DESC:FIELD
The present disclosure relates to a paint formulation and a process for its preparation. Particularly, the present disclosure relates to a paint formulation based on isocyanate-free polyurethane technology for automotive refinish.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
Automotive refinish paints are used in automobiles for both protection and decoration purposes. Conventional automotive refinish paints use polyurethane intermediate as they are durable and perform well. However, the polyurethane intermediate uses a group of chemical compounds called isocyanates, which are toxic, moisture sensitive, causes skin irritation and asthma on prolonged exposure as it is hazardous to human health. Hence, there exists a need for alternate solutions to limit or eliminate the use of isocyanates. Isocyanate free polyurethane paint composition has sought to address the health and safety concerns stemming from isocyanates and their residuals.
The automotive body refinish units lacks facilities for heat-assisted curing and conventional polyurethane intermediate coat paint takes longer time (2-3 hours) to cure after primer application and time-to-buff (buffer time) for topcoat applications. Typical approaches of fast curing of the formulation may lead to a shorter pot life.
Therefore, there is, felt a need for a paint formulation that can mitigate the drawbacks mentioned hereinabove or at least provide a useful alternative.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows.
An object of the present disclosure is to ameliorate one or more problems of the prior art or to at least provide a useful alternative.
Another object of the present disclosure is to provide a paint formulation.
Still another object of the present disclosure is to provide a paint formulation for automotive refinish.
Yet another object of the present disclosure is to provide a paint formulation that is based on isocyanate-free polyurethane technology for automotive refinish.
Another object of the present disclosure is to provide a paint formulation that has low toxicity, quick repair, and energy saving technology.
Still another object of the present disclosure is to provide a paint formulation that cures at ambient temperature.
Yet another object of the present disclosure is to provide a process for the preparation of a paint formulation.
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 paint formulation. The paint formulation comprises a base composition (A) comprising at least one acetoacetate modified acrylic resin and at least one first excipient; and a cross-linker composition (B) comprising at least one ketimine modified acrylic resin and at least one second excipient.
The present disclosure further relates to a process for the preparation of a paint formulation. The process comprises the step of mixing predetermined amounts of at least one acetoacetate modified acrylic resin and at least one first excipient at a first predetermined conditions to obtain a base composition (A). Separately, predetermined amounts of at least one ketimine modified acrylic resin and at least one second excipient is mixed at second predetermined conditions to obtain a cross-linker composition (B). The base composition (A) and the cross-linker composition (B) are mixed in a mass ratio in the range of 1:1 to 3:1 to obtain the paint formulation.
DETAILED DESCRIPTION
The present disclosure relates to a paint formulation and a process for its preparation. Particularly, the present disclosure relates to a paint formulation based on isocyanate-free polyurethane technology for automotive refinish.
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.
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.
As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed elements.
Automotive refinish paints are used in automobiles for both protection and decoration purposes. Conventional automotive refinish paints use polyurethane intermediate as they are durable and perform well. However, the polymer uses a group of chemical compounds called isocyanates, which are toxic, moisture sensitive, causes skin irritation and asthma on prolonged exposure as it is hazardous to human health. Hence, there exists a need for alternate solutions to limit or eliminate the use of isocyanates. Isocyanate free polyurethane paint composition has sought to address the health and safety concerns stemming from isocyanates and their residuals.
The automotive body refinish units lacks facilities for heat-assisted curing and conventional polyurethane intermediate coat paint takes longer time (2-3 hours) to cure after primer application and time-to-buff (buffer time) for topcoat applications. Typical approaches of fast curing of the formulation may lead to a shorter pot life.
The present disclosure provides a paint formulation and a process for its preparation.
The present disclosure solves the problem of toxic effect of isocyanate by providing isocyanate free paint formulation that cures in a faster manner, that has high productivity, and is easily formulated as two component systems.
In an aspect, the present disclosure provides a paint formulation comprising:
a. a base composition (A) comprising:
i. at least one acetoacetate modified acrylic resin;
ii. at least one first excipient; and
b. a cross-linker composition (B) comprising:
i. at least one ketimine modified acrylic resin; and
ii. at least one second excipient.
In an embodiment of the present disclosure, the paint formulation comprises:
a. a base composition (A) comprising:
i. 20 mass% to 40 mass% of at least one acetoacetate modified acrylic resin;
ii. 60 mass% to 80 mass% of at least first excipient;
wherein the mass% of all the components is with respect to the total mass of the base composition (A); and
b. a cross-linker composition (B) comprising:
i. 15 mass% to 30 mass% of at least one ketimine modified acrylic resin; and
ii. 70 mass% to 85 mass% of at least one second excipient,
wherein the mass% of all the components is with respect to the total mass of the cross-linker composition (B).
In an embodiment of the present disclosure, a mass ratio of the base composition (A) to the crosslinking composition (B) is in the range of 1:1 to 3:1. In an exemplary embodiment of the present disclosure, the mass ratio of the base composition (A) to the crosslinking composition (B) is 2:1.
The specific mass ratio of the base composition (A) to the crosslinking composition (B) which is in the range of 1:1 to 3:1 is crucial in order to achieve the paint formulation having desirable properties such as lesser sanding time (25 to 30 minutes), quick repair property, optimum curing time and the like. If the mass ratio is less than 1:1, then the curing of the paint formulation is so fast that its pot life becomes too low. If the mass ratio is greater than 3:1, then the curing of the paint formulation is slow and it is not sandable within 25 to 30 minutes. Hence, the paint formulation is not usable for interior design purpose.
In an embodiment, the base composition (A) and the cross-linker composition (B) is mixed in a predetermined ratio, prior to application.
In accordance with the present disclosure, the acetoacetate modified acrylic resin can be selected from SETALUX 17-7202, SETAL 26-3705, SETALUX 17-1450 and SETALUX 57-7205. In accordance with an exemplary embodiment of the present disclosure, the acetoacetate modified acrylic resin (SETALUX 17-1450) is characterized by having a viscosity of Z2-Z4 Gardner Holdt (3500 cP to 6000 cP) and a density in the range of 8.3 ± 0.1 lbs/gal (994 kg/m3).
The predetermined amount of the acetoacetate modified acrylic resin is in the range of 20 mass% to 40 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the acetoacetate modified acrylic resin is 28 mass%.
In accordance with an embodiment of the present disclosure, the first excipient can be selected from the group consisting of:
• at least one dispersing agent;
• at least one rheological agent;
• at least one anti-settling sag controlling agent;
• at least one fluid medium;
• at least one anticorrosion pigment;
• at least one opacity enabler;
• at least one filler;
• at least one pigment;
• at least one binder;
• at least one surface tension modifying agent; and
a combination thereof.
The dispersing agent can be selected from BYK111 - copolymer with acidic group, BYK118 - linear polymer with highly polar, different pigment-affinic groups, BYK116 - high molecular weight, acrylate copolymer with pigment affinic groups, - solutions of high molecular weight block copolymers with pigment affinic groups such as BYK163, BYK161, BYK180-alkylolammonium salt of a copolymer with acidic groups, BYK2000-modified acrylate block copolymer, BYK2055- high molecular-weight, copolymer with pigment affinic groups, Additol XL 6577- low molecular weight resin and EFKA 5044 - unsaturated polyamide, and acid ester salts. In an exemplary embodiment of the present disclosure, the dispersing agent is BYK111 -copolymer with acidic group.
The predetermined amount of the dispersing agent is in the range of 0.2 mass% to 1 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the dispersing agent is 0.7 mass%.
The rheological agent can be selected from organic derivative of hectorite clay such as BENTONE 27, BENTONE 38, organic derivative of a bentonite clay such as BENTONE 52, BENTONE 34, BENTONE SD-1, BENTONE 57- modified bentonite clay, BENTONE SD-3 -organic derivative of a smectite clay (hectorite), BENTONE HD - highly beneficiated smectite clay, BENTONE –AD - Highly refined hectorite clay, and BENTONE-CT - untreated natural hectorite clay. In an exemplary embodiment of the present disclosure, the rheological agent is BENTONE 27 - organic derivative of hectorite clay.
The predetermined amount of the rheological agent is in the range of 0.5 mass% to 2 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the rheological agent is 1 mass%.
The anti-settling sag controlling agent can be selected from organic compound wax, M-P-A 1078 X, M-P-A 60X, M-P-A 1075, M-P-A 2000X, M-P-A 4020, THIXIN R- Non-hygroscopic organic derivative of castor oil, THIXIN E–Castor oil organic derivative, TIXOGEL MPZ- organoclay, CLAYTONE 40-Organophilic bentonite, and BENTOLITE L-10- calcium bentonite. In an exemplary embodiment of the present disclosure, the anti-settling sag controlling agent is M-P-A 1078 X. The anti-settling sag-controlling agents are highly efficient and are supplied as a soft paste dispersed in an organic solvent. These are chemically organic waxes.
The predetermined amount of the anti-settling sag controlling agent is in the range of 2 mass% to 6 mass% with respect to the total mass of the base composition (A). In an embodiment of the present disclosure, the amount of the anti-settling sag controlling agent is 4 mass%.
The fluid medium can be selected from acetate solvent, ethyl acetate, butyl acetate, methoxy propyl acetate, 3-methoxy butyl acetate, Iso-butyl acetate, ethyl glycol acetate, Iso propyl acetate, butyl glycol acetate, and ethyl carbitol acetate. In an exemplary embodiment of the present disclosure, the fluid medium is butyl acetate.
The predetermined amount of the fluid medium is in the range of 10 mass% to 15 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the fluid medium is 12 mass%.
The opacity enabler is titanium dioxide (TiO2). Titanium oxide can be selected from rutile titanium dioxide and anatase titanium dioxide pigment. In an exemplary embodiment of the present disclosure, the opacity enabler is titanium dioxide rutile BLR 601.
The predetermined amount of the opacity enabler is in the range of 3 mass% to 7 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the opacity enabler is 6 mass%.
The anticorrosion pigment can be selected from zinc phosphate complex and zinc oxide. In an exemplary embodiment of the present disclosure, the anticorrosion pigment is zinc phosphate.
The predetermined amount of the anticorrosion pigment is in the range of 2 mass% to 6 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the anticorrosion pigment is 4 mass%.
The filler can be selected from micro barytes, talc, and micronized calcite. In an exemplary embodiment of the present disclosure, the filler is a mixture of micro barytes 2 micron, steatite 90, and micronised calcite.
The predetermined amount of the filler is in the range of 5 mass% to 50 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, micro barytes 2 micron is present in an amount of 17 mass%, steatite 90 is present in an amount of 7 mass%, and micronised calcite is present in an amount of 15 mass%.
The micro barytes having particle size 2 microns improve the sandability of the paint and if other particle size is used then it affects the sanding property of the paint.
The pigment/colorant can be selected from carbon black and synthetic yellow oxide of iron. In an exemplary embodiment of the present disclosure, the pigment/colorant is a mixture of carbon black 2429G/600F and synthetic yellow oxide of iron.
The predetermined amount of the pigment/colorant is in the range of 0.1 mass% to 2 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, carbon black 2429G/600F is present in an amount of 0.05 mass% and synthetic yellow oxide of iron is present in an amount of 0.2 mass%.
The binder can be selected from modified thermoplastic resin, SETALUX 2120 XS 40 - Thermoplastic acrylic copolymer solution, SETALUX 2117 XS 30 - Thermoplastic acrylic copolymer solution, PARALOID B 99-Thermoplastic acrylic resin, SETALUX 17-1261 - Thermoplastic acrylic resin solution, SETALUX 17-1246- Thermoplastic acrylic resin solution, SETALUX 17-1265-Thermoplastic acrylic resin solution and SETALUX 2127 XX 60 - Thermoplastic acrylic resin. In an exemplary embodiment of the present disclosure, the binder is SETALUX 2120 XS 40.
The predetermined amount of the binder is in the range of 3 mass% to 7 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the binder is 5 mass%.
The surface tension modifying agent can be selected from a solution of polyether modified polydimethylsiloxane(BYK 300), polyester-modified polymethylalkylsiloxane (BYK 315) and polyether-modified polymethylalkylsiloxane (BYK 325). In an exemplary embodiment of the present disclosure, the surface tension modifying agent is BYK 300.
The predetermined amount of the surface tension modifying agent is in the range of 0.01 mass% to 1 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the surface tension modifying agent is 0.05 mass%.
In accordance with an exemplary embodiment of the present disclosure, the ketimine modified acrylic resin (SETALUX 10-1440) is characterized by having a viscosity of D-G Gardner Holdt (100 cP to 160 cP) and a density of 7.97 ± 0.1 lbs/gal (955 kg/m3).
The predetermined amount of the ketimine modified acrylic resin is in the range of 15 mass% to 30 mass% with respect to the total mass of the cross-linker composition (B). In an exemplary embodiment of the present disclosure, the amount of ketimine modified acrylic resin is 21 mass%.
In accordance with an embodiment of the present disclosure, the second excipient can be selected from:
• at least one acetate solvent;
• at least one ketonic solvent; and
• at least one alcoholic solvent.
The acetate solvent can be selected from ethyl acetate, butyl acetate, methoxy propyl acetate, 3-methoxy butyl acetate, iso-butyl acetate, ethyl glycol acetate, iso propyl acetate, butyl glycol acetate, and ethyl carbitol acetate. In an exemplary embodiment of the present disclosure, the acetate solvent is butyl acetate.
The predetermined amount of the acetate solvent is in the range of 10 mass% to 15 mass% with respect to the total mass of the cross-linker composition (B). In an exemplary embodiment of the present disclosure, the amount of the acetate solvent is 11 mass%.
The ketonic solvent can be selected from methyl amyl ketone, methyl iso butyl ketone (MIBK), Di-iso butyl ketone, methyl ethyl ketone, acetyl acetone, methyl propyl ketone, diethyl ketone, and cyclohexanone ketone. In an exemplary embodiment of the present disclosure, the ketone solvent is a mixture of methyl amyl ketone and methyl iso butyl ketone (M I B K).
The predetermined amount of the ketonic solvent is in the range of 40 mass% to 50 mass% with respect to the total mass of the cross-linker composition (B). In an exemplary embodiment of the present disclosure, methyl amyl ketone is present in an amount of 19 mass% and methyl iso butyl ketone (M I B K) is present in an amount of 24 mass%.
The alcoholic solvent can be selected from butanol, sec-butanol, iso-butanol, iso-propyl alcohol, ethanol, methanol and diacetone alcohol. In an exemplary embodiment of the present disclosure, the alcoholic solvent is butanol.
The predetermined amount of the alcoholic solvents is in the range of 20 mass% to 30 mass% with respect to the total mass of the cross-linker composition (B). In an exemplary embodiment of the present disclosure, the amount of the alcoholic solvent is 25 mass%.
In another aspect, the present disclosure provides a process for the preparation of a paint formulation.
The process comprises the following steps:
I. mixing at least one acetoacetate modified acrylic resin and at least one first excipient at first predetermined conditions to obtain a base composition (A);
II. separately, mixing at least one ketimine modified acrylic resin and at least one second excipient at second predetermined conditions to obtain a cross-linker composition (B); and
III. mixing the base composition (A) and the cross-linker composition (B) in a mass ratio in the range of 1:1 to 3:1 for a time period in the range of 1 minute to 5 minutes to obtain the paint formulation.
The process for preparation of the paint formulation is described in detail herein below.
STEP I: Preparation of the base composition (A):
In a first substep of step I, predetermined amounts of at least one acetoacetate modified acrylic resin, at least one dispersing agent, at least one rheological agent, at least one anti-settling sag control agent, and at least one fluid medium are mixed under stirring at a speed in the range of 300 rpm to 900 rpm for a time period in the range of 5 minutes to 15 minutes to obtain a first slurry.
In accordance with an exemplary embodiment of the present disclosure, the acetoacetate modified acrylic resin (SETALUX 17-1450) is characterized by having a viscosity of Z2-Z4 Gardner Holdt (3500 cP to 6000 cP) and a density in the range of 8.3 ± 0.1 lbs/gal (994 kg/m3).
The predetermined amount of the acetoacetate modified acrylic resin is in the range of 20 mass% to 40 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the acetoacetate modified acrylic resin is 28 mass%.
The dispersing agent can be selected from BYK111 - copolymer with acidic group, BYK118 - linear polymer with highly polar, different pigment-affinic groups, BYK116 - high molecular weight, acrylate copolymer with pigment affinic groups, - solutions of high molecular weight block copolymers with pigment affinic groups such as BYK163, BYK161, - BYK180-alkylolammonium salt of a copolymer with acidic groups, BYK2000-modified acrylate block copolymer, BYK2055- high molecular-weight, copolymer with pigment affinic groups, Additol XL 6577- low molecular weight resin and EFKA 5044 - unsaturated polyamide, and acid ester salts. In an exemplary embodiment of the present disclosure, the dispersing agent is BYK111 -copolymer with acidic group.
The predetermined amount of the dispersing agent is in the range of 0.2 mass% to 1 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the dispersing agent is 0.7 mass%.
The rheological agent can be selected from organic derivative of hectorite clay such as BENTONE 27, BENTONE 38, organic derivative of a bentonite clay such as BENTONE 52, BENTONE 34, BENTONE SD-1, BENTONE 57- modified bentonite clay, BENTONE SD-3 -organic derivative of a smectite clay (hectorite), BENTONE HD - highly beneficiated smectite clay, BENTONE –AD - Highly refined hectorite clay, and BENTONE-CT - untreated natural hectorite clay. In an exemplary embodiment of the present disclosure, the rheological agent is BENTONE 27 - organic derivative of hectorite clay.
The predetermined amount of the rheological agent is in the range of 0.5 mass% to 2 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the rheological agent is 1 mass%.
The anti-settling sag controlling agent can be selected from organic compound wax, M-P-A 1078 X, M-P-A 60X, M-P-A 1075, M-P-A 2000X, M-P-A 4020, THIXIN R- Non-hygroscopic organic derivative of castor oil, THIXIN E–Castor oil organic derivative, TIXOGEL MPZ- organoclay, CLAYTONE 40-Organophilic bentonite, and BENTOLITE L-10- calcium bentonite. In an exemplary embodiment of the present disclosure, the anti-settling sag controlling agent is M-P-A 1078 X.
The predetermined amount of the anti-settling sag controlling agent is in the range of 2 mass% to 6 mass% with respect to the total mass of the base composition (A). In an embodiment of the present disclosure, the amount of the anti-settling sag controlling agent is 4 mass%.
The fluid medium can be selected from acetate solvent, ethyl acetate, butyl acetate, methoxy propyl acetate, 3-methoxy butyl acetate, Iso-butyl acetate, ethyl glycol acetate, iso propyl acetate, butyl glycol acetate, and ethyl carbitol acetate. In an exemplary embodiment of the present disclosure, the fluid medium is butyl acetate.
The predetermined amount of the fluid media is in the range of 10 mass% to 15 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the fluid medium is 12 mass%.
In a second substep of step I, predetermined amounts of at least one opacity enabler, at least one anticorrosion pigment, at least one filler, and at least one pigment are added to the first slurry at a stirring speed in the range of 300 rpm to 700 rpm followed by raising the stirring speed in the range of 900 rpm to 1200 rpm for a time period in the range of 20 minutes to 50 minutes to obtain a second slurry.
The opacity enabler is titanium dioxide. Titanium dioxide can be selected from rutile titanium dioxide and anatase grade titanium dioxide pigment. In an exemplary embodiment of the present disclosure, the opacity enabler is titanium dioxide rutile BLR 601.
The predetermined amount of the opacity enabler is in the range of 3 mass% to 7 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the opacity enabler is 6 mass%.
The anticorrosion pigment can be selected from zinc phosphate complex and zinc oxide. In an exemplary embodiment of the present disclosure, the anticorrosion pigment is zinc phosphate.
The predetermined amount of the anticorrosion pigment is in the range of 2 mass% to 6 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the anticorrosion pigment is 4 mass%.
The filler can be selected from micro barytes, talc, and micronized calcite. In an exemplary embodiment of the present disclosure, the filler is a mixture of micro barytes 2 micron, steatite 90, and micronised calcite.
The predetermined amount of the filler is in the range of 5 mass% to 50 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, micro barytes 2 micron is present in an amount of 17 mass%, steatite 90 is present in an amount of 7 mass%, and micronised calcite is present in an amount of 15 mass%.
The pigment/colorant can be selected from carbon black and synthetic yellow oxide of iron. In an exemplary embodiment of the present disclosure, the pigment/colorant is a mixture of carbon black 2429G/600F and synthetic yellow oxide of iron.
The predetermined amount of the pigment/colorant is in the range of 0.1 mass% to 2 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, carbon black 2429G/600F is present in an amount of 0.05 mass% and the synthetic yellow oxide of iron is present in an amount of 0.2 mass%.
In a third substep of step I, the second slurry is ground in a sand mill by passing the slurry twice through grinding media to obtain a homogeneous slurry followed by flushing the sand mill with the fluid medium and the acetoacetate modified acrylic resin.
In an embodiment of the present disclosure, the flushing of the sand mill is carried out twice.
The grinding media in the sand mill is zinc silicate (ZrSiO3) having a particle size in the range of 1.0 mm to 1.2 mm. In an exemplary embodiment of the present disclosure, the grinding media has a particle size of 1.1 mm.
The slurry viscosity of the homogenous solution during grinding is in the range of 70 KU to 90 KU (560 cP to 1140 cP). In an exemplary embodiment of the present disclosure, the slurry viscosity of the homogenous solution during grinding is 80 KU (809 cP).
The sand mill grinding of the slurry is carried out at a temperature below 70 °C. In an exemplary embodiment of the present disclosure, the sand mill grinding of the slurry is carried out at 45°C.
The flow rate is in the range of 90 Kg/h to 110 Kg/h. In an exemplary embodiment of the present disclosure, the flow rate is 105 Kg/h.
In a fourth substep of Step I, the homogeneous slurry is mixed with predetermined amounts of the fluid medium, at least one binder, and at least one surface tension modifying agent under stirring at a speed in the range of 900 rpm to 1200 rpm for a time period in the range of 30 minutes to 60 minutes to obtain the base composition (A).
The binder can be selected from modified thermoplastic resin, SETALUX 2120 XS 40 - Thermoplastic acrylic copolymer solution, SETALUX 2117 XS 30 - Thermoplastic acrylic copolymer solution, PARALOID B 99-Thermoplastic acrylic resin, SETALUX 17-1261 - Thermoplastic acrylic resin solution, SETALUX 17-1246- Thermoplastic acrylic resin solution, SETALUX 17-1265-Thermoplastic acrylic resin solution and SETALUX 2127 XX 60 - Thermoplastic acrylic resin. In an exemplary embodiment of the present disclosure, the binder is SETALUX 2120 XS 40.
The predetermined amount of the binder is in the range of 3 mass% to 7 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the binder is 5 mass%.
The surface tension modifying agent can be selected from a solution of polyether modified polydimethylsiloxane, (BYK 300), polyester-modified polymethylalkylsiloxane (BYK 315) and polyether-modified polymethylalkylsiloxane (BYK 325). In an exemplary embodiment of the present disclosure, the surface tension modifying agent is SILICONE#BYK 300.
The predetermined amount of the surface tension modifying agent is in the range of 0.01 mass% to 1 mass% with respect to the total mass of the base composition (A). In an exemplary embodiment of the present disclosure, the amount of the surface tension modifying agent is 0.05 mass%.
STEP II: Preparation of a cross-linker composition (B):
In a substep of Step II, predetermined amounts of at least one ketimine modified acrylic resin and at least one acetate solvent, at least one ketonic solvent, and at least one alcoholic solvent are mixed under stirring at a speed in the range of 300 rpm to 900 rpm for a time period in the range of 30 minutes to 50 minutes to obtain the cross-linker composition (B).
In accordance with an exemplary embodiment of the present disclosure, the ketimine modified acrylic resin (SETALUX 10-1440) is characterized by having a viscosity of D-G Gardner Holdt (100 cP to 160 cP) and a density of 7.97 ± 0.1 lbs/gal (955 kg/m3).
The predetermined amount of the ketimine modified acrylic resin is in the range of 15 mass% to 30 mass% with respect to the total mass of the cross-linker composition (B). In an exemplary embodiment of the present disclosure, the amount of ketimine modified acrylic resin is 21 mass%.
The acetate solvent can be selected from ethyl acetate, butyl acetate, methoxy propyl acetate, 3-methoxy butyl acetate, iso-butyl acetate, ethyl glycol acetate, iso propyl acetate, butyl glycol acetate, and ethyl carbitol acetate. In an exemplary embodiment of the present disclosure, the acetate solvent is butyl acetate.
The predetermined amount of the acetate solvent is in the range of 10 mass% to 15 mass% with respect to the total mass of the cross-linker composition (B). In an exemplary embodiment of the present disclosure, the amount of the acetate solvent is 11 mass%.
The ketone solvent can be selected from methyl amyl ketone, methyl iso butyl ketone (MIBK), Di-iso butyl ketone, methyl ethyl ketone, acetyl acetone, methyl propyl ketone, diethyl ketone, and cyclohexanone ketone. In an exemplary embodiment of the present disclosure, the ketone solvent is a mixture of methyl amyl ketone and methyl iso butyl ketone (M I B K).
The predetermined amount of the ketone solvent is in the range of 40 mass% to 50 mass% with respect to the total mass of the cross-linker composition (B). In an exemplary embodiment of the present disclosure, methyl amyl ketone is present in an amount of 19 mass% and methyl iso butyl ketone (M I B K) is present in an amount of 24 mass%.
The alcoholic solvent can be selected from butanol, sec-butanol, iso-butanol, iso-propyl alcohol, ethanol, methanol and diacetone alcohol. In an exemplary embodiment of the present disclosure, the alcoholic solvent is butanol.
The predetermined amount of the alcoholic solvents is in the range of 20 mass% to 30 mass% with respect to the total mass of the cross-linker composition (B). In an exemplary embodiment of the present disclosure, the amount of the alcoholic solvent is 25 mass%.
STEP III: Preparation of a paint formulation:
The base composition (A) obtained in Step I and the cross-linker composition (B) obtained in Step II are manually mixed in a mass ratio in the range of 1:1 to 3:1 for a time period in the range of 1 minute to 5 minutes to obtain the paint formulation.
The present disclosure provides a low toxicity, quick repair (25-30 mins) and energy saving intermediate coat paint formulation based on isocyanate-free polyurethane technology that cures under ambient conditions for automotive refinish. The paint formulation of the present disclosure also has high productivity and higher performance that will cure in a much shorter time (25-30 mins) at room temperature as compared to those currently being used in the industry (2-3 hours). It does not require additional heating equipments such as UV lab for curing as compared to conventional products. Further, it is easily handled by the labourers hence, saves energy. The paint formulation of the present disclosure offers a faster return in terms of service and productivity as there is less material waste in the body refinish units.
The paint formulation of the present disclosure avoids the use of isocyanates, which are toxic, moisture sensitive, and hazardous to human health. Thus, the paint formulation of the present disclosure is safe and does not cause health hazards such as skin irritation and long-term asthma.
The paint formulation of the present disclosure has high productivity and higher performance in a much shorter time (25-30 mins) compared to those currently being used in the industry (2-3 hours).
The paint formulation of the present disclosure not only involves green chemistry but also avoids very hazardous substances, shortens the curing time and lowers the overall labor, thereby saving energy.
The process for the preparation of the paint formulation is simple and economical.
The foregoing description of the embodiments has been provided for purposes of illustration and not intended to limit the scope of the present disclosure. Individual components of a particular embodiment are generally not limited to that particular embodiment but are interchangeable. Such variations are not to be regarded as a departure from the present disclosure, and all such modifications are considered to be within the scope of the present disclosure.
The present disclosure is further described in light of the following experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. The following experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial scale.
EXPERIMENTAL DETAILS
Experiment 1: Process for the preparation of the paint formulation in accordance with the present disclosure
Example 1:
I) Preparation of a base composition (A):
28 grams of SETALUX 17-1450 (acetoacetate modified acrylic resin), 0.7 grams of BYK 111 (dispersing agent), 1 gram of BENTONE 27 paste (rheological agent), 4 grams of MPA-1078 X (anti-settling sag control agent) were mixed with 12 grams of butyl acetate (fluid medium) in a mixer under stirring at 600 rpm for 10 minutes to obtain a first slurry. 6 grams of titanium dioxide rutile BLR 601 (opacity enabler), 4 grams of zinc phosphate (anticorrosion pigment), 17 grams of micro barytes 2 micron (filler), 7 grams of Steatite 90 (filler), 15 grams of micronized calcite (filler), 0.05 grams of carbon black 2429G/600F (pigment) and 0.2 grams of synthetic yellow oxide of iron (pigment) were added to the first slurry at 400 rpm followed by raising the stirring speed to 1000 rpm for 35 minutes to obtain a second slurry. The second slurry was ground in a sand mill by passing the slurry twice through the grinding medium of sand mill to obtain a homogeneous slurry followed by flushing and cleaning the sand mill with the 1.5 grams of butyl acetate (fluid medium) and 2 grams of SETALUX 17-1450 (synthetic acetoacetate modified acrylic resin) to obtain a washing. The step of flushing and cleaning was repeated twice. The media used for grinding was ZrSiO3 (having particle size of 1.1 mm). The viscosity of the homogeneous slurry was 80 KU (809 cP). The process of sand mill grinding was carried out below 70 °C at a flow rate of 105 Kg/h. No. of passes was 2, H.G. (µ) 25, % charge 80%. The washings obtained from the step of mill flushing and cleaning were added to the homogenous solution under stirring at 400 rpm for 10 minutes to obtain a resultant homogeneous slurry. The resultant homogeneous slurry was mixed with 4 grams of butyl acetate (fluid medium), 5 grams of SETALUX 2120 XS 40 (binder), and 0.05 grams of SILICONE#BYK 300 (surface tension modifying agent) under stirring at 1000 rpm for 35 minutes to obtain the base composition (A). Viscosity of the base composition (A) was adjusted with butyl acetate (fluid medium) to 79 ± 3 KU (560 cP).
II) Preparation of a cross-linker composition (B):
21 grams of SETALUX 10-1440 (ketimine modified acrylic resin), 11 grams of butyl acetate (acetate solvent), 19 grams of methyl amyl ketone (ketonic solvent), 24 grams of methyl iso butyl ketone M I B K (ketonic solvent) and 25 grams of butanol (alcoholic solvent) were mixed under stirring at 400 rpm for 40 minutes below 60 °C to obtain the cross-linker composition (B).
III) Preparation of the paint formulation:
The so obtained base composition (A) in step I and the cross-linker composition (B) in step II were mixed manually by spatula in a mass ratio of 2:1 for a 2 minutes to obtain the paint formulation.
Example 2: Comparative Example
The same procedure of Example 1 was followed except the SETALUX 17-1450 was not added in the base composition and SETALUX 10-1440 was not added in the cross-linker composition to obtain a paint formulation. The paint formulation of the comparative example was used for comparative studies.
Example 3: Commercial paint formulation
A commercial paint formulation was used for comparative studies. The formulation of the commercial paint comprises a base composition (A) and a cross-linker composition (B) as given in Tables 1a and 1b.
Table 1a: Preparation of a base composition (A):
Base 'A' Part formulation
Sr. No. General Component Description Quantity (g)
1 Hydroxyl functional acrylic resin 28
2 Unsaturated polyamide 0.5
3 Organic derivative of hectorite clay 3
4 Organic compound wax 2
5 Aromatic hydrocarbon solvent 9
6 TiO2 Rutile 7
7 Micro barytes 21
8 Talc 10
9 Micronised calcite 19
10 PU Black Paints for color 0.5
TOTAL 100
Table 1b: Preparation of a cross-linker composition (B):
Hardener 'B' Part formulation
Sr. No. General Component Description Quantity (g)
1 Hexamethylene diisocyanate aliphatic based polyisocyanate 35
2 Hexamethylene diisocyanate trimer based polyisocyanate 32
3 Organic compound reagent (moisture scavenger ) 1
4 Acetate solvent 32
TOTAL 100
The base composition (A) and the cross-linker composition (B) were mixed manually by spatula in a mass ratio of 100:10 and 40% thinner for 2 minutes to obtain the paint formulation (commercial paint formulation).
Experiment 2: Characterization of the paint formulation of the present disclosure
The base composition (A) and the cross-linker composition (B) prepared in Experiment 1 were tested for their stability (normal stability- at 25 °C and accelerator stability at 60 °C). The stability data for the base composition (A) are summarized in the Tables 2a and 2b and the stability data for the cross-linker composition (B) are summarized in the Tables 3a and 3b.
Table 2a: Accelerator stability of base composition (A)
Stability data of base composition (A)
Accelerator Stability
Sr. No. Parameter Initial Incubator 60 °C for 10 Days Incubator 60 °C for 20 Days Incubator 60 °C for 30 Days
1 Settling No Settling No Settling No Settling No Settling
2 Viscosity Stormer (KU) Krebs units 80 KU 82 KU 83 KU 83 KU
3 Shade (Color) OK OK OK OK
4 HG (Hegman Gauge) 25 µm 25 µm 25 µm 25 µm
5 OK/NOT OK OK OK OK OK
Table 2b: Normal stability data of base composition (A)
Stability data of base composition (A)
Normal Stability (Room Temp)
Sr. No. Parameter Initial For 1 month For 3 months For 6 months For 9 months For 1 Year
1 Settling No Settling No Settling No Settling No Settling No Settling No Settling
2 Viscosity Stormer (KU) Krebs units 80 KU 82 KU 82 KU 82 KU 83 KU 83 KU
3 Shade (Color) OK OK OK OK OK OK
4 HG (Hegman Gauge) 25 µm 25 µm 25 µm 25 µm 25 µm 25 µm
5 OK/NOT OK OK OK OK OK OK OK
Table 3a: Accelerator stability data of cross-linker composition (B)
Stability data of cross-linker composition (B)
Accelerator Stability
Sr. No. Parameter Initial Incubator 40 °C for 10 Days Incubator 40 °C for 20 Days Incubator 40 °C for 30 Days
1 Settling No Settling No Settling No Settling No Settling
2 Viscosity on F/C B4 in Second) 12 12 12 13
3 Shade (Color) OK OK OK OK
4 OK/NOT OK OK OK OK OK
Table 3b: Normal stability data of cross-linker composition (B)
Stability data of cross-linker composition (B)
Normal Stability (Room Temp)
Sr. No. Parameter Initial For 1 month For 3 months For 6 months For 9 months For 1 Year
1 Settling No Settling No Settling No Settling No Settling No Settling No Settling
2 Viscosity Stormer (KU) Krebs units 12 12 12 12 12 13
3 Shade (Color) OK OK OK OK OK OK
4 OK/NOT OK OK OK OK OK OK OK
From the Tables 2a and 2b, it is observed that the base composition (A) has the accelerator stability at 60 °C for 30 days and has the normal stability at room temperature for 1 year. From the Tables 3a and 3b, it is observed that the cross-linker composition (B) has the accelerator stability at 40 °C for 30 days and has the normal stability at room temperature for 1 year. This indicates that the consistency of the base composition of the present disclosure will not change at room temperature for at least one year and even at 60 °C for at least 30 days and the cross-linker composition of the present disclosure will not change at room temperature for at least one year and even at 40 °C for at least 30 days.
Experiment 3: Performance study of the paint formulation of Experiment 1
A. The paint formulation prepared in accordance with Experiment 1 was tested for its performance by applying it on automobile body parts at two different auto refinish body shop. Table 4 below shows the details of the paint coats applied and the results observed.
Table 4: Performance test of the paint formulation of Experiment 1 and the commercial paint formulation
Paint formulation of Example 1 Example 3- Commercial paint formulation Example 2- paint formulation of the comparative example
1st place 2nd place
Mixing ratio By Volume By Volume By Volume By Volume
Part A 100 100 100 100
Part B 50 50 10 50
Part C Nil Nil 40 Nil
Color & Appearance Light Grey Light Grey Light Grey Light Grey
Number of Coat Application 2 Coat 2 Coat 2 coat 2 coat
Finishing Smooth & dry finish Smooth & dry finish Smooth & dry finish Not Good and Not upto the mark
Pinhole & other effect Nil Nil Nil Occurance of pinhole and other effects
Sanding Paper P320 followed by P400 P320 followed by P400 P320 followed by P400 P320 followed by P400
Sandability nature Powdery Powdery Powdery Does not cure and not sandable
Hiding power Excellent Excellent Excellent No hiding power
DFT (approximate) 45-48µ 45-48µ 45-48µ No uniform film formation
Sanding after 15 minute Sandable, no clogging Sandable, no clogging Sandable after 2 hours if sanding done before 2 hours not sandable and clogging on paper Paints does not cure and not sandable.
Not working
Sanding after 20 minute Sandable, no clogging Sandable, no clogging Not applicable Not applicable
Sanding after 30 minute Sandable, no clogging Sandable, no clogging Not applicable Not applicable
Sanding after 40 minute Sandable, no clogging Sandable, no clogging Not applicable Not applicable

Application Condition:-
Temperature: 26 °C 26 °C 26 °C 26 °C 26 °C
Humidity: 60% 60% 60% 60% 60%
Sanding Paper: - P320 (Machine Sanding) P320 followed by P400 P320 followed by P400 P320 followed by P400 P320 followed by P40
From Table 4, it is observed that the paint formulation of the present disclosure has lesser sanding time (within 25-30 minutes) as compared to the commercial paint formulation (2-3 hours), thereby saving time by 70-75 %. Further, the paint formulation of the present disclosure showed better properties such as drying, *sanding and *hiding as compared to the paint formulations of examples 2 and 3. The faint formulation of Example 2, wherein resin SETALUX 17-1450 and SETALUX 10-1440 are not present in the paint formulation, does not cure and dry, is not stable and settle at bottom of the paint container, is not sandable and many paints defects are seen on the paint film, paint application is not uniform and does not show performance properties such as adhesion, sanding, and the like. The fain formulation of Example 2 having such defects cannot be used for auto refinish paint system.
Hence, both the resins SETALUX 17-1450/ SETALUX 10-1440 are essential and important in the paint formulation to obtain the desired properties.
*sanding: The goal of sanding is to smooth down the surface, levelling the surface and to provide adhesion for the top coat.
*Hiding: Hiding power is the ability to hide the surface of an object. When applied too thin, a coating lacks sufficient hiding power. The hiding power of paint measures its ability to obscure a background of contrasting color. Hiding power is also known as opacity and contrast ratio.
B. Automobile body part (car door) initially coated/painted with polyester putty was used for the experiment. The paint formulation prepared in Experiment 1 was applied as intermediate coat paint formulation (primer) on the polyster putty coated car door. After curing of the paint formulation, a color base coat and a clear coat were applied on the automobile part. The time required for curing the various coats was measured and shown in Table 5.
Table 5: Dent Repair performance of the paint formulation of Example 1 and the commercial paint formulation
Dent Repair of Auto-Refinish Coatings-Time in Minutes
Products Commercial paint formulation
(Example 3) Paint formulation of Example 1 Comparative Paint formulation of Example 2
Polyester Putty 20-30 20-30 20-30
Primer 120-150 25-30 Does not cure and not working
Color Base Coat 10-15 10-15 10-15
Clear Coat 120-150 120-150 120-150
Total 270 175 Not acceptable
Total Time saving in % 35-40

The results of Table 5 showed that the time required for curing of the paint formulation of the present disclosure was 25 minutes to 30 minutes which is less as compared to the paint formulations of Examples 2and 3. Hence, it saves overall time by 35% to 40% for the entire process of dent repair thereby, enhancing the productivity and the properties such as drying, sanding and hiding.
TECHNICAL ADVANCEMENTS
The present disclosure described herein above has several technical advantages including, but not limited to, the realization of;
? a paint formulation for automotive finish that:
• is isocyanate-free;
• has low toxicity;
• has quick repair ability;
• is energy saving intermediate coat; and
• cures under ambient conditions.
? a process for the preparation of a paint formulation that;
• is simple and economical.
Throughout this specification, the word “comprise”, or variations such as “comprises” or “comprising, will be understood to imply the inclusion of a stated element, integer or step,” or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or results. While certain embodiments of the inventions have been described, these embodiments have been presented by way of example only, and are not intended to limit the scope of the inventions. Variations or modifications to the formulation of this invention, within the scope of the invention, may occur to those skilled in the art upon reviewing the disclosure herein. Such variations or modifications are well within the spirit of this invention.
The numerical values given for various physical parameters, dimensions and quantities are only approximate values and it is envisaged that the values higher than the numerical value assigned to the physical parameters, dimensions and quantities fall within the scope of the invention unless there is a statement in the specification to the contrary.
While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated that many additional features can be added and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation. ,CLAIMS:WE CLAIM:
1. A paint formulation comprising:
a. a base composition (A) comprising:
- at least one acetoacetate modified acrylic resin; and
- at least one first excipient; and
b. a cross-linker composition (B) comprising:
- at least one ketimine modified acrylic resin; and
- at least one second excipient.
2. The formulation as claimed in claim 1, wherein
a) said base composition (A) comprises:
i. 20 mass% to 40 mass% of said acetoacetate modified acrylic resin; and
ii. 60 mass% to 80 mass% of said first excipient,
wherein the mass% is with respect to the total mass of the base composition (A); and
b) said cross-linker composition (B) comprises:
i. 15 mass% to 30 mass% of said ketimine modified acrylic resin; and
ii. 70 mass% to 85 mass% of said second excipient,
wherein the mass% is with respect to the total mass of the cross-linker composition (B).
3. The formulation as claimed in claim 1, wherein a mass ratio of said base composition (A) to said cross-linker composition (B) is in the range of 1:1 to 3:1.
4. The formulation as claimed in claims 1 and 2, wherein said first excipient is selected from the group consisting of:
i. at least one dispersing agent;
ii. at least one rheological agent;
iii. at least one anti-settling sag controlling agent;
iv. at least one fluid medium;
v. at least one anticorrosion pigment;
vi. at least one opacity enabler;
vii. at least one filler;
viii. at least one pigment;
ix. at least one binder;
x. at least one surface tension modifying agent; and
a combination thereof.
5. The formulation as claimed in claim 4, wherein said dispersing agent is at least one selected from the group consisting of copolymer with acidic group (BYK111), linear polymer with highly polar, different pigment-affinic groups (BYK118), high molecular weight, acrylate copolymer with pigment affinic groups (BYK116), solutions of high molecular weight block copolymers with pigment affinic groups (BYK161, BYK163), alkylolammonium salt of a copolymer with acidic groups (BYK180), modified acrylate block copolymer (BYK2000), high molecular-weight, copolymer with pigment affinic groups (BYK2055), low molecular weight resin (Additol XL 6577), and unsaturated polyamide and acid ester salts (EFKA 5044); and wherein said dispersing agent is present in an amount in the range from 0.2 mass% to 1 mass% with respect to the total mass of said base composition (A).
6. The formulation as claimed in claim 4, wherein said rheological agent is at least one selected from the group consisting of organic derivative of hectorite clay, organic derivative of bentonite clay, modified bentonite clay, organic derivative of smectite clay, highly beneficiated smectite clay, highly refined hectorite clay, and untreated natural hectorite clay; and wherein said rheological agent is present in an amount in the range from 0.5 mass% to 2 mass% with respect to the total mass of said base composition (A); and
wherein said anti-settling sag controlling agent is at least one selected from the group consisting of organic compound wax, non-hygroscopic organic derivative of castor oil (THIXIN R), Castor oil organic derivative (THIXIN E), organoclay (TIXOGEL MPZ), organophilic bentonite (CLAYTONE 40), and calcium bentonite (BENTOLITE L-10); and wherein said anti-settling sag controlling agent is present in an amount in the range of 2 mass% to 6 mass% with respect to the total mass of said base composition (A).
7. The formulation as claimed in claim 4, wherein said fluid medium is at least one selected from the group consisting of ethyl acetate, butyl acetate, methoxy propyl acetate, 3-methoxy butyl acetate, iso-butyl acetate, ethyl glycol acetate, iso propyl acetate, butyl glycol acetate, and ethyl carbitol acetate; and wherein said fluid medium is present in an amount in the range of 10 mass% to 15 mass% with respect to the total mass of said base composition (A); and
wherein said opacity enabler is titanium dioxide; and wherein said opacity enabler is present in an amount in the range of 3 mass% to 7 mass% with respect to the total mass of said base composition (A).
8. The formulation as claimed in claim 4, wherein said anticorrosion pigment is at least one selected from the group consisting of zinc phosphate complex and zinc oxide; and wherein said anticorrosion pigment is present in an amount in the range of 2 mass% to 6 mass% with respect to the total mass of said base composition (A); and
wherein said filler is at least one selected from the group consisting of microbarytes, talc, and micronized calcite; and wherein said filler is present in an amount in the range of 5 mass% to 50 mass% with respect to the total mass of said base composition (A).
9. The formulation as claimed in claim 4, wherein said pigment is at least one selected from the group consisting of carbon black, and synthetic yellow oxide of iron; and wherein said pigment is present in an amount in the range from 0.1 mass% to 2 mass% with respect to the total mass of said base composition (A);
wherein said binder is at least one selected from the group consisting of thermoplastic acrylic copolymer solution, and thermoplastic acrylic resin solution; and wherein said binder is present in an amount in the range from 3 mass% to 7 mass% with respect to the total mass of said base composition (A); and
wherein said surface tension modifying agent is at least one selected from the group consisting of solution of polyether-modified polydimethylsiloxane (BYK 300), polyester-modified polymethylalkylsiloxane (BYK 315) and polyether-modified polymethylalkylsiloxane (BYK 325); and wherein said surface tension modifying agent is present in an amount in the range from 0.01 mass% to 1 mass% with respect to the total mass of said base composition (A).
10. The formulation as claimed in claims 1 and 2, wherein said second excipient is selected from the group consisting of:
i. at least one acetate solvent;
ii. at least one ketonic solvent; and
iii. at least one alcoholic solvent.
11. The formulation as claimed in claim 10, wherein said acetate solvent is at least one selected from the group consisting of ethyl acetate, butyl acetate, methoxy propyl acetate, 3-methoxy butyl acetate, iso-butyl acetate, ethyl glycol acetate, iso propyl acetate, butyl glycol acetate, and ethyl carbitol acetate; and wherein said acetate solvent is present in an amount in the range of 10 mass% to 15 mass% with respect to the total mass of said cross-linker composition (B);
wherein said ketonic solvent is at least one selected from the group consisting of methyl amyl ketone, methyl iso butyl ketone (MIBK), Di-iso butyl ketone, methyl ethyl ketone, acetyl acetone, methyl propyl ketone, diethyl ketone, and cyclohexanone ketone; and wherein said ketonic solvent is present in an amount in the range of 40 mass% to 50 mass% with respect to the total mass of said cross-linker composition (B); and
wherein said alcoholic solvent is at least one selected from the group consisting of butanol, sec-butanol, iso-butanol, iso-propyl alcohol, ethanol, methanol, and diacetone alcohol; and wherein said alcoholic solvent is present in an amount in the range of 20 mass% to 30 mass% with respect to the total mass of said cross-linker composition (B).
12. A process for the preparation of a paint formulation, said process comprising the following steps:
I. mixing at least one acetoacetate modified acrylic resin and at least one first excipient at first predetermined conditions to obtain a base composition (A);
II. separately, mixing at least one ketimine modified acrylic resin and at least one second excipient at second predetermined conditions to obtain a cross-linker composition (B); and
III. mixing said base composition (A) and said cross-linker composition (B) in a mass ratio in the range of 1:1 to 3:1 for a time period in the range of 1 minute to 5 minutes to obtain the paint formulation.
13. The process as claimed in claim 12, wherein said base composition (A) is prepared by the following substeps:
(i) mixing predetermined amounts of at least one acetoacetate modified acrylic resin, at least one dispersing agent, at least one rheological agent, at least one anti-settling sag control agent, and at least one fluid medium under stirring at a speed in the range of 300 rpm to 900 rpm for a time period in the range of 5 minutes to 15 minutes to obtain a first slurry;
(ii) adding predetermined amounts of at least one opacity enabler, at least one anticorrosion pigment, at least one filler, and at least one pigment to said first slurry at a stirring speed in the range of 300 rpm to 700 rpm followed by raising the stirring speed in the range of 900 rpm to 1200 rpm for a time period in the range of 20 minutes to 50 minutes to obtain a second slurry;
(iii) grinding said second slurry in a sand mill to obtain a homogeneous slurry; and
(iv) mixing said homogeneous slurry with predetermined amounts of said fluid medium, at least one binder, and at least one surface tension modifying agent under stirring at a speed in the range of 900 rpm to 1200 rpm for a time period in the range of 30 minutes to 60 minutes to obtain said base composition (A).
14. The process as claimed in claim 12, wherein said cross-linker composition (B) is prepared by mixing predetermined amounts of at least one ketimine modified acrylic resin, at least one acetate solvent, at least one ketonic solvent, and at least one alcoholic solvent under stirring at a speed in the range of 300 rpm to 900 rpm for a time period in the range of 30 minutes to 50 minutes to obtain said cross-linker composition (B).
15. The process as claimed in claim 13, wherein said dispersing agent is at least one selected from the group consisting of copolymer with acidic group (BYK111), linear polymer with highly polar, different pigment-affinic groups (BYK118), high molecular weight, acrylate copolymer with pigment affinic groups (BYK116), solutions of high molecular weight block copolymers with pigment affinic groups (BYK161), solutions of high molecular weight block copolymers with pigment affinic groups (BYK163), alkylolammonium salt of a copolymer with acidic groups (BYK180), modified acrylate block copolymer (BYK2000), high molecular-weight, copolymer with pigment affinic groups (BYK2055), low molecular weight resin (Additol XL 6577), and unsaturated polyamide and acid ester salts (EFKA 5044); and wherein said dispersing agent is present in an amount in the range of 0.2 mass% to 1 mass% with respect to the total mass of said first excipient.
16. The process as claimed in claim 13, wherein said rheological agent is at least one selected from the group consisting of organic derivative of hectorite clay, organic derivative of a bentonite clay, modified bentonite clay, organic derivative of a smectite clay, highly beneficiated smectite clay, highly refined hectorite clay, and untreated natural hectorite clay; and wherein said rheological agent is present in an amount in the range of 0.5 mass% to 2 mass% with respect to the total mass of said first excipient; and
wherein said anti-settling sag controlling agent is at least one selected from the group consisting of organic compound wax, non-hygroscopic organic derivative of castor oil (THIXIN R), Castor oil organic derivative (THIXIN E), organoclay (TIXOGEL MPZ), organophilic bentonite (CLAYTONE 40), and calcium bentonite (BENTOLITE L-10); and wherein said anti-settling sag controlling agent is present in an amount in the range of 2 mass% to 6 mass% with respect to the total mass of said base composition (A).
17. The process as claimed in claim 13, wherein said fluid medium is at least one selected from the group consisting of ethyl acetate, butyl acetate, methoxy propyl acetate, 3-methoxy butyl acetate, Iso-butyl acetate, ethyl glycol acetate, Iso propyl acetate, butyl glycol acetate, and ethyl carbitol acetate; and wherein said fluid medium is present in an amount in the range of 10 mass% to 15 mass% with respect to the total mass of said base composition (A); and
wherein said opacity enabler is titanium dioxide; and wherein said opacity enabler is present in an amount in the range of 3 mass% to 7 mass% with respect to the total mass of said first excipient.
18. The process as claimed in claim 13, wherein said anticorrosion pigment is at least one selected from the group consisting of zinc phosphate complex and zinc oxide; and wherein said anticorrosion pigment is present in an amount in the range of 2 mass% to 6 mass% with respect to the total mass of said base composition (A); and
wherein said filler is at least one selected from the group consisting of microbarytes, talc, and micronized calcite; and wherein said filler is present in an amount in the range of 5 mass% to 50 mass% with respect to the total mass of said base composition (A).
19. The process as claimed in claim 13, wherein said pigment is at least one selected from the group consisting of carbon black, and synthetic yellow oxide of iron; and wherein said pigment is present in an amount in the range of 0.1 mass% to 2 mass% with respect to the total mass of said base composition (A);
wherein said binder is at least one selected from the group consisting of thermoplastic acrylic copolymer solution, and thermoplastic acrylic resin solution; and wherein said binder is present in an amount in the range of 3 mass% to 7 mass% with respect to the total mass of said base composition (A); and
wherein said surface tension modifying agent is at least one selected from the group consisting of solution of polyether modified polydimethylsiloxane (BYK 300), polyester-modified polymethylalkylsiloxane (BYK 315) and polyether-modified polymethylalkylsiloxane (BYK 325); and wherein said surface tension modifying agent is present in an amount in the range of 0.01 mass% to 1 mass% with respect to the total mass of said base composition (A).
20. The process as claimed in claim 14, wherein said acetate solvent is at least one selected from the group consisting of ethyl acetate, butyl acetate, methoxy propyl acetate, 3-methoxy butyl acetate, Iso-butyl acetate, ethyl glycol acetate, Iso propyl acetate, butyl glycol acetate, and ethyl carbitol acetate; and wherein said acetate solvent is present in an amount in the range of 10 mass% to 15 mass% with respect to the total mass of said cross-linker composition (B);
wherein said ketonic solvent is at least one selected from the group consisting of methyl amyl ketone, methyl iso butyl ketone (MIBK), Di-iso butyl ketone, methyl ethyl ketone, acetyl acetone, methyl propyl ketone, diethyl ketone, and cyclohexanone ketone; and wherein said ketonic solvent is present in an amount in the range of 40 mass% to 50 mass% with respect to the total mass of said cross-linker composition (B); and
wherein said alcoholic solvent is at least one selected from the group consisting of butanol, sec-butanol, iso-butanol, iso-propyl alcohol, ethanol, methanol, and diacetone alcohol; and wherein said alcoholic solvent is present in an amount in the range of 20 mass% to 30 mass% with respect to the total mass of said cross-linker composition (B).

Dated this 04th day of October, 2022

_______________________________
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