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A Thickener Composition And Preparation Method Thereof

Abstract: ABSTRACT A THICKENER COMPOSITION AND PREPARATION METHOD THEREOF The present disclosure provides a water dispersible thickener composition 5 comprising: a reaction product of at least three polyols, at least one polyisocyanate, at least one modifying agent; and at least one capping agent, wherein the modifying agent has a pendant ionic group. The present disclosure further provides a process of preparing thickener composition, a clear coat formulation comprising the thickener composition, a pigmented latex paint formulation and a method for 10 thickening an aqueous composition. 23

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Patent Information

Application #
Filing Date
28 March 2024
Publication Number
40/2025
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
Parent Application

Applicants

ASIAN PAINTS LTD.
Research & Technology Center, Asian Paints Limited, C3-B1, TTC MIDC, Pawane Village, Turbhe, Navi Mumbai – 400703, India

Inventors

1. BANERJEE, Rakesh
C/O Asian Paints Limited, R&T Centre, Plot No C3-B/1 TTC MIDC Pawane, Thane - Belapur Road, Turbhe, Navi Mumbai, Maharashtra - 400 703, India
2. PAUL, Subham
C/O Asian Paints Limited, R&T Centre, Plot No C3-B/1 TTC MIDC Pawane, Thane - Belapur Road, Turbhe, Navi Mumbai, Maharashtra - 400 703, India
3. SHYAMROY, Subarna
C/O Asian Paints Limited, R&T Centre, Plot No C3-B/1 TTC MIDC Pawane, Thane - Belapur Road, Turbhe, Navi Mumbai, Maharashtra - 400 703, India

Specification

FORM 2
THE PATENTS ACT, 1970 (39 of 1970) & THE PATENTS RULES, 2003
COMPLETE SPECIFICATION (See section 10, rule 13)
1. Title of the invention: A THICKENER COMPOSITION AND PREPARATION METHOD
THEREOF
2. Applicant(s)
NAME NATIONALITY ADDRESS
ASIAN PAINTS LTD. Indian Research & Technology Center, Asian Paints Limited, C3-B1, TTC MIDC, Pawane Village, Turbhe, Navi Mumbai – 400703, India
3. Preamble to the description
COMPLETE SPECIFICATION
The following specification particularly describes the invention and the manner in which it
is to be performed.

FIELD OF INVENTION
[0001] The present disclosure broadly relates to a thickener composition. In particular, the present disclosure provides water dispersible thickener, and formulation comprising the thickener thereof.
BACKGROUND OF INVENTION
[0002] The surface of an object being exposed to harsh conditions such as sun, rain, ice, and wind, leads to wear and tear of the object. These harsh conditions lead to scratches or dents, rotting of wood, rust on metal articles, and cracking of cement objects. A commonly approached technique to extend the life of an article is by the application of a coating on the surface of such articles to block the direct exposure to these conditions. Surface coatings are specifically engineered for certain objects and/or conditions. Moreover, surface coatings are applied for decorative purposes to add color, lustre and finishing to an object. Thus, coatings serve two purposes, to protect and/or decorate an object.
[0003] Nowadays the application of surface coating has extended its arms into various realms by incorporation of thickeners or rheological additives in the coating compositions. The thickeners are those additives which can be added in a small amounts to increase the viscosity or consistency of a liquid or mixture. It further enhances and modifies the rheology of these coating systems and improves the coverage, application properties, paint’s viscosity, and prevents sagging. These systems can be selected from paints, protective/decorative/paper coatings, household detergents, cosmetics, personal care items, adhesives, sealants, inks, and drilling fluid.
[0004] EP0307775A2 discloses a water dispersible, modified polyurethane thickener which is the reaction product of polyisocyanate, polyether polyol, modifying agent containing at least one pendant hydrophobic group and at least two active hydrogen moieties and capping agent. The modified polyurethane may also

include a second type of modifying agent and does not have a pendant hydrophobic
group.
[0005] US005973063A discloses a polyurethane thickener especially suitable for
clear aqueous systems comprised of the reaction product of one or more
polyisocyanates, one or more polyether polyols, one or more branched capping
agents comprising a branched alcohol and additional one or more modifying agents
having at least two moieties reactive with component polyisocyanate or the
polyether polyol and at least one hydrophobic group.
[0006] US4079028 and US4155892 discloses thickeners prepared by reacting at
least one water soluble polyether polyol and a diisocyanate with at least one
monofunctional hydrophobic organic compound, usually an organic
monoisocyanate.
[0007] US4496708 discloses polyurethane thickeners for latex paints having
water-soluble comb-like polymers containing a few pendant internal hydrophobic
groups.
[0008] However, existing thickeners still face challenges in achieving complete
dispersion in water-based formulations, high shear viscosity and in maintaining
desired levelling. Further different thickeners are necessary for clear and pigmented
formulations. Accordingly, there is a need in the state of art to obtain thickeners to
overcome said shortcomings, to provide good dispersibility, higher thickening
efficiency, sag and levelling as well as suitable for both clear and pigmented
formulations.
SUMMARY OF THE INVENTION
[0009] In a first aspect of the present disclosure, there is provided a water
dispersible thickener composition comprising a reaction product of: a) at least three
polyols; b) at least one polyisocyanate; c) at least one modifying agent; and d) at
least one capping agent, wherein the modifying agent have a pendant ionic group
selected from a group consisting of dimethylol propionic acid, dimethylol butanoic
acid, 4-aminobenzenesulfonic acid, 1-amino-3-napthol-4-sulfonic acid, 2-
aminobenzenesulfonic acid, 3-amino-1-propanesulfonic acid, taurine, β-amino

acids, diaminobenzenesulfonic acid, 5,6-diamino-naphthalene-1-sulfonic acid, 3-phenylenediamine-4-sulfonic acid, 2,5-diaminobenzenesulfonic acid, 2-amino-5-(4-aminophenyl)benzenesulfonic acid, citric acid, tyrosine, hydroxybutyric acids, hydroxypropionic acids, and dihydroxy-butyric acid.
[00010] In a second aspect of the present disclosure, there is provided a method of preparing the water dispersible thickener composition as disclosed herein, the method comprising: (a) contacting at least one polyisocyanate and at least three polyols to form a reaction mixture; (b) contacting at least one capping agent, at least one modifying agent and the reaction mixture to obtain a first mixture; and (c) contacting the first mixture and a catalyst to obtain the water dispersible thickener composition.
[00011] In a third aspect of the present disclosure, there is provided a clear coat formulation comprising the thickener composition as disclosed herein. [00012] In a fourth aspect of the present disclosure, there is provided a pigmented latex paint formulation comprising the thickener composition as disclosed herein. [00013] In a fifth aspect of the present disclosure, there is provided a method for thickening an aqueous composition, the method comprising: contacting the thickener composition with the aqueous composition, wherein the aqueous composition is selected from a group consisting of a lacquer, a varnish, a paint, a putty, a thick coating, a waterproof coating, an ink, a slurry, and a paper coating color.
[00014] These and other features, aspects, and advantages of the present subject matter will be better understood with reference to the following appended claims and description. This summary is provided to introduce a selection of concepts in a simplified form. This summary is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used to limit the scope of the claimed subject matter.
DESCRIPTION OF THE INVENTION
[00015] Those skilled in the art will be aware that the present disclosure is subject
to variations and modifications other than those specifically described. It is to be

understood that the present disclosure includes all such variations and
modifications. The disclosure also includes all such steps, features, compositions,
and compounds referred to or indicated in this specification, individually or
collectively, and any and all combinations of any or more of such steps or features.
Definitions
[00016] For convenience, before further description of the present disclosure,
certain terms employed in the specification, and examples are delineated here.
These definitions should be read in the light of the remainder of the disclosure and
understood as by a person of skill in the art. The terms used herein have the
meanings recognized and known to those of skill in the art, however, for
convenience and completeness, particular terms and their meanings are set forth
below.
[00017] The articles “a”, “an” and “the” are used to refer to one or to more than one
(i.e., to at least one) of the grammatical object of the article.
[00018] The terms “comprise” and “comprising” are used in the inclusive, open
sense, meaning that additional elements may be included. It is not intended to be
construed as “consists of only”.
[00019] Throughout this specification, unless the context requires otherwise the
word “comprise”, and variations such as “comprises” and “comprising”, will be
understood to imply the inclusion of a stated element or step or group of elements
or steps but not the exclusion of any other element or step or group of elements or
steps.
[00020] The term “polyols” refers to compounds that contain multiple hydroxyl
groups. In thickener compositions, polyols can react with other components to form
urethane linkages, contributing to the formation of the polymer network. The
number of hydroxyl groups in a polyol can influence the crosslinking density of the
polymer network, and thus the properties of the thickener. For the purpose of the
present disclosure, the polyols include but are not limited to polyol 1, polyol 2 and
polyol 3, wherein the polyols are polyethylene glycols (PEG) having molecular
weight in a range of 200 – 600 g/mol, 2500-5000 g/mol and 7000-16000 g/mol
respectively.

[00021] The term “polyisocyanate” refers to compounds that contain multiple
isocyanate groups. These compounds generally obtained by the polymerization of
monomers with a highly reactive isocyanate functional group. For the purpose of
the present disclosure, the polyisocyanate include but are not limited 1,6-
hexamethylene diisocyanate (HDI), trimethyl-hexamethylene diisocyanate
(TMDI), isophorone diisocyanate, 1-isocyanato-3- isocyanatomethyl-3,5,5-
trimethylcyclohexane, 2,6- toluene diisocyanate, 2,4-toluene diisocyanate, 4,4’-
methylene diphenyl diisocyanate, 1,10-decamethylene diisocyanate, 1,4-
cyclohexylene diisocyanate, 1,5-naphthylene diisocyanate, 1,5-
tetrahydronaphthylene diisocyanate, and combinations thereof.
[00022] The term “modifying agent” refers to vital additives used in almost every coating and pigments to adjust the rheological characteristics. Apart from getting desired viscosity, these additives also help in controlling shelf stability, ease of application, open time/wet edge, and sagging. For the purpose of the present disclosure, the modifying agent include but are not limited to dimethylol propionic acid, dimethylol butanoic acid, 4-aminobenzoicsulfonic acid, 1-amino-3-napthol-4-sulfonic acid, 2-aminobenzenesulfonic acid, 3-amino-1-propanesulfonic acid, taurine, β-amino acids, diaminobenzenesulfonic acid, 5,6-diamino-naphthalene-1-sulfonic acid, 3-phenylenediamine-4-sulfonic acid, 2,5-diaminobenzenesulfonic acid, 2-amino-5-(4-aminophenyl)benzenesulfonic acid, citric acid, tyrosine, hydroxybutyric acids, hydroxypropionic acids, and dihydroxy-butyric acid. [00023] The term “capping agent” refers to the compounds which use to cap the ends of the polymer chain. This prevents further reaction of the chain ends. Additionally, the use of the capping agent reduces the toxicity of the polymer and, most importantly, increases the low shear viscosity efficiency. For the purpose of the present disclosure, the capping agent includes but is not limited to a branched aliphatic, cycloaliphatic, or aromatic compound having an amine or hydroxyl moiety.
[00024] The term “additive” refers to an add-on component in a specific composition. In an aspect of the present disclosure, the additive includes but are not

limited to a surfactant, a biocide, a solvent, an antifoaming agent, a pH regulator, a
coalescence agent, an encapsulating agent and combinations thereof.
[00025] The term “surfactant” refers to the compounds which can decrease the
surface tension or interfacial tension between two liquids, a liquid and a gas, or a
liquid and a solid.
[00026] The term “biocide” refers to the compounds that may be added to a coating
formulation to prevent the growth of microorganisms, such as bacteria and fungi.
This can enhance the shelf life and durability of the coating.
[00027] The term “solvent” refers to a liquid component of a solution or a reaction
mixture to enable the complete dispersal of a solute or reactant and thereby facilitate
the reaction.
[00028] The term “anti-foaming agent” refers to chemical additives which can help
to reduce or eliminate the formation of foam during the mixing and application of
the coating, which can improve the appearance and performance of the final
coating.
[00029] The term “pH regulator” refers to a chemical reagent which regulates or
maintains the pH of a reaction mixture or a system in a specific pH range.
[00030] The term “coalescent agents” refers to the compounds used in dispersion
paints to regulate the film formation process of the polymeric binder particles.
These agents also allow a solid film to form under unpropitious conditions. These
compounds soften the polymer, allowing a solid uniform continuous film as the
paint dries.
[00031] The term “reducing strength” or “tinting strength” refers to the property
related to colour strength of paint bases or coating formulations. It is checked by
adding colorant paste to evaluate the reduction in color strength of the final solution.
The higher the reducing strength, higher is the coloration which may be due to
flocculation. The lesser the reducing strength, lesser the flocculation indicating
clearer coating formulation. In an aspect of the present disclosure, the pigmented
latex or clear coat formulation comprising the thickener of the present disclosure
exhibits lesser reducing strength and hence provides a stable and clear coating
formulations without any flocculation.

[00032] Ratios, concentrations, amounts, and other numerical data may be presented herein in a range format. It is to be understood that such range format is used merely for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. [00033] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the disclosure, the preferred methods, and materials are now described. All publications mentioned herein are incorporated herein by reference.
[00034] As discussed in the background, commercially available or previously reported thickeners are not compatible for clear coating as well as for pigmented coating with respect to good rheological properties. Further there is a need for thickeners with superior efficiency in thickening aqueous compositions under high shear conditions with improved dispersing efficiency in pigmented paints with acceptable sag and levelling. Accordingly, the present disclosure provides a thickener composition as a reaction product of a combination of polyols, a modifying agent, and a capping agent with polyisocyanate. The reaction product is a modified polyurethane which is hydrophobic and has a pendant ionic group. The modifying agent has the pendant ionic group and reactive moieties capable of reacting with polyisocyanates. The present disclosure provides a thickener composition obtained from at least one polyisocyanate with high molecular weight of polyethylene glycol and a low molecular weight polyethylene glycol along with small molecule modifying agents having two or more hydroxy group with one ionic group and one or more long chain hydrophobic capping agent. The thickeners of the present disclosure exhibit high shear viscosity in a clear coat as well as pigmented composition. The thickeners are stable and has increased dispersibility of the pigment and extenders while still attaining acceptable levels of other important characteristics of the paints. The thickeners are water dispersible

modified polyurethane which additionally exhibits improved low shear viscosity
for a low to high PVC latex paint composition with acceptable paint stability.
[00035] The polyurethane thickeners of the present disclosure are reaction product
of: (a) at least three polyols; (b) at least one polyisocyanate; (c) at least one
modifying agent; and (d) at least one capping agent, wherein the modifying agent
have a pendant ionic group selected from a group consisting of dimethylol
propionic acid, dimethylol butanoic acid, 4-amino-3-sulfonic acid, 1-amino-3-
napthol-4-sulfonic acid, 4-aminobenzenesulfonic acid, 2-aminobenzenesulfonic
acid, 3-amino-1-propanesulfonic acid, taurine, β-amino acids, diamino
benzenesulfonic acid, 5,6-diamino-naphthalene-1-sulfonic acid, 3-
phenylenediamine-4-sulfonic acid, 2,5-diaminobenzenesulfonic acid, 2-amino-5-(4-aminophenyl)benzenesulfonic acid, citric acid, tyrosine, hydroxybutyric acids, hydroxypropionic acids, and dihydroxy-butyric acid.
[00036] The present disclosure demonstrates that the reaction between aliphatic isocyanates with high molecular weight of polyethylene glycol (PEG) and a low molecular weight polyethylene glycol with a small molecule having two or more hydroxy group with one ionic group and one or more long chain hydrophobic capping agent is useful for increasing viscosity of clear water-based system as well as having thickening efficiency in pigmented latex paints with improved dispersibility. The present disclosure also provides a thickener which has high thickening efficiency for a clear coating composition. The thickener has a capability to easily disperse in water in presence of water compatible solvents or non-ionic surfactants.
[00037] The present disclosure is not to be limited in scope by the specific embodiments described herein, which are intended for the purposes of exemplification only. Functionally equivalent products, compositions, and methods are clearly within the scope of the disclosure, as described herein.
[00038] In an embodiment of the present disclosure, there is provided a water dispersible thickener composition comprising a reaction product of: (a) at least three polyols; (b) at least one polyisocyanate; (c) at least one modifying agent; and (d) at least one capping agent, wherein the modifying agent have a pendant ionic group

selected from a group consisting of dimethylol propionic acid, dimethylol butanoic acid, 4-aminobenzenesulfonic acid, 1-amino-3-napthol-4-sulfonic acid, 2-aminobenzenesulfonic acid, 3-amino-1-propanesulfonic acid, taurine, β-amino acids, diaminobenzenesulfonic acid, 5,6-diamino-naphthalene-1-sulfonic acid, 3-phenylenediamine-4-sulfonic acid, 2,5-diaminobenzenesulfonic acid, 2-amino-5-(4-aminophenyl)benzenesulfonic acid, citric acid, tyrosine, hydroxybutyric acids, hydroxypropionic acids, and dihydroxy-butyric acid. In another embodiment of present disclosure, wherein the modifying agent is selected from dimethylol propionic acid, dimethylol butanoic acid or combinations thereof. In one another embodiment of present disclosure, the modifying agent is dimethylol propionic acid.
[00039] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the at least three polyols are a combination of polyol 1, polyol 2 and polyol 3.
[00040] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyol 1 is in a weight range of 0.4 to 0.8%(w/w), with respect to total weight of the thickener composition. In another embodiment of the present disclosure, the polyol 1 is in a weight range of 0.5 to 0.7%(w/w), with respect to total weight of the thickener composition.
[00041] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyol 1 has an average molecular weight in a range of 200 – 600 g/mol.
[00042] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyol 2 is in weight range of 60 to 75%(w/w), with respect to total weight of the thickener composition. In another embodiment of the present disclosure, the polyol 2 is in a weight range of 65 to 74%(w/w), with respect to total weight of the thickener composition.
[00043] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyol 2 has an average molecular weight in a range of 2500-5000 g/mol. In another embodiment of the present

disclosure, the polyol 2 has an average molecular weight in a range of 3000-5000 g/mol.
[00044] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyol 3 is in weight range of 12 to 20%(w/w), with respect to total weight of the thickener composition. In another embodiment of the present disclosure, the polyol 3 is in a weight range of 13 to 19%(w/w), with respect to total weight of the thickener composition.
[00045] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyol 3 has an average molecular weight in a range of 6000-16000 g/mol. In another embodiment of the present disclosure, wherein the polyol 3 has an average molecular weight in a range of 8000-10000 g/mol.
[00046] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyol 1 is selected from PEG-200, PEG-400 or PEG-600. In another embodiment of the present disclosure, the polyol 1 is PEG-400.
[00047] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyol 2 is selected from PEG- 2500, PEG -3350, or PEG-4000. In another embodiment of the present disclosure, the polyol 2 is PEG-4000.
[00048] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyol 3 is selected from PEG- 6000, PEG-8000, PEG-10000 or PEG-14000. In another embodiment of the present disclosure, the polyol 3 is PEG-8000.
[00049] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyisocyanate is selected from a group consisting of 1,6-hexamethylene diisocyanate (HDI), trimethyl-hexamethylene diisocyanate (TMDI), isophorone diisocyanate, 1-isocyanato-3-isocyanatomethyl-3,5,5-trimethylcyclohexane, 2,6-toluene diisocyanate, 2,4-toluene diisocyanate, 4,4’-methylene diphenyl diisocyanate, 1,10-decamethylene

diisocyanate, 1,4-cyclohexylene diisocyanate, 1,5-naphthylene diisocyanate, 1,5-tetrahydronaphthylene diisocyanate, and combinations thereof.
[00050] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyisocyanate is 1,6-hexamethylene diisocyanate (HDI), and trimethyl-hexamethylene diisocyanate (TMDI). [00051] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyisocyanate is in a weight range of 4 to 8%(w/w), with respect to total weight of the thickener composition. In another embodiment of the present disclosure, the polyisocyanate is in a weight range of 6 to 8%(w/w), with respect to total weight of the thickener composition. [00052] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the capping agent is selected from a group consisting of a branched aliphatic, cycloaliphatic, or aromatic compound having a hydroxyl or amine moiety.
[00053] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the capping agent is a branched alcohol or a branched amine having Formula I
R1
R2 (CH2)n CH2 —X
R3
wherein X is hydroxy(-OH) or amine(NH2);
R1 is selected from hydrogen, C1-C5 alkyl;
R2 is C4-C10 alkyl optionally substituted with -COOH or -SO3H;
R3 is C6-C20 alkyl optionally substituted with -COOH or -SO3H, and
n is an integer is selected from 0, 1, 2, or 3.
[00054] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the capping agent is a branched alcohol or amine has a carbon content in a range of 10 to 30. In another embodiment of the

present disclosure, the branched alcohol is selected from hexyl decanol, octyl dodecanol or combinations thereof.
[00055] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the capping agent is in a weight range of 0.2 to 6%(w/w), with respect to total weight of the thickener composition. In another embodiment of the present disclosure, the capping agent is in a weight range of 2 to 6%(w/w), with respect to total weight of the thickener composition. [00056] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the modifying agent is in a weight range of 0.1 to 4%, with respect to total weight of the thickener composition. In another embodiment of the present disclosure, the modifying agent is in a weight range of 0.1 to 1%, with respect to total weight of the thickener composition.
[00057] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyol is present in an amount ranging from 0.50 to 5.00 moles per mole of the polyisocyanate.
[00058] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the modifying agent is present in an amount ranging from 0.015 to 1.000 moles per mole of the polyisocyanate. [00059] In an embodiment of the present disclosure, there is provided a thickener composition as disclosed herein, wherein the polyisocyanate to polyols are in a weight ratio range of 1:1 to 1:20.
[00060] In an embodiment of the present disclosure, there is provided a method of preparing the water dispersible thickener composition as disclosed herein, the method comprising: (a) contacting at least one polyisocyanate and at least three polyols to form a reaction mixture; (b) contacting at least one capping agent, at least one modifying agent and the reaction mixture to obtain a first mixture; (c) contacting the first mixture with a catalyst to obtain the water dispersible thickener composition. In another embodiment of the present disclosure, the first mixture and the catalyst is mixed, and the mixture is stirred at a temperature of 120℃. [00061] In an embodiment of present disclosure, there is provided a method of preparing the water dispersible thickener composition as disclosed herein, wherein

the catalyst is selected from dibutyltin dilaurate (DBTDL), tin dioxalate, zinc acetate, lithium stearate, monobutyltin oxide (MBTO) or combinations thereof. In another embodiment of present disclosure, the catalyst is selected from dibutyltin dilaurate (DBTDL), tin dioxalate, or zinc acetate. In more embodiment of present disclosure, the catalyst is dibutyltin dilaurate (DBTDL).
[00062] In an embodiment of present disclosure there is provided a method of preparing the water dispersible thickener composition as disclosed herein, wherein the polyol should be moisture free prior to reacting with the polyisocyanate, modifying agent, and capping agent. In another embodiment of present disclosure, the polyol has moisture content of < 0.1%.
[00063] In an embodiment of the present disclosure, there is provided a clear coat formulation comprising the thickener composition as disclosed herein. [00064] In an embodiment of the present disclosure, there is provided there is provided a clear coat formulation comprising the thickener composition as disclosed herein, wherein the thickener composition is in a weight range of 0.3 to 0.7% with respect to the formulation.
[00065] In an embodiment of the present disclosure, there is provided a pigmented latex paint formulation comprising the thickener composition as disclosed herein. [00066] In an embodiment of the present disclosure, there is provided a pigmented latex paint formulation comprising the thickener composition as disclosed herein, wherein the thickener composition is in a weight range of 0.7 to 1.3% with respect to the formulation. In another embodiment of the present disclosure, the thickener composition is in a weight range of 0.9 to 1.2% with respect to the formulation. [00067] In an embodiment of the present disclosure, there is provided a pigmented latex paint formulation comprising the thickener composition as disclosed herein, wherein the formulation further comprises of at least one additive selected from a group consisting of a surfactant, a biocide, a solvent, an antifoaming agent, a pH regulator, a coalescence agent, an encapsulating agent, and combinations thereof. [00068] In an embodiment of the present disclosure, there is provided a method for thickening an aqueous composition, the method comprising: contacting the thickener composition as disclosed herein with an aqueous composition, wherein

the aqueous composition is selected from a group consisting of a lacquer, a varnish, a paint, a putty, a thick coating, a waterproof coating, an ink, a slurry, and a paper coating color.
[00069] Although the subject matter has been described in considerable detail with reference to certain examples and implementations thereof, other implementations are possible.
EXAMPLES
[00070] The disclosure will now be illustrated with working examples, which is intended to illustrate the working of disclosure and not intended to take restrictively to imply any limitations on the scope of the present disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood to one of ordinary skill in the art to which this disclosure belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice of the disclosed methods and compositions, the exemplary methods, devices, and materials are described herein. It is to be understood that this disclosure is not limited to particular methods, and experimental conditions described, as such methods and conditions may apply.
Example 1
Thickener composition
[00071] The thickener composition of the present disclosure is a reaction product of (a) polyol 1, polyol 2 and polyol 3, (b) polyisocyanates such as 1,6-hexamethylene diisocyanate (HDI) and trimethyl-hexamethylene diisocyanate (TMDI), (c) octyl dodecanol as capping agent and (d) 2,2-dimethylol propionic acid as modifying agent.
Method of preparing the thickener composition:
[00072] The water dispersible thickener composition (C1) was prepared by contacting 1,6-hexamethylene diisocyanate (HDI) (5.43 wt%) and trimethyl-hexamethylene diisocyanate (TMDI) 2.19 wt%) with mixture of polyols i.e., polyol 1 (PEG-400, 0.63 wt%), polyol 2 (PEG-4000, 67.83 wt%), and polyol 3 (PEG-8000,

17.98 wt%) to form a reaction mixture. 2-octyl-1-dodecanol (5.67 wt%) and 2,2-dimethylol propionic acid (0.25 wt%) were contacted with the reaction mixture which led to the formation of the first mixture. Dibutyltin laurate (catalyst) was added to the first mixture and the resulting mixture was stirred for at least 2 hours at 120 °C to form a solid polymer. About 20-35% of solid polymer was used and the desired thickener was obtained using water-solvent mixture. Butyldiglycol (BDG, co-solvent) to water was maintained at a volume ratio range of 1:3 to 1:5. Similarly wherever required surfactants were used and the anionic surfactant to water volume ratio was maintained at 1:3.
[00073] In order to obtain a stable thickener composition, it was observed that the polyols should be moisture-free. Accordingly, prior to mixing with polyisocyanate, the polyols were vacuumed at 120°C for more than 2 hours and were cooled to 50°C. Further, in the method of preparing the composition it was observed that any variation in temperature caused the thickener to gelate, hence the temperature of the preparation method was maintained at 120℃ to retain the flowability. [00074] In a similar manner composition (C2) was prepared without using any modifying agent.
Example 2
Determination of reducing strength (RS)
[00075] The reducing strength of thickener compositions was analysed by as per
ASTM E308, ASTM D387 and ISO 787 standards.
[00076] The reducing strength of composition (C1) and composition (C2) was
analyzed. It was observed that composition (C2) without DMPA exhibited a
reducing strength (RS) value of around 112-115 for pigmented systems while
composition (C1) with DMPA exhibited reducing strength (RS) value of around
100-101 which indicated that even without incorporation of any surfactant the
thickener of the present disclosure had tremendous pigment dispersion ability
which led to zero flocculation. The zero flocculation indicated the development of
clear coating on the surface.
Example 3

Preparation of clear coat and pigmented latex formulation
[00077] A pigmented latex formulation was prepared from the thickener composition of the present disclosure. The formulation was obtained by contacting thickener of Example 1 (1 wt%), water (16.45 wt%), dispersing agent (1.85 wt%), propylene glycol (2.75 wt%), titanium oxide and filler/extender (36.4 wt%), neutralizing agent (0.3 wt%), defoamer (0.3 wt%), in can stabilizer (0.85 wt%), coalescing agent (2 wt%), emulsion (38 wt%) and additives (0.2 wt%). [00078] A clear coat formulation was prepared from the thickener composition of the present disclosure. The formulation was obtained by adding thickener of Example 1 at 0.7% by weight with respect to the formulation. The thickener was mixed thoroughly. The formulation was then applied to a substrate and allowed to dry. The final clear coat formulation demonstrated excellent flow, levelling and sag resistance.
Example 4
Method of thickening of an aqueous composition
[00079] Thickening an aqueous composition was carried out by contacting the thickener of the present disclosure with an aqueous composition. Thickener of Example 1 was mixed with an aqueous composition such as a paint. The obtained paint provided desired levelling, sag, and flow properties. The aqueous composition is also selected from a lacquer, a varnish, a putty, a thick coating, a waterproof coating, an ink, a slurry, or a paper coating color.
ADVANTAGES OF THE PRESENT DISCLOSURE
[00080] The water dispersible thickener composition as disclosed in the present disclosure comprises modified polyurethanes. The thickener includes selected hydrophilic or hydrophobic segments using a specific mixture of polyols as co-reactant for the isocyanate component. The thickener of the present disclosure works for clear as well for pigmented latex paints systems. It has a well-balanced thickening action both in the low shear range and in the high shear range with

improved dispersibility of the pigment and extenders. It improves mid to high shear viscosity for low to high polyvinyl chloride paints, dispersibility of the pigments/extenders, tinter compatibility, flow levelling, sag resistance, brush applications, uniform coloring and stability improvement of paints. By selecting specific polyisocyanate, polyether polyols and branched capping agents, the properties of the thickener can be tailored to meet specific requirements of the paint formulation, such as desired reactivity, molecular weight, and hydrophobicity or hydrophilicity. The thickener of the present disclosure is easily dispersible in water in presence of water compatible solvents or non-ionic surfactants. The thickener of the present disclosure shows thickening efficiency with water due to intramolecular association and thickening efficiency within coating due to intermolecular association, hence suitable for clear coating composition. Advantageously the thickener of the present disclosure has unique ability of pigment dispersion, flocculation, and tinting/reducing strength improvement. The backbone of the composition itself acts as a surfactant due to pendant ionic group, which leads to improved pigment dispersion ability. The process for preparing the thickener composition is straightforward and involves readily available starting materials and conventional reaction conditions.
[00081] These advantages make the water dispersible thickener composition and coating formulation suitable for a wide range of applications, including but not limited to coatings, adhesives, and sealants, where performance and durability are of paramount concern.

I/We Claim:
1. A water dispersible thickener composition comprising a reaction product of:
(a) at least three polyols;
(b) at least one polyisocyanate;
(c) at least one modifying agent; and
(d) at least one capping agent,
wherein the modifying agent has a pendant ionic group selected from a group consisting of dimethylol propionic acid, dimethylol butanoic acid, 4-aminobenzenesulfonic acid, 1-amino-3-napthol-4-sulfonic acid, 2-aminobenzene sulfonic acid, 3-amino-1-propanesulfonic acid, taurine, β-amino acids, diamino benzenesulfonic acid, 5,6-diamino-naphthalene-1-sulfonic acid, 3-phenylenediamine-4-sulfonic acid, 2,5-diamino benzene sulfonic acid, citric acid, tyrosine, hydroxybutyric acids, hydroxypropionic acids, and dihydroxy-butyric acid.
2. The thickener composition as claimed in claim 1, wherein the at least three polyols are a combination of polyol 1, polyol 2 and polyol 3.
3. The thickener composition as claimed in claim 2, wherein the polyol 1 is in a weight range of 0.4 to 0.8% (w/w), with respect to total weight of the thickener composition.
4. The thickener composition as claimed in claim 2, wherein the polyol 1 has an average molecular weight in a range of 200 – 600 g/mol.
5. The thickener composition as claimed in claim 2, wherein the polyol 2 is in a weight range of 60 to 75% (w/w), with respect to total weight of the thickener composition.
6. The thickener composition as claimed in claim 2, wherein the polyol 2 has an average molecular weight in a range of 2500-5000 g/mol.
7. The thickener composition as claimed in claim 2, wherein the polyol 3 is in a weight range of 12 to 20% (w/w), with respect to total weight of the thickener composition.
8. The thickener composition as claimed in claim 2, wherein the polyol 3 has an average molecular weight in a range of 6000-16000 g/mol.

9. The thickener composition as claimed in claim 2, wherein the polyol 1 is selected from polyethylene glycol -200 (PEG-200), PEG-400 or PEG-600.
10. The thickener composition as claimed in claim 2, wherein the polyol 2 is selected from PEG- 2500, PEG-3350 or PEG-4000.
11. The thickener composition as claimed in claim 2, wherein the polyol 3 is selected from PEG- 6000, PEG-8000, PEG-10000 or PEG-14000.
12. The thickener composition as claimed in claim 1, wherein the polyisocyanate is selected from 1,6-hexamethylene diisocyanate (HDI), trimethyl-hexamethylene diisocyanate (TMDI), isophorone diisocyanate, 1-isocyanato-3-isocyanatomethyl-3,5,5-trimethylcyclohexane, 2,6- toluene diisocyanate, 2,4-toluene diisocyanate, 4,4’-methylene diphenyl diisocyanate, 1,10-decamethylene diisocyanate, 1,4-cyclohexylene diisocyanate, 1,5-naphthylene diisocyanate, 1,5-tetrahydronaphthylene diisocyanate, or combinations thereof.
13. The thickener composition as claimed in claim 1, wherein the polyisocyanate is in a weight range of 4 to 8% (w/w), with respect to total weight of the thickener composition.
14. The thickener composition as claimed in claim 1, wherein the capping agent is selected from a group consisting of a branched aliphatic, cycloaliphatic, or aromatic compound having an amine or hydroxyl moiety.
15. The thickener composition as claimed in claim 1, wherein the capping agent is a branched alcohol or a branched amine having Formula I
R1
R2 (CH2)n CH2 —X
R3
wherein X is hydroxy(-OH) or amine(NH2);
R1 is selected from hydrogen, or C1-C5 alkyl;
R2 is C4-C10 alkyl optionally substituted with -COOH or -SO3H;
R3 is C6-C20 alkyl optionally substituted with -COOH or -SO3H, and

n is an integer selected from 0 to 3.
16. The thickener composition as claimed in claim 15, wherein the branched alcohol or amine has a carbon content in a range of 10 to 30.
17. The thickener composition as claimed in claim 1, wherein the capping agent is in a weight range of 0.2 to 6% (w/w), with respect to total weight of the thickener composition.
18. The thickener composition as claimed in claim 1, wherein the modifying agent is in weight range of 0.1 to 4% (w/w), with respect to total weight of the thickener composition.
19. The thickener composition as claimed in claim 1, wherein the at least three polyol is present in an amount ranging from 0.50 to 5.00 moles per mole of the polyisocyanate.
20. The thickener composition as claimed in claim 1, wherein the at least one modifying agent is present in an amount ranging from 0.015 to 1.000 moles per mole of the polyisocyanate.
21. The thickener composition as claimed in claim 1, wherein the polyisocyanate to polyols are in weight ratio range of 1:1 to 1:20.
22. A method of preparing the water dispersible thickener composition as claimed in claim 1, the method comprising:

(a) contacting at least one polyisocyanate and at least three polyols to form a reaction mixture;
(b) contacting at least one capping agent, at least one modifying agent and the reaction mixture to obtain a first mixture; and
(c) contacting the first mixture with a catalyst to obtain the water dispersible thickener composition.

23. A clear coat formulation comprising the thickener composition as claimed in any one of the claims 1-21.
24. The clear coat formulation as claimed in claim 23, wherein the thickener composition is in a weight in a range of 0.3 to 0.7% with respect to the formulation.

25. A pigmented latex paint formulation comprising the thickener composition as claimed in any one of the claims 1-21.
26. The pigmented latex formulation as claimed in claim 25, wherein the thickener composition is in a weight in a range of 0.7 to 1.3% with respect to the formulation.
27. The formulation as claimed in any one of the claims 23-26, further comprising at least one additive selected from a group consisting of a surfactant, a biocide, a solvent, an antifoaming agent, a pH regulator, a coalescence agent, and an encapsulating agent.
28. A method for thickening an aqueous composition, the method comprising:
contacting the thickener composition as claimed in any one of the claims 1-21 with the aqueous composition,
wherein the aqueous composition is selected from a group consisting of a lacquer, a varnish, a paint, a putty, a thick coating, a waterproof coating, an ink, a slurry, and a paper coating color.

Documents

Application Documents

# Name Date
1 202421025332-STATEMENT OF UNDERTAKING (FORM 3) [28-03-2024(online)].pdf 2024-03-28
2 202421025332-POWER OF AUTHORITY [28-03-2024(online)].pdf 2024-03-28
3 202421025332-FORM 1 [28-03-2024(online)].pdf 2024-03-28
4 202421025332-DECLARATION OF INVENTORSHIP (FORM 5) [28-03-2024(online)].pdf 2024-03-28
5 202421025332-COMPLETE SPECIFICATION [28-03-2024(online)].pdf 2024-03-28
6 202421025332-Proof of Right [29-08-2024(online)].pdf 2024-08-29
7 202421025332-FORM 18 [18-08-2025(online)].pdf 2025-08-18