyamines with aliphatic fatty acids, such as the VERSAMID series of materials commercially available from BASF (Germany).

[0055] In addition, any of the above polyamine adducts can be used. The polyamine adducts can be formed by reacting a polyamine with a suitable reactive compound, such as an epoxy resin. This reaction reduces the free amine content in the curing agent, making it more useful in low temperature and / or high humidity environments.

[0056] According to the present disclosure, polyamines can include polyetheramines, such as Jeffamines commercially available from Huntsman Corp. (USA), including, but not limited to, Jeffamine D-230, Jeffamine D-400, Jeffamine 600, Jeffamine 1000, Jeffamine 2005, and Jeffamine 2070.

[0057] Alternatively or additionally, the crosslinking agent (b) may comprise a polyamide. Suitable polyamides may be prepared by reacting a polyamine with a polycarboxylic acid or by ring-opening polymerization of a lactam. Non-limiting examples of suitable polyols are those described above, and non-limiting examples of suitable polyamines are those described above. Suitable lactams include, but are not limited to, β-propiolactam, γ-butyrolactam, δ-valerolactam, ε-caprolactam, and mixtures thereof. Specifically, the polyamide may contain the reaction product of a dimer fatty acid with a polyethyleneamine and a small amount of a monomeric fatty acid. The dimer fatty acid is prepared by oligomerization of a monomeric fatty acid. The polyethyleneamine may be any higher polyethyleneamine, such as diethylenetriamine, triethylenetetramine, or tetraethylenepentamine, with diethylenetriamine being the most commonly used. When polyamides are used as crosslinkers, they may impart one or more desirable properties to the intumescent coating, such as corrosion resistance, water resistance, and / or good flexibility.

[0058] Alternatively or additionally, the crosslinking agent (b) may comprise a polyepoxide. Non-limiting examples of suitable polyepoxides are those described above.

[0059] Alternatively or additionally, the crosslinking agent (b) may comprise an aminoplast resin. Suitable aminoplast resins may be obtained from the condensation reaction of an aldehyde, such as formaldehyde, with a compound containing at least two amine or amide groups per molecule. Suitable examples of aldehydes include, but are not limited to, formaldehyde, acetaldehyde, crotonaldehyde, and benzaldehyde. Suitable examples of compounds containing at least two amine or amide groups include, but are not limited to, melamine, urea, and benzoguanamine. Preferably, the aminoplast resin may be etherified with an alcohol, such as methanol, ethanol, butanol, or a mixture thereof. Suitable aminoplast resins that may be used in accordance with the present disclosure may be exemplified by Maprenal® Amino Resins, such as Maprenal MF 612 / 70B, Maprenal MF 613 / 71B, and Maprenal MF 650 / 55IB, available commercially from Prefere Resin Holding GmbH (Germany); Cymel® Amino Crosslinkers, such as Cymel 303, Cymel 202, Cymel 1161, Cymel 325, and Cymel 1133, available commercially from Allnex Industries (Germany); and Setamine® amino resins, such as Setamine US-138 BB-70 and Setamine US-146 BB-72, available commercially from Allnex (Germany).

[0060] Alternatively or additionally, the crosslinker (b) may comprise a phenoplast resin. Suitable phenoplast resins may be obtained by either acid-catalyzed (novolac) or base-catalyzed (resol) addition polymerization of phenol and formaldehyde. Suitable phenoplast resins that may be used in accordance with the present disclosure may be exemplified by EPON™ Epoxy Novolac resins, such as EPON™ Resin SU-8, commercially available from Hexion Inc. (USA).

[0061] Alternatively or additionally, the crosslinking agent (b) may comprise a polyisocyanate. Non-limiting examples of suitable polyisocyanates are those described above.

[0062] Alternatively or additionally, crosslinker (b) can comprise a polythiol. Suitable polythiols include, but are not limited to, polysulfide thiols, polyether thiols, polyester thiols, pentaerythritol-based thiols, or combinations thereof. A particularly suitable polythiol is Thioplast G4, available from Akzo Nobel Functional Chemicals GmbH & Co. KG (Germany).

[0063] Alternatively or additionally, the cross-linking agent (b) may comprise a polyol. Non-limiting examples of suitable polyols are those described above.

[0064] As mentioned above, when the film-forming resin (a) comprises an epoxy resin, the crosslinker (b) comprises a polyamine, a polythiol, or a combination thereof; specifically, when the film-forming resin (a) comprises an epoxy resin, the crosslinker (b) comprises a polyamine.

[0065] The intumescent coating composition can include any suitable amount of crosslinker (b). For example, the intumescent coating composition can include more than 5% by weight, e.g., more than 8% by weight, or more than 10% by weight, or more than 12% by weight, or more than 15% by weight of crosslinker (b). The intumescent coating composition can include, for example, less than 40% by weight, e.g., less than 35% by weight, or less than 32% by weight, or less than 30% by weight, or less than 28% by weight, or less than 25% by weight of film-forming resin. The intumescent coating composition can include the crosslinker (b) in an amount ranging between any of the values ​​recited above, such as 5 to 40 wt. %, or 8 to 35 wt. %, or 10 to 35 wt. %, or 10 to 30 wt. %, or 10 to 28 wt. %, or 12 to 25 wt. %, where the weight percentage is based on the total solids weight of the intumescent coating composition.

[0066] The intumescent coating composition may further include a compound (c) that provides an inflation gas upon thermal decomposition. The inflation gas serves to foam and expand the intumescent composition when exposed to high temperatures, e.g., above 150°C, or flame. As a result of this expansion, a thick, multi-cellular char forms, which serves to insulate and protect the underlying substrate. Any suitable source of inflation gas that can be used in the intumescent composition of the present disclosure is a nitrogen-containing material. Suitable nitrogen-containing materials include, but are not limited to, melamine, phosphates, guanidine, methylolated melamine, hexamethoxymethylmelamine, urea, dimethylurea, melamine pyrophosphate, dicyandiamide, guanylurea phosphate, and glycine. Other conventional inflation gas sources, such as materials that liberate carbon dioxide, may also be used. Suitable examples of materials that liberate carbon dioxide include alkaline earth metals, such as calcium carbonate or magnesium carbonate. Compounds that release water vapor upon decomposition upon heating, such as calcium hydroxide, magnesium dihydroxide, or aluminum trihydroxide, can also be used, as can expandable graphite. Other examples of such compounds are borate sources, such as boric acid and boric acid derivatives, such as boric acid esters and metal borates. Specifically, the compound (c) that provides expansion gas upon thermal decomposition can include melamine, melamine derivatives, guanidine, methylol melamine, hexamethoxymethyl melamine, urea, dimethyl urea, melamine pyrophosphate, dicyandiamide, guanylurea phosphate, glycine, alkaline earth metal carbonates, calcium hydroxide, magnesium dihydroxide, aluminum trihydroxide, expandable graphite, or mixtures thereof.

[0067] For example, a compound (c) that provides an expansion gas upon thermal decomposition, such as melamine, may be used in the intumescent coating composition of the present disclosure in an amount of 1% by weight or more, e.g., 2% by weight or more, or 3% by weight or more. The composition according to the present disclosure may contain, for example, less than 10% by weight, or less than 8% by weight, or less than 7% by weight, or less than 5% by weight of the compound (c) that provides an expansion gas upon thermal decomposition. The composition may contain, for example, less than 10% by weight, or less than 8% by weight, or less than 7% by weight, or less than 5% by weight of the compound (c) that provides an expansion gas upon thermal decomposition in an amount ranging between any of the values ​​recited above, e.g., 1 to 10% by weight, or 2 to 7% by weight. The weight percentages are based on the total solids weight of the intumescent coating composition.

[0068] The intumescent coating composition of the present disclosure includes, inter alia, (a) a film-forming resin, (b) a crosslinker, and (c) a compound that provides an expanding gas upon thermal decomposition. According to the present disclosure, compounds (a)-(c) are different from one another.

[0069] The expandable coating composition of the present disclosure may further comprise an epoxy-reactive diluent. Preferably, the epoxy-reactive diluent is operable to reduce the viscosity of the composition.

[0070] Suitable epoxy-reactive diluents can be produced by any suitable method. Such epoxy-reactive diluents can be formed from the reaction of a compound containing an aliphatic epoxide functional group, such as a diglycidyl ether, with an aliphatic alcohol or polyol. Examples of suitable compounds containing epoxide functional groups include, but are not limited to, monoglycidyl ethers, diglycidyl ethers, triglycidyl ethers, and mixtures thereof. Examples of suitable alcohols and polyols include, but are not limited to, hexanediol, butanediol, glycerol, trimethylolpropane, trimethylolethane, pentaerythritol, neopentyl glycol, and mixtures thereof. Specifically, the epoxy-reactive diluent can include a diglycidyl ether of an aliphatic alcohol. Preferably, the epoxy-reactive diluent can include the diglycidyl ether of hexanediol and / or the diglycidyl ether of neopentyl glycol.

[0071] The intumescent coating composition of the present disclosure, when present, may comprise reactive epoxy diluents in an amount of at or above 1 wt%, e.g., at or above 2 wt%, or at or above 3 wt%, or at or above 4 wt%, or at or above 5 wt%, or at or above 6 wt%. The intumescent coating composition, when present, may comprise reactive epoxy diluents in an amount of less than or equal to 30 wt%, e.g., less than or equal to 20 wt%, or less than or equal to 15 wt%, or less than or equal to 10 wt%. The intumescent coating composition, when present, may comprise reactive epoxy diluents in an amount ranging between any of the values ​​recited above, e.g., 1 to 30 wt%, e.g., 2 to 20 wt%, or 3 to 15 wt%, or 5 to 10 wt%. The weight percentages are based on the total solids weight of the intumescent coating composition.

[0072] The expandable coating composition of the present disclosure may further comprise a phosphate compound. As used herein, the term "phosphate compound" refers to any phosphorus-containing material, including phosphoric acid or its condensation or dehydration products (including oxides), or salts, esters, amides, or other derivatives of any of the foregoing. The phosphate compound may include a variety of materials, such as phosphoric acid, mono- and diammonium phosphates, triphenyl phosphate, tris-(2-chloroethyl) phosphate, tris-(2-chloroisopropyl) phosphate, ammonium polyphosphate, melamine pyrophosphate, and combinations thereof. Ammonium polyphosphate has the formula (NH4) n+2 P n O 3n+1 where n is an integer of at least 2, and preferably n is an integer of at least 50.

[0073] The intumescent coating composition of the present disclosure, when present, may comprise a phosphate compound in an amount of at or above 15% by weight, e.g., at or above 20% by weight, or at or above 25% by weight, or at or above 30% by weight, or at or above 35% by weight, or at or above 40% by weight. The intumescent coating composition, when present, may comprise a phosphate compound in an amount of less than 55% by weight, e.g., less than 50% by weight, or less than 45% by weight, or less than 40% by weight, or less than 35% by weight. The intumescent coating composition, when present, may comprise a phosphate compound in an amount ranging between any of the above-mentioned values, e.g., 15 to 55% by weight, e.g., 20 to 50% by weight, or 25 to 40% by weight, or 40 to 55% by weight. The weight percentages are based on the total solids weight of the intumescent coating composition.Phosphorus is believed to function as a char promoter in the intumescent composition.

[0074] The expandable coating composition of the present disclosure may further comprise a borate compound. As used herein, the term "borate compound" refers to any boron-containing material containing boric acid or its condensation or dehydration products (including oxides), or any salt or ester of the foregoing. According to the present disclosure, the borate compound may include ammonium pentaborate, boric acid, metal borates such as zinc borate, boron oxide, sodium borate, potassium borate, ammonium borate, borate esters such as butyl borate and phenyl borate, or mixtures thereof.

[0075] The intumescent coating composition of the present disclosure, when present, may comprise a borate compound in an amount of at or above 5% by weight, e.g., at or above 6% by weight, or at or above 7% by weight, or at or above 8% by weight, or at or above 9% by weight, or at or above 10% by weight. The intumescent coating composition, when present, may comprise a borate compound in an amount of less than at or above 35% by weight, e.g., less than at or above 30% by weight, or less than at or above 25% by weight, or less than at or above 20% by weight. The intumescent coating composition, when present, may comprise a borate compound in an amount ranging between any of the values ​​recited above, e.g., 5 to 35% by weight, or 5 to 30% by weight, or 9 to 15% by weight. The weight percentages are based on the total solids weight of the intumescent coating composition.

[0076] The expandable coating composition of the present disclosure may further comprise an aluminum compound. As used herein, the term "aluminum compound" refers to any aluminum-containing material. Typically, the aluminum compound may comprise an inorganic aluminum compound. Suitable aluminum compounds may include aluminum hydroxide, aluminum oxide (alumina), aluminum salts such as aluminum chloride, and combinations thereof. For example, the aluminum compound may include aluminum hydroxide and / or aluminum oxide.

[0077] The intumescent coating composition of the present disclosure, when present, may comprise aluminum compounds in an amount greater than or equal to 0.1 wt%, e.g., greater than or equal to 0.2 wt%, or greater than or equal to 0.3 wt%, or greater than or equal to 0.5 wt%, or greater than or equal to 1 wt%, or greater than or equal to 3 wt%, or greater than or equal to 5 wt%. The intumescent coating composition, when present, may comprise aluminum compounds in an amount less than or equal to 10 wt%, e.g., less than or equal to 9 wt%, or less than or equal to 8 wt%, or less than or equal to 5 wt%, or less than or equal to 3 wt%, or less than or equal to 1 wt%, or less than or equal to 0.7 wt%. When present, the intumescent coating composition can include the aluminum compound in an amount ranging between any of the above-mentioned values, for example, 0.1 to 10 wt. %, or 0.2 to 8 wt. %, or 0.3 to 1 wt. %, where the weight percentages are based on the total solids weight of the intumescent coating composition.

[0078] The expandable coating composition of the present disclosure may further comprise a silica compound. As used herein, the term "silica compound" refers to any silicon-containing material, including silicic acid, its condensation products or dehydration products (including oxides), or any salt or ester of the foregoing. Suitable silica compounds may include fumed silica, quartz, or silica-containing materials, such as bentonite or kaolin, or mixtures thereof.

[0079] The intumescent coating composition of the present disclosure, when present, may contain silica compounds in an amount greater than or equal to 0.1 wt%, e.g., greater than or equal to 0.2 wt%, or greater than or equal to 0.3 wt%, or greater than or equal to 0.4 wt%, or greater than or equal to 0.5 wt%. The intumescent coating composition, when present, may contain silica compounds in an amount less than or equal to 5 wt%, e.g., less than or equal to 3 wt%, or less than or equal to 2 wt%, or less than or equal to 1 wt%, or less than or equal to 0.8 wt%. The intumescent coating composition, when present, may contain silica compounds in an amount ranging between any of the values ​​recited above, e.g., 0.1 to 5 wt%, or 0.4 to 1 wt%. The weight percentages are based on the total solids weight of the intumescent coating composition.

[0080] The expandable coating composition of the present disclosure may include a borate compound, an aluminum compound, or a silica compound. Thus, the expandable coating composition of the present disclosure may contain, for example, one of a borate compound, an aluminum compound, or a silica compound. For example, the expandable coating composition may include a borate compound. Alternatively, the expandable coating composition may include an aluminum compound or a silica compound. On the other hand, the expandable coating composition may also include a combination of two or more of a borate compound, an aluminum compound, and / or a silica compound. For example, the expandable coating composition according to the present disclosure may include an aluminum compound and a silica compound, or a borate compound and an aluminum compound, or a borate compound and a silica compound. The expandable coating composition may include a borate compound, an aluminum compound, and a silica compound.

[0081] The intumescent coating composition of the present disclosure may further comprise titanium dioxide (TiO). When present, the intumescent coating composition according to the present disclosure may comprise TiO in an amount of at or greater than 5% by weight, e.g., at or greater than 6% by weight, or at or greater than 7% by weight, or at or greater than 8% by weight, or at or greater than 9% by weight, or at or greater than 10% by weight. When present, the intumescent coating composition may comprise TiO in an amount of less than 20% by weight, e.g., less than 19% by weight, or less than 18% by weight, or less than 17% by weight, or less than 15% by weight, or less than 13% by weight, or less than 10% by weight. When present, the intumescent coating composition can include TiO in an amount ranging between any of the above-mentioned values, for example, 5-20 wt. %, or 5-10 wt. %, or 10-18 wt. %, where the weight percentage is based on the total solids weight of the intumescent coating composition.

[0082] Specifically, the intumescent coating composition may contain a borate compound, an aluminum compound, or a silica compound in the above ranges in combination with TiO2 and a phosphate source. Such an intumescent coating composition provides an intumescent coating with desirable char formation, particularly in combination with desirable adhesion to the substrate. "Desired char formation" means that the char is not easily cracked or removed by direct flame blasting, and the expansion coefficient, which is the ratio between the thickness of the char and the thickness of the coating film, may be 5 to 25, for example, 7 to 20. "Desired adhesion" means that the char remains substantially intact during direct flame blasting, and no significant detachment of the char from the substrate occurs during or after the fire test.

[0083] According to the present disclosure, the intumescent coating composition can be applied to a portion of a substrate surface by any means standard in the art, such as electrocoating, spray application, electrostatic spray application, dipping, rolling, brushing, etc. The intumescent coating composition of the present invention can be applied to provide various dry film thicknesses ("DFT") as needed. The intumescent coating composition can be applied to a portion of a substrate surface to obtain a dry coating thickness ranging from 0.1 to 15 mm, e.g., 0.2 to 14 mm, or 0.5 to 13 mm, or 0.5 to 12 mm, or 0.7 to 10 mm. The thickness can be determined in accordance with DIN EN ISO 2178:2016. As used herein, "dry coating thickness" is the thickness of a coating applied to a portion of a substrate surface and measured on the substrate after the coating has cured. The desired dry film thickness ("DFT") can vary depending on the application. For use on architectural structural components, a DFT ranging from 0.1 to 15 mm, e.g., 0.3 to 1 mm, or 3 to 15 mm, can be suitable. For use in lithium batteries, a DFT in the range of 0.2 to 5 mm, for example 0.2 to 1 mm, or 1 to 5 mm, may be suitable.

[0084] Alternatively, the intumescent coating composition of the present disclosure can be formed into a self-supporting film or sheet. Generally, the intumescent coating composition of the present disclosure can be formed into a film or sheet by any technique known to those skilled in the art, such as by impregnating a mesh with the coating by a casting process. The film or sheet can be cured to form a cured, intumescent, self-supporting film or sheet before applying the cured, intumescent, self-supporting film or sheet to a substrate. It is also within the scope of the present disclosure for an uncured film or sheet to be applied to a substrate after the forming step and then subsequently cured to obtain a cured intumescent layer according to the present disclosure. The film or sheet can be applied to the substrate through an adhesive. The intumescent coating composition can be formed into a self-supporting film or sheet having a dry film thickness ranging from 0.1 to 15 mm, e.g., from 0.2 to 14 mm, or from 0.5 to 13 mm, or from 0.5 to 12 mm, or from 0.7 to 10 mm.

[0085] The intumescent coating compositions of the present disclosure may further comprise one or more additional additives suitable for use in intumescent coatings, including zinc sources, acid sources, reinforcing fillers, carbon sources, inorganic fillers, rheological additives, organic solvents, pigments, foam stabilizers, and combinations thereof.

[0086] The zinc source can contribute to the formation of small cell structures in the char. Small char cells can provide better insulation for the substrate and better maintain the integrity of the char and adhere to the substrate. Therefore, cracking and breakage of the char from the substrate are minimized, providing greater protection for the underlying substrate. Suitable examples of zinc sources include, but are not limited to, zinc oxide, zinc salts such as zinc borate and zinc phosphate, zinc carbonate, and zinc metal.

[0087] Suitable examples of acid sources can include, but are not limited to, ammonium phosphate, ammonium polyphosphate, diammonium diphosphate, diammonium pentaborate, phosphoric acid generating materials, boric acid, metal or organic borates, and combinations thereof.

[0088] It should be understood that many of the components of the intumescent coating composition can serve more than one function in the composition. For example, the phosphorus compound, zinc source, borate compound, and compound that provides inflation gas upon thermal decomposition can each be provided by a separate feedstock, or alternatively, a single material can be the source of more than one of these components. For example, melamine pyrophosphate can provide a source of both phosphorus and inflation gas, zinc borate can provide a zinc source and a borate source, and zinc phosphate can provide a zinc source and a phosphate source.

[0089] The reinforcing filler may be selected from a number of conventionally used materials, including fibrous and platelet reinforcing materials, which may be more suitable than other fillers. Examples of fibrous reinforcing materials include glass fiber, ceramic fibers such as aluminum oxide / silicon oxide, graphite fiber, mineral fiber, and basalt fiber. Platelet reinforcing materials include hammer mill glass flake, mica, and wollastonite. Other suitable fillers include metal oxides, clay, talc, silica, diatomaceous earth, Lapinus fiber, and various pigments. The reinforcing filler is believed to help control the expansion of the fire-resistant composition before and during char formation so that the resulting char is rigid and uniform. When present, reinforcing fillers, such as glass fiber and / or mineral fiber, are typically present in the intumescent coating composition in an amount of 5.0% by weight or less, e.g., 4% by weight or less, e.g., 3% by weight or less. Intumescent coating compositions according to the present disclosure may include reinforcing fillers in amounts of, for example, at or above 0.1 wt %, e.g., at or above 0.2 wt %, at or above 0.5 wt %, or at or above 1 wt %. Intumescent coating compositions may include reinforcing fillers in amounts ranging between any of the above-mentioned values, e.g., 0.1-5.0 wt %, or 1-4 wt %. The weight percentages are based on the total solids weight of the intumescent coating composition.

[0090] The intumescent coating composition of the present disclosure may further comprise a fibrous reinforcing material. According to the present disclosure, the fibrous reinforcing material may comprise mineral fibers, ceramic fibers, glass fibers, carbon fibers, basalt fibers, or mixtures thereof. When present, the intumescent coating composition of the present disclosure may comprise the fibrous reinforcing material in an amount of at or greater than 0.1 wt %, for example, at or greater than 0.2 wt %, or at or greater than 0.5 wt %, or at or greater than 0.7 wt %, or at or greater than 1 wt %, or at or greater than 1.5 wt %. When present, the intumescent coating composition may comprise fibrous reinforcement in an amount of 5.0% or less by weight, e.g., 4.5% or less by weight, or 4.0% or less by weight, or 3.5% or less by weight, or 3.0% or less by weight, or 2.5% or less by weight. When present, the intumescent coating composition may comprise fibrous reinforcement in an amount ranging between any of the values ​​recited above, e.g., 0.5 to 5.0% by weight, or 0.7 to 4.0% by weight, or 1.0 to 3.0% by weight. The weight percentages are based on the total solids weight of the intumescent coating composition.

[0091] The intumescent coating composition of the present disclosure may also contain various conventional additives, such as rheological additives, organic solvents, foam stabilizers, pigments, flame spread control agents, and the like. These components may be added in various amounts as needed. Typically, when additional additives are used, they are present in a total amount of 1% by weight or more, e.g., 2% by weight or more, or 5% by weight or more, or 10% by weight or more. When present, the additional additives may be present, for example, in an intumescent coating composition according to the present disclosure, in an amount of less than 20% by weight, e.g., less than 15% by weight, or less than 12% by weight. The intumescent coating composition may include the optional additional additives in an amount ranging between any of the values ​​recited above, e.g., 1 to 20% by weight, e.g., 2 to 20% by weight, or 5 to 15% by weight. The weight percentages are based on the total solids weight of the intumescent coating composition.

[0092] The intumescent coating composition can be either a one-component ("1K") or a multi-component composition, e.g., two-component ("2K") or more than two-component. As used herein, a "1K composition" refers to a composition in which all coating components are maintained in the same container after manufacture, during storage, etc. A 1K composition can be applied to a substrate and cured by any conventional means, such as heating, forced air, etc. An intumescent coating composition can also be multi-component, which will be understood as a composition in which the various components are maintained separately until just prior to application. For example, the composition can be packaged as a 2K system, with the film-forming resin in a first package (A) and the crosslinker in a second package (B), whereby all other components used in the coating composition can be used in any combination in either package (A) or package (B), or both, or some or all can be in one or more additional packages (C). The individual packages are mixed before using the intumescent composition. In particular, the intumescent coating composition can be a two-component ("2K") coating composition.

[0093] The expandable coating composition can be in the form of a thick material, such as a mastic. The composition is solvent-free and is particularly suitable for spray application. If desired, dilution can be achieved with various conventional solvents, such as xylene, methylene chloride, or 1,1,1-trichloroethane.

[0094] The intumescent coating composition may be applied by any means standard in the art, such as electrocoating, spray application, electrostatic spray application, dipping, rolling, brushing, and the like, including robotic application.

[0095] As mentioned above, in the method of the present disclosure, the expandable coating composition is cured by irradiating it with pulsed infrared radiation. As used herein, the term "pulse" refers to radiation emitted in time-limited portions (pulses). The term "infrared radiation" refers to electromagnetic radiation having a wavelength in the range of 780 nm to 1 mm. Thus, the term "pulsed infrared radiation" refers to electromagnetic radiation having a wavelength in the infrared spectrum range that is irradiated in pulses. The pulses have a pulse duration at a pulse frequency.

[0096] The terms "cure," "cured," or similar terms, when used in connection with the intumescent coating compositions described herein, mean that at least a portion of the components forming the coating composition have cured to form a coating. Pulsed infrared radiation can be irradiated on the intumescent coating composition to form an at least partially cured intumescent coating or an at least partially cured intumescent film or sheet. As used herein, the term "at least partially cured" means that reaction of at least a portion of the reactive groups of the components of the intumescent coating composition occurs. In accordance with the present disclosure, pulsed infrared radiation can be irradiated on the intumescent coating composition to form a fully cured intumescent coating or a fully cured intumescent film or sheet. Full cure is achieved when further curing does not result in significant further improvement in the coating properties, for example, the hardness of the cured coating or cured self-supporting film or sheet. The hardness of the cured coating or cured self-supporting film or sheet may be determined by Shore hardness, such as by determining the Shore D hardness at room temperature using a Shore D durometer in the range of 40 to 90, or by determining the Shore A hardness at room temperature using a Shore A durometer of at least 50.

[0097] According to the present disclosure, pulsed infrared radiation may be applied for a time period of less than 50 minutes, or less than 40 minutes, or less than 35 minutes, or less than 30 minutes, or less than 25 minutes, or less than 20 minutes, or less than 15 minutes, or less than 10 minutes to form a cured coating or a cured self-supporting film or sheet. According to the present disclosure, pulsed infrared radiation may be applied for a time period of at least 2 minutes, or at least 4 minutes, or at least 5 minutes, or at least 6 minutes, or at least 8 minutes to form a cured coating or a cured self-supporting film or sheet. According to the present disclosure, pulsed infrared radiation may be applied for a time period ranging from any of the above-mentioned values, for example, from 2 minutes to 50 minutes, or from 2 minutes to 35 minutes, or from 2 minutes to 30 minutes, or from 4 minutes to 25 minutes, or from 5 minutes to 20 minutes, or from 6 minutes to 15 minutes, or from 8 minutes to 10 minutes to form a cured coating or a cured self-supporting film or sheet. Compared to curing an intumescent coating composition in an oven, shorter curing times may be achieved, resulting in energy savings. This method also offers high efficiency, since the infrared emitter is activated immediately after switching on, without a long preheating period, and only the desired partial area (e.g., the substrate on which the swellable coating composition is applied) is heated.

[0098] When pulsed infrared radiation is used, energy is transferred to the coating composition not primarily through thermal convection or conduction, but through invisible electromagnetic waves in the infrared spectrum at the speed of light, since electromagnetic waves propagate in the same manner and at the same speed as light waves. The infrared radiation penetrates the substrate surface quickly and effectively, ensuring rapid curing of the applied expandable coating composition or the formed self-supporting film or sheet. This allows for the transfer of radiation with high energy density, thus enabling highly energy-efficient curing of the coating composition according to the present disclosure. Faster, more energy-efficient curing at lower temperatures can be achieved.

[0099] According to the present disclosure, the surface temperature of the substrate during irradiating the applied intumescent coating composition with pulsed infrared radiation in (II) to form a cured intumescent coating can be less than 100°C, or less than 90°C. According to the present disclosure, the surface temperature of the substrate during irradiating the applied intumescent coating composition with pulsed infrared radiation in (II) to form a cured intumescent coating can be at least 60°C, for example, at least 70°C. The surface temperature of the substrate during irradiating the applied intumescent coating composition with pulsed infrared radiation in (II) to form a cured intumescent coating can be in the range of 60°C to 100°C, for example, 70°C to 90°C. The surface temperature of the substrate can be determined according to DIN EN 60584-1:2014.

[0100] The pulsed infrared radiation according to the present disclosure may have a peak wavelength of at least 3 μm. As used herein, the term "peak wavelength" refers to the maximum emission wavelength of the pulsed infrared radiation. The pulsed infrared radiation used in the methods of the present disclosure may have a peak wavelength of 10 μm or less, for example, 6 μm or less, or 4 μm or less. The pulsed infrared radiation used in the methods of the present application may range between any of the above-mentioned values, for example, 3 μm to 10 μm, or 3 μm to 6 μm, or 3 μm to 4 μm.

[0101] According to the present disclosure, pulsed infrared light can be emitted with a pulse duration of at least 5 μs, for example, at least 8 μs, or at least 10 μs. As used herein, the term "pulse duration," also referred to as "pulse width," refers to the full width at half maximum (FWHM) amplitude of the pulse of pulsed infrared light. Pulsed infrared light can be emitted with a pulse duration of 100 μs or less, for example, 75 μs or less, or 50 μs or less, or 25 μs or less, or 15 μs or less, or 14 μs or less, or 12 μs or less. Pulsed infrared radiation according to the present disclosure may be irradiated with a pulse duration ranging between any of the values ​​mentioned above, for example, from 5 μs to 12 μs, or from 8 μs to 12 μs, or from 10 μs to 12 μs, or from 5 μs to 14 μs, or from 8 μs to 14 μs, or from 10 μs to 14 μs, or from 5 μs to 15 μs, or from 8 μs to 15 μs, or from 10 μs to 15 μs, or from 5 μs to 25 μs, or from 8 μs to 25 μs, or from 10 μs to 25 μs, or from 5 μs to 50 μs, or from 8 μs to 50 μs, or from 10 μs to 50 μs, or from 5 μs to 75 μs, or from 8 μs to 75 μs, or from 10 μs to 75 μs, or from 5 μs to 100 μs, or from 8 μs to 100 μs, or from 10 μs to 100 μs.

[0102] In particular, pulsed infrared radiation according to the present disclosure that is applied to form a cured coating or a cured self-supporting film or sheet can have a peak wavelength in the range of 3 μm to 10 μm, e.g., 3 μm to 6 μm, with a pulse duration of less than 100 μs, e.g., less than 25 μs, or less than 14 μs.

[0103] Pulsed infrared radiation according to the present disclosure may be irradiated at a pulse frequency of at least 350 Hz, e.g., at least 370 Hz, or at least 390 Hz, or at least 400 Hz. As used herein, the term "pulse frequency" refers to the number of pulses per second of pulsed infrared radiation. Pulsed radiation according to the present disclosure may be irradiated at a pulse frequency of 450 Hz or less, e.g., 430 Hz. Pulsed infrared radiation may be irradiated at a pulse frequency ranging from 350 Hz to 450 Hz, e.g., from 350 Hz to 430 Hz, or from 370 Hz to 450 Hz, or from 370 Hz to 430 Hz, or from 390 Hz to 450 Hz, or from 390 Hz to 430 Hz, or from 400 Hz to 450 Hz, or from 400 Hz to 430 Hz. According to the present disclosure, pulsed infrared light may be irradiated at a pulse frequency ranging between any of the values ​​mentioned above, for example, 350 Hz to 450 Hz, or 370 Hz to 450 Hz, or 390 Hz to 450 Hz, or 400 Hz to 450 Hz.

[0104] Pulsed infrared radiation according to the present disclosure has a power of at least 250 W / cm 2 , e.g., at least 270 W / cm 2 , or at least 290W / cm 2 As used herein, the term "impact energy" refers to the total radiant power of electromagnetic radiation received by a surface per unit area. Pulsed radiation according to the present disclosure may be irradiated with an impingement energy of 350 W / cm. 2 or 350W / cm 2 Less than, for example, 330W / cm 2 or 330W / cm 2 Less than or equal to 320W / cm 2 or 320W / cm 2 Pulsed infrared radiation may be irradiated with an impulse energy of less than 250 W / cm. 2 ~350W / cm 2 , or 250W / cm 2 ~330W / cm 2 , or 250W / cm 2 ~320W / cm 2, or 270 W / cm 2 ~350W / cm 2 , or 270 W / cm 2 ~330W / cm 2 , or 270 W / cm 2 ~320W / cm 2 , or 290 W / cm 2 ~350W / cm 2 , or 290 W / cm 2 ~330W / cm 2 , or 290 W / cm 2 ~320W / cm 2 can be irradiated with an impact energy of

[0105] According to the present disclosure, pulsed infrared radiation can be provided by an infrared light source including a surface comprising a ceramic composition. The ceramic composition can absorb heat and emit pulsed infrared radiation, specifically having a peak wavelength in the range mentioned above. According to the present disclosure, the infrared light source can include a surface including a ceramic composition capable of absorbing heat and emitting pulsed infrared radiation. Preferably, the infrared light source can include a surface including a ceramic composition capable of absorbing heat and emitting pulsed infrared radiation in the range of 3 μm to 10 μm. The use of pulsed infrared radiation generated by the ceramic composition can have a positive effect on the curing of the expandable coating composition according to the present disclosure.

[0106] For curing, the infrared emitting surface of the infrared light source can face the surface of the substrate on which the intumescent coating composition to be cured is applied, or the surface of the self-supporting film or sheet to be cured. Herein, the distance between the infrared emitting surface of the infrared light source and the surface of the substrate on which the intumescent coating composition to be cured is applied, or the surface of the self-supporting film or sheet to be cured, can be at least 5 cm, for example, at least 10 cm, or at least 15 cm. Herein, the distance between the infrared emitting surface of the infrared light source and the surface of the substrate on which the intumescent coating composition to be cured is applied, or the surface of the self-supporting film or sheet to be cured, can be at or less than 50 cm, for example, at or less than 45 cm, or at or less than 40 cm, or at or less than 35 cm, or at or less than 30 cm, or at or less than 25 cm, or at or less than 20 cm, or at or less than 15 cm. The infrared emitting surface of the infrared light source can face the surface of the substrate onto which the curing intumescent coating composition is applied, or the surface of the self-supporting film or sheet, at a distance ranging between any of the values ​​mentioned above, for example, 5 cm to 50 cm, or 5 cm to 30 cm, or 5 cm to 15 cm, or 10 cm to 20 cm, or 15 cm to 25 cm.

[0107] According to the present disclosure, the infrared light source can face the surface of the substrate or the surface of the self-supporting film or sheet on which the intumescent coating composition to be cured is applied from at least one side. At least one or more infrared light sources of the present disclosure can surround the surface of the substrate or the surface of the self-supporting film or sheet on which the intumescent coating composition to be cured is applied from at least one side. Suitable arrangements of infrared light sources are described, for example, in EP 1 690 842 A1 (especially paragraphs

[0044] to

[0049] ) and WO 2011 / 015164 (especially pages 12-13). The infrared light source according to the present disclosure can have any desired shape, for example, the shape of a rod, a tube, a flat plate, or a curved plate.

[0108] The infrared light source may further include a heat source for directly or indirectly heating the ceramic composition. Heat transfer from the heat source may involve various heat transfer methods, including radiation, convection, contact, or transfer via a thermally conductive material between the heat source and the ceramic composition. The infrared light source may further include a carrier material for heat absorption and / or heat transfer from the heat source to the ceramic composition. The carrier material may include one or more of the following materials: Fe, SiO2, 3Al2O3·2SiO2, and / or 2Al2O3·1SiO2 (mullite), Al, or Cu. Furthermore, the infrared light source may include a reflector device. The ceramic composition may generate infrared light and, in particular, may radiate infrared light in undesired directions. The reflector device, which may include one or more reflectors, may be applied to reflect infrared light radiated in undesired directions and redirect the infrared light to a specific area, such as the surface of a substrate on which the coating composition to be cured is applied, or the surface of a self-supporting film or sheet to be cured.

[0109] Ceramic compositions according to the present disclosure may include (a) (ai) a metal oxide component including a metal element selected from the group consisting of alkaline earth elements, transition metal elements, lanthanides, and actinides, and (a-ii) oxygen, and (b) a mullite balance component including 3Al2O3·2SiO2 and / or 2Al2O3·SiO2 (mullite). Suitable examples of the metal oxide component (a) include, but are not limited to, Cr2O3, ZrO2, Ho2O3, Fe2O3, LaCrO3, CeO2, YO3, YCrO3, Gd2O3, MgAl2O4, MgCrO4, CaCrO4, YCrO3, CuO, La2O3, CuCrO4, and FeCrO3. The ceramic composition may consist of the metal oxide component (a) and the mullite balance component (b).

[0110] The ceramic composition may comprise at least 0.1 wt.%, e.g., at least 0.5 wt.%, e.g., at least 1.0 wt.%, e.g., at least 5.0 wt.%, of metal oxide component (a) based on the total weight of the ceramic composition. The ceramic composition may comprise less than 70.0 wt.%, e.g., less than 60.0 wt.%, e.g., less than 50.0 wt.%, e.g., less than 40.0 wt.%, e.g., less than 30.0 wt.%, e.g., less than 20.0 wt.%, of metal oxide component (a) based on the total weight of the ceramic composition. The ceramic composition may comprise 0.1 to 70.0 wt%, or 0.5 to 70.0 wt%, or 1.0 to 70.0 wt%, or 5.0 to 70.0 wt%, or 0.1 to 60.0 wt%, or 0.5 to 60.0 wt%, or 1.0 to 60.0 wt%, or 5.0 to 60.0 wt%, or 0.1 to 50.0 wt%, or 0.5 to 50.0 wt%, or 1.0 to 50.0 wt%, or 5.0 to 50.0 wt%, based on the total weight of the ceramic composition. The metal oxide component (a) may be contained in an amount ranging from 0.1 to 40.0% by weight, or from 0.5 to 40.0% by weight, or from 1.0 to 40.0% by weight, or from 5.0 to 40.0% by weight, or from 0.1 to 30.0% by weight, or from 0.5 to 30.0% by weight, or from 1.0 to 30.0% by weight, or from 5.0 to 30.0% by weight, or from 0.1 to 20.0% by weight, or from 0.5 to 20.0% by weight, or from 1.0 to 20.0% by weight, or from 5.0 to 20.0% by weight. According to the present disclosure, the ceramic composition may comprise the metal oxide component (a) in the range of 0.1 to 70.0 wt %, for example, 0.5 to 60.0 wt %, for example, 0.5 to 50.0 wt %, for example, 1.0 to 40.0 wt %, for example, 1.0 to 30.0 wt %, for example, 5.0 to 20.0 wt %, based on the total weight of the ceramic composition.

[0111] The ceramic composition may comprise at least 30.0 wt.%, e.g., at least 40.0 wt.%, e.g., at least 50.0 wt.%, e.g., at least 60.0 wt.%, e.g., at least 70.0 wt.%, e.g., at least 80.0 wt.% of a mullite balance component (b) based on the total weight of the ceramic composition. The ceramic composition may comprise at or less than 99.9 wt.%, at or less than 99.5 wt.%, e.g., at or less than 99.0 wt.%, e.g., at or less than 95.0 wt.% of a mullite balance component (b) based on the total weight of the ceramic composition. The ceramic composition may comprise 30.0 to 99.9 wt%, or 30.0 to 99.5 wt%, or 30.0 to 99.0 wt%, or 30.0 to 95.0 wt%, or 40.0 to 99.9 wt%, or 40.0 to 99.5 wt%, or 40.0 to 99.0 wt%, or 40.0 to 95.0 wt%, or 50.0 to 99.9 wt%, or 50.0 to 99.5 wt%, or 50.0 to 99.0 wt%, or 50.0 to 95.0 wt%, based on the total weight of the ceramic composition. The mullite balance component (b) may be in the range of 60.0 to 99.9 wt%, 60.0 to 99.5 wt%, 60.0 to 99.0 wt%, 60.0 to 95.0 wt%, 70.0 to 99.9 wt%, 70.0 to 99.5 wt%, 70.0 to 99.0 wt%, 70.0 to 95.0 wt%, 80.0 to 99.9 wt%, 80.0 to 99.5 wt%, 80.0 to 99.0 wt%, or 80.0 to 95.0 wt%. According to the present disclosure, the ceramic composition may comprise a mullite balance component (b) in the range of 30.0 to 99.9 wt %, or 40.0 to 99.9 wt %, or 50.0 to 99.5 wt %, or 60.0 to 99.0 wt %, or 70.0 to 95.0 wt %, or 80.0 to 95.0 wt %, based on the total weight of the ceramic composition.

[0112] The ceramic composition can be processed by standard ceramic processing procedures known to those skilled in the art. The ceramic composition according to the present disclosure can be ground into a fine powder by conventional grinding procedures, such as arc milling, mixed until homogeneity is achieved, and melted, typically at a temperature of 2,600°C. Melting can be carried out in an oxidizing atmosphere, such as air. The resulting molten material can be ground to a particle size, for example, in the range of 100 to 250 μm, and the powder can then be formed into a desired shape. Suitable procedures for processing ceramic compositions are disclosed, for example, in WO 99 / 01401 A1. The process of forming the ceramic composition can include high-pressure processing of the ceramic composition using a press to form the formed body of an object produced from the ceramic composition. The process of forming the ceramic composition into an object can further include further temperature treatments, such as sintering processes, and, if necessary, further pressure processes. Shaping the ceramic composition to form any object can include standard forming procedures, such as mechanical processing, powder processing, or ceramic injection molding. Thus, the ceramic composition can be formed into almost any shape by standard ceramic forming procedures.

[0113] According to the present disclosure, the intumescent coating composition or cured self-supporting film or sheet may be applied to any substrate known in the art, such as automotive substrates, marine substrates, industrial substrates, heavy equipment, packaging substrates, lumber, wood flooring and furniture, apparel, electronics including housings and circuit boards, consumer electronics such as housings for computers, notebooks, smartphones, tablets, televisions, gaming devices, computing equipment, computer accessories, MP3 players, etc., glass and transparencies, sporting goods such as golf balls, etc. The substrate to which the intumescent coating composition is applied may comprise a material selected from metal, plastic, ceramic, glass, wood, paper, paperboard, rubber, leather, textiles, existing coatings, or mixtures thereof.

[0114] The substrate may be part of a structure or a vehicle. As used herein, "structure" refers to buildings, bridges, transportation infrastructure, oil rigs, oil platforms, water towers, power transmission towers, support structures, wind turbines, walls, piers, docks, levees, dams, shipping containers, trailers, battery components, batteries, and any part of any metal structure exposed to a corrosive environment. As used herein, "vehicle" refers in its broadest sense to all types of vehicles, including, but not limited to, cars, trucks, buses, tractors, harvesters, heavy machinery, vans, golf carts, motorcycles, bicycles, rail cars, subway cars, airplanes, helicopters, boats of all sizes, and the like. The substrate may be part of a battery or a battery component.

[0115] The present disclosure further relates to substrates coated according to the methods of the present disclosure.

[0116] Additionally, the present disclosure is directed to articles comprising substrates coated according to the methods of the present disclosure.

[0117] An article according to the present disclosure may include a battery or a battery component. The battery may be, for example, an electric vehicle battery. According to the present disclosure, the battery may be a lithium-ion battery. As used herein, the term "battery component" refers to any component found in a battery, for example, a lithium-ion battery. According to the present disclosure, the battery component may be an electric vehicle battery component. The battery component may include an electrode, a battery cell, a battery shell, a battery module, a battery pack, a battery box, a battery cell casing, a pack shell, a battery lid, a battery tray, a thermal management system, a battery housing, a module housing, a module track, a battery side plate, a battery cell enclosure, a cooling module, a cooling tube, a cooling fin, a cooling plate, a bus bar, a battery frame, an electrical connection, a metal wire, a copper or aluminum conductor or cable, or any combination thereof.

[0118] The battery may include exterior wall elements defining a housing, and optionally interior wall elements, with the expandable coating composition or self-supporting film or sheet applied at least partially to the exterior and / or interior of either of the exterior wall elements, and / or to any side of either of the interior wall elements, if present. The exterior and / or interior wall elements may include composite, steel, aluminum, polycarbonate, or combinations thereof.

[0119] The battery, particularly a lithium-ion battery, may be a battery pack including a plurality of individual battery cells, with the intumescent coating composition or self-supporting film or sheet positioned between at least two of the individual battery cells to insulate them from each other in an expanded and, optionally, charred state. The battery may further include one or more additional flame-retardant materials and / or fire mitigation means, such as within and / or around the battery. For example, one or more additional flame-retardant materials and / or fire mitigation means may be wrapped or otherwise positioned between the battery cells or around or within the battery housing. Suitable examples of flame-retardant materials and / or fire mitigation means include glass fiber, mineral wool, silica, silica fiber, alumina, Kevlar, Nomex, calcium silicate, calcium silicate fiber, or combinations thereof, which may be, for example, in a sheet or other self-supporting form. Foams, such as polyurethane / polyurea foams with flame retardants, may also be used. Physical barriers, such as cooling fins interposed between battery cells, mica boards, aerogel blankets, mineral / glass / carbon fiber blankets, or combinations thereof, may also be used.

[0120] The article according to the present disclosure can be a battery or a battery component.

[0121] It is also within the scope of the present invention to apply a coating composition or a self-supporting film or sheet to a portion of the article adjacent to the battery between the battery and the article to provide fire protection to the article and its user. In such cases, conventional batteries or batteries according to the present disclosure may be used. The article may be, for example, a mobile phone, a tablet, or a laptop computer.

[0122] Alternatively, the article may include a vehicle, such as a hybrid or electric car, bus, or truck. In such vehicles, due to the weight of the battery, it is common for batteries, particularly lithium-ion batteries, to be positioned as a flat battery pack below the vehicle body, e.g., the floor of the vehicle body. In such cases, the intumescent coating or self-supporting film or sheet may be applied to the vehicle floor adjacent to the battery between the battery and the vehicle body. This allows the vehicle body, particularly the passenger cabin, to be protected by the cured intumescent coating or self-supporting film or sheet in the event of battery thermal runaway or battery fire, preventing the fire from spreading to the passenger cabin, and limiting the temperature rise in the passenger cabin for an extended period of time so that passengers have sufficient time to safely escape from the vehicle in the event of such an event. Alternatively, the article may include a structure.

[0123] The present disclosure further relates to the use of an intumescent coating composition according to the present disclosure in a method for curing an intumescent coating composition by irradiating the composition with pulsed infrared radiation.The present disclosure further relates to the use of pulsed infrared radiation in a method for curing an intumescent coating composition.

[0124] As used herein, unless expressly specified otherwise, all numbers, such as those expressing values, ranges, amounts, or percentages, may be read as if preceded by the word "about," even if the term does not explicitly appear.

[0125] The following examples are intended to illustrate the present disclosure and should not be construed as limiting the disclosure in any way. [Brief explanation of the drawings]

[0126] [Figure 1] Figure 1 shows intumescent coatings cured using pulsed infrared light at 50% power from 20 cm for 14 minutes (a), at 100% power from 30 cm for 7 minutes (b), and at 90°C for 25 minutes using oven heating (c). [Figure 2] Figure 1 shows char formation after 5 minutes at 1200°C for intumescent coatings cured for 10 days using (a) oven heating at 90°C for 120 minutes, (b) pulsed infrared at 50% power from 20 cm for 30 minutes, (c) pulsed infrared at 100% power from 30 cm for 20 minutes, and (d) room temperature. [Example]

[0127] Preparation of Expandable Coating Composition Coating formulations were prepared using the ingredients shown in Table 1 (base formulation) and Table 2 (hardener formulation). [Table 1] [Table 2]

[0128] The base for the formulations was prepared by dispersing all components in a disperser equipped with a 0.75-1 kW Brook Crompton motor at a rotation speed of 2000-3000 rpm and a dispersing plate diameter of 80-90 mm until the particles in the formulation were less than 100 microns in size. The curing agent for the coating formulations was prepared by dispersing all components in a disperser equipped with a 0.75-1 kW Brook Crompton motor at a rotation speed of 2000-3000 rpm and a dispersing plate diameter of 80-90 mm until the particles in the formulation were less than 100 microns in size. Just before application, the base and curing agent were mixed in the relative amounts shown in Tables 1 and 2. The base and curing agent were mixed with a mixer or spatula until the mixture was homogeneous in color and free of lumps. The coating formulations were applied to 150 x 75 x 1.2 mm aluminum panels using an airless spray application.

[0129] Curing coated substrates using pulsed infrared and conventional curing Substrates coated with the intumescent coating compositions shown above were cured using a pulsed infrared light source IR.X Infrarot Modul D2 commercially available from SPS Group GmbH (Germany). The following settings of the pulsed infrared light source were applied, as shown in Table 3: [Table 3]

[0130] The pulsed infrared light source faced the substrate coated with the coating composition to be cured at various distances, as shown in Table 4. The light source IR.X Infrarot Modul D2 has a power of 2000 W when 100% power is applied. Therefore, 50% power represents 1000 W of power. [Table 4]

[0131] Cure time refers to the time to achieve a cured coating that is dry enough to handle. Dry enough to handle means that the coated surface or film, when subjected to typical handling pressures, does not show undesirable marks, peeling, loosening, wrinkling, or other forms of distortion, as can be determined by a Shore A hardness tester, which must exceed 55. Thickness was determined according to DIN EN ISO 2178:2016.

[0132] Conventional curing is achieved using heated air in an oven at 90°C for 30 minutes, after which the coating is dry enough to handle. Cure times are significantly longer to achieve a cured coating.

[0133] Fire testing of cured intumescent coatings Coatings applied to 150x75x1.2mm aluminum panels and cured by pulsed infrared radiation, as well as oven curing at room temperature (approximately 25°C), were subjected to a 10-minute torch test at 1200±50°C. The temperature of the backside of the aluminum panel was monitored. Additionally, the expansion coefficient was determined, which indicates the ratio between the char thickness before the fire test and the cured coating. The results are summarized in Table 5 below. [Table 5]

[0134] As can be seen from the above results, curing using pulsed infrared radiation results in similar fire performance of the intumescent coating compared to conventionally cured intumescent coatings. Cure times can be significantly reduced while maintaining the fire performance of the cured coating. The following is further disclosed in relation to the present invention. [1] 1. A method of imparting fire resistance to a substrate, comprising: (I) (i) applying an intumescent coating composition to a portion of a surface of the substrate, or (ii) forming the intumescent coating composition into a self-supporting film or sheet; (II) irradiating (i) the applied intumescent coating composition or (ii) the self-supporting film or sheet with pulsed infrared light to form a cured intumescent coating or a cured self-supporting film or sheet, and applying the self-supporting film or sheet to a portion of a surface of the substrate. [2] The expandable coating composition comprises: (a) a film-forming resin; (b) a cross-linking agent; (c) a compound that provides an expanding gas upon thermal decomposition. [3] [2] The method according to [2], wherein the film-forming resin (a) comprises an epoxy resin, an acrylic resin, a polyurethane resin, a polyvinyl resin, a urea-formaldehyde resin, a polyimide resin, a melamine resin, a polyester resin, a cyanate resin, a copolymer thereof, or a mixture thereof. [4] The method according to [2] or [3], wherein the film-forming resin (a) comprises an epoxy resin. [5] The method according to any one of [2] to [4], wherein the crosslinking agent (b) comprises a polyamine, such as a polyetheramine, a polyamide, a polyepoxide, an aminoplast resin, a phenolic resin, a polyisocyanate, a polythiol, a polyol, a copolymer thereof, or a mixture thereof. [6] The method according to any one of [2] to [5], wherein the crosslinking agent (b) contains a polyamine. [7] The method according to any one of [2] to [6], wherein the compound (c) that provides an expanding gas upon thermal decomposition comprises melamine, a melamine derivative, guanidine, methylol melamine, hexamethoxymethyl melamine, urea, dimethyl urea, melamine pyrophosphate, dicyandiamide, guanylurea phosphate, glycine, an alkaline earth metal carbonate, calcium hydroxide, magnesium dihydroxide, aluminum trihydroxide, expandable graphite, or a mixture thereof. [8] The method according to any one of [2] to [7], wherein the compound (c) that provides an expanding gas upon thermal decomposition comprises melamine, a melamine derivative, methylol melamine, hexamethoxymethyl melamine, melamine pyrophosphate, or a mixture thereof. [9] The method of any of the preceding claims, wherein the expandable coating composition comprises an epoxy reactive diluent.

[10] [9] The method of [9], wherein the epoxy-reactive diluent comprises a diglycidyl ether of an aliphatic alcohol.

[11] The method of any of the preceding claims, wherein the expandable coating composition comprises a phosphate compound.

[12]

[11] The method according to

[11] , wherein the phosphate compound comprises phosphoric acid, monoammonium phosphate and diammonium phosphate, triphenyl phosphate, tris-(2-chloroethyl) phosphate, tris-(2-chloroisopropyl) phosphate, ammonium polyphosphate, and melamine pyrophosphate.

[13] The method of any of the preceding claims, wherein the expandable coating composition comprises a borate compound.

[14]

[13] The method of

[13] , wherein the borate compound comprises ammonium pentaborate, boric acid, a metal borate, boron oxide, sodium borate, potassium borate, ammonium borate, butyl borate, phenyl borate, or a mixture thereof.

[15] The method of any of the preceding claims, wherein the expandable coating composition comprises an aluminum compound.

[16]

[15] The method according to

[15] , wherein the aluminum compound comprises aluminum hydroxide, aluminum oxide, aluminum chloride, or a mixture thereof.

[17] The method of any of the preceding claims, wherein the expandable coating composition comprises a silica compound.

[18]

[17] The method of

[17] , wherein the silica compound comprises fumed silica, quartz, or a mixture thereof.

[19] The intumescent coating composition comprises TiO 2 2. The method according to claim 1, wherein the first and second electrodes are connected to each other.

[20] The method of any preceding claim, wherein the intumescent coating composition comprises a fibrous reinforcement material.

[21]

[20] The method according to

[20] , wherein the fibrous reinforcement comprises mineral fibers, ceramic fibers, glass fibers, carbon fibers, basalt fibers, or mixtures thereof.

[22] Any of the preceding methods, wherein the intumescent coating composition is applied to the substrate at a dry film thickness in the range of 0.1 mm to 15 mm, or the intumescent coating composition is formed into a self-supporting film or sheet having a dry film thickness in the range of 0.1 mm to 15 mm.

[23] Any of the above-mentioned methods, wherein the pulsed infrared radiation has a peak wavelength in the range of 3 μm to 10 μm, for example, 3 μm to 6 μm.

[24] Any of the preceding methods, wherein the pulsed infrared radiation is irradiated with a pulse duration of less than 100 μs.

[25] The method according to any one of the above, wherein the pulsed infrared rays are irradiated with a pulse duration in the range of 5 μs to 15 μs, for example, 8 μs to 12 μs, or 10 μs to 14 μs.

[26] The method according to any one of the above, wherein the pulsed infrared rays are irradiated with a pulse frequency of 350 Hz to 450 Hz, or 400 Hz to 450 Hz.

[27] The pulsed infrared rays are irradiated with an impact energy of 250 W / cm 2 ~350 W / cm 2 The method according to any one of the above.

[28] The method according to any one of the above, wherein the pulsed infrared rays are irradiated for a time of less than 25 minutes, or less than 20 minutes, or less than 15 minutes, or less than 10 minutes to form a cured coating or a cured self-supporting film or sheet.

[29] The method according to any one of the above, wherein the surface temperature of the substrate in (II) is less than 100 °C, or less than 90 °C.

[30] The method according to any one of the above, wherein the pulsed infrared radiation surface of the infrared light source in (II) is at a distance of 5 cm to 50 cm, for example, 5 cm to 30 cm, or 5 cm to 15 cm, or 10 cm to 20 cm, or 15 cm to 25 cm, facing the surface of the substrate coated with the coating composition to be cured, or the surface of the self-supporting film or sheet to be cured.

[31] The method according to any one of the above, wherein the pulsed infrared rays are provided by an infrared light source including a surface containing a ceramic composition capable of absorbing heat and emitting infrared rays having a peak wavelength in the range of 3 μm to 10 μm.

[32] The method according to any one of the above, wherein a part of the surface of the substrate to which the coating composition or the self-supporting film or sheet is applied contains a material selected from metal, plastic, ceramic, glass, wood, paper, cardboard, rubber, leather, fabric, an existing coating, or a mixture thereof.

[33] Use of an expandable coating composition in a method of curing an expandable coating composition by irradiating with pulsed infrared rays.

[34] Use of pulsed infrared rays in a method of curing an expandable coating composition.

[35] A substrate coated according to the method according to any one of [1] to

[32] .

[36] An article comprising the substrate according to

[35] .

[37] The article according to

[36] , wherein the article includes a battery or a battery component.

[38] The article according to

[37] , wherein the battery is a lithium ion battery.

[39] The article of

[37] or

[38] , wherein the battery comprises an electric vehicle battery or an electric vehicle battery component.

[40] The article according to any one of

[37] to

[39] , wherein the battery comprises outer wall elements defining a housing and, optionally, inner wall elements, and the expandable coating composition or self-supporting film or sheet is applied at least partially to the outside and / or inside of any of the outer wall elements, and / or, if present, to any side of any of the inner wall elements.

[41]

[40] The article of

[40] , wherein any of the exterior wall elements and / or interior wall elements comprises composite, steel, aluminum, polycarbonate, or a combination thereof.

[42] The article of any of

[37] to

[41] , wherein the battery is a battery pack including a plurality of individual battery cells, the coating composition or self-supporting film or sheet is positioned to insulate at least two of the individual battery cells from each other in an expanded state and optionally in a charred state, and the battery optionally includes one or more additional flame retardant materials and / or fire mitigation means.

[43] The article according to any one of

[37] to

[39] , wherein the battery component comprises an electrode, a battery cell, a battery shell, a battery module, a battery pack, a battery box, a battery cell casing, a pack shell, a battery lid, a battery tray, a thermal management system, a battery housing, a module housing, a module tracker, a battery side plate, a battery cell enclosure, a cooling module, a cooling tube, a cooling fin, a cooling plate, a bus bar, a battery frame, an electrical connection, a metal wire, a copper or aluminum conductor or cable, or any combination thereof.

[44] The method of claim 36, wherein the article comprises a vehicle.

[45] The method of claim 36, wherein the article comprises a structure.

Claims

1. 1. A method of imparting fire resistance to a substrate, comprising: (I) (i) applying an intumescent coating composition to a portion of a surface of the substrate, or (ii) applying an intumescent coating composition formed into a self-supporting film or sheet to a portion of a surface of the substrate; (II) irradiating (i) the applied intumescent coating composition or (ii) the self-supporting film or sheet with pulsed infrared light to form a cured intumescent coating or a cured self-supporting film or sheet on a portion of a surface of the substrate, Moreover, the expandable coating composition is (a) a film-forming resin; (b) a cross-linking agent; and (c) a compound that provides an expansion gas upon thermal decomposition; one or both of (a) and (b) are liquids; Moreover, the substrate comprises a material selected from metal, plastic, ceramic, paper, paperboard, rubber, leather, textile, a pre-existing coating, or a mixture thereof.

2. 10. The method of claim 1, wherein the film-forming resin (a) comprises an epoxy resin, an acrylic resin, a polyurethane resin, a polyvinyl resin, a urea-formaldehyde resin, a polyimide resin, a melamine resin, a polyester resin, a cyanate resin, a copolymer thereof, or a mixture thereof.

3. The method of claim 1 or 2, wherein the film-forming resin (a) comprises an epoxy resin.

4. 3. The method of claim 1 or 2, wherein the crosslinking agent (b) comprises a polyamine, the polyamine comprising a polyetheramine, a polyamide, a polyepoxide, an aminoplast resin, a phenolic resin, a polyisocyanate, a polythiol, a polyol, a copolymer thereof, or a mixture thereof.

5. The method of claim 1 or 2, wherein the cross-linking agent (b) comprises a polyamine.

6. 3. The method of claim 1 or 2, wherein the compound (c) that provides an expanding gas upon thermal decomposition comprises melamine, a melamine derivative, guanidine, methylol melamine, hexamethoxymethyl melamine, urea, dimethyl urea, melamine pyrophosphate, dicyandiamide, guanylurea phosphate, glycine, an alkaline earth metal carbonate, calcium hydroxide, magnesium dihydroxide, aluminum trihydroxide, expandable graphite, or a mixture thereof.

7. 3. The method of claim 1 or 2, wherein the compound (c) that provides an expanding gas upon thermal decomposition comprises melamine, a melamine derivative, a methylolated melamine, hexamethoxymethyl melamine, melamine pyrophosphate, or a mixture thereof.

8. The method of claim 1 or 2, wherein the expandable coating composition comprises an epoxy reactive diluent.

9. The method of claim 8 , wherein the epoxy-reactive diluent comprises a diglycidyl ether of an aliphatic alcohol.

10. The method of claim 1 or 2, wherein the expandable coating composition comprises a phosphate compound.

11. 11. The method of claim 10, wherein the phosphate compounds include phosphoric acid, mono- and di-ammonium phosphate, triphenyl phosphate, tris-(2-chloroethyl) phosphate, tris-(2-chloroisopropyl) phosphate, ammonium polyphosphate, melamine pyrophosphate.

12. The method of claim 1 or 2, wherein the expandable coating composition comprises a borate compound.

13. 13. The method of claim 12, wherein the borate compound comprises ammonium pentaborate, boric acid, metal borates, boron oxide, sodium borate, potassium borate, ammonium borate, butyl borate, phenyl borate, or a mixture thereof.

14. The method of claim 1 or 2, wherein the intumescent coating composition comprises an aluminum compound.

15. 15. The method of claim 14, wherein the aluminum compound comprises aluminum hydroxide, aluminum oxide, aluminum chloride, or a mixture thereof.

16. The method of claim 1 or 2, wherein the expandable coating composition comprises a silica compound.

17. 17. The method of claim 16, wherein the silica compound comprises fumed silica, quartz, or a mixture thereof.

18. The expandable coating composition comprises TiO ２ 3. The method of claim 1 or 2, comprising:

19. The method of claim 1 or 2, wherein the intumescent coating composition comprises a fibrous reinforcement material.

20. 20. The method of claim 19, wherein the fibrous reinforcement comprises mineral fibers, ceramic fibers, glass fibers, carbon fibers, basalt fibers, or mixtures thereof.

21. 3. The method of claim 1 or 2, wherein the intumescent coating composition is applied to the substrate at a dry film thickness ranging from 0.1 mm to 15 mm, or the intumescent coating composition is formed into a self-supporting film or sheet having a dry film thickness ranging from 0.1 mm to 15 mm.

22. 3. The method according to claim 1, wherein the pulsed infrared radiation has a peak wavelength in the range of 3 μm to 10 μm.

23. The method of claim 1 or 2, wherein the pulsed infrared radiation is applied with a pulse duration of less than 100 μs.

24. 3. The method of claim 1, wherein the pulsed infrared radiation is applied with a pulse duration in the range of 5 μs to 15 μs.

25. The method according to claim 1 or 2, wherein the pulsed infrared radiation is irradiated at a pulse frequency of 350 Hz to 450 Hz, or 400 Hz to 450 Hz.

26. The pulsed infrared ray is 250 W / cm ２ ~350 W / cm ２ The method according to claim 1 or 2, wherein the irradiation is performed with an impact energy of 0.05 wt.

27. 3. The method of claim 1 or 2, wherein the pulsed infrared radiation is applied for a period of less than 25 minutes, or less than 20 minutes, or less than 15 minutes, or less than 10 minutes to form a cured coating or a cured self-supporting film or sheet.

28. The method according to claim 1 or 2, wherein the surface temperature of the substrate in (II) is less than 100°C, or less than 90°C.

29. 3. The method according to claim 1 or 2, wherein the pulsed infrared emitting surface of the infrared light source in (II) faces the surface of the substrate on which the coating composition to be cured has been applied, or the surface of the self-supporting film or sheet to be cured, at a distance of 5 cm to 50 cm.

30. 3. The method of claim 1 or 2, wherein the pulsed infrared radiation is provided by an infrared light source comprising a surface comprising a ceramic composition capable of absorbing heat and emitting infrared radiation having a peak wavelength in the range of 3 μm to 10 μm.

31. Use of an intumescent coating composition in a method for curing the intumescent coating composition by irradiating it with pulsed infrared radiation.

32. Use of pulsed infrared radiation in a method for curing an intumescent coating composition.

Images