DESC:FIELD
The present disclosure relates to a polyaspartic ester amine binder and a coating composition made therefrom.
DEFINITIONS
As used in the present disclosure, the following terms are generally intended to have the meaning as set forth below, except to the extent that the context in which it is used indicates otherwise.
Tensile strength: The term “tensile strength refers to the maximum amount of tensile stress a material can withstand before it fails or breaks. It is a measure of the material's ability to resist deformation under tension or stretching forces.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
Polyaspartic ester amines are the key component of the polyurea coating compositions. The polyaspartic ester amines are secondary amines that are derived from a primary polyamine and dialkyl maleate. The polyaspartic ester amine resin are prepared by the conversion of primary amine to a secondary amine by the Michael addition reaction. The Michael addition reaction uses dialkyl maleate of different alkyl chain lengths as the Michael substrate, which influences the conversion of a primary amine to a secondary amine.
The conventional process for the preparation of the secondary amine uses a higher amount of dialkyl maleate to achieve the complete conversion of primary amine to a secondary amine. However, the so obtained secondary amine contains an excess amount of dialkyl maleate, which is difficult to remove completely.
The conventional polyaspartic ester amines with secondary amines alone fail to provide the desired tensile strength to the cured film.
Therefore, there is felt a need to provide a polyaspartic ester amine binder and a coating composition made therefrom, that mitigates the aforesaid drawbacks or at least provide an alternative solution.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows.
An object of the present disclosure is to ameliorate one or more problems of the background or to at least provide a useful alternative.
Another object of the present disclosure is to provide a polyaspartic ester amine binder.
Yet another object of the present disclosure is to provide a coating composition.
Still another object of the present disclosure is to provide a process for the preparation of a coating composition.
Yet another object of the present disclosure is to provide a process for the preparation of a coating composition comprising polyaspartic ester amine binder.
Still another object of the present disclosure is to provide a simple and cost-effective process for the preparation of a coating composition.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.
SUMMARY
The present disclosure relates to a polyaspartic ester amine binder which is characterized by having an amine value in the range of 170 mg KOH/g to 220 mg KOH/g and viscosity in the range of 160 centipoise to 1000 centipoise.
The polyaspartic ester amine binder is a reaction product of 10 wt% to 55 wt% of a primary amine and 45 wt% to 90 wt% of a dialkyl ester, wherein the wt% of each ingredient is with respect to the total weight of the polyaspartic ester amine binder.
The mole ratio of the primary amine to the dialkyl ester is in the range of 1: 1.5 to 1:1.9.
In an embodiment of the present disclosure, the polyaspartic ester amine binder is a primary amine terminated polyaspartic ester amine binder.
The primary amine is at least one selected from the group consisting of isophorone diamine (IPDA), bis-p-aminocyclohexymethane (PACM), and polyetheramine. The dialkyl ester is at least one selected from the group consisting of dibutyl maleate (DMB), diethyl maleate (DEM) and dioctyl maleate (DOM).
Further, the present disclosure relates to a coating composition comprising an amine component and an isocyanate component. The amine component comprises a polyaspartic ester amine binder, optionally a primary amine, at least one filler, at least one defoamer and a mixture of plasticizers. The isocyanate component comprises at least one aliphatic polyisocyanate, at least one aromatic polyisocyanate and a solvent, wherein a ratio of the amine component to the isocyanate component is in the range of 1:1 to 1:1.5.
In accordance with the present disclosure, the amine component comprises 5 wt% to 20wt% of the polyaspartic ester amine binder, 0 wt% to 1 wt% of the primary amine, 20 wt % to 35 wt % of the filler, 0.1 wt % to 1 wt % of the defoamer, and 2 wt % to 15 wt % of the mixture of plasticizers, wherein the wt% of each ingredient is with respect to the total weight of the amine component.
In accordance with the present disclosure, the isocyanate component comprises 1 wt% to 10 wt% of the aliphatic polyisocyanate, 20 wt% to 40 wt% of the aromatic polyisocyanate and 5 wt% to 20 wt% of the solvent, wherein the wt% of each ingredient is with respect to the total weight of the isocyanate component.
In accordance with the present disclosure, the filler is at least one selected from the group consisting of titanium dioxide, barium sulphate, calcium oxide, stearates, molecular sieve, and micronized, highly porous, crystalline aluminosilicate.
The defoamer is VOC-free silicone-containing defoamer.
The mixture of plasticizers is a mixture of a phthalate plasticizer and a non-phthalate plasticizer.
The phthalate plasticizer is diisononyl phthalate and the non-phthalate plasticizer is at least one selected from the group consisting of alkylsulfonic acid ester with phenol (ASE) (Mesamoll group) and di(isononyl) cyclohexane-1,2-dicarboxylate (Hexamoll DINCH).
The aliphatic polyisocyanate is at least one selected from the group consisting of methylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate (HDI), 4-4’-dicyclohexylmethane diisocyanate (H12MDI) and methylene-bis(4-cyclohexylisocyanate) and their dimers, trimers and prepolymers.
The aromatic polyisocyanate is toluidine diisocyanate.
The solvent is selected from the group consisting of xylene, ortho-xylene and C9 naphtha.
The primary amine is at least one selected from the group consisting of isophorone diamine (IPDA), bis-p-aminocyclohexymethane (PACM), and polyetheramine.
The dialkyl ester is at least one selected from the group consisting of dibutyl maleate (DMB), diethyl maleate (DEM) and dioctyl maleate (DOM).
The process for the preparation of a coating composition comprises a step of preparing an amine component and preparing an isocyanate component. Predetermined amounts of at least one primary amine, optionally a catalyst and an anhydride are charged in a reactor followed by adding a predetermined amount of at least one dialkyl ester over a predetermined time period at a first predetermined temperature to obtain a first mixture and the first mixture is heated gradually to a second predetermined temperature to obtain the polyaspartic ester amine binder. Predetermined amounts of the polyaspartic ester amine binder, optionally a primary amine and a filler are mixed in a reactor at a stirring speed in the range of 300 rpm to 600 rpm for a time period in the range of 1 minute to 40 minutes to obtain an intermediate amine mixture. Predetermined amounts of a defoamer and a mixture of plasticizers are mixed to the intermediate amine mixture at a stirring speed in the range of 300 rpm to 600 rpm to obtain the amine component. Separately, nitrogen is sparged in a reactor for a time period in the range of 5 minutes to 25 minutes, followed by mixing predetermined amounts of a solvent and an aromatic polyisocyanate at a stirring speed in the range of 100 rpm to 400 rpm for a time period in the range of 30 minute to 60 minutes to obtain an intermediate isocyanate mixture. A predetermined amount of an aliphatic polyisocyanate is mixed with the intermediate isocyanate mixture for a time period in the range of 10 minutes to 40 minutes under the stirring speed in the range of 100 rpm to 400 rpm to obtain the isocyanate component. The amine component and the isocyanate component are mixed in a predetermined ratio to obtain the coating composition, wherein the ratio of the amine component to the isocyanate component is in the range of 1:1 to 1:1.5.
In accordance with the present disclosure, the predetermined amount of the polyaspartic ester amine binder is in the range of 5 wt% to 20 wt%. The predetermined amount of the primary amine is in the range of 0 wt% to 10 wt%. The predetermined amount of the filler is in the range of 20 wt% to 35 wt%. The predetermined amount of the defoamer is in the range of 0.1 wt% to 1 wt% and the predetermined amount of the plasticizer is in the range of 2 wt% to 30 wt%, wherein the wt % of each ingredient is with respect to the total weight of the amine component.
In accordance with the present disclosure, the predetermined amount of the aliphatic polyisocyanate is in the range of 1 wt% to 10 wt%. The predetermined amount of the aromatic polyisocyanate is in the range of 20 wt% to 40 wt%. The predetermined amount of the solvent is in the range of 5 wt% to 20 wt%, wherein said wt% of each ingredient is with respect to the total weight of the isocyanate component.
The primary amine is at least one selected from the group consisting of isophorone diamine (IPDA), bis-p-aminocyclohexymethane (PACM), and polyetheramine.
The dialkyl ester is at least one selected from the group consisting of dibutyl maleate (DMB), diethyl maleate (DEM) and dioctyl maleate (DOM).
The catalyst is selected from the group consisting of dibutylin oxide and dibutylin dilaurate and the anhydride is maleic anhydride.
The anhydride is maleic anhydride.
In accordance with the present disclosure, the predetermined amount of the primary amine is in the range of 15 wt% to 50 wt%. The predetermined amount of the dialkyl ester is in the range of 45 wt% to 90 wt%. The predetermined amount of the catalyst is in the range of 0 wt% to 0.05 wt% and the predetermined amount of the anhydride is in the range of 0 wt% to 5 wt%, wherein the wt% of each ingredient is with respect to the total weight of the polyaspartic ester amine binder.
In accordance with the present disclosure, the predetermined time period is in the range of 1 hour to 7 hours. The first predetermined temperature is in the range of 30 ºC to 45ºC and the second predetermined temperature is in the range of 50 ºC to 90 ºC.
DETAILED DESCRIPTION
The present disclosure relates to a polyaspartic ester amine binder and a coating composition made therefrom.
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.
Polyaspartic ester amines are the key component of the polyurea coating compositions. The polyaspartic ester amines are secondary amines that are derived from a primary polyamine and dialkyl maleate. The polyaspartic ester amine resin are prepared by the conversion of primary amine to a secondary amine by the Michael addition reaction. The Michael addition reaction uses dialkyl maleate of different alkyl chain lengths as the Michael substrate, which influences the conversion of a primary amine to a secondary amine.
The conventional process for the preparation of the secondary amine uses a higher amount of dialkyl maleate to achieve the complete conversion of primary amine to a secondary amine. However, the so obtained secondary amine contains an excess amount of dialkyl maleate, which is difficult to remove completely. The conventional polyaspartic ester amines with secondary amines alone fail to provide the desired tensile strength to the cured film.
The present disclosure provides a polyaspartic ester amine binder and a coating composition made therefrom.
The present disclosure provides a polyaspartic ester amine binder that has higher mechanical properties. The coating composition made therefrom has longer pot life, ease of application and improved tensile strength.
The process of the present disclosure is simple, economical, and results in providing the polyaspartic ester amine binder comprising primary and secondary amino groups.
In an aspect of the present disclosure, there is provided a polyaspartic ester amine binder.
In accordance with the embodiment of the present disclosure, the polyaspartic ester amine binder which is characterized by having an amine value in the range of 170 mg KOH/g to 220 mg KOH/g and viscosity in the range of 160 centipoise to 1000 centipoise.
In an exemplary embodiment of the present disclosure, the polyaspartic ester amine binder has an amine value 185 mgKOH/g. In another exemplary embodiment of the present disclosure, the polyaspartic ester amine binder has an amine value 190 mgKOH/g.
In an embodiment of the present disclosure, the polyaspartic ester amine has viscosity in the range of 160 centipoise to 1000 centipoise, which corresponds to the A-W range of Gardener’s viscosity scale. In an exemplary embodiment of the present disclosure, the polyaspartic ester amine binder has viscosity in the range of 300 to 320 centipoise. In another exemplary embodiment of the present disclosure, the polyaspartic ester amine binder has viscosity in the range of 280 to 300 centipoise.
In accordance with an embodiment of the present disclosure, the polyaspartic ester amine binder is a reaction product of:
a. 10 wt% to 55 wt% of a primary amine; and
b. 45 wt% to 90 wt% of a dialkyl ester;
wherein the wt% of each ingredient is with respect to the total weight of the polyaspartic ester amine binder.
In an embodiment of the present disclosure, the polyaspartic ester amine binder is a primary amine terminated polyaspartic ester amine binder.
In accordance with the present disclosure, a mole ratio of the primary amine to the dialkyl ester is in the range of 1:1.5 to 1:1.9. In an exemplary embodiment of the present disclosure, the mole ratio of the primary amine to the dialkyl ester is 1:1.64. In another an exemplary embodiment of the present disclosure, the mole ratio of the primary amine to the dialkyl ester is 1:1.82.
In accordance with the present disclosure, the primary amine is at least one selected from the group consisting of isophorone diamine (IPDA), bis-p-aminocyclohexymethane (PACM), and polyetheramine (Jefamine D2000 and Jefamine D230). In an exemplary embodiment of the present disclosure, the primary amine is isophorone diamine (IPDA). In another exemplary embodiment of the present disclosure, the primary amine is bis-p-aminocyclohexymethane (PACM) and (Diaminopolypropylene Glycol; Poly(propylene glycol) bis(2-aminopropyl ether) (Jefamine-D230).
In accordance with the present disclosure, the dialkyl ester is at least one selected from the group consisting of dibutyl maleate (DMB), diethyl maleate (DEM) and dioctyl maleate (DOM). In an exemplary embodiment of the present disclosure, the dialkyl ester is dibutyl maleate. In another exemplary embodiment of the present disclosure, the dialkyl ester is diethyl maleate.
In an embodiment, the higher ratio of dialkyl maleate increases the conversion of primary diamine to secondary aspartate amine. In an embodiment of the present disclosure, the excess dialkyl maleate can be retained partially or fully in the polyaspartic ester amine. The excess dialkyl maleate will act as a plasticizer in the polyurea coating composition, by adjusting appropriately against other plasticizers present in the polyurea coating composition. Further, the higher ratio of dialkyl ester increases the conversion of primary diamine to secondary aspartate amine.
The excess of dialkyl maleate in the polyaspartic ester amine acts as plasticizer in the finished good and as per the role of other plasticizers, thereby achieved higher elongation, pot life and maintains the desired tensile strength.
The amine value in the polyaspartic ester amine binder is crucial to obtain desired mechanical properties, tensile strength and pot life.
In another aspect of the present disclosure, there is provided a coating composition.
In accordance with the present disclosure, the coating composition comprises:
A. an amine component comprises:
a. a polyaspartic ester amine binder;
b. optionally a primary amine;
c. at least one filler;
d. at least one defoamer; and
e. a mixture of plasticizers,
B. an isocyanate component comprises:
a. at least one aliphatic polyisocyanate;
b. at least one aromatic polyisocyanate; and
c. a solvent,
wherein a ratio of the amine component to the isocyanate component is in the range of 1:1 to 1:1.5.
In accordance with an embodiment of the present disclosure, the amine component comprises:
a. 5 wt% to 20 wt% of the polyaspartic ester amine binder;
b. 0 wt% to 10 wt% of the primary amine;
c. 20 wt% to 35 wt% of the filler;
d. 0.1 wt% to 1 wt% of the defoamer; and
e. 2 wt% to 30 wt% of the plasticizer,
wherein the wt% of each ingredient is with respect to the total weight of the amine component.
In an embodiment of the present disclosure, the amine component comprises a polyaspartic ester amine binder, optionally a primary amine, at least one filler, at least one defoamer; and a mixture of plasticizers.
In an embodiment of the present disclosure, the polyaspartic ester amine binder is a reaction product of:
a. 10 wt% to 55 wt% of a primary amine; and
b. 45 wt% to 90 wt% of a dialkyl ester;
wherein the wt% of each ingredient is with respect to the total weight of the polyaspartic ester amine binder.
In an embodiment of the present disclosure, the primary amine is at least one selected from the group consisting of isophorone diamine (IPDA), bis-p-aminocyclohexymethane (PACM), and polyetheramine (Jefamine D2000 and Jefamine D230). In an exemplary embodiment of the present disclosure, the primary amine is Jefamine D-2000.
In an embodiment of the present disclosure, the filler is at least one selected from the group consisting of titanium dioxide, barium sulphate (Bartyes), calcium oxide, stearates, molecular sieve and micronized, highly porous, crystalline aluminosilicate. In an exemplary embodiment of the present disclosure, the filler is titanium dioxide and barium sulphate.
In an embodiment of the present disclosure, the filler is a mixture of titanium dioxide and barium sulphate. Titanium dioxide is present in an amount in the range of 1% to 5% and barium sulphate is present in an amount in the range of 95% to 99%, wherein the amounts are with respect to the mixture.
In an embodiment of the present disclosure, the defoamer is VOC-free silicone-containing defoamer (BYK 1799).
In an embodiment of the present disclosure, the plasticizer is at least one selected from the group consisting of a phthalate plasticizer and a non-phthalate plasticizer.
The phthalate plasticizer is diisononyl phthalate (DINP).
The non-phthalate plasticizer is at least one selected from the group consisting of alkylsulfonic acid ester with phenol (ASE) (Mesamoll group), di(isononyl) cyclohexane-1,2-dicarboxylate (Hexamoll DINCH). In an exemplary embodiment of the present disclosure, the non-phthalate is alkylsulfonic acid ester with phenol (ASE) (Mesamoll group). In another exemplary embodiment of the present disclosure, the non-phthalate plasticizer is di(isononyl) cyclohexane-1,2-dicarboxylate (Hexamoll DINCH).
In an exemplary embodiment of the present disclosure, the amine component comprises:
a. 14.41 wt% of polyaspartic ester amine binder;
b. 26.5 wt% of titanium dioxide (filler);
c. 0.46 wt% of BYK 1799 (defoamer); and
d. 3 wt% of alkylsulfonic acid ester with phenol (ASE) (Mesamoll group) (non-phthalate plasticizer),
wherein the wt% of each ingredient is with respect to the total weight of the amine component.
In another exemplary embodiment of the present disclosure, the amine component comprises:
a. 14.41 wt% of polyaspartic ester amine binder;
b. 26.5 wt% of titanium dioxide (filler);
c. 0.46 wt% of BYK 1799 (defoamer); and
d. 8 wt% of diisononyl phthalate (phthalate based plasticizer),
wherein the wt% of each ingredient is with respect to the total weight of the amine component.
In still another exemplary embodiment of the present disclosure, the amine component comprises:
a. 14.41 wt% of polyaspartic ester amine binder;
b. 26.5 wt% of titanium dioxide (filler);
c. 0.46 wt% of BYK 1799 (defoamer);
d. 4 wt% of diisononyl phthalate (phthalate based plasticizer); and
e. 6 wt% of mesamoll (non-phthalate platsicizer),
wherein the wt% of each ingredient is with respect to the total weight of the amine component.
In an embodiment of the present disclosure, the isocyanate component comprises at least one aliphatic polyisocyanate, at least one aromatic polyisocyanate and a solvent.
In an embodiment of the present disclosure, the aliphatic polyisocyanate is at least one selected from the group consisting of methylene diisocyanate, isophorone diisocyanate (IPDI), hexamethylene diisocyanate (HDI), 4-4’-dicyclohexylmethane diisocyanate (H12MDI) and methylene-bis(4-cyclohexylisocyanate) and their dimers, trimers and prepolymers. In an exemplary embodiment of the present disclosure, the aliphatic polyisocyanate is isophorone diisocyanate (IPDI).
In an embodiment of the present disclosure, the aromatic polyisocyanate is toluidine diisocyanate (TDI).
In an embodiment of the present disclosure, the solvent is selected from the group consisting of xylene, ortho-xylene and C9 naphtha. In an exemplary embodiment of the present disclosure, the solvent is ortho-xylene.
In an exemplary embodiment of the present disclosure, the isocyanate component comprises:
a. 1.2 wt% of IPDI (aliphatic polyisocyanate);
b. 31 wt% of TDI (aromatic polyisocyanate); and
c. 13 wt% of ortho-xylene (solvent).
wherein the wt% of each ingredient is with respect to the total weight of the isocyanate component.
In an embodiment of the present disclosure, the ratio of the amine component (NH and/or NH2) to the isocyanate (NCO) component is in the range of 1:1 to 1:1.5. In an exemplary embodiment of the present disclosure, the ratio of the amine component to the isocyanate component is 1:1.18. In another exemplary embodiment of the present disclosure, the ratio of the amine component to the isocyanate component is 1:1.32.
The coating composition comprising polyaspartic ester amine binder of the present disclosure has good pot life which results in ease of application and good mechanical properties to the coat. The excess of isocyanate is required to adjust the pot life and mechanical properties. When the amine value is lower, the properties are lower and the pot life is higher and vice a versa. Furthermore, the use of phthalate plasticizer i.e. DINP helps in attaining good pot life.
The coating composition of the present disclosure is applied through brush and roller applications on surfaces which is advantageous as compared to the polyurea applications that generally employs plural gun sprays due to the fast reaction of amine and isocyanate for high-performance coating applications.
In yet another aspect of the present disclosure, there is provided a process for the preparation of the coating composition.
The process for the preparation of the coating composition comprises a step of preparing an amine component and a step of preparing an isocyanate component.
In accordance with the present disclosure, the process of preparation of the amine component comprises following steps:
(i) charging a reactor with predetermined amounts of at least one primary amine, optionally a catalyst and an anhydride, followed by adding a predetermined amount of at least one dialkyl ester over a predetermined time period at a first predetermined temperature to obtain a first mixture; and heating the first mixture gradually to a second predetermined temperature to obtain the polyaspartic ester amine binder,
(ii) mixing predetermined amounts of the polyaspartic ester amine binder in accordance with the present disclosure, optionally a primary amine and a filler in a reactor at a stirring speed in the range of 300 rpm to 600 rpm for a time period in the range of 1 minute to 40 minutes to obtain an intermediate amine mixture;
(iii) mixing predetermined amounts of a defoamer and a mixture of plasticizers to the intermediate amine mixture at a stirring speed in the range of 300 rpm to 600 rpm to obtain the amine component.
In accordance with the present disclosure, the process of preparation of the isocyanate component comprises following steps:
(i) separately, sparging nitrogen in a reactor for a time period in the range of 5 minutes to 25 minutes, followed by mixing predetermined amounts of a solvent and an aromatic polyisocyanate at a stirring speed in the range of 100 rpm to 400 rpm for a time period in the range of 30 minute to 70 minutes to obtain an intermediate isocyanate mixture; and
(ii) mixing predetermined amount of an aliphatic polyisocyanate to the intermediate iscynate mixture for a time period in the range of 10 minutes to 40 minutes under the stirring speed in the range of 100 rpm to 400 rpm to obtain the isocyanate component.
In an embodiment of the present disclosure, the predetermined amounts of
• the primary amine is in the range of 15 wt% to 50 wt%;
• the dialkyl ester is in the range of 45 wt% to 90 wt%;
• the catalyst is in the range of 0 wt% to 0.05 wt%; and
• the anhydride is in the range of 0 wt% to 5 wt%,
wherein the wt% of each ingredient is with respect to the total weight of the polyaspartic ester amine binder.
In an embodiment of the present disclosure, the predetermined time period is in the range of 1 hour to 7 hours. In an exemplary embodiment of the present disclosure, the predetermined time period is 3 hours.
In an embodiment of the present disclosure, the first predetermined temperature is in the range of 30 ºC to 45ºC. In an exemplary embodiment of the present disclosure, the first predetermined temperature is 40 ºC.
In an embodiment of the present disclosure, the second predetermined temperature is in the range of 50 ºC to 90 ºC. In an exemplary embodiment of the present disclosure, the second predetermined temperature is raised from 50 ºC to 80 ºC.
In an embodiment of the present disclosure, the polyaspartic ester amine binder is characterized by having an amine value in the range of 170 mgKOH/g to 220 mgKOH/g and viscosity in the range of 160 centipoise to 1000 centipoise. In an exemplary embodiment of the present disclosure, the polyaspartic ester amine binder has viscosity 300 to 320 centipoise (gardener’s scale: L-M). In another exemplary embodiment of the present disclosure, the polyaspartic ester amine binder has viscosity 280 to 300 centipoise (gardener’s scale: K-L).
In accordance with the present disclosure, the catalyst is selected from the group consisting of dibutyltin oxide and dibutyltin dilaurate. In an exemplary embodiment of the present disclosure, the catalyst is dibutyltin oxide.
In accordance with the present disclosure, the anhydride is maleic anhydride.
The polyaspartic ester amine binder incorporated with maleic anhydride (maximum 3 wt%) provides faster drying and better mechanical properties (Tensile Strength and elongation at break (%EE)) of polyaspartic ester amines.
The polyaspartic ester amine binder with maleic anhydride helps in achieving the higher mechanical properties.
In an exemplary embodiment of the present disclosure, the polyaspartic ester amine binder comprises:
• 36.4 wt% of isophorone diamine (IPDA);
• 63.58 wt% of dibutyl maleate; and
• 0.02 wt% of dibutyltin oxide;
wherein the wt% of each ingredient is with respect to the total weight of the polyaspartic ester amine binder.
In another exemplary embodiment of the present disclosure, the polyaspartic ester amine binder comprises:
• 15.24 wt% of bis-p-aminocyclohexamethane and 27.46 wt% of Jefamine D230;
• 54.3 wt% of dibutyl maleate; and
• 3 wt% of maleic anhydride
wherein the wt% of each ingredient is with respect to the total weight of the polyaspartic ester amine binder.
In still another exemplary embodiment of the present disclosure, the polyaspartic ester amine binder comprises:
• 23.4 wt% of bis-p-aminocyclohexamethane and 27.46 wt% of Jefamine D230;
• 76.58 wt% of diethyl maleate; and
• 0.02 wt% of dibutyltin oxide;
wherein the wt% of each ingredient is with respect to the total weight of the polyaspartic ester amine binder.
In accordance with the present disclosure, the amine component and the isocyanate component are mixed in a predetermined ratio to obtain a coating composition.
In an embodiment of the present disclosure, the ratio of the amine component to the isocyanate component is in the range of 1:1 to 1:1.5. In an exemplary embodiment of the present disclosure, the ratio of the amine component to the isocyanate component is 1:1.32. In another exemplary embodiment of the present disclosure, the ratio of the amine component to the isocyanate component is 1:1.06.
In an exemplary embodiment of the present disclosure, the stirring speed is 450 rpm.
In an exemplary embodiment of the present disclosure, the time period is 15 minutes.
In an embodiment of the present disclosure,
• the predetermined amount of the polyaspartic ester amine binder is in the range of 5 wt% to 20 wt%;
• the predetermined amount of the primary amine is in the range of 0 wt% to 10 wt%;
• the predetermined amount of the filler is in the range of 20 wt% to 35 wt%;
• the predetermined amount of the defoamer is in the range of 0.1 wt% to 1 wt%; and
• the predetermined amount of the plasticizer is in the range of 2 wt% to 30 wt%,
wherein the weight % of each ingredient is with respect to the total weight of the amine component.
In an embodiment of the present disclosure, the predetermined amounts of
• the predetermined amount of the aliphatic polyisocyanate is in the range of 1 wt% to 10 wt%;
• the predetermined amount of the aromatic polyisocyanate is in the range of 20 wt% to 40 wt%; and
• the predetermined amount of the solvent is in the range of 5 wt% to 20 wt%,
wherein the weight % of each ingredient is with respect to the total weight of the isocyanate component.
In an embodiment of the present disclosure, the polyaspartic ester amine is prepared in accordance with the present disclosure.
In an embodiment of the present disclosure, the amine component comprises a polyaspartic ester amine binder, optionally a primary amine, at least one filler, at least one defoamer and a mixture of plasticizers.
In an embodiment of the present disclosure, the primary amine is at least one selected from the group consisting of isophorone diamine (IPDA), bis-p-aminocyclohexymethane (PACM), and polyetheramine (Jefamine D2000 and Jefamine D230). In an exemplary embodiment of the present disclosure, the primary amine is Jefamine D-2000.
In an embodiment of the present disclosure, the filler is at least one selected from the group consisting of titanium dioxide, barium sulphate (Bartyes), calcium oxide, stearates, molecular sieve and micronized, highly porous, crystalline aluminosilicate. In an exemplary embodiment of the present disclosure, the filler is titanium dioxide and barium sulphate.
In an embodiment of the present disclosure, the defoamer is VOC-free silicone-containing defoamer (BYK 1799).
In an embodiment of the present disclosure, the plasticizer is at least one selected from the group consisting of a phthalate plasticizer and a non-phthalate plasticizer.
The phthalate plasticizer is diisononyl phthalate (DINP).
The non-phthalate plasticizer is selected from the group consisting of alkylsulfonic acid ester with phenol (ASE) (Mesamoll group), di(isononyl) cyclohexane-1,2-dicarboxylate (Hexamoll DINCH). In another exemplary embodiment of the present disclosure, the non-phthalate plasticizer is Mesamoll.
In an embodiment of the present disclosure, the isocyanate component comprises at least one aliphatic polyisocyanate, at least one aromatic polyisocyanate and a solvent.
In an embodiment of the present disclosure, the aliphatic polyisocyanate is selected from the group consisting of methylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate (HDI), 4-4’-dicyclohexylmethane diisocyanate (H12MDI) and methylene-bis(4-cyclohexylisocyanate) and their dimers, trimers and prepolymers. In an exemplary embodiment of the present disclosure, the aliphatic polyisocyanate is isophorone diisocyanate (IPDI).
In an embodiment of the present disclosure, the aromatic polyisocyanate is toluidine diisocyanate (TDI).
In an embodiment of the present disclosure, the isocyanate (NCO) content is in the range of 3 % to 8 %. In an exemplary embodiment of the present disclosure, the NCO content is 6%.
In an embodiment of the present disclosure, the isocyanate equivalent is in the range of 600 to 800. In an exemplary embodiment of the present disclosure, the isocyanate equivalent is 700.
In an embodiment of the present disclosure, the amine equivalent of the amine component (Part A of the coating composition) is in the range of 800 to 1700. In an exemplary embodiment of the present disclosure, the amine equivalent of the amine component is 909. In another exemplary embodiment of the present disclosure, the amine equivalent of the amine component is 1266.
In an embodiment of the present disclosure, the amine value of the amine component (Part A of the coating composition) is in the range of 40 to 75. In an exemplary embodiment of the present disclosure, the amine value is 44.31. In another exemplary embodiment of the present disclosure, the amine value is 63.71.
In an embodiment of the present disclosure, the solvent is selected from the group consisting of xylene, ortho-xylene and C9 naphtha. In an exemplary embodiment of the present disclosure, the solvent is ortho-xylene.
The process for the preparation of the polyaspartic ester amine binder and the coating composition thereof in accordance with the present disclosure is simple, economic and is convenient for industrial scale-up.
The coating composition of the present disclosure is prepared by mixing the amine component and the isocyanate component in a ratio in the range of 1:1 to 1:1.5.
The coating composition of the present disclosure can be used in water proofing applications.
The coating composition of the present disclosure can provide enhanced mechanical properties such as tensile strength, % elongation, crack bridging ability and the like and increased pot life for ease of application.
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 described in light of the following experiments which are set forth for illustration purposes only and not to be construed for limiting the scope of the disclosure. The following experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial scale.
EXPERIMENTAL DETAILS:
Experiment 1(A): Process for the preparation of a polyaspartic ester amine binder in accordance with the present disclosure
General procedure: The predetermined amounts of at least one primary amine, optionally a catalyst and an anhydride were mixed at 100 rpm, followed by adding a predetermined amount of at least one dialkyl ester over 3 hours through a peristaltic pump at 40 ºC to obtain a first mixture. The so obtained first mixture (after the complete addition of dialkyl maleate) was heated gradually to raise the temperature to 50 ºC, 60 ºC, 70 ºC and finally to 80 ºC to obtain the polyaspartic ester amine binder.
The polyaspartic ester amine binders were prepared in Examples E1 to E17 by following the general procedure as above. The predetermined amounts of the specific ingredients of the polyaspartic ester amine binder are as given in Table 1.
Table 1: Predetermined amounts (wt%) of the ingredients used in examples E1-E17
Ingredients and their function E1 E2 E3 E4 E5 E6 E7 E8 E9 E10
Sr. no. Materials Function/Broad class
1. PACM: bis-p-aminocyclohexymethane Primary amine 0 15.24 0 0 0 0 0 0 15 36.4
2. IPDA: isophorone diamine 35 0 15.24 32.8 32.8 29.4 30 18.4 18 0
3. D-2000 Jefamine 0 0 0 0 0 0 6.56 0 0 0
4. Benzyl amine 0 0 0 0 0 0 0 16.4 0 0
5. D-230- Jefamine 0 27.46 27.46 0 0 3.3 0 0 0 0
6. DEM: diethyl maleate Dialkyl ester 0 0 0 0 0 0 0 0 0 0
7. DBM: dibutyl maleate 65 54.3 54.3 66.7 66.45 66.8 62.94 65.2 67 62.4
8. DBTO: dibutyl tin oxide Catalyst 0 0 0 0 0 0 0 0 0 0
9. MA: maleic anhydride Anhydride 0 3 3 0.5 0.75 0.5 0.5 0 0 1.2
10. Amine value 220 182 185 191 184 187 193 187 182 175
11. Viscosity (Gardener scale) 160-200(G-H) 220-240 (I-J) 280-300 (K-L) 220-240 (I-J) 300-320 (L-M) 200-220 (H-I) 280-300 (K-L) 40 (A) 240-280 (J-K) 1000 (W)

Ingredients and their function E11 E12 E13 E14 E15 E16 E17
Sr. no. Materials Function
1. PACM: bis-p-aminocyclohexymethane Primary amine 36.4 23.44 23.4 35.7 40 36.4 35
2. IPDA: isophorone diamine 0 0 0 0 0 0 2.5
3. D-2000 Jefamine 0 0 0 0 0 0 0
4. Benzyl amine 0 0 0 0 0 0 0
5. D-230- Jefamine 0 0 0 0 0 0 0
6. DEM: diethyl maleate Dialkyl ester 0 0 76.58 64.28 60 12 44
7. DBM: dibutyl maleate 63.58 76.56 0 0 0 51.6 18.5
8. DBTO: dibutyl tin oxide Catalyst 0.02 0 0.02 0.02 0 0 0
9. MA: maleic anhydride Anhydride 0 0 0 0 0 0 0
10. Amine value 190 113 124 200 212 194 200
11. Viscosity in centipoise and in Gardener scale 460-500 centipoise (R-S) 60-80 (B-C) 40-60 (A-B) 550-600 (T-U) 900-1000 (V-W) 460-500 (R-S) 1000 (W)

Experiment 1 (B): Process for preparation of an amine component in accordance with the present disclosure
General procedure: The predetermined amounts of the polyaspartic ester amine binder as prepared in experiment 1 (A), optionally the primary amine and the filler were mixed in a reactor at 450 rpm in cowl stirrer for 15 minutes to obtain an intermediate amine mixture. The predetermined amounts of the defoamer and the mixture of plasticizers was added to the intermediate amine mixture at 450 rpm to obtain the amine component. The mixing was carried out in twin shaft high speed dispenser/high speed dispenser.
Experiment 1 (C): Process for preparation of an isocyanate component in accordance with the present disclosure
General procedure: An isocyanate component in accordance with the present disclosure was prepared in twin shaft high speed dispenser which was completely moisture free. Nitrogen was purged for 15 minutes before charging and continued up to the batch completion. The predetermined amounts of the aromatic polyisocyanate and the solvent were mixed in a reactor (dispenser) at 300 rpm for 40 minutes to obtain an intermediate isocyanate mixture. The predetermined amounts of the aliphatic polyisocyanate was added to the intermediate isocyanate mixture at 300 rpm for 30 minutes to obtain the isocyanate component.
Experiment 1 (D): Process for preparation of a coating composition in accordance with the present disclosure
General procedure: The so obtained amine component (as prepared in experiment 1 (B)) and the so obtained isocyanate component (as prepared in experiment 1 (C)) were mixed in 1:1.06 weight ratio to obtain the coating composition. The so obtained coating compositions showed good pot life and mechanical properties.
The coating compositions were prepared in Examples C1 to C10 by following the general procedure as above. The predetermined amounts of the specific ingredients of the coating composition (amine component+ isocyanate component) are as given in Table 1.
Table 2: Predetermined amounts of the ingredients of the amine component and the isocyanate component used in examples C1-C10
Ingredients and their function C1 C2 C3 C4 C5 C6 C7
Sr. no. Materials Function
PART A: An amine component
1. Polyaspartic ester amine binder of Example 11 of Example 11 of Example 11 of Example 4 of Example 4 of Example 4 of Example 13
14.41 14.41 14.41 15 15 15 15
2. D-2000-Jefamine Primary amine 0 0 0 5 0 3 0
3. Titanium dioxide, barium sulphate Filler 26.5 26.5 26.5 26.5 26.5 26.5 26.5
4. BYK 1799 Defoamer 0.46 0.46 0.46 0.46 0.46 0.46 0.46
5. DINP: Diisononyl phthalate Phthalate Plasticizer 0 8 4 0 0 0 0
6. Mesamoll Non- Phthalate Plasticizer 3 0 6 3 3 3 0
7. Amine value 61.7 55.44 53.3 62.3 63.71 62.9 44.31
8. Amine equivalent 909.23 1011.90 1052.53 900.48 880.55 891.89 1266.07
PART B: An isocyanate component
9. IPDI: Isophorone diisocyanate Aliphatic polyisocyanate 1.2 1.2 1.2 1.2 1.2 1.2 1.2
10. MDI and TDI: toluidine diisocyanate Aromatic polyisocyanate 31 31 31 31 31 31 31
11. Ortho xylene solvent 13 13 13 13 13 13 13
12. % NCO content 6 6 6 6 6 6 6
13. NCO equivalent 700 700 700 700 700 700 700
14. PART A: PART B 1:1.06 1:1.18 1:1.23 1:1.33 1:1.3 1:1.32 1:1.1

Ingredients and their function C8 C9 C10
Sr. no. Materials Function
PART A: An amine component
1. Polyaspartic ester amine binder of Example 13 of Example 13 of Example 14
15 11 14.41
2. D-2000-Jefamine Primary amine 3 3 0
3. Titanium dioxide, Barium sulphate (Bartyes) Filler 26.5 26.5 26.5
4. BYK 1799 Defoamer 0.46 0.46 0.46
5. DINP: Diisononyl phthalate Phthalate Plasticizer 6 6 8
6. Mesamoll Non- Phthalate Plasticizer 4 4 0
7. Amine value 36.55 47.43 68.8
8. Amine equivalent 1534.88 1182.79 815.40
PART B: An isocyanate component
9. IPDI: Isophorone diisocyanate Aliphatic polyisocyanate 1.2 1.2 1.2
10. MDI and TDI: toluidine diisocyanate Aromatic polyisocyanate 31 31 31
11. Ortho xylene solvent 13 13 13
12. % NCO content 6 6 6
13. NCO equivalent 700 700 700
14. PART A: PART B 1:1.13 1:38 1:21

Experiment 2: Characterization study of the coating composition in accordance with the present disclosure
(I) Physico-chemical properties analysis of a coating composition in accordance with the present disclosure
Composition C1 C2 C3 C4 C5 C6 C7 C8 C9 C10
% solids 85-92 85-92 85-92 85-92 85-92 85-92 85-92 85-92 85-92 85-92
Water Resistance (immersion test 4 h) Pass Pass Pass Pass Pass Pass Pass Pass Pass Pass
Chalking resistance Chalking after 350 hours Chalking after 350 hours Chalking after 350 hours Chalking after 350 hours Chalking after 350 hours Chalking after 350 hours Chalking after 350 hours Chalking after 350 hours Chalking after 350 hours Chalking after 350 hours
Ease of Application Good Good Good Good Good Good Good Good Good Good
Pot life 15 minutes 30 minutes 35 minutes 15 minutes 20 minutes 17 minutes 35 minutes 35 minutes 40 minutes 35 minutes
Mechanical properties
Tensile strength- Pull off Adhesion ( M.Pa) 13.34 9.5 8 8.2 7.6 8 5 5 6 5.5
Elongation at break (%EE) 342 540 560 400 380 385 400 400 350 360

From Table 2, it is observed that the physicochemical properties of the coating composition are as desired. Low amine value of the polyaspartic ester amine binder helps to achieve high pot life and low mechanical properties and with the higher amine value in the polyaspartic ester amine binder, pot life is less and high tensile properties. Therefore, the amine value is crucial in the polyaspartic ester amine binder.
The coating composition comprising polyaspartic ester amine binder of the present disclosure has good pot life which results in ease of application and good mechanical properties to the coat. The excess of isocyanate was required to adjust the pot life and mechanical properties. When the amine value is lower, the properties are lower and the pot life is higher and vice a versa. Furthermore, the use of phthalate plasticizer i.e. DINP helps in attaining good pot life.
The coating composition of the present disclosure can be applied through brush and roller applications on surfaces which is advantageous as compared to the polyurea applications that generally employs plural gun sprays due to the fast reaction of amine and isocyanate for high-performance coating applications.
TECHNICAL ADVANCEMENTS
The present disclosure described hereinabove has several technical advantages including, but not limited to, the realization of;
? a polyaspartic ester amine binder that:
• comprises both primary amine and secondary amine;
• reduces amount of plasticizer when used in a coating composition;
• avoids removal of excess dialkyl maleate; and
• produces a coating composition having enhanced mechanical properties (tensile strength, % elongation, crack bridging ability); and
? a process for the preparation of the polyaspartic ester amine that
• is simple, economic and environment friendly; 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 objects 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 ester amine binder is characterized by having
• an amine value in the range of 170 mg KOH/g to 220 mg KOH/g; and
• viscosity in the range of 160 centipoise to 1000 centipoise.
2. The polyaspartic ester amine binder as claimed in claim 1 being a reaction product of:
a. 10 wt% to 55 wt% of a primary amine; and
b. 45 wt% to 90 wt% of a dialkyl ester;
wherein said wt% of each ingredient is with respect to the total weight of said polyaspartic ester amine binder.
3. The polyaspartic ester amine binder as claimed in claim 2, wherein a mole ratio of said primary amine to said dialkyl ester is in the range of 1: 1.5 to 1:1.9.
4. The polyaspartic ester amine binder as claimed in claim 2, wherein
• said primary amine is at least one selected from the group consisting of isophorone diamine (IPDA), bis-p-aminocyclohexymethane (PACM), and polyetheramine; and
• said dialkyl ester is at least one selected from the group consisting of dibutyl maleate (DMB), diethyl maleate (DEM) and dioctyl maleate (DOM).
5. The polyaspartic ester amine binder as claimed in claim 1 is a primary amine terminated polyaspartic ester amine binder.
6. A coating composition comprising
A. an amine component comprising
a. a polyaspartic ester amine binder;
b. optionally a primary amine;
c. at least one filler;
d. at least one defoamer; and
e. a mixture of plasticizers,
B. an isocyanate component comprising
a. at least one aliphatic polyisocyanate;
b. at least one aromatic polyisocyanate; and
c. a solvent,
wherein a ratio of said amine component to said isocyanate component is in the range of 1:1 to 1:1.5.
7. The coating composition as claimed in claim 6, wherein said amine component comprises:
a. 5 wt% to 20wt% of said polyaspartic ester amine binder;
b. 0 wt% to 10 wt% of said primary amine;
c. 20 wt % to 35 wt % of said filler;
d. 0.1 wt % to 1 wt % of said defoamer; and
e. 2 wt % to 15 wt % of said mixture of plasticizers,
wherein said wt% of each ingredient is with respect to the total weight of said amine component.
8. The coating composition as claimed in claim 6, wherein said isocyanate component comprises:
a. 1 wt% to 10 wt% of said aliphatic polyisocyanate;
b. 20 wt% to 40 wt% of said aromatic polyisocyanate; and
c. 5 wt% to 20 wt% of said solvent,
wherein said wt% of each ingredient is with respect to the total weight of said isocyanate component.
9. The coating composition as claimed in claim 6, wherein said primary amine is at least one selected from the group consisting of isophorone diamine (IPDA), bis-p-aminocyclohexymethane (PACM), and polyetheramine.
10. The coating composition as claimed in claim 6, wherein said filler is at least one selected from the group consisting of titanium dioxide, barium sulphate, calcium oxide, stearates, molecular sieve and micronized , highly porous, crystalline aluminosilicate.
11. The coating composition as claimed in claim 6, wherein said defoamer is VOC-free silicone-containing defoamer.
12. The coating composition as claimed in claim 6, wherein said mixture of plasticizers is a mixture of a phthalate plasticizer and a non-phthalate plasticizer.
13. The coating composition as claimed in claim 6, wherein said aliphatic polyisocyanate is at least one selected from the group consisting of methylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate (HDI), 4-4’-dicyclohexylmethane diisocyanate (H12MDI) and methylene-bis(4-cyclohexylisocyanate) and their dimers, trimers and prepolymers.
14. The coating composition as claimed in claim 6, wherein said aromatic polyisocyanate is toluidine diisocyanate.
15. The coating composition as claimed in claim 6, wherein said solvent is selected from the group consisting of xylene, ortho-xylene and C9 naphtha.
16. The coating composition as claimed in claim 6, wherein said polyaspartic ester amine binder is characterized by having
• an amine value in the range of 170 mg KOH/g to 220 mg KOH/g; and
• viscosity in the range of 160 centipoise to 1000 centipoise.
17. The coating composition as claimed in claim 6, wherein said polyaspartic ester amine binder being a reaction product of:
a. 10 wt% to 55 wt% of a primary amine; and
b. 45 wt% to 90 wt% of a dialkyl ester,
wherein said wt% of each ingredient is with respect to the total weight of said polyaspartic ester amine binder.
18. The coating composition as claimed in claim 17, wherein a molar ratio of said primary amine to said dialkyl ester in said polyaspartic ester amine binder is in the range of 1:1.5 to 1:1.9.
19. The coating composition as claimed in claim 17, wherein
• said primary amine is at least one selected from the group consisting of isophorone diamine (IPDA), bis-p-aminocyclohexymethane (PACM), and polyetheramine; and
• said dialkyl ester is at least one selected from the group consisting of dibutyl maleate (DMB), diethyl maleate (DEM) and dioctyl maleate (DOM).
20. The coating composition as claimed in claim 12, wherein said phthalate plasticizer is diisononyl phthalate and said non-phthalate plasticizer is at least one selected from the group consisting of alkylsulfonic acid ester with phenol (ASE) (Mesamoll group) and di(isononyl) cyclohexane-1,2-dicarboxylate (Hexamoll DINCH).
21. A process for the preparation of a coating composition, wherein said process comprises the following steps:
A. preparing an amine component:
(i) charging a reactor with predetermined amounts of at least one primary amine, optionally a catalyst and an anhydride, followed by adding a predetermined amount of at least one dialkyl ester over a predetermined time period at a first predetermined temperature to obtain a first mixture; and heating said first mixture gradually to a second predetermined temperature to obtain said polyaspartic ester amine binder,
(i) mixing predetermined amounts of said polyaspartic ester amine binder, optionally a primary amine and a filler in a reactor at a stirring speed in the range of 300 rpm to 600 rpm for a time period in the range of 1 minute to 40 minutes to obtain an intermediate amine mixture;
(ii) mixing predetermined amounts of a defoamer and a mixture of plasticizers to said intermediate amine mixture at a stirring speed in the range of 300 rpm to 600 rpm to obtain said amine component,
B. preparing an isocyanate component:
(i) separately, sparging nitrogen in a reactor for a time period in the range of 5 minutes to 25 minutes, followed by mixing predetermined amounts of a solvent and an aromatic polyisocyanate at a stirring speed in the range of 100 rpm to 400 rpm for a time period in the range of 30 minute to 60 minutes to obtain an intermediate isocyanate mixture; and
(ii) mixing a predetermined amount of an aliphatic polyisocyanate to said intermediate isocyanate mixture for a time period in the range of 10 minutes to 40 minutes under said stirring speed in the range of 100 rpm to 400 rpm to obtain said isocyanate component,
C. mixing said amine component and said isocyanate component in a predetermined ratio to obtain said coating composition,
wherein said ratio of said amine component to said isocyanate component is in the range of 1:1 to 1:1.5.
22. The process as claimed in claim 21, wherein
• said predetermined amount of said polyaspartic ester amine binder is in the range of 5 wt% to 20 wt%;
• said predetermined amount of said primary amine is in the range of 0 wt% to 10 wt%;
• said predetermined amount of said filler is in the range of 20 wt% to 35 wt%;
• said predetermined amount of said defoamer is in the range of 0.1 wt% to 1 wt%; and
• said predetermined amount of said plasticizer is in the range of 2 wt% to 30 wt%,
wherein said wt % of each ingredient is with respect to the total weight of said amine component.
23. The process as claimed in claim 21, wherein
• said predetermined amount of said aliphatic polyisocyanate is in the range of 1 wt% to 10 wt%;
• said predetermined amount of said aromatic polyisocyanate is in the range of 20 wt% to 40 wt%; and
• said predetermined amount of said solvent is in the range of 5 wt% to 20 wt%,
wherein said wt % of each ingredient is with respect to the total weight of said isocyanate component.
24. The process as claimed in claim 21, wherein
• said primary amine is at least one selected from the group consisting of isophorone diamine (IPDA), bis-p-aminocyclohexymethane (PACM), and polyetheramine;
• said dialkyl ester is at least one selected from the group consisting of dibutyl maleate (DMB), diethyl maleate (DEM) and dioctyl maleate (DOM);
• said catalyst is selected from the group consisting of dibutyltin oxide and dibutyltin dilaurate; and
• said anhydride is maleic anhydride.
25. The process as claimed in claim 21, wherein
• said predetermined amount of said primary amine is in the range of 15 wt% to 50 wt%;
• said predetermined amount of said dialkyl ester is in the range of 45 wt% to 90 wt%;
• said predetermined amount of said catalyst is in the range of 0 wt% to 0.05 wt%; and
• said predetermined amount of said anhydride is in the range of 0 wt% to 5 wt%,
wherein said wt% of each ingredient is with respect to the total weight of said polyaspartic ester amine binder.
26. The process as claimed in claim 21, wherein
• said predetermined time period is in the range of 1 hour to 7 hours;
• said first predetermined temperature is in the range of 30 ºC to 45ºC; and
• said second predetermined temperature is in the range of 50 ºC to 90 ºC.
Dated this 29th day of November, 2023

_______________________________
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