DESC:FIELD
The present disclosure relates to a binder, a process for the preparation of a binder and a coating composition made therefrom. Particularly, the present disclosure relates to a single-component Polyaspartic polyurethane urea binder.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
Conventionally, 2K Polyaspartic coating composition having an aliphatic polyaspartic based binder is formed by an aspartic acid ester compound having an amino group and an aliphatic and/or alicyclic polyisocyanate composition having an isocyanate group. The aliphatic polyaspartic binder containing coating composition is conventionally used in a wide range of applications such as various coating material, flooring material, waterproofing material, and the like. Although the prior art uses aspartate esters in the manufacturing of coatings, a further improvement in the properties with respect to flexibility, adhesion, durability, combined with balanced cure speed remains a challenge.
Further, a two component polyaspartic urea based coating composition is conventionally known and used. However, the two component polyaspartic urea based coating composition has a relatively shorter pot life for application due to the fast reactivity of polyaspartic amines with isocyanates. Furthermore, the two component polyaspartic urea based coating composition cannot be applied directly on damp surfaces (having moisture content > 10%).
Therefore, there is felt a need for a 1K moisture curable Polyaspartic polyurethane urea binder and a coating composition made therefrom that mitigates the drawbacks mentioned hereinabove or at least provides a useful alternative.
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 binder.
Another object of the present disclosure is to provide a Polyaspartic polyurethane urea binder.
Still another object of the present disclosure is to provide a Polyaspartic polyurethane urea binder based on a polyaspartic ester amino polyol.
Yet another object of the present disclosure is to provide a single-component Polyaspartic polyurethane urea binder that is moisture curable.
Still another object of the present disclosure is to provide a binder that can be applied directly on damp substrates/surfaces (having moisture contents of >10% to 70%).
Yet another object of the present disclosure is to provide a binder that has comparatively high solid content (80% to 95%).
Still another object of the present disclosure is to provide a process for the preparation of a binder.
Yet another object of the present disclosure is to provide a simple, efficient and eco-friendly process for the preparation of a Polyaspartic polyurethane urea binder.
Still another object of the present disclosure is to provide a process for the preparation of a Polyaspartic polyurethane urea binder that is feasible on a large/commercial scale.
Yet another object of the present disclosure is to provide a coating composition comprising a Polyaspartic polyurethane urea binder.
Still another object of the present disclosure is to provide a coating composition that has a longer pot life.
Yet another object of the present disclosure is to provide a process for the preparation of a coating composition that is simple and efficient.
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 Polyaspartic polyurethane urea binder being a product of a polyaspartic ester amino polyol and an isocyanate compound, wherein the polyaspartic ester amino polyol is a reaction product of a maleated polyol and at least one amine.
The binder comprises a first catalyst, a first fluid medium and optionally a chain extender.
A molar ratio of the polyaspartic ester amino polyol to the isocyanate compound is in the range of 1:1.1 to 1:3.
The polyaspartic ester amino polyol is characterized by having an amine value in the range of 1 mg/KOH to 15 mg/KOH and a hydroxyl value in the range of 1 mg/KOH to 26 mg/KOH.
The maleated polyol being a product of a polyol, a second catalyst, maleic anhydride, optionally a viscosity modifying agent and optionally a second fluid medium.
The maleated polyol is characterized by having an acid value in the range of 1 mg/KOH to 5 mg/KOH; a viscosity in the range of 900 centipoise to 15000 centipoise.
The polyol is selected from the group consisting of polypropylene glycol, polycaprolactone polyol, a linear aliphatic polycarbonate polyester polyol and poly tetrahydrofuran polyol.
The second catalyst is dibutyl tin oxide.
The second fluid medium is selected from the group consisting of ortho xylene, meta xylene, para xylene and Solvent C IX.
The viscosity modifying agent is selected from the group consisting of butanol, pentanol, hexanol, heptanol, isooctanol, neooctanol and decanol.
The amine is selected from the group consisting of polyetheramine, 4,4 diamino dicyclohexyl methane, isophorone diamine and 3-aminopropyl trimethoxysilane.
The isocyanate compound is selected from the group consisting of isophorone diisocyanate, methylene diphenyl diisocyanate, hydrogenated methylenedicyclohexyl diisocyanate and toluene diisocyanate.
The first catalyst is dibutyl tin dilaurate.
The first fluid medium is selected from the group consisting of methoxy propyl acetate, solvent C IX and butyl acetate.
The chain extender is selected from the group consisting of diethylene glycol, 2-Methyl-1,3-propanediol, and butanediol.
The maleated polyol is a Maleic anhydride (MA) modified polyol (poly ether/poly ester polyol).
The Polyaspartic polyurethane urea binder is characterized by having:
• a free NCO content in the range of 2% to 6%;
• a solid content in the range of 80% to 95%; and
• a viscosity in the range of 900 centipoise to 15000 centipoise.
The binder comprises a polyol selected from the group consisting of polypropylene glycol, polycaprolactone polyol, a linear aliphatic polycarbonate polyester polyol and poly tetrahydrofuran polyol.
Further, the present disclosure relates to a process for the preparation of a Polyaspartic polyurethane urea binder. The process comprises the step of mixing predetermined amounts of a polyol, maleic anhydride, a second catalyst, optionally viscosity modifying agent and optionally a second fluid medium at a temperature in the range of 160 ºC to 240 ºC to obtain a maleated polyol. The maleated polyol is cooled to a temperature in the range of 40 ºC to 100 ºC followed by adding a predetermined amount of an amine at a temperature in the range of 40 ºC to 100 ºC for a time period in the range of 5 hours to 20 hours to obtain a polyaspartic ester amino polyol. The polyaspartic ester amino polyol is mixed with predetermined amounts of an isocyanate compound, a first fluid medium, a first catalyst, optionally a chain extender and the polyol in the presence of nitrogen at a temperature in the range of 40 ºC to 100 ºC to obtain the Polyaspartic polyurethane urea binder.
A molar ratio of the polyaspartic ester amino polyol to the isocyanate compound is in the range of 1:1.1 to 1:3.
The predetermined amount of the polyol is in the range of 80 mass% to 99.5 mass% with respect to the total mass of the maleated polyol. The predetermined amount of maleic anhydride is in the range of 0.1 mass% to 3 mass% with respect to the total mass of the maleated polyol. The predetermined amount of the isocyanate is in the range of 5 mass% to 15 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. The predetermined amount of the first catalyst is in the range of 0.01 mass% to 0.2 mass% with respect to the total mass of the maleated polyol. The predetermined amount of the viscosity modifying agent is in the range of 0 mass% to 5 mass% with respect to the total mass of the maleated polyol. The predetermined amount of the first fluid medium is in the range of 0 mass% to 15 mass% with respect to the total mass of the maleated polyol. The predetermined amount of the amine is in the range of 0.1 mass% to 15 mass% with respect to the total mass of the polyaspartic ester amino polyol. The predetermined amount of the second catalyst is in the range of 0.005 mass% to 0.1 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. The predetermined amount of the second fluid medium is in the range of 5 mass% to 20 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. The predetermined amount of the chain extender is in the range of 0 mass% to 20 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder.
The polyol is selected from the group consisting of polypropylene glycol, polycaprolactone polyol, a linear aliphatic polycarbonate polyester polyol and poly tetrahydrofuran polyol.
The amine is selected from the group consisting of polyetheramine, 4, 4 diamino dicyclohexyl methane, isophorone diamine and 3-aminopropyl trimethoxysilane.
The isocyanate compound is selected from the group consisting of isophorone diisocyanate, methylene diphenyl diisocyanate, hydrogenated methylenedicyclohexyl diisocyanate and toluene diisocyanate.
The viscosity modifying agent is selected from the group consisting of butanol, pentanol, hexanol, heptanol, isooctanol, neooctanol and decanol.
The first catalyst dibutyl tin dilaurate.
The second catalyst is dibutyl tin oxide.
The first fluid medium is selected from the group consisting of methoxy propyl acetate, solvent C IX and butyl acetate.
The second fluid medium is selected from the group consisting of ortho xylene, meta xylene, para xylene and solvent C IX.
The chain extender is selected from the group consisting of diethylene glycol, 2-Methyl-1,3-propanediol, and butanediol.
The maleated polyol is a Maleic anhydride (MA) modified polyol (poly ether/poly ester polyol).
Furthermore, the present disclosure relates to a coating composition. The coating composition comprises a Polyaspartic polyurethane urea binder, at least one filler, a defoamer, at least one thixotropy additive, a dispersing agent, a third catalyst, a moisture scavenger, a third fluid medium, optionally a pigment and optionally a plasticizer.
The coating composition comprises 10 mass% to 55 mass% of the Polyaspartic polyurethane urea binder, 5 mass% to 50 mass% of the filler, 0.05 mass% to 2 mass% of the defoamer, 0.01 mass% to 5 mass% of the thixotropy additive, 0.05 mass% to 5 mass% of the dispersing agent, 0.01 mass% to 3 mass% of the third catalyst, 0.05 mass% to 6 mass% of the moisture scavenger, 5 mass% to 35 mass% of the third fluid medium, 0 mass% to 35 mass% of the plasticizer and 0 mass% to 20 mass% of the pigment wherein the mass% of each ingredient is with respect to the total mass of the coating composition.
The plasticizer is selected from the group consisting of phthalate plasticizers and non-phthalate plasticizers, wherein the phthalate plasticizer is diisononyl phthalate and the non-phthalate plasticizer is selected from the group consisting of alkylsulfonic acid ester with phenol (ASE) and di(isononyl) cyclohexane-1,2-dicarboxylate.
The filler is selected from the group consisting of barium sulfate, calcium carbonate and magnesium silicate.
The defoamer is selected from the group consisting of silicone-free defoamer, defoamers based on polysiloxanes and defoamers based on polymethylalkylsiloxane.
The thixotropy additive is selected from the group consisting of fumed silica after-treated with dimethyldichlorosilane, organically modified phyllosilicates, bentonite clay and polyamide.
The dispersing agent is selected from the group consisting of alkylammonium salt of copolymers, soya lecithin-A complex (mixture of phospholipids, glycolipids, triglycerides, phosphatidylcholines, phosphatidylethanolamines and phosphatidylinositols), salt of unsaturated polyamine amides and acid polyesters, solution of modified polyurethane and solution of polymeric phosphoric acid ester.
The pigment is titanium dioxide.
The third catalyst is selected from dibutyltin dilaurate and dimorpholinodiethyl ether.
The moisture scavenger is selected from the group consisting of molecular sieve, monofunctional isocyanate (additive Ti) and ethyl orthoformate (additive OF).
The third fluid medium is selected from the group consisting of solvent C IX, butyl acetate, xylene and methoxy propyl acetate.
Still further, the present disclosure relates to a process for the preparation of the coating composition. The process comprises a step of mixing of predetermined amounts of a dispersing agent and optionally a plasticizer in a reactor at a temperature in the range of 20 oC to 40 oC for a time period in the range of 10 minutes to 40 minutes under at a stirring speed in the range of 400 rpm to 600 rpm to obtain a first mixture. Predetermined amounts of a filler, optionally a pigment and a moisture scavenger are mixed in the first mixture at a temperature in the range of 20 oC to 40 oC for a time period in the range of 20 minutes to 70 minutes at a stirring speed in the range of 600 rpm to 1200 rpm to obtain a second mixture. Predetermined amounts of a Polyaspartic polyurethane urea binder, a third catalyst, a defoamer, a thixotropy additive and a third fluid medium is mixed to the second mixture at a temperature in the range of 20 oC to 40 oC for a time period in the range of 10 minutes to 50 minutes at a stirring speed in the range of 600 rpm to 1200 rpm to obtain the coating composition.
The plasticizer is selected from the group consisting of phthalate plasticizers and non-phthalate plasticizers, wherein the phthalate plasticizer is diisononyl phthalate and the non-phthalate plasticizer is selected from the group consisting of alkylsulfonic acid ester with phenol (ASE) and di(isononyl) cyclohexane-1,2-dicarboxylate.
The filler is selected from the group consisting of barium sulfate, calcium carbonate and magnesium silicate.
The defoamer is selected from the group consisting of silicone-free defoamer, defoamers based on polysiloxanes and defoamers based on polymethylalkylsiloxane.
The thixotropy additive is selected from the group consisting of fumed silica after-treated with dimethyldichlorosilane, organically modified phyllosilicates, bentonite clay and polyamide.
The dispersing agent is selected from the group consisting of alkylammonium salt of copolymers, soya lecithin-A complex (mixture of phospholipids, glycolipids, triglycerides, phosphatidylcholines, phosphatidylethanolamines and phosphatidylinositols) salt of unsaturated polyamine amides and acid polyesters, solution of modified polyurethane and solution of polymeric phosphoric acid ester.
The pigment is titanium dioxide.
The third catalyst is selected from dibutyltin dilaurate and dimorpholinodiethyl ether.
The moisture scavenger is selected from the group consisting of the moisture scavenger is selected from the group consisting of molecular sieve, monofunctional isocyanate (additive Ti) and ethyl orthoformate (additive OF).
The third fluid medium is selected from the group consisting of solvent C IX, butyl acetate, xylene and methoxy propyl acetate.
The predetermined amount of the Polyaspartic polyurethane urea binder is in the range of 10 mass% to 55 mass%, the predetermined amounts of the plasticizer is in the range of 0 mass% to 35 mass%, the predetermined amount of the filler is in the range of 5 mass% to 50 mass%, the predetermined amount of the defoamer is in the range of 0.05 mass% to 2 mass%, the predetermined amount of the thixotropy additive is in the range of 0.01 mass% to 5 mass%, the predetermined amount of the dispersing agent is in the range of 0.05 mass% to 5 mass%, the predetermined amount of the third catalyst is in the range of 0.01 mass% to 3 mass%, the predetermined amount of the moisture scavenger is in the range of 0.05 mass% to 6 mass%, the predetermined amount of the third fluid medium is in the range of 5 mass% to 35 mass% and the predetermined amount of the pigment is in the range of 0 mass% to 20 mass%, wherein the mass% of each ingredient is with respect to the total mass of the coating composition.
The coating composition is characterized by having a pot life in the range of 8 hours to 24 hours.
DETAILED DESCRIPTION
The present disclosure relates to a binder, a process for the preparation of a binder and a coating composition made therefrom. Particularly, the present disclosure relates to a single-component Polyaspartic polyurethane urea binder.
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.
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.
Conventionally, 2K polyaspartic coating composition having an aliphatic polyaspartic based binder is formed by an aspartic acid ester compound having an amino group and an aliphatic and/or alicyclic polyisocyanate composition having an isocyanate group. The aliphatic polyaspartic binder containing coating composition is conventionally used in a wide range of applications such as various coating materials, flooring materials, waterproofing material, and the like. Although the prior art uses aspartate esters in the manufacturing of coatings, a further improvement in properties with respect to flexibility, adhesion, and durability, combined with balanced cure speed remains a challenge.
Further, a two component polyaspartic urea based coating composition is conventionally known and used. However, the two component polyaspartic urea based coating composition has a relatively shorter pot life for application due to the fast reactivity of polyaspartic amines with isocyanates. Furthermore, the two component polyaspartic urea based coating composition cannot be applied directly on damp surfaces (having moisture content > 10%).
The present disclosure provides a binder, a process for the preparation of a binder and a coating composition made therefrom. Particularly, the present disclosure provides a single-component Polyaspartic polyurethane urea binder.
In a first aspect, the present disclosure provides a Polyaspartic polyurethane urea binder being a product of a polyaspartic ester amino polyol and an isocyanate compound, wherein the polyaspartic ester amino polyol is a reaction product of a maleated polyol and at least one amine.
In an embodiment of the present disclosure, the polyaspartic ester amino polyol is present in an amount in the range of 10 mass% to 85 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder.
In an embodiment of the present disclosure, the isocyanate compound is selected from the group consisting of isophorone diisocyanate, methylene diphenyl diisocyanate, hydrogenated methylenedicyclohexyl diisocyanate and toluene diisocyanate. In an exemplary embodiment of the present disclosure, the isocyanate compound is toluene diisocyanate (TDI) and methylene diphenyl diisocyante (PMDI). In another exemplary embodiment of the present disclosure, the isocyanate compound is methylene diphenyl diisocyanate (MDI). In still another exemplary embodiment of the present disclosure, the isocyanate compound is hydrogenated methylene diphenyl diisocyanate (H12MDI). In yet another exemplary embodiment of the present disclosure, the isocyanate compound is isophorone diisocyanate (IPDI).
In an embodiment of the present disclosure, the isocyanate compound is present in an amount in the range of 5 mass% to 15 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder.
In an embodiment of the present disclosure, the binder comprises a first catalyst, a first fluid medium, optionally a chain extender.
In an embodiment of the present disclosure, the binder comprises a polyol selected from the group consisting of PPG 4000, polycaprolactone (CAPA-2201A), a linear aliphatic polycarbonate polyester polyol (desmophen C1200) and polytetrahydrofuran polyol.
In an embodiment of the present disclosure, the first catalyst is dibutyl tin dilaurate.
In an embodiment of the present disclosure, the first catalyst is present in an amount in the range of 0.005 mass% to 0.1 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder.
In an embodiment of the present disclosure, the first fluid medium is selected from the group consisting of methoxy propyl acetate, solvent C IX and butyl acetate. In an exemplary embodiment of the present disclosure, the first fluid medium is methoxy propyl acetate. In another exemplary embodiment of the present disclosure, the first fluid medium is butyl acetate. In still another exemplary embodiment of the present disclosure, the first fluid medium is solvent C IX.
Solvent C IX refers to an aromatic hydrocarbon solvent. It is a petroleum naphtha refinery stream, also known as "Solvent naphtha, (petroleum), light aromatic" or “C9 solvent”.
In an embodiment of the present disclosure, the first fluid medium is a combination of solvent C IX and butyl acetate. In another embodiment of the present disclosure, the first fluid medium is a combination of methoxy propyl acetate and solvent C IX.
In an embodiment of the present disclosure, the first fluid medium is present in an amount in the range of 5 mass% to 20 mass% with respect to the total amount of the Polyaspartic polyurethane urea binder.
In an embodiment of the present disclosure, the chain extender is selected from the group consisting of diethylene glycol, 2-Methyl-1,3-propanediol, and butanediol. In an exemplary embodiment of the present disclosure, the chain extender is diethylene glycol.
In an embodiment of the present disclosure, the chain extender is present in an amount in the range of 0 mass% to 5 mass% with respect to the total amount of the Polyaspartic polyurethane urea binder.
In an embodiment of the present disclosure, the molar ratio of the polyaspartic ester amino polyol to the isocyanate compound is in the range of 1:1.1 to 1:3.
In an embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is moisture-curable and has a free isocyanate content (NCO) in the range of 2% to 6%.
In an embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is one component binder; is moisture curable; has a high-solid content in the range of 80% to 95%and is directly applicable on a damp surface having a moisture content up to 70% by self-priming application.
The polyaspartic ester amino polyol is characterized by having an amine value in the range of 1 mg/KOH to 15 mg/KOH and a hydroxyl value in the range of 1 mg/KOH to 26 mg/KOH.
In an embodiment of the present disclosure, the polyaspartic ester amino polyol being a reaction product of a maleated polyol and at least one amine.
In an embodiment of the present disclosure, the amine is selected from the group consisting of polyetheramines (Jeffamine D2000), 4,4 diamino dicyclohexyl methane, isophorone diamine and 3-aminopropyl trimethoxysilane. In an exemplary embodiment of the present disclosure, the amine is polyetheramines (Jeffamine D2000). In another exemplary embodiment of the present disclosure, the amine is 4,4 diamino dicyclohexyl methane (PACM). In still another exemplary embodiment of the present disclosure, the amine is isophorone diamine (IPDA). In yet another exemplary embodiment of the present disclosure, the amine is 3-aminopropyl trimethoxysilane.
In an embodiment of the present disclosure, the amine is present in an amount in the range of 0.1 mass% to 15 mass% with respect to the total mass of the polyaspartic ester amino polyol.
In accordance with the embodiment of the present disclosure, the maleated polyol is a product of polyol, a second catalyst, maleic anhydride, optionally a viscosity modifying agent and optionally a second fluid medium.
In an embodiment of the present disclosure, the polyol is selected from the group consisting of polypropylene glycol, polycaprolactone polyol, a linear aliphatic polycarbonate polyester polyol and poly tetrahydrofuran polyol. In an exemplary embodiment of the present disclosure, the polyol is polypropylene glycol (PPG-4000). In another exemplary embodiment of the present disclosure, the glycol is polypropylene glycol (PPG-2000). In another exemplary embodiment of the present disclosure, the glycol is polytetrahydrofuran polyol 2000.
In an embodiment of the present disclosure, the polyol is present in an amount in the range of 80 mass% to 99.5 mass% with respect to the total mass of the maleated polyol.
In an embodiment of the present disclosure, the maleic anhydride is present in an amount in the range of 0.1 mass% to 3 mass% with respect to the total mass of the maleated polyol.
In an embodiment of the present disclosure, the second catalyst is dibutyl tin oxide.
In an embodiment of the present disclosure, the second catalyst is present in an amount in the range of 0.01 mass% to 0.2 mass% with respect to the total mass of the maleated polyol.
In an embodiment of the present disclosure, the viscosity modifying agent is selected from the group consisting of butanol, pentanol, hexanol, heptanol, isooctanol, neooctanol and decanol. In an exemplary embodiment of the present disclosure, the viscosity modifying agent is isooctanol.
Isooctanol is added to adjust the viscosity when polytetrahydrofuran polyol is added as polyol.
In an embodiment of the present disclosure, the viscosity modifying agent is present in an amount in the range of 0 mass% to 5 mass% with respect to the total mass of the maleated polyol.
In an embodiment of the present disclosure, the second fluid medium is selected from the group consisting of ortho xylene, meta xylene, para xylene and solvent C IX. In an exemplary embodiment of the present disclosure, the first fluid medium is orthoxylene.
In an embodiment of the present disclosure, the second fluid medium is present in an amount in the range of 0 mass% to 15 mass% with respect to the total mass of the maleated polyol.
In an embodiment of the present disclosure, the maleated polyol is a Maleic anhydride (MA) modified polyol (poly ether/poly ester polyol).
The maleated polyol is characterized by having an acid value in the range of 1 mg/KOH to 5 mg/KOH and a viscosity in the range of 900 centipoise to 15000 centipoise. In an exemplary embodiment of the present disclosure, the acid value is 3 mg/KOH and the viscosity is 1700 centipoise (Gardener’s scale Y). In another exemplary embodiment of the present disclosure, the acid value is 2 mg/KOH and the viscosity is 1000 centipoise (Gardener’s scale W).
The one-component (1K) Polyaspartic polyurethane urea binder that is moisture-curable, has free NCO content in the range of 2% to 6%, has high-solid content in the range of 80% to 95% and viscosity in the range of 900 centipoise to 15000 centipoise.The binder is directly applicable on a damp surface having a moisture content up to 70% by self-priming application.
In a second aspect, the present disclosure provides a process for the preparation of a Polyaspartic polyurethane urea binder. The process comprises the following steps:
(i) mixing predetermined amounts of a polyol, maleic anhydride, a second catalyst, optionally viscosity modifying agent and optionally a second fluid medium at a temperature in the range of 160 ºC to 240 ºC to obtain a maleated polyol;
(ii) cooling the maleated polyol to a temperature in the range of 40 ºC to 100 ºC followed by adding a predetermined amount of an amine at a temperature in the range of 40 ºC to 100 ºC and maintaining for a time period in the range of 5 hours to 20 hours to obtain a polyaspartic ester amino polyol; and
(iii) mixing the polyaspartic ester amino polyol with a predetermined amount of an isocyanate compound, a first fluid medium, a first catalyst, optionally a chain extender and the polyol in the presence of nitrogen at a temperature in the range of 40 ºC to 100 ºC to obtain the Polyaspartic polyurethane urea binder.
The process is described in detail below.
In the first step, the predetermined amounts of a polyol, maleic anhydride, a second catalyst, optionally viscosity modifying agent and optionally a second fluid medium are mixed at a temperature in the range of 160 ºC to 240 ºC to obtain a maleated polyol.
In an embodiment of the present disclosure, the polyol is selected from the group consisting of polypropylene glycol, polycaprolactone polyol, a linear aliphatic polycarbonate polyester polyol and poly tetrahydrofuran polyol. In an exemplary embodiment of the present disclosure, the polyol is polypropylene glycol (PPG-4000). In another exemplary embodiment of the present disclosure, the glycol is polypropylene glycol (PPG-2000). In another exemplary embodiment of the present disclosure, the glycol is polytetrahydrofuran polyol 2000.
In an embodiment of the present disclosure, the polyol is present in an amount in the range of 80 mass% to 99.5 mass% with respect to the total mass of the maleated polyol. In an exemplary embodiment of the present disclosure, the polyol is present in an amount of 98.9 mass% with respect to the total mass of the maleated polyol. In another exemplary embodiment of the present disclosure, the polyol is present in an amount of 99.4 mass% with respect to the total mass of the maleated polyol. In still another exemplary embodiment of the present disclosure, the polyol is present in an amount of 84.8 mass% with respect to the total mass of the maleated polyol. In yet another exemplary embodiment of the present disclosure, the polyol is present in an amount of 84 mass% with respect to the total mass of the maleated polyol.
In an embodiment of the present disclosure, the maleic anhydride is present in an amount in the range of 0.1 mass% to 3 mass% with respect to the total mass of the maleated polyol. In an exemplary embodiment of the present disclosure, maleic anhydride is present in an amount of 2.06 mass% with respect to the total mass of the maleated polyol. In another exemplary embodiment of the present disclosure, maleic anhydride is present in an amount of 2 mass% with respect to the total mass of the maleated polyol. In still another exemplary embodiment of the present disclosure, maleic anhydride is present in an amount of 1 mass% with respect to the total mass of the maleated polyol. In yet another exemplary embodiment of the present disclosure, maleic anhydride is present in an amount of 1.2 mass% with respect to the total mass of the maleated polyol.
In an embodiment of the present disclosure, the second catalyst is dibutyl tin oxide.
In an embodiment of the present disclosure, the second catalyst is present in an amount in the range of 0.01 mass% to 0.2 mass% with respect to the total mass of the maleated polyol. In an exemplary embodiment of the present disclosure, the amount of the second catalyst is 0.1 mass% with respect to the total mass of the maleated polyol. In another exemplary embodiment of the present disclosure, the amount of the second catalyst is 0.06 mass% with respect to the total mass of the maleated polyol.
In an embodiment of the present disclosure, the viscosity modifying agent is selected from the group consisting of butanol, pentanol, hexanol, heptanol, isooctanol, neooctanol and decanol. In an exemplary embodiment of the present disclosure, the viscosity modifying agent is isooctanol.
Isooctanol is added to adjust the viscosity when polytetrahydrofuran polyol is added as polyol.
In an embodiment of the present disclosure, the viscosity modifying agent is present in an amount in the range of 0 mass% to 5 mass% with respect to the total mass of the maleated polyol. In an exemplary embodiment of the present disclosure, the amount of the viscosity modifying agent is 3 mass% with respect to the total mass of the maleated polyol. In another exemplary embodiment of the present disclosure, the amount of the viscosity modifying agent is 2.5 mass% with respect to the total mass of the maleated polyol.
In an embodiment of the present disclosure, the second fluid medium is selected from the group consisting of ortho xylene, meta xylene, para xylene and solvent C IX. In an exemplary embodiment of the present disclosure, the second fluid medium is orthoxylene.
In an embodiment of the present disclosure, the second fluid medium is present in an amount in the range of 0 mass% to 15 mass% with respect to the total mass of the maleated polyol. In an exemplary embodiment of the present disclosure, the amount of the second fluid medium is 10.58 mass% with respect to the total mass of the maleated polyol. In another exemplary embodiment of the present disclosure, the amount of the second fluid medium is 13.9 mass% with respect to the total mass of the maleated polyol.
In an embodiment of the present disclosure, the maleated polyol is a Maleic anhydride (MA) modified polyol (poly ether/poly ester polyol).
In the second step, the maleated polyol is cooled to a temperature in the range of 40 ºC to 100 ºC followed by adding a predetermined amount of an amine at a temperature in the range of 40 ºC to 100 ºC and maintaining for a time period for a time period in the range of 5 hours to 20 hours to obtain a polyaspartic ester amino polyol.
In an embodiment of the present disclosure, the maleated polyol is a Maleic anhydride (MA) modified polyol (poly ether/poly ester polyol).
In an embodiment of the present disclosure, the amine is selected from the group consisting of polyetheramines (Jeffamine D2000), 4,4 diamino dicyclohexyl methane, isophorone diamine and 3-aminopropyl trimethoxysilane. In an exemplary embodiment of the present disclosure, the amine is polyetheramines (Jeffamine D2000). In another exemplary embodiment of the present disclosure, the amine is 4,4 diamino dicyclohexyl methane (PACM). In still another exemplary embodiment of the present disclosure, the amine is isophorone diamine (IPDA). In yet another exemplary embodiment of the present disclosure, the amine is 3-aminopropyl trimethoxysilane.
In an embodiment of the present disclosure, the amine is present in an amount in the range of 0.1 mass% to 15 mass% with respect to the total mass of the polyaspartic ester amino polyol. In an exemplary embodiment of the present disclosure, the amine is present in an amount of 4.5 mass% with respect to the total mass of the polyaspartic ester amino polyol. In another exemplary embodiment of the present disclosure, the amine is present in an amount of 11 mass% with respect to the total mass of the polyaspartic ester amino polyol. In still another exemplary embodiment of the present disclosure, the amine is present in an amount of 0.2 mass% with respect to the total mass of the polyaspartic ester amino polyol. In yet another exemplary embodiment of the present disclosure, the amine is present in an amount of 0.6 mass% with respect to the total mass of the polyaspartic ester amino polyol.
In an embodiment of the present disclosure, the time period is in the range of 5 hours to 20 hours.
In the third step, the polyaspartic ester amino polyol is mixed with a predetermined amount of an isocyanate compound, a first fluid medium and a first catalyst, optionally a chain extender and the polyol in the presence of nitrogen at a temperature in the range of 40 ºC to 100 ºC to obtain the Polyaspartic polyurethane urea binder.
In an embodiment of the present disclosure, the isocyanate compound is selected from the group consisting of isophorone diisocyanate, methylene diphenyl diisocyanate, hydrogenated methylenedicyclohexyl diisocyanate and toluene diisocyanate. In an exemplary embodiment of the present disclosure, the isocyanate compound is toluene diisocyanate (TDI) and methylene diphenyl diisocyante (PMDI). In another exemplary embodiment of the present disclosure, the isocyanate compound is methylene diphenyl diisocyanate (MDI). In still another exemplary embodiment of the present disclosure, the isocyanate compound is hydrogenated methylene diphenyl diisocyanate (H12MDI). In yet another exemplary embodiment of the present disclosure, the isocyanate compound is isophorone diisocyanate (IPDI).
In an embodiment of the present disclosure, the isocyanate compound is present in an amount in the range of 5 mass% to 15 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. In an exemplary embodiment of the present disclosure, the isocyanate compound is present in amount of 12 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. In another exemplary embodiment of the present disclosure, the isocyanate compound is present in amount of 10 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. In still another exemplary embodiment of the present disclosure, the isocyanate compound is present in amount of 13.91 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. In yet another exemplary embodiment of the present disclosure, the isocyanate compound is present in amount of 11.19 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder.
In an embodiment of the present disclosure, the first catalyst is dibutyl tin dilaurate.
In an embodiment of the present disclosure, the first catalyst is present in an amount in the range of 0.005 mass% to 0.1 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. In an exemplary embodiment of the present disclosure, the first catalyst is present in an amount of 0.01 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder.
In an embodiment of the present disclosure, the first fluid medium is selected from the group consisting of methoxy propyl acetate, solvent C IX and butyl acetate. In an exemplary embodiment of the present disclosure, the first fluid medium is methoxy propyl acetate. In another exemplary embodiment of the present disclosure, the first fluid medium is butyl acetate. In still another exemplary embodiment of the present disclosure, the first fluid medium is solvent C IX.
In an embodiment of the present disclosure, the first fluid medium is a combination of solvent C IX and butyl acetate. In another embodiment of the present disclosure, the first fluid medium is a combination of methoxy propyl acetate and solvent C IX.
In an embodiment of the present disclosure, the first fluid medium is present in an amount in the range of 5 mass% to 20 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. In an exemplary embodiment of the present disclosure, the first fluid medium is present in an amount of 10 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. In another exemplary embodiment of the present disclosure, the first fluid medium is present in an amount of 13.04 mass% with respect to the total mass of the Polyaspartic polyurethane -urea binder. In still another exemplary embodiment of the present disclosure, the first fluid medium is present in an amount of 13.63 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder.
In an embodiment of the present disclosure, the chain extender is selected from the group consisting of diethylene glycol, 2-Methyl-1,3-propanediol, and butanediol. In an exemplary embodiment of the present disclosure, the chain extender is diethylene glycol.
In an embodiment of the present disclosure, the chain extender is present in an amount in the range of 0 mass% to 5 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. In an exemplary embodiment of the present disclosure, the chain extender is present in an amount of 3 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder. In another exemplary embodiment of the present disclosure, the chain extender is present in an amount of 0.86 mass% with respect to the total mass of the Polyaspartic polyurethane urea binder.
In an embodiment of the present disclosure, the molar ratio of the polyaspartic ester amino polyol to the isocyanate compound is in the range of 1:1.1 to 1:3.
In an embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is moisture-curable and has a free isocyanate content (NCO) in the range of 2% to 6%.
In a third aspect, the present disclosure provides a coating composition. The coating composition comprises the following:
a. a Polyaspartic polyurethane urea binder;
b. at least one filler;
c. a defoamer;
d. at least one thixotropy additive;
e. a dispersing agent;
f. a third catalyst;
g. a moisture scavenger;
h. a third fluid medium;
i. optionally a pigment; and
j. optionally a plasticizer.
In accordance with the embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is present in the amount in the range of 10 mass% to 55 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is present in the amount of 20 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is present in the amount of 40 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is present in the amount of 50 mass% with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is present in the amount of 35 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the filler is selected from the group consisting of barium sulfate, calcium carbonate and magnesium silicate. In an exemplary embodiment of the present disclosure, the filler is barium sulfate. In another exemplary embodiment of the present disclosure, the filler is calcium carbonate. In still another exemplary embodiment of the present disclosure, the filler is magnesium silicate. In yet another exemplary embodiment of the present disclosure, the filler is a mixture of magnesium silicate, barium sulfate and calcium carbonate.
In an embodiment of the present disclosure, the filler is present in an amount in the range of 5 mass% to 50 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the filler is present in amount of 30 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the filler is present in amount of 39 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the filler is present in amount of 25 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the defoamer is selected from the group consisting of silicone-free defoamer (BYK057), defoamers based on polysiloxanes (BYK1760/BYK530) and defoamers based on polymethylalkylsiloxane (BYK085). In an exemplary embodiment of the present disclosure, the defoamer is based on polysiloxanes (BYK1760/BYK530). In another exemplary embodiment of the present disclosure, the defoamer is based on polymethylalkylsiloxane (BYK085). In still another exemplary embodiment of the present disclosure, the defoamer is silicone-free defoamer (BYK057).
In an embodiment of the present disclosure, the defoamer is present in an amount in the range of 0.05 mass% to 2 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the defoamer is present in an amount of 0.1 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the defoamer is present in an amount of 0.2 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the defoamer is present in an amount of 0.05 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the thixotropy additive is selected from the group consisting of fumed silica after-treated with dimethyldichlorosilane (Aerosil R972), organically modified phyllosilicates (Garamite 1958), bentonite clay and polyamide (Cravallac Ultra). In an exemplary embodiment of the present disclosure, the thixotropy additive is fumed silica after-treated with dimethyldichlorosilane (Aerosil R972). In another exemplary embodiment of the present disclosure, the thixotropy additive is organically modified phyllosilicates (Garamite 1958). In still another exemplary embodiment of the present disclosure, the thixotropy additive is bentonite clay. In yet another exemplary embodiment of the present disclosure, the thixotropy additive is polyamide (Cravallac Ultra). In still another exemplary embodiment of the present disclosure, the thixotropy additive is Aerosil R972 and Cravallac Ultra.
In an embodiment of the present disclosure, the thixotropy additive is present in an amount in the range of 0.01 mass% to 5 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the thixotropy additive is present in an amount of 2 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the thixotropy additive is present in an amount of 0.5 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the thixotropy additive is present in an amount of 1.55 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the dispersing agent is selected from the group consisting of alkylammonium salt of copolymers (BYK 9076), soya lecithin-A complex (mixture of phospholipids, glycolipids, triglycerides, phosphatidylcholines, phosphatidylethanolamines and phosphatidylinositols), a salt of unsaturated polyamine amides and acid polyesters (Antiterra U), solution of modified polyurethane (DBYK 163) and solution of polymeric phosphoric acid ester (BYK 110). In an exemplary embodiment of the present disclosure, the dispersing agent is soya lecithin-A complex (mixture of phospholipids, glycolipids, triglycerides, phosphatidylcholines, phosphatidylethanolamines and phosphatidylinositols). In another exemplary embodiment of the present disclosure, the dispersing agent is solution of a salt of unsaturated polyamine amides and acid polyesters (Antiterra U). In still another exemplary embodiment of the present disclosure, the dispersing agent is solution of polymeric phosphoric acid ester (BYK 110).
In an embodiment of the present disclosure, the dispersing agent is present in an amount in the range of 0.05 mass% to 5 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the dispersing agent is present in an amount of 0.05 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the dispersing agent is present in an amount of 1.85 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the dispersing agent is present in an amount of 0.1 mass% with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the dispersing agent is present in an amount of 0.25 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the third catalyst is dibutyltin dilaurate and dimorpholinodiethyl ether. In an exemplary embodiment of the present disclosure, the third catalyst is dibutyltin dilaurate. In another exemplary embodiment of the present disclosure, the third catalyst is dimorpholinodiethyl ether.
In an embodiment of the present disclosure, the third catalyst is present in an amount in the range of 0.01 mass% to 3 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the third catalyst is present in an amount of 0.1 with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the third catalyst is present in an amount of 1.3 with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the third catalyst is present in an amount of 2 with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the third catalyst is present in an amount of 1 with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the moisture scavenger is selected from the group consisting of molecular sieve, monofunctional isocyanate (additive Ti) and ethyl orthoformate (additive OF). In an exemplary embodiment of the present disclosure, the moisture scavenger is molecular sieve. In another exemplary embodiment of the present disclosure, the moisture scavenger is additive Ti.
In an embodiment of the present disclosure, the moisture scavenger is present in an amount in the range of 0.05 mass% to 6 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the moisture scavenger is present in an amount of 4.8 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the moisture scavenger is present in an amount of 3 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the moisture scavenger is present in an amount of 1 mass% with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the moisture scavenger is present in an amount of 0.05 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the third fluid medium is selected from the group consisting of solvent C IX, butyl acetate, xylene and methoxy propyl acetate. In an exemplary embodiment of the present disclosure, the third fluid medium is solvent C IX. In another exemplary embodiment of the present disclosure, the third fluid medium is butyl acetate. In still another exemplary embodiment of the present disclosure, the third fluid medium is xylene. In yet another exemplary embodiment of the present disclosure, the third fluid medium is methoxy propyl acetate. In still another embodiment of the present disclosure the fluid medium is a mixture of solvent C IX and butyl acetate.
In an embodiment of the present disclosure, the third fluid medium is present in an amount in the range of 5 mass% to 35 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the third fluid medium is present in an amount of 30 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the third fluid medium is present in an amount of 10 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the third fluid medium is present in an amount of 17 mass% with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the third fluid medium is present in an amount of 25 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the plasticizer is selected from the group consisting of phthalate plasticizers and non-phthalate plasticizers, wherein the phthalate plasticizer is diisononyl phthalate and the non-phthalate plasticizer is selected from the group consisting of alkylsulfonic acid ester with phenol (ASE) (Mesamoll group) and di(isononyl) cyclohexane-1,2-dicarboxylate (Hexamoll DINCH). In an exemplary embodiment of the present disclosure, the plasticizer is alkylsulfonic acid ester with phenol (ASE) (Mesamoll group).
In an embodiment of the present disclosure, the plasticizer is present in an amount in the range of o mass% to 35 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the plasticizer is present in an amount of 10.75 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the plasticizer is present in an amount of 20 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the plasticizer is present in an amount of 24.4 mass% with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the plasticizer is present in an amount of 18 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the pigment is titanium dioxide.
In an embodiment of the present disclosure, the pigment is present in an amount in the range of 0 mass% to 20 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the pigment is present in an amount of 5 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the pigment is present in an amount of 15 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the pigment is present in an amount of 2 mass% with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the pigment is present in an amount of 3 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the coating composition comprising the Polyaspartic polyurethane urea binder can be applied on a substrate as a membrane/film for water proofing application.
In a fourth aspect, the present disclosure provides a process for the preparation of coating composition. The process comprises the following steps.
a) mixing predetermined amounts of a dispersing agent and optionally a plasticizer in a reactor at a temperature in the range of 20 oC to 40 oC for a time period in the range of 10 minutes to 40 minutes at a stirring speed in the range of 400 rpm to 600 rpm to obtain a first mixture;
b) mixing predetermined amounts of a filler, optionally a pigment and a moisture scavenger in the first mixture at a temperature in the range of 20 oC to 40 oC for a time period in the range of 20 minutes to 70 minutes at a stirring speed in the range of 600 rpm to 1200 rpm to obtain a second mixture; and
c) mixing predetermined amounts of a Polyaspartic polyurethane urea binder, a third catalyst, a defoamer, a thixotropy additive and a third fluid medium to the second mixture at a temperature in the range of 20 oC to 40 oC for a time period in the range of 10 minutes to 50 minutes at a stirring speed in the range of 600 rpm to 1200 rpm to obtain the coating composition.
The process is explained in detail.
In a first step, predetermined amounts of a dispersing agent and optionally a plasticizer are mixed in a reactor at a temperature in the range of 20 oC to 40 oC for a time period in the range of 10 minutes to 40 minutes at a stirring speed in the range of 400 rpm to 600 rpm to obtain a first mixture.
In an embodiment of the present disclosure, the dispersing agent is selected from the group consisting of alkylammonium salt of copolymers (BYK 9076), soya lecithin-A complex (mixture of phospholipids, glycolipids, triglycerides, phosphatidylcholines, phosphatidylethanolamines and phosphatidylinositols), solution of a salt of unsaturated polyamine amides and acid polyesters (Antiterra U), solution of modified polyurethane (DBYK 163) and solution of polymeric phosphoric acid ester (BYK 110). In an exemplary embodiment of the present disclosure, the dispersing agent is soya lecithin-A complex (mixture of phospholipids, glycolipids, triglycerides, phosphatidylcholines, phosphatidylethanolamines and phosphatidylinositols). In another exemplary embodiment of the present disclosure, the dispersing agent is solution of a salt of unsaturated polyamine amides and acid polyesters (Antiterra U). In still another exemplary embodiment of the present disclosure, the dispersing agent is solution of polymeric phosphoric acid ester (BYK 110).
In an embodiment of the present disclosure, the dispersing agent is present in an amount in the range of 0.05 mass% to 5 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the dispersing agent is present in an amount of 0.05 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the dispersing agent is present in an amount of 1.85 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the dispersing agent is present in an amount of 0.1 mass% with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the dispersing agent is present in an amount of 0.25 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the plasticizer is selected from the group consisting of phthalate plasticizers and non-phthalate plasticizers, wherein the phthalate plasticizer is diisononyl phthalate and the non-phthalate plasticizer is selected from the group consisting of di (isononyl) cyclohexane-1, 2-dicarboxylate (Hexamoll DINCH). In an exemplary embodiment of the present disclosure, the plasticizer is alkylsulfonic acid ester with phenol (ASE) (Mesamoll group).
In an embodiment of the present disclosure, the plasticizer is present in an amount in the range of o mass% to 35 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the plasticizer is present in an amount of 10.75 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the plasticizer is present in an amount of 20 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the plasticizer is present in an amount of 24.4 mass% with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the plasticizer is present in an amount of 18 mass% with respect to the total mass of the coating composition.
In a second step, predetermined amounts of a filler, optionally a pigment and a moisture scavenger are mixed in the first mixture at a temperature in the range of 20 oC to 40 oC for a time period in the range of 20 minutes to 70 minutes at a stirring speed in the range of 600 rpm to 1200 rpm to obtain a second mixture.
In an embodiment of the present disclosure, the filler is selected from the group consisting of barium sulfate, calcium carbonate and magnesium silicate. In an exemplary embodiment of the present disclosure, the filler is barium sulfate. In another exemplary embodiment of the present disclosure, the filler is calcium carbonate. In still another exemplary embodiment of the present disclosure, the filler is magnesium silicate. In yet another exemplary embodiment of the present disclosure, the filler is a mixture of magnesium silicate, barium sulfate and calcium carbonate.
In an embodiment of the present disclosure, the filler is present in an amount in the range of 5 mass% to 50 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the filler is present in amount of 30 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the filler is present in amount of 39 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the filler is present in amount of 25 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the pigment is titanium dioxide.
In an embodiment of the present disclosure, the pigment is present in an amount in the range of 0 mass% to 20 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the pigment is present in an amount of 5 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the pigment is present in an amount of 15 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the pigment is present in an amount of 2 mass% with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the pigment is present in an amount of 3 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the moisture scavenger is selected from the group consisting of molecular sieve, monofunctional isocyanate (additive Ti) and ethyl orthoformate (additive OF). In an exemplary embodiment of the present disclosure, the moisture scavenger is molecular sieves. In another exemplary embodiment of the present disclosure, the moisture scavenger is Additive Ti.
In an embodiment of the present disclosure, the moisture scavenger is present in an amount in the range of 0.05 mass% to 6 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the moisture scavenger is present in an amount of 4.8 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the moisture scavenger is present in an amount of 3 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the moisture scavenger is present in an amount of 1 mass% with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the moisture scavenger is present in an amount of 0.05 mass% with respect to the total mass of the coating composition.
In a third step, predetermined amounts of a Polyaspartic polyurethane urea binder, a third catalyst, a defoamer, a thixotropy additive and a third fluid medium are mixed to the second mixture at a temperature in the range of 20 oC to 40 oC for a time period in the range of 10 minutes to 50 minutes at a stirring speed in the range of 600 rpm to 1200 rpm to obtain the coating composition.
In an embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is present in the amount in the range of 10 mass% to 55 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is present in the amount of 50 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is present in the amount of 20 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the Polyaspartic polyurethane urea binder is present in the amount of 35 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the third catalyst is selected from dibutyltin dilaurate and dimorpholinodiethyl ether. In an exemplary embodiment of the present disclosure, the third catalyst is dibutyltin dilaurate. In another exemplary embodiment of the present disclosure, the third catalyst is dimorpholinodiethyl ether.
In an embodiment of the present disclosure, the third catalyst is present in an amount in the range of 0.01 mass% to 3 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the third catalyst is present in an amount of 0.1 with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the third catalyst is present in an amount of 1.3 with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the third catalyst is present in an amount of 2 with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the third catalyst is present in an amount of 1 with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the defoamer is selected from the group consisting of silicone-free (BYK057), defoamer based on polysiloxanes (BYK1760/BYK530) and defoamer based on polymethylalkylsiloxane (BYK085). In an exemplary embodiment of the present disclosure, the defoamer is based on polysiloxanes (BYK1760/BYK530). In another exemplary embodiment of the present disclosure, the defoamer is based on polymethylalkylsiloxane (BYK085). In still another exemplary embodiment of the present disclosure, the defoamer is silicone-free (BYK057).
In an embodiment of the present disclosure, the defoamer is present in an amount in the range of 0.05 mass% to 2 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the defoamer is present in an amount of 0.1 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the defoamer is present in an amount of 0.2 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the defoamer is present in an amount of 0.05 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the thixotropy additive is selected from the group consisting of fumed silica after-treated with dimethyldichlorosilane (Aerosil R972), organically modified phyllosilicates (Garamite 1958), bentonite clay and polyamide (Cravallac Ultra). In an exemplary embodiment of the present disclosure, the thixotropy additive is fumed silica after-treated with dimethyldichlorosilane (Aerosil R972). In another exemplary embodiment of the present disclosure, the thixotropy additive is organically modified phyllosilicates (Garamite 1958). In still another exemplary embodiment of the present disclosure, the thixotropy additive is bentonite clay. In yet another exemplary embodiment of the present disclosure, the thixotropy additive is polyamide (Cravallac Ultra). In still another exemplary embodiment of the present disclosure, the thixotropy additive is Aerosil R972 and Cravallac Ultra.
In an embodiment of the present disclosure, the thixotropy additive is present in an amount in the range of 0.01 mass% to 5 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the thixotropy additive is present in an amount of 2 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the thixotropy additive is present in an amount of 0.5 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the thixotropy additive is present in an amount of 1.55 mass% with respect to the total mass of the coating composition.
In an embodiment of the present disclosure, the third fluid medium is selected from the group consisting of solvent C IX, butyl acetate, xylene and methoxy propyl acetate. In an exemplary embodiment of the present disclosure, the third fluid medium is solvent C IX. In another exemplary embodiment of the present disclosure, the third fluid medium is butyl acetate. In still another exemplary embodiment of the present disclosure, the third fluid medium is xylene. In yet another exemplary embodiment of the present disclosure, the third fluid medium is methoxy propyl acetate. In still another embodiment of the present disclosure the fluid medium is a mixture of solvent C IX and butyl acetate.
In an embodiment of the present disclosure, the third fluid medium is present in an amount in the range of 5 mass% to 35 mass% with respect to the total mass of the coating composition. In an exemplary embodiment of the present disclosure, the third fluid medium is present in an amount of 30 mass% with respect to the total mass of the coating composition. In another exemplary embodiment of the present disclosure, the third fluid medium is present in an amount of 10 mass% with respect to the total mass of the coating composition. In still another exemplary embodiment of the present disclosure, the third fluid medium is present in an amount of 17 mass% with respect to the total mass of the coating composition. In yet another exemplary embodiment of the present disclosure, the third fluid medium is present in an amount of 25 mass% with respect to the total mass of the coating composition.
The coating composition is characterized by having a pot life in the range of 8 hours to 24 hours.
The foregoing description of the embodiments has been provided for purposes of illustration and is 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 illustrated herein below with the help of the following non-limiting examples. The examples disclosed under these examples herein are intended merely to facilitate an understanding of how the embodiments herein may be practiced and to further enable those of skill in the art to practice the embodiments herein. Accordingly, the experiments should not be construed as limiting the scope of embodiments herein. These laboratory-scale experiments can be scaled up to an industrial/ commercial scale and the results obtained can be extrapolated to industrial/ commercial scale.
EXPERIMENTAL DETAILS
EXAMPLES
Step (I): Experiment 1 (A): Process for the preparation of a maleated polyol in accordance with the present disclosure
General procedure: The predetermined amounts of a polyol, maleic anhydride, a second catalyst, optionally a viscosity modifying agent and optionally a second fluid medium were mixed at a temperature in the range of 160 ? to 200 ? to obtain a maleated polyol.
The maleated polyol were prepared in Examples E1 to E6 by following the general procedure as above. The predetermined amounts of the specific ingredients of the maleated polyol are as given in Table 1.
Table 1: Predetermined amounts (mass %) of the ingredients used in examples E1-E6
Ingredients and their function E1
(mass %) E2
(mass %) E3
(mass %) E4
(mass %) E5
(mass %) E6
(mass %)
Sr. no. Materials Function/Broad class
1 Polypropylene glycol 2000 Polyol 98.9 0 0 0 0 0
2 Polypropylene glycol 4000 0 99.4 98.7 0 0 0
3 Polytetrahydrofuran polyol 2000 0 0 0 84 84.8 84.3
4 polycaprolactone 0 0 0 0 0 0
5 Iso octanol (only used when PolyTHF is used) Viscosity modifying agent 0 0 0 0 2.5 3
6 Maleic anhydride Anhydride 1 0.5 1.2 2 2.06 2.06
7 DBTO: dibutyl tin oxide Second Catalyst 0.1 0.1 0.1 0.1 0.06 0.06
8 Ortho xylene Second Fluid medium 0 0 0 13.9 10.58 10.58
Properties of maleated polyol
9 Acid value mg/KOH 3 1 2 2 2 2
10 Viscosity (Gardner scale and in centipoise) --- Y-Z
(1700-2300 centipoise) V-W
(900-1000 centipoise) W-X
1000-1300 centipoise) Z6
(15000 centipoise) Z6
(15000 centipoise) Z6
(15000 centipoise)
11 solid content --- 100 100 100 86 89 89
It is observed from Table 1 that the so obtained maleated polyol has amine value in the range of 1 mg/KOH to 5 mg/KOH, viscosity in the range of 900 centipoise to 15000 centipoise and solid content in the range of 80% to 100%.
Step (II): Experiment 1 (B): Process for the preparation of a polyaspartic ester amino polyol in accordance with the present disclosure
General procedure: Predetermined amount of the maleated polyol obtained in Experiment 1(A), was cooled to a temperature in the range of 40 ºC to 100 ºC, followed by adding a predetermined amount of an amine at a temperature in the range of 40 ºC to 100 ºC and maintaining for a time period in the range of 5 hours to 20 hours to obtain a polyaspartic ester amino polyol.
The polyaspartic ester amino polyol were prepared in Examples E7 to E16 by following the general procedure as above. The predetermined amounts of the specific ingredients of the polyaspartic ester amino polyol are as given in Table 2a and Table 2b.
Table 2a: Predetermined amounts (mass %) of the ingredients used in examples E7-E11
Ingredients and their function E 7
(mass %) E 8
(mass %) E 9
(mass %) E 10
(mass %) E 11
(mass %)
Sr.No. Materials Function/Broad class
1 Maleated polyol Polyol 95.5 (of E 1) 98.8 (of E 2) 99.8 (of E 2) 99.6 (of E 2) 99.55 (of E 2)
2 Polyetheramines: Jeffamine D230 Amine 4.5 1.2 0 0 0
3 Polyetheramines: Jeffamine D2000 0 0 0.2 0.4 0
4 4,4 diamino dicyclohexyl methane (PACM) 0 0 0 0 0
5 Isophorone diamine (IPDA) 0 0 0 0 0.45
6 (3-aminopropyl)trimethoxysilane 0 0 0 0 0
Properties of polyaspartic ester amino polyol
7 Amine value (mg/KOH) 1 to 15 mg/KOH 11 5 0.5 1 3.5
8 Viscosity (Gardener’s scale) W to Z2 Z-Z1
(2300-2500 centipoise) W-X
(1000-1300 centipoise) V-W
(900-1000 centipoise) V-W
(900-1000 centipoise) W-X
(1000-1300 centipoise)
9 Solid Content 99.4 99.5 99.4 99.2 99.5

Table 2b: Predetermined amounts (mass %) of the ingredients used in examples E12-E16
Ingredients and their function E 12
(mass %) E 13
(mass %) E 14
(mass %) E 15
(mass %) E 16
(mass %)
Sr. no. Materials Function/Broad class
1 Maleated derivative/polyol Polyol 98.96 (of E 3) 99.4 (of E 3) 98.9 (of E 3) 89 (of E 3) 90 (of E 5)
2 Polyetheramines: Jeffamine D230 Amine 0 0 0 0 0
3 Polyetheramines: Jeffamine D2000 0 0.6 0.6 11 0
4 4,4 diamino dicyclohexyl methane (PACM) 0 0 0 0 2
5 Isophorone diamine (IPDA) 1.04 0 0 0 0
6 (3-aminopropyl)trimethoxysilane 0 0 0.5 0 0
7 C-IX solvent/aromatic solvent, Ortho xylene (this is required when poly THF is used) Fluid medium
0 0 0 0 8
Properties of polyaspartic ester amino polyol
8 Amine value 6 0.6 2.6 5 10.6
9 Viscosity (Gardener’s scale) Z-Z1
(2300-2500 centipoise) X-Y
(1300-1700 centipoise) Z-Z1
(2300-2500 centipoise) Y-Z
(1700-2300 centipoise) Z5-Z6
(10000-15000centipoise)
10 Solid Content 99.3 99.6 99.7 99.6 80
It is observed from Table 2a and Table 2b that the so obtained polyaspartic ester amino polyol has the amine value in the range of 1 mg/KOH to 15 mg/KOH, the hydroxyl value in the range of 1 mg/KOH to 26 mg/KOH and the solid content in the range of 80% to 100%.
Step (III): Experiment 1 (C): Process for the preparation of 1K Polyaspartic polyurethane urea binder in accordance with the present disclosure
General procedure: The polyaspartic ester amino polyol as prepared in experiment 1(B) was mixed with a predetermined amount of an isocyanate compound, a first fluid medium, a first catalyst, optionally a chain extender and the polyol in the presence of nitrogen at 40 ºC to 100 ºC to obtain Polyaspartic polyurethane urea binder (1K).
The 1K Polyaspartic polyurethane urea binder were prepared in Examples E17 to E28 by following the general procedure as above. The predetermined amounts of the specific ingredients of the Polyaspartic polyurethane urea binder are as given in Table 3a and Table 3b.
Table 3a: Predetermined amounts (mass %) of the ingredients used in examples E17-E22
Ingredients and their function E 17
(mass%) E 18
(mass%) E 19
(mass%) E 20
(mass%) E 21
(mass%) E 22
(mass%)
Sr. no. Materials Function/Broad class
1 PPG 4000 (Optional) Polyol 0 0 0 75.65 0 73.45
2 CAPA-2201A 0 0 0 0 0 0
3 Desmophen C 1200: a linear aliphatic polycarbonate polyester polyol 0 0 0 0 0 0
4 Polyaspartic ester amino polyol Polyol 82 of Example 9 75 of Example 12 72.17 of Example 12 0 82 of Example 12 0

5

Diethylene glycol Chain extender 0 3 0.86 0 0 0
6 Isocyanate: toluene diisocyanate (TDI) Isocyanate compound 3 12 0 9.56 4 ---
7 Isophorone diisocyanate (IPDI) 0 0 13.91
0 5 13.27
8 Methylene diphenyl diisocyanate (PMDI) 5 0 0 1.73 0 0
9 H12MDI- Methylenedicyclohexyl Diisocyanate 0 0 0 0 0 0
Total diisocyanate --- 8 12 13.91 11.29 9 13.27
10 Methoxy propyl acetate (MPA)/ solvent C IX (C9)/
butyl acetate (BA)/combination First fluid medium 10 10 13.04 13.04 9 13.27
11 DBTDL: dibutyl tin dilaurate First catalyst 0.01 0.01 0.0086 0.0086 0.01 0.008
Table 3b: Predetermined amounts (mass %) of the ingredients used in examples E23-E28
Ingredients and their function E 23
(mass%) E 24
(mass%) E 25
(mass%) E 26
(mass%) E 27
(mass%) E 28
(mass%)
Sr. no. Materials Function/Broad class
1 PPG 4000 (Optional) Polyol 0 64.60 0 0 0 0
2 CAPA-2201A 0 0 0 0 13.63 0
3 Desmophen C 1200- a linear aliphatic polycarbonate polyester polyol 0 0 0 0 0 13.27
4 Polyaspartic ester amino polyol
Polyol 80 of Example 13 15.04 of Example 13
78.70 of Example 14 74.70 of Example 13 63.63 of Example 13 61.94 of Example 13

5

Diethylene glycol Chain extender 0 0 0 0 0 0
6 Isocyanate: toluene diisocyanate (TDI) Isocyanate compound 10 11.50 12.03 4.46 9.09 8.84
7 isophorone diisocyanate (IPDI) 0 0 0 0 0 3.53

8 Methylene diphenyl diisocyanate (PMDI) 0 0 0 0 0 0
9 H12MDI- Methylenedicyclohexyl Diisocyanate 0 0 0 8.92 0 0
Total diisocyanate --- 10 11.50 12.03 13.38 9.09 12.37
10 Methoxy propyl acetate (MPA)/solvent C IX (C9)/
butyl acetate (BA) or combination First Fluid medium 10 8.84 9.25 12.5 13.63 12.38
11 DBTDL: dibutyl tin dilaurate First catalyst 0.01 0.008 0.009 0.0089 0.009 0.0088
Experiment 2: Preparation of the coating composition in accordance with the present disclosure.
General procedure: The predetermined amount of a dispersing agent was mixed optionally with a plasticizer in a reactor at a temperature in the range of 20 oC to 40 oC in the range of 10 minutes to 40 minutes at a stirring speed in the range of 400 rpm to 600 rpm to obtain a first mixture. The predetermined amounts of a filler, optionally a pigment and a moisture scavenger were mixed in the first mixture at a temperature in the range of 20 oC to 40 oC for a time period in the range of 20 minutes to 70 minutes at a stirring speed in the range of 600 rpm to 1200 rpm to obtain a second mixture. The predetermined amounts of a Polyaspartic polyurethane urea binder, a third catalyst, a defoamer, a thixotropy additive and a third fluid medium was mixed with the second mixture at a temperature in the range of 20 oC to 40 oC for a time period in the range of 10 minutes to 50 minutes at a stirring speed in the range of 600 rpm to 1200 rpm to obtain the coating composition.
The coating composition was prepared in Examples C1 to C8 by following the general procedure as above. The predetermined amounts of the specific ingredients of the coating composition are as given in Table 4.
Table 4: Predetermined amounts (mass %) of the ingredients used in examples C1-C8
Coating composition C1 C2 C3 C4 C5 C6 C7 C8
Function of ingredients Ingredient Example 20
(mass%) Example 22(mass%) Example 23(mass%) Example 24(mass%) Example 25(mass%) Example 26(mass%) Example 27(mass%) Example 28(mass%)
Binder Polyaspartic amine binder 20 20 45 40 50 24.3 15 35
Plasticizer Phthalate plasticizer: diisononyl phthalate 15 0 0 18 0 0 29 0
non-phthalate plasticizer: alkylsulfonic acid ester with phenol (ASE) (Mesamoll group) 0 20 0 0 0 14 0 0
non-phthalate plasticizer: di(isononyl) cyclohexane-1,2-dicarboxylate (Hexamoll DINCH) 0 0 10.75 0 0 0 0 24.4
Filler Barytes (barium sulfate) 15 30 6 0 0 15 0 0
calcium carbonate 15 0 7 0 24.3 15 25 10
magnesium silicate 0 0 26 15 0 10 0 0
defoamer BYK057 0 0 0 0 0 0 0 1
BYK1760 0.1 0 0 0 0 0 2 0
BYK530 0 0 0.05 0.1 0 0.05 0 0
BYK085 0 0.1 0 0 0.2 0 0 0
Thixotropy additive Aerosil R972 :fumed silica after-treated with DDS (dimethyldichlorosilane) 0.05 0 0.1 0 0 0 0 0
Garamite 1958: organically modified phyllosilicates 0 0.5 0 1 0 0 0 0.1
Bentone clay: Bentonite Clay 0 0 0 0 2 0 0.1 0
Cravallac Ultra: polyamide 1.5 0 0 0 0 0.5 0 0
Dispersing agent BYK 9076 0 0 0 0 0 0 0 1
Soya lecithin-A complex 0.25 0 0 0 0 0 1.85 0
Antiterra U 0 0.05 0.1 0 0.05 0 0
DBYK 163 0 0 0 0 1 0 0 0
BYK 110 0 0.1 0 0 0 0 0 0
Third Catalyst DBDTL: Dibutyltin dilaurate 0.1 1.3 0 0 2 1 2 0
DMDEE: dimorpholinodiethyl ether 0 0 0.05 1 0 0 0 0.5
Moisture scavenger Molecular sieve/additive Ti/additive OF 1 3 3 4.8 4.5 0.1 0.05 1
Third Fluid Medium solvent C IX 0 0 5 0 14 0 0 15
MPA 0 25 0 15 0 0 0 0
Butyl acetate 0 0 0 0 0 17 0 10
xylene 30 0 0 0 0 0 10 0
Pigment TiO2 2 0 3 5 2 3 15 2
The so obtained coating compositions tested for a pot life and the pot life of the coating compositions of the present disclosure is in the range of 8 hours to 24 hours. The pot life (finished product’s working time for applications on substrate). Here, the pot life means time considered when a container is opened and the material is exposed to moisture in the air during application. The pot life is related to the final coating composition C1 to C8 and it depends on 1K formulation (polyasparatic polyurethane urea binder) and the environmental conditions such as humidity and temperature, typically it ranges from 8 to 24 hrs.
Experiment 3: Characterization of Polyaspartic polyurethane urea binder in accordance with the present disclosure.
The analysis of Physio-chemical properties of Polyaspartic polyurethane urea binders of Examples E17 to E28 in accordance with the present disclosure is summarized in Table 5.
Table 5: Analysis of Physio-chemical properties of Polyaspartic polyurethane urea binder in accordance with the present disclosure
Sr. No Properties of the binder E17 E18 E19 E20 E21 E22 E23 E24 E25 E26 E27 E28
1. %NCO content 2 to 6% 2 to 6% 2 to 6% 3 to 5% 2 to 5% 4 to 5% 3 to 6% 3 to 5% 3 to 5 % 3 to 5% 3 to 5% 3 to 5%
2. Viscosity (Gardner scale viscosity and in centipoise) Z-Z6
2300 to 15000 centipoise Z3-Z6
4500 to 15000 centipoise Z2-Z5
3500 to 10000 centipoise V-Y
900 to 1700 centipoise Z3-Z5
4500 to 10000 centipoise V
900 centipoise X-Z
1300 to 2300 centipoise W-X
1000 to 1300 centipoise Z-Z3
2300 to 4500 centipoise X-Z1
1300 to 2500 centipoise Z-Z2
2300 to 3500 centipoise Z-Z2
2300 to 3500 centipoise
3. Solid Content 86 -89 86-88 86-89 86-88 86-88 86-88 85-90% 85-90 85-90 85-88 85-88 85-88
It is observed from Table 5 that the so obtained polyaspartic polyurethane urea binders in accordance with the present disclosure have the % NCO in the range of 2% to 6%, the viscosity in the range of 900 centipoise to 15000 centipoise and the solid content in the range of 80% to 95%.
Experiment 4: Characterization of the coating composition in accordance with the present disclosure.
Physio-chemical properties analysis of a coating composition of C1 to C6 in accordance with the present disclosure is summarized in Table 6.
Table 6: Analysis of Physio-chemical properties of the coating composition in accordance with the present disclosure
Properties of the coating composition C1: Polyaspartic polyurethane urea binder of Example 20 C2: Polyaspartic polyurethane urea binder of Example 22 C3: Polyaspartic polyurethane urea binder of Example 23 C4: Polyaspartic polyurethane urea binder of Example 25 C5: Polyaspartic polyurethane urea binder of Example 26 C6: Polyaspartic polyurethane urea binder of Example 27
14 Days Tensile strength @ 300 microns to 1500 microns(Mpa) Tacky films observed upto 48 hours Tacky films observed upto 48 hours 1.2 to 4 1.2 to 4 2 to 5 2 to 5
14D %E @ 300 microns to 1500 microns thickness of the coating films 150-700 150-700 440 to 750 450 to 800
Adhesion (Mpa) after ponding on damp/damp surface (15-70 % moisture) 0.9 to 1.75 0.9 to 1.75 1.25 to 1.5 1.2 to 1.32
Adhesion (Mpa) after ponding on dry surface 1.5 to 2.2 1.5 to 2.2 1.2 to 1.35 1.15 to 1.3
Adhesion on damp surface 1.1 to 2 1.1 to 2 1.3 1.25
Adhesion on dry surface 1.7 to 2.5 1.7 to 2.5 1.25 1.2
14 D Crack Bridging ability (CBA) @ 300 microns to 1500 microns(Dry surface application) 4 to 8 4 to 8 5.6 6.6
14 D Crack Bridging ability (CBA) @ 300 microns to 1500 microns (Damp surface applications) 2 to 6 2 to 6 4.7 5.5
From Table 6, it is observed that the physicochemical properties of the coating composition are as desired. 4% to 6% of isocyanate content (NCO), values of viscosity in the range of W to Z3 (Gardener scale) and >80% solid content of the Polyaspartic polyurethane urea binder helps to achieve direct application on a dry and damp surface adhesion (moisture content >10%) with higher pot life and desired mechanical properties.
The coating composition comprising Polyaspartic polyurethane urea binder of the present disclosure has good pot life (in the range of 8 hours to 24 hours), which results in ease of application, good mechanical properties to the coat and good adhesion on dry and damp surfaces.
The coating composition of the present disclosure can be applied through brush and roller on surfaces which is advantageous as compared to the urea applications that generally employ plural gun sprays due to the fast reaction of amine and isocyanate for high-performance coating applications.
TECHNICAL ADVANCEMENTS
The present disclosure described herein above has several technical advantages including, but not limited to, the realization of;
? a Polyaspartic polyurethane urea binder that:
• is moisture curable;
• has longer pot life;
• is directly applicable on damp surfaces;
• has a high-solid content; and
• produces a coating composition having enhanced mechanical properties (crack bridging ability, adhesion on damp surface, adhesion on dry surface)
? a process for the preparation of a Polyaspartic polyurethane urea binder that:
• simple, efficient and environment friendly; and
• is feasible on a large/commercial scale;
and
? a coating composition that:
• has increased pot life;
• has ease of application; and
• has faster drying time.
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 Polyaspartic polyurethane urea binder being a product of
a) a polyaspartic ester amino polyol; and
b) an isocyanate compound,
wherein said polyaspartic ester amino polyol is a reaction product of a maleated polyol and at least one amine.

2. The binder as claimed in claim 1 comprises a first catalyst, a first fluid medium, and optionally a chain extender.
3. The binder as claimed in claim 1, wherein a molar ratio of said polyaspartic ester amino polyol to said isocyanate compound is in the range of 1:1.1 to 1:3.
4. The binder as claimed in claim 1, wherein said polyaspartic ester amino polyol is characterized by having:
• an amine value in the range of 1 mg/KOH to 15 mg/KOH; and
• a hydroxyl value in the range of 1 mg/KOH to 26 mg/KOH.
5. The binder as claimed in claim 1, wherein said maleated polyol being a product of
• a polyol;
• a second catalyst;
• maleic anhydride;
• optionally a viscosity modifying agent; and
• optionally a second fluid medium.

6. The binder as claimed in claim 1, wherein said maleated polyol is characterized by having:
• an acid value in the range of 1 mg/KOH to 5 mg/KOH; and
• a viscosity in the range of 900 centipoise to 15000 centipoise.
7. The binder as claimed in claim 5, wherein
• said polyol is selected from the group consisting of polypropylene glycol, polycaprolactone polyol, a linear aliphatic polycarbonate polyester polyol and poly tetrahydrofuran polyol;
• said second catalyst is dibutyl tin oxide (DBTO);
• said second fluid medium is selected from the group consisting of ortho xylene, meta xylene, para xylene and Solvent C IX; and
• said viscosity modifying agent is selected from the group consisting of butanol, pentanol, hexanol, heptanol, isooctanol, neooctanol and decanol.
8. The binder as claimed in claim 1, wherein
• said amine is selected from the group consisting of polyetheramine, 4,4 diamino dicyclohexyl methane, isophorone diamine and 3-aminopropyl trimethoxysilane; and
• said isocyanate compound is selected from the group consisting of isophorone diisocyanate, methylene diphenyl diisocyanate, hydrogenated methylenedicyclohexyl diisocyanate and toluene diisocyanate.
9. The binder as claimed in claim 2, wherein
a. said first catalyst is dibutyl tin dilaurate;
b. said first fluid medium is selected from the group consisting of methoxy propyl acetate, solvent C IX and butyl acetate; and
c. said chain extender is selected from the group consisting of diethylene glycol, 2-methyl-1,3-propanediol, and butanediol.
10. The binder as claimed in claim 1, wherein said maleated polyol is a maleic anhydride (MA) modified polyol (poly ether/poly ester polyol).
11. The binder as claimed in claim 1 is characterized by having:
• free NCO content in the range of 2% to 6%;
• solid content in the range of 80% to 95%; and
• viscosity in the range of 900 centipoise to 15000 centipoise.
12. The binder as claimed in claim 1 comprises a polyol selected from the group consisting of polypropylene glycol, polycaprolactone polyol, a linear aliphatic polycarbonate polyester polyol and poly tetrahydrofuran polyol.
13. A process for the preparation of a Polyaspartic polyurethane urea binder, said process comprising the following steps:
(i) mixing predetermined amounts of a polyol, a maleic anhydride, a second catalyst, optionally a viscosity modifying agent and optionally a second fluid medium at a temperature in the range of 160 ºC to 240 ºC to obtain a maleated polyol;
(ii) cooling said maleated polyol to a temperature in the range of 40 ºC to 100 ºC followed by adding a predetermined amount of an amine at a temperature in the range of 40 ºC to 100 ºC and maintaining for a time period in the range of 5 hours to 20 hours to obtain a polyaspartic ester amino polyol; and
(iii) mixing said polyaspartic ester amino polyol with predetermined amounts of an isocyanate compound, a first fluid medium and a first catalyst, optionally a chain extender and said polyol, in the presence of nitrogen at a temperature in the range of 40 ºC to 100 ºC to obtain said Polyaspartic polyurethane urea binder.
14. The process as claimed in claim 13, wherein a molar ratio of said polyaspartic ester amino polyol to said isocyanate compound is in the range of 1:1.1 to 1:3.
15. The process as claimed in claim 13, wherein said predetermined amount of
• said polyol is in the range of 80 mass% to 99.5 mass% with respect to the total mass of said maleated polyol;
• said maleic anhydride is in the range of 0.1 mass% to 3 mass% with respect to the total mass of said maleated polyol;
• said isocyanate is in the range of 5 mass% to 15 mass% with respect to the total mass of said Polyaspartic polyurethane urea binder;
• said first catalyst is in the range of 0.01 mass% to 0.2 mass% with respect to the total mass of said maleated polyol;
• said viscosity modifying agent is in the range of 0 mass% to 5 mass% with respect to the total mass of said maleated polyol;
• said first fluid medium is in the range of 0 mass% to 15 mass% with respect to the total mass of said maleated polyol;
• said amine is in the range of 0.1 mass% to 15 mass% with respect to the total mass of said polyaspartic ester amino polyol;
• said second catalyst is in the range of 0.005 mass% to 0.1 mass% with respect to the total mass of said Polyaspartic polyurethane urea binder;
• said second fluid medium is in the range of 5 mass% to 20 mass% with respect to the total mass of said Polyaspartic polyurethane urea binder; and
• said chain extender is in the range of 0 mass% to 20 mass% with respect to the total mass of said Polyaspartic polyurethane urea binder.
16. The process as claimed in claim 13, wherein
• said polyol is selected from the group consisting of polypropylene glycol, polycaprolactone polyol, a linear aliphatic polycarbonate polyester polyol and poly tetrahydrofuran polyol;
• said amine is selected from the group consisting of polyetheramine, 4,4 diamino dicyclohexyl methane, isophorone diamine and 3-aminopropyl trimethoxysilane;
• said isocyanate compound is selected from the group consisting of isophorone diisocyanate, methylene diphenyl diisocyanate, hydrogenated methylenedicyclohexyl diisocyanate and toluene diisocyanate;
• said viscosity modifying agent is selected from the group consisting of butanol, pentanol, hexanol, heptanol, isooctanol, neooctanol and decanol;
• said first catalyst is dibutyl tin dilaurate;
• said second catalyst is dibutyl tin oxide;
• said first fluid medium is selected from the group consisting of methoxy propyl acetate, solvent C IX and butyl acetate;
• said second fluid medium is selected from the group consisting of ortho xylene, meta xylene, para xylene and solvent C IX; and
• said chain extender is selected from the group consisting of diethylene glycol, 2-Methyl-1,3-propanediol, and butanediol.
17. The process as claimed in claim 13, wherein said maleated polyol is a Maleic anhydride (MA) modified polyol (poly ether/poly ester polyol).
18. A coating composition comprises
a. a polyaspartic polyurethane urea binder as claimed in claim 1;
b. at least one filler;
c. a defoamer;
d. at least one thixotropy additive;
e. a dispersing agent;
f. a third catalyst;
g. a moisture scavenger;
h. a third fluid medium;
i. optionally a pigment; and
j. optionally a plasticizer.
19. The coating composition as claimed in claim 18, wherein said composition comprises:
a. 10 mass% to 55 mass% of said polyaspartic polyurethane urea binder;
b. 5 mass% to 50 mass% of said filler;
c. 0.05 mass% to 2 mass% of said defoamer;
d. 0.01 mass% to 5 mass% of said thixotrophy additive;
e. 0.05 mass% to 5 mass% of said dispersing agent;
f. 0.01 mass% to 3 mass% of said third catalyst;
g. 0.05 mass% to 6 mass% of said moisture scavenger;
h. 5 mass% to 35 mass% of said third fluid medium;
i. 0 mass% to 35 mass% of said plasticizer; and
j. 0 mass% to 20 mass% of said pigment,
wherein said mass% of each ingredient is with respect to the total mass of said coating composition.
20. The coating composition as claimed in claim 18, wherein
• said plasticizer is selected from the group consisting of phthalate plasticizers and non-phthalate plasticizers, wherein said phthalate plasticizer is diisononyl phthalate; and said non-phthalate plasticizer is selected from the group consisting of alkylsulfonic acid ester with phenol (ASE) and di(isononyl) cyclohexane-1,2-dicarboxylate;
• said filler is selected from the group consisting of barium sulfate, calcium carbonate and magnesium silicate;
• said defoamer is selected from the group consisting of silicone-free defoamer, defoamers based on polysiloxanes and defoamers based on polymethylalkylsiloxane;
• said thixotropy additive is selected from the group consisting of fumed silica after-treated with dimethyldichlorosilane, organically modified phyllosilicates, bentonite clay and polyamide;
• said dispersing agent is selected from the group consisting of alkylammonium salt of copolymers, soya lecithin-A complex (mixture of phospholipids, glycolipids, triglycerides, phosphatidylcholines, phosphatidylethanolamines and phosphatidylinositols), salt of unsaturated polyamine amides and acid polyesters, solution of modified polyurethane and solution of polymeric phosphoric acid ester;
• said pigment is titanium dioxide;
• said third catalyst is selected from dibutyltin dilaurate and dimorpholinodiethyl ether;
• said moisture scavenger is selected from the group consisting of molecular sieve, monofunctional isocyanate (additive Ti) and ethyl orthoformate (additive OF); and
• said third fluid medium is selected from the group consisting of solvent C IX, butyl acetate, xylene and methoxy propyl acetate.
21. A process for the preparation of a coating composition, said process comprises the following steps:
a) mixing predetermined amounts of a dispersing agent and optionally a plasticizer in a reactor at a temperature in the range of 20 oC to 40 oC for a time period in the range of 10 minutes to 40 minutes at a stirring speed in the range of 400 rpm to 600 rpm to obtain a first mixture;
b) mixing predetermined amounts of a filler, optionally a pigment and a moisture scavenger in said first mixture at a temperature in the range of 20 oC to 40 oC for a time period in the range of 20 minutes to 70 minutes at a stirring speed in the range of 600 rpm to 1200 rpm to obtain a second mixture; and
c) mixing predetermined amounts of a polyaspartic polyurethane urea binder as claimed in claim 1, a third catalyst, a defoamer, a thixotropy additive and a third fluid medium to said second mixture at a temperature in the range of 20 oC to 40 oC for a time period in the range of 10 minutes to 50 minutes at a stirring speed in the range of 600 rpm to 1200 rpm to obtain said coating composition.
22. The process as claimed in claim 21, wherein
• said plasticizer is selected from the group consisting of phthalate plasticizers and non-phthalate plasticizers, wherein said phthalate plasticizer is diisononyl phthalate; and said non-phthalate plasticizer is selected from the group consisting of alkylsulfonic acid ester with phenol (ASE)and di(isononyl) cyclohexane-1,2-dicarboxylate;
• said filler is selected from the group consisting of barium sulfate, calcium carbonate and magnesium silicate;
• said defoamer is selected from the group consisting of silicone-free defoamer, defoamers based on polysiloxanes and defoamers based on polymethylalkylsiloxane;
• said thixotropy additive is selected from the group consisting of fumed silica after-treated with dimethyldichlorosilane, organically modified phyllosilicates, bentonite clay and polyamide;
• said dispersing agent is selected from the group consisting of alkylammonium salt of copolymers, soya lecithin-A complex (mixture of phospholipids, glycolipids, triglycerides, phosphatidylcholines, phosphatidylethanolamines and phosphatidylinositols), salt of unsaturated polyamine amides and acid polyesters, solution of modified polyurethane and solution of polymeric phosphoric acid ester;
• said pigment is titanium dioxide;
• said third catalyst is selected from dibutyltin dilaurate and dimorpholinodiethyl ether;
• said moisture scavenger is selected from the group consisting of molecular sieve, monofunctional isocyanate (additive Ti) and ethyl orthoformate (additive OF); and
• said third fluid medium is selected from the group consisting of solvent C IX, butyl acetate, xylene and methoxy propyl acetate.
23. The process as claimed in claim 21, wherein said predetermined amounts of
• said polyaspartic polyurethane urea binder is in the range of 10 mass% to 55 mass%;
• said plasticizer is in the range of 0 mass% to 35 mass%;
• said filler is in the range of 5 mass% to 50 mass%;
• said defoamer is in the range of 0.05 mass% to 2 mass%;
• said thixotropy additive is in the range of 0.01 mass% to 5 mass%;
• said dispersing agent is in the range of 0.05 mass% to 5 mass%;
• said third catalyst is in the range of 0.01 mass% to 3 mass%;
• said moisture scavenger is in the range of 0.05 mass% to 6 mass%;
• said third fluid medium is in the range of 5 mass% to 35 mass%; and
• said pigment is in the range of 0 mass% to 20 mass%,
wherein said mass% of each ingredient is with respect to the total mass of said coating composition.
24. The coating composition as claimed in claim 18 is characterized by having a pot life in the range of 8 hours to 24 hours.

Dated this 13th day of July, 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