Self cross-linking grouting composition

Abstract

The present invention disclosed relates to a self cross-linking grouting composition developed to enhance cost-effectiveness without compromising performance by adapting an alternative alkyd polyurethane dispersion that offers better performance at lower cost, thereby providing cost- effective alternatives to conventional grouting materials. The present invention discloses a self- cross linking grouting composition comprising a one-component alkyd polyurethane dispersion, at least one filler, at least one consistency development agent, at least one thickener, and at least one additive. The composition exhibits enhanced performance characteristics, including improved adhesion, durability, and mechanical strength, making it suitable for various construction and repair applications.

Description

[0001] SELF CROSS-LINKING GROUTING COMPOSITION

[0002] CROSS-REFERENCE TO RELATED APPLICATIONS AND PRIORITY

[0003] The present application claims priority from Indian application number 202421045129 filed on 11thJune 2024.

[0004] TECHNICAL FIELD OF THE INVENTION

[0005] The present invention relates to grouting compositions. More specifically, it relates to a self-cross linking grouting composition comprising a one component alkyd polyurethane dispersion.

[0006] BACKGROUND OF THE INVENTION

[0007] Cementitious grout compositions are widely used as filler and binder material for filling the gaps and cracks on the surface and joining the tiles. However, it comes with disadvantages as cementitious grouts require precise mixing ratios, immediate application due to limited work time, and often exhibit inconsistent application, resulting in uneven surfaces and compromised durability. Additionally, these grouts can be challenging to clean and require more maintenance over time. Thus, several polymers modified grouting compositions have been developed in the state of the art.

[0008] In the state of the art, the Chinese application ‘CN102070874A’ disclosed a high-permeability and high-strength epoxy grouting material comprises the following components in part by weight: 25 to 50 parts of epoxy resin, 1 to 15 parts of linear intermediate, 30 to 100 parts of carbonyl compound, 5 to 30 parts of active diluent, 10 to 20 parts of polyamine, 0 to 3 parts of silane coupling agent, 0 to 6 parts of titanate surfactant and 0.5 to 6 parts of accelerator.

[0009] In the state of the art, the European application ‘EP2861544B ’ disclosed a grout based on a mixture of polyurethane resins and acrylic cross-linking aqueous dispersion for tile coating. The grout provides an improved color stability and resistance of the white or the color of the grout itself making it virtually free from yellowing and alterations of the original color without requiring an amine component.

[0010] In the state of the art, the ‘US3859233A’ disclosed a grout composition comprising an acrylic latex, a white inorganic filler, and a finely divided clay, sand, colorants, agents to control the rate of drying, fungicides, antifoaming agents, wetting agents, and thickeners. The developed grout composition exhibits resistance to soiling and ease of cleanability, simple to apply. In the state of the art, the US application ‘US20090044727A1’ disclosed an epoxy additive useful in making a water-soluble grout. The kit for preparing the additive comprises of (a) an epoxy resin selected from the group consisting of (i) a liquid bisphenol A-type epoxy resin, (ii) a liquid bisphenol F-type epoxy resin, (iii) a liquid epoxy phenol novolacs resin, and (iv) an admixture of two or more of any of (i)-(iii); and (b) a composition comprising an admixture of (i) an amine hardener, (ii) a hydrophobic additive and (iii) water.

[0011] However, each type of grouting composition has its own set of disadvantages. For instance, 2K / 3K epoxy amine adduct-based formulas need to be precisely mixed in specific ratios and utilized promptly due to their restricted pot life and workability duration. Also, these 2K / 3K epoxy amine adduct formulas are categorized as hazardous and possess toxic properties.

[0012] Thus, researchers are focusing more on non-hazardous IK water-based PU dispersion grout as it possesses many advantages over cement-based, two- or three-part epoxy-based grout and even premixed acrylic binder grout systems. Polyurethane grouts offer greater flexibility, longer work times, and an easier-to-maintain solution compared to traditional cementitious grout. Nevertheless, polyurethane dispersions also have their disadvantages with respect to cost and performance properties required for joint fillers.

[0013] In order to overcome the above-mentioned disadvantage, the polyurethane is modified via alkyd as it has excellent wetting, dispersion properties, and cost effectiveness. However, limited work has been conducted on the use of alkyd PU dispersions in grouting composition, as it has been restricted to film or coating formations only.

[0014] Therefore, there is a need to develop a cost-effective alkyd polyurethane grouting composition that is an eco-friendly and non-toxic water-based system with improved workability and pot life.

[0015] OBJECTS OF THE INVENTION

[0016] An object of the present invention is to provide self cross-linking grouting composition.

[0017] Another object of the present invention is to provide a self cross-linking grouting composition comprising one-component alkyd polyurethane dispersion.

[0018] Yet another object of the present invention is to provide a one-component alkyd polyurethane dispersion.

[0019] Still another object of the present disclosure is to provide an alkyd based self cross-linking grouting composition that has workability, is easy to clean up during application, and is fast drying and non-cracking. Yet another object of the present invention is to provide a quick-drying, high-strength, and durable mortar composition.

[0020] Still another object of the present invention is to provide a VOC free, polyurethane-based cementitious composition.

[0021] Yet another object of the present invention is to provide a coating composition used on metal, wood, and masonry surfaces.

[0022] Still another object of the present invention is to provide a lamination having excellent heat insulation properties.

[0023] SUMMARY

[0024] This summary is provided to introduce concepts related to a self cross-linking grouting composition. This summary is not intended to identify essential features of the claimed subject matter, nor is it intended for use in determining or limiting the scope of the disclosed subject matter.

[0025] In an aspect of the present invention, a self cross-linking grouting composition is described herein. The self cross-linking grouting composition of the present invention comprises a one component alkyd polyurethane dispersion. The alkyd polyurethane dispersion having an alkyd polyurethane polymer dispersed therein. The alkyd polyurethane dispersion is obtained by reacting at least one hydroxy -functionalized alkyd polymer, at least one isocyanate moiety, at least one chain extending agent, and at least one emulsifier.

[0026] In another aspect of the present invention, the at least one hydroxy-functionalized alkyd polymer is obtainable by reacting at least one fatty acid, at least one dibasic acid, and at least one polyol moiety.

[0027] Yet in another aspect of the present invention, the self cross-linking grouting composition further comprises at least one filler. Further, the self cross-linking grouting composition comprises at least one consistency development agent. The self cross-linking grouting composition further comprises at least one thickener. Further, the self cross-linking grouting composition comprises at least one additive.

[0028] Yet still in another aspect of the present invention, the self cross-linking grouting composition is used for filling gaps, voids, and cracks on surfaces, joining tiles, masonry, mosaics, and other types of building material, sealing joints, and coating surfaces. DETAILED DESCRIPTION

[0029] Reference throughout the specification to “various embodiments,” “some embodiments,” “one embodiment,” or “an embodiment” means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, appearances of the phrases “in various embodiments,” “in some embodiments,” “in one embodiment,” or “in an embodiment” in places throughout the specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures or characteristics may be combined in any suitable manner in one or more embodiments.

[0030] The words "comprising," "having," "containing," and "including," and other forms thereof, are intended to be equivalent in meaning and be open ended in that an item or items following any one of these words is not meant to be an exhaustive listing of such item or items or meant to be limited to only the listed item or items. It must also be noted that, the singular forms "a," "an," and "the" include plural references unless the context clearly dictates otherwise. Although any methods similar or equivalent to those described herein can be used in the practice or testing of embodiments of the present disclosure, the exemplary methods are described. The disclosed embodiments are merely exemplary of the disclosure, which may be embodied in various forms. Various modifications to the embodiment are readily apparent to those skilled in the art, and the generic principles herein may be applied to other embodiments. However, one of ordinary skill in the art may readily recognize that the present disclosure is not intended to be limited to the embodiments illustrated but is to be accorded the widest scope consistent with the principles and features described herein. The detailed description of the invention will be described hereinafter.

[0031] In accordance with an embodiment of the present subject matter, a self cross-linking grouting composition (interchangeably referred to as ‘grouting composition’ or ‘the composition’) for application in joining tile, masonry, mosaics, and other types of building materials, as well as for filling joints and voids between such materials, is described herein.

[0032] In an aspect of the present invention, the self cross-linking grouting composition comprises one- component alkyd polyurethane dispersion (interchangeably referred to as ‘alkyd PUD’, or ‘alkyd polyurethane dispersion’).

[0033] In an embodiment, the one-component alkyd polyurethane dispersion is dispersed in water to obtain the self cross-linking grouting composition.

[0034] Herein, the grouting composition is a water-based grouting composition. In an embodiment of the present invention, the one component alkyd polyurethane dispersion is in a range of 5 wt.% to 50 wt.% of the total weight of self cross-linking grouting composition, preferably 10 wt.% to 35 wt.%, and more preferably 20 wt.% to 30 wt.% of the total weight of the self cross-linking grouting composition.

[0035] In another aspect of the present invention, the one component alkyd polyurethane dispersion is obtained from the reaction of at least one hydroxy-functionalized alkyd polymer, at least one isocyanate moiety, at least one chain extending agent, and at least one emulsifier.

[0036] In an embodiment of the present invention, the at least one hydroxy-functionalized alkyd polymer (interchangeably referred to as ‘alkyd polymer’) is a reaction product of at least one fatty acid, at least one dibasic acid, and at least one polyol moiety.

[0037] In another embodiment, the hydroxy-functionalized alkyd polymer comprises the at least one fatty acid in a range of 50 to 80 wt.% of the hydroxy -functionalized alkyd polymer, preferably 60 wt.% to 80 wt.% of the alkyd polymer. Further, the hydroxy-functionalized alkyd polymer comprises the at least one dibasic acid in a range of 10 wt.% to 30 wt.% of the hydroxy-functionalized alkyd polymer, preferably 11 wt.% to 20 wt.%. Further, the hydroxy-functionalized alkyd polymer comprises the at least one polyol moiety in a range of 10 wt.% to 30 wt.% of the alkyd polymer, preferably 10 wt.% to 20 wt.% of the alkyd polymer.

[0038] In another embodiment, the at least one hydroxy-functionalized alkyd polymer comprises the fatty acid. The at least one fatty acid is selected from, but not limited to, vegetable oil fatty acids such as soybean oil fatty acids, linseed oil fatty acids, dehydrated castor oil, tung oil fatty acids, sunflower oil fatty acids, and the alike.

[0039] Due to the presence of oil in the form of fatty acids in the hydroxy-functionalized alkyd polymer of the alkyd polyurethane dispersion, an excellent balance between hardness and flexibility is achieved. The added flexibility due to hydroxy-functionalized alkyd polymer helps the grout withstand minor structural movements without cracking or breaking, which can be particularly beneficial in areas prone to such fluctuations, such as bridges, highways, and industrial settings.

[0040] Moreover, the hydroxy-functionalized alkyd polymer comprising fatty acid chains of the composition helps to enhance the grout’s strength and durability while also allowing a certain degree of flexibility, which is crucial, especially in areas where there is slight movement or vibration. This allows it to increase the saponification resistance, water immersion service, and alkali resistance when used on concrete, mortar, and cementitious masonry surfaces.

[0041] In a related embodiment, the hydroxy-functionalized alkyd polymer comprises the dibasic acid. The dibasic acids added herein contribute to the polyurethane synthesis, enabling cross-linking, improved curing, chain extension, hydrophilicity, and cross-link density control. In the context of the present invention, the dibasic acid is selected from, but not limited to, a group consisting of phthalic acid, isophthalic acid, maleic acid, malonic acid, succinic acid, glutaric acid, adipic acid, azelaic acid, or their anhydrides, and mixtures thereof.

[0042] In a related embodiment, the hydroxy-functionalized alkyd polymer comprises the polyol moiety. Herein, the polyol moiety is selected from a group of non-glycols such as pentaerythritol, trimethylol propane, dipentaerythritol, and alike.

[0043] In another embodiment, the fatty acid interacts with the polyol and isocyanate moiety in the presence of an emulsifier / intemal surfactant and dibasic acid to obtain a one-component alkyd polyurethane dispersion. A modification of polyurethane polymer with alkyd function enables an excellent balance between hardness and flexibility in the one-component alkyd polyurethane dispersion.

[0044] In a related embodiment of the present invention, the one component alkyd polyurethane dispersion comprises at least one isocyanate moiety, which is selected from a diisocyanate, or a polyisocyanate.

[0045] The at least one isocyanate moiety is selected from a group comprising tetramethylene diisocyanate, pentamethylene 1,5 -diisocyanate, hexamethylene diisocyanate (1,6- diisocyanatohexane), octamethylene diisocyanate, decamethylene diisocyanate, and dodecamethylene diisocyanate, 2,2,4-trimethylhexamethylene diisocyanate, 4,4’- dicychohexylemethane diisocyanate, 2,2-diphenylmethane diisocyanate, 4,4-diphenylmethane diisocyanate, 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, 1,2-phenylene diisocyanate , 1,3-phenylene diisocyanate, 1,4-phenylene diisocyanate, triphenyl methane-4,4’,4”-triisocyanate, naphthylene- 1,5-diisocyanate, polyphenyl polymethylene polyisocyanate, 1,2-xylylene diisocyanate, 1,3- xylylene diisocyanate, 1,4-xylylene diisocyanate, m-tetramethylxylyene diisocyanate (TMXDI), tetramethylene 1,4-diisocyanate, pentamethylene 1,5-diisocyanate, hexamethylene 1,6-diisocyanate, decamethylene diisocyanate, 1,12-dodecane diisocyanate, 2- methyl-l,5-pentamethylene diisocyanate, 8yclobutene-l,3-diisocyanate, 1,2-cyclohexane diisocyanate, 1,3-cyclohexane diisocyanate, 1,4-cyclohexane diisocyanate, 2,4- methylcyclohexane diisocyanate, 2,6-methylcyclohexane diisocyanate, 4,4’- di cyclohexyldiisocyanate, 2,4’ -di cyclohexyldiisocyanate, bis(isocyanatomethyl)-cyclohexane diisocyanate, isophorone diisocyanate or a mixture thereof.

[0046] In a related embodiment of the present invention, the one component alkyd polyurethane dispersion comprises a chain extending agent selected from, but not limited to, at least one of a diamine, ethylene diamine, 1,6-hexane diol, 1,4 butanediol, and l,3-bis(aminomethyl)cyclohexane (1,3-BAC).

[0047] In a related embodiment of the present invention, the one component alkyd polyurethane dispersion comprises the at least one emulsifier. Herein, the emulsifier is selected from dimethylol propionic acid (DMPA) and dimethylol propionic acid (DMBA).

[0048] In a preferred embodiment, the one component alkyd polyurethane dispersion comprises the at least one hydroxy-functionalized alkyd polymer in a range of 40 wt.% to 80 wt.% of the alkyd polyurethane dispersion, preferably 40 wt.% to 60 wt.% of the alkyd polyurethane dispersion. The alkyd polyurethane dispersion comprises the at least one isocyanate moiety in a range of 20 wt.% to 50 wt.% of the alkyd polyurethane dispersion, preferably 30 wt.% to 40 wt.% of the alkyd polyurethane dispersion. The alkyd polyurethane dispersion comprises the at least one chain extending agent in a range of 1 wt.% to 20 wt.% of the alkyd polyurethane dispersion, preferably 1 wt.% to 10 wt.% of the alkyd polyurethane dispersion. The alkyd polyurethane dispersion comprises the at least one emulsifier in a range of 1 wt.% to 20 wt.% of the alkyd polyurethane dispersion, preferably 1 wt.% to 10 wt.% of the alkyd polyurethane dispersion.

[0049] In a preferred embodiment, the one component alkyd polyurethane dispersion is obtainable by reacting the at least one hydroxy-functionalized alkyd polymer, the at least one isocyanate moiety, and the emulsifier in the presence of a catalyst, followed by neutralization with a tertiary amine.

[0050] In yet another aspect of the present invention, the self-cross linking grouting composition comprises a one-component alkyd polyurethane dispersion, at least one filler, at least one consistency development agent, at least one thickener, and at least one additive.

[0051] In a preferred aspect, the grouting composition further comprises the alkyd polyurethane dispersion, at least one filler in a range of 50 wt.% to 90 wt.% based on the total weight of the grouting composition, at least one consistency development agent in a range of 0.1 wt.% to 0.5 wt.% based on the total weight of the grouting composition; and at least one thickener in a range of 0.1 wt.% to 1 wt.% based on the total weight of the grouting composition.

[0052] In an embodiment of the present invention, the alkyd polyurethane grouting composition further comprises the at least one filler is present in an amount in the range of 50 wt.% to 90 wt.% based on the total weight of the grouting composition. The at least one filler is selected from, but not limited to a colored sand, calcium carbonate, dolomite, silica quartz, colorsil-jet black, and a combination thereof. The incorporation of colored pigments / fillers into the grouting composition prevents the release of pigments on the surface of tiles, ceramics, or mosaics, thereby simplifying the cleaning process.

[0053] Preferably, the inert surface silica quartz is added to the alkyd polyurethane grouting composition to get the original shade. The silica quartz added is white or colored and has excellent color leaching resistance in neutral, acidic, and basic water and in organic solvents.

[0054] In another embodiment of the present invention, the self-cross linking grouting composition further comprises the at least one consistency development agent selected from hydroxyethyl cellulose, hydroxymethyl cellulose, (hydroxypropyl) methyl cellulose, and the alike. The consistency development agent is added in the range of 0.1 wt.% to 0.5 wt.% and preferably 0.1 wt.% to 0.3 wt.% of the overall grouting composition, to improve the application consistency and ease of application, and smoothness.

[0055] In yet another embodiment, the self cross-linking grouting composition further comprises a thickener such as alkali swellable acrylic emulsions. The grouting composition comprises the thickener in the range of 0.1 wt.% to 1 wt.% and preferably 0.25 wt.% to 0.45 wt.% of the overall grouting composition, to improve the settling resistance and transportation stability.

[0056] In yet another embodiment, the grouting composition further comprises one or more other additives selected from but not limited to defoamer, pH stabilizer, non-ionic surfactant, stabilizing agent, freeze-thaw stability agent, co-solvent, in-can preservatives, cross-linking agent, and a combination thereof.

[0057] In a related embodiment, the defoamer is selected from one or more mineral oil bases, silicone oil bases, and a combination thereof. The defoamer in the grouting composition is added to reduce / eliminate foam during processing and applications of the composition, thereby preventing a plurality of defects, like the formation of pin holes in the grouting.

[0058] In a related embodiment, the pH stabilizer is selected from one or more amines, polyamines, or any combination thereof. The pH stabilizer in the grouting composition is added to provide stability to the composition during storage. Herein, the pH stabilizer in the grouting composition is added in the range of 0.1 wt.% to 1 wt.% of the overall grouting composition and preferably 0.4 wt.% to 0.8 wt.% of the overall grouting composition.

[0059] In a related embodiment, the non-ionic surfactants, such as alcohol ethoxylate dilution grade is added during grinding / mixing for composition stabilization. Herein, the non-ionic surfactants are added in the range of 0.1 wt.% to 1.5 wt.% of the overall grouting composition and preferably 0.3 wt.% to 0.9 wt.% of the overall grouting composition.

[0060] In a related embodiment, the stabilizing agent, such as soya by-product, is used to provide stabilization and anti-settling properties to fillers / sands. Also, a co-solvent such as hydrophobic glycol, xylene ether is optionally added to the grouting composition.

[0061] In a related embodiment, the stabilizing agent, as soya based stabilizing agent, is added in the range of 0.05 wt.% to 0.75 wt.% of the overall grouting composition and preferably 0.08 wt.% to 0.5 wt.% of the overall grouting composition to provide stabilization and anti-settling properties to fillers / sands. Also, a co-solvent such as hydrophobic glycol ether is added in the range of 0.2 wt.% to 1 wt.% of the overall grouting composition and preferably 0.25 wt.% to 0.7 wt.% of the overall grouting composition.

[0062] In a related embodiment, the freeze-thaw stability agent, such as tri-ethylene glycol, Propane-1, 2- diol, is added to aid in freeze-thaw resistance with improved storage stability and to get desirable application consistency in the composition. Herein, the freeze-thaw stability agent is added in the range of 0.0.05 wt.% to 1.5 wt.% of the overall grouting composition, and preferably 0.08 wt.% to 0.5 wt.% of the overall grouting composition.

[0063] In a related embodiment, one or more preservatives, such as methyl chloro-isothiazolinone and methylisothiazolinone, are added to protect a product formula from bacteria, mold, and yeast in order to maintain product quality and performance. Herein, the preservatives are added in the range of 0.01 wt.% to 0.25 wt.% of the overall grouting composition and preferably 0.08 wt.% to 0.15 wt.% of the overall grouting composition to protect a product formula from bacteria, mold, and yeast in order to maintain product quality and performance.

[0064] In a related embodiment, the herbicide and algaecide present in grouting composition are encapsulated biocides. The encapsulated biocide selected from diuron, octylisothiazolinone, is added to provide long-term protection. The herbicide and algaecide comprises an encapsulated (controlled release) dry film preservative to provide extended long-term resistance to algae, fungal / mold resistance, and protection from surface fungal and algal growth. Herein, the encapsulated biocide is added in the range of 0.05 wt.% to 1.5 wt.% of the overall grouting composition, and preferably 0.1 wt.% to 0.5 wt.% of the overall grouting composition.

[0065] In a related embodiment, the cross-linking agent, at least one metal based cross-linker selected from the group consisting of iron, cobalt, and manganese complexes is added to the grouting composition, preferably Borchi® OXY-Coat 1101. Herein, the cross-linking agent is added in the range of 0.08 wt.% to 1.5 wt.%, and preferably 0.1 wt.% to 1 wt.% of the overall grouting composition to promote snail trail resistance, improved self cross-linking surface hydrophobicity, and water repellency.

[0066] In another aspect of the present invention, the self cross-linking polyurethane grouting composition is used to join tiles, masonry, mosaics, and other types of building materials and to fill joints and voids between such materials.

[0067] In another aspect of the present invention, the method for preparing one-component alkyd polyurethane dispersion (hereafter ‘PUD’) for the purpose of incorporating in the self cross-linking grouting composition is disclosed and comprises various steps.

[0068] The method for preparing the one-component alkyd polyurethane dispersion includes a step of mixing a dibasic acid, fatty acid, polyol moiety, and a catalyst such as dibutyl tin oxide and a solvent such as xylene to obtain a reaction mixture, followed by heating until a prerequisite acid number is attained. The method includes a step of cooling the reaction mixture and applying a vacuum to remove solvent and water from the mixture to achieve a moisture level less than 0.1% and to obtain hydroxy-functionalized alkyd polymer.

[0069] Further, the method for preparing the one component alkyd polyurethane dispersion includes a step of adding the at least one hydroxy-functionalized alkyd polymer, at least one emulsifier, and a catalyst in a reactor equipped with an anchor stirrer, followed by the addition of at least one isocyanate moiety, and rinsing with acetone to obtain a mixture polymer. Further, the method includes a step of neutralizing the mixture by adding an amine such as a tertiary amine, and digestion for 30 minutes to obtain a neutralized polymer.

[0070] The method includes a step of extension of neutralized prepolymer via at least one chain extending agent for 60 minutes to obtain a prepolymer. In the next step, the prepolymer is then transferred to a dispersion vessel and mixed with the addition of deionized water and defoamer to obtain the one- component alkyd polyurethane dispersion.

[0071] In an embodiment, the one-component alkyd polyurethane dispersion has a viscosity in a range of 10 to 45 poise with 100% active content as per Brookfield viscometer @ 25 °C.

[0072] In another embodiment, the one-component alkyd polyurethane dispersion has a glass transition temperature in the range of 65 °C to 75 °C.

[0073] Here, the one-component alkyd polyurethane dispersion incorporates at least one hydroxyfunctionalized alkyd polymer and at least one isocyanate moiety into a single dispersion to chemically alter into a single, unique compound with inseparable constituents.

[0074] Herein, the one-component alkyd polyurethane dispersion is solvent-free.

[0075] In another embodiment, a method for preparing the alkyd polyurethane grouting composition comprising various steps is disclosed herein. The method includes a step of blending the alkyd polyurethane dispersion and at least one additive for 20 min at 800 to 900 rpm on a high-speed dispenser to obtain a uniform mixture. The method includes a step of transferring the uniform mixture to a bowl of a planetary mixer, followed by the addition of at least one filler slowly with constant mixing for the next 30 min to ensure uniform mixing of the ingredients in the composition. Further, the method includes a step of adding at least one consistency agent to ensure the required consistency of the composition. Further, the method includes a step of adding at least one thickener.

[0076] Herein, the double planetary mixer having twin rectangular paddle shape blades with multiple metal scrapers and side Teflon scrapers is utilized. When the rectangular blades are in revolution and rotation running at the same time, the material flows up and down as well as around the inner cylinder, which reaches the mixing effect in a very short time.

[0077] In one embodiment, the one-component alkyd polyurethane dispersion is self-cross-linkable in nature due to the oxidatively curing mechanism of conjugated double bonds present in the oil / fatty acid part of the hydroxy-functionalized alkyd polymer in the presence of a small amount of heavy metal compound. Thus, the alkyd polyurethane dispersion has not only been used as a binder for grouting composition but also for a variety of one-component coatings for wood (floors and furniture), plastic (machine housings), leather, and metal.

[0078] Further, for a better understanding of the present disclosure and associated method, the following examples are discussed.

[0079] Example 1-3 illustrates the preparation of one component alkyd polyurethane dispersion. The physical properties of alkyd polyurethane dispersion were evaluated and discussed herein. The percentage (%) solid content was determined as per WI4001 oven heating @ 105 °C for 90 min. The viscosities were measured by Brookfield viscometer @ 25°C. The pH of the dispersion was measured by a pH meter @ 25 °C. The particle size of the dispersion was measured using the Zeta sizer instrument.

[0080] Example 1: Alkyd polyurethane dispersion A

[0081] Step I: A dry four-neck round-bottom flask equipped with a Teflon blade stirrer, Dean-Stark, and a vertical condenser was arranged. 670 g of distilled soya fatty acid, 170 g pentaerythritol -98, 110 g isophthalic acid, 0.5 g dibutyl tin oxide, and 49.5 g ortho xylene were charged in the setup. Further, the mixture was heated to 235 °C under a nitrogen atmosphere, wherein the azeotropic distillation started at 175 °C. The heating continued till the acid value of less than 4 mg KOH / g of sample was achieved. After achieving the acid number, the reaction mixture is cooled from 235 °C to 175 °C. Further, the vacuum was applied to the reaction mixture, followed by the removal of ortho xylene and water. After getting the moisture level less than 0.1%, the vacuum was released, and the obtained hydroxy functionalized alkyd polymer was cooled to 50°C under a nitrogen atmosphere.

[0082] Step II: 396.6 g of the hydroxy functionalized alkyd polymer was taken in another four-neck glass reactor equipped with an anchor stirrer, followed by the addition of 50.51 g dimethylol propionic acid (DMPA) and 0.5 g of dibutyltin dilaurate. 252.52 g of isophorone diisocyanate was charged after 15 minutes of mixing, followed by rinsing with 235 g of acetone to obtain a prepolymer mixture by maintaining the temperature between 60 to 65 °C.

[0083] The prepolymer mixture was then neutralized with 30 g of tri ethylamine over 30 minutes of digestion. The neutralized prepolymer was then extended with a mixture of 47 g 1,6-hexanediol and 60 g acetone. The complete extension was held for a further 60 minutes. The prepolymer mixture was then transferred to a dispersion vessel and mixed at 1000 to 1200 rpm. A mixture of 1 g BYK 024 and 1100 g deionized water was added to the prepolymer over 15 minutes of time to obtain an alkyd polyurethane dispersion A.

[0084] Example 2: Alkyd polyurethane dispersion B

[0085] Step I: A dry four-neck round-bottom flask equipped with a Teflon blade stirrer, Dean-Stark, and a vertical condenser was arranged. 1340 g of distilled soya fatty acid, 340 g pentaerythritol-98, 240 g phthalic anhydride, 1 g dibutyl tin oxide, and 79 g ortho xylene were charged in the setup. The mixture was heated to 235 °C under a nitrogen atmosphere, with azeotropic distillation started at 175 °C. The heating continued till the acid value of less than 4 mg KOH / g of sample was achieved. After achieving the acid number, the reaction mixture was cooled from 235 °C to 175 °C. Further, the vacuum was applied, and the ortho xylene and water were removed from the reaction mixture. After getting the moisture level less than 0.1%, the vacuum was released, and the hydroxy functionalized alkyd polymer was cooled to 50°C under a nitrogen atmosphere.

[0086] Step II: 618.6 g of the hydroxy functionalized alkyd polymer was taken in another four-neck glass reactor equipped with an anchor stirrer, and 72.2 g dimethylolpropionic acid and 0.5 g of dibutyl tin oxide were added. After 15 minutes of mixing, 309.3 g of isophorone diisocyanate was charged over the 15-minute time, followed by rinsing with 200 g of acetone and the temperature 60 °C to 65°C was maintained.

[0087] The prepolymer mixture was then neutralized with 50 g of triethylamine over 30 minutes of digestion. The neutralized prepolymer mixture was then transferred to a dispersion vessel and mixed at 1000 to 1200 rpm. The dispersion was then chain extended with a mixture of 60 g ethylene diamine and 540 g DI water. A mixture of 1 g BYK 024 and 1450 g deionized water was added to the prepolymer over 15 minutes. The obtained mixture was considered an alkyd polyurethane dispersion B.

[0088] Example 3: Hydroxy-Functionalized Alkyd polyurethane dispersion C

[0089] Step I: A dry four-neck round-bottom flask equipped with a Teflon blade stirrer, Dean-Stark, and a vertical condenser was arranged. 1340 g of distilled soya fatty acid, 340 g pentaerythritol-98, 220 g isophthalic acid, 1 g dibutyl tin oxide, and 99 g ortho xylene were charged in the set-up. Further, the mixture was heated to 235 °C under a nitrogen atmosphere, wherein the azeotropic distillation started at 175 °C. The heating continued till the acid value of less than 4 mg KOH / g of sample was achieved. After achieving the acid number, the reaction mixture is cooled from 235 °C to 175 °C. Further, the vacuum was applied to the reaction mixture, followed by the removal of ortho xylene and water. After getting the moisture level less than 0.1%, the vacuum was released, and the hydroxy functionalized alkyd polymer was cooled to 50 °C under a nitrogen atmosphere. Step II: 1134 g of the hydroxy functionalized alkyd polymer was taken in another four-neck glass reactor equipped with an anchor stirrer, followed by the addition of 144.4 g dimethylol propionic acid (DMPA) and 1 g of dibutyltin dilaurate. After 15 minutes of mixing, 721.6 g of Isophorone diisocyanate was charged over the 15-minute time, followed by rinsing with 500 g of Acetone and the temperature between 60 °C to 65 °C was maintained.

[0090] The prepolymer mixture was then neutralized with 98 g of tri ethylamine over 30 minutes of digestion. The neutralized prepolymer mixture was then transferred to a dispersion vessel and mixed at 1000 to 1200 rpm. A mixture of 2g BYK 024 and 3000g deionized water was added to the prepolymer over 15 minutes. The dispersion was then chain extended with a mixture of 60 g ethylene diamine and 540 g DI water. The dispersion was held for the next 30 minutes at high rpm. Acetone used in prepolymer was then removed at 55 to 60 °C under vacuum. The complete acetone quantity was removed and cooled to 35 °C to obtain an alkyd polyurethane dispersion C. Further, the properties of the obtained alkyd polyurethane dispersion C is provided in tabulated form in Table 1.

[0091] Table 1: Characterization of the alkyd polyurethane dispersion C

[0092] Example 4: Self cross-linking polyurethane grouting composition

[0093] A blend of alkyd polyurethane dispersion C was synthesized as described in Example 3, which was mixed for 20 min at 800-900 rpm on a high-speed disperser. Further, the prepared blend was taken in a bowl of a planetary mixer, followed by the addition of the colored sand (filler) slowly for the next 30 minutes to ensure uniform mixing. Further, solutions for defoamer, pH stabilizer, non-ionic surfactant, stabilizing agent, freeze-thaw stability agent, co-solvent, in-can preservatives, biocide, cross-linker, consistency development agent and thickener were added for the next 30 minutes for consistency adjustment. The components of Table 2 were blended to obtain the self-cross-linkable grouting composition.

[0094] Table 2: Alkyd polyurethane grouting composition

[0095] Example 5-9: Alkyd polyurethane grouting compositions

[0096] Different grouting compositions are prepared with the same process as mentioned in Example 4. The charging amount of one-component alkyd polyurethane dispersion, different additives, consistency development agent, cross-linker and thickener are provided in tabulated form in Table 3.

[0097] Referring to Table 3 below, the amounts of selected constituents, such as consistency development agent and thickener, binder, and solvent, were altered (i.e., +1.5%, 1.5%) in the grout compositions. For instance, in the examples, the following constituents were altered:

[0098] In examples 5 and 5 A: thickener wt.%,

[0099] In examples 6 and 6A: cellulose ether wt.%,

[0100] In examples 7 and 7A: defoamer wt.%,

[0101] In examples 8 and 8A, the alkyd polyurethane grouting composition was altered by fabricating a change in the amount of dispersion, and

[0102] In examples 9 and 9A: solvent optimization.

[0103] In example ‘ready sample’ was selected as SP100™ UBI by MYK lati crete

[0104] After preparation, the compositions were allowed to cure under the same processing conditions. The comparative grouts were set up for a series of tests to measure the hardness, scratch resistance, weight loss, and water absorption (ASTM D 471), including testing for specific gravity (density), shore A and shore D hardness (ASTM D2240); the specific gravity (density) was measured by filling a WPL cup of 100 ml volume, and the weight of the material in the cup was recorded; For the hardness test, a standard 3 mm bed was prepared and filled with the material and allowed to harden at ambient temperature for 24 hours; Shore A hardness was then recorded for each tested grout after 24 hours. Furthermore, the ease of cleaning on the tile (smoothed surface tile as well as matt / rough surface tile) surface after 2 hrs.; drying is evaluated by dampening the surface for 1 to 2 min and scrubbing it by using nylon scrubber; ease of application on the tile is examined by using the metal palti patra and to check the applicability and filling tendency of grout in tile joints. Moreover, a prepared ready sample (SP100™ UBI by MYK laticrete) bought from the market was used as a blank for a comparative study.

[0105] Table 3: Different grouting compositions Table 4: Test results for different grouting compositions prepared as per Table 3 Referring to Table 4, the prepared grouting compositions indicated the following properties:

[0106] • Excellent flowability / grouting ability (ease of application) by putty blade if stirred before application, thereby indicating shear thinning behavior;

[0107] • Cleanability after 24 hrs. of drying;

[0108] • Weight loss is less than 0.5 %;

[0109] • No reduction in Shore A and Shore D hardness in water dip condition when dipped in water for 24 hrs.

[0110] • Water beading effect after 24 hrs. for curing;

[0111] • Specific gravity of each of the compositions was maintained within a certain range, indicating the workability, ease of application and consistency.

[0112] Further, it was tested with Needle Scratch hardness as per ISO 1518 -1 : 2019 (Needle is made up of Hard Stainless Steel with a hemispherical ball 01m (Tungsten Carbide) on a 3 mm thick cured bed of grout.

[0113] Example 10: Comparative study

[0114] Example 5 was selected for further comparative study of self cross-linking polyurethane grouting composition with acrylic-based grouting composition (styrene acrylic emulsion, 50% solid), PUD- based grouting composition (Bayhydrol®UH2606), and blend of acrylic-based grouting composition and PUD-based grouting composition.

[0115] Along with the grouting composition discussed in example 5, different grouting compositions such as acrylic-based grouting composition (I), blend of acrylic-polyurethane-based grouting composition (II), and PUD-based grouting composition (III) are prepared and thoroughly evaluated. The charging amount of components is provided in tabulated form in Table 5.

[0116] Table 5: Different grouting compositions for comparative study

[0117] Table 6: Test results for different grouting compositions prepared as per Table 5

[0118]

[0119] It is evident from Table 6 that the self cross-linking grouting composition developed as per the present disclosure is superior in performance as compared to the conventional water-borne acrylic, acrylic-polyurethane-based grout composition, and polyurethane-based grout compositions. In view of the conventionally used materials, water absorption after 7 days of curing is lower, higher shore hardness, scratch resistance, and reduced % weight loss. The ease of cleaning the disclosed self cross-linking grouting composition (See Example 5).

[0120] While the present invention has been particularly described, in conjunction with a specific preferred embodiment, it is evident that many alternatives, modifications, and variations will be apparent to those skilled in the art considering the foregoing description. It is therefore contemplated that the appended claims will embrace any such alternatives, modifications, and variations, such as falling within the true scope and spirit of the present invention.

[0121] In accordance with the embodiment, the developed self cross-linking grouting composition demonstrated the following application: • Filling gaps, voids, and cracks on surfaces.

[0122] • Joining tiles, masonry, mosaics, and other types of building materials. Preferably, Internal and external applications in finishing for glazed, ceramic, porcelain, vitrified & fully vitrified tiles & natural stones

[0123] • Sealing joints such as Tile seal grout (smooth paste-like) for DIY applications. • Coating surfaces.

[0124] • Binder for a variety of one-component coatings for wood (floors and furniture), plastic (machine housings), leather, and metal.

[0125] In accordance with the embodiment, the alkyd polyurethane dispersion-based grouting composition demonstrated the following advantages as below,

[0126] • One component in nature, ready to use, self-crosslinking, fast strength developing, easy cleaning, stain proof, color-perfect tile joint filler / grout compositions.

[0127] • Algae and fungus / mold growth resistant and eco-friendly, non-toxic grouting composition

[0128] • Excellent hardness development, excellent resistance to settling during road transportation,

[0129] • Avoiding dust release while plant processing and site mixing.

[0130] • Fast curing nature, excellent water dip resistance and retaining its hardness in water dip condition, uniform and consistent upon application, and scratch-proof in water dip condition after full cure for three days

[0131] • Shrink-free, slump-free, non-sag gives edge-to-edge grouting finish with zero to nil shrinkage when applied vertically or horizontally

[0132] • Less than 0.2 % weight loss after Scratch Hardness - constant - loading method (as per ISO 1518 -1 : 2019)

[0133] • Passes with 5 Kg of load when tested with ISO 1518 -1 : 2019 on a 3 mm thick bed.

[0134] • Shows excellent capacity to bear a 5 kg scratch load compared to other existing grouts

[0135] • Excellent elasticity and flexibility on hardening, making it suitable for tiling applications subject to vibrations and / or deformations.

[0136] Although implementations for the self cross-linking grouting composition have been described in language specific to structural features and / or methods, it is to be understood that the appended claims are not necessarily limited to the specific features or methods described. Rather, the specific features and methods are disclosed as examples of implementations of the self cross-linking grouting composition.

Claims

WE CLAIM:

1. A self cross-linking grouting composition comprising a one-component alkyd polyurethane dispersion having an alkyd polyurethane polymer dispersed therein, wherein the alkyd polyurethane polymer is a reaction product of: i) at least one hydroxy-functionalized alkyd polymer; ii) at least one isocyanate moiety; iii) at least one chain extending agent; and iv) at least one emulsifier.

2. The composition as claimed in claim 1, wherein the one component alkyd polyurethane dispersion is in a range of 5 wt.% to 50 wt.% of the total weight of the grouting composition.

3. The composition as claimed in claim 1, wherein the hydroxy-functionalized alkyd polymer is a reaction product of at least one fatty acid, at least one dibasic acid, and at least one polyol moiety.

4. The composition as claimed in claim 3, wherein the at least one fatty acid is selected from a group consisting of soybean oil fatty acid, linseed oil fatty acid, dehydrated castor oil, tung oil fatty acid, sunflower oil fatty acid, and a mixture thereof.

5. The composition as claimed in claim 3, wherein the dibasic acid is selected from a group of wherein the dibasic acid is at least one selected from a group consisting of phthalic acid, isophthalic acid, maleic acid, malonic acid, succinic acid, glutaric acid, adipic acid, azelaic acid, or anhydrides thereof.

6. The composition as claimed in claim 3, wherein the at least one polyol moiety is selected from a group consisting of polyethylene glycol, polypropylene glycol, polyisobutylene glycol, polytetrahydrofuran diol, polycarbonate diol, polycaprolactone triol, polyethylene adipate diol, poly-1, 4-butanediol adipate diol, poly-hexanediol adipate diol, and a mixture thereof.

7. The composition as claimed in claim 1, wherein the at least one isocyanate component is selected from a group consisting of hexamethylene-l,6-diisocyanate, 2,2,4- trimethylhexamethylene diisocyanate, 4,4'-dicychohexylemethane diisocyanate, 2,2-diphenylmethane diisocyanate, 4,4-diphenylmethane diisocyanate, 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, 1,2-phenylene diisocyanate, 1,3-phenylene diisocyanate, 1,4- phenylene diisocyanate, triphenyl methane-4,4',4"-triisocyanate, naphthylene- 1,5- diisocyanate, polyphenyl polymethylene polyisocyanate, 1,2- xylylene diisocyanate, 1,3- xylylene diisocyanate, 1,4-xylylene diisocyanate, m-tetramethylxylyene diisocyanate (TMXDI), tetramethylene 1,4-diisocyanate, pentamethylene 1,5 -diisocyanate, decamethylene diisocyanate, 1,12-dodecane diisocyanate, 2-methyl-l,5-pentamethylene diisocyanate, cyclobutane- 1, 3 -diisocyanate, 1, 2-cy cl ohexane diisocyanate, 1,3 -cyclohexane diisocyanate, 1,4-cy cl ohexane diisocyanate, 2, 4-methylcy cl ohexane diisocyanate, 2,6- methylcyclohexane diisocyanate, 4,4'-dicyclohexyldiisocyanate, 2,4'- dicyclohexyldiisocyanate, bis(isocyanatomethyl)-cyclohexane diisocyanate, isophorone diisocyanate or a mixture thereof.

8. The composition as claimed in claim 1, wherein at least one chain extending agent is selected from a group consisting of diamine, ethylene diamine, 1,6-hexane diol, and 1,3- bis(aminomethyl)cyclohexane (1,3-BAC), 1,4 -butanediol.

9. The composition as claimed in claim 1, wherein the at least one emulsifier is selected from a group consisting of dimethylol propionic acid (DMPA), dimethylol butanoic acid (DMBA), citric acid, tartaric acid, diphenolic acid, hydroxymethylpropionic acid, and trimethylolpropionic acid, and a mixture thereof.

10. The composition as claimed in claim 1, wherein the alkyd polyurethane dispersion comprises: i) the at least one hydroxy-functionalized alkyd polymer in a range of 40 wt.% to 80 wt.% of the alkyd polyurethane dispersion; ii) the at least one isocyanate moiety in a range of 20 wt.% to 50 wt.% of the alkyd polyurethane dispersion; iii) the at least one chain extending agent in a range of 1 wt.% to 20 wt.% of the alkyd polyurethane dispersion; and iv) the at least one emulsifier in a range of 1 wt.% to 20 wt.% of the alkyd polyurethane dispersion.

11. The composition as claimed in claim 1, comprises:at least one metal based cross-linker in a range of 0.08 wt.% to 1.5 wt.% based on the total weight of the grouting composition; at least one filler in a range of 50 wt. % to 90 wt.% based on the total weight of the grouting composition; at least one consistency development agent in a range of 0.1 wt.% to 0.5 wt.% based on the total weight of the grouting composition; and at least one thickener in a range of 0.1 wt.% to 1 wt.% based on the total weight of the grouting composition.

12. The composition as claimed in claim 11, wherein the at least one metal based cross-linker selected from a group consisting of iron, cobalt, and manganese complexes; the at least one filler is selected from colored sand, calcium carbonate, dolomite, silica quartz, and a combination thereof; the at least one consistency development agent is selected from at least one of hydroxyethyl cellulose, hydroxymethyl cellulose, (hydroxypropyl) methyl cellulose, and the alike; and the at least one thickener is an alkali swellable acrylic emulsion.

13. The composition as claimed in claim 1, comprises at least one additive selected from a group of a defoamer, a pH stabilizer, a non-ionic surfactant, a stabilizing agent, a freeze-thaw stability agent, a co-solvent, an in-can preservative and a combination thereof.

14. The composition as claimed in claim 13, wherein the defoamer is selected from a mineral oil base, a silicone oil base, or a combination thereof; the pH stabilizer is selected from an amine, polyamine, or any combination thereof; the freeze-thaw stability agent is selected from a tri-ethylene glycol, Propane- 1 ,2-diol, or any combination thereof; and the preservative is selected from a methyl chloro-isothiazolinone, methylisothiazolinone, or any combination thereof.

15. The composition as claimed in claim 1 is used for filling gaps, voids, and cracks on surfaces; joining tiles, masonry, mosaics, and other types of building material, sealing joints; and coating surfaces.

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