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Adhesive Composition And A Process For Its Preparation

Abstract: ABSTRACT ADHESIVE COMPOSITION AND A PROCESS FOR ITS PREPARATION The present disclosure provides an adhesive composition and a process for its preparation. The adhesive composition comprises a base component and a hardener component. The adhesive composition of the present disclosure is used as a waterproof coating below the tiles. Further, the adhesive composition of the present disclosure is used as a tile grout to fill gaps between tile joints. The adhesive composition of the present disclosure, have the properties such as waterproofing, stain resistance, and abrasion resistance. Further, the present disclosure provides a simple process for the preparation of the adhesive composition.

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Patent Information

Application #
Filing Date
01 September 2023
Publication Number
10/2025
Publication Type
INA
Invention Field
POLYMER TECHNOLOGY
Status
Email
Parent Application

Applicants

KANSAI NEROLAC PAINTS LIMITED
NEROLAC HOUSE, GANPATRAO KADAM MARG, LOWER PAREL, MUMBAI-400013, MAHARASHTRA, INDIA

Inventors

1. NIKAM LAXMAN SHANKAR
Lodha Casa Essenza CHSL, C Wing, Flat No.1006, Mahajanwadi, Western Express Highway, Opp. Thakur Mall, Mira Road-East, Thane-401107, Maharashtra, India
2. MARATHE MUKUL SHRIKANT
“Shreeman” Bungalow, Old Katrap road, Opp RBL Bank, Kulgaon, Badalapur-421503, Maharashtra, India
3. KHAIRNAR SUNIL RAVAN
Magdalena D-wing, Flat No 602, Casa Rio, Palva City, Kalyan Shil Phata Road, Nilje Gaon, Thane-421204, Maharashtra, India
4. PATIL SHIVKUMAR
Morgana C-wing, Flat No 302, Casa Rio, Palva City, Kalyan Shil Phata Road, Nilje Gaon, Thane-421204, Maharashtra, India

Specification

DESC:FIELD
The present disclosure relates to a field of construction and masonry application. Particularly, the present disclosure relates to an adhesive composition and a process for its preparation.
DEFINITIONS
As used in the present disclosure, the following terms are generally intended to have the meaning as set forth below, except to the extent that the context in which they are used, indicate otherwise.
2K adhesive composition: The term “2K adhesive composition” refers to two component epoxy-polyurethane adhesive. In 2K adhesive composition the first component (base component) and the second component (hardener component) are blended to form the adhesive composition.
Pre-Polymer: The term “pre-polymer” refers to a substance which represents an intermediate stage in polymerization and can be manipulated before completion of polymerization. The pre-polymer can be either a monomer or an oligomer which is capable of undergoing further polymerization to form a large polymer material with a high molecular weight.
Epoxy equivalent weight (EEW): The term “epoxy equivalent weight (EEW)” refers to the number of grams of epoxy resin required to give 1 mole of epoxy groups.
Hydrophilic-lipophilic balance (HLB): The term “hydrophilic-lipophilic balance (HLB)” refers to the balance of the size and strength of the hydrophilic and lipophilic moieties of a surfactant molecule.
Reactive content: The term “Reactive content” in accordance with the present disclosure refers to the chemical groups or functional molecules that are present in a prepolymer, which are capable of reacting with other molecules to form a polymer chain.
Taber Abrasion resistance: The term “Taber Abrasion resistance” refers to materials resistance to wear and tear caused by friction and abrasion. The Taber Abrasion is a standardized test method that simulates the wear and tear caused by repeated rubbing or scratching of a material. The test involves using a Taber Abraser, a machine that applies a controlled amount of pressure and friction to the material, while moving it back and forth.
Efflorence: The term “efflorence” refers to a crystalline deposit of salts that can form when water is present in or on brick, concrete, stone, stucco or other building surfaces.
Tensile Adhesion test: The term “tensile adhesion test” refers to the test that is used to evaluate the adhesive strength of materials, particularly in the field of adhesives, coatings, and composites. The test helps to determine the bond strength between two surfaces, which is essential for ensuring the integrity and reliability of various applications. The adhesion is measured by the tensile pull on a Dolly glued to the coating surface. The force is applied through the center of the Dolly by a hydraulically loaded pin.
Shear Adhesion test: The term “shear adhesion test” refers to the shear strength of a bond between two surfaces, which is essential for ensuring the integrity and reliability of various applications. The shear adhesion test measures the force required to cause a bonded surface to slide or deform along its interface, typically in a direction perpendicular to the surface.
Cementitious tile adhesive: The term “cementitious tile adhesive” refers to the cement based powder adhesive which is used to fix tiles on walls and floors.
Cementitious tile grout: the term “cementitious tile grout” refers to the cement based powder product that is used to fill the gaps between two tiles.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
There are many types of adhesive compositions such as cementitious tile adhesive, dispersion tile adhesive, epoxy tile adhesive, and the like available in the market for masonry applications. However, these conventional adhesives are suitable for only single application i.e. fixing tiles.
The conventional adhesive compositions does not have the properties that can provide waterproof coating against rising dampness on the concrete walls, stain resistance, and the like. Different compositions are required for different application that increase the cost and time. Moreover, these different compositions require different solvent which are toxic, flammable, and add on to the cost of the product.
Therefore, there is felt a need to provide an adhesive composition that can mitigate the drawbacks mentioned hereinabove or at least provides an alternative solution.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows.
An object of the present disclosure is to ameliorate one or more problems of the background or to at least provide a useful alternative.
Another object of the present disclosure is to provide an adhesive composition.
Still another object of the present disclosure is to provide a 2k adhesive composition.
Yet another object of the present disclosure is to provide an adhesive composition that has enhanced abrasion resistance and water proofing properties.
Still another object of the present disclosure is to provide an adhesive composition that is stain free.
Yet another object of the present disclosure is to provide a process for the preparation of an adhesive composition.
Still another object of the present disclosure is to provide a simple, economical and environment friendly process for the preparation of an adhesive composition.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.
Summary
The present disclosure provides an adhesive composition and a process for its preparation.
In an aspect, the present disclosure provides an adhesive composition.
The adhesive composition comprises:
(A) a base component comprising:
i) a predetermined amount of a base resin;
ii) a predetermined amount of a plasticizer;
iii) a predetermined amount of a pre-polymer;
iv) a predetermined amount of a first filler;
v) a predetermined amount of a first pigment;
vi) a predetermined amount of a first additive; and
vii) q.s water.
and
(B) a hardener component comprising:
i) a predetermined amount of a hardener resin;
ii) a predetermined amount of an accelerated curing agent;
iii) a predetermined amount of a second filler;
iv) a predetermined amount of a second pigment; and
v) a predetermined amount of a second additive.
A mass ratio of the base component to the hardener component is in the range of 3:1 to 7:1 prior to application on a substrate.
In an embodiment of the present disclosure, the predetermined amount of the base resin is in the range of 10 mass% to 25 mass%, the predetermined amount of the plasticizer is in the range of 12 mass% to 25 mass%, the predetermined amount of the pre-polymer is in the range of 5 mass% to 15 mass%, the predetermined amount of the first filler is in the range of 45 mass% to 65 mass%, the predetermined amount of the first pigment is in the range of 1 mass% to 5 mass%, and the predetermined amount of the first additive is in the range of 2 mass% to 10 mass%, wherein mass% of each ingredient is with respect to the mass of the base component.
In an embodiment of the present disclosure, the predetermined amount of the hardener resin is in the range of 20 mass% to 40 mass%, the predetermined amount of the accelerated curing agent is in the range of 1 mass% to 4 mass%, the predetermined amount of the second filler is in the range of 55 mass% to 75 mass%, the predetermined amount of the second pigment is in the range of 1 mass% to 3 mass%, and the predetermined amount of the second additive is in the range of 1 mass% to 10 mass%, wherein mass% of each component is with respect to the total mass% of hardener component.
In an embodiment of the present disclosure, the base resin is unmodified liquid epoxy resin (Lapox B11).
In an embodiment of the present disclosure, the plasticizer is selected from alkyl sulphonic acid ester, esters of phthalic acid, diethylehexyl terephthalate, diisononyl cyclohexane dicarboxylate, and biobased plasticizers based on epoxidized plant oils, cardanol, and citrates.
In an embodiment of the present disclosure, the pre-polymer is selected from the group consisting of blocked polyoxypropylene glycol and toluene diisocyanate and branched polymer with ether and urethane groups based on blocked polyoxypropylene glycol and toluene diisocyanate (DESMOCAP 14 CNB).
In an embodiment of the present disclosure, the first filler and the second filler are independently a carbonate mineral. The carbonate mineral is selected from the group calcium carbonate (calcite powder) (Micron CARB 1240).
In an embodiment of the present disclosure, the first pigment and the second pigment are independently titanium dioxide (Nanotox 207).
In an embodiment of the present disclosure, the first additive is selected from a first rheology modifier, a first surfactant, and a preservative.
In an embodiment of the present disclosure, the hardener resin is selected from the group consisting of aliphatic polyamide, modified aliphatic polyamide, aromatic polyamide, modified aromatic polyamide, primary polyamide, secondary polyamide, and tertiary polyamide.
In an embodiment of the present disclosure, the accelerated curing agent is an aromatic tertiary amine.
In an embodiment of the present disclosure, the second additive is selected from the group consisting of second rheology modifier, a second surfactant, and a thixotropic agent.
In an embodiment of the present disclosure, the substrate is selected from the group consisting of concrete wall, plaster wall, glass panel, metal panel, wooden panel, plaster board, and gypsum board.
In an embodiment of the present disclosure, the polyoxypropylene glycol and toluene diisocyanate is blocked with at least one component selected from alkyl phenol and renewable blocking agent; and wherein the renewable blocking agent is cashew nutshell liquid.
In an embodiment of the present disclosure, the first rheology modifier and the second rheology modifier are independently selected from the group consisting of bentonite clay, sodium montmorillonite, and calcium montmorillonite.
In an embodiment of the present disclosure, the first surfactant and the second surfactant are independently an anionic surfactant, wherein the anionic surfactant is selected from the group consisting of sodium lauryl ether sulphate (SELS 28%), sodium lauryl sulphate, ammonium lauryl sulphate, sodium lauryl sarcosinate, sodium dodecyl sulphate, sodium myreth sulphate, sodium pareth sulphate, and magnesium laureth sulphate.
In an embodiment of the present disclosure, the aromatic tertiary amine is 2,4,6-tris (dimethyl aminomethyl) phenol (Lapox AC 14).
In an embodiment of the present disclosure, the preservative is a mixture of formaldehyde, methyl chloride, and methylisothiazolinone.
In an embodiment of the present disclosure, the thixotropic agent is fumed silica (Aerosil 200).
In an embodiment of the present disclosure, the base resin have an epoxy equivalent weight in the range of 180 g/mol to 190 g/mol, the base resin have viscosity in the range of 10000 centipoise to 15000 centipoise, the pre-polymer have a reactive content in is in the range of 2.4 mass% to 2.7 mass% with respect to the total mass of the pre-polymer, wherein the reactive content is an isocyanate group, and the pre-polymer have an epoxy equivalent weight in the range of 900 g/mol to 930g/mol.
In an embodiment of the present disclosure, the accelerated curing agent have an amine value in the range of 580 mg KOH/gm to 650 mg KOH/gm, the hardener resin have an amine value in the range of 390 mg KOH/gm to 450 mg KOH/gm, and the thixotropic agent have a specific area in the range of 150 m2/gm to 250 m2/gm.
In an embodiment of the present disclosure, the first surfactant and the second surfactant independently have hydrophilic–lipophilic balance (HLB) value in the range of 8 to 16, and the first filler and the second filler independently have a particle size in the range of 1 micron to 15 micron.
In another aspect the present disclosure, provides a process for the preparation of an adhesive composition. The process comprises the steps of:
(A) preparing a base component by the following steps:
i) charging a predetermined amount of water in a first mixer followed by adding a predetermined amount of a base resin under stirring and sequentially adding predetermined amounts of a plasticizer, a pre-polymer, a first surfactant, and a pigment under stirring at a first predetermined speed to obtain an intermediate mixture; and
ii) adding predetermined amounts of a first rheology modifier, a first filler, and a preservative to the intermediate mixture under stirring at a second predetermined speed to obtain the base component;
(B) preparing a hardener component by the following steps:
(a) charging a predetermined amount of a hardener resin in a second mixer followed by adding a predetermined amount of an accelerated curing agent under stirring and adding predetermined amounts of a second surfactant and a second pigment under stirring at a third predetermined speed to obtain a resultant mixture; and
(b) sequentially adding predetermined amounts of a second rheology modifier, a second filler and a thixotropic agent in the resultant mixture under stirring at a fourth predetermined speed to obtain the hardener component; and
(C) mixing the base component and the hardener component in a predetermined mass ratio to obtain the adhesive composition prior to application on a substrate.
In an embodiment of the present disclosure, the predetermined amount of water is in the range of 1 mass% to 5 mass% with respect to total mass of the base component.
In an embodiment of the present disclosure, the base resin is selected from unmodified liquid epoxy resin.
In an embodiment of the present disclosure, the predetermined amount of the base resin is in the range of 10 mass% to 25 mass% % with respect to total mass of the base component.
In an embodiment of the present disclosure, the plasticizer is selected from the group consisting of alkyl sulphonic acid ester, esters of phthalic acid, diethylehexyl terephthalate, diisononyl cyclohexane dicarboxylate, and biobased plasticizers based on epoxidized plant oils, cardanol, and citrates.
In an embodiment of the present disclosure, the predetermined amount of the plasticizer is in the range of 12 mass% to 25 mass% with respect to total mass of the base component.
In an embodiment of the present disclosure, the prepolymer is selected from the group consisting of blocked polyoxypropylene glycol and toluene diisocyanate, and branched polymer with ether and urethane groups based on blocked polyoxypropylene glycol and toluene diisocyanate, wherein the polyoxypropylene glycol and toluene diisocyanate is blocked with at least one component selected from alkyl phenol and renewable blocking agent, and wherein the renewable blocking agent is cashew nutshell liquid.
In an embodiment of the present disclosure, the predetermined amount of the pre-polymer is in the range of 5 mass% to 15 mass% with respect to total mass of the base component.
In an embodiment of the present disclosure, the first surfactant is an anionic surfactant, wherein the anionic surfactant is selected from the group consisting of sodium lauryl ether sulphate, sodium lauryl sulphate, ammonium lauryl sulphate, sodium lauryl sarcosinate, sodium dodecyl sulphate, sodium myreth sulphate, sodium pareth sulphate, and magnesium laureth sulphate.
In an embodiment of the present disclosure, the predetermined amount of the first surfactant is in the range of 2 mass% to 4 mass% with respect to the total mass of the base component.
In an embodiment of the present disclosure, the first pigment is titanium dioxide.
In an embodiment of the present disclosure, the predetermined amount of the first pigment is in the range of 1 mass% to 5 mass% with respect to total mass of the base component.
In an embodiment of the present disclosure, the first rheology modifier is selected from the group consisting of bentonite clay, sodium montmorillonite, and calcium montmorillonite.
In an embodiment of the present disclosure, the first rheology modifier is in the range of 0.5 mass% to 3 mass% with respect to the total mass of the base component.
In an embodiment of the present disclosure, the first filler is a carbonate mineral, wherein the carbonate mineral is calcium carbonate (calcite powder).
In an embodiment of the present disclosure, the predetermined amount of the first filler is in the range of 45 mass% to 65 mass% with respect to total mass of the base component.
In an embodiment of the present disclosure, the first preservative is selected from formaldehyde, methyl chloride, and methylisothiazolinone.
In an embodiment of the present disclosure, the predetermined amount of the first preservative is in the range of 0.1 mass% to 0.5 mass% with respect to total mass of the base component.
In an embodiment of the present disclosure, the hardener resin is selected from the group consisting of aliphatic polyamide, modified aliphatic polyamide, aromatic polyamide, modified aromatic polyamide, primary polyamide, secondary polyamide, and tertiary polyamide.
In an embodiment of the present disclosure, the predetermined amount of the hardener resin is in the range of 20 mass% to 40 mass% with respect to total mass of the hardener component.
In an embodiment of the present disclosure, the accelerated curing agent is an aromatic tertiary amine, and the aromatic tertiary amine is 2,4,6-tris (dimethyl aminomethyl) phenol.
In an embodiment of the present disclosure, the predetermined amount of the accelerated curing agent is in the range of 1 mass% to 4 mass% with respect to total mass of the hardener component.
In an embodiment of the present disclosure, the second surfactant is an anionic surfactant, wherein the anionic surfactant is selected from the group consisting of sodium lauryl ether sulphate, sodium lauryl sulphate, ammonium lauryl sulphate, sodium lauryl sarcosinate, sodium dodecyl sulphate, sodium myreth sulphate, sodium pareth sulphate, and magnesium laureth sulphate.
In an embodiment of the present disclosure, the predetermined amount of the second surfactant is in the range of 1 mass% to 3.5 mass% with respect to the total mass of the hardener component.
In an embodiment of the present disclosure, the second pigment is titanium dioxide.
In an embodiment of the present disclosure, the predetermined amount of the second pigment is in the range of 1 mass% to 3 mass% with respect to total mass of the hardener component.
In an embodiment of the present disclosure, the second rheology modifier is selected from the group consisting of bentonite clay, sodium montmorillonite, and calcium montmorillonite.
In an embodiment of the present disclosure, the predetermined amount of the second rheology modifier is in the range of 1 mass% to 5 mass% with respect to the total mass of the hardener component.
In an embodiment of the present disclosure, the second filler is a carbonate mineral, wherein the carbonate mineral is calcium carbonate (calcite powder).
In an embodiment of the present disclosure, the predetermined amount of the second filler is in the range of 55 mass% to 75 mass% with respect to total mass of the hardener component.
In an embodiment of the present disclosure, the thixotropic agent is fumed silica.
In an embodiment of the present disclosure, the predetermined amount of the thixotropic agent is in the range from 0.1 mass% to 3 mass% with respect to the total amount of the hardener component.
In an embodiment of the present disclosure, the substrate is selected from the group consisting of concrete wall, plaster wall, glass panel, metal panel, wooden panel, plaster board, and gypsum board.
In an embodiment of the present disclosure, the stirring is performed after adding each ingredient for a time period in the range of 5 minutes to 30 minutes, the first predetermined speed is in the range of 200 rpm to 400 rpm, the second predetermined speed is in the range of 800 rpm to 1200 rpm, the third predetermined speed is in the range of 200 rpm to 400 rpm, and the fourth predetermined speed is in the range of 800 rpm to 1200 rpm
In an embodiment of the present disclosure, the mass ratio of the base component to the hardener component is in the range of 3:1 to 7:1.
DETAILED DESCRIPTION
The present disclosure relates to an adhesive composition and a process for its preparation.
Embodiments are provided so as to thoroughly and fully convey the scope of the present disclosure to the person skilled in the art. Numerous details are set forth, relating to specific components, and methods, to provide a complete understanding of embodiments of the present disclosure. It will be apparent to the person skilled in the art that the details provided in the embodiments should not be construed to limit the scope of the present disclosure. In some embodiments, well-known processes, well-known apparatus structures, and well-known techniques are not described in detail.
The terminology used, in the present disclosure, is only for the purpose of explaining a particular embodiment and such terminology shall not be considered to limit the scope of the present disclosure. As used in the present disclosure, the forms "a,” "an," and "the" may be intended to include the plural forms as well, unless the context clearly suggests otherwise. The terms "comprises," "comprising," “including,” and “having,” are open ended transitional phrases and therefore specify the presence of stated features, integers, steps, operations, elements, modules, units and/or components, but do not forbid the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. The particular order of steps disclosed in the method and process of the present disclosure is not to be construed as necessarily requiring their performance as described or illustrated. It is also to be understood that additional or alternative steps may be employed.
As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed elements.
The terms first, second, third, etc., should not be construed to limit the scope of the present disclosure as the aforementioned terms may be only used to distinguish one element, component, region, layer or section from another component, region, layer or section. Terms such as first, second, third etc., when used herein do not imply a specific sequence or order unless clearly suggested by the present disclosure.
There are many types of adhesive compositions such as cementitious tile adhesive, dispersion tile adhesive, epoxy tile adhesive, and the like available in the market for masonry applications. However, these conventional adhesives are suitable for only single application i.e. fixing tiles.
The conventional adhesive compositions does not have the properties that can provide waterproof coating against rising dampness on the concrete walls, stain resistance, and the like. Different compositions are required for different applications that increase the cost and time. Moreover, these different compositions require different solvent which are toxic, flammable, and add on to the cost of the product.
The present disclosure provides an adhesive composition and a process for its preparation.
The adhesive composition comprises a base component comprising a predetermined amount of a base resin, a predetermined amount of a plasticizer, a predetermined amount of a pre-polymer, a predetermined amount of a first filler, a predetermined amount of a first pigment, a predetermined amount of a first additive, and q.s water, and a hardener component comprising a predetermined amount of a hardener resin, a predetermined amount of an accelerated curing agent, a predetermined amount of a second filler, a predetermined amount of a second pigment, and a predetermined amount of a second additive.
In an embodiment of the present disclosure, a mass ratio of the base component to the hardener component is in the range of 3:1 to 7:1 prior to application on a substrate. In an exemplary embodiment of the present disclosure, the mass ratio of the base component to the hardener component is in the range of 4:1 (80:20) prior to application on a substrate.
In an embodiment of the present disclosure, the substrate is selected from the group consisting of concrete wall, plaster wall, glass panel, metal panel, wooden panel, plaster board, and gypsum board.
In an embodiment of the present disclosure, the base resin is unmodified liquid epoxy resin (bisphenol A diglycidyl ether) (Lapox B11).
In an embodiment of the present disclosure, the base resin have an epoxy equivalent weight in the range of 180 g/mol to 190 g/mol.
In an embodiment of the present disclosure, the base resin can have a viscosity in the range of 10000 centipoise to 15000 centipoise.
In an embodiment of the present disclosure, the predetermined amount of the base resin is in the range of 10 mass% to 25 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the base resin is in the range of 12 mass% to 20 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the base resin is 14.1 mass%.
In an embodiment of the present disclosure, the plasticizer is selected from the group consisting of alkyl sulphonic acid ester, esters of phthalic acid, diethylehexyl terephthalate, diisononyl cyclohexane dicarboxylate, and biobased plasticizers based on epoxidized plant oils, cardanol, and citrates. In an exemplary embodiment of the present disclosure, the plasticizer is esters of phthalic acid.
In an exemplary embodiment of the present disclosure, the esters of phthalic acid is phthalic acid dibutyl ester.
In an embodiment of the present disclosure, the predetermined amount of the plasticizer is in the range of 12 mass% to 25 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the plasticizer is in the range of 15 mass% to 20 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the plasticizer is 15.45 mass%.
In an embodiment of the present disclosure, the pre-polymer is selected from the group consisting of blocked polyoxypropylene glycol and toluene diisocyanate and branched polymer with ether and urethane groups based on blocked polyoxypropylene glycol and toluene diisocyanate.
In an embodiment of the present disclosure, the polyoxypropylene glycol and toluene diisocyanate is blocked with at least one component selected from alkyl phenol and renewable blocking agent, and wherein the renewable blocking agent is cashew nutshell liquid. In an exemplary embodiment of the present disclosure, the prepolymer is branched polymer with ether and urethane groups based on blocked isocyanates (DESMOCAP 14 CNB).
In an embodiment of the present disclosure, the pre-polymer have a reactive content in the range of 2.4 mass % to 2.7 mass% with respect to the total mass of the pre-polymer.
In accordance with the present disclosure, the reactive content in the pre-polymer is an isocyanate group.
In an embodiment of the present disclosure, the pre-polymer have epoxy equivalent weight in the range of 900 g/mol to 930 g/mol.
In an embodiment of the present disclosure, the predetermined amount of the pre-polymer is in the range of 5 mass% to 15 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the pre-polymer is in the range of 8 mass% to 10 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the pre-polymer is 9.4 mass% with respect to the total mass of the base component.
In an embodiment of the present disclosure, the first filler is a carbonate mineral, wherein the carbonate mineral is calcium carbonate (calcite powder)(Micron Carb 1240).
In an embodiment of the present disclosure, the particle size of the first filler is in range of 1 micron to 15 micron.
In an embodiment of the present disclosure, the predetermined amount of the first filler is in the range of 45 mass% to 65 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the first filler is in the range of 50 mass% to 60 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the first filler is 51.25 mass% with respect to the total mass of the base component.
In an embodiment of the present disclosure, the first pigment is titanium dioxide (Nanotox 207).
In an embodiment of the present disclosure, colorants are incorporated to impart color to the adhesive composition.
In an embodiment of the present disclosure, the colorants are selected from the group consisting of purple, blue, green, yellow, orange, red, brown, black, white, and fluorescent colors.
In an embodiment of the present disclosure, the predetermined amount of the first pigment is in the range of 1 mass% to 5 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the first pigment is in the range of 2 mass% to 4 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the first pigment is 3.53 mass% with respect to the total mass of the base component.
In an embodiment of the present disclosure, the first additive is selected from first rheology modifier, a first surfactant, and a preservative.
In an embodiment of the present disclosure, the predetermined amount of the first additive is in the range of 2 mass% to 10 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the first additive is in the range of 3 mass% to 6 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the first additive is present in an amount of 4.27 mass%.
In an embodiment of the present disclosure, the first rheology modifier is selected from the group consisting of bentonite clay, sodium montmorillonite, and calcium montmorillonite. In an embodiment of the present disclosure, the first rheology modifier is bentonite clay.
In an embodiment of the present disclosure, the predetermined amount of the first rheology modifier is in the range of 0.5 mass% to 3 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the first rheology modifier is in the range of 1 mass% to 2 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the first rheology modifier is 1.17 mass% with respect to the total mass of the base component.
In an embodiment of the present disclosure, the first surfactant is an anionic surfactant, wherein the anionic surfactant is selected from the group consisting of sodium lauryl ether sulphate (Sles 28%), sodium lauryl sulphate, ammonium lauryl sulphate, sodium lauryl sarcosinate, sodium dodecyl sulphate, sodium myreth sulphate, sodium pareth sulphate, and magnesium laurate sulphate. In an exemplary embodiment of the present disclosure, the first surfactant is sodium lauryl ether sulphate liquid.
In an embodiment of the present disclosure, the first surfactant have hydrophilic–lipophilic balance (HLB) value in the range of 8 to 16.
In an embodiment of the present disclosure, the predetermined amount of the first surfactant is in the range of 2 mass% to 4 mass% with respect to the total mass of the base component. In an embodiment of the present disclosure, the predetermined amount of the first surfactant is in the range of 2.5 mass% to 3 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the first surfactant is 2.9 mass% with respect to the total mass of the base component.
In an embodiment of the present disclosure, the preservative is a mixture of formaldehyde, methyl chloride, and methylisothiazolinone (Nipacide CFX 2).
In an embodiment of the present disclosure, the predetermined amount of the preservative is in the range of 0.1 mass% to 0.5 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the preservative is in the range of 0.2 mass% to 0.3 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the preservative is 0.2 mass% with respect to the total mass of the base component.
In an embodiment of the present disclosure, water is selected from UV treated water, demineralized water, and reverse osmosis (RO) water. In an exemplary embodiment of the present disclosure, water is UV treated water.
In an embodiment of the present disclosure, the hardener resin is selected from the group consisting of aliphatic polyamide, modified aliphatic polyamide, aromatic polyamide, modified aromatic polyamide, primary polyamide, secondary polyamide, and tertiary polyamide. In an exemplary embodiment of the present disclosure, the hardener resin is an aliphatic polyamide (Synopol). In an embodiment of the present disclosure, the hardener resin have an amine value in the range of 390 mg KOH/gm to 450 mg KOH/gm.
In an embodiment of the present disclosure, the predetermined amount of the hardener resin is in the range of 20 mass% to 40 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the hardener resin is in the range of 25 mass% to 30 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the hardener resin is 28 mass%.
In an embodiment of the present disclosure, the accelerated curing agent is an aromatic tertiary amine.
In an embodiment of the present disclosure, the aromatic tertiary amine is 2,4,6-tris(dimethyl aminomethyl) phenol (Lapox AC 14).
In an embodiment of the present disclosure, the accelerated curing agent have an amine value in the range of 580 mg KOH/gm to 650 mg KOH/gm.
In an embodiment of the present disclosure, the predetermined amount of the accelerated curing agent is in the range of 1 mass% to 4 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the accelerated curing agent is in the range of 1.5 mass% to 3 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the accelerated curing agent is 2 mass% with respect to the total mass of the hardener component.
In an embodiment of the present disclosure, the second filler is a carbonate mineral, wherein the carbonate mineral is calcium carbonate (calcite powder).
In an embodiment of the present disclosure, the particle size of the second filler is in range of 1 micron to 15 micron.
In an embodiment of the present disclosure, the predetermined amount of the second filler is in the range of 55 mass% to 75 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the second filler is in the range of 60 mass% to 70 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the second filler is 64 mass% with respect to the total mass of the hardener component.
The second filler have a particle size in the range of 1 micron to 15 micron.
In an embodiment of the present disclosure, the second pigment is titanium dioxide (NONOTOX 207).
In an embodiment of the present disclosure, colorants are incorporated to impart color to the adhesive composition.
In an embodiment of the present disclosure, the colorants are selected from the group consisting of purple, blue, green, yellow, orange, red, brown, black, white, and fluorescent colors.
The pigment provides color, opacity, and gloss to the adhesive composition.
In an embodiment of the present disclosure, the predetermined amount of the second pigment is in the range of 1 mass% to 3 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the second pigment is in the range of 1.5 mass% to 2 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the second pigment is 1.5 mass% with respect to the total mass of the hardener component.
In an embodiment of the present disclosure, the second additive is selected from the group consisting of second rheology modifier, a second surfactant, and a thixotropic agent. In an exemplary embodiment of the present disclosure, the second additive is a mixture of second rheology modifier, a second surfactant, and a thixotropic agent.
In an embodiment of the present disclosure, the predetermined amount of the second additive is in the range of 1 mass% to 10 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the second additive is in the range of 3.7 mass% to 7 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the second additive is 4.5 mass% with respect to the total mass of the hardener component.
In an embodiment of the present disclosure, the second rheology modifier is selected from the group consisting of bentonite clay, sodium montmorillonite, and calcium montmorillonite. In an exemplary embodiment of the present disclosure, the second rheology modifier is bentonite clay (Riobent SD 2).
In an embodiment of the present disclosure, the predetermined amount of the second rheology modifier is in the range of 1 mass% to 5 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the second rheology modifier is in the range of 1.5 mass% to 3 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the second rheology modifier is 1.75 mass% with respect to the total mass of the hardener component.
In an embodiment of the present disclosure, the second surfactant is an anionic surfactant, wherein the anionic surfactant is selected from the group consisting of sodium lauryl ether sulphate (SELS 28%), sodium lauryl sulphate, ammonium lauryl sulphate, sodium lauroyl sarcosinate, sodium dodecyl sulphate, sodium myreth sulphate, sodium pareth sulphate, and magnesium laureth sulphate. In an exemplary embodiment of the present disclosure, the second surfactant is sodium lauryl ether sulphate (SELS 28%).
In an embodiment of the present disclosure, the second surfactant has hydrophilic–lipophilic balance (HLB) value in the range of 8 to 16.
In an embodiment of the present disclosure, the predetermined amount of the second surfactant is in the range of 1 mass% to 3.5 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the second surfactant is in the range of 1.7 mass% to 2 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the second surfactant is 1.75 mass% with respect to the total mass of the hardener component.
In an embodiment of the present disclosure, the thixotropic agent is fumed silica. In an exemplary embodiment of the present disclosure, the thixotropic agent is hydrophilic fumed silica (Aerosil 200).
In an embodiment of the present disclosure, the predetermined amount of the thixotropic agent is in the range from 0.1 mass% to 3 mass% with respect to the total amount of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the thixotropic agent is in the range from 0.5 mass% to 2 mass% with respect to the total amount of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the thixotropic agent is 1 mass% with respect to the total amount of the hardener component.
In an embodiment of the present disclosure, the thixotropic agent have a specific surface area in the range of 150 m2/gm to 250 m2/gm.
In an embodiment of the present disclosure, the thixotropic agent have a particle size in the range of 8 nm to 15 nm.
In another aspect, the present disclosure provides a process for the preparation of an adhesive composition.
The process comprises the steps of:
(A) preparing a base component by the following steps:
i) charging a predetermined amount of water in a first mixer followed by adding a predetermined amount of a base resin under stirring at a first predetermined speed and sequentially adding predetermined amounts of a plasticizer, a pre-polymer, a first surfactant, and a pigment under stirring at the first predetermined speed to obtain an intermediate mixture;
ii) adding predetermined amounts of a first rheology modifier, a first filler, and a preservative to the intermediate mixture under stirring at a second predetermined speed to obtain the base component;
(B) preparing a hardener component by the following steps:
(a) charging a predetermined amount of a hardener resin in a second mixer followed by adding a predetermined amount of an accelerated curing agent under stirring at a third predetermined speed and adding predetermined amounts of a second surfactant and a second pigment under stirring at the third predetermined speed to obtain a resultant mixture; and
(b) sequentially adding predetermined amounts of a second rheology modifier, a second filler and a thixotropic agent in the resultant mixture under stirring at a fourth predetermined speed to obtain the hardener component; and
(C) mixing the base component and the hardener component in a predetermined mass ratio to obtain the adhesive composition prior to the application on a substrate.
The process is described in detail.
In a first step of preparing a base component, a predetermined amount of water is charged in a first mixer followed by adding a predetermined amount of a base resin under stirring and sequentially predetermined amounts of a plasticizer, a pre-polymer, a first surfactant, and a pigment are added under stirring at a first predetermined speed to obtain an intermediate mixture.
In an embodiment of the present disclosure, the first predetermined stirring speed is in the range of 200 rpm to 400 rpm. In an exemplary embodiment of the present disclosure, the first predetermined stirring speed is 300 rpm.
In an embodiment of the present disclosure, water is selected from the group consisting of UV treated water, demineralized water, and reverse osmosis (RO) water. In an exemplary embodiment of the present disclosure, water is UV treated water.
In an embodiment of the present disclosure, the predetermined amount of water is in the range of 1 mass% to 5 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the water is in the range of 2 mass% to 4 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of water is 2 mass% with respect to the total mass of the base component.
In accordance with the present disclosure, the other ingredients get dispersed in water. In accordance with the present disclosure, water, base resin (epoxy resin), and pre-polymer are mixed to make sufficient quantity to disperse the pigments and fillers.
Addition of small amount of water along with the epoxy resin and the pre-polymer during the process of preparing the base component improves the dispersion of pigments and fillers in the adhesive composition.
In an embodiment of the present disclosure, the base resin is unmodified liquid epoxy resin (bisphenol A diglycidyl ether).
In an embodiment of the present disclosure, the base resin have epoxy equivalent weight in the range of 180g/mol to190g/mol.
In an embodiment of the present disclosure, the base resin have viscosity in the range of 10000 centipoise to 15000 centipoise.
The base resin reacts with the hardener resin to form a crosslinked adhesive composition which provides adhesion properties and waterproofing properties, to the film obtained from the adhesive composition.
In accordance with the present disclosure, the reaction proceeds through by abstraction of hydrogen atom from the secondary alcohol of tertiary amine by epoxy group that results into ether linkage. Branched polymer having ether and urethane groups with blocked isocyanates reacts with hydroxy functions in amine crosslinkers and epoxy resins to form hybrid epoxy urethane polymers with (-NH-COO) urethane linkage. Incorporation of branched polymer having ether and urethane groups with blocked isocyanate imparts flexibility to the film (epoxy amine cured film) obtained by applying the adhesive composition of the present disclosure. The reaction is represented by scheme I as:
………. (I)
In an embodiment of the present disclosure, the predetermined amount of the base resin is in the range of 10 mass% to 25 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the base resin is in the range of 12 mass% to 20 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the base resin is 14.1 mass% with respect to the total mass of the base component
In an embodiment of the present disclosure, the first mixer is selected from the group consisting of pug mill, and high speed disperser. In an exemplary embodiment of the present disclosure, the mixer is high speed disperser.
In an embodiment of the present disclosure, the plasticizer is selected from the group consisting of alkyl sulphonic acid ester, esters of phthalic acid, diethylehexyl terephthalate, diisononyl cyclohexane dicarboxylate, and biobased plasticizers based on epoxidized plant oils, cardanol, and citrates. In an exemplary embodiment of the present disclosure, the plasticizer is esters of phthalic acid.
In an exemplary embodiment of the present disclosure, the esters of phthalic acid is phthalic acid dibutyl ester.
In an embodiment of the present disclosure, the predetermined amount of the plasticizer is in the range of 12 mass% to 25 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the plasticizer is in the range of 15 mass% to 20 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the plasticizer is 15.45 mass% with respect to the total mass of the base component.
The plasticizer present in the adhesive composition imparts flexibility to the film.
In an embodiment of the present disclosure, the pre-polymer is selected from the group consisting of blocked polyoxypropylene glycol and toluene diisocyanate and branched polymer with ether and urethane groups based on blocked polyoxypropylene glycol and toluene diisocyanate.
In an embodiment of the present disclosure, the polyoxypropylene glycol and toluene diisocyanate is blocked with at least one component selected from alkyl phenol and renewable blocking agent, and wherein the renewable blocking agent is cashew nutshell liquid. In an exemplary embodiment of the present disclosure, the prepolymer is branched polymer with ether and urethane groups based on blocked isocyanates.
In an embodiment of the present disclosure, the pre-polymer have a reactive content in the range of 2.4 mass % to 2.7 mass% with respect to the total mass of the pre-polymer.
In accordance with the present disclosure, the reactive content in the pre-polymer is an isocyanate group.
In an embodiment of the present disclosure, the pre-polymer have the epoxy equivalent weight in the range of 900 g/mol to 930g/mol.
In an embodiment of the present disclosure, the predetermined amount of the pre-polymer is in the range of 5 mass% to 15 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the pre-polymer is in the range of 8 mass% to 10 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the pre-polymer is 9.4 mass% with respect to the total mass of the base component.
The pre-polymer used in the composition reacts with epoxy groups and amine groups thereby providing adhesion properties and waterproofing properties to the film obtained by applying the adhesive composition of the present disclosure.
In an embodiment of the present disclosure, the first surfactant is an anionic surfactant. The anionic surfactant is selected from the group consisting of sodium lauryl ether sulphate, sodium lauryl sulphate, ammonium lauryl sulphate, sodium lauroyl sarcosinate, sodium dodecyl sulphate, sodium myreth sulphate, sodium pareth sulphate, and magnesium laureth sulphate. In an exemplary embodiment of the present disclosure, the first surfactant is sodium lauryl ether sulphate.
In an embodiment of the present disclosure, the first surfactant have hydrophilic–lipophilic balance (HLB) value in the range of 8 to 16.
The anionic surfactant used in the composition reduces the surface tension between the base resin and water. Further, the anionic surfactant also reduces the surface tension between the first fillers and the first pigments and helps them to disperse in the adhesive composition.
In an embodiment of the present disclosure, the predetermined amount of the first surfactant is in the range of 2 mass% to 4 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the first surfactant is in the range of 2.5 mass% to 3 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the first surfactant is 2.9 mass% with respect to the total mass of the base component.
In an embodiment of the present disclosure, the first pigment is titanium dioxide
In an embodiment of the present disclosure, the predetermined amount of the first pigment is in the range of 1 mass% to 5 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the first pigment is in the range of 2 mass% to 4 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the first pigment is 3.53 mass% with respect to the total mass of the base component.
In a second step of preparing the base component, a predetermined amount of a first rheology modifier, a first filler, and a preservative is added to the intermediate mixture under stirring at a second predetermined speed to obtain the base component.
In an embodiment of the present disclosure, the first rheology modifier is selected from the group consisting of bentonite clay, sodium montmorillonite, and calcium montmorillonite. In an exemplary embodiment of the present disclosure, the first rheology modifier is bentonite clay.
The rheology modifiers are used for their swelling capacity. The rheology modifier swells and imparts desired in-can and application rheology to the adhesive composition.
In an embodiment of the present disclosure, the predetermined amount of the first rheology modifier is in the range of 0.5 mass% to 3 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the first rheology modifier is in the range of 1 mass% to 2 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the first rheology modifier is 1.17 mass% with respect to the total mass of the base component.
In an embodiment of the present disclosure, the second predetermined speed is in the range of 800 rpm to 1200 rpm. In an exemplary embodiment of the present disclosure, the second predetermined speed is 1000 rpm.
In an embodiment of the present disclosure, the first filler is a carbonate mineral. The carbonate is calcium carbonate (calcite powder).
In an embodiment of the present disclosure, the particle size of the first filler is in range of 1 micron to 15 microns.
In an embodiment of the present disclosure, the predetermined amount of the first filler is in the range of 45 mass% to 65 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the first filler is in the range of 50 mass% to 60 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the first filler is 51.25 mass% with respect to the total mass of the base component
The first filler used in the adhesive composition act as a thickening agent in the adhesive composition, fills the gap between pigment particles and increase the volume of the adhesive composition.
In an embodiment of the present disclosure, the preservative is a mixture of formaldehyde, methyl chloride, and methylisothiazolinone (Nipacide CF X2).
In an embodiment of the present disclosure, the predetermined amount of the preservative is in the range of 0.1 mass% to 0.5 mass% with respect to the total mass of the base component. In a particular embodiment of the present disclosure, the predetermined amount of the preservative is in the range of 0.2 mass% to 0.3 mass% with respect to the total mass of the base component. In an exemplary embodiment of the present disclosure, the predetermined amount of the preservative is 0.2 mass% with respect to the total mass of the base component.
The preservative used in the composition prevents the growth of bacteria and fungus in the base component.
In a first step of preparing the hardener component, a predetermined amount of a hardener resin is charged in a second mixer followed by adding a predetermined amount of an accelerated curing agent under stirring and adding predetermined amounts of a second surfactant and a second pigment under stirring at a third predetermined speed to obtain a resultant mixture.
In an embodiment of the present disclosure, the third predetermined stirring speed is in the range of 200 rpm to 400 rpm. In an exemplary embodiment of the present disclosure, the third predetermined stirring speed is 300 rpm
In an embodiment of the present disclosure, the hardener resin is selected from the group consisting of aliphatic polyamide, modified aliphatic polyamide, aromatic polyamide, modified aromatic polyamide, primary amine, secondary amine, and tertiary amine. In an exemplary embodiment of the present disclosure, the hardener resin is aliphatic polyamide (Synopol 160).
In an embodiment of the present disclosure, the hardener resin have an amine value in the range of 390 mg KOH/gm to 450 mg KOH/gm.
In an embodiment of the present disclosure, the predetermined amount of the hardener resin is in the range of 20 mass% to 40 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the hardener resin is in the range of 25 mass% to 30 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the hardener resin is 28 mass% with respect to the total mass of the hardener component.
The hardener resin used in the composition reacts with a base resin wherein the hardener resin opens epoxide ring of the base resin and form the desired structure which gives adhesion and waterproofing properties to the film obtained by applying the adhesive composition of the present disclosure.
In an embodiment of the present disclosure, the accelerated curing agent is an aromatic tertiary amine. In an embodiment of the present disclosure, the aromatic tertiary amine is 2,4,6-tris (dimethyl aminomethyl) phenol (Lapox Ac 14).
In an embodiment of the present disclosure, the accelerated curing agent have an amine value in the range of 580 mg KOH/gm to 650 mg KOH/gm.
The accelerated curing agents used in the adhesive composition of the present disclosure help to increase the reaction speed of the base component and the hardener component by providing extra reactive site to the base resin.
In an embodiment of the present disclosure, the predetermined amount of the accelerated curing agent is in the range of 1 mass% to 4 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the accelerated curing agent is in the range of 1.5 mass% to 3 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the accelerated curing agent is 2 mass% with respect to the total mass of the hardener component.
In an embodiment of the present disclosure, the second mixer is selected from the group consisting of pug mill, and high-speed disperser.
In an embodiment of the present disclosure, the second surfactant is an anionic surfactant. The anionic surfactant is selected from the group consisting of sodium lauryl ether sulphate, sodium lauryl sulphate, ammonium lauryl sulphate, sodium lauroyl sarcosinate, sodium dodecyl sulphate, sodium myreth sulphate, sodium pareth sulphate, and magnesium laureth sulphate. In an exemplary embodiment of the present disclosure, the second surfactant is sodium lauryl ether sulphate (SELS 28%).
In an embodiment of the present disclosure, the second surfactant have hydrophilic–lipophilic balance (HLB) value in the range of 8 to 16.
The anionic surfactants used in the adhesive composition of the present disclosure reduce the surface tension between the base resin and water. Further, the anionic surfactants used in the composition of the present disclosure also reduces the surface tension between the first fillers and the first pigments and help them to disperse in the adhesive composition.
In an embodiment of the present disclosure, the predetermined amount of the second surfactant is in the range of 1 mass% to 3.5 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the second surfactant is in the range of 1.7 mass% to 2 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the second surfactant is 1.75 mass% with respect to the total mass of the hardener component.
In an embodiment of the present disclosure, the second pigment is titanium dioxide.
The pigment provides color, opacity, and gloss to the adhesive composition.
In an embodiment of the present disclosure, the predetermined amount of the second pigment is in the range of 1 mass% to 3 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the second pigment is in the range of 1.5 mass% to 2 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the second pigment is 1.5 mass% with respect to the total mass of the hardener component.
In a final step of preparing the hardener component, predetermined amounts of a second rheology modifier, a second filler and a thixotropic agent are added sequentially in the resultant mixture under stirring at a fourth predetermined speed to obtain the hardener component.
In an embodiment of the present disclosure, the fourth predetermined stirring speed is in the range of 800 rpm to 1200 rpm. In an exemplary embodiment of the present disclosure, the fourth predetermined stirring speed is 1000 rpm.
In an embodiment of the present disclosure, the second rheology modifier is selected from the group consisting of bentonite clay, sodium montmorillonite, and calcium montmorillonite. In an exemplary embodiment of the present disclosure, the second rheology modifier is bentonite clay.
In accordance with the present disclosure, the rheology modifiers is used for their swelling capacity.
Further, when the adhesive composition is kept as such (stored), the rheology modifier absorb water and becomes a thick/viscous material, which acts as a separate system in the adhesive composition (product) thereby giving in can stability to the adhesive composition. Furthermore, when the adhesive composition is applied by brush/roller/putty knife, i.e. when a pressure is applied on the adhesive composition, the adhesive composition becomes thin and easy to apply (shear thinning phenomenon).
In an embodiment of the present disclosure, the predetermined amount of the second rheology modifier is in the range of 1 mass% to 5 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the second rheology modifier is in the range of 1.5 mass% to 3 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the second rheology modifier is 1.75 mass% with respect to the total mass of the hardener component.
In an embodiment of the present disclosure, the second filler is a carbonate mineral. The carbonate mineral is calcium carbonate (calcite powder).
In an embodiment of the present disclosure, the particle size of the second filler is in range of 1 micron to 15 micron.
In an embodiment of the present disclosure, the predetermined amount of the second filler is in the range of 55 mass% to 75 mass% with respect to the total mass of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the second filler is in the range of 60 mass% to 70 mass% with respect to the total mass of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the second filler is 64 mass% with respect to the total mass of the hardener component.
The second filler used in the composition acts as a thickening agent to the adhesive composition, fills the gap between pigment particles and increase the volume of the adhesive composition.
In an embodiment of the present disclosure, the thixotropic agent is hydrophilic fumed silica (Aerosil 200).
In an embodiment of the present disclosure, the predetermined amount of the thixotropic agent is in the range from 0.1 mass% to 3 mass% with respect to the total amount of the hardener component. In a particular embodiment of the present disclosure, the predetermined amount of the thixotropic agent is in the range from 0.5 mass% to 2 mass% with respect to the total amount of the hardener component. In an exemplary embodiment of the present disclosure, the predetermined amount of the thixotropic agent is 1 mass% with respect to the total amount of the hardener component.
In an embodiment of the present disclosure, the thixotropic agent have a specific surface area in the range of 150 m2/gm to 250 m2/gm.
In an embodiment of the present disclosure, the thixotropic agent have a particle size in the range of 8 nm to 15 nm.
In accordance with the present disclosure, the thixotropic agent imparts thixotropic property to the hardener component which makes it less viscous when subjected to applied stress.
In an embodiment of the present disclosure, the stirring is performed after adding each ingredient for a time period in the range of 5 minutes to 30 minutes. In an exemplary embodiment of the present disclosure, the stirring is performed after adding each ingredient for a time period of 15 minutes.
The so obtained base component is mixed with the hardener component in a mass ratio in the range of 3:1 to 7:1 to obtain the adhesive composition. In an exemplary embodiment of the present disclosure, the so obtained base component is mixed with the hardener component in a mass ratio of 4:1 (80:20) to obtain the adhesive composition.
In an embodiment of the present disclosure, the substrate is selected from the group consisting of concrete wall, plaster wall, glass panel, metal panel, wooden panel, plaster board, and gypsum board.
In an embodiment of the present disclosure, a curing time of the adhesive composition is in the range of 20 minutes to 50 minutes. In an embodiment of the present disclosure, a curing time of the adhesive composition is in the range of 20 hours to 30 hours. In an exemplary embodiment of the present disclosure, the curing time of the adhesive composition is 24 hours.
The adhesive composition of the present disclosure, is used for tile fixing on different surfaces such as ceramic, glass, metals, wood, plasterboards, gypsum board and the like. The adhesive composition of the present disclosure is used as a waterproofing coating that is used against rising dampness on interior masonry surfaces and waterproofing membrane for below the tile application in bathroom and toilets. The hardener component and the base component are mixed in a predetermined ratio and diluted with 50% water to form brushable slurry. This slurry is applied in two coats with brush on the porous concrete panel which is replica of interior masonry wall affected by rising dampness, followed by putty and painting system. It is observed that there is no dampness.
The adhesive composition of the present disclosure is compatible with water. As it is compatible with water, the tools is easily cleaned with water.
The adhesive composition of the present disclosure is used as a waterproof coating below the tiles. It is observed that there is no water penetration from positive side of the waterproof coating. Further, the adhesive composition of the present disclosure is used as a tile grout to fill gaps between tile joints. The adhesive composition of the present disclosure, have the properties such as waterproofing, stain resistance, abrasion resistance and it is tinted with water-based pigments.
The foregoing description of the embodiments has been provided for purposes of illustration and not intended to limit the scope of the present disclosure. Individual components of a particular embodiment are generally not limited to that particular embodiment but are interchangeable. Such variations are not to be regarded as a departure from the present disclosure, and all such modifications are considered to be within the scope of the present disclosure.
The present disclosure is further described in light of the following experiments which are set forth for illustration purposes only and not to be construed for limiting the scope of the disclosure. The following experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial scale.
EXPERIMENTAL DETAILS
Experiment No 1: A process for preparation of the adhesive composition in accordance with the present disclosure.
General Procedure
(A) Process for preparation of base component.
Predetermined amount of water was charged in a high speed disperser (first mixer) followed by adding a predetermined amount of a base resin under stirring at 300 rpm and sequentially adding predetermined amounts of a plasticizer, a pre-polymer, a first surfactant, and a pigment under the stirring to obtain an intermediate mixture. Predetermined amounts of a first rheology modifier, a first filler, and a preservative were added in the intermediate mixture under stirring at 1000 rpm to obtain the base component, wherein the stirring was performed for 20 minutes after adding each ingredient.
Details of the ingredients and amounts are provided in table 1.
(B) Process for preparation of hardener component.
A predetermined amount of a hardener resin was charged in a second mixer followed by adding a predetermined amount of an accelerated curing agent under stirring at 300 rpm and adding predetermined amounts of a second surfactant and a second pigment under the stirring to obtain a resultant mixture. Predetermined amounts of a second rheology modifier, a second filler and a thixotropic agent were sequentially added in the resultant mixture under stirring at 1000 rpm to obtain the hardener component, wherein the stirring was performed for 20 minutes after adding each ingredient.
Details of the ingredients and amounts are provided in table 1.
(C) Mixing the base component and hardener component
The base component obtained in step (A) and the hardener component obtained in step (B) were mixed in a mass ratio of 80:20 (4:1) at the time of application to obtain the adhesive composition. Table 1 illustrates the details of the ingredients with their respective amounts.
Table 1: Adhesive composition in accordance with the present disclosure .
Sr. No Ingredients Function Experiment No 1
(in gm)
Trade name Chemical name
(A) Base composition
1 UV WATER Water Fluid medium 2
2 LAPOX B 11 Bisphenol A diglycidyl ether (unmodified) Base resin 14.1
3 -- Phthalic acid dibutyl ester Plasticizer 15.45
4 DESMOCAP 14 CNB Branched polymer with ether and urethane group Prepolymer 9.4
5 SLES 28% Sodium lauryl ether sulphate liquid First surfactant 2.9
6 NANOTOX 207 Titanium dioxide First pigment 3.53
7 RIOBENT SD 2 Bentonite clay First rheology modifier 1.17
8 MICRON CARB 1240 Calcium carbonate First filler 51.25
9 NIPACIDE CFX 2 Formaldehyde + chloromethyl and methylisothiazolinone Preservative 0.2
Total 100
(B) Hardener composition
1 SYNPOL 160 Polyamide resin with high amine value Hardener Resin 28
2 LAPOX AC 14 2,4,6-tris liquid (dimethyl aminomethyl) phenol Acceleraed Curing Agent 2
3 SLES 28% sodium lauryl ether sulphate liquid Second Surfactant 1.75
4 NANOTOX 207 titanium dioxide Second pigment 1.5
5 RIOBENT SD 2 bentonite clay Second rheology modifier 1.75
6 MICRON CARB 1240 calcium carbonate Second filler 64
7 AEROSIL 200 hydrophilic fumed silica Thixotropic agent 1
Total 100
Experiment No 2: Characterization of the adhesive composition.
The adhesive composition obtained in experiment 1 of the present disclosure was subjected for the evaluation of the characteristics.
• Viscosity
The adhesive composition obtained in experiment 1 was subjected for evaluation of the viscosity on a Penetrometer. The penetrometer is an instrument used to measure the consistency/viscosity of a material by assessing how deeply a standard needle or cone penetrates into the sample under specific conditions. The process is commonly used for testing the consistency/viscosity of semi-solid substances. Table 2 demonstrates the results of the viscosity measurement.
Table 2: Viscosity of the adhesive composition prepared in accordance with the present disclosure.
Sr. no Property Adhesive composition of experiment 1 of the present disclosure Conventional adhesive composition
1. Viscosity on Penetrometer 245 mm 240 mm
From table 2 it is observed that the viscosity/consistency of the adhesive composition prepared in accordance with the present disclosure is higher than the conventional adhesive composition. The higher penetrometer reading suggests that the adhesive composition has a higher consistency or tackiness, which is suitable for different applications or ensuring proper application and performance.
• Stain resistance test
The adhesive composition (paste) obtained in experiment 1 was used to fill the joints between two tiles (Maximum joined width and depth is 5x5 mm) followed by curing for 24 hours. Different stains were applied on the cured adhesive joint and were kept for 30 minutes. After 30 minutes the stains were cleaned with 5% soap solution to check if it can be removed. The results are demonstrated in table 3.
Table 3: Stain resistance test of the adhesive composition prepared in accordance with the present disclosure.
Sr. no Stain Stain resistance
Adhesive composition of experiment 1 of the present disclosure Conventional adhesive composition
1. Turmeric 8 5
2. Grease 9 7
3. Oil crayons 8 6
4. Wax crayons 8 6
5. Pen 7 6
6. Marker 7 6
7. Pencil 7 6
8. Total rating 54 42
(higher values indicates good stain resistance).
From Table 3 it is observed that the stain resistance of the adhesive composition prepared in accordance with the present disclosure is better than the stain resistance of the conventional adhesive composition.
• Taber Abrasion resistance test
The adhesive composition (paste) obtained in experiment 1 was applied at a uniform thickness on a plane, rigid panel. After curing for 7 days, the surface was abraded by rotating the panel under weighted abrasive wheels.
The abrasion resistance was calculated as “loss in weight” at a specific number of abrasion cycles, as a loss in weight per cycle, or as a number of cycles required to remove a unit amount of the adhesive thickness. The Taber abrasion test was performed by ASTM D 4060 standard test method for abrasion resistance. The results are demonstrated in table 4.
Table 4: Taber abrasion resistance of the adhesive composition prepared in accordance with the present disclosure.
Sr. no Taber abrasion resistance
(ASTM D 4060) Adhesive composition of experiment 1 of the present disclosure Conventional adhesive composition
1 Material loss in grams/1000 Cycle 4 4.8
From Table 4 it is observed that the material loss of the adhesive composition prepared in accordance with the present disclosure is less than the conventional adhesive composition. Thus, the adhesive composition prepared in accordance with the present disclosure has better abrasion resistance as compared to the conventional adhesive composition.
• Water proofing performance on walls
The adhesive composition (paste) obtained in experiment 1 was diluted with 50% water to obtain homogeneous slurry. The homogeneous slurry was applied with the help of brush on a porous concrete panel of a size 300 mm width x 300 mm length x 25 mm thickness followed by curing for 2 hours to obtain a first coat. Similar another coat of freshly prepared adhesive slurry (homogeneous paste diluted with 50% water) was applied on the first coat followed by curing for 24 hours to obtain a second coat.
Two coats of the cement putty were applied over the second coat by keeping the gap of 4 hours to 6 hours between two coats (two coats of cement putty) followed by drying for 24 hours to obtain a putty coat.
An interior water based primer at 100% dilution was applied over the putty coat followed by drying for 4 hours to 6 hours to obtain a primer coat.
Two coats of topcoat (Interior paint) at 40% dilution with water were applied on the primer coat by keeping a gap of 4 hours to 6 hours between the two coats to obtain a top coat on the panel. The top coat on the panel was allowed to cure at 25±50 ºC and relative humidity 55±5 for 7 days to obtain cured panels. The cured panels were kept in water tray for 7 days in such a way that 75% panel were deeped in water, observed the panel for dampness and efflorescence. The results are demonstrated in table 5.
Table 5: Water proofing properties (on walls) of the adhesive composition prepared in accordance with the present disclosure.
Sr. no Properties Adhesive composition of experiment 1 of the present disclosure Conventional adhesive composition
1. Rising Dampness No dampness observed (Tested for 28 days then discarded) Dampness observed after 24 hours
2. Efflorescence No efflorescence observed (Tested for 28 days then discarded) Efflorescence observed after 48 hours
From Table 5 it is observed that the adhesive composition prepared in accordance with the present disclosure have excellent dampness resistance than the conventional adhesive composition. Further the adhesive composition prepared in accordance with the present disclosure has excellent efflorescence resistance than the conventional adhesive composition.
• Water proofing performance below the tiles
The adhesive composition (paste) obtained in experiment 1 was diluted with 50% water to obtain homogeneous slurry. The slurry was applied with the help of brush on a porous concrete panel (size 300 mm width x 300 mm length x 25 mm thickness) followed by curing for 2 hours to obtain a first coat. Similar another coat of freshly prepared adhesive slurry (homogeneous paste diluted with 50% water) was applied on the first coat followed by curing for 24 hours to obtain a second coat.
A cementitious tile adhesive was applied on the second coat to fix tiles on it. (Replica of bathroom/toilet floor). Further, tile gaps were filled with cementitious tile grout followed by curing for 7 days and fixing square shape ponding accessories over it with the help of silicone sealant and curing for 24 hours and adding water to cheek if there was any water coming from other side of the porous concrete panel. The results are demonstrated in table 6.
Table 6: Water proofing properties (below the tiles) of the adhesive composition prepared in accordance with the present disclosure.
Sr. no Properties Adhesive composition of experiment 1 of the present disclosure Conventional adhesive composition
1. Rising Dampness No damp patches observed (Tested for 28 days then discarded) Damp patches observed after 2 days of application
From Table 6 it is observed that the adhesive composition prepared in accordance with the present disclosure shows excellent waterproofing properties when applied below the tile as compared to the conventional adhesive composition.
• Tensile adhesion test
The adhesive composition (paste) obtained in experiment 1 was applied on a concrete tile (M25 grade) followed by notching with 6 mm notcher and fixing 50 mm tile over it and cured for 24 hours.
A 50 mm dolly was applied over the 50 mm tile with epoxy adhesive (Araldite) and cured for 13 days to obtain an assembly of the dolly and tile. The dolly was pulled with the help of pull off adhesion tester to check how much force is required to remove this assembly of dolly and tile from the bond/adhesion formed between the tiles. The results are demonstrated in table 7.
Table 7: Tensile adhesion test of the adhesive composition prepared in accordance with the present disclosure.
Sr. no Properties Adhesive composition of experiment 1 of the present disclosure Conventional adhesive composition
1. Tensile adhesion test
IS 15477:2019
(dry condition) 2.74 Mpa 1.04 Mpa
From Table 7 it is observed that the adhesive composition of the present disclosure have better tensile adhesion as compared to the conventional adhesive composition.
• Shear Adhesion test
The adhesive composition (paste) obtained in experiment 1 was applied on two ceramic tiles of dimensions10 cm length x 10 cm breadth with the help of 6 mm notcher followed by fixing the tiles over one another in such a way that they will be overlapped for 9 centimeters and 1 centimeter tile area will be free to obtain bonded tiles. The bonded tiles were cured for 14 days. Shear adhesion test as per IS 15477:2019 in a UTM - Universal testing machine was performed on the cured tiles. Table 8 demonstrates the result of the shear adhesion test.
Table 8: Shear adhesion test of the adhesive composition prepared in accordance with the present disclosure.
Sr. no Properties Adhesive composition of experiment 1 of the present disclosure Conventional adhesive composition
1. Shear adhesion test
IS 15477:2019
(dry condition) 6.72 Mpa 4.89 Mpa
From Table 8 it is observed that the adhesive composition of the present disclosure have better shear adhesion when compared to the conventional adhesive composition.
TECHNICAL ADVANCEMENTS
The present disclosure described herein above has several technical advantages including, but not limited to, the realization of:
? an adhesive composition that:
• is waterproof;
• is stain free;
• has abrasion resistance; and
• is environment friendly.
and
? a process for the preparation of an adhesive composition that;
• is simple and economical.
Throughout this specification, the word “comprise”, or variations such as “comprises” or “comprising, will be understood to imply the inclusion of a stated element, integer or step,” or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or results. While certain embodiments of the inventions have been described, these embodiments have been presented by way of example only, and are not intended to limit the scope of the inventions. Variations or modifications to the formulation of this invention, within the scope of the invention, may occur to those skilled in the art upon reviewing the disclosure herein. Such variations or modifications are well within the spirit of this invention.
The numerical values given for various physical parameters, dimensions and quantities are only approximate values and it is envisaged that the values higher than the numerical value assigned to the physical parameters, dimensions and quantities fall within the scope of the invention unless there is a statement in the specification to the contrary.
While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated that many additional features is added and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation.

,CLAIMS:WE CLAIM:

1. An adhesive composition comprising:
(A) a base component comprising:
i. a predetermined amount of a base resin;
ii. a predetermined amount of a plasticizer;
iii. a predetermined amount of a pre-polymer;
iv. a predetermined amount of a first filler;
v. a predetermined amount of a first pigment;
vi. a predetermined amount of a first additive; and
vii. q.s water;
and
(B) a hardener component comprising:
i) a predetermined amount of a hardener resin;
ii) a predetermined amount of an accelerated curing agent;
iii) a predetermined amount of a second filler;
iv) a predetermined amount of a second pigment; and
v) a predetermined amount of a second additive;
wherein a mass ratio of said base component to said hardener component is in the range of 3:1 to 7:1 prior to application on a substrate.

2. The composition as claimed in claim 1, wherein
i. said predetermined amount of said base resin is in the range of 10 mass% to 25 mass%;
ii. said predetermined amount of said plasticizer is in the range of 12 mass% to 25 mass%;
iii. said predetermined amount of said pre-polymer is in the range of 5 mass% to 15 mass%;
iv. said predetermined amount of said first filler is in the range of 45 mass% to 65 mass%;
v. said predetermined amount of said first pigment is in the range of 1 mass% to 5 mass%; and
vi. said predetermined amount of said first additive is in the range of 2 mass% to 10 mass%.
wherein mass% of each ingredient is with respect to the total mass% of said base component.

3. The composition as claimed in claim 1, wherein
i) said predetermined amount of said hardener resin is in the range of 20 mass% to 40 mass%;
ii) said predetermined amount of said accelerated curing agent is in the range of 1 mass% to 4 mass%;
iii) said predetermined amount of said second filler is in the range of 55 mass% to 75 mass%;
iv) said predetermined amount of said second pigment is in the range of 1 mass% to 3 mass%; and
v) said predetermined amount of said second additive is in the range of 1 mass% to 10 mass%;
wherein mass% of each component is with respect to the total mass% of said hardener component.
4. The composition as claimed in claim 1, wherein
• said base resin is an unmodified liquid epoxy resin;
• said plasticizer is selected from the group consisting of alkyl sulphonic acid ester, esters of phthalic acid, diethylehexyl terephthalate, diisononyl cyclohexane dicarboxylate, and biobased plasticizers based on epoxidized plant oils, cardanol, and citrates;
• said prepolymer is selected from the group consisting of blocked polyoxypropylene glycol and toluene diisocyanate, and branched polymer with ether and urethane groups based on blocked polyoxypropylene glycol and toluene diisocyanate;
• said first filler and said second filler are independently a carbonate mineral, wherein said carbonate mineral is calcium carbonate (calcite powder);
• said first pigment and said second pigment are independently titanium dioxide;
• said first additive is selected from a first rheology modifier, a first surfactant, and a preservative;
• said hardener resin is selected from the group consisting of aliphatic polyamide, modified aliphatic polyamide, aromatic polyamide, modified aromatic polyamide, primary polyamide, secondary polyamide, and tertiary polyamide;
• said accelerated curing agent is an aromatic tertiary amine;
• said second additive is selected from the group consisting of a second rheology modifier, a second surfactant, and a thixotropic agent; and
• said substrate is selected from the group consisting of concrete wall, plaster wall, glass panel, metal panel, wooden panel, plaster board, and gypsum board.
5. The composition as claimed in 4, wherein
i) said polyoxypropylene glycol and toluene diisocyanate is blocked with at least one component selected from alkyl phenol and renewable blocking agent; and wherein said renewable blocking agent is cashew nutshell liquid;
ii) said first rheology modifier and said second rheology modifier are independently selected from the group consisting of bentonite clay, sodium montmorillonite, and calcium montmorillonite;
iii) said first surfactant and said second surfactant are independently an anionic surfactant, wherein said anionic surfactant is selected from the group consisting of sodium lauryl ether sulphate, sodium lauryl sulphate, ammonium lauryl sulphate, sodium lauryl sarcosinate, sodium dodecyl sulphate, sodium myreth sulphate, sodium pareth sulphate, and magnesium laureth sulphate;
iv) said aromatic tertiary amine is 2,4,6-tris (dimethyl aminomethyl) phenol;
v) said preservative is a mixture of formaldehyde, methyl chloride, and methylisothiazolinone; and
vi) said thixotropic agent is fumed silica.
6. The composition as claimed in claim 4, wherein
i) said base resin have an epoxy equivalent weight in the range of 180 g/mol to 190 g/mol;
ii) said base resin have a viscosity in the range of 10000 centipoise to 15000 centipoise;
iii) said pre-polymer have a reactive content in the range of 2.4 mass % to 2.7 mass% with respect to the total mass of said pre-polymer; wherein said reactive content is an isocyanate group; and
iv) said pre-polymer have an epoxy equivalent weight in the range of 900 g/mol to 930 g/mol.
7. The composition as claimed in claim 4, wherein
i) said accelerated curing agent have an amine value in the range of 580 mg KOH/gm to 650 mg KOH/gm;
ii) said hardener resin have an amine value in the range of 390 mg KOH/gm to 450 mg KOH/gm; and
iii) said thixotropic agent have a specific area in the range of 150 m2/gm to 250 m2/gm.
8. The composition as claimed in claim 4, wherein
i) said first surfactant and said second surfactant independently have hydrophilic–lipophilic balance (HLB) value in the range of 8 to 16; and
ii) said first filler and said second filler independently have a particle size in the range of 1 micron to 15 micron;
9. A process for preparation of an adhesive composition, said process comprising the following steps:
(A) preparing a base component by the following steps:
i) charging a predetermined amount of water in a first mixer followed by adding a predetermined amount of a base resin under stirring and sequentially adding predetermined amounts of a plasticizer, a pre-polymer, a first surfactant, and a first pigment under stirring at a first predetermined speed to obtain an intermediate mixture;
ii) adding predetermined amounts of a first rheology modifier, a first filler, and a preservative to said intermediate mixture under stirring at a second predetermined speed to obtain said base component;
(B) preparing a hardener component by the following steps:
(a) charging a predetermined amount of a hardener resin in a second mixer followed by adding a predetermined amount of an accelerated curing agent under stirring and adding predetermined amounts of a second surfactant and a second pigment under stirring at a third predetermined speed to obtain a resultant mixture; and
(b) sequentially adding predetermined amounts of a second rheology modifier, a second filler and a thixotropic agent in said resultant mixture under stirring at a fourth predetermined speed to obtain said hardener component; and
(C) mixing said base component and said hardener component in a predetermined mass ratio to obtain said adhesive composition prior to application on a substrate.
10. The process as claimed in claim 9, wherein
i) said predetermined amount of water is in the range of 1 mass% to 5 mass% with respect to total mass of said base component;
ii) said base resin is unmodified liquid epoxy resin; and
iii) said predetermined amount of said base resin is in the range of 10 mass% to 25 mass% % with respect to total mass of said base component.
11. The process as claimed in claim 9, wherein
i) said plasticizer is selected from the group consisting of alkyl sulphonic acid ester, esters of phthalic acid, diethylehexyl terephthalate, diisononyl cyclohexane dicarboxylate, and biobased plasticizers based on epoxidized plant oils, cardanol, and citrates; and
ii) said predetermined amount of said plasticizer is in the range of 12 mass% to 25 mass% with respect to total mass of said base component.
12. The process as claimed in claim 9, wherein
i) said prepolymer is selected from the group consisting of blocked polyoxypropylene glycol and toluene diisocyanate, and branched polymer with ether and urethane groups based on blocked polyoxypropylene glycol and toluene diisocyanate; wherein said polyoxypropylene glycol and toluene diisocyanate is blocked with at least one component selected from alkyl phenol and renewable blocking agent; and wherein said renewable blocking agent is cashew nutshell liquid;
ii) said predetermined amount of said pre-polymer is in the range of 5 mass% to 15 mass% with respect to total mass of said base component;
iii) said first surfactant is an anionic surfactant, wherein said anionic surfactant is selected from the group consisting of sodium lauryl ether sulphate, sodium lauryl sulphate, ammonium lauryl sulphate, sodium lauroyl sarcosinate, sodium dodecyl sulphate, sodium myreth sulphate, sodium pareth sulphate, and magnesium laureth sulphate;
iv) said predetermined amount of the first surfactant is in the range of 2 mass% to 4 mass% with respect to the total mass of the base component;
v) said first pigment is titanium dioxide; and
vi) said predetermined amount of said first pigment is in the range of 1 mass% to 5 mass% with respect to total mass of said base component.
13. The process as claimed in claim 9, wherein
i) said first rheology modifier is selected from the group consisting of bentonite clay, sodium montmorillonite, and calcium montmorillonite;
ii) said first rheology modifier is in the range of 0.5 mass% to 3 mass% with respect to the total mass of the base component;
iii) said first filler is a carbonate mineral, wherein said carbonate mineral is calcium carbonate (calcite powder); and
iv) said predetermined amount of said first filler is in the range of 45 mass% to 65 mass% with respect to total mass of said base component;
v) said first preservative is selected from the group consisting of formaldehyde, methyl chloride, and methylisothiazolinone; and
vi) said predetermined amount of said preservative is in the range of 0.1 mass% to 0.5 mass% with respect to total mass of said base component.
14. The process as claimed in claim 11, wherein
i) said hardener resin is selected from the group consisting of aliphatic polyamide, modified aliphatic polyamide, aromatic polyamide, modified aromatic polyamide, primary polyamide, secondary polyamide, and tertiary polyamide;
ii) said predetermined amount of said hardener resin is in the range of 20 mass% to 40 mass% with respect to total mass of said hardener component;
iii) said accelerated curing agent is an aromatic tertiary amine and wherein said aromatic tertiary amine is 2,4,6-tris (dimethyl aminomethyl) phenol; and
iv) said predetermined amount of said accelerated curing agent is in the range of 1 mass% to 4 mass% with respect to total mass of said hardener component.
15. The process as claimed in claim 9, wherein
i) said second surfactant is an anionic surfactant selected, wherein said anionic surfactant is selected from the group consisting of sodium lauryl ether sulphate, sodium lauryl sulphate, ammonium lauryl sulphate, sodium lauryl sarcosinate, sodium dodecyl sulphate, sodium myreth sulphate, sodium pareth sulphate, and magnesium laureth sulphate; and
ii) said predetermined amount of the second surfactant is in the range of 1 mass% to 3.5 mass% with respect to the total mass of the hardener component.
16. The process as claimed in claim 9, wherein
i) said second pigment is titanium dioxide;
ii) said predetermined amount of said second pigment is in the range of 1 mass% to 3 mass% with respect to total mass of said hardener component;
iii) said second rheology modifier is selected from the group consisting of bentonite clay, sodium montmorillonite, and calcium montmorillonite; and
iv) said predetermined amount of said second rheology modifier is in the range of 1 mass% to 5 mass% with respect to the total mass of the hardener component.

17. The process as claimed in claim 9, wherein
i) said second filler is a carbonate mineral, wherein said carbonate mineral is calcium carbonate (calcite powder);
ii) said predetermined amount of said second filler is in the range of 55 mass% to 75 mass% with respect to total mass of said hardener component;
iii) said thixotropic agent is fumed silica;
iv) said predetermined amount of said thixotropic agent is in the range from 0.1 mass% to 3 mass% with respect to the total amount of the hardener component; and
v) said substrate is selected from the group consisting of concrete wall, plaster wall, glass panel, metal panel, wooden panel, plaster board, and gypsum board.
18. The process as claimed in claim 9, wherein
i) said stirring is performed after adding each ingredient for a time period in the range of 5 minutes to 30 minutes;
ii) said first predetermined speed is in the range of 200 rpm to 400 rpm;
iii) said second predetermined speed is in the range of 800 rpm to 1200 rpm;
iv) said third predetermined speed is in the range of 200 rpm to 400 rpm; and
v) said fourth predetermined speed is in the range of 800 rpm to 1200 rpm.
19. The process as claimed in claim 9, said predetermined mass ratio of said base component to said hardener component is in the range of 3:1 to 7:1.

Dated this 30th day of August, 2024

_______________________________
MOHAN RAJKUMAR DEWAN, IN/PA – 25
OF R. K. DEWAN & CO.
AUTHORIZED AGENT OF APPLICANT

TO,
THE CONTROLLER OF PATENTS
THE PATENT OFFICE, AT MUMBAI

Documents

Application Documents

# Name Date
1 202321058850-STATEMENT OF UNDERTAKING (FORM 3) [01-09-2023(online)].pdf 2023-09-01
2 202321058850-PROVISIONAL SPECIFICATION [01-09-2023(online)].pdf 2023-09-01
3 202321058850-PROOF OF RIGHT [01-09-2023(online)].pdf 2023-09-01
4 202321058850-FORM 1 [01-09-2023(online)].pdf 2023-09-01
5 202321058850-DECLARATION OF INVENTORSHIP (FORM 5) [01-09-2023(online)].pdf 2023-09-01
6 202321058850-FORM-26 [15-09-2023(online)].pdf 2023-09-15
7 202321058850-FORM-5 [30-08-2024(online)].pdf 2024-08-30
8 202321058850-FORM 18 [30-08-2024(online)].pdf 2024-08-30
9 202321058850-ENDORSEMENT BY INVENTORS [30-08-2024(online)].pdf 2024-08-30
10 202321058850-COMPLETE SPECIFICATION [30-08-2024(online)].pdf 2024-08-30