PD055059IN-SC
FORM 2
THE PATENTS ACT, 1970
(39 of 1970)
&
THE PATENTS RULES, 2003
COMPLETE SPECIFICATION
(See section 10, rule 13)
1. Title of the invention: ANTI-EFFLORESCENCE ADDITIVE COMPOSITION AND PROCESS THEREOF
2. Applicant(s)
NAME
NATIONALITY
ADDRESS
ASIAN PAINTS LIMITED
Indian
Research & Technology Center, Asian Paints Limited, C3-B1, TTC MIDC, Pawane Village, Turbhe, Navi Mumbai – 400703, India
3. Preamble to the description
COMPLETE SPECIFICATION
The following specification particularly describes the invention and the manner in which it is to be performed.
1
FIELD OF INVENTION
[0001]
The present disclosure broadly relates to concrete products. In particular, the present disclosure relates to the coating of concrete products. The present disclosure further provides an additive composition for the coating of concrete products that eliminates the efflorescence. 5
BACKGROUND OF INVENTION
[0002]
Efflorescence is a fine, white, powdery precipitate of water-soluble salts left on the surface of masonry as the water evaporates. Water migrates and rises in the pores present in the building materials such as brick, concrete, stone, stucco. 10 The main component of efflorescence is CaCO3 and other chemicals such as Na2CO3, K2CO3, CaSO4. The formation of efflorescence on the surface of masonry depends on the presence of water-soluble salts (especially Ca2+), the presence of water and the presence of channels along which water can migrate to the surface of masonry. During hydration of the mortar mix or paints, water soluble chemicals 15 such as Ca(OH)2 are formed. During the drying of the mixture, these water-soluble chemicals migrate with water to the surface of masonry and then react with the CO2 or SO2 in the air to form the respective carbonate or sulphate salt. The salts left behind appear as white patches or deposits altering the aesthetics of the buildings.
[0003]
There are two types of efflorescence, primary (early, short-term) 20 efflorescence and secondary efflorescence. Primary efflorescence is the result of salts which leach out from the mortar mix upon evaporation of water from the mixture. Secondary efflorescence is the result of salts which leach out of the concrete with water which moves through the concrete substrate, either continuously or intermittently, or with water which comes from exposure of the 25 concrete surface to alternate wetting and drying.
[0004]
Currently, the anti-efflorescence additives which are commercially available or reported previously in literature, are hydrophobic materials such as silanes and silicones which reduce water uptake or hydrophobic additives such as butyl stearate, a rosin and fatty acid-based additive, rosin stabilized with polyvinyl 30 alcohol, hydrophobic acrylic polymer. The organosilanes and silicone emulsions 2
have a high cost while use of a completely new polymer will require redesign of the
coating system.
[0005]
US20160137870 A1 and CA2912257 A1 disclose an anti-efflorescence composition comprising from 1% to 60% by weight of at least one of a homo polymer solution of acrylic, a hydrolysed polyvinyl alcohol or a combination 5 thereof, and water. The composition disclosed therein eliminates the efflorescence that occurs on new pavers, stones, concrete bricks or concrete furniture because of high humidity.
[0006]
US9353005B2 discloses a process for the production of powder re-dispersible in water, which is used to reduce the efflorescence in hydraulically set 10 systems, said powder comprising: an organic component, a water-soluble organic polymeric protective colloid and, optionally, one or more further additives.
[0007]
WO2000023393A1 relates to a liquid-state efflorescence-inhibiting agent which causes low air-entrainment to a cement composition, which has storage stability at low temperatures. The efflorescence-inhibiting agent discloses therein 15 comprises one or more species of C8-C18 fatty acid alkaline metal salts, wherein the content of the C12-C16 fatty acid alkaline metal salts is not less than 80 % by weight.
[0008]
WO1995004008A1 discloses a dry cement mixture having anti-efflorescence properties, comprising a substantially uniform mixture of a hydraulic cement having from 0.01 to 3 weight percent of at least one C14-C22 fatty alcohol. 20
[0009]
US5595594A1 discloses an anti-efflorescence admixture for concrete products comprising: a) a tall oil fatty acid, and b) an unsaturated fatty acid having 8-28 carbon atoms, in a weight ratio of tall oil fatty acid to unsaturated fatty acid of 1:10 to 2:1; wherein 2 to 50% by weight of the acid of a) and b) being optionally in salt form with at least one salt-forming member selected from an alkanolamine or 25 an alkylamine.
[00010]
Thus, the interest towards silicon free water-based anti-efflorescence additive has grown due to low cost and easy workability. There is a dire need in the art to develop a low-cost silicone-free and solvent free aqueous anti-efflorescence additive that is easy to incorporate/ apply even in the letdown stage of a paint/mortar 30 mix and provided excellent anti-efflorescence effect.
3
SUMMARY OF THE INVENTION
[00011] In a first aspect of the present disclosure, there is provided an additive composition comprising: (a) an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof; (b) a C4 – C20 5 monoepoxide functional monomer; and (c) at least one alkali metal salt solution, wherein the additive composition has an acid number in the range of 100 to 200 mg KOH/g.
[00012]
In a second aspect of the present disclosure, there is provided a process of preparing the additive composition, the process comprising contacting 10 unsaturated vegetable oil fatty acids, a monoepoxide functional monomer, and at least one alkali metal salt solution to obtain the additive composition.
[00013] In a third aspect of the present disclosure, there is provided an anti-efflorescence formulation comprising: (a) water; (b) polymer selected from the group consisting of acrylic polymers, styrene acrylic polymers, vinyl acrylic 15 copolymer, epoxy polymer, polyester, polyurethane, polysiloxane, fluorinated polymer, and mixtures thereof; (c) organic and inorganic pigments and fillers, and (d) the additive composition as disclosed herein, wherein the additive composition weight percentage is in the range of 0.1 to 2 % based on the total weight of the formulation. 20
[00014]
In a fourth aspect of the present disclosure, there is provided a composition comprising the anti-efflorescence formulation as disclosed herein.
[00015] In a fifth aspect of the present disclosure, there is provided a method of preventing efflorescence on surfaces of a substrate by the incorporation of the additive composition as disclosed herein or the anti-efflorescence formulation as 25 disclosed herein.
[00016] In a sixth aspect of the present disclosure, there is provided an efflorescence inhibiting composition comprising: (a) chemically modified adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof, (b) alkali metal salt solution, wherein the efflorescence inhibiting 30 composition has an acid number less than 300 mg KOH/g.
4
[00017] These and other features, aspects, and advantages of the present subject matter will be better understood with reference to the following description and appended claims. This summary is provided to introduce a selection of concepts in a simplified form. This summary is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used to limit the scope 5 of the claimed subject matter.
BRIEF DESCRIPTION OF THE ACCOMPANYING FIGURES
[00018]
In order that the disclosure may be readily understood and put into practical effect, reference will now be made to exemplary embodiments as illustrated with reference to the accompanying figures. The figures together with a 10 detailed description below, are incorporated in and form part of the specification, and serve to further illustrate the embodiments and explain various principles and advantages, in accordance with the present disclosure wherein:
[00019]
Figure 1 depicts the salt migration observed on the aerated cement panels coated with additive compositions A1, A2, A3 and A6 on day 1, day 14 and day 21, 15 in accordance with an embodiment of the present disclosure.
DESCRIPTION OF THE INVENTION
[00020] Those skilled in the art will be aware that the present disclosure is subject to variations and modifications other than those specifically described. It is to be 20 understood that the present disclosure includes all such variations and modifications. The disclosure also includes all such steps, features, compositions, and compounds referred to or indicated in this specification, individually or collectively, and any and all combinations of any or more of such steps or features.
Definitions 25
[00021] For convenience, before further description of the present disclosure, certain terms employed in the specification, and examples are delineated here. These definitions should be read in the light of the remainder of the disclosure and understood as by a person of skill in the art. The terms used herein have the meanings recognized and known to those of skill in the art, however, for 30 5
convenience and completeness, particular terms and their meanings are set forth
below.
[00022] The articles “a”, “an” and “the” are used to refer to one or to more than one (i.e., to at least one) of the grammatical object of the article.
[00023] The terms “comprise” and “comprising” are used in the inclusive, open 5 sense, meaning that additional elements may be included. It is not intended to be construed as “consists of only”.
[00024] Throughout this specification, unless the context requires otherwise the word “comprise”, and variations such as “comprises” and “comprising”, will be understood to imply the inclusion of a stated element or step or group of element or 10 steps but not the exclusion of any other element or step or group of element or steps.
[00025] The term “monoepoxide functional monomer” refers to a type of monomer molecule that contains one epoxide (oxirane) group. An epoxide group consists of an oxygen atom bonded to two adjacent carbon atom, forming a three-membered ring structure. 15
[00026] The term “adduct” refers to a molecular complex or compound formed by the combination of two or more distinct chemical species. The combination typically occurs through a chemical reaction or interaction, leading to the formation of a new entity with properties different from those of the individual components. In the context of the claimed invention, adduct refers to a Diels-Alder adduct of 20 diene selected from the group consisting of unsaturated fatty acids, unsaturated cyclic compounds, and mixtures thereof with dienophile selected from the group consisting of maleic anhydride, fumaric acid, maleic acid, mono alkyl ester of fumaric acid, dialkyl ester of fumaric acid, acrylic acid, C1-C12 alkyl ester of acrylic acid, methacrylic acid, C1-C12 alkyl ester of methacrylic acid, itaconic acid, C1-C12 25 alkyl ester of itaconic acid, C1-C12 alkyl ester of maleic acid, and mixtures thereof. Further, chemically modified adduct as used herein refers to the modification of the Diels-Alder adduct with an epoxy functional compound such as a C4 to C20 glycidyl ester or a glycidyl ether.
[00027] The term “unsaturated cyclic compounds” refers to organic compounds 30 that contain a cyclic (ring) structure and have one or more double or triple bonds
6
between the carbon atoms in the ring. In an aspect of the present disclosure,
the unsaturated cyclic compounds include but are not limited to rosin, terpenes, polyterpenes, terpeneoid, a resin acid (abietic acid), colophony, terpene resin, terpene-phenol resin, and derivatives thereof. [00028] The term “unsaturated vegetable oil fatty acids” refers to a fatty acid 5 derived from vegetable oils that contain one or more carbon-carbon double bonds in its hydrocarbon chain. The unsaturated vegetable oil fatty acids in the context of the present disclosure are preferably C10-C20 unsaturated vegetable oil fatty acids. Vegetable oils such as soybean oil, linseed oil, sunflower oil, castor oil, tall oil, corn oil, canola oil, rapeseed oil, palm kernel oil, cottonseed oil, peanut oil, coconut oil, 10 palm oil, tung oil, safflower oil often contain a significant proportion of unsaturated fatty acids.
[00029]
The term "dienophile" refers to an electron-deficient compound that contains either a double bond or a triple bond and has ability to react with a diene in a cycloaddition reaction (Diel's alder reaction). In an aspect of the present 15 disclosure, the dienophile is selected from the group consisting of maleic anhydride, fumaric acid, maleic acid, mono alkyl ester of fumaric acid, dialkyl ester of fumaric acid, acrylic acid, C1-C12 alkyl ester of acrylic acid, methacrylic acid, C1-C12 alkyl ester of methacrylic acid, itaconic acid, C1-C12 alkyl ester of itaconic acid, C1-C12 alkyl ester of maleic acid, and mixtures thereof. 20
[00030] The term “acid number” refers to a quantitative measure of the amount of acidic substances present in a sample of a chemical compound. It is expressed as the amount of potassium hydroxide (KOH) in milligrams required to neutralize one gram equivalent of acidic substance in the sample. The “acid number” in the present context is between 100 to 200 mg KOH/g. This acid value number helps in 25 achieving a balance of hydrophobicity and hydrophilicity.
[00031] The term “C4 – C20 monoepoxide functional monomer” refers to monomer molecule with an epoxide (oxirane) group having a carbon chain length ranging from 4 to 20 carbon atoms.
[00032] The term “alkali” refers to a substance that is used to neutralize acids or 30 acidic components on the additives in the coating compositions, to form a salt and 7
thereby
adjust the pH of the coating composition and to enhance its stability and performance. In an aspect of the present disclosure, the alkali is selected from sodium hydroxide, potassium hydroxide, ammonium hydroxide, primary amine, secondary amine, tertiary amine or alkanolamine.
[00033]
The term “primary amine” refers to a type of amine that has the general 5 formula RCH2NH2, wherein R is an alkyl or aryl group. The examples for primary amines include, but are not limited to methyl amine, ethyl amine, and propyl amine.
[00034]
The term “secondary amine” refers to a type of amine that has the general formula R2CHNH, where R is an alkyl or aryl group. The example for secondary amine includes but is not limited to dimethylamine. 10
[00035]
The term “tertiary amine” refers to a type of amine that has the general formula R3N, wherein R is an alkyl or aryl group. The example for tertiary amine includes but is not limited to trimethylamine.
[00036]
The term “alkanolamine” refers to a type of amine that has both an amino group (-NR2) and an alcohol group (-OH) attached to the same molecule, wherein 15 R is hydrogen, alkyl or aryl group. Alkanolamines are also known as amino alcohols. In an aspect of the present disclosure, alkanolamines includes, but is not limited to N,N-dimethylaminoethanol.
[00037]
The term “pigments” refers to solid particles that are added to the coating composition to provide colour, and opacity to the coating film. In an aspect of the 20 present disclosure, the pigments are selected from a group consisting of titanium oxide, zirconium oxide, zinc oxide, silicon oxide, and aluminum oxide, aluminum pigments, iron pigments, copper pigments, bismuth pigments, and manganese pigments.
[00038]
The term “fillers” refers to substances that are added to coating 25 composition to improve the physical and optical properties of the coating film, such as hardness, durability, scratch resistance, hiding power, and transparency, while also reducing costs and enhancing sustainability. In an aspect of present disclosure, the fillers are selected from a group consisting of silica, zinc oxide, barium sulfate, calcium carbonate, marble powder, dolomite, steatite, and talc. 30 8
[00039]
The term “thickener” refers to a substance used to increase the viscosity of a liquid formulation/composition, which enhances its flow properties, stability, and application characteristics.
[00040] The term “dispersing agent” refers to a substance that helps to stabilize and evenly distribute solid particles within a coating composition. It helps in 5 maintaining a uniform suspension of pigments, fillers, and other solid materials in the coating compositions.
[00041] The term “super plasticizer additive refers to an admixture that is used in coatings compositions, particularly, in concrete and mortar mixtures to enhance the flow properties and workability of the material. 10
[00042] The term “wetting agent” refers to a substance that lowers the surface tension of the coating composition and facilitate the adhesion of the coating composition to the substrate by ensuring that the coating composition can fully wet or cover the surface.
[00043]
Ratios, concentrations, amounts, and other numerical data may be 15 presented herein in a range format. It is to be understood that such range format is used merely for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For 20 example, 100 to 200 mg KOH/g should be interpreted to include not only the explicitly recited limits of 100 to 200 mg KOH/g but also to include sub-ranges, such as 120 to 180 mg KOH/g, 140 to 160 mg KOH/g and so forth, as well as individual amounts, including fractional amounts, within the specified ranges, such as 110 mg KOH/g, 130 mg KOH/g, 150 mg KOH/g, 170 mg KOH/g, 190 mg 25 KOH/g, and so on.
[00044] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the 30 9
disclosure, the preferred methods, and materials are now described. All publications
mentioned herein are incorporated herein by reference.
[00045]
As discussed in the background, the anti-efflorescence additives which are commercially available or reported previously in literature, are hydrophobic materials such as silanes and silicones which reduce water uptake or hydrophobic 5 additives such as butyl stearate, a rosin and fatty acid-based additive, rosin stabilized with polyvinyl alcohol, hydrophobic acrylic polymer. The organosilanes and silicone emulsions have a high cost while use of a completely new polymer will require redesign of the coating system. In order to overcome the aforementioned challenges, the present disclosure provides an additive which can potentially 10 eliminate or prevent efflorescence. Accordingly, the present disclosure provides an additive composition comprising an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof; a C4 – C20 monoepoxide functional monomer; and at least one alkali metal salt solution, wherein the additive composition has an acid number in the range of 100 to 200 mg KOH/g. The specific 15 acid value helps in firstly forming a stable dispersion of the additive composition. Further, it helps to block the open pores or capillaries of the substrate upon which the additive composition is coated, and thereby reduces the migration of salt and prevents efflorescence. Furthermore, the presence of hydrophobic groups in the additive composition reduces water migration to the surface of substrate, which 20 reduces the dissolved salt migration to surface. The anti-efflorescence additive as disclosed herein is silicon free and in liquid form that is easy to incorporate even in the letdown stage of a paint or a mortar mixture, without any additional processing aids or solvents.
[00046]
In an embodiment of the present disclosure, there is provided an additive 25 composition comprising: (a) an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof; (b) a C4 – C20 monoepoxide functional monomer; and (c) at least one alkali metal salt solution, wherein the additive composition has an acid number in the range of 100 to 200 mg KOH/g. 30 10
[00047]
In an embodiment of the present disclosure, there is provided an additive composition as disclosed herein, wherein the additive composition has an acid number in the range of 120 to 180 mg KOH/g. In another embodiment of the present disclosure, the additive composition has an acid number in the range of 120 to 170 mg KOH/g. In yet another embodiment of the present disclosure, the additive 5 composition has an acid number in the range of 145 to 160 mg KOH/g.
[00048]
In an embodiment of the present disclosure, there is provided an additive composition as disclosed herein, wherein the C4 – C20 monoepoxide functional monomer is selected from a group consisting of glycidyl ester of versatic acid 10, aromatic monoepoxide based on para-tertiary butyl phenol, aliphatic monoepoxide 10 based on C12-C14 alcohol, monoepoxide based on phenol, monoepoxide based on o-cresol, monoepoxide based on p-tertiary butyl phenol, and monoepoxide based on n-butanol. In another embodiment of the present disclosure, the C4 – C20 monoepoxide functional monomer is selected from a group consisting of glycidyl ester of versatic acid 10, aromatic monoepoxide based on para-tertiary butyl phenol, 15 and aliphatic monoepoxide based on C12-C14 alcohol.
[00049]
In an embodiment of the present disclosure, there is provided an additive composition as disclosed herein, wherein the adduct is a Diels-Alder adduct of diene selected from the group consisting of unsaturated fatty acids, unsaturated cyclic compounds, and mixtures thereof with dienophile selected from the group 20 consisting of maleic anhydride, fumaric acid, maleic acid, mono alkyl ester of fumaric acid, dialkyl ester of fumaric acid, acrylic acid, C1-C12 alkyl ester of acrylic acid, methacrylic acid, C1-C12 alkyl ester of methacrylic acid, itaconic acid, C1-C12 alkyl ester of itaconic acid, C1-C12 alkyl ester of maleic acid, and mixtures thereof. In another embodiment of the present disclosure, the adduct is a Diels-Alder adduct 25 of diene selected from the group consisting of unsaturated fatty acids, unsaturated cyclic compounds, and mixtures thereof with dienophile selected from the group consisting of maleic anhydride, fumaric acid, maleic acid, mono alkyl ester of fumaric acid, and mixtures thereof.
11
[00050]
In an embodiment of the present disclosure, there is provided an additive composition as disclosed herein, wherein the diene is a combination of unsaturated fatty acids, and unsaturated cyclic compounds.
[00051]
In an embodiment of the present disclosure, there is provided an additive composition as disclosed herein, wherein the unsaturated vegetable oil fatty acid is 5 derived from an unsaturated vegetable oil selected from the group consisting of soybean oil, linseed oil, sunflower oil, castor oil, dehydrated castor oil, tall oil, corn oil, canola oil, rapeseed oil, palm kernel oil, cottonseed oil, peanut oil, coconut oil, palm oil, tung oil, safflower oil, and combinations thereof. In another embodiment of the present disclosure, the unsaturated vegetable oil fatty acid is derived from an 10 unsaturated vegetable oil selected from the group consisting of soybean oil, linseed oil, tung oil, tall oil and combinations thereof.
[00052]
In an embodiment of the present disclosure, there is provided an additive composition as disclosed herein, wherein the unsaturated cyclic compound is selected from the group consisting of rosin, terpenes, polyterpenes, terpeneoid, a 15 resin acid (abietic acid), colophony, terpene resin, terpene-phenol resin, and derivatives thereof. In another embodiment of the present disclosure, the unsaturated cyclic compound is selected from the group consisting of rosin, terpenes, polyterpenes, a resin acid (abietic acid) and derivatives thereof.
[00053]
In an embodiment of the present disclosure, there is provided an additive 20 composition as disclosed herein, wherein the additive composition comprises additional ingredients selected from the group consisting of defoamers, biocides, in-can preservatives, thickeners, wetting agent, dispersing agents, super plasticizer additive and combinations thereof.
[00054]
In an embodiment of the present disclosure, there is provided an additive 25 composition as disclosed herein, wherein the unsaturated vegetable oil fatty acid, unsaturated cyclic compound, dienophile, and C4 to C20 monoepoxide functional monomer is present in a weight ratio range of 0.25:1:0.2:0.3 to 1.6:1:0.5:1.5. In another embodiment of the present disclosure, the unsaturated vegetable oil fatty acid, unsaturated cyclic compound, dienophile, and C4 to C20 monoepoxide 30 functional monomer is present in a weight ratio range of 0.35:1:0.2:0.4 to 12
1.
55:1:0.5:1.2. In yet another embodiment of the present disclosure, the unsaturated vegetable oil fatty acid, unsaturated cyclic compound, dienophile, and C4 to C20 monoepoxide functional monomer is present in a weight ratio range of 0.5:1:0.2:0.5 to 1.5:1:0.5:1.
[00055]
In an embodiment of the present disclosure, there is provided an additive 5 composition as disclosed herein, wherein the additive composition optionally comprises, additional ingredients selected from the group consisting of defoamers, biocides, in-can preservatives, thickeners, wetting agent, dispersing agents, super plasticizer additive and combinations thereof.
[00056]
In an embodiment of the present disclosure, there is provided an additive 10 composition comprising: (a) an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof; (b) a C4 – C20 monoepoxide functional monomer; (c) at least one alkali salt solution; and (d) defoamers, wherein the additive composition has an acid number in the range of 100 to 200 mg KOH/g. 15
[00057]
In an embodiment of the present disclosure, there is provided an additive composition comprising: (a) an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof; (b) a C4 – C20 monoepoxide functional monomer; (c) at least one alkali salt solution; (d) defoamers; and (e) biocides, wherein the additive composition has an acid number 20 in the range of 100 to 200 mg KOH/g.
[00058]
In an embodiment of the present disclosure, there is provided an additive composition comprising: (a) an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof; (b) a C4 – C20 monoepoxide functional monomer; (c) at least one alkali salt solution; (d) 25 defoamers; (e) biocides; and (f) in-can preservatives, wherein the additive composition has an acid number in the range of 100 to 200 mg KOH/g.
[00059]
In an embodiment of the present disclosure, there is provided an additive composition comprising: (a) an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof; (b) a C4 – C20 30 monoepoxide functional monomer; (c) at least one alkali salt solution; (d) 13
defoamers; (e) biocides; (f) in
-can preservatives; and (g) thickeners, wherein the additive composition has an acid number in the range of 100 to 200 mg KOH/g.
[00060]
In an embodiment of the present disclosure, there is provided an additive composition comprising: (a) an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof; (b) a C4 – C20 5 monoepoxide functional monomer; (c) at least one alkali salt solution; (d) defoamers; (e) biocides; (f) in-can preservatives; (g) thickeners; and (h) wetting agent, wherein the additive composition has an acid number in the range of 100 to 200 mg KOH/g.
[00061]
In an embodiment of the present disclosure, there is provided an additive 10 composition comprising: (a) an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof; (b) a C4 – C20 monoepoxide functional monomer; (c) at least one alkali salt solution; (d) defoamers; (e) biocides; (f) in-can preservatives; (g) thickeners; (h) wetting agent; and (i) dispersing agent, wherein the additive composition has an acid number in 15 the range of 100 to 200 mg KOH/g.
[00062]
In an embodiment of the present disclosure, there is provided an additive composition comprising: (a) an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof; (b) a C4 – C20 monoepoxide functional monomer; (c) at least one alkali salt solution; (d) 20 defoamers; (e) biocides; (f) in-can preservatives; (g) thickeners; (h) wetting agent; (i) dispersing agent; and (j) super plasticizer additive, wherein the additive composition has an acid number in the range of 100 to 200 mg KOH/g.
[00063]
In an embodiment of the present disclosure, there is provided an additive composition as disclosed herein, wherein the alkali is selected from sodium 25 hydroxide, potassium hydroxide, ammonium hydroxide, primary amine, secondary amine, tertiary amine or alkanolamine. In another embodiment of the present disclosure, the alkali is selected from sodium hydroxide, primary amine, secondary amine, tertiary amine or alkanolamine.
[00064]
In an embodiment of the present disclosure, there is provided a process of 30 preparing the additive composition, wherein the process comprises contacting 14
unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, a monoepoxide functional monomer, and at least one alkali metal salt solution to obtain the additive composition.
[00065] In an embodiment of the present disclosure, there is provided an anti-efflorescence formulation comprising: (a) water; (b) polymer selected from the 5 group consisting of acrylic polymers, styrene acrylic polymers, vinyl acrylic copolymer, epoxy polymer, polyester, polyurethane, polysiloxane, fluorinated polymer, and mixtures thereof; (c) organic and inorganic pigments and fillers; and (d) the additive composition as disclosed herein; wherein the additive composition weight percentage is in the range of 0.1 to 2 % based on the total weight of the 10 formulation. In another embodiment of the present disclosure, the additive composition weight percentage is in the range of 0.5 to 1.5 % based on the total weight of the formulation. In a further embodiment of the present disclosure, the additive composition weight percentage is in the range of 0.8 to 1.2 % based on the total weight of the formulation. 15
[00066] In an embodiment of the present disclosure, there is provided an anti-efflorescence formulation as disclosed herein, wherein the organic and inorganic pigments are selected from a group consisting of titanium oxide, zirconium oxide, zinc oxide, silicon oxide, and aluminum oxide, aluminum pigments, iron pigments, copper pigments, bismuth pigments, and manganese pigments; and fillers are 20 selected from a group consisting of silica, zinc oxide, barium sulfate, calcium carbonate, marble powder, dolomite, steatite, and talc. In another embodiment of the present disclosure, the organic and inorganic pigments are selected from a group consisting of titanium oxide, zirconium oxide, zinc oxide, and silicon oxide; and fillers are selected from a group consisting of calcium carbonate, marble powder, 25 dolomite, steatite, and talc.
[00067]
In an embodiment of the present disclosure, there is provided a composition comprising the anti-efflorescence formulation as disclosed herein.
[00068] In an embodiment of the present disclosure, there is provided a composition as disclosed herein, wherein the composition is selected from coating 30 mix, concrete mix, and mortar mix.
15
[00069]
In an embodiment of the present disclosure, there is provided a method of preventing efflorescence on surfaces of a substrate by the incorporation of the additive as disclosed herein or the anti-efflorescence formulation as disclosed herein.
[00070] In an embodiment of the present disclosure, there is provided a method as 5 disclosed herein, wherein the substrate is selected from pavers, concrete bricks, stones or concrete furniture.
[00071]
In an embodiment of the present disclosure, there is provided an efflorescence inhibiting composition comprising: (a) chemically modified adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and 10 mixtures thereof, (b) alkali metal salt solution, wherein the efflorescence inhibiting composition has an acid number less than 300 mg KOH/g.
[00072]
In an embodiment of the present disclosure, there is provided an efflorescence inhibiting composition as disclosed herein, wherein the acid number is in between 100 to 200 mg KOH/g. In another embodiment of the present 15 disclosure, the acid number is in between 145 to 160 mg KOH/g.
[00073]
In an embodiment of the present disclosure, there is provided an efflorescence inhibiting composition as disclosed herein, wherein the chemically modified adduct is prepared by treating Diels Alder adduct of unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof with a 20 monoepoxide selected from a glycidyl ester of branched C4 – C20 carboxylic acid, aliphatic monoepoxide based on C12-C14 alcohol, or aromatic monoepoxide based on para-tertiary butyl phenol.
[00074] In an embodiment of the present disclosure, there is provided an efflorescence inhibiting composition as disclosed herein, wherein the alkali salt is 25 selected from sodium salt, potassium salt, or ammonium salt. In another embodiment of the present disclosure, the alkali salt is sodium salt.
[00075]
Although the subject matter has been described in considerable detail with reference to certain examples and implementations thereof, other implementations are possible. 30
EXAMPLES
16
[00076]
The disclosure will now be illustrated with working examples, which is intended to illustrate the working of disclosure and not intended to take restrictively to imply any limitations on the scope of the present disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood to one of ordinary skill in the art to which this disclosure 5 belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice of the disclosed methods and compositions, the exemplary methods, devices, and materials are described herein. It is to be understood that this disclosure is not limited to particular methods, and experimental conditions described, as such methods and conditions may apply. 10
Specific rosin/fatty acid ratio, maleic anhydride modification, monoepoxide content and specific acid value is required to attain the desired anti-efflorescence property.
Example 1 Additive composition/ Efflorescence inhibiting composition 15
[00077] The additive composition/ efflorescence inhibiting composition of the present disclosure comprises (Table 1):
Table 1
Broad category
A1
B1
C1 Unsaturated vegetable oil fatty acids
Linseed oil fatty acid
Tung oil fatty acid
Tall oil fatty acid Unsaturated cyclic compounds
Rosin
Abietic acid
Rosin
Dienophile
Maleic anhydride
Maleic acid
Fumaric acid C4 – C20 monoepoxide
Aliphatic monoepoxide
Glycidyl ester of versatic acid 10
Aromatic monoepoxide based 17
functional monomer
based on C12-C14 alcohol
on para-tertiary butyl phenol Alkali salt solution
Sodium hydroxide
Potassium hydroxide
N,N-dimethylaminoethanol
Example 2 Process of preparation of the additive composition/ efflorescence inhibiting composition
[00078]
The detailed process for the preparation of the additive composition/ 5 efflorescence inhibiting composition of the present disclosure is provided herein below.
[00079] The additive composition/ efflorescence inhibiting composition A1 was prepared as per the following setup. A reactor with a stirrer, condenser, and temperature controller was taken for the reaction. 30 grams of rosin (unsaturated 10 cyclic compound) and 20 grams of linseed oil fatty acid (unsaturated vegetable oil fatty acid) were charged to the reactor to obtain a first mixture. The first mixture was heated up to 90℃ to homogenize the mass. Subsequently, 10 grams of maleic anhydride (dienophile) was charged to the reactor to obtain a second mixture. The second mixture was then heated up to a temperature in a range of 170 to 180℃ and 15 maintained for 60 minutes followed by cooling to a temperature of 100℃ to obtain a Diel’s alder adduct of rosin, and linseed oil fatty acid with maleic anhydride. 20 grams of aliphatic monoepoxide based on C12 to C14 alcohol (C4 – C20 monoepoxide functional monomer) was added to the reactor to obtain a third mixture. The third mixture was then heated up to a temperature in a range of 150 to 160℃ for 3 hours 20 to obtain a chemically modified adduct. The chemically modified adduct was then cooled to 60℃ and neutralized with sodium hydroxide solution (alkali salt solution) and diluted with demineralized water (DM water) to attain an additive composition/ 18
efflorescence inhibiting composition (A1) with a pH of 9 and solid content of 50% solids.
[00080] Similarly, additive compositions/ efflorescence inhibiting composition, B1, and C1 as disclosed in Example 1, were prepared using the process as disclosed herein. The compositions for A1, B1, and C1 are provided in Table 2. 5
Table 2
Composition
Unsaturated vegetable oil fatty acids
(grams)
Unsaturated cyclic compounds
(grams)
Dienophile
(grams)
C4–C20 monoepoxide functional monomer
(grams)
A1
20
30
10
20
B1
20
30
10
15
C1
20
30
10
15
[00081]
Further, for comparative purposes, additive compositions A2, A3, A4, A5, and A6 were prepared by varying (a) components, and (b) the weight of rosin, and linseed oil fatty acid, used in the additive composition A1. The composition for A2 10 to A6 is provided in Table 3.
Table 3
Composition
Unsaturated cyclic compound
Unsaturated vegetable oil fatty acid
Dienophile
C4-C20 monoepoxide functional monomer
Rosin
(grams)
Linseed oil fatty acid
(grams)
Maleic anhydride
(grams)
Aliphatic monoepoxide based on C12 to C14 alcohol (grams)
A2
51.42
48.58
-
-
19
A3
43.94
41.52
14.54
-
A4
25
25
10
20
A5
20
30
10
20
A6
30
20
10
32
Example 3 Analysis of the additive composition/ efflorescence inhibiting composition with respect to the acid number
5
[00082] The additive compositions/ efflorescence inhibiting composition as prepared in Example 2, were analysed with respect to their acid numbers. The analysis is provided in Table 4.
Table 4
Composition
Acid number
A1
160
B1
160
C1
160
A2
194
A3
305
A4
165
A5
165
A6
90
10
[00083] From Table 4, it was observed that, in additive compositions/ efflorescence inhibiting compositions A1, B1, and C1, comprising the combination of unsaturated vegetable fatty acid oil with an adduct formed by the reaction between an unsaturated cyclic compound and dienophile, modified with C4-C20 monoepoxide functional monomer, had acid number in a preferred range. 15
[00084] Similarly, for the additive compositions/ efflorescence inhibiting composition A4, and A5 comprising the combination unsaturated vegetable fatty 20
acid oil with an adduct formed by the reaction between an unsaturated cyclic
compound and dienophile, modified with C4-C20 monoepoxide functional monomer as in additive composition A1, in the specified ratio also had acid number in desired range.
[00085] Further, the analysis of additive compositions/ efflorescence inhibiting 5 composition A2 and A3 revealed that, in the absence of either a dienophile or a C4-C20 monoepoxide functional monomer, or both, led to significantly elevated acid values and reduction of the hydrophobicity of the additive, which is not desirable.
[00086] Moreover, it was noted that, in the additive composition/ efflorescence inhibiting composition A6, the use of aliphatic monoepoxide based on C12 to C14 10 alcohol beyond the desired weight range, resulted in a decrease in acid value.
Example 4
Preparation of the anti-efflorescence formulation:
[00087]
To prepare an anti-efflorescence formulation, 35 % by weight of water, 30 % by weight of styrene acrylic emulsion-based binder, and 1% by weight of additive 15 composition/ efflorescence inhibiting composition as prepared in Example 2, were added into a mixing vessel and mixed until uniform mixture was obtained. Further, 18 % by weight of titanium dioxide and 11% by weight calcium carbonate were added to this mixture, followed by the addition of 1% by weight of wetting and dispersing agent with 4% by weight of water and mixed using a homogenizer and 20 blender until a homogenous mixture of anti-efflorescence formulation with uniform consistency was obtained.
Example 5
Preparation of a composition comprising the anti-efflorescence formulation
25
[00088]
To prepare a coating mix, 98% by weight of the anti-efflorescence formulation of example 4 was taken in a mixing vessel. Then additives such as 1% by weight low shear HEUR based thickener, 0.9% by weight fatty alcohol ethoxylates (wetting agents), and 0.1% by weight mineral oil based defoamers were 21
added to the mixture and mixed using a mechanical mixer or a magnetic stirrer at
low speed for about 15 minutes until a uniform coating mixture was obtained.
(b) Concrete mix
[00089]
A concrete mix was prepared by taking 1 part by weight of cement, 2 parts by weight of sand and 4 parts by weight of aggregates with 1% by weight of 5 superplasticizer additive (by weight of cement) into a mixing vessel. It was mixed using a mechanical mixer at low speed for about 5 minutes to obtain a uniform mixture. 2% by weight of the anti-efflorescence formulation (by weight of cement) as prepared in Example 4 were gradually added into this mixture, along with 0.5 parts of water, followed by mixing for 5 minutes, until a homogenous concrete mix 10 was obtained.
(c) Mortar mix
[00090]
A mortar mix was prepared by taking 1 part by weight of cement, 3 parts by weight of sand with 1% by weight of superplasticizer additive (by weight of cement) into a mixing vessel. It was mixed using a mechanical mixer at low speed 15 for about 5 minutes to obtain a uniform mixture. 2% by weight of the anti-efflorescence formulation (by weight of cement) as prepared in Example 4 were gradually added into this mixture, along with 0.5 parts of water, followed by mixing for 5 minutes, until a homogenous mortar mix was obtained.
Example 6 20 Evaluation of an efflorescence inhibiting composition
[00091] The efflorescence inhibiting composition as prepared in Example 2 was evaluated by applying it to aerated cement panels. The sides of each panel were sealed using a waterproofing paint. A single coat of anti-efflorescence formulation as prepared in Example 4 was applied over the panel. After allowing for 24 hours 25 of drying, two additional coats of wall putty were applied. Subsequently, the panels were coated with a pink high PVC paint, which contained 50% PVC based on an aqueous styrene acrylic emulsion. Once the application process was complete, the panels were submerged in a 20% sodium chloride salt solution for experimental
22
evaluation. Observations were recorded regarding salt migration on days 1, 14, and
21 (Figure 1). The result of the evaluation is summarized in the Table 5.
[00092]
Further, it is to be noted that, the efflorescence inhibiting composition thus prepared can also be used for pavers, concrete bricks, stones, or concrete furniture.
Table 5 5 Sample Results after 1 day Results after 14 days Results after 21 days
Blank (without additive)
No salt observed
Salt observed
Salt observed
A1
No salt observed
No salt observed
No salt observed
B1
No salt observed
No salt observed
No salt observed
C1
No salt observed
No salt observed
No salt observed
A2
No salt observed
No salt observed
Salt observed
A3
No salt observed
Salt observed
Salt observed
A4
No salt observed
No salt observed
No salt observed
A5
No salt observed
No salt observed
No salt observed
A6
No salt observed
No salt observed
Salt observed
[00093]
It can be inferred that, the panels coated with additive compositions A1, B1, C1, A4, and A5, as disclosed in present disclosure, along with paint coat exhibited no efflorescence or salt formation even after 21 days.
10
ADVANTAGES OF THE PRESENT DISCLOSURE
[00094] The present disclosure provides an additive composition comprising an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof, which is modified with a C4 – C20 monoepoxide functional monomer; and treated with at least one alkali metal salt solution. The 15 additive composition/ efflorescence inhibiting composition as disclosed in present disclosure can eliminate or prevent efflorescence, a common issue in water-based paints and primers. Further, additive composition/ efflorescence inhibiting composition as disclosed herein can be easily incorporated into the paint/coating 23
formulations without the need for additional solvents, making it more convenient and efficient. Further, the additive composition/ efflorescence inhibiting composition as disclosed herein has optimal acid value, which results in high water resistance or hydrophobicity, which enables the composition to prevent efflorescence for a longer duration without the need for expensive additives such as 5 silanes and silicones.
24
I/We Claim:
1. An additive composition comprising:
(a) an adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof;
(b) a C4 – C20 monoepoxide functional monomer; and 5
(c) at least one alkali salt solution,
wherein the additive composition has an acid number in the range of 100 to 200 mg KOH/g.
2. The additive composition as claimed in claim 1, wherein the additive composition has an acid number in the range of 120 to 180 mg KOH/g. 10 3. The additive composition as claimed in claim 1, wherein the C4 – C20 monoepoxide functional monomer is selected from a group consisting of glycidyl ester of versatic acid 10, aromatic monoepoxide based on para-tertiary butyl phenol, aliphatic monoepoxide based on C12-C14 alcohol, monoepoxide based on phenol, monoepoxide based on o-cresol, monoepoxide based on p-tertiary butyl phenol, and 15 monoepoxide based on n-butanol.
4. The additive composition as claimed in claim 1, wherein the adduct is a Diels-Alder adduct of diene selected from the group consisting of unsaturated fatty acids, unsaturated cyclic compounds, and mixtures thereof with dienophile selected from the group consisting of maleic anhydride, fumaric acid, maleic acid, mono alkyl 20 ester of fumaric acid, dialkyl ester of fumaric acid, acrylic acid, C1-C12 alkyl ester of acrylic acid, methacrylic acid, C1-C12 alkyl ester of methacrylic acid, itaconic acid, C1-C12 alkyl ester of itaconic acid, C1-C12 alkyl ester of maleic acid, and mixtures thereof.
5. The additive composition as claimed in claim 4, wherein the diene is a 25 combination of unsaturated fatty acids, and unsaturated cyclic compounds. 6. The additive composition as claimed in claim 1, wherein the unsaturated vegetable oil fatty acid is derived from an unsaturated vegetable oil selected from the group consisting of soybean oil, linseed oil, sunflower oil, castor oil, dehydrated
25
castor oil, tall oil, corn oil, canola oil, rapeseed oil, palm kernel oil, cottonseed oil, peanut oil, coconut oil, palm oil, tung oil, safflower oil, and combinations thereof.
7. The additive composition as claimed in claim 1, wherein the unsaturated cyclic compound is selected from the group consisting of rosin, terpenes, polyterpenes, terpeneoid, a resin acid (abietic acid), colophony, terpene resin, terpene-phenol 5 resin, and derivatives thereof.
8. The additive composition as claimed in claim 1, wherein the unsaturated vegetable oil fatty acid, unsaturated cyclic compound, dienophile, and C4 to C20 monoepoxide functional monomer is present in a weight ratio range of 0.25:1:0.2:0.3 to 1.6:1:0.5:1.5. 10
9. The additive composition as claimed in claim 1 optionally comprises, ingredients selected from the group consisting of defoamers, biocides, in-can preservatives, thickeners, wetting agent, dispersing agents, super plasticizer additive, and combinations thereof. 10. The additive composition as claimed in claim 1, wherein the alkali is selected 15 from sodium hydroxide, potassium hydroxide, ammonium hydroxide, primary amine, secondary amine, tertiary amine or alkanolamine.
11. A process of preparing the additive composition, the process comprising contacting unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, a monoepoxide functional monomer, and at least one alkali metal salt solution to 20 obtain the additive composition. 12. An anti-efflorescence formulation comprising:
(a) water; and
(b) polymer selected from the group consisting of acrylic polymers, styrene acrylic polymers, vinyl acrylic copolymer, epoxy polymer, polyester, 25 polyurethane, polysiloxane, fluorinated polymer, and mixtures thereof.
(c) organic and inorganic pigments and fillers, and
(d) the additive composition as claimed in any one of the claims 1-10, wherein the additive composition weight percentage is in the range of 0.1 to 2 % based on the total weight of the formulation. 30 26
13. The anti-efflorescence formulation as claimed in claim 12, wherein the organic and inorganic pigments are selected from a group consisting of titanium oxide, zirconium oxide, zinc oxide, silicon oxide, aluminum oxide, aluminum pigments, iron pigments, copper pigments, bismuth pigments, manganese pigments, and combinations thereof; and the fillers are selected from a group consisting of silica, 5 zinc oxide, barium sulfate, calcium carbonate, marble powder, dolomite, steatite, talc, and combinations thereof. 14. A composition comprising the anti-efflorescence formulation as claimed in claim 12. 15. The composition as claimed in claim 14, wherein the composition is selected 10 from coating mix, concrete mix, and mortar mix.
16. A method of preventing efflorescence on surfaces of a substrate by the incorporation of the additive composition as claimed in any one of the claims 1-10 or the anti-efflorescence formulation as claimed in claim 12. 17. The method as claimed in claim 16, wherein the substrate is selected from 15 pavers, concrete bricks, stones or concrete furniture. 18. An efflorescence inhibiting composition comprising (a) chemically modified adduct based on unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof; (b) alkali salt solution; 20 wherein the efflorescence inhibiting composition has an acid number less than 300 mg KOH/g. 19. The efflorescence inhibiting composition as claimed in claim 18, wherein the acid number is in between 100 to 200 mg KOH/g. 20. The efflorescence inhibiting composition as claimed in claim 18, wherein the 25 chemically modified adduct is prepared by treating Diels Alder adduct of unsaturated vegetable oil fatty acids, unsaturated cyclic compounds, and mixtures thereof with a monoepoxide selected from a glycidyl ester of branched C4 – C20 carboxylic acid, aliphatic monoepoxide based on C12-C14 alcohol, or aromatic monoepoxide based on para-tertiary butyl phenol. 30 27
21. The efflorescence inhibiting composition as claimed in claim 18, wherein the alkali salt is selected from sodium salt, potassium salt, or ammonium salt.