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A Coating Composition And A Process For Its Preparation

Abstract: ABSTRACT A COATING COMPOSITION AND A PROCESS FOR ITS PREPARATION The present disclosure relates to a coating composition and a process for its preparation. The coating composition comprises a siloxane modified acrylic polyol polymer, at least one curing agent, at least one fluid medium, at least one additive, optionally at least one acid catalyst, optionally nanoparticles, and optionally at least one polyolefinic component. The present disclosure also provides a process for the preparation of siloxane modified acrylic polyol polymer. The coating composition of the present disclosure has a self-cleaning, easy to clean and anti-graffiti properties.

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Patent Information

Application #
Filing Date
25 November 2020
Publication Number
21/2022
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
Parent Application
Patent Number
Legal Status
Grant Date
2023-07-10
Renewal Date

Applicants

ASIAN PAINTS LIMITED
6A Shantinagar, Santacruz (E) Mumbai Maharashtra INDIA 400 055

Inventors

1. MIRCHANDANI, Girish
c/o Asian Paints Ltd.,R&T Centre Turbhe Navi Mumbai Maharashtra INDIA 400703
2. BENDALE, Nitin
c/o Asian Paints Ltd.,R&T Centre Turbhe Navi Mumbai Maharashtra INDIA 400703
3. BASUTKAR, Sachin
c/o Asian Paints Ltd.,R&T Centre Turbhe Navi Mumbai Maharashtra INDIA 400703
4. SHYAMROY, Subarna
c/o Asian Paints Ltd.,R&T Centre Turbhe Navi Mumbai Maharashtra INDIA 400703
5. BHOWMICK, Shibaji
c/o Asian Paints Ltd.,R&T Centre Turbhe Navi Mumbai Maharashtra INDIA 400703

Specification

DESC:FIELD
The present disclosure relates to a coating composition and a process for its preparation.
DEFINITIONS
As used in the present disclosure, the following terms are generally intended to have the meaning as set forth below, except to the extent that the context in which they are used indicates otherwise.
Flow and leveling additive: The term “flow and leveling additive” refers to a molecule/compound which improves the flow and levelling of the coating and provides a defect free uniform appearance.
Anti-graffiti coating: The term “anti-graffiti coating” refers to a coating that prevents graffiti paint from bonding to surfaces.
Slip property: The term “slip property” refers to a co-efficient of friction of the coating surface.
Mar resistance property: The term “mar resistance property” refers to the resistance to physical damage on the surface of the coating during its lifespan.
Viscosity on Gardner Scale: The term “viscosity on Gardner Scale” refers to the measurement of kinetic viscosity of liquids in BYK-Gardner bubble viscosity tubes. The viscosity of the liquid being tested is directly proportional to the amount of time that it takes the bubble in the tube to rise. A bubble that rises quickly shows a low range of viscosity.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
Dust deposition on various surfaces such as household and industrial appliances is a major concern affecting aesthetic value of coated surfaces. Especially, oil stains and oily dust on coating surfaces are very difficult to remove from the coating surfaces. To address this problem, self-cleaning coating compositions and coatings which are easy to clean are produced. To achieve self and easy cleaning coatings, specialty raw materials based on fluorinated and fluorosilicone binders and additives are used. These specialty raw materials are required in high amounts to achieve enhanced self/easy cleaning property. However, the fluorinated and fluorosilicone binders and additives are high cost, making the self/easy cleaning coating expensive.
Further, low molecular weight polydimethyl siloxane based glycols/polyols are often blended in paints and coating compositions for the applications such as (i) the modification of the surface energy (stratification), (ii) anti-graffiti property, and (iii) flow and leveling property. However, in these applications, incorporation of polydimethyl siloxane based glycols/polyols during synthesis leads to either opacification or translucency of the paints and the coating composition.
Therefore, there is felt a need to provide a coating composition and a process for the preparation of a coating composition that mitigates the drawback mentioned herein above.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows:
An object of the present disclosure is to ameliorate one or more problems of the prior art or to at least provide a useful alternative.
Another object of the present disclosure is to provide a coating composition.
Still another object of the present disclosure is to provide a coating composition, which when applied on a surface can be cleaned easily.
Yet another object of the present disclosure is to provide a coating composition that has an anti-graffiti property.
Still another object of the present disclosure is to provide a coating composition that is fluorine free and durable.
Yet another object of the present disclosure is to provide a coating composition which can dry wipe the stains without the use of hazardous solvents.
Yet another object of the present disclosure is to provide a coating composition which is economical.
Still another object of the present disclosure is to provide a coating composition which comprises siloxane modified acrylic polyol polymer.
Yet another object of the present disclosure is to provide a process for the preparation of siloxane modified acrylic polyol polymer.
Another object of the present disclosure is to provide a process for the preparation of a coating composition.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.
SUMMARY
The present disclosure relates to a coating composition. The coating composition comprises 60 to 70 mass% of a siloxane modified acrylic polyol polymer, 5 to 40 mass% of at least one curing agent, 15 to 25 mass% of at least one fluid medium; 0.1 to 3 mass% of at least one additive, optionally 0.5 to 1.5 mass% of at least one acid catalyst, optionally 0.1 to 5 mass% of nanoparticles, and optionally 0.1 to 5 mass% of at least one polyolefinic component, wherein mass % of each component is with respect to the total mass of the composition.
The present disclosure further relates to a process for the preparation of a siloxane modified acrylic polyol polymer. The process comprises mixing predetermined amounts of at least one first monomer, at least one second monomer, at least one siloxane monomer, and at least one first initiator, in at least one fluid medium in a reactor at a first predetermined temperature for a first predetermined time period in the presence of an inert gas to obtain a mixture; digesting the mixture at a second predetermined temperature for a second predetermined time period to obtain a digested mixture; adding a second initiator to the digested mixture followed by reacting at a third predetermined temperature for a third predetermined time period to obtain a reaction mixture; cooling the reaction mixture to a fourth predetermined temperature followed by mixing in a second fluid medium for a fourth predetermined time period to obtain a cooled mixture having a solid content in the range of 40 to 80 mass% of the total mass of the siloxane modified acrylic polyol polymer; and filtering said cooled mixture to obtain the siloxane modified acrylic polyol polymer.
The present disclosure still further relates to a process for the preparation of a coating composition. The process comprising mixing predetermined amounts of at least one curing agent, at least one fluid medium, at least one additive, optionally an acid catalyst, and optionally nanoparticles to a predetermined amount of siloxane modified acrylic polyol polymer of the present disclosure at a fifth predetermined temperature for fifth predetermined time period to obtain the coating composition.
DETAILED DESCRIPTION
Embodiments are provided so as to thoroughly and fully convey the scope of the present disclosure to the person skilled in the art. Numerous details are set forth, relating to specific components, and methods, to provide a complete understanding of embodiments of the present disclosure. It will be apparent to the person skilled in the art that the details provided in the embodiments should not be construed to limit the scope of the present disclosure. In some embodiments, well-known processes, well-known apparatus structures, and well-known techniques are not described in detail.
The terminology used, in the present disclosure, is only for the purpose of explaining a particular embodiment and such terminology shall not be considered to limit the scope of the present disclosure. As used in the present disclosure, the forms "a,” "an," and "the" may be intended to include the plural forms as well, unless the context clearly suggests otherwise. The terms "comprises," "comprising," “including,” and “having,” are open ended transitional phrases and therefore specify the presence of stated features, integers, steps, operations, elements, modules, units and/or components, but do not forbid the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. The particular order of steps disclosed in the method and process of the present disclosure is not to be construed as necessarily requiring their performance as described or illustrated. It is also to be understood that additional or alternative steps may be employed.
Coating applied on the surfaces such as household and industrial appliances loses its aesthetic value because of the dust deposition. Hence, maintaining the cleanliness of the applied coating is a significant challenge which can be addressed by the use of self-cleaning coatings and the coating compositions which can be easily cleaned. To prepare self-cleaning and easy cleaning coatings, cross-linked polymers based on high-cost fluorinated and fluorosilicone binders and additives are conventionally used which make the self/easy cleaning coating expensive.
In an aspect, the present disclosure provides a coating composition. The coating composition comprises 60 to 70 mass% of a siloxane modified acrylic polyol polymer, 5 to 40 mass% of at least one curing agent, 15 to 25 mass% of at least one first fluid medium, 0.1 to 3 mass% of at least one additive, optionally 0.5 to 1.5 mass% of at least one acid catalyst, optionally 0.1 to 5 mass% of at least one nanoparticle, and optionally 0.1 to 5 mass% of at least one polyolefinic component with respect to the total mass of the composition.
In accordance with the present disclosure, the siloxane modified acrylic polyol polymer is a product of 0.1 to 10 mass% of a siloxane monomer, 90 to 99.9 mass% of an acrylic polyol with respect to the total mass of the siloxane modified acrylic polyol polymer.
In accordance with an embodiment of the present disclosure, the siloxane monomer is in the range of 0.1 to 5 mass% of the total mass of the siloxane modified acrylic polyol polymer.
In accordance with another embodiment of the present disclosure, the siloxane monomer is in the range of 0.1 to 1 mass% of the total mass of the siloxane modified acrylic polyol polymer.
In accordance with the present disclosure, the predetermined amount of the siloxane modified acrylic polyol polymer is in the range of 60 to 70 mass% with respect to the total mass of the coating composition. In an exemplary embodiment, the predetermined amount of siloxane modified acrylic polyol polymer is 65 mass%.
In accordance with the present disclosure, the siloxane monomer has an average molecular weight in the range of 500 g/mole to 4,000 g/mole.
In accordance with the present disclosure, the siloxane monomer is functionalized using the compound selected from vinyl, acryl, hydroxyl, alkoxy, epoxy, amine and carboxyl. In an exemplary embodiment, the siloxane monomer is functionalized using an acrylic compound.
In accordance with the present disclosure, the acrylic polyol component has a hydroxyl value in the range of 50 mg KOH/g to 200 mg KOH/g.
In accordance with the present disclosure, the acrylic polyol has an acid value in the range of 0 to 25 mg KOH/g on solids. In accordance with an embodiment of the present disclosure, the acrylic polyol has an acid value in the range of 5 to 15 mg KOH/g.
In accordance with the present disclosure, the acrylic polyol has a glass transition temperature (Tg) in the range of -60 to +60 °C. In accordance with an embodiment of the present disclosure, the acrylic polyol has a glass transition temperature (Tg) in the range of 20 to 50 °C.
In accordance with the present disclosure, the acrylic polyol has an average molecular weight in the range of 1000 to 30000 Da. In accordance with an embodiment of the present disclosure, the acrylic polyol has an average molecular weight in the range of 2000 to 20000 Da.
In accordance with the present disclosure, the acrylic polyol is a product of a first monomer and a second monomer.
In accordance with the present disclosure, the first monomer is a hydroxy acrylate monomer at least one selected from the group consisting of hydroxyl ethyl acrylate, hydroxyl-ethoxyethyl acrylate, hydroxyl-poly(ethoxy)ethyl acrylate, hydroxymethyl acrylate, hydroxypropyl acrylate, hydroxylbutyl acrylate, hydroxyethyl methacrylate, hydroxyl-ethoxyethyl methacrylate, hydroxyl-poly(ethoxy)ethyl methacrylate, hydroxymethyl methacrylate, hydroxypropyl methacrylate, and hydroxylbutyl methacrylate. In an exemplary embodiment, the first monomer is a hydroxyl ethyl methacrylate.
In accordance with the present disclosure, the second monomer is selected from the group consisting of acrylate monomer, vinyl monomer and carboxyl functional monomer.
In accordance with the present disclosure, the acrylate monomer is at least one selected from the group consisting of alkyl (C1-C20) acrylate monomer, and alkyl (C1-C20) methacrylate monomer. Other longer chain acrylic monomers can also be used.
In accordance with an embodiment of the present disclosure, the acrylate monomer is selected from the group consisting of methyl acrylate monomer, ethyl acrylate monomer, n-propyl acrylate monomer, isopropyl acrylate monomer, n-butyl acrylate monomer, isobutyl acrylate monomer, sec-butyl acrylate monomer, tert-butyl acrylate monomer, n-pentyl acrylate monomer, neopentyl acrylate monomer, n-hexyl acrylate monomer, cyclohexyl acrylate monomer, n-octyl acrylate monomer, 2- ethylhexyl acrylate monomer, lauryl acrylate monomer, cetyl acrylate monomer, stearyl acrylate monomer, eicosyl acrylate monomer and isobornyl acrylate monomer.
In accordance with another embodiment of the present disclosure, the acrylate monomer is selected from the group consisting of methyl methacrylate monomer, ethyl methacrylate monomer, n-propyl methacrylate monomer, isopropyl methacrylate monomer, n-butyl methacrylate monomer, isobutyl methacrylate monomer, sec-butyl methacrylate monomer, tert-butyl methacrylate monomer, n-pentyl methacrylate monomer, neopentyl methacrylate monomer, n-hexyl methacrylate monomer, cyclohexyl methacrylate monomer, n-octyl methacrylate monomer, 2- ethylhexyl methacrylate monomer, lauryl methacrylate monomer, cetyl methacrylate monomer, stearyl methacrylate monomer, eicosyl methacrylate monomer and isobornyl methacrylate monomer.
In accordance with the present disclosure, the vinyl monomer is selected from the group consisting of styrene, alpha-methyl styrene and para-methyl styrene.
In accordance with the present disclosure, the carboxyl functional monomer is selected from the group consisting of acrylic acid, methacrylic acid, fumaric acid, crotonic acid, itaconic acid, maleic acid, cinnamic acid and 2-acrylamide-2-methylpropanesulfonic acid.
In an exemplary embodiment of the present disclosure, the second monomer is a mixture of butyl acrylate, butyl methacrylate, methyl methacrylate, and methacrylic acid.
In accordance with the present disclosure, the curing agent is at least one selected from the group consisting of polyisocyanate, blocked polyisocyanates, isocyanate functional silanes, melamine formaldehyde, urea formaldehyde, unimolecular amines, unimolecular amides, unimolecular amido-amines, unimolecular imido-amines, polyamines, polyamides, polyamido-amines, benzoguanamine formaldehyde and polyimido-amines. In an exemplary embodiment, the curing agent is melamine formaldehyde.
In accordance with an embodiment of the present disclosure, amino resin such as melamine formaldehyde or urea formaldehyde containing an imino group is used as a curing agent. The melamine resin is selected from the group consisting of methyl melamine resin, butyl melamine resin, mixed alkyl melamine resin containing high imino groups, methylated melamine resin containing high imino groups and butylated melamine resin containing high imino groups. The solid content of the melamine resin is in the range of 70 to 100 mass%. Cymel 323, Cymel 325, Cymei 1130 and Cymel U 65 are some examples of aminoplastic resins from Allnex. Melamine formaldehyde without imino group are also used as a curing agent.
In accordance with the present disclosure, the amount of the curing agent is in the range of 5 to 40 mass% with respect to the total mass of the coating composition. In an exemplary embodiment, the predetermined amount of the curing agent is 12 mass%.
In accordance with the present disclosure, the fluid medium is at least one selected from the group consisting of aromatic hydrocarbons, aliphatic esters, alcohols, ketones, ethers and glycol ethers. In accordance with an embodiment of the present disclosure, the fluid is are selected from butyl acetate, butyl carbitol acetate, butanol, ortho xylene, and methyl isobutyl ketone.
In accordance with the present disclosure, the amount of the at least one fluid medium is in the range of 15 to 25 mass% with respect to the total mass of the coating composition. In an exemplary embodiment, the amount of the fluid medium is 21 mass%.
In accordance with the present disclosure, the acid catalyst is at least one selected from the group consisting of p-toluene sulfonic acid, dodecylbenzene sulfonic acid, amineblocked alkylated benzene sulfonic acids, and phosphoric acids. The acid catalyst are used to enhance the cross linking reaction between the siloxane modified acrylic polyol polymer and curing agent (amino resin).
In accordance with the present disclosure, the amount of the acid catalyst is in the range of 0.5 to 1.5 mass% with respect to the total mass of the coating composition. In an exemplary embodiment, the amount of the acid catalyst is 1 mass%.
The acid catalyst is added for certain types of curing agents such as melamine formaldehyde and urea formaldehyde (amino resins) to accelerate the cross-linking reaction between the siloxane modified acrylic polyol polymer and the curing agent (such as melamine formaldehyde). The quantity and content of the acid catalyst depends on the reactivity of the amino resin. Certain amino such as imino functional melamine formaldehyde does not require the acid catalyst or very low content of acid catalyst since it is self-catalyzed. Other less reactive types require higher quantity of the acid catalyst.
In accordance with the present disclosure, the nanoparticles are selected from the group consisting of silica nanoparticles, alumina nanoparticles, titania nanoparticles, carbon nanotubes, graphene nanoparticles and zinc oxide nanoparticles. In accordance with an embodiment of the present disclosure, the nanoparticle is silica nanoparticle.
In accordance with the present disclosure, the amount of the nanoparticles in the range of 0.1 to 5 mass% with respect to the total mass of the coating composition.
In accordance with the present disclosure, a particle size of the nanoparticles is in the range of 1 nm to 200 nm. In accordance with an embodiment of the present disclosure, the particle size of the silica nanoparticles is <100 nm.
In accordance with the present disclosure, the nanoparticles are surface treated with a hydrophobic group. The hydrophobic group is an alkyl disilazane at least one selected from the group consisting of hexamethyldisilazane, alkysilanes, alkylchlorosilanes and dimethyldichlorosilane. In accordance with an embodiment of the present disclosure, the hydrophobic group is hexamethyldisilazane.
In accordance with the present disclosure, the polyolefinic component is selected from the group consisting of polypropylene, polyethylene and copolymers of polypropylene and polyethylene. In accordance with an embodiment of the present disclosure, the polyolefinic component is polyproplylene.
In accordance with the present disclosure, the polyolefinic component is grafted on the siloxane modified acrylic polyol polymer.
In accordance with the present disclosure, the siloxane modified acrylic polyol polymer is mixed with a polyolefinic component and heated at a temperature in the range of 120 °C to 170 °C in the presence of the fluid medium, to obtain the desired grafting. In accordance with an embodiment of the present disclosure, the fluid medium is selected from the group consisting of aromatic, aliphatic, cycloaliphatic hydrocarbons, esters, ketones, and glycol ethers.
In accordance with the present disclosure, the amount of the polyolefinic component is in the range of 0.1 to 5 mass% with respect to the total mass of the coating composition.
In accordance with the present disclosure, the polyolefinic component has an average molecular weight, as measured by using gel permeation chromatography, in the range of 3,000 to 30,000 Da. The polyolefinic component has an acid value in the range of 30 mg KOH/g to 100 mg KOH/g.
In accordance with the present disclosure, the additive is at least one selected from the group consisting of wetting agent, dispersing agent, fluorosurfactant, plasticizer, flow and levelling additive, rheological agent, defoamer, adhesion promoter and silane.
In accordance with the present disclosure, the wetting agent is a block copolymer with ionic or non-ionic pigment affinic groups. In accordance with an embodiment of the present disclosure, the wetting agent is at least one selected from the group consisting of Disperbyk 102, Disperbyk 103, Disperbyk 160, Disperbyk 161, Disperbyk 162, Disperbyk 163, Disperbyk 142, Disperbyk 145, Disperbyk 2001, Disperbyk 2010, Disperbyk 2020, Disperbyk 2025, and Disperbyk 9076.
In accordance with the present disclosure, the dispersing agent is a block copolymer with ionic or non-ionic pigment affinic groups. In accordance with an embodiment of the present disclosure, the dispersing agent is at least one selected from Disperbyk 102, Disperbyk 103, Disperbyk 160, Disperbyk 161, Disperbyk 162, Disperbyk 163, Disperbyk 142, Disperbyk 145, Disperbyk 2001, Disperbyk 2010, Disperbyk 2020, Disperbyk 2025, and Disperbyk 9076 from BYK.
In accordance with the present disclosure, the fluorosurfactant is at least one selected from fluorinated acrylic copolymer and non-ionic solvent based fluoropolymer. In accordance with an embodiment of the present disclosure, the fluorosurfactant is at least one selected from Capstone ST 200 and Capstone FS 22 from DuPont.
In accordance with the present disclosure, the plasticizer is, a phthalate or non-phthalate, at least one selected from diisononyl phthalate, diisodecycl phthalate, bis(2-ethylhexyl) terephthalate and bis(2-ethylhexyl) adipate.
In accordance with the present disclosure, the flow and levelling additive is at least one selected from polyacrylate and polydimethylsiloxane.
In accordance with the present disclosure, the rheological agent is at least one selected from the group consisting of polyurea, ethyl cellulose, hydrogenetaed castor oil, fumed silica, clay and polyamide wax.
In accordance with the present disclosure, the defoamer is at least one selected from mineral oil and polydimethylsiloxane.
In accordance with the present disclosure, the adhesion promoter is at least one selected from mercaptosilane, isocyanate functional silane, epoxysilane and aminosilane.
In accordance with the present disclosure, the silane is an organosilane at least one selected from methyl trimethoxysilane, ethyltrimethoxysilane and ethyltriethoxysilane.
In accordance with the present disclosure, the amount of at least one additive is in the range of 0.1 to 3 mass% with respect to the total mass of the coating composition. In an exemplary embodiment, the amount of the additive is 0.5 mass%.
In accordance with an embodiment of the present disclosure, the coating composition comprises 0.05 to 0.3 mass% of a curing catalyst with respect to the total mass of the coating composition to obtain an anti-graffiti composition.
In accordance with the present disclosure, the curing catalyst is selected from the group consisting of dibutyltin dilaurate, dibutyltin diacetate, titanium 5 tetrabutoxide, 1,4-diazabicyclo[2,2,2]-octane, metal dionate complex, isooctate salts of Co, Zn and Bi, 2-ethylhexoate salts of Co, Zn and Bi, and acetoacetate complexes of Zn and Ti.
In another aspect, the present disclosure provides a process for the preparation of a siloxane modified acrylic polyol polymer.
Initially predetermined amounts of at least one first monomer, at least one second monomer, at least one siloxane monomer and at least one first initiator are mixed in at least one first fluid medium in a reactor at a first predetermined temperature for a first predetermined time period in the presence of an inert gas to obtain a mixture (step (i)).
In accordance with the present disclosure, the first monomer is a hydroxy acrylate monomer at least one selected from the group consisting of hydroxyl ethyl acrylate, hydroxyl-ethoxyethyl acrylate, hydroxyl-poly(ethoxy)ethyl acrylate, hydroxymethyl acrylate, hydroxypropyl acrylate, hydroxylbutyl acrylate, hydroxyethyl methacrylate, hydroxyl-ethoxyethyl methacrylate, hydroxyl-poly(ethoxy)ethyl methacrylate, hydroxymethyl methacrylate, hydroxypropyl methacrylate, and hydroxylbutyl methacrylate. In an exemplary embodiment, the first monomer is hydroxyl ethyl methacrylate.
In accordance with the present disclosure, an amount of the first monomer is in the range of 10 to 40 mass% with respect to the total mass of the monomer mixture. In an exemplary embodiment, the amount of the first monomer is 14.12 mass%.
In accordance with the present disclosure, the second monomer is selected from the group consisting of acrylate monomer, vinyl monomer and carboxyl functional monomer.
In accordance with the present disclosure, an amount of the second monomer is in the range of 40 to 80 mass% with respect to the total mass of the monomer mixture. In an exemplary embodiment, the amount of the second monomer is 44.86 mass%.
In accordance with the present disclosure, the acrylate monomer is at least one selected from the group consisting of alkyl (C1-C20) acrylate monomer, and alkyl (C1-C20) methacrylate monomer.
In accordance with an embodiment of the present disclosure, the acrylate monomer is selected from the group consisting of methyl acrylate monomer, ethyl acrylate monomer, n-propyl acrylate monomer, isopropyl acrylate monomer, n-butyl acrylate monomer, isobutyl acrylate monomer, sec-butyl acrylate monomer, tert-butyl acrylate monomer, n-pentyl acrylate monomer, neopentyl acrylate monomer, n-hexyl acrylate monomer, cyclohexyl acrylate monomer, n-octyl acrylate monomer, 2- ethylhexyl acrylate monomer, lauryl acrylate monomer, cetyl acrylate monomer, stearyl acrylate monomer, eicosyl acrylate monomer and isobornyl acrylate monomer.
In accordance with another embodiment of the present disclosure, the acrylate monomer is selected from the group consisting of methyl methacrylate monomer, ethyl methacrylate monomer, n-propyl methacrylate monomer, isopropyl methacrylate monomer, n-butyl methacrylate monomer, isobutyl methacrylate monomer, sec-butyl methacrylate monomer, tert-butyl methacrylate monomer, n-pentyl methacrylate monomer, neopentyl methacrylate monomer, n-hexyl methacrylate monomer, cyclohexyl methacrylate monomer, n-octyl methacrylate monomer, 2- ethylhexyl methacrylate monomer, lauryl methacrylate monomer, cetyl methacrylate monomer, stearyl methacrylate monomer, eicosyl methacrylate monomer and isobornyl methacrylate monomer.
In accordance with the present disclosure, the vinyl monomer is selected from the group consisting of styrene, alpha-methyl styrene, and para-methyl styrene.
In accordance with the present disclosure, the carboxyl functional monomer is selected from the group consisting of acrylic acid, methacrylic acid, fumaric acid, crotonic acid, itaconic acid, maleic acid, cinnamic acid, and 2-acrylamide-2-methylpropanesulfonic acid.
In an exemplary embodiment, the second monomer is a mixture of butyl acrylate, butyl methacrylate, methyl methacrylate, and methacrylc acid.
In accordance with the present disclosure, the siloxane monomer is selected from the group consisting of polydimethoxysilane monoacrylate, polydimethoxysilane diacrylate, polydimethoxysilane methacrylate, and polydimethylsiloxane dimethacrylate.
In accordance with an embodiment of the present disclosure, the siloxane monomers have pendant alkyl, hydroxyl or alkoxy group. In an exemplary embodiment, the siloxane monomer is polydimethoxysilane monoacrylate.
In accordance with the present disclosure, an amount of the siloxane monomer is in the range of 0.1 to 10 mass% with respect to the total mass of the monomer mixture.
In accordance with an embodiment of the present disclosure, an amount of siloxane monomer is in the range of 0.1 to 5 mass% with respect to the total mass of the monomer mixture.
In accordance with another embodiment of the present disclosure, an amount of siloxane monomer is in the range of 0.1 to 1 mass% with respect to the total mass of the monomer mixture.
In an exemplary embodiment, the amount of the siloxane monomer is 0.25 mass%. In another exemplary embodiment, the amount of siloxane monomer is 0.5 mass%. In still another exemplary embodiment, the amount of the siloxane monomer is 0.75 mass%.
In accordance with the present disclosure, the siloxane monomer is functionalized by using a compound selected from vinyl, acrylic, hydroxyl, alkoxy, epoxy, amine and carboxyl. In accordance with an embodiment of the present disclosure, the siloxane monomer is functionalized by using an acrylic compound.
In accordance with the present disclosure, an amount of the first initiator is in the range of 1 to 10 mass% with respect to the total mass of the monomer mixture. In an exemplary embodiment, the amount of the initiator is 5 mass% of the monomer mixture.
In accordance with the present disclosure, the first fluid medium is in the range of 20 to 40 mass% of the monomer mixture
In an exemplary embodiment, the amount of the first fluid medium is about 30 mass%.
In accordance with the present disclosure, the first predetermined temperature is in the range of 30 to 160 °C. In an exemplary embodiment, the first predetermined temperature is 140 °C. The first predetermined temperature depends on the type of first initiator used for the process for the preparation of siloxane modified acrylic polyol polymer.
In accordance with the present disclosure, the first predetermined time period is in the range of 2 to 6 hours. In an exemplary embodiment, the first predetermined temperature is 4 hours.
In accordance with the present disclosure, the inert gas is selected from nitrogen, argon, xenon, and carbon dioxide.
In accordance with the present disclosure, a polyolefin is added in step (i).
In accordance with an embodiment of the present disclosure, the polyolefin is grafted on the siloxane modified acrylic polyol polymer. The siloxane modified acrylic polyol component is mixed with a polyolefinic component and heated at a temperature in the range of 120 °C to 170 °C in the presence of a fluid medium, to obtain the desired grafting. In accordance with the present disclosure, the fluid medium is at least one selected from the group consisiting of aromatic, aliphatic, cycloaliphatic hydrocarbons, esters, ketones, and glycol ethers
In accordance with the present disclosure, the polyolefinic component has average molecular weight as measured using gel permeation chromatography in the range of 3,000 to 30,000, and an acid value in the range of 30 mg KOH/g to 100 mg KOH/g.
The mixture is digested at a second predetermined temperature for a second predetermined time period to obtain a digested mixture (step (ii)).
In accordance with the present disclosure, the second predetermined time period is in the range of 30 minutes to 90 minutes. In accordance with the present disclosure, the second predetermined time period is 60 minutes.
In accordance with the present disclosure, the second predetermined temperature is in the range of 30?C to 160 ?C. In accordance with the present disclosure, the second predetermined temperature is 140 ?C .
A second initiator is added to the digested mixture followed by reacting at a third predetermined temperature for a third predetermined time period to obtain a reaction mixture (step (iii)).
In accordance with the present disclosure, a ratio of the second initiator to the digestion mixture is in the range of 0.01:1 to 0.5:1. In an exemplary embodiment, the ratio of the second initoator to the digestion mixture is 0.03:1.
In accordance with the present disclosure, the first initiator and the second initiator are same or different and are at least one selected from the group consisting of azobisisobutyronitrile, tertiary butyl perbenzoate, dimethyl 2,2'- azobis(2-methylpropionate), ditertiary butyl peroxide, dicumyl peroxide, ditertiary amylperoxide, redox polymerization initiator, benzoyl peroxide/amine initiator, tert-butylperoxy 2-ethylhexyl carbonate, benzoyl peroxide, 1,1-bis(tert-amylperoxy)cyclohexane, tert-butyl hydroperoxide, tert-butyl peracetate. In an exemplary embodiment, the first initiator is tertiary butyl perbenzoate.
In accordance with the present disclosure, the third predetermined time period is in the range of 30 minutes to 90 minutes. In accordance with an exemplary embodiment, the third predetermined time period is 60 minutes.
In accordance with the present disclosure, the third predetermined temperature is in the range of 60 ?C to 160 ?C. In an exemplary embodiment of the present disclosure, the third predetermined temperature is 140 °C. The reaction mixture is cooled to a fourth predetermined temperature followed by mixing in a second fluid medium for a fourth predetermined time period to obtain a cooled mixture having a solid content in the range of 40 to 80 mass% of the total mass of the siloxane modified acrylic polyol polymer (step (iv)).
In accordance with the present disclosure, the fourth predetermined temperature is in the range of 60 to 90 °C. In an exemplary embodiment, the fourth predetermined temperature is 75 °C.
In accordance with the present disclosure, the fourth predetermined time period is in the range of 5 to 20 minutes. In an exemplary embodiment, the fourth predetermined time period is 12±3 minutes.
In accordance with the present disclosure, the fluid medium and the second fluid medium are same or different and are at least one selected from the group consisting of aromatic hydrocarbons, aliphatic esters, alcohols, ketones, ethers and glycol ethers.
In accordance with an embodiment of the present disclosure, the first fluid medium and second fluid medium are same or different and are selected from the group consisting of o-xylene, butyl acetate,and methyl isobutyl ketone. In an exemplary embodiment, the first fluid medium is o-xylene.
In an exemplary embodiment, the second fluid medium is butyl acetate.
In accordance with the present disclosure, an amount of the second fluid medium is added to attain solid content in the range of 40 to 80 mass% with respect to the total mass of the polymer.
The cooled mixture is filtered to obtain the siloxane modified acrylic polyol polymer (step (v)).
In still another aspect, the present disclosure provides a process for the preparation of a coating composition.
The process comprises mixing predetermined amounts of at least one curing agent, at least one second fluid medium, at least one additive, optionally an acid catalyst, optionally a nanoparticles, and optionally a polyolefinic component to a predetermined amount of a predetermined amounts of siloxane modified acrylic polyol polymer of the present disclosure at a fifth predetermined temperature for fifth predetermined time period to obtain the coating composition.
In accordance with the present disclosure, the predetermined amount of the siloxane modified acrylic polyol polymer is in the range of 60 to 70 mass% with respect to the total mass of the coating composition. In an exemplary embodiment, the predetermined amount of siloxane modified acrylic polyol polymer is 65 mass%.
In accordance with the present disclosure, the amount of the curing agent is in the range of 5 to 40 mass% with respect to the total mass of the coating composition. In an exemplary embodiment, the predetermined amount of the curing agent is 12 mass%.
In accordance with the present disclosure, the amount of the at least one fluid medium is in the range of 15 to 25 mass% with respect to the total mass of the coating composition. In an exemplary embodiment, the amount of the fluid medium is 20.2 mass%.
In accordance with the present disclosure, the amount of at least one additive is in the range of 0.1 to 3 mass% with respect to the total mass of the coating composition. In an exemplary embodiment, the amount of the additive is 0.5 mass%.
In accordance with the present disclosure, the amount of the acid catalyst is in the range of 0.5 to 1.5 mass% with respect to the total mass of the coating composition. In an exemplary embodiment, the amount of the first catalyst is 1 mass%.
In accordance with the present disclosure, the amount of the nanoparticles in the range of 0.1 to 5 mass% with respect to the total mass of the coating composition.
In accordance with the present disclosure, the amount of the polyolefinic component in the range of 0.1 to 5 mass% with respect to the total mass of the coating composition. The polyolefinic component is grafted on the siloxane modified acrylic polyol polymer. The siloxane modified acrylic polyol polymer is mixed with a polyolefinic component and heated at a temperature in the range of 120 °C to 170 °C in the presence of the fluid medium, to obtain the desired grafting. In accordance with the present disclosure, the solvent fluid medium is at least one selected from the group consisting of aromatic, aliphatic, cycloaliphatic hydrocarbons, esters, ketones, and glycol ethers.
In accordance with the present disclosure, the fifth predetermined temperature is in the range of 20 to 60°C. In accordance with the present disclosure, the fifth predetermined temperature is 40 °C.
In accordance with the present disclosure, the fifth predetermined time period is in the range of 20 to 180 minutes. In an exemplary embodiment, the fifth predetermined time period is 60 minutes.
The coating composition of the present disclosure has passed the repellency test for the permanent black marker, even after 50 double rub by cotton cloth.
The coating composition of the present disclosure has passed wet turmeric test, xylene rub test (50 double rubs), humidity test (IS-101, 500 hours), hot water resistance test (40° C for 200 hours), flexibility test (conical mandrel 10 to 30 mm), direct impact test (0.98kg*40cm*0.025 in), cross cut adhesion test (2*2 mm), and re-coatability test.
The coating composition of the present disclosure provides the smooth and glossy appearance of the coated surfaces. In accordance with the present disclosure, the coating composition provides the gloss in the range of 95 to 99 unit at 60 ° angle.
Monomers with siloxane functionality have low surface energy. Modification of the acrylic polyol by the monomer with siloxane functionality imparts slip, mar and anti-graffiti properties to the coating composition. The resultant coating composition is stain resistant and easy to clean. Further, inclusion of low quantities of monomers with siloxane functionality makes the coating composition economical.
Incorporation of the siloxane modified acrylic polyol polymer along with silica nanoparticles provides a facile route to improve the easy cleaning property of the coating composition.
In accordance with an embodiment of the present disclosure, the coating composition is provided in the form of 1 pack system and 2 pack system.
In 1 pack system, the siloxane modified acrylic polyol polymer and the curing agent are present in 1 system and can be directly applied on a substrate as a coating.
In 2 pack system, the siloxane modified acrylic polyol polymer and curing agent are present in separate packs and need to be mixed before the application.
The siloxane modified acrylic polyol polymer and curing agent can be stored together in a single pack. In an embodiment of the present disclosure, siloxane modified acrylic polyol polymer and curing agent (blocked polyisocyanate) are in a single pack system. In another embodiment, siloxane acrylic polyol polymer, curing agent (melamine formaldehyde) and acid catalyst (blocked) are in a single pack. In still another embodiment, siloxane modified acrylic polyol polymer and curing agent (blocked polyisocyanate) are in separate packs. In yet another exemplary embodiment, siloxane modified acrylic polyol polymer and acid catalyst are in first pack, and curing agent (melamine formaldehyde) in a second pack.
In accordance with the embodiments of the present disclosure, the coating composition is cured at an ambient temperature or at an elevated temperature. In accordance with an embodiment of the present disclosure, curing is done at ambient temperature
In accordance with another embodiment, the curing is done at elevated temperatures in the range of 80 to 150 ?C by using the curing agent (amino resins).
In accordance with an embodiment of the present disclosure, coating composition can be applied by using conventional techniques, such as spray, brush, and dip coating.
In accordance with the embodiments of the present disclosure, the dry film thickness of the coating composition is in the range of 1 µm to 50 µm thickness.
The coating composition of the present disclosure is highly durable, fluorine free and has good self cleaning property.
The coating composition of the present disclosure has easy cleaning property without the use of any hazardous solvents.
The coating composition of the present disclosure is capable of being cleaned only by the use of dry wiping for any permanent marker stains, crayon stains, white board marker stains, sketch pen stains.
The coating composition of the present disclosure has anti-graffiti property, desired slip property, desired mar property and economical.
The foregoing description of the embodiments has been provided for purposes of illustration and not intended to limit the scope of the present disclosure. Individual components of a particular embodiment are generally not limited to that particular embodiment, but, are interchangeable. Such variations are not to be regarded as a departure from the present disclosure, and all such modifications are considered to be within the scope of the present disclosure.
The present disclosure is further described in light of the following experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. The following experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial scale.
EXPERIMENTAL DETAILS
Experiment 1: A process for the preparation of siloxane modified acrylic polyol polymer (acrylic polyol resin) in accordance with the present disclosure
The acrylic polyol polymer was synthesized by using free radical polymerization. A four neck reactor with a condenser, stirrer, nitrogen inlet and metering pump was taken. The formulation of siloxane modified acrylic polyol polymer are given in Table 1. A first fluid medium (ortho xylene) was charged to the reactor. The monomers (mixture of first monomer, second monomer and siloxane monomer), and a first initiator (tertiary butyl perbenzoate) were mixed to the first fluid medium into the reactor over a period of 4 hours at 142±2 °C to obtain a mixture. The mixture was then digested at 142 °C for 1 hour to obtain a digested mixture. A second initiator (tertiary butyl perbenzoate) was added to the digested mixture and the batch was continued for 1 hour at 142 °C to obtain a reaction mixture. The reaction mixture was then cooled to 75±5 °C followed by mixing in a second fluid medium (butyl acetate) for 12±3 minutes to obtain a cooled mixture having 60 mass% of solid content. The cooled mixture was then discharged after filtration to obtain the siloxane modified acrylic polyol polymer.
Table 1: Formulation of siloxane modified acrylic polyol polymers
S.N. Material/Parameter 1A 1B 1C 1D
1 Butyl acrylate Second monomer 4.45 4.69 4.44 4.19
2 Butyl methacrylate Second monomer 26.79 26.3 26.3 26.3
3 Polydimethylsiloxane monoacrylate (viscosity of 56.8 mm2/s at 25 °C, specific gravity of 0.97 at 25 °C and refractive index of 1.4063) Siloxane monomer 0 0.25 0.5 0.75
4 Methyl methacrylate Second monomer 11.87 11.87 11.87 11.87
5 Hydroxyethyl methacrylate First monomer 14.12 14.12 14.12 14.12
6 Methacrylic acid Second monomer 1.75 1.75 1.75 1.75
7 Tertiary butyl perbenzoate Initiator
(first and second initiator) 2.66 2.66 2.66 2.66
8 O-Xylene Fluid medium 26.46 26.46 26.46 26.46
9 Butyl acetate Fluid medium 11.9 11.9 11.9 11.9
Total (mass%) 100 100 100 100
Solid content in mass% (determined by drying in an air circulating oven at 120 °C for 1 hour) 60 60 61 61
Gardener viscosity at 25 °C Y-Z Z-Z1 Z-Z1 Z-Z1
Table 2 below demonstrates the characterization of siloxane modified acrylic polyol polymers (examples 2-4) with desired easy cleaning property prepared in accordance with the present disclosure. Examples 1, 5 and 6 of Table 2 are not in accordance with the present disclosure.
Table 2: Examples of property testing of the siloxane modified acrylic polyol polymers
S.N. Acrylic polymer with different loading of siloxane monomer Repellency test: a marker (Camlin permanent black marker)
Repellency test after 50 double rub by cotton cloth: a marker (Camlin permanent black marker) Wet Turmeric test* Xylene Rub Test (50 double rubs) Humidity test -500 hrs (IS-101) Hot water resistance (40° C)-200 Hrs. Flexibility (Conical mandrel)
10-30 mm Direct Impact (0.98kg* 40cm* 0.025 in) Cross cut adhesion
(2*2 mm) Recoatability
1 Polymer 1A 1 1 1 Passes Micro blistering observed Micro blistering observed Passes Passes Passes Passes
2 Polymer 1B 6 5 7 Passes Passes (No blisters) Passes (No blisters) Passes Passes Passes Passes
3 Polymer 1C 8 7 8 Passes Passes (No blisters) Passes (No blisters) Passes Passes Passes Passes
4 Polymer 1D 9 8 8 Passes Passes (No blisters) Passes (No blisters) Passes Passes Passes Passes
5 Polymer 1A blended with 3 mass% of additive 1 3 2 4 Passes Passes (No blisters) Passes (No blisters) Passes Passes Passes Fail
6 Polymer 1A blended with 3 mass% of additive 2 2 2 3 Passes Passes (No blisters) Passes (No blisters) Passes Passes Passes Inferior
Additive 1: BYK Silclean 3700 (Hydroxyl functional siloxane additive); additive 2: Disperlon L280 (Hydroxyl functional siloxane additive); rating scale for marker test: Visual Rating 1=Poor and Visual Rating 10= Excellent; *Wet turmeric test: Wet turmeric powder placed on panel for few minutes and removed by dry cloth.
It was observed from Table 2 that the incorporation of siloxane monomers at low quantities (below 1%) in the siloxane modified acrylic polyol polymers (examples 2-4) demonstrated an easy cleaning property (with permanent marker and turmeric stain). The polymer of examples 2-4 also improved humidity and hot water resistance. The easy cleaning properties of the polymer of the present disclosure were better than that blended with high loading of additives (3 mass%) (Table 2, examples 5 and 6).
Further, it was observed that the additives hampered the recoatability property whereas polymer of the present disclosure passed the recoatability test.
Experiment 2: A process for the preparation of a coating composition in accordance with the present disclosure
The coating composition prepared in accordance with the present disclosure is given in Table 3. The high speed disperser equipment was cleaned and the following ingredients were added under slow stirring speed at ambient temperature for 60 minutes. The process of preparing the coating composition involved adding additives to adjust the electrical resistivity/conductivity and fluid medium to adjust viscosity.
Table 3: Example of coating composition
Ingredients Names of ingredient Mass%
Siloxane modified acrylic polyol polymer Siloxane modified acrylic polyol polymer of example 1B or 1C or 1D 65
Fluid medium Butyl acetate 5.8
Fluid medium Butyl carbitol acetate 2
Fluid medium Butanol 1
Fluid medium O-xylene 4
Flow and levelling additive Polyacrylate flow levelling agent 0.3
Additive (to increase conductivity of coating to enable spray application) Cationic additive from EFKA 0.2
Fluid medium (for viscosity adjustment) O-xylene 1.3
Curing agent Melamine formaldehyde 12
Fluid medium O-xylene 5.2
Fluid medium Butanol 2.2
Acid catalyst Acid catalyst 1
TOTAL 100
The viscosity of the coating compositions was 42 seconds at 30 ?C, and the solid content of the coating composition is 50 mass%.
The appearance and gloss of the coating compositions were smooth and glossy (95 to 98 unit at 60°) as measured using BYK Glossometer.
Application procedure:
The properties of the coating composition was checked after spray application of the coating composition (20 to 25 microns dry film thickness (DFT)), flash off 10 to 12 minutes and baking at 140°C for 30 min.
Table 4: Liquid contact angle and surface energy of the films
Polymer code Contact Angle(°) Surface free energy (mN/m)
Water Di iodomethane Total Energy Non-Polar Polar
1A 85 54.5 33 28.9 4.1
1B 102.1 72.7 21.5 20.3 1.2
1C 102.1 72.5 21.6 20.5 1.2
1D 102.9 72.6 21.5 20.5 1

From Table 4, it was observed that the water contact angle was increased upon incorporation of the siloxane monomer in the coating composition. The surface energy of the films formed using the coating composition of the present disclosure was reduced and thereby aided in the easy cleaning property.
TECHNICAL ADVANCEMENTS AND ECONOMICAL SIGNIFICANCE
The present disclosure described herein above has several technical advantages including, but not limited to, the realization of a coating composition that,
- has self cleaning, easy to clean and anti-graffiti properties;
- is fluorine free and higly durable;
- can be dry wiped without the use of hazardous solvents;
- capable of being cleaned only by the use of dry wiping of any permanent marker stains, crayon stains, white board marker stains, or sketch pen stains;
- has desired slip property;
- has desired mar resistance property; and
a process for preparing the coating composition that
- is simple and economical.
Throughout this specification the word “comprise”, or variations such as “comprises” or “comprising, will be understood to imply the inclusion of a stated element, integer or step,” or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or results. While certain embodiments of the inventions have been described, these embodiments have been presented by way of example only, and are not intended to limit the scope of the inventions. Variations or modifications to the formulation of this invention, within the scope of the invention, may occur to those skilled in the art upon reviewing the disclosure herein. Such variations or modifications are well within the spirit of this invention.
The numerical values given for various physical parameters, dimensions and quantities are only approximate values and it is envisaged that the values higher than the numerical value assigned to the physical parameters, dimensions and quantities fall within the scope of the invention unless there is a statement in the specification to the contrary.
While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated that many additional features can be added and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation.
One of the objects of the Patent Law is to provide protection to new technologies in all fields and domain of technologies. The new technologies shall or may contribute in the country economy growth by way of involvement of new efficient and quality method or product manufacturing in India.
To provide the protection of new technologies by patenting the product or process will contribute significant for innovation development in the country. Further by granting patent the patentee can contribute in manufacturing the new product or new process of manufacturing by him or by technology collaboration or through the licensing.
The applicant submits that the present disclosure will contribute in country economy, which is one of the purposes to enact the Patents Act, 1970. The product in accordance with present invention will be in great demand in country and worldwide due to novel technical features of a present invention is a technical advancement in the coating composition. The technology in accordance with present disclosure will provide product cheaper, saving in time of total process of manufacturing. The saving in production time will improve the productivity, and cost cutting of the product, which will directly contribute to economy of the country.
The product will contribute new concept in the disinfection, wherein patented process and product will be used. The present disclosure will replace the whole concept of coating composition being used in the world from several decades. The product is developed in the national interest and will contribute to country economy.
The economy significance details requirement may be called during the examination. Only after filing of this Patent application, the applicant can work publically related to present disclosure product/process/method. The applicant will disclose all the details related to the economic significance contribution after the protection of invention.


,CLAIMS:WE CLAIM:
1. A coating composition comprising:
• 60 to 70 mass% of a siloxane modified acrylic polyol polymer;
• 5 to 40 mass% of at least one curing agent;
• 15 to 25 mass% of at least one fluid medium;
• 0.1 to 3 mass% of at least one additive;
• optionally, 0.5 to 1.5 mass% of at least one acid catalyst;
• optionally, 0.1 to 5 mass% of at least one nanoparticle; and
• optionally, 0.1 to 5 mass% of at least one polyolefinic component;
wherein all the percentages are with respect to the total mass of the composition.
2. The coating composition as claimed in claim 1, wherein said siloxane modified acrylic polyol polymer is a product of:
• 0.1 to 10 mass% of a siloxane monomer with respect to the total mass of the siloxane modified acrylic polyol polymer; and
• 90 to 99.9 mass% of an acrylic polyol with respect to the total mass of the siloxane modified acrylic polyol polymer.
3. The coating composition as claimed in claim 1, wherein said siloxane modified acrylic polyol polymer is a product of:
• 0.1 to 5 mass% of a siloxane monomer with respect to the total mass of the siloxane modified acrylic polyol polymer; and
• 95 to 99.9 mass% of an acrylic polyol with respect to the total mass of the siloxane modified acrylic polyol polymer.
4. The coating composition as claimed in claim 1, wherein said siloxane modified acrylic polyol polymer is a product of:
• 0.1 to 1 mass% of a siloxane monomer with respect to the total mass of the siloxane modified acrylic polyol polymer; and
• 99 to 99.9 mass% of an acrylic polyol with respect to the total mass of the siloxane modified acrylic polyol polymer.
5. The coating composition as claimed in claims 2 to 4, wherein said acrylic polyol component has a hydroxyl value in the range of 50 mg KOH/g to 200 mg KOH/g.
6. The coating composition as claimed in claims 2 to 4, wherein said siloxane monomer has an average molecular weight in the range of 500 g/mole to 4,000 g/mole.
7. The coating composition as claimed in claims 2 to 4, wherein said siloxane monomer is functionalized by using a compound selected from the group consisting of vinyl, acryl, hydroxyl, alkoxy, epoxy, amine and carboxyl.
8. The coating composition as claimed in claim 1, wherein said curing agent is at least one selected from the group consisting of polyisocyanate, blocked polyisocyanates, isocyanate functional silanes, melamine-formaldehyde, urea formaldehyde, unimolecular amines, unimolecular amides, unimolecular amido-amines, unimolecular imido-amines, polyamines, polyamides, polyamido-amines, benzoguanamine formaldehyde and polyimido-amines.
9. The coating composition as claimed in claim 1, wherein said fluid medium is at least one selected from the group consisting of aromatic hydrocarbons, aliphatic esters, alcohols, ketones, ethers and glycol ethers.
10. The coating composition as claimed in claims 1 and 9, wherein said fluid medium is selected from butyl acetate, butyl carbitol acetate, butanol, ortho xylene and methyl isobutyl ketone.
11. The coating composition as claimed in claim 1, wherein said acid catalyst is at least one selected from the group consisting of p-toluene sulfonic acid, dodecylbenzene sulfonic acid, amine blocked alkylated benzene sulfonic acids, and phosphoric acids.
12. The coating composition as claimed in claim 1, wherein said nanoparticles are selected from the group consisting of silica nanoparticles, alumina nanoparticles, titania nanoparticles, carbon nanotubes, graphene nanoparticles and zinc oxide nanoparticles; and wherein a particle size of said nanoparticles is in the range of 1 nm to 200 nm.
13. The coating composition as claimed in claims 1 and 12, wherein said nanoparticles are surface treated with a hydrophobic group; wherein said hydrophobic group is an alkyl disilazane selected from the group consisting of hexamethyldisilazane, alkylsilanes, alkylchlorosilanes and dimethyldichlorosilane.
14. The coating composition as claimed in claim 1, wherein said polyolefinic component is selected from the group consisting of polypropylene, polyethylene and copolymers of polypropylene and polyethylene; and wherein said polyolefinic component is grafted on said siloxane modified acrylic polyol polymer.
15. The coating composition as claimed in claim 1, wherein said polyolefinic component has an average molecular weight is in the range of 3,000 to 30,000 Da measured by using gel permeation chromatography; and said polyolefinic component has an acid value in the range of 30 mg KOH/g to 100 mg KOH/g.
16. The coating composition as claimed in claim 1, wherein said additive is at least one selected from the group consisting of wetting agent, dispersing agent, fluorosurfactant, plasticizer, flow and levelling additive, rheological agent, defoamer, adhesion promoter and silane.
17. The coating composition as claimed in claim 16, wherein said wetting agent is a block copolymer with ionic or non-ionic pigment affinic groups; said dispersing agent is a block copolymer with ionic or non-ionic pigment affinic groups; said fluorosurfactant is at least one selected from fluorinated acrylic copolymer and non-ionic solvent based fluoropolymer; said plasticizer is, a phthalate or a non-phthalate, at least one selected from the group consisting of diisononyl phtahalte, bis(2-ethylhexyl) terephthalate and bis(2-ethylhexyl) adipate; said flow and levelling additive is at least one selected from polyacrylate and polydimethylsiloxane; said rheological agent is at least one selected from the group consisting of polyurea, ethyl cellulose, hydrogenetaed castor oil, fumed silica, clay and polyamide wax; said defoamer is at least one selected from mineral oil and polydimethylsiloxane; said adhesion promoter is at least one selected from mercaptosilane, isocyanate functional silane, epoxysilane, and aminosilane; and said silane is an organosilane at least one selected from methyl trimethoxysilane, ethyltrimethoxysilane and ethyltriethoxysilane.
18. The coating composition as claimed in claim 1, wherein said coating composition comprises 0.05 to 0.3 mass % of a curing catalyst with respect to the total mass of the coating composition to obtain an anti-graffiti composition.
19. The coating composition as claimed in claim 18, wherein said curing catalyst is selected from the group consisting of dibutyltin dilaurate, dibutyltin diacetate, titanium 5 tetrabutoxide, 1,4-diazabicyclo[2,2,2]-octane, metal dionate complex, isooctate salts of Co, Zn and Bi, 2-ethylhexoate salts of Co, Zn and Bi, and acetoacetate complexes of Zn and Ti.
20. A process for the preparation of a siloxane modified acrylic polyol polymer, said process comprising the following steps:
(i) mixing predetermined amounts of at least one first monomer, at least one second monomer, at least one siloxane monomer, and at least one first initiator in at least one first fluid medium in a reactor at a first predetermined temperature for a first predetermined time period in the presence of an inert gas to obtain a mixture;
(ii) digesting said mixture at a second predetermined temperature for a second predetermined time period to obtain a digested mixture;
(iii) adding a second initiator to said digested mixture followed by reacting at a third predetermined temperature for a third predetermined time period to obtain a reaction mixture;
(iv) cooling said reaction mixture to a fourth predetermined temperature followed by mixing a second fluid medium for a fourth predetermined time period to obtain a cooled mixture having a solid content in the range of 40 to 80 mass% of the total mass of the siloxane modified acrylic polyol polymer; and
(v) filtering said cooled mixture to obtain said siloxane modified acrylic polyol polymer.
21. The process as claimed in claim 20, wherein the predetermined amounts of
• said first monomer is in the range of 10 to 40 mass% with respect to the total mass of the mixture;
• said second monomer is in the range of 40 to 80 mass% with respect to the total mass of the mixture;
• said siloxane monomer is in the range of 0.1 to 10 mass% with respect to the total mass of the mixture;
• said initiator is in the range of 1 to 10 mass% with respect to the total mass of the mixture; and
• said first fluid medium is in the range of 20 to 40 mass% of monomer mixture.
22. The process as claimed in claim 20, wherein said first monomer is a hydroxy acrylate monomer at least one selected from the group consisting of hydroxyl ethyl acrylate, hydroxyl-ethoxyethyl acrylate, hydroxyl-poly(ethoxy)ethyl acrylate, hydroxymethyl acrylate, hydroxypropyl acrylate, hydroxylbutyl acrylate, hydroxyethyl methacrylate, hydroxyl-ethoxyethyl methacrylate, hydroxyl-poly(ethoxy)ethyl methacrylate, hydroxymethyl methacrylate, hydroxypropyl methacrylate, and hydroxylbutyl methacrylate.
23. The process as claimed in claim 20, wherein said second monomer is selected from the group consisting of acrylate monomer, vinyl monomer and carboxyl functional monomer.
24. The process as claimed in claim 23, wherein said acrylate monomer is at least one selected from the group consisting of alkyl (C1-C20) acrylate monomer and alkyl (C1-C20) methacrylate monomer; said vinyl monomer is selected from the group consisting of styrene, alpha-methyl styrene and para-methyl styrene; said carboxyl functional monomer is selected from the group consisting of acrylic acid, methacrylic acid, fumaric acid, crotonic acid, itaconic acid, maleic acid, cinnamic acid and 2-acrylamide-2-methylpropanesulfonic acid.
25. The process as claimed in claim 20, wherein said siloxane monomer is selected from the group consisting of polydimethoxysilane monoacrylate, polydimethoxysilane diacrylate, polydimethoxysilane methacrylate and polydimethylsiloxane dimethacrylate.
26. The process as claimed in claims 20 and 25, wherein said siloxane monomer is functionalized by using a compound selected from the group consisting of vinyl, acryl, hydroxyl, alkoxy, epoxy, amine and carboxyl.
27. The process as claimed in claim 20, wherein said first fluid medium and said second fluid medium are same or different and are selected from the group consisting of o-xylene, butyl acetate and methyl isobutyl ketone;.
28. The process as claimed in claim 20, wherein said first predetermined temperature is in the range of 30 to 160°C; said first predetermined time period is in the range of 2 to 6 hours; said second predetermined time period is in the range of 30 minutes to 90 minutes; and said second predetermined temperature is in the range of 30 to 160 °C.
29. The process as claimed in claim 20, wherein said first initiator and second initiator are same or different and are selected from the group consisting of azobisisobutyronitrile, tertiary butyl perbenzoate, dimethyl 2,2'- azobis(2-methylpropionate), ditertiary butyl peroxide, dicumyl peroxide, ditertiary amylperoxide, redox polymerization initiator, benzoyl peroxide/amine initiator, tert-butylperoxy 2-ethylhexyl carbonate, benzoyl peroxide, 1,1-bis(tert-amylperoxy)cyclohexane, tert-butyl hydroperoxide, tert-butyl peracetate; and wherein a ratio of said second initiator to said digestion mixture is in the range of 0.01:1 to 0.5:1.
30. The process as claimed in claim 20, wherein said third predetermined time period is in the range of 30 minutes to 90 minutes; and said third predetermined temperature is in the range of 60 to 160 °C.
31. The process as claimed in claim 20, wherein said second fluid medium is added to attain the solid content in the range of 40 to 80 mass%; said fourth predetermined temperature is in the range of 60 to 90 °C; and said fourth predetermined time period is in the range of 5 to 20 minutes.
32. The process as claimed in claim 20, wherein a polyolefinic component is added in step (i) in an amount in the range of 0.1 to 5 mass%; and wherein said polyolefinic component is grafted on said siloxane modified acrylic polyol polymer.
33. A process for the preparation of a coating composition, said process comprising mixing predetermined amounts of at least one curing agent, at least one fluid medium, at least one additive, optionally at least one acid catalyst, and optionally nanoparticles to a predetermined amount of siloxane modified acrylic polyol polymer as claimed in claims 1 to 32, at a fifth predetermined temperature for a fifth predetermined time period to obtain the coating composition.
34. The process as claimed in claim 33, wherein the predetermined amounts of
• said siloxane modified acrylic polyol polymer is in the range of 60 to 70 mass%;
• said curing agent is in the range of 5 to 40 mass%;
• said at least one fluid medium is in the range of 15 to 25 mass%;
• said at least one additive is in the range of 0.1 to 3 mass%;
• said acid catalyst is in the range of 0.5 to 1.5 mass%; and
• said nanoparticles is in the range of 0.1 to 5 mass%,
wherein all the percentages are with respect to the total mass of the composition.

35. The process as claimed in claim 33, wherein said fifth predetermined temperature is in the range of 20 to 60 °C; and said fifth predetermined time period is in the range of 20 to 180 minutes.

Documents

Application Documents

# Name Date
1 202021051419-STATEMENT OF UNDERTAKING (FORM 3) [25-11-2020(online)].pdf 2020-11-25
2 202021051419-PROVISIONAL SPECIFICATION [25-11-2020(online)].pdf 2020-11-25
3 202021051419-PROOF OF RIGHT [25-11-2020(online)].pdf 2020-11-25
4 202021051419-POWER OF AUTHORITY [25-11-2020(online)].pdf 2020-11-25
5 202021051419-FORM 1 [25-11-2020(online)].pdf 2020-11-25
6 202021051419-DECLARATION OF INVENTORSHIP (FORM 5) [25-11-2020(online)].pdf 2020-11-25
7 202021051419-ENDORSEMENT BY INVENTORS [25-11-2021(online)].pdf 2021-11-25
8 202021051419-COMPLETE SPECIFICATION [25-11-2021(online)].pdf 2021-11-25
9 202021051419-FORM 18 [26-11-2021(online)].pdf 2021-11-26
10 202021051419-FER.pdf 2022-05-30
11 202021051419-FORM 3 [08-06-2022(online)].pdf 2022-06-08
12 202021051419-OTHERS [24-11-2022(online)].pdf 2022-11-24
13 202021051419-FORM-26 [24-11-2022(online)].pdf 2022-11-24
14 202021051419-FER_SER_REPLY [24-11-2022(online)].pdf 2022-11-24
15 202021051419-CLAIMS [24-11-2022(online)].pdf 2022-11-24
16 202021051419-US(14)-HearingNotice-(HearingDate-28-03-2023).pdf 2023-02-28
17 202021051419-Correspondence to notify the Controller [25-03-2023(online)].pdf 2023-03-25
18 202021051419-Written submissions and relevant documents [12-04-2023(online)].pdf 2023-04-12
19 202021051419-Response to office action [30-05-2023(online)].pdf 2023-05-30
20 202021051419-PatentCertificate10-07-2023.pdf 2023-07-10
21 202021051419-IntimationOfGrant10-07-2023.pdf 2023-07-10

Search Strategy

1 SEARCHstrategyE_30-05-2022.pdf

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