Abstract: ABSTRACT POLYOL EMULSION AND A PROCESS FOR ITS PREPARATION The present disclosure relates to a polyol emulsion. The polyol emulsion comprises a polyol; at least one plasticizer; at least one surface active agent; at least one defoamer; optionally, at least one additive and q.s. water. The present disclosure further relates to a process for preparation of a polyol emulsion. The polyol emulsion of the present disclosure is highly stable, has long shelf life and has excellent flow and leveling during application.
DESC:FIELD
The present disclosure relates to a polyol emulsion and a process for its preparation.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
Emulsion and epoxy paints are well known for wall and floor coatings. With increasing requirements on performance, polyurethane coatings are used in various cases for high-performance architectural coatings. However, conventional polyurethane coatings are solvent-based, which may cause strong odor, high volatile organic compound (VOC) emissions and a fire/explosion hazard, especially for interior applications.
The cementitious flooring compositions are widely used for obtaining smooth and chemically and mechanically resistant flooring. In many such applications, the epoxy resin based flooring compositions become an appropriate solution, due to the fact that they often provide aesthetically pleasing and glossy surfaces. On the other hand, the epoxy resin based flooring compositions suffer from certain disadvantages such as undesired blushing effects that may occur, especially at lower temperatures. Furthermore, the chemicals involved (i.e. epoxides and amines) in the epoxy resin based flooring compositions are increasingly considered hazardous.
Conventionally, the polymer cement hybrid is prepared from castor oil based polyol emulsion that includes castor oil and mono-epoxides which are combined with methylene diphenyl diisocyanate (MDI) and cement. However, the pot life of this polyol emulsion is very less and therefore, not optimally processable.
Therefore, there is, felt a need to develop a polyol emulsion which obviates the drawbacks mentioned herein above.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows.
An object of the present disclosure is to ameliorate one or more problems of the prior art or to at least provide a useful alternative.
Another object of the present disclosure is to provide a polyol emulsion.
Yet another object of the present disclosure is to provide a polyol emulsion that is highly stable and has a long shelf life.
Still another object of the present disclosure is to provide a simple and an environment friendly process for the preparation of a polyol emulsion.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.
SUMMARY
The present disclosure relates to a polyol emulsion. The polyol emulsion comprises a polyol; at least one plasticizer; at least one surface active agent; at least one defoamer; optionally, at least one additive and q.s. water.
The present disclosure further relates to a process for preparation of a polyol emulsion. The process comprises the step of mixing predetermined amounts of a polyol and at least one plasticizer under stirring at a first predetermined speed for a first predetermined time period to obtain a pre-emulsion. Separately, predetermined amounts of at least one surface active agent, at least one defoamer and optionally, at least one additive are mixed in water under stirring at a second predetermined speed for a second predetermined time period to obtain a mixture. The stirring speed of the mixture is raised to a third predetermined speed and the pre-emulsion is added gradually to the mixture over a third predetermined time period to obtain the polyol emulsion.
DETAILED DESCRIPTION
The present disclosure relates to a polyol emulsion 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.
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.
The use of vegetable oil as a raw material to prepare a polyol emulsion for various applications is known in the art. However, since the long-chain structure of the vegetable oil is an aliphatic straight chain and is highly flexible, the mechanical properties and the stability of the polyol emulsion prepared therefrom are not ideal.
Conventionally, the polymer cement hybrid is prepared from castor oil based polyol emulsion that includes castor oil and mono-epoxides which are combined with methylene diphenyl diisocyanate (MDI) and cement. However, the pot life of the polyol emulsion is very less and therefore, not optimally processable.
The present disclosure provides a polyol emulsion and a process for its preparation.
In an aspect, the present disclosure provides a polyol emulsion comprising:
i. a polyol;
ii. at least one plasticizer;
iii. at least one surface active agent;
iv. at least one defoamer;
v. optionally, at least one additive; and
vi. q.s. water.
In an embodiment of the present disclosure, the polyol emulsion comprises:
i. 30 to 60 wt% of polyol;
ii. 5 to 30 wt% of at least one plasticizer;
iii. 2 to 8 wt% of at least one surface active agent;
iv. 0.1 to 3 wt% of at least one defomer ;
v. 0 to 5 wt % of at least one additive; and
vi. q.s. water.
wherein the mass% of each component is with respect to the total mass of the emulsion.
In accordance with the present disclosure, the polyol can be selected from 12-hydroxy-9-cis-octadecenoic acid, and modified 12-hydroxy-9-cis-octadecenoic acid. In an exemplary embodiment of the present disclosure, the polyol is a 12-hydroxy-9-cis-octadecenoic acid. In another exemplary embodiment of the present disclosure, the polyol is a modified 12-hydroxy-9-cis-octadecenoic acid.
12-hydroxy-9-cis-octadecenoic acid is modified by using at least one component selected from mono-epoxide and low molecular weight polyols.
In accordance with the present disclosure, 12-hydroxy-9-cis-octadecenoic acid polyol is blended with wide range of mono-epoxide to get desired hydroxyl value. In an embodiment of the present disclosure, 12-hydroxy-9-cis-octadecenoic acid which is a bifunctional polyol is blended/modified with a long aliphatic chain epoxide, wherein the aliphatic chain can be C8-C14. In an exemplary embodiment of the present disclosure, 12-hydroxy-9-cis-octadecenoic acid which is a bifunctional polyol is blended/modified with C12 mono epoxide.
The plasticizer can be selected from diisononyl phthalate (DINP), bis(2-ethylhexyl) phthalate (also known as dioctyl phthalate-DOP), and , benzoates, benzyl phthalates (Santicizer®160) and diisopropylbenzene (Benzoflex®9-88). In an exemplary embodiment of the present disclosure, the plasticizer is dibutyl phthalate (DBP).
In an embodiment, the amount of plasticizer is balanced in such a way that the final polyol emulsion accommodates any kind of hydrophilic low molecular weight glycols to obtain higher hydroxyl value. The desirable hydrophobicity with long term stability in the polyol emulsion of the present disclosure is achieved by maintaining a specific ratio of 12-hydroxy-9-cis-octadecenoic acid to the plasticizer such as diisononyl phthalate (DINP), dioctyl phthalate (DOP), and dibutyl phthalate (DBP).
The surface active agent can be selected from sorbitan ester, cis-monoalkyl ether of a polyethylene glycol, C8-C30 fatty alcohol ethoxylates, alkylphenol alkoxylates, polyoxyethylene polyoxypropylene block copolymers, C8-C22 fatty acid esters of polyoxyethylene glycol, ethoxylated monoglycerides, ethoxylated diglycerides, sorbitan esters, ethoxylated sorbitan esters, C8-C22 fatty acid glycol esters and block copolymers of ethylene oxide and propylene oxide.
In accordance with the present disclosure, C8-C30 fatty alcohol ethoxylate is selected from capryl alcohol ethoxylate, lauryl alcohol ethoxylate, myristyl alcohol ethoxylate, cetyl alcohol ethoxylate, stearyl alcohol ethoxylate, cetearyl alcohol ethoxylate, sterol ethoxylate, oleyl alcohol ethoxylate and behenyl alcohol ethoxylate.
Alkylphenol alkoxylate is octylphenol ethoxylates.
In an embodiment of the present disclosure, the surface active agent is C8-C30 alcohol ethoxylates. In an exemplary embodiment of the present disclosure, the surface active agent is myristyl alcohol ethoxylate.
In another embodiment of the present disclosure, the surface active agent is a mixture of sorbitan ester and cis-monoalkyl ether of a polyethylene glycol. In accordance with the present disclosure, a mass ratio of the sorbitan ester to the cis-monoalkyl ether of a polyethylene glycol is in the range of 1:0.1 to 1:1. Cis-monoalkyl ether of a polyethylene glycol is Tergitol (a secondary ethoxylated alcohol).
In accordance with the present disclosure, the mixture of surface active agents is used to get maximum stability of the polyol emulsion with excellent flowability and levelling during applications.
The defoamer is oil based defoamer.
The oil based defoamer is selected from BYK 033, BYK-030, AM1512, Antimussol AC, Antimussol NS 22, Antimussol P, Antimussol V1, Indofoam 1011 and FOAM BLAST® 320CT. In an exemplary embodiment of the present disclosure, the defoamer is BYK 033.
The additive can be selected from biocide, sorbitol, glycerol, polyethylene glycol (PEG), 1,2-ethanediol, 1,2- propanediol, 1,3-propanediol, neopentylglycol, diethylene glycol, triethylene glycol, isomeric dipropylene glycols, tripropylene glycols, isomeric butanediols, pentanediols, hexanediols, heptanediols, octanediols, nonanediols, decanediols, undecanediols, 1,3- and 1,4-cyclohexanedimethanol, hydrogenated bisphenol A, dimeric fatty alcohols, 1,1,1-trimethylolethane, 1,1,1-trimethylolpropane, glycerol, pentaerythritol, sugar alcohols, sugars (sucrose) and low molecular weight alkoxylation products of dihydric and polyhydric alcohols.
Isomeric butanediol is selected from 1,2-, 1,3-, and 1,4-butandediol
Sugar alcohol is selected from xylitol, sorbitol and mannitol.
In an exemplary embodiment of the present disclosure, the low molecular weight glycol is diethylene glycol (DEG). In another exemplary embodiment of the present disclosure, the low molecular weight glycol is triethylene glycol (TEG).
The low molecular weight polyhydroxyl molecules are generally not incorporated in non-pigmented hydrophobic polyol emulsion due to significant hydrophilicity of low molecular weight polyol and lower pot life during curing. However, in accordance with the present disclosure, a stable, hydrophobic polyol emulsion of different hydroxyl value is obtained through incorporation of low molecular weight glycols such as sorbitol, glycerol, PEG, DEG and the like.
In an embodiment of the present disclosure, the biocide is Nipacid CFX.
In a first exemplary embodiment of the present disclosure, the polyol emulsion comprises 53.2 mass% of 12-hydroxy-9-cis-octadecenoic acid(polyol) which is modified with 5.5 mass% of C12 mono epoxide (mono-epoxide), 8.2 mass% of DBP (plasticizer), 0.5 mass% of mineral oil (defoamer), 0.1 mass% of Nipacid CFX (additive-biocide), 3 mass% of myristyl alcohol ethoxylate (surfactant), and 29.5 mass% of water, wherein the mass% of each component is with respect to the total mass of the emulsion.
In a second exemplary embodiment of the present disclosure, the polyol emulsion comprises 46.4 mass% of 12-hydroxy-9-cis-octadecenoic acid(polyol) which is modified with 10.5 mass% of C12 mono epoxide (mono-epoxide), 10 mass% of DBP (plasticizer), 0.5 mass% of mineral oil (defoamer), 0.1 mass% of Nipacid CFX (additive-biocide), 3 mass% of cetyl alcohol ethoxylate (surfactant), and 30 mass% of water, wherein the mass% of each component is with respect to the total mass of the emulsion.
In a third exemplary embodiment of the present disclosure, the polyol emulsion comprises 36 mass% of 12-hydroxy-9-cis-octadecenoic acid(polyol), 25.4 mass% of DBP (plasticizer), 5 mass% of TEG (low molecular weight glycol-additive), 0.5 mass% of mineral oil (defoamer), 0.1 mass% of Nipacid CFX (additive-biocide), 3 mass% of myristyl alcohol ethoxylate (surfactant), and 30 mass% of water, wherein the mass% of each component is with respect to the total mass of the emulsion.
In a fourth exemplary embodiment of the present disclosure, the polyol emulsion comprises 36 mass% of 12-hydroxy-9-cis-octadecenoic acid(polyol), 25 mass% of DBP (plasticizer), 5 mass% of DEG (low molecular weight glycol-additive), 0.5 mass% of mineral oil (defoamer), 0.1 mass% of Nipacid CFX (additive-biocide), 3 mass% of cetyl alcohol ethoxylate (surfactant), and 30.4 mass% of water, wherein the mass% of each component is with respect to the total mass of the emulsion.
In another aspect, the present disclosure provides a process for the preparation of a polyol emulsion.
The process comprises the step of mixing predetermined amounts of a polyol and at least one plasticizer under stirring at a first predetermined speed for a first predetermined time period to obtain a pre-emulsion. Separately, predetermined amounts of at least one surface active agent, at least one defoamer and optionally, at least one additive are mixed in water under stirring at a second predetermined speed for a second predetermined time period to obtain a mixture. The stirring speed of the mixture is raised to a third predetermined speed and the pre-emulsion is gradually added to the mixture over a third predetermined time period to obtain the polyol emulsion.
In accordance with the present disclosure, the polyol can be selected from 12-hydroxy-9-cis-octadecenoic acid, and modified 12-hydroxy-9-cis-octadecenoic acid and the predetermined amount of polyol is in the range of 30 mass% to 60 mass%.
12-hydroxy-9-cis-octadecenoic acid is modified by using at least one component selected from mono-epoxide and low molecular weight polyols.
In an exemplary embodiment of the present disclosure, the polyol is C12 mono-epoxide modified 12-hydroxy-9-cis-octadecenoic acid and the predetermined amount of C12 mono-epoxide modified 12-hydroxy-9-cis-octadecenoic acid is 58.7 mass%. In another exemplary embodiment of the present disclosure, the predetermined amount of C12 mono-epoxide modified 12-hydroxy-9-cis-octadecenoic acid is 56.9 mass%. In still another exemplary embodiment of the present disclosure, the polyol is 12-hydroxy-9-cis-octadecenoic acid and the predetermined amount of 12-hydroxy-9-cis-octadecenoic acid is 36 mass%.
In accordance with the present disclosure, the plasticizer can be selected from diisononyl phthalate (DINP), bis(2-ethylhexyl) phthalate (also known as dioctyl phthalate-DOP), and dibutyl phthalate (DBP) and the predetermined amount of plasticizer is in the range from 5 mass% to 30 mass%. In an exemplary embodiment of the present disclosure, the plasticizer is DBP and the amount of DBP is 8.2 mass%. In another exemplary embodiment of the present disclosure, the amount of DBP is 10 mass%. In still another exemplary embodiment, the amount of DBP is 25.4 mass%. In yet another exemplary embodiment, the amount of DBP is 25 mass%.
In accordance with the present disclosure, the surface active agent can be selected from sorbitan ester, cis-monoalkyl ether of a polyethylene glycol, C8-C30 fatty alcohol ethoxylates, alkylphenol alkoxylates, polyoxyethylene polyoxypropylene block copolymers, C8-C22 fatty acid esters of polyoxyethylene glycol, ethoxylated monoglycerides, ethoxylated diglycerides, sorbitan esters, ethoxylated sorbitan esters, C8-C22 fatty acid glycol esters and block copolymers of ethylene oxide and propylene oxide.
In accordance with the present disclosure, C8-C30 fatty alcohol ethoxylate is selected from capryl alcohol ethoxylate, lauryl alcohol ethoxylate, myristyl alcohol ethoxylate, cetyl alcohol ethoxylate, stearyl alcohol ethoxylate, cetearyl alcohol ethoxylate, sterol ethoxylate, oleyl alcohol ethoxylate and behenyl alcohol ethoxylate.
Alkylphenol alkoxylate is octylphenol ethoxylates.
The predetermined amount of surface active agent is in the range of 2 mass% to 8 mass%.
In an embodiment of the present disclosure, the surface active agent is C8-C30 alcohol ethoxylates. In an exemplary embodiment of the present disclosure, the surface active agent is myristyl alcohol ethoxylate.
In accordance with the present disclosure, the defoamer is oil based defoamer.
The oil based defoamer is selected from BYK 033, BYK-030, AM1512, Antimussol AC, Antimussol NS 22, Antimussol P, Antimussol V1, Indofoam 1011 and FOAM BLAST® 320CT.
The predetermined amount of defoamer is in the range from 0.1 mass% to 3 mass%. In an exemplary embodiment of the present disclosure, the defoamer is BYK 033 and the amount of BYK 033 is 0.5 mass%.
In accordance with the present disclosure, the additive is selected from biocide, sorbitol, glycerol, polyethylene glycol (PEG), 1,2-ethanediol, 1,2- propanediol, 1,3-propanediol, neopentylglycol, diethylene glycol, triethylene glycol, isomeric dipropylene glycols, tripropylene glycols, isomeric butanediols, pentanediols, hexanediols, heptanediols, octanediols, nonanediols, decanediols, undecanediols, 1,3- and 1,4-cyclohexanedimethanol, hydrogenated bisphenol A, dimeric fatty alcohols, 1,1,1-trimethylolethane, 1,1,1-trimethylolpropane, glycerol, pentaerythritol, sugar alcohols, sugars (sucrose) and low molecular weight alkoxylation products of dihydric and polyhydric alcohols.
Isomeric butanediol is selected from 1,2-, 1,3-, and 1,4-butandediol
Sugar alcohol is selected from xylitol, sorbitol and mannitol.
The biocide is Nipacid CFX.
The amount of additive is in the range from 0 mass% to 5 mass%. In an exemplary embodiment of the present disclosure, the amount of Nipacid CFX is 0.1 mass%. In another exemplary embodiment of the present disclosure, the amount of TEG is 5 mass%. In still another embodiment of the present disclosure, the amount of DEG is 5 mass%.
In an embodiment of the present disclosure, the first predetermined speed is in the range of 600 rpm to 800 rpm. In an exemplary embodiment of the present disclosure, the first predetermined speed is 700 rpm.
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 third predetermined speed is in the range of 1000 rpm to 2000 rpm.
In an embodiment of the present disclosure, the first and the second predetermined time period is independently in the range of 2 minutes to 10 minutes. In an exemplary embodiment, the first and the second predetermined time period is 5 minutes.
In an embodiment of the present disclosure, the third predetermined time period is in the range of 10 minutes to 50 minutes. In an exemplary embodiment, the third predetermined time period is 20 minutes.
In accordance with the present disclosure, the polyol emulsion is used in floor coatings, in constructions and several civil engineering applications.
Conventional castor oil emulsions are generally made with very high loading of castor oil (more than 55%) with mono epoxide and lower dose of plasticizer which leads to oil layer separation after certain time. However, the present disclosure provides the use of lower amount of castor oil (still managing the hydroxy value) modified with multifunctional glycol with higher loading of plasticizer that results in improved properties of the emulsion such as shelf life, pot life and flow and levelling.
The foregoing description of the embodiments has been provided for purposes of illustration and not intended to limit the scope of the present disclosure. Individual components of a particular embodiment are generally not limited to that particular embodiment but are interchangeable. Such variations are not to be regarded as a departure from the present disclosure, and all such modifications are considered to be within the scope of the present disclosure.
The present disclosure is further described in light of the following experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. The following experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial scale.
EXPERIMENTAL DETAILS
Experiment 1: Process for the preparation of polyol emulsion in accordance with the present disclosure
General process for the preparation of a polyol emulsion
Predetermined amounts of polyol and plasticizer were mixed under stirring at a speed of 700 rpm for 5 minutes to obtain a pre-emulsion. Separately, predetermined amounts of mineral oil (defoamer), Nipacid CFX (additive), sorbitan monolaurate (surfactant) and Tergitol (surfactant) were mixed in water under stirring at a speed of 1000 rpm for 5 minutes to obtain a mixture. The speed of the mixture was raised to 1500 rpm and the pre-emulsion was gradually added to the mixture over 20 minutes and continued stirring for 5 minutes to obtain a polyol emulsion.
Examples 1 to 4:
The polyol emulsions were prepared by following the above general process. The specific components with specific amounts used in examples 1 to 4 are summarized in Table 1.
Table 1
Components Example 1 Example 2 Example 3 Example 4
Polyol
(12-hydroxy-9-cis-octadecenoic acid) 12-hydroxy-9-cis-octadecenoic acid 53.2 g 12-hydroxy-9-cis-octadecenoic acid 46.4 g 12-hydroxy-9-cis-octadecenoic acid
36 g 12-hydroxy-9-cis-octadecenoic acid
36 g
C12 mono epoxy 5.5 g 10.5 g - -
Plasticizer
(DBP) 8.2 g 10 g 25.4 25
Defoamer
(Mineral oil- BYK 033) 0.5 g 0.5 g 0.5 g 0.5 g
Additive Nipacid CFX 0.1 g 0.1 g 0.1 g 0.1 g
DEG - - - 5 g
TEG - - 5 g -
Surface active agents myristyl alcohol ethoxylate 3 g 3 g 3 g 3 g
Water 29.5 g 29.5 g 30 g 30.4 g
Total 100 g 100 g 100 g 100 g
Experiment 2: Characterization of the Polyol emulsion of the present disclosure
The polyol emulsions prepared according to the examples 1-4 were characterized for the parameters such as viscosity, % NVM (Non volatile matter) and pot life (minutes). Table 2 below summarizes the characterization values of the polyol emulsions of examples 1 to 4 prepared according to the present disclosure.
Table 2: Characterization of the polyol emulsions of Examples 1 to 4
Parameters Example 1 Example 2 Example 3 Example 4
Viscosity ( cP) 150 145 170 160
% NVM 70% 70% 70.02 70.1
pH 5.6 5.8 5.5 5.6
Comparative Example:
An emulsion was prepared and used to perform the comparative studies. The emulsion comprised 32 kg of demineralized water, 60 kg of 12-hydroxy-9-cis-octadecenoic acid, 10 kg of Polypox R24 (monoepoxides), 1.85 kg of Wallinat SML (sorbitan, monolaurate), 0.1 kg of Vanquish 100 (antimicrobial/ antifungal additive), 1.2 kg of Byk 501 (silicone-free air release additive), 1 kg of Natrosol Type 250LR (thickener) and 0.65 kg of Tergitol 15S40 (surfactant).
The results are summarized in Table 3.
Table 3: Comparative studies
Performance Properties Emulsion of comparative example Polyol emulsion of Example 3
Pot life 10-12 min 16-18 min
Surface Defect Pinhole, blister Zero surface defect
Flow and levelling Poor, application marks Excellent
Compressive Strength (MPa) 32.6 41.5
Flexural Strength (MPa) 13.5 18.2
Tensile Strength (MPa) 6.4 9.3
From Table 3, it is observed that the polyol emulsion of the present disclosure has pot life, compressive strength, flexural strength and tensile strength are greater than those of the comparative emulsion. Thus, the polyol emulsion of the present disclosure is highly stable having long shelf life and excellent flow and leveling with zero surface defects during application. Whereas, the comparative emulsion has poor flow and leveling with pinholes and blister formation (surface defects) during application.
Experiment 3: Stability and shelf life studies for the polyol emulsion of the present disclosure
The polyol emulsion prepared in Example 3 in accordance with the present disclosure was studied for stability and shelf life. The results are summarized in Table 4.
Table 4: Stability data for polyol emulsion of Example 3
Parameters Initial Sample After 2 month at Oven (at 55 °C) After 6 month at RT
Viscosity (cP) 302 304 307
% NVM 66.02 66.2 66.1
Pot life (Minutes) 16 16 16
Flow Leveling 10/10 10/10 10/10
Pinhole 10/10 10/10 10/10
Compressive Strength (MPa) 40.7 40.5 40.5
The result of Table 4 indicates that the polyol emulsion (as prepared in example 3) was highly stable having long shelf life and excellent flow and leveling during application. There were no major changes observed in the parameters of the initial polyol emulsion and polyol emulsion after 6 months. The polyol emulsion remained stable even after 6 months at room temperature having viscosity 307 cP, %NVM 66.1, pot life of 16 minutes, excellent flow leveling and pinhole, and compressive strength of 40.5 MPa.
TECHNICAL ADVANCEMENTS
The present disclosure described herein above has several technical advantages including, but not limited to, the realization of;
? a polyol emulsion that;
• is highly stable;
• has long shelf life;
• has excellent flow and levelling during applications; and
• is economic; and
? a process for the preparation of a polyol emulsion that;
• is simple, economic, efficient and environmental friendly.
Throughout this specification the word “comprise”, or variations such as “comprises” or “comprising, will be understood to imply the inclusion of a stated element, integer or step,” or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or results. While certain embodiments of the inventions have been described, these embodiments have been presented by way of example only, and are not intended to limit the scope of the inventions. Variations or modifications to the formulation of this invention, within the scope of the invention, may occur to those skilled in the art upon reviewing the disclosure herein. Such variations or modifications are well within the spirit of this invention.
The numerical values given for various physical parameters, dimensions and quantities are only approximate values and it is envisaged that the values higher than the numerical value assigned to the physical parameters, dimensions and quantities fall within the scope of the invention unless there is a statement in the specification to the contrary.
While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated that many additional features can be added and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation. ,CLAIMS:WE CLAIM:
1. A polyol emulsion comprising:
i. a polyol;
ii. at least one plasticizer;
iii. at least one surface active agent;
iv. at least one defoamer;
v. optionally, at least one additive; and
vi. q.s. water.
2. The emulsion as claimed in claim 1 comprises:
i. 30 to 60 mass% of said polyol;
ii. 5 to 30 mass% of said plasticizer;
iii. 2 to 8 mass% of said surface active agent;
iv. 0.1 to 3 mass% of said defoamer ;
v. 0 to 5 mass% of said additive; and
vi. q.s. water,
wherein the mass% of each component is with respect to the total mass of the emulsion.
3. The emulsion as claimed in claim 1, wherein said polyol is selected from the group consisting of 12-hydroxy-9-cis-octadecenoic acid and modified 12-hydroxy-9-cis-octadecenoic acid, wherein said modified 12-hydroxy-9-cis-octadecenoic acid is modified with mono-epoxide.
4. The emulsion as claimed in claim 3, wherein 12-hydroxy-9-cis-octadecenoic acid is modified by using at least one component selected from mono-epoxide and low molecular weight polyols.
5. The emulsion as claimed in claim 1, wherein said plasticizer is selected from the group consisting of diisononyl phthalate (DINP), dioctyl phthalate-DOP, dibutyl phthalate (DBP), benzoates, benzyl phthalates and diisopropylbenzene.
6. The emulsion as claimed in claim 1, wherein said surface active agent is at least one selected from the group consisting of sorbitan ester, cis-monoalkyl ether of a polyethylene glycol, C8-C30 fatty alcohol ethoxylates, alkylphenol alkoxylates, polyoxyethylene polyoxypropylene block copolymers, C8-C22 fatty acid esters of polyoxyethylene glycol, ethoxylated monoglycerides, ethoxylated diglycerides, sorbitan esters, ethoxylated sorbitan esters, C8-C22 fatty acid glycol esters and block copolymers of ethylene oxide and propylene oxide;
wherein said C8-C30 fatty alcohol ethoxylates are selected from capryl alcohol ethoxylate, lauryl alcohol ethoxylate, myristyl alcohol ethoxylate, cetyl alcohol ethoxylate, stearyl alcohol ethoxylate, cetearyl alcohol ethoxylate, sterol ethoxylate, oleyl alcohol ethoxylate and behenyl alcohol ethoxylate.
7. The emulsion as claimed in claim 1, wherein said defoamer is oil based defoamer; wherein said oil based defoamer is selected from BYK 033, BYK-030, AM1512, Antimussol AC, Antimussol NS 22, Antimussol P, Antimussol V1, Indofoam 1011 and FOAM BLAST® 320CT.
8. The emulsion as claimed in claim 1, wherein said additive is at least one selected from the group consisting of biocide, sorbitol, glycerol, polyethylene glycol (PEG)1,2-ethanediol, 1,2- propanediol, 1,3-propanediol, neopentylglycol, diethylene glycol, triethylene glycol, isomeric dipropylene glycols, tripropylene glycols, isomeric butanediols, pentanediols, hexanediols, heptanediols, octanediols, nonanediols, decanediols, undecanediols, 1,3- and 1,4-cyclohexanedimethanol, hydrogenated bisphenol A, dimeric fatty alcohols, 1,1,1-trimethylolethane, 1,1,1-trimethylolpropane, glycerol, pentaerythritol, sugar alcohols, sugars and low molecular weight alkoxylation products of dihydric and polyhydric alcohols.
9. A process for the preparation of a polyol emulsion, said process comprising the following steps:
a) mixing predetermined amounts of a polyol and at least one plasticizer under stirring at a first predetermined speed for a first predetermined time period to obtain a pre-emulsion;
b) separately, mixing predetermined amounts of at least one surface active agent, at least one defoamer and optionally, at least one additive in water under stirring at a second predetermined speed for a second predetermined time period to obtain a mixture; and
c) raising the stirring speed to a third predetermined speed and gradually, adding said pre-emulsion to said mixture over a third predetermined time period to obtain said polyol emulsion.
10. The process as claimed in claim 9, wherein said polyol is selected from the group consisting of 12-hydroxy-9-cis-octadecenoic acid and modified 12-hydroxy-9-cis-octadecenoic acid.
11. The process as claimed in claim 9, wherein 12-hydroxy-9-cis-octadecenoic acid is modified by using at least one component selected from mono-epoxide and low molecular weight polyols.
12. The process as claimed in claim 9, wherein said plasticizer is selected from the group consisting of diisononyl phthalate (DINP), dioctyl phthalate-DOP and dibutyl phthalate (DBP).
13. The process as claimed in claim 9, wherein said first predetermined speed is in the range of 600 rpm to 800 rpm; and said first predetermined time period is in the range of 2 minutes to 10 minutes.
14. The process as claimed in claim 9, wherein said surface active agent is at least one selected from the group consisting of sorbitan ester, cis-monoalkyl ether of a polyethylene glycol, C8-C30 fatty alcohol ethoxylates, alkylphenol alkoxylates, polyoxyethylene polyoxypropylene block copolymers, C8-C22 fatty acid esters of polyoxyethylene glycol, ethoxylated monoglycerides, ethoxylated diglycerides, sorbitan esters, ethoxylated sorbitan esters, C8-C22 fatty acid glycol esters and block copolymers of ethylene oxide and propylene oxide.
15. The process as claimed in claim 9, wherein said defoamer is oil based defoamer; wherein said oil based defoamer is selected from BYK 033, BYK-030, AM1512, Antimussol AC, Antimussol NS 22, Antimussol P, Antimussol V1, Indofoam 1011 and FOAM BLAST® 320CT.
16. The process as claimed in claim 9, wherein said additive is selected from the group consisting of biocide, sorbitol, glycerol, polyethylene glycol (PEG), 1,2-ethanediol, 1,2- propanediol, 1,3-propanediol, neopentylglycol, diethylene glycol, triethylene glycol, isomeric dipropylene glycols, tripropylene glycols, isomeric butanediols, pentanediols, hexanediols, heptanediols, octanediols, nonanediols, decanediols, undecanediols, 1,3- and 1,4-cyclohexanedimethanol, hydrogenated bisphenol A, dimeric fatty alcohols, 1,1,1-trimethylolethane, 1,1,1-trimethylolpropane, glycerol, pentaerythritol, sugar alcohols, sugars (sucrose) and low molecular weight alkoxylation products of dihydric and polyhydric alcohols.
17. The process as claimed in claim 9, wherein said second predetermined speed is in the range of 800 rpm to 1200 rpm; and said second predetermined time period is in the range of 2 minutes to 10 minutes.
18. The process as claimed in claim 9, wherein said third predetermined speed is in the range of 1000 rpm to 2000 rpm; and said third predetermined time period is in the range of 10 minutes to 50 minutes.
19. The process as claimed in claim 9, wherein said predetermined amounts of said polyol is in the range of 30 to 60 mass%; said plasticizers in the range of 5 to 30 mass%; said surface active agent is in the range of 2 to 8 mass%; said defoamer is in the range of 0.1 to 2 mass%; and said additive is in the range of 0 to 5 mass%; and q.s. water,
wherein the mass% of each component is with respect to the total mass of the emulsion.
Dated this 27th day of September, 2022
_______________________________
MOHAN RAJKUMAR DEWAN, IN/PA – 25
of R.K.DEWAN & CO.
Authorized Agent of Applicant
TO,
THE CONTROLLER OF PATENTS
THE PATENT OFFICE, AT MUMBAI
| # | Name | Date |
|---|---|---|
| 1 | 202121044217-STATEMENT OF UNDERTAKING (FORM 3) [29-09-2021(online)].pdf | 2021-09-29 |
| 2 | 202121044217-PROVISIONAL SPECIFICATION [29-09-2021(online)].pdf | 2021-09-29 |
| 3 | 202121044217-PROOF OF RIGHT [29-09-2021(online)].pdf | 2021-09-29 |
| 4 | 202121044217-POWER OF AUTHORITY [29-09-2021(online)].pdf | 2021-09-29 |
| 5 | 202121044217-FORM 1 [29-09-2021(online)].pdf | 2021-09-29 |
| 6 | 202121044217-DECLARATION OF INVENTORSHIP (FORM 5) [29-09-2021(online)].pdf | 2021-09-29 |
| 7 | 202121044217-FORM 18 [27-09-2022(online)].pdf | 2022-09-27 |
| 8 | 202121044217-ENDORSEMENT BY INVENTORS [27-09-2022(online)].pdf | 2022-09-27 |
| 9 | 202121044217-COMPLETE SPECIFICATION [27-09-2022(online)].pdf | 2022-09-27 |
| 10 | 202121044217-FER.pdf | 2024-03-11 |
| 11 | 202121044217-FORM 3 [19-04-2024(online)].pdf | 2024-04-19 |
| 12 | 202121044217-MARKED COPIES OF AMENDEMENTS [23-08-2024(online)].pdf | 2024-08-23 |
| 13 | 202121044217-FORM-26 [23-08-2024(online)].pdf | 2024-08-23 |
| 14 | 202121044217-FORM 13 [23-08-2024(online)].pdf | 2024-08-23 |
| 15 | 202121044217-FER_SER_REPLY [23-08-2024(online)].pdf | 2024-08-23 |
| 16 | 202121044217-CLAIMS [23-08-2024(online)].pdf | 2024-08-23 |
| 17 | 202121044217-AMMENDED DOCUMENTS [23-08-2024(online)].pdf | 2024-08-23 |
| 18 | 202121044217-PatentCertificate22-01-2025.pdf | 2025-01-22 |
| 19 | 202121044217-IntimationOfGrant22-01-2025.pdf | 2025-01-22 |
| 1 | 202121044217_SSE_06-03-2024.pdf |