DESC:FIELD
The present disclosure relates to a coating composition and a process of its preparation. Particularly, the present disclosure relates to a polyurethane coating composition that demonstrates self-healing properties.
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 indicate otherwise.
Self-healing: The term “self-healing” refers to the property of a material to recover itself from any physical damage.
Self-healing polymer: The term “self-healing polymer” refers to the class of the polymers that have the capability to recover or heal the material from any of the physical damages by responding to the damages in the material.
2K coating system: The term “2K coating system” refers to two component polyurethane solvent borne systems. In 2K solvent borne polyurethane system, a polyisocyanate hardener is reacted with a medium containing a polyhydroxyl polyester binder or blend of polyhydroxyl polyester binder & polyhydroxy acrylic binder.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
Wood is increasingly used in indoor and outdoor applications such as constructions, furniture and the like. While in use, the wood products are subjected to damages due to mechanical aggressions, abrasion, scratches, moisture, heat, solvents and the like. These damages can be repaired by applying coating on the wood products. Generally, the coating is applied on the wooden products to perform two functions. The first function is to enhance the aesthetics/appearance of the wooden product and the second function is to preserve or to protect the aesthetic/appearance from any damages. There are various coating composition which are applied on the wooden products to protect them from the damages such as polyester based coating composition, polyurethane based coating composition and the like.
The polyurethane (PU) based self-healing coating composition are applied on the wooden products to protect them from any damages. However, the conventional polyurethane (PU) based self-healing coating composition are soft and hard block based thermoplastic polyurethanes (TPU). They are primarily made from polyether polyols which are solids at ambient temperature and require softening and re-solidifying process to demonstrate the self-healing property. Further, the other self-healing coating composition used for protecting the wooden products involves dynamic bonds such as diels-alder, dithiols, diselenide, imine, metal-ligand and the like. All these conventional coating compositions require external triggers such as elevated temperature, pH, UV-IR light and the like for healing.
Further, the coating composition containing encapsulated healing agents are used for protecting the wooden products. However, by using the coating containing encapsulated healing agents, healing cannot be repeated multiple times as the encapsulated capsules get exhausted.
Therefore, there is felt a need to provide a coating composition that mitigates the drawbacks mentioned herein above or at least provides an alternative solution.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows:
It is an object of the present disclosure to ameliorate one or more problems of the background or to at least provide a useful alternative.
An object of the present disclosure is to provide a coating composition.
Another object of the present disclosure is to provide a self-healing coating composition.
Still another object of the present disclosure is to provide a self-healing two-component (2K) coating composition.
Yet another object of the present disclosure is to provide a coating composition that heals the damages at 20 °C to 60 °C (ambient) temperature.
Still another object of the present disclosure is to provide a coating composition that heals the damages at 20 °C to 60 °C (ambient) temperature for multiple times.
Yet another object of the present disclosure is to provide a coating composition that demonstrates healing of scratches on cured coating film without heat-softening.
Still another object of the present disclosure is to provide a coating composition that heals the damages without the incorporation of any dynamic covalent bonds such as diels-Alder, dithiols, diselenide, imine, metal-ligand and the like.
Yet another object of the present disclosure is to provide a simple process for the preparation of a coating composition.
Still another object of the present disclosure is to provide a process for the preparation of a polyester polyol.
Yet another object of the present disclosure is to provide a process for the preparation of an acrylic polyol.
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 comprising a hydroxy functional polymer component comprising a polyester polyol and optionally an acrylic polyol, an isocyanate component, a catalyst, a flow and leveling additive and a fluid medium, wherein a ratio of OH equivalent weight of the hydroxy functional polymer component to NCO equivalent weight of the isocyanate component is in the range of 1:0.5 to 1:2.
In an embodiment of the present disclosure, the hydroxyl functional polymer component comprises a mixture of the polyester polyol and the acrylic polyol.
In an embodiment of the present disclosure, the polyester polyol is characterized by having an acid value in the range of 0.1 mg KOH/g to 10 mg KOH/g and an OH value in the range of 80 mg KOH/g to 140 mg KOH/g and the acrylic polyol is characterized by having an OH value in the range of 80 mg KOH/g to 140 mg KOH/g.
The hydroxy functional polymer component is present in an amount in the range of 40 mass% to 60 mass%, the isocyanate component is present in an amount in the range of 30 mass% to 70 mass%, the catalyst is present in an amount in the range of 0.01 mass% to 1 mass%, the flow and leveling additive is present in an amount in the range of 0.1 mass% to 3 mass% and the fluid medium is present in an amount in the range of 1 mass% to 30 mass%, wherein the mass% of each ingredient is with respect to the total mass of the coating composition.
The fluid medium is present in an amount in the range of 2 mass% to 10 mass% with respect to the total mass of the coating composition.
The polyester polyol is present in an amount in the range of 5 mass% to 100 mass% and the acrylic polyol is present in an amount in the range of 0 mass% to 95 mass%, wherein the mass% of each ingredient is with respect to the total mass of the hydroxy functional polymer component.
The isocyanate component is selected from an aliphatic polyisocyanate and an aromatic polyisocyanate, wherein the aliphatic polyisocyanate is selected from a dimer and trimer of isophorone diisocyanate and dimer of hexamethylene diisocyanate (HDI) and trimer of hexamethylene diisocyanate (HDI) and the aromatic polyisocyanate is selected from toluene diisocyanate based aromatic polyisocyanate and diphenylmethane diisocyanate based aromatic polyisocyanate.
The catalyst is a first catalyst and a second catalyst, wherein said first catalyst is selected from the group consisting of monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate, tetra-n-butyl titanate and a second catalyst is selected from the group consisting of dibutylin oxide, monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate and tetra-n-butyl titanate
The flow and leveling additive is selected from a group consisting of silicon based flow additive 10% solution in O-xylene, a solution of a polyether-modified polydimethylsiloxane, solution of a polyacrylate, polyether-modified polydimethylsiloxane and a low viscosity acrylate polymer.
The fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, solvent naphtha (petroleum) light aromatic and mixture thereof.
In an embodiment of the present disclosure, the polyester polyol of the coating composition is a product of at least one polyol, a macrodiol, at least one polyacid, the second catalyst, the fluid medium and a performance additive, and the acrylic polyol is a product of at least one acrylic monomer, a hydroxyl-functional acrylic monomer, the fluid medium and an initiator.
The polyol is selected from the group consisting of neopentyl glycol, 2-methyl-1, 3-propanediol (MP diol), hexane diol, 1,3 propane diol, 1,2 propane diol, 1,4 butane diol, glycerine, ethylene glycol, diethylene glycol, butyl ethyl propanediol, trimethylolpropane, pentaerythritol, cyclohexane dimethanol and mixture thereof.
The macrodiol is selected from the group consisting of polycaprolactone polyol, polyester polyol, polyether polyol, polyesterpolyether polyol and polycarbonate polyol.
The polyacid is selected from the group consisting of adipic acid, terephthalic acid, isophthalic acid, hexahydro phthalic anhydride, cyclohexane dicarboxylic acid and mixture thereof.
The second catalyst is selected from the group consisting of dibutylin oxide, monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate and tetra-n-butyl titanate.
The fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, a solvent naphtha (petroleum) light aromatic and mixture thereof.
The performance additive is selected from the group consisting of triphenyl phosphite, hypophosphorous acid and pentaerythritol tetrakis(3-(3,5-Di-tertiary-butyl-4-hydroxyphenyl) propionate).
In an embodiment of the present disclosure, the acrylic monomer is selected from the group consisting of butyl acrylate, styrene, methyl methacrylate, methacrylic acid, acrylic acid, isobutyl acrylate, isobutyl methacrylate, cyclohexyl methacrylate, stearyl acrylate, stearyl methacrylate, octyl methacrylate, tertiary butyl methacrylate, a synthetic saturated monocarboxylic acid with a highly branched structure containing ten carbon atoms (Vevoa 10 monomer) ,ethyl hexyl acrylate and mixture thereof.
In an embodiment of the present disclosure, the hydroxyl-functional acrylic monomer is selected from the group consisting of 2-hydroxy ethyl acrylate, 2-hydroxy propyl methyl acrylate and 2-hydroxyl ethyl methacrylate.
The fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, butyl acetate, methoxy propyl acetate, a solvent naphtha (petroleum) light aromatic and mixture thereof.
The initiator is selected from the group consisting of tertiary butylperoxybenzoate (TBPB), di-tertiary-butyl peroxide (DTBP) and tert-butylperoxy 2-ethylhexyl carbonate (TBEC).
The polyol is present in an amount in the range of 30 mass% to 60 mass%, the macrodiol is present in an amount in the range of 1 mass% to 20 mass%, the polyacid is present in an amount in the range of 35 mass% to 60 mass%, the second catalyst is present in an amount in the range of 0.01 mass% to 2 mass%, the fluid medium is present in an amount in the range of 1 mass% to 30 mass% and the performance additive is present in an amount in the range of 0.1 mass% to 1 mass%, wherein the mass% of each ingredient is with respect to the total mass of the polyester polyol.
The fluid medium is present in an amount in the range of 2 mass% to 10 mass% with respect to the total mass of the polyester polyol.
The acrylic monomer is present in an amount in the range of 65 mass% to 85 mass%, the hydroxyl-functional acrylic monomer is present in an amount in the range of 10 mass% to 25 mass%, the fluid medium is present in an amount in the range of 15 mass% to 35 mass% and the initiator is present in an amount in the range of 2 mass% to 10 mass%, wherein the mass% of each ingredient is with respect to the total mass of the acrylic polyol.
Further, the present disclosure relates to a process for the preparation of a coating composition. The process comprises a step of of mixing predetermined amounts of a polyester polyol and optionally an acrylic polyol in a container under stirring at a speed in the range of 100 rpm to 1000 rpm for a time period in the range of 10 minutes to 30 minutes to obtain a first mixture. The predetermined amounts of a fluid medium and a first catalyst are added to the first mixture under stirring for a time period in the range of 10 minutes to 30 minutes to obtain a homogenized mixture. A predetermined amount of a flow and leveling additive is added to the homogenized mixture under stirring at a speed in the range of 50 rpm to 100 rpm for a time period in the range of 10 minutes to 20 minutes to obtain a hydroxy functional polymer component. A predetermined amount of an isocyanate component is mixed with the hydroxy functional polymer component under stirring for a time period in the range of 5 minutes to 15 minutes at a room temperature to obtain the coating composition, wherein a ratio of OH equivalent weight of the hydroxy functional polymer component to NCO equivalent weight of the isocyanate component is in the range of 1:0.5 to 1:2.
In an embodiment of the present disclosure, the polyester polyol is prepared by mixing predetermined amounts of at least one polyol, a macrodiol, at least one polyacid, a second catalyst, a performance additive and the fluid medium in a reactor to obtain a second mixture. The second mixture is polymerized under nitrogen at a temperature in the range of 180 ºC to 240 ºC to obtain a polymerized mixture and the polymerized mixture is cooled to a temperature in the range of 100 ºC to 150 ºC, followed by adding the first fluid medium and further cooling to a temperature in the range of 30 ºC to 40 ºC to obtain the polyester polyol.
In an embodiment of the present disclosure, the acrylic polyol is prepared by heating a predetermined amount of a fluid medium in a reactor to a temperature in the range of 100 ºC to 150 ºC under nitrogen and maintaining the temperature to obtain a heated fluid medium. Predetermined amounts of at least one acrylic monomer, a hydroxyl-functional acrylic monomer and an initiator are mixed to obtain a third mixture and the third mixture is added dropwise to the heated fluid medium over a time period in the range of 2 hours to 6 hours, followed by stirring for a time period in the range of 30 minutes to 120 minutes to obtain the acrylic polyol.
In an embodiment of the present disclosure, the polyester polyol is present in an amount in the range of 5 mass% to 100 mass% and the acrylic polyol is present in an amount in the range of 0 mass% to 95 mass%, wherein the mass% of each ingredient is with respect to the total mass of the hydroxy functional polymer component.
The polyester polyol is present in an amount in the range of 2 mass% to 50 mass%, the acrylic polyol is present in an amount in the range of 20 mass% to 50 mass%, the fluid medium is present in an amount in the range of 1 mass% to 30 mass%, the first catalyst is present in an amount in the range of 2 mass% to 10 mass%, the flow and leveling additive is present in an amount in the range of 0.1 mass% to 3 mass% and the isocyanate component is present in an amount in the range of 30 mass% to 70 mass%, wherein the mass% of each ingredient is with respect to the total mass of the coating composition.
The fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, a solvent naphtha (petroleum) light aromatic and mixture thereof, the first catalyst is selected from the group consisting of monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate, tetra-n-butyl titanate; the flow and leveling additive is selected from a group consisting of silicon based flow additive 10% solution in O-xylene, solution of a polyether-modified polydimethylsiloxane, solution of a polyacrylate, polyether-modified polydimethylsiloxane and low viscosity acrylate polymer; and the isocyanate component is selected from an aliphatic polyisocyanate and an aromatic polyisocyanate, wherein the aliphatic polyisocyanate is a dimer and trimer of isophorone diisocyanate and dimer of hexamethylene diisocyanate (HDI) and trimer of hexamethylene diisocyanate (HDI) and the aromatic polyisocyanate is selected from toluene diisocyanate based aromatic polyisocyanate and diphenylmethane diisocyanate based aromatic polyisocyanate
The polyol is present in an amount in the range of 30 mass% to 60 mass%, the macrodiol is present in an amount in the range of 1 mass% to 20 mass%, the polyacid is present in an amount in the range of 35 mass% to 60 mass%, the second catalyst is present in an amount in the range of 0.01 mass% to 2 mass%, the fluid medium is present in an amount in the range of 1 mass% to 30 mass% and the performance additive is present in an amount in the range of 0.1 mass% to 1 mass%, wherein the mass% of each ingredient is with respect to the total mass of the polyester polyol.
The polyol is selected from the group consisting of neopentyl glycol, 2-methyl-1,3-propanediol (MP diol), hexane diol, 1,3 propane diol, 1,2 propane diol, 1,4 butane diol, glycerine, ethylene glycol, diethylene glycol, butyl ethyl propanediol, trimethylolpropane, pentaerythritol and, cyclohexane dimethanol and mixture thereof.
The macrodiol is selected from the group consisting of polycaprolactone polyol, polyester polyol, polyether polyol, polyesterpolyether polyol and polycarbonate polyol.
The polyacid is selected from the group consisting of adipic acid, terephthalic acid, isophthalic acid, hexahydro phthalic anhydride, cyclohexane dicarboxylic acid and mixture thereof.
The second catalyst is selected from the group consisting of dibutylin oxide, monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate and tetra-n-butyl titanate.
The performance additive is selected from the group consisting of triphenyl phosphite, hypophosphorous acid and pentaerythritol tetrakis(3-(3,5-Di-tertiary-butyl-4-hydroxyphenyl) propionate).
The fluid medium is at least one selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, a solvent naphtha (petroleum) light aromatic and mixture thereof.
In an embodiment of the present disclosure, the polyester polyol is characterized by having an acid value in the range of 0.1 mg KOH/g to 10 mg KOH/g and an OH value in the range of 80 mg KOH/g to 140 mg KOH/g.
In an embodiment of the present disclosure, the acrylic polyol is characterized by having an OH value in the range of 80 mg KOH/g to 140 mg KOH/g.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWING
The present disclosure will now be described with the help of the accompanying drawing, in which:
Figure 1 illustrates (A) an optical microscopic image of scratch by knife on wooden panel coated with the self-healing coating composition before healing; (B) an optical microscopic image of self-healed scratch by knife on the wooden panel after 24 hours; (C) an optical microscopic image of scratch by key on the wooden panel coated with the self-healing coating composition before healing; (D) an optical microscopic image of self-healed scratch by key on the wooden panel after 24 hours in accordance with the present disclosure.
DETAILED DESCRIPTION
The present disclosure relates to a coating composition and a process of its preparation. Particularly, the present disclosure relates to a polyurethane coating composition that demonstrates self-healing properties.
Embodiments, of the present disclosure, will now be described with reference to the accompanying drawing.
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 for 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.
As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed elements.
The terms first, second, third, etc., should not be construed to limit the scope of the present disclosure as the aforementioned terms may be only used to distinguish one element, component, region, layer or section from another component, region, layer or section. Terms such as first, second, third etc., when used herein do not imply a specific sequence or order unless clearly suggested by the present disclosure.
Wood is increasingly used in indoor and outdoor applications such as constructions, furniture and the like. While in use, the wood products are subjected to damages due to mechanical aggressions, abrasion, scratches, moisture, heat, solvents and the like. These damages can be repaired by applying coating on the wood products. Generally, the coating is applied on the wooden products to perform two functions. The first function is to enhance the aesthetics/appearance of the wooden product and the second function is to preserve or to protect the aesthetic/appearance from any damages. There are various coating composition which are applied on the wooden products to protect them from the damages such as polyester based coating composition, polyurethane based coating composition and the like.
The polyurethane (PU) based self-healing coating composition are applied on the wooden products to protect them from any damages. However, the conventional polyurethane (PU) based self-healing coating composition are soft and hard block based thermoplastic polyurethanes (TPU). They are primarily made from polyether polyols which are solids at ambient temperature and require softening and re-solidifying process to demonstrate the self-healing property. Further, the other self-healing coating composition used for protecting the wooden products involves dynamic bonds such as diels-alder, dithiols, diselenide, imine, metal-ligand and the like. All these conventional coating compositions require external triggers such as elevated temperature, pH, UV-IR light and the like for healing.
Further, the coating composition containing encapsulated healing agents are used for protecting the wooden products. However, by using the coating containing encapsulated healing agents, healing cannot be repeated multiple times as the encapsulated capsules get exhausted.
The present disclosure provides a coating composition that has a self-healing property and is able to heal the damages at 20 °C to 60 °C (ambient) temperature for multiple times. Further, the present disclosure provides a coating composition that is simple and durable.
In a first aspect, the present disclosure provides a coating composition. Particularly, the present disclosure relates to a polyurethane coating composition that demonstrates self-healing properties.
In accordance with the embodiment of the present disclosure, the coating composition comprises:
a. a hydroxy functional polymer component comprising a polyol and optionally an acrylic polyol;
b. an isocyanate component;
c. a catalyst;
d. a flow and leveling additive; and
e. a fluid medium,
wherein a ratio of OH equivalent weight of the hydroxy functional polymer component to NCO equivalent weight of the isocyanate component is in the range of 1:0.5 to 1:2.
In an exemplary embodiment of the present disclosure, the ratio of OH equivalent weight of the hydroxy functional polymer component to NCO equivalent weight of the isocyanate component is 1:1. In another exemplary embodiment of the present disclosure, the ratio of OH equivalent weight of the hydroxy functional polymer component to NCO equivalent weight of the isocyanate component is 1:0.8. In yet another exemplary embodiment of the present disclosure, the ratio of OH equivalent weight of the hydroxy functional polymer component to NCO equivalent weight of the isocyanate component is 1: 1.2.
The mass ratio (in the claimed range) of the hydroxy functional polymer component to the isocyanate component is important as low isocyanate (NCO) causes partial curing leading to impaired mechanical properties such as drying, hardness and the like and excess of NCO causes cheesy film and slow drying.
In an embodiment of the present disclosure, the hydroxyl functional polymer component comprises a mixture of the polyester polyol and the acrylic polyol.
In an embodiment of the present disclosure, the polyester polyol is characterized by having an acid value in the range of 0.1 mg KOH/g to 10 mg KOH/g and an OH value in the range of 80 mg KOH/g to 140 mg KOH/g and non-volatile matter in the range of 60% to 80%. The acrylic polyol is characterized by having an OH value in the range of 80 mg KOH/g to 140 mg KOH/g and non-volatile matter (NVM) in the range of 65% to 80%.
In an exemplary embodiment of the present disclosure, the polyester polyol is characterized by having an acid value in the range of 4 mg KOH/g to 6 mgKOH/g and an OH value in the range of 100 mg KOH/g to 120 mgKOH/g and non-volatile matter (NVM-solid content) of 75%. In an exemplary embodiment of the present disclosure, the acrylic polyol is characterized by having an OH value 110 mg KOH/g and non-volatile matter (NVM-soild content) of 70%.
In an embodiment of the present disclosure, the resulting hydroxyl functional polymer component of a polyester polyol and acrylic polyol is characterized by having a hydroxyl value in the range of 80 mg KOH/g to 140 mg KOH/g.
In an embodiment of the present disclosure, the coating composition comprises the hydroxy functional polymer component in an amount in the range of 40 mass% to 60 mass%, the isocyanate component in an amount in the range of 30 mass% to 70 mass%, the catalyst in an amount in the range of 0.01 mass% to 1 mass%, the flow and leveling additive in an amount in the range of 0.1 mass% to 3 mass% and the fluid medium in an amount in the range of 2 mass% to 30 mass%, wherein the mass% of each ingredient is with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the polyester polyol is present in an amount in the range of 5 mass% to 100 mass% and the acrylic polyol is present in an amount in the range of 0 mass% to 95 mass%, wherein the mass% of each ingredient is with respect to the total mass of the hydroxy functional polymer component.
In an embodiment of the present disclosure, the isocyanate component is selected from an aliphatic polyisocyanate and an aromatic polyisocyanate, wherein the aliphatic polyisocyanate is selected from a dimer and trimer of isophorone diisocyanate and dimer of hexamethylene diisocyanate (HDI) and trimer of hexamethylene diisocyanate (HDI) (desmodur N3390) and the aromatic polyisocyanate is selected from toluene diisocyanate based aromatic polyisocyanate (desmodur L75) and diphenylmethane diisocyanate based aromatic polyisocyanate (desmodur VL or desmodur VL50). In an exemplary embodiment of the present disclosure, the isocyanate component is hexamethylene diisocyanate (desmodur N3390) diluted form (28% solid). In another exemplary embodiment of the present disclosure, the isocyanate component is aromatic polyisocyanate based on toluene diisocyanate diluted form (desmodur L75) (28% solid).
In an embodiment of the present disclosure, the catalyst is a first catalyst and a second catalyst, wherein the first catalyst is selected from the group consisting of monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate, tetra-n-butyl titanate and the second catalyst is selected from the group consisting of dibutylin oxide, monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate and tetra-n-butyl titanate. In an exemplary embodiment of the present disclosure, the first catalyst is dibutyl tin dilaurate.
In an embodiment of the present disclosure, the flow and leveling additive is selected from the group of silicon based flow additive 10% solution in O-xylene, solution of a polyether-modified polydimethylsiloxane (BYK 306), solution of a polyacrylate (BYK 358), polyether-modified polydimethylsiloxane (BYK 331) and low viscosity acrylate polymer (Resiflow LV). In an exemplary embodiment of the present disclosure, the flow and leveling additive is silicon based flow additive 10% solution in O-xylene.
In an embodiment of the present disclosure, the fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, a solvent naphtha (petroleum) light aromatic (solvent CIX) and mixture thereof. In an exemplary embodiment of the present disclosure, the fluid medium is ortho-xylene and butyl acetate (50:50 ratio).
In accordance with the present disclosure, the polyester polyol is a product of:
a. at least one polyol;
b. a macrodiol;
c. at least one polyacid;
d. the second catalyst;
e. the fluid medium; and
f. a performance additive, and
the acrylic polyol is a product of:
a. at least one acrylic monomer;
b. a hydroxyl-functional acrylic monomer;
c. the fluid medium and
d. an initiator.
In an embodiment of the present disclosure, the polyol is selected from the group consisting of neopentyl glycol, 2-methyl-1,3-propanediol (MP diol), hexane diol, 1,3 propane diol, 1,2 propane diol, 1,4 butane diol, glycerine, ethylene glycol, diethylene glycol, butyl ethyl propanediol, trimethylolpropane, pentaerythritol,cyclohexane dimethanol and mixture thereof. In an exemplary embodiment of the present disclosure, the polyol is neopentyl glycol, trimethylol propane and pentaerythritol.
In an embodiment of the present disclosure, the macrodiol is selected from the group consisting of polycaprolactone polyol, polyester polyol, polyether polyol, polyesterpolyether polyol and polycarbonate polyol. In an exemplary embodiment of the present disclosure, the macrodiol is polycaprolactone polyol (CAPA 2101A).
In an embodiment of the present disclosure, the macrodiol is characterized by having molecular weight in the range of 700 to 4000 and hydroxyl (OH) value in the range from 20 mgKOH/g to 150 mgKOH/g.
The macrodiol exhibits self-healing property due to its viscoelastic property.
In an embodiment of the present disclosure, the polyacid is selected from the group consisting of adipic acid, terephthalic acid, isophthalic acid, hexahydrophthalic anhydride, cyclohexane dicarboxylic acid and mixture thereof. In an exemplary embodiment of the present disclosure, the polyacid is adipic acid, isophthalic acid and hexahydrophthalic acid.
In an embodiment of the present disclosure, the second catalyst is selected from the group consisting of dibutylin oxide, monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate and tetra-n-butyl titanate. In an exemplary embodiment of the present disclosure, the second catalyst is dibutylin oxide (DBTO).
In an embodiment of the present disclosure, the fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, solvent naphtha (petroleum) light aromatic (reffered as solvent CIX) and mixture thereof. In an exemplary embodiment of the present disclosure, the fluid medium is ortho-xylene.
In an embodiment of the present disclosure, the performance additive is selected from the group consisting of triphenyl phosphite, hypophosphorous acid and pentaerythritol tetrakis(3-(3,5-Di-tertiary-butyl-4-hydroxyphenyl) propionate) (irgonox 1010). In an exemplary embodiment of the present disclosure, the performance additive is triphenyl phosphite.
Triphenyl phosphite is used as a performance additive to improve the color of the resin.
In an embodiment of the present disclosure, the acrylic monomer is selected from the group consisting of butyl acrylate, styrene, methyl methacrylate, methacrylic acid, acrylic acid, isobutyl acrylate, isobutyl methacrylate, cyclohexyl methacrylate, stearyl acrylate, stearyl methacrylate, octyl methacrylate, tertiary butyl methacrylate, a synthetic saturated monocarboxylic acid with a highly branched structure containing ten carbon atoms (Vevoa 10 monomer), ethyl hexyl acrylate and mixture thereof.
In an embodiment of the present disclosure, the hydroxyl-functional acrylic monomer is selected from the group consisting of 2-hydroxy ethyl acrylate, 2-hydroxy propyl methyl acrylate and 2-hydroxyl ethyl methacrylate.
In an embodiment of the present disclosure, the fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, ortho-xylene, butyl acetate, methoxy propyl acetate, solvent CIX and mixture thereof. In an exemplary embodiment of the present disclosure, the fluid medium is butyl acetate.
In an embodiment of the present disclosure, the initiator is selected from the group consisting of tertiary Butylperoxybenzoate (TBPB), Di-tertiary-butyl peroxide (DTBP) and tert-Butylperoxy 2-ethylhexyl carbonate (TBEC). In an exemplary embodiment of the present disclosure, the initiator is tert-Butylperoxy 2-ethylhexyl carbonate (TBEC).
In an embodiment of the present disclosure, the polyester polyol comprises the polyol in an amount in the range of 30 mass% to 60 mass%, the macrodiol in an amount in the range of 1 mass% to 20 mass%, the polyacid in an amount in the range of 35 mass% to 60 mass%, the second catalyst in an amount in the range of 0.01 mass% to 2 mass%, the fluid medium in an amount in the range of 1 mass% to 30 mass% and the performance additive in an amount in the range of 0.1 mass% to 1 mass%, wherein the mass% of each ingredient is with respect to the total mass of the polyester polyol.
In an embodiment of the present disclosure, the polyester polyol comprises the fluid medium in an amount in the range of 2 mass% to 10 mass% with respect to the total mass of the polyester polyol.
In an embodiment of the present disclosure, the acrylic polyol comprises the acrylic monomer in an amount in the range of 65 mass% to 85 mass%, the hydroxyl-functional acrylic monomer in an amount in the range of 10 mass% to 25 mass%, the fluid medium in an amount in the range of 15 mass% to 35 mass% and the initiator in an amount in the range of 2 mass% to 15 mass%, wherein the mass% of each ingredient is with respect to the total mass of the acrylic polyol.
In a first exemplary embodiment of the present disclosure, the polyester polyol comprises:
• 33.2 mass% of neopentyl glycol, 8.1 mass% of trimethylol propane and 0.5 mass% of pentaerythritol as a polyol component;
• 2.8 mass% of adipic acid, 40.2 mass% of isophthalic acid, and 10.9 mass% of hexahydrophthalic anhydride as a polyacid;
• 0.1 mass% of dibutylin oxide (DBTO) as the second catalyst;
• 4 mass% of ortho-xylene as the fluid medium; and
• 0.2 mass% of triphenyl phosphite as a performance additive,
wherein the mass% of each ingredient is with respect to the total mass of the polyester polyol.
In a second exemplary embodiment of the present disclosure, the polyester polyol comprises:
• 28.9 mass% of neopentyl glycol, 6.9 mass% of trimethylol propane and 0.5 mass% of pentaerythritol as a polyol component;
• 12.5 mass% of CAPA-caprolactone polyol as a macrodiol;
• 2.4 mass% of adipic acid, 35 mass% of isophthalic acid, and 9.5 mass% of hexahydrophthalic anhydride as a polyacid;
• 0.1 mass% of dibutylin oxide (DBTO) as the second catalyst;
• 4 mass% of ortho-xylene as the fluid medium; and
• 0.2 mass% of triphenyl phosphite as a performance additive,
wherein the mass% of each ingredient is with respect to the total mass of the polyester polyol.
In an exemplary embodiment of the present disclosure, the acrylic polyol comprises:
• 15.6 mass% of butyl acrylate, 8 mass% of styrene, 10 mass% of Veova, 13.6 mass% of methyl methacrylate, 0.4 mass% of methacrylic acid as an acrylic monomer;
• 18 mass% of HEMA as a hydroxyl-functional acrylic monomer;
• 28.7 mass% butyl acetate as a fluid medium; and
• 5.7 mass% tertiary butyl peroxy 2-ethyl hexyl carbonate as an initiator,
wherein the mass% of each ingredient is with respect to the total mass of the acrylic polyol.
The coating composition is 2K coating composition.
The coating composition of the present disclosure can be applied on the substrate by the conventional methods of paint application. The coating composition of the present disclosure can be applied as a top coat for wooden finishes. The coating composition of the present disclosure when applied on the wooden substrate can heal the scratches at an ambient temperature (25 °C to 60 °C) for multiple times without any external stimulus and within the time duration from 5 minutes to 15 days. Moreover, the coating composition of the present disclosure demonstrates healing of the scratches on cured coating film without heat-softening.
The coating composition can be optionally heated to any elevated temperature or can be provided with any external stimulus rubbing, buffing till the coating integrity is not disturbed to provide the healing faster.
In a second aspect, the present disclosure provides a process for the preparation of a coating composition.
In an embodiment of the present disclosure, the process for the preparation of the coating composition comprises the following steps:
(i) mixing predetermined amounts of a polyester polyol and optionally an acrylic polyol in a container under stirring at a speed in the range of 100 rpm to 1000 rpm for a time period in the range of 10 minutes to 30 minutes to obtain a first mixture;
(ii) adding predetermined amounts of a fluid medium and a first catalyst to the first mixture under stirring for a time period in the range 10 minutes to 30 minutes to obtain a homogenized mixture;
(iii) adding a predetermined amount of a flow and leveling additive to the homogenized mixture under stirring at a speed in the range of 50 rpm to 100 rpm for a time period in the range of 10 minutes to 20 minutes to obtain a hydroxy functional polymer component; and
(iv) mixing a predetermined amount of an isocyanate component to the hydroxy functional polymer component at a room temperature for a time period in the range of 5 minutes to 15 minutes at a room temperature to obtain the coating composition,
wherein a ratio of OH equivalent weight of the hydroxy functional polymer component to NCO equivalent weight of the isocyanate component is in the range of 1:0.5 to 1:2.
The process for the preparation of the coating composition is explained in detail.
In a first step, the predetermined amounts of a polyester polyol and optionally an acrylic polyol are mixed in a container under stirring at a speed in the range of 100 rpm to 1000 rpm for a time period in the range of 10 minutes to 30 minutes to obtain a first mixture.
In an embodiment of the present disclosure, the predetermined amounts of the polyester polyol and the acrylic polyol are mixed in a container under stirring at a speed in the range of 100 rpm to 1000 rpm for a time period in the range of 10 minutes to 30 minutes to obtain a first mixture.
In an exemplary embodiment of the present disclosure, the stirring is carried out at 500 rpm for 20 minutes to obtain a first mixture.
In a second step, the predetermined amounts of a fluid medium and a first catalyst are added to the first mixture for a time period in the range of 10 minutes to 30 minutes to obtain a homogenized mixture.
In an exemplary embodiment of the present disclosure, the addition of the fluid medium and the catalyst is carried out for 20 minutes.
In an embodiment of the present disclosure, the fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, solvent CIX and mixture thereof. In an exemplary embodiment of the present disclosure, the fluid medium is a combination of ortho-xylene and butyl acetate (50:50 ratio).
In an embodiment of the present disclosure, the first catalyst is selected from the group consisting of monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate, tetra-n-butyl titanate.de In an exemplary embodiment of the present disclosure, the first catalyst is dibutyl tin dilaurate.
The catalyst is organometallic catalyst.
In a third step, a predetermined amount of a flow and leveling additive is added to the homogenized mixture under stirring at a speed in the range of 50 rpm to 100 rpm for a time period in the range of 10 minutes to 20 minutes to obtain a hydroxy functional polymer component.
In an embodiment of the present disclosure, the flow and leveling additive is selected from the group of silicon based flow additive 10% solution in O-xylene, solution of a polyether-modified polydimethylsiloxane (BYK 306), solution of a polyacrylate (BYK 358), polyether-modified polydimethylsiloxane (BYK 331) and low viscosity acrylate polymer (Resiflow LV). In an exemplary embodiment of the present disclosure, the additive is silicon based flow additive 10% solution in O-xylene.
In an exemplary embodiment of the present disclosure, the stirring is carried out at 80 rpm for 15 minutes to obtain a polyol component.
In a fourth step, a predetermined amount of an isocyanate component is mixed to the hydroxy functional polymer component at a room temperature for a time period in the range of 5 minutes to 15 minutes at a room temperature to obtain the coating composition.
In an embodiment of the present disclosure, the isocyanate component is selected from an aliphatic polyisocyanate and an aromatic polyisocyanate, wherein the aliphatic polyisocyanate is selected from a dimer and trimer of isophorone diisocyanate and a dimer of hexamethylene diisocyanate (HDI) and trimer of hexamethylene diisocyanate (HDI) and the aromatic polyisocyanate is selected from toluene diisocyanate based aromatic polyisocyanate (desomodur L75) and diphenylmethane diisocyanate based aromatic polyisocyanate (desmodur VL or desmodur VL50). In an exemplary embodiment of the present disclosure, the isocyanate component is HDI trimer (desmodur N3390). In another exemplary embodiment of the present disclosure, the isocyanate component is TDI (desmodur L75).
The isocyanate component is used for curing the polymer.
In an exemplary embodiment of the present disclosure, the mixing is carried out at room temperature for 10 minutes to obtain the coating composition.
In an embodiment of the present disclosure, the ratio of OH equivalent weight of a hydroxy functional polymer component to NCO equivalent weight of an isocyanate component is in the range of 1:0.5 to 1:2. In an exemplary embodiment of the present disclosure, the ratio of OH equivalent weight of a hydroxy functional polymer component to NCO equivalent weight of an isocyanate component is 1:1. In another exemplary embodiment of the present disclosure, the ratio of OH equivalent weight of a hydroxy functional polymer component to NCO equivalent weight of an isocyanate component is 1: 0.8. In still another exemplary embodiment of the present disclosure, the ratio of OH equivalent weight of a hydroxy functional polymer component to NCO equivalent weight of an isocyanate component is 1:1.2.
In an embodiment of the present disclosure, the polyester polyol is present in an amount in the range of 5 mass% to 100 mass% and the acrylic polyol is present in an amount in the range of 0 mass% to 95 mass%, wherein the mass% of each ingredient is with respect to the total mass of the hydroxy functional polymer component.
In another embodiment of the present disclosure, the polyester polyol is present in the range of 2 mass% to 50 mass%, the acrylic polyol is present in the range of 20 mass% to 50 mass%, the fluid medium is present in the range of 1 mass% to 30 mass%, the first catalyst is present in the range of 0.01 mass% to 1 mass%, the flow and leveling additive is present in the range of 0.1 mass% to 3 mass% and the isocyanate component is present in the range of 30 mass% to 70 mass%, wherein the mass% of each ingredient is with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the fluid medium is present in an amount in the range of 2 mass% to 10 mass% in the coating composition.
In accordance with the present disclosure, the polyester polyol is prepared by following steps:
(i) mixing predetermined amounts of at least one polyol, a macrodiol, at least one polyacid, a second catalyst, a performance additive and the fluid medium in a reactor to obtain a second mixture;
(ii) polymerizing the second mixture under nitrogen at a temperature in the range of 180 ºC to 240 ºC to obtain a polymerized mixture; and
(iii) cooling the polymerized mixture to a temperature in the range of 100 ºC to 150 ºC followed by adding the fluid medium and further cooling to a temperature in the range of 30 ºC to 40 ºC to obtain the polyester polyol.
The process for the preparation of the polyester polyol is explained in detail.
In a first step, predetermined amounts of at least one polyol, a macrodiol, at least one polyacid, a second catalyst, a performance additive and a fluid medium are mixed in a reactor to obtain a second mixture.
In an embodiment of the present disclosure, the polyol is selected from the group consisting of neopentyl glycol, 2-methyl-1,3-propanediol (MP diol), hexane diol, , 1,3 propane diol, 1,2 propane diol, 1,4 butane diol, glycerine, ethylene glycol, diethylene glycol, butyl ethyl propanediol, trimethylolpropane, pentaerythritol, cyclohexane dimethanol and mixture thereof. In an exemplary embodiment of the present disclosure, the polyol is neopentyl glycol, trimethylol propane and pentaerythritol. In an embodiment of the present disclosure, the macrodiol is selected from the group consisting of polycaprolactone polyol, polyester polyol, polyether polyol, polyesterpolyether polyol and polycarbonate polyol. In an exemplary embodiment of the present disclosure, the macrodiol is polycaprolactone polyol. In another exemplary embodiment of the present disclosure, the macrodiol is CAPA 2101A.
In an embodiment of the present disclosure, the polyacid is selected from the group consisting of adipic acid, terephthalic acid, isophthalic acid, hexahydro phthalic anhydride, cyclohexane dicarboxylic acid and mixture thereof. In an exemplary embodiment of the present disclosure, the polyacid is adipic acid, isophthalic acid and hexahydrophthalic anhydride.
In an embodiment of the present disclosure, the second catalyst is selected from the group consisting of dibutylin oxide, monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate and tetra-n-butyl titanate. In an exemplary embodiment of the present disclosure, the catalyst is DBTO.
In an embodiment of the present disclosure, the performance additive is selected from triphenyl phosphite, hypophosphorous acid and pentaerythritol tetrakis(3-(3,5-Di-tertiary-butyl-4-hydroxyphenyl) propionate) (irgonox 1010). In an exemplary embodiment of the present disclosure, the performance additive is triphenyl phosphite.
In an embodiment of the present disclosure, the fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, solvent CIX and mixture thereof. In an exemplary embodiment of the present disclosure, the fluid medium is ortho-xylene.
In a second step, the second mixture is polymerized under nitrogen at a temperature in the range of 180 ºC to 240 ºC to obtain a polymerized mixture.
In an exemplary embodiment of the present disclosure, the polymerization temperature is 230 ºC.
In a third step, the polymerized mixture is cooled to a temperature in the range of 100 ºC to 150 ºC followed by adding the fluid medium and further cooling to a temperature in the range of 30 oC to 40 oC to obtain the polyester polyol.
The so obtained polyester polyol is in liquid form.
In an exemplary embodiment of the present disclosure, the polymerized mixture is cooled at 130 ºC followed by adding ortho-xylene and further cooled at 35 ºC.
In an embodiment of the present disclosure, the polyol is present in the range of 30 mass% to 60 mass%, the macrodiol is present in the range of 1 mass% to 20 mass%, the polyacid is present in the range of 35 mass% to 60 mass%, the second catalyst is present in the range of 0.01 mass% to 2 mass%, the fluid medium is in the range of 1 mass% to 30 mass% and the performance additive is in the range of 0.1 mass% to 1 mass%, wherein the mass% of each ingredient is with respect to the total mass of the polyester polyol.
In an embodiment of the present disclosure, the fluid medium is present in an amount in the range of 2 mass% to 10 mass% in the polyester polyol.
In an embodiment of the present disclosure, the polyester polyol is characterized by having an acid value in the range of 0.1 mg KOH/g to 10 mg KOH/g and an OH value in the range of 80 mg KOH/g to 140 mg KOH/g and non-volatile matter (NVM-solid content) in the range of 60% to 80%. In an exemplary embodiment of the present disclosure, the polyester polyol is characterized by having an acid value of 5 mg KOH/g and an OH value of 110 mg KOH/g and non-volatile matter (NVM-solid content) is 70%.
In accordance with the present disclosure, the acrylic polyol is prepared by following steps:
(i) heating a predetermined amount of a fluid medium in a reactor to a temperature in the range of 100 ºC to 150 ºC under nitrogen and maintaining the temperature to obtain a heated fluid medium;
(ii) mixing predetermined amounts of at least one acrylic monomer, a hydroxyl-functional acrylic monomer and an initiator to obtain a third mixture; and
(iii) adding dropwise the third mixture to the heated fluid medium over a time period in the range of 2 hours to 6 hours, followed by stirring for a time period in the range of 30 minutes to 120 minutes to obtain the acrylic polyol.
The process for the preparation of the acrylic polyol is explained in detail.
In a first step, a predetermined amount of a fluid medium is heated in a reactor to a temperature in the range of 100 ºC to 150 ºC under nitrogen and the temperature is maintained to obtain a heated fluid medium.
In an embodiment of the present disclosure, the fluid medium is at least one selected from the group consisting of ortho-xylene, butyl acetate, ortho-xylene, butyl acetate, methoxy propyl acetate, solvent CIX. In an exemplary embodiment of the present disclosure, the fluid medium is butyl acetate.
In an exemplary embodiment, the fluid medium is heated in a reactor at 130 ºC.
In a second step, predetermined amounts of at least one acrylic monomer, a hydroxyl-functional acrylic monomer and an initiator are mixed to obtain a third mixture.
In an embodiment of the present disclosure, the acrylic monomer is selected from the group consisting of butyl acrylate, styrene, methyl methacrylate, methacrylic acid, acrylic acid, isobutyl acrylate, isobutyl methacrylate, cyclohexyl methacrylate, stearyl acrylate, stearyl methacrylate, octyl methacrylate, tertiary butyl methacrylate, a synthetic saturated monocarboxylic acid with a highly branched structure containing ten carbon atoms (Vevoa 10 monomer), ethyl hexyl acrylate and mixture thereof. In an exemplary embodiment of the present disclosure the acrylic monomer is a combination of styrene, butyl acrylate, methyl acrylate, and methacrylic acid and Vevoa 10 monomer.
In an embodiment of the present disclosure, the hydroxyl- functional acrylic monomer is selected from the group consisting of 2-hydroxy ethyl acrylate, 2-hydroxy propyl methyl acrylate and 2- hydroxyl ethyl methacrylate. In an exemplary embodiment of the present disclosure, the hydroxyl-functional acrylic monomer is 2-hydroxy ethyl methacrylate (HEMA).
In an embodiment of the present disclosure, the initiator is selected from the group consisting of tertiary butylperoxybenzoate (TBPB), Di-tertiary-butyl peroxide (DTBP) and tert-Butylperoxy 2-ethylhexyl carbonate (TBEC). In an exemplary embodiment of the present disclosure, the initiator is tert-Butylperoxy 2-ethylhexyl carbonate (TBEC).
In a third step, the third mixture is added dropwise to the heated fluid medium over a time period in the range of 2 hours to 6 hours, followed by stirring for a time period in the range of 30 minutes to 120 minutes to obtain the acrylic polyol.
In an exemplary embodiment of the present disclosure, the third mixture is added to the heated fluid medium over 4 hours, followed by stirring for 60 minutes to obtain the acrylic polyol.
In an embodiment of the present disclosure, the acrylic monomer is present in the range of 65 mass% to 85 mass%, the hydroxyl-functional acrylic monomer is present in the range of 10 mass% to 25 mass%, the fluid medium is present in the range of 15 mass% to 35 % and the initiator is present in the range of 2 mass% to 10 mass%, wherein the mass% of each ingredient is with respect to the total mass of the acrylic polyol.
The acrylic polyol is characterized by having an OH value in the range of 80 mg KOH/g to 140 mg KOH/g and non-volatile matter (NVM) in the range of 65% to 80%. In an exemplary embodiment of the present disclosure, the acrylic polyol is characterized by having an OH value of 110 mg KOH/g and non-volatile matter (NVM) is 75 %.
The process for the preparation of the coating composition in accordance with the present disclosure is simple, economic and is convenient for industrial scale-up.
The coating composition of the present disclosure provides good gloss, self-healing even after 2000 hours of QUV-B. Further, the coating composition obtained in accordance with the present disclosure, provides healing to the substrate without requiring any external trigger such as temperature, pH, UV-IR light and the like. Thus, it is self-healing coating composition which heals at ambient temperature and does not require any stimulus. The scratches are healed multiple times. The polyurethane coating composition in accordance with the present disclosure is a clear composition and can be applied as a top coat for wood finishes.
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 purposes 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 a polyester polyol in accordance with the present disclosure
General procedure: The preparation of a the polyester polyol was carried out in a reactor provided with a distilling column filed with Raschig rings and dean-stark. Dean stark was used for effective removal of water generated during reaction and rasching rings were used to avoid the polyol losses.
The predetermined amounts of at least one polyol, a macrodiol, at least one polyacid, a second catalyst, a performance additive and the fluid medium were mixed in a reactor to obtain a second mixture. The second mixture was polymerized under nitrogen at 230 ºC to obtain a polymerized mixture having acid value of in the range of 1 mgKOH/g to 10 mgKOH/g. The polymerized mixture was cooled down to 130 ºC followed by adding the fluid medium and further cooled at 35 ºC to obtain the polyester polyol. The solid content of so obtained polyester polyol is 75%. The so obtained polyester polyol had an acid value of 5 mgKOH/g and an OH value of 110 mgKOH/g.
The polyester polyols were prepared in Examples P1 and P2 by following the general procedure as above. The predetermined amounts of the specific ingredients of the polyester polyols are as given in table 1.
Table 1: Predetermined amounts of the ingredients used in examples P1 and P2
Ingredients and their function P1 P2
Sr. no. Materials Function Weight in grams Weight in grams
1. Neopentyl glycol Polyol 33.2 28.9
2. Trimethylol propane Polyol 8.1 6.9
3. Pentaerythritol Polyol 0.5 0.5
4. CAPA-caprolactone polyol macrodiol ---- 12.5
5. Adipic acid polyacid 2.8 2.4
6. Isophthalic acid polyacid 40.2 35
7. Hexahydrophthalic anhydride Polyacid 10.9 9.5
8. DBTO-dibutylin Oxide Second catalyst 0.1 0.1
9. Triphenyl phosphite Performance Additive 0.2 0.2
10. Ortho-xylene Fluid medium 4 4
Total 100 100
Experiment 1 (B): Process for preparation of an acrylic polyol (P3) in accordance with the present disclosure
The preparation of the acrylic polyol was carried out in a reactor provided with a condenser and nitrogen inlet. 28.7 g of butyl acetate (fluid medium) was heated in a reactor to 130 ºC under nitrogen and the temperature was maintained to obtain a heated butyl acetate. In a separate flask, 15.6 g of butyl acrylate (acrylic monomer), 8 g of styrene (acrylic monomer), 10 g of VeoVa (acrylic monomer), 18 g of HEMA (hydroxyl-functional acrylic monomer), 13.6 g of methyl methacrylate (acrylic monomer), 0.4 g of methacrylic acid (acrylic monomer) and 5.7 g of tertiary Butyl peroxy 2-ethyl hexyl carbonate (TBEC) (peroxide initiator) were mixed to obtain a third mixture. The so obtained third mixture is added dropwise to the heated butyl acetate over 4 hours, followed by stirring for 60 minutes to obtain the acrylic polyol. The so obtained acrylic polyol has 70% solid and an OH value of 110 mgKOH/g.
Experiment 1 (C): Process for preparation of a coating composition in accordance with the present disclosure
General procedure: Predetermined amounts of the polyester polyol (as prepared in Experiment 1 (A) and the acrylic polyol (as prepared in Experiment 1(B)) were mixed in a stain-less steel container under stirring at 500 rpm for 15 minutes to obtain a first mixture. The predetermined amounts of a fluid medium and a first catalyst to the first mixture under stirring for minutes to 20 minutes to obtain a homogenized mixture. A predetermined amount of a flow and leveling additive was added to the homogenized mixture under stirring at 100 rpm for 15 minutes to obtain a hydroxy functional polymer component. A predetermined amount of an isocyanate component was added into the hydroxy functional polymer component A and mixed well for 5 minutes to 10 minutes at a room temperature to obtain the coating composition. A ratio of OH equivalent weight of the hydroxy functional polymer component and NCO equivalent weight of the isocyanate component wass in the range of 1:0.5 to 1:2.
The coating compositions were prepared in Examples E1 and E6 by following the general procedure as above. Further, comparative coating compositions were also prepared with the ingredients details as mentioned in the ‘comparative examples E1 to E3’. The comparative coating composition E1 was based on only polyester polyol P1 (without macrodiols), the comparative coating composition E2 was based on only acrylic polyol and the comparative coating composition E3 wass based on the acrylic polyol and polyester polyol P1 (without macrodiols). The predetermined amounts of the specific ingredients of the coating compositions are as given in Table 2.
Table 2: Predetermined amounts of the ingredients used in examples E1 to E6 and comparative examples E1 to E3
Ingredients and their function E1
E2
E3 E4 E5 E6 E7 Comparative E1 Comparative E2 Comparative E3
Sr. no. Materials Function
PART A
1. Acrylic Polyol (P3) of Experiment 1 (B) Resin 41 36.8 23 36.8 36.8 36.8 --- --- 46 23
2. Polyester Polyol P1 of Experiment 1 (A) Resin --- --- --- --- --- --- --- 46 --- 23
3. Polyester Polyol P2 Experiment 1 (A) Resin 5 9.2 23 9.2 9.2 9.2 46 --- --- ----
4. Tin complex 10% solution in O-xylene (dibutyl tin dilaurate) First Catalyst 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3
5. Silicon based flow Additive 10% solution in O-xylene Flow and levelling 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5
6. O-xylene + butyl acetate (50:50) fluid medium 3.2 3.2 3.2 3.2 3.2 3.2 3.2 3.2 3.2 3.2
Part B
7. Aliphatic isocyanate: hexamethylene diisocyanate (HDI) trimer diluted in butyl acetate and O-xylene solvent mixture (28% solid) Aliphatic polyisocyanat 50 50 50 40 60 --- 50 50 50 50
8. Aromatic polyisocyanate: TDI: Toluene diisocyanate diluted form (28% solid) Aromatic polyisocyanat --- --- --- --- --- 50 ---- --- --- ---
9. Acrylic polyol P3 : Polyester polyol P2 ratio 90:10 80:20 50:50 80:20 80:20 80:20 ---- --- --- 50:50
10. OH:NCO ratio 1:1 1:1 1:1 1:0.8 1:1.2 1:1 1:1 1:1 1:1 1:1
For the sake of brevity, multiple number of experiments are not included in the specification. However, the other ingredients having similar functionality can be used in the preparation of the coating composition of the present disclosure and the coating composition will give similar results.
Experiment 1(D): Method of applying a coating composition in accordance with the present disclosure
A substrate such as wooden panel was coated with the coating composition as prepared in Experiment 1(C) followed by curing for 7 days at room temperature.
The so obtained coated wooden panel was further tested for self-healing and other properties.
Experiment 2: Characterization study of the coating in accordance with the present disclosure
(I) Self-healing property testing:
The coating compositions prepared in accordance with the present disclosure were subjected to the characterization studies in order to study the self-healing properties by using Crockmeter instrument.
% Gloss recovery was correlated to % self-healing and was determined as follow (reference: Coatings 2021, 11, 1328).
Coating composition as prepared in Experiment 1(C) was applied on a wooden panel and allowed to cure for 7 days at ambient temperature. After this time % SH was determined. Initial gloss of coating was measured, then same coating was subjected to 5 cycles of scratches using 3M 9 micron polishing paper by crockmeter instrument. Gloss was measured immediately on scratched area and coating was kept at ambient temperature for healing and gloss was measured after 24 hours % self-healing was measured by using following formula
The results of the test are summarized in Table 3 below.
(II) Physico-chemical properties analysis of a coating composition in accordance with the present disclosure
The coating compositions were evaluated for their physico-chemical properties. Table 3 below shows the properties of the coating compositions with appropriate values.
Table 3: Physicochemical properties of the coating composition in accordance with the present disclosure
Performance property E1
E2
E3 E4 E5 E6 E7 Comparative E1 Comparative E2 Comparative E3
Initial Gloss at 60 ºC 95 96 93 95 94 92 91 89 94 91
Gloss after scratches at 60 ºC 74 73 78 74 73 60 71 74 74 73
Gloss recovery after 24 hours at 60 ºC 92 94 92 92 92 75 90 80 90 84
% Self-healing 85.7 91.3 93.3 85.71 90.47 46.87 95 40 70 61.1
% Gloss retention after 2000 hours QUV-B 99 99 99 99 99 50 99 97 99 97
% Self-healing after 2000 hours QUV-B 83 91 92 85 90 38 94 35 60 50
Ease of Application Good Good Good Good Good Good Good Good Good Good
From Table 3, it is observed that the coating compositions (E1-E5 and E7) prepared in accordance with the present disclosure showed good % self-healing, gloss recovery after 24 hours and % gloss retention after 2000 hours QUV-B as compared to the comparative coating compositions (1 to 3). The comparative coating compositions show poor % self-heaing and % Self-healing after 2000 hours QUV-B. However, the coating composition (E6) which is prepared in accordance with the present disclosure but by using aromatic polyisocyanate based on toluene diisocyante exhibits poor-self-healing property due to the rigid nature of the TDI as compared to aliphatic long chain HDI trimer. The rigid nature of TDI imparts hardness to the coating film and had less viscoelastic property as compared to HDI trimer based coating composition. Further, the rheological properties of the coating compositions in accordance with the present disclosure show good ease of application.
Figure 1 (A-D) illustrates the self-healing property of the coating composition E3 (50:50 of polyester polyol P2 (with macrodiol) and acrylic polyol P3) in accordance with the present disclosure, indicating the importance of macrodiol in the polyester polyol
TECHNICAL ADVANCEMENTS
The present disclosure described herein above has several technical advantages including, but not limited to, the realization of;
? a coating composition that:
• heals the damages at 20 ºC to 60 ºC;
• heals the damages multiple times;
• heals the damages without the incorporation of any dynamic covalent bonds such as diels-Alder, dithiols, diselenide, imine, metal-ligand and the like; and
• has attractive and aesthetic finish; and
? a process for the preparation of a coating composition that is
• simple and economic.
The embodiments herein and the various features and advantageous details thereof are explained with reference to the non-limiting embodiments in the following description. Descriptions of well-known components and processing techniques are omitted so as to not unnecessarily obscure the embodiments herein. The examples used herein are intended merely to facilitate an understanding of ways in which the embodiments herein may be practiced and to further enable those of skill in the art to practice the embodiments herein. Accordingly, the examples should not be construed as limiting the scope of the embodiments herein.
The foregoing description of the specific embodiments so fully reveal the general nature of the embodiments herein that others can, by applying current knowledge, readily modify and/or adapt for various applications such specific embodiments without departing from the generic concept, and, therefore, such adaptations and modifications should and are intended to be comprehended within the meaning and range of equivalents of the disclosed embodiments. It is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation. Therefore, while the embodiments herein have been described in terms of preferred embodiments, those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the embodiments as described herein.
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 disclosure to achieve one or more of the desired object or results.
Any discussion of documents, acts, materials, devices, articles or the like that has been included in this specification is solely for the purpose of providing a context for the disclosure. It is not to be taken as an admission that any or all of these matters form a part of the prior art base or were common general knowledge in the field relevant to the disclosure as it existed anywhere before the priority date of this application.
The numerical values mentioned for the various physical parameters, dimensions or quantities are only approximations and it is envisaged that the values higher/lower than the numerical values assigned to the parameters, dimensions or quantities fall within the scope of the disclosure, unless there is a statement in the specification specific to the contrary.
While considerable emphasis has been placed herein on the components and component parts of the preferred embodiments, it will be appreciated that many embodiments can be made and that many changes can be made in the preferred embodiments without departing from the principles of the disclosure. These and other changes in the preferred embodiment as well as other embodiments 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. ,CLAIMS:WE CLAIM:
1. A coating composition comprising:
a. a hydroxy functional polymer component comprising polyester polyol and optionally an acrylic polyol;
b. an isocyanate component;
c. a catalyst;
d. a flow and leveling additive; and
e. a fluid medium,
wherein a ratio of OH equivalent weight of said hydroxy functional polymer component to NCO equivalent weight of said isocyanate component is in the range of 1:0.5 to 1:2.
2. The composition as claimed in claim 1, wherein said hydroxyl functional polymer component comprises a mixture of said polyester polyol and said acrylic polyol.
3. The composition as claimed in claim 1, wherein
• said polyester polyol is characterized by having
? an acid value in the range of 0.1 mg KOH/g to 10 mg KOH/g; and
? an OH value in the range of 80 mg KOH/g to 140 mg KOH/g; and
• said acrylic polyol is characterized by having an OH value in the range of 80 mg KOH/g to 140 mg KOH/g.
4. The composition as claimed in claim 1, wherein
• said hydroxy functional polymer component is present in an amount in the range of 40 mass% to 60 mass%;
• said isocyanate component is present in an amount in the range of 30 mass% to 70 mass%;
• said catalyst is present in an amount in the range of 0.01 mass% to 1 mass%;
• said flow and leveling additive is present in an amount in the range of 0.1 mass% to 3 mass%; and
• said fluid medium is present in an amount in the range of 1 mass% to 30 mass%,
wherein said mass% of each ingredient is with respect to the total mass of said coating composition.
5. The composition as claimed in claim 4, wherein said fluid medium is present in an amount in the range of 2 mass% to 10 mass% with respect to the total mass of said coating composition.
6. The composition as claimed in claim 1, wherein
• said polyester polyol is present in an amount in the range of 5 mass% to 100 mass%; and
• said acrylic polyol is present in an amount in the range of 0 mass% to 95 mass%,
wherein said mass% of each ingredient is with respect to the total mass of said hydroxy functional polymer component.
7. The composition as claimed in claim 1, wherein said isocyanate component is selected from an aliphatic polyisocyanate and an aromatic polyisocyanate, wherein said aliphatic polyisocyanate is selected from a dimer and trimer of isophorone diisocyanate and dimer of hexamethylene diisocyanate (HDI) and trimer of hexamethylene diisocyanate (HDI); and said aromatic polyisocyanate is selected from toluene diisocyanate based aromatic polyisocyanate and diphenylmethane based aromatic polyisocyanate.
8. The composition as claimed in claim 1, wherein said catalyst is a first catalyst and a second catalyst, wherein
• said first catalyst is selected from the group consisting of monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate, tetra-n-butyl titanate and; and
• said second catalyst is selected from the group consisting of dibutylin oxide, monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate and tetra-n-butyl titanate.
9. The composition as claimed in claim 1, wherein said flow and leveling additive is selected from a group consisting of silicon based flow additive 10% solution in O-xylene, a solution of a polyether-modified polydimethylsiloxane, solution of a polyacrylate, polyether-modified polydimethylsiloxane and a low viscosity acrylate polymer.
10. The composition as claimed in claim 1, wherein said fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, and a solvent naphtha (petroleum) light aromatic and mixture thereof .
11. The composition as claimed in claim 1, wherein
said polyester polyol is a product of:
a. at least one polyol;
b. a macrodiol;
c. at least one polyacid;
d. said second catalyst;
e. said fluid medium; and
f. a performance additive, and
said acrylic polyol is a product of:
a. at least one acrylic monomer;
b. a hydroxyl-functional acrylic monomer;
c. said fluid medium and
d. an initiator.
12. The composition as claimed in claim 11, wherein
• said polyol is selected from the group consisting of neopentyl glycol, 2-methyl-1,3-propanediol (MP diol), hexane diol, 1,3 propane diol, 1,2 propane diol, 1,4 butane diol, glycerine, ethylene glycol, diethylene glycol, butyl ethyl propanediol, trimethylolpropane, pentaerythritol, cyclohexane dimethanol and mixture thereof;
• said macrodiol is selected from the group consisting of polycaprolactone polyol, polyester polyol, polyether polyol, polyesterpolyether polyol and polycarbonate polyol;
• said polyacid is selected from the group consisting of adipic acid, terephthalic acid, isophthalic acid, hexahydro phthalic anhydride, cyclohexane dicarboxylic acid and mixture thereof;
• said second catalyst is selected from the group consisting of dibutylin oxide, monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate and tetra-n-butyl titanate;
• said fluid medium is at least one selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, a solvent naphtha (petroleum) light aromatic; and
• said performance additive is selected from the group consisting of triphenyl phosphite, hypophosphorous acid and pentaerythritol tetrakis(3-(3,5-Di-tertiary-butyl-4-hydroxyphenyl) propionate).
13. The composition as claimed in claim 11, wherein
• said acrylic monomer is selected from the group consisting of butyl acrylate, styrene, methyl methacrylate, methacrylic acid, acrylic acid, isobutyl acrylate, isobutyl methacrylate, cyclohexyl methacrylate, stearyl acrylate, stearyl methacrylate, octyl methacrylate, tertiary butyl methacrylate, a synthetic saturated monocarboxylic acid with a highly branched structure containing ten carbon atoms (Vevoa 10 monomer), ethyl hexyl acrylate and mixture thereof;
• said hydroxyl-functional acrylic monomer is selected from the group consisting of 2-hydroxy ethyl acrylate, 2-hydroxy propyl methyl acrylate and 2- hydroxyl ethyl methacrylate;
• said fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, a solvent naphtha (petroleum) light aromatic and mixture thereof; and
• said initiator is selected from the group consisting of tertiary butylperoxybenzoate (TBPB), di-tertiary-butyl peroxide (DTBP) and tert-butylperoxy 2-ethylhexyl carbonate (TBEC).
14. The composition as claimed in claim 11, wherein
• said polyol is present in an amount in the range of 30 mass% to 60 mass%;
• said macrodiol is present in an amount in the range of 1 mass% to 20 mass%;
• said polyacid is present in an amount in the range of 35 mass% to 60 mass%;
• said second catalyst is present in an amount in the range of 0.01 mass% to 2 mass%;
• said fluid medium is present in an amount in the range of 1 mass% to 30 mass%; and
• said performance additive is present in an amount in the range of 0.1 mass% to 1 mass%,
wherein said mass% of each ingredient is with respect to the total mass of said polyester polyol.
15. The composition as claimed in claim 13, wherein said fluid medium is present in an amount in the range of 2 mass% to 10 mass% with respect to the total mass of said polyester polyol.
16. The composition as claimed in claim 11, wherein
• said acrylic monomer is present in an amount in the range of 65 mass% to 85 mass%;
• said hydroxyl-functional acrylic monomer is present in an amount in the range of 10 mass% to 25 mass%;
• said fluid medium is present in an amount in the range of 15 mass% to 35 mass%; and
• said initiator is present in an amount in the range of 2 mass% to 10 mass%,
wherein said mass% of each ingredient is with respect to the total mass of said acrylic polyol.
17. A process for the preparation of a coating composition, wherein said process comprises the following steps:
(i) mixing predetermined amounts of a polyester polyol and optionally an acrylic polyol in a container under stirring at a speed in the range of 100 rpm to 1000 rpm for a time period in the range of 10 minutes to 30 minutes to obtain a first mixture;
(ii) adding predetermined amounts of a fluid medium and a first catalyst to said first mixture under stirring for a time period in the range of 10 minutes to 30 minutes to obtain a homogenized mixture;
(iii) adding a predetermined amount of a flow and leveling additive to said homogenized mixture under stirring at a speed in the range of 50 rpm to 100 rpm for a time period in the range of 10 minutes to 20 minutes to obtain a hydroxy functional polymer component; and
(iv) mixing a predetermined amount of an isocyanate component to said hydroxy functional polymer component at a room temperature for a time period in the range of 5 minutes to 15 minutes at a room temperature to obtain said coating composition,
wherein a ratio of OH equivalent weight of said hydroxy functional polymer component to NCO equivalent weight of said isocyanate component is in the range of 1:0.5 to 1:2.
18. The process as claimed in claim 17, wherein said polyester polyol is prepared by following steps:
(i) mixing with predetermined amounts of at least one polyol, a macrodiol, at least one polyacid, a second catalyst, a performance additive and said fluid medium in a reactor to obtain a second mixture;
(ii) polymerizing said second mixture under nitrogen at a temperature in the range of 180 ºC to 240 ºC to obtain a polymerized mixture; and
(iii) cooling said polymerized mixture to a temperature in the range of 100 ºC to 150 ºC, followed by adding said first fluid medium and further cooling to a temperature in the range of 30 oC to 40 oC to obtain said polyester polyol.
19. The process as claimed in claim 17, wherein said acrylic polyol is prepared by following steps:
(i) heating a predetermined amount of a fluid medium in a reactor to a temperature in the range of 100 ºC to 150 ºC under nitrogen and maintaining said temperature to obtain a heated fluid medium;
(ii) mixing predetermined amounts of at least one acrylic monomer, a hydroxyl-functional acrylic monomer and an initiator to obtain a third mixture; and
(iii) adding dropwise said third mixture to said heated fluid medium over a time period in the range of 2 hours to 6 hours, followed by stirring for a time period in the range of 30 minutes to 120 minutes to obtain said acrylic polyol.
20. The process as claimed in claim 17, wherein
• said polyester polyol is present in an amount in the range of 5 mass% to 100 mass%; and
• said acrylic polyol is present in an amount in the range of 0 mass% to 95 mass%,
wherein said mass% of each ingredient is with respect to the total mass of said hydroxy functional polymer component.
21. The process as claimed in claim 17, wherein
• said polyester polyol is present in an amount in the range of 2 mass% to 50 mass%;
• said acrylic polyol is present in an amount in the range of 20 mass% to 50 mass%;
• said fluid medium is present in an amount in the range of 1 mass% to 30 mass%;
• said first catalyst is present in an amount in the range of 0.01 mass% to 1 mass%;
• said flow and leveling additive is present in an amount in the range of 0.1 mass% to 3 mass%; and
• said isocyanate component is present in an amount in the range of 30 mass% to 70 mass%,
wherein said mass% of each ingredient is with respect to the total mass of said coating composition.
22. The process as claimed in claim 17, wherein
• said fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, a solvent naphtha (petroleum) light aromatic and mixture thereof;
• said first catalyst is selected from the group consisting of monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate and tetra-n-butyl titanate;
• said flow and leveling additive is selected from a group consisting of silicon based flow additive 10% solution in O-xylene, solution of a polyether-modified polydimethylsiloxane, solution of a polyacrylate, polyether-modified polydimethylsiloxane and low viscosity acrylate polymer; and
• said isocyanate component is selected froman aliphatic polyisocyanate and aromatic polyisocyanate, wherein said aliphatic polyisocyanate is selected from a dimer and trimer of isophorone diisocyanate and dimer of hexamethylene diisocyanate (HDI) and trimer of hexamethylene diisocyanate (HDI); and said aromatic polyisocyanate is selected from toluene diisocyanate based aromatic polyisocyanate and diphenylmethane diisocyanate based aromatic polyisocyanate.
23. The process as claimed in claim 18, wherein
• said polyol is present in an amount in the range of 30 mass% to 60 mass%;
• said macrodiol is present in an amount in the range of 1 mass% to 20 mass%;
• said polyacid is present in an amount in the range of 35 mass% to 60 mass%;
• said second catalyst is present in an amount in the range of 0.01 mass% to 2 mass%;
• said fluid medium is present in an amount in the range of 1 mass% to 30 mass%; and
• said performance additive is present in an amount in the range of 0.1 mass% to 1 mass%,
wherein said mass% of each ingredient is with respect to the total mass of said polyester polyol.
24. The process as claimed in claim 18, wherein
• said polyol is selected from the group consisting of neopentyl glycol, 2-methyl-1,3-propanediol (MP diol), hexane diol, 1,3 propane diol, 1,2 propane diol, 1,4 butane diol, glycerine, ethylene glycol, diethylene glycol, butyl ethyl propanediol, trimethylolpropane, pentaerythritol, cyclohexane dimethanol and mixture thereof;
• said macrodiol is selected from the group consisting of polycaprolactone polyol, polyester polyol, polyether polyol, polyesterpolyether polyol and polycarbonate polyol;
• said polyacid is selected from the group consisting of adipic acid, terephthalic acid, isophthalic acid, hexahydro phthalic anhydride, cyclohexane dicarboxylic acid and mixture thereof;
• said second catalyst is selected from the group consisting of dibutylin oxide, monobutyl tin oxide, dibutyl tin dilaurate, dimethyl tin dilaurate, dioctyl tin dilaurate and tetra-n-butyl titanate;
• said performance additive is selected from the group consisting of triphenyl phosphite, hypophosphorous acid and pentaerythritol tetrakis(3-(3,5-Di-tertiary-butyl-4-hydroxyphenyl) propionate); and
• said fluid medium is selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, a solvent naphtha (petroleum) light aromatic and mixture thereof.
25. The process as claimed in claim 19, wherein
• said acrylic monomer is present in an amount in the range of 65 mass% to 85 mass%;
• said hydroxyl-functional acrylic monomer is present in an amount in the range of 10 mass% to 25 mass%;
• said fluid medium is present in an amount in the range of 15 mass% to 35 mass%; and
• said initiator is present in an amount in the range of 2 mass% to 10 mass%,
wherein said mass% of each ingredient is with respect to the total mass of said acrylic polyol.
26. The process as claimed in claim 19, wherein
• said fluid medium is at least one selected from the group consisting of ortho-xylene, butyl acetate, methoxy propyl acetate, a solvent naphtha (petroleum) light aromatic;
• said acrylic monomer is selected from the group consisting of butyl acrylate, styrene, methyl methacrylate, methacrylic acid, acrylic acid, isobutyl acrylate, isobutyl methacrylate, cyclohexyl methacrylate, stearyl acrylate, stearyl methacrylate, octyl methacrylate, tertiary butyl methacrylate, a synthetic saturated monocarboxylic acid with a highly branched structure containing ten carbon atoms (Vevoa 10 monomer) , ethyl hexyl acrylate and mixture thereof;
• said hydroxyl-functional acrylic monomer is selected from the group consisting of 2-hydroxy ethyl acrylate, 2-hydroxy propyl methyl acrylate and 2-hydroxyl ethyl methacrylate; and
• said initiator is selected from the group consisting of tertiary Butylperoxybenzoate (TBPB), Di-tertiary-butyl peroxide (DTBP) and tert-Butylperoxy 2-ethylhexyl carbonate (TBEC).
27. The process as claimed in claim 17 and claim 18, wherein
• said polyester polyol is characterized by having
? an acid value in the range of 0.1 mg KOH/g to 10 mg KOH/g; and
? an OH value in the range of 80 mg KOH/g to 140 mg KOH/g.
28. The process as claimed in claim 19, wherein said acrylic polyol is characterized by having
• an OH value in the range of 80 mg KOH/g to 140 mg KOH/g.

Dated this 22nd day of March, 2024

_______________________________
MOHAN RAJKUMAR DEWAN, IN/PA – 25
OF R. K. DEWAN & CO.
AUTHORIZED AGENT OF APPLICANT

TO,
THE CONTROLLER OF PATENTS
THE PATENT OFFICE, AT MUMBAI