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A Coating Composition, An Article, Method Related Thereto And Applciations Thereof

Abstract: “A COATING COMPOSITION, AN ARTICLE, METHOD RELATED THERETO AND APPLCIATIONS THEREOF” ABSTRACT The present disclosure relates to a coating composition comprising combination of aminopolysiloxane sol, phosphorylated titania sol, sulfopolyester and additive. The composition provides for improved corrosion resistance and improved formability to a substrate including but not limited to metal and alloy. The disclosure further relates to an article comprising the composition, wherein the composition is in the form of film having highest level of adhesion. The disclosure also relates to method of preparing the composition, method of preparing the article and to a method of coating a substrate with the composition. FIGURE 4

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Patent Information

Application #
Filing Date
30 March 2021
Publication Number
40/2022
Publication Type
INA
Invention Field
POLYMER TECHNOLOGY
Status
Email
Parent Application
Patent Number
Legal Status
Grant Date
2023-10-10
Renewal Date

Applicants

TATA STEEL LIMITED
Jamshedpur-831001, Jharkhand, India

Inventors

1. RACHNA JAIN
C/o Tata Steel Limited, Jamshedpur – 831001, Jharkhand, India
2. MANISH KUMAR BHADU
C/o Tata Steel Limited, Jamshedpur – 831001, Jharkhand, India
3. PUJA KUMARI
C/o Tata Steel Limited, Jamshedpur – 831001, Jharkhand, India
4. NITISH RANJAN GOUTAM
C/o Tata Steel Limited, Jamshedpur – 831001, Jharkhand, India
5. AMAR NATH BHAGAT
C/o Tata Steel Limited, Jamshedpur – 831001, Jharkhand, India
6. SHAIK SHAMSHODDIN
C/o Tata Steel Limited, Jamshedpur – 831001, Jharkhand, India
7. ATANU RANJAN PAL
C/o Tata Steel Limited, Jamshedpur – 831001, Jharkhand, India
8. TAPAN KUMAR ROUT
C/o Tata Steel Limited, Jamshedpur – 831001, Jharkhand, India

Specification

Claims:WE CLAIM:

1. A composition comprising combination of-
a. Aminopolysiloxane sol
b. Phosphorylated titania sol
c. Sulfopolyester; and
d. Additive.
2. The composition as claimed in claim 1, wherein the aminopolysiloxane sol is a combination of epoxy silane and aminoalkyl trialkoxy silane.
3. The composition as claimed in claim 1, wherein the phosphorylated titania sol is a combination of titanium alkoxide, chelating agent, phosphoric acid and solvent.
4. The composition as claimed in claim 1, wherein the additive is selected from a group comprising lubricant, flexibilizer, surface tension reducer (surfactant), corrosion inhibitor and combinations thereof.
5. The composition as claimed in claim 4, wherein the composition comprises combination of aminopolysiloxane sol, phosphorylated titania sol, sulfopolyester, lubricant, flexibilizer, surface tension reducer (surfactant) and corrosion inhibitor.
6. The composition as claimed in claim 2, wherein the epoxy silane is selected from a group comprising ethyl ethoxy tetra epoxy silane, butyl butoxy tetra epoxy silane and combinations thereof; and wherein the epoxy silane is in an amount ranging from about 0.8 wt% to 5 wt%.
7. The composition as claimed in claim 2, wherein the aminoalkyl trialkoxy silane is selected from a group comprising 3-(N-ethyl aminoisobutyl) tributoxy silane, 3(-N-isopropyl aminoisobutyl) mono ethyl di-propyl silane and combinations thereof; and wherein the aminoalkyl trialkoxy silane is in an amount ranging from about 0.5 wt% to 2 wt%.
8. The composition as claimed in claim 3, wherein the titanium alkoxide is selected from a group comprising triethanolamine titanate, titanium isopropoxide, tetra-n-butyl titanate and combinations thereof; and wherein the titanium alkoxide is in an amount ranging from about 2 wt% to 5 wt%.
9. The composition as claimed in claim 3, wherein the chelating agent is selected from a group comprising lactic acid, 3-hydroxybutyric acid, 3-hydroxypentanoic acid and combinations thereof; and wherein the chelating agent is in an amount ranging from about 1 wt% to 2.5 wt%.
10. The composition as claimed in claim 9, wherein the chelating agent is selected from a combination comprising- combination of lactic acid and 3-hydroxybutyric acid in a ratio of about 1:1; combination of lactic acid and 3-hydroxypentanoic acid in a ratio of about 1:1 and combination of 3-hydroxybutyric acid and 3-hydroxypentanoic acid in a ratio of about 1 :1.
11. The composition as claimed in claim 3, wherein the phosphoric acid is in an amount ranging from about 1 wt% to 3 wt%.
12. The composition as claimed in claim 3, wherein the solvent is selected from a group comprising demineralized water and combinations thereof; and wherein the solvent is in an amount ranging from about 63 wt% to 90 wt%.
13. The composition as claimed in claim 1, wherein the sulfopolyester is in an amount ranging from about 2 wt% to 10 wt%.
14. The composition as claimed in claim 4, wherein the corrosion inhibitor is selected from a group comprising magnesium sulfate and wherein the corrosion inhibitor is in an amount ranging from about 0.3 wt% to 2 wt%.
15. The composition as claimed in claim 4, wherein the flexibilizer is selected from a group comprising hexylene glycol, propylene glycol, ethylene glycol and combinations thereof; and wherein the flexibilizer is in an amount ranging from about 2 wt% to 4 wt%.
16. The composition as claimed in claim 4, wherein the surface tension reducer (surfactant) is selected from a group comprising of non-foaming silicon; and wherein the surface tension reducer is in an amount ranging from about 0.1 wt% to 0.5 wt%.
17. The composition as claimed in claim 4, wherein the lubricant is processed/pretreated polypropylene wax and wherein the lubricant is in an amount ranging from about 0.5 wt% to 3 wt%.
18. A method of preparing the composition as claimed in claim 1, said method comprising- mixing of aminopolysiloxane sol, the phosphorylated titania sol, sulfo-polyester and the additive to obtain the composition.
19. The method as claimed in claim 18, wherein the method of preparing the composition comprises:
- preparing the aminopolysiloxane sol;
- preparing the phosphorylated titania sol;
- mixing the aminopolysiloxane sol and the phosphorylated titania sol to obtain mixture- A;
- mixing the sulfopolyester and the mixture-A to obtain mixture-B;
- mixing the additive comprising the corrosion inhibitor, the flexibilizer and the surface tension reducer (surfactant) and the mixture-B to obtain mixture-C; and
- mixing the additive comprising lubricant and the mixture-C to obtain the composition.
20. The method as claimed in claim 19, wherein preparing the aminopolysiloxane sol comprises mixing the epoxy silane and the aminoalkyl trialkoxy silane at a speed ranging from about 600 rpm to 800 rpm for a duration ranging from about 1 hour to 2 hours to obtain the aminopolysiloxane sol.
21. The method as claimed in claim 19, wherein preparing the phosphorylated titania sol comprises-
- mixing the titanium alkoxide and the chelating agent, followed by heating;
- adding the diluted phosphoric acid and mixing to obtain solution, followed by stirring with demineralized water and holding the solution;
22. The method as claimed in 21, wherein the heating is carried out at a temperature ranging from about 60 ºC to 70 ºC by purging nitrogen for a duration ranging from about 15 minutes to 20 minutes.
23. The method as claimed in claim 21, wherein the holding time of the solution is ranging from about 24 hours to 48 hours.
24. The method as claimed in claim 19, wherein the mixing of the aminopolysiloxane sol and the phosphorylated titania sol is carried out at a speed ranging from about 600 rpm to 800 rpm for a duration ranging from about 1 to 2 hours to obtain the mixture-A.
25. The method as claimed in claim 19, wherein the mixing of the mixture-A and the sulfopolyester is carried out in low shear mixer at a speed ranging from about 400 rpm to 600 rpm for a duration ranging from about 15 to 20 minutes to obtain the mixture-B.
26. The method as claimed in claim 19, wherein the mixing of the corrosion inhibitor, the flexibilizer and the surface tension reducer (surfactant) and the mixture-B is carried out at a speed ranging from about 600 rpm to 800 rpm for a duration ranging from about 15 to 20 minutes to obtain the mixture-C.
27. The method as claimed in claim 19, wherein the mixing of the lubricant and the mixture-C is carried out in high shear mixer at a speed ranging from about 1200 to 1500 rpm for a duration ranging from about 1 to 2 hours.
28. An article comprising the composition as claimed in claim 1.
29. The article as claimed in claim 28, wherein the composition is in a form of a film on surface of the article, wherein the thickness of the film is ranging from about 0.5 nm to 3000 nm.
30. The article as claimed in claim 29, wherein the film has highest level of adhesion with the article, having ASTM class of about 5B, according to American standard test method (ASTM).
31. The article as claimed in claim 28, wherein the article has corrosion resistance from salt spray test ranging from about 200 to 250 hours.
32. The article as claimed in claim 28, wherein the article has fracture point ranging from about 45 KN to 90 KN.
33. A method of producing the article as claimed in claim 28, wherein the method comprising- coating a substrate with the composition as claimed in claim 1, followed by curing to obtain the article.
34. The method as claimed in claim 33, wherein the coating is carried out by technique selected from a group comprising spray coating, dip coating, roll coating, wiping method and combinations thereof.
35. The method as claimed in claim 33, wherein the curing is carried out at a temperature ranging from about 90 to 1000C of peak metal temperature for a duration ranging from about 2 to 3 seconds.
36. A method of coating a substrate with the composition as claimed in claim 1 for improving corrosion resistance of the substrate, wherein the coating is carried out by a technique selected from a group comprising spray coating, dip coating, roll coating, wiping method and combinations thereof.
37. The method as claimed in claim 36, wherein the method comprises curing coated substrate at a temperature ranging from about 90 to 1000C for a duration ranging from about 2 to 3 seconds.
38. The method as claimed in claim 37, wherein the coated substrate has corrosion resistance from salt spray test ranging from about 200 to 250 hours; and wherein the coated substate has fracture point ranging from about 45 KN to 90 KN.
39. The method as claimed in claim 36, wherein the substrate is selected from a group comprising metal, alloy and combinations thereof.

Dated this 30th day of March 2021
Signature:
Name: Sridhar R
To: Of K&S Partners, Bangalore
The Controller of Patents Agent for the Applicant
The Patent Office, at Kolkata IN/PA No. 2598


, Description:TECHNICAL FIELD
The present disclosure relates to a field of material science. The present disclosure particularly relates to a coating composition which provides for a protective coating on a substrate. More particularly, the composition provides for improved formability and improved corrosion resistance for a substrate, such as metals and alloys, including but not limited to galvannealed metals, galvannealed alloys, galvanized metal and galvanized alloys. The present disclosure further relates to a method of preparing said coating composition. The present disclosure further relates to an article comprising said composition. The disclosure also relates to method of coating a substrate with said composition for improving formability and corrosion resistance of coated substrate.

BACKGROUND OF THE DISCLOSURE
Untreated metal surfaces are subject to corrosion which can lead to rust development, weakening, discoloration and failure of the surface. For instance, the metallic substrates are prone to get the high rust in open atmosphere. Zinc coating is the viable solution to reduce its red rust tendency which is opted by several industries and the opted method of application of zinc coating over iron substrate is hot dip coating. This versatile process of hot dipping creates a magnitude of the thickness which can protect the steel from corrosion atmospheres at some degree. However, to achieve the high salt resistance, the zinc coating is not a feasibility solution so, conversion coatings like phosphating, chromating are applied over the zinc coating.

Metal objects to which surface treatments and coatings are applied can be grouped into several categories. In some industrial applications, the metal is formed into a 3-dimensional object after which any combination of surface treatments and or coating applications may be made. In a second category of industrial applications, surface treatments and or coatings are applied to the metal prior to forming when the metal is in the form of a flat sheet which is typically rolled into a coil. For many coating applications within this category, special properties are desirable to facilitate rolling and forming operations. For coatings such as organic passivates, it may be desirable to have a high degree of hardness and block-resistance to facilitate rolling, however conventional coatings of high hardness frequently possess poor forming properties in that the integrity of the coating and ultimately its corrosion resistance is compromised by forming operations.

Thus, there exists a need for development of coating composition/solution which provides beneficial effect in terms of corrosion resistance and forming operations.

STATEMENT OF THE DISCLOSURE
Accordingly, the present disclosure provides for a coating composition which is simple, economical and provides for improved corrosion resistance and improved formability properties. Said coating composition comprises combination of – aminopolysiloxane sol; phosphorylated titania sol, sulfopolyester and additive.

The present disclosure further relates to a method of preparing the composition, said method comprising- mixing the aminopolysiloxane sol, the phosphorylated titania sol, the sulfopolyester and the additive to obtain the composition.

The present disclosure further relates to an article comprising the composition described above, wherein the article has corrosion resistance measured by salt spray hours ranging from about 200 hours to 250 hours; and the composition in form of film on the article has highest level of adhesion of about 5B.

The present disclosure further relates to a method of coating a substrate with the composition described above for improving corrosion resistance and formability properties of a substrate, wherein the coating is carried out by technique including but not limited to spray coating, dip coating, roll coating and wiping method.

BRIEF DESCRIPTION OF THE ACCOMPANYING FIGUREs
In order that the present 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 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, where:

Figure 1 illustrates the schematics of preparation of phosphorylated titania sol, wherein the Formula III, IV and V represent titanium alkoxide.

Figure 2 illustrates the schematics of preparation of Aminopolysiloxane sol, wherein the Formula I represent epoxy silane; and the Formula II represent aminoalkyl trialkoxy silane.
Figure 3 illustrates the schematics of combination of the aminopolysiloxane sol (APS) and phosphorylated titania sol (PTS).

Figure 4 illustrates the schematics of grafting of the combination of aminopolysiloxane sol (APS) and phosphorylated titania sol (PTS) with sulfopolyester.

Figure 5 illustrates the formability plot of galvannealed (GA) substrate coated with the composition, the substrate was oiled and non-oiled, respectively.

Figure 6 illustrates the formability plot of galvanized (GI) substrate coated with the composition and uncoated galvanized (GI) substrate, the substrate was oiled and non-oiled, respectively.

DETAILED DESCRIPTION OF THE DISCLOSURE
Definitions:
Unless otherwise defined, all terms used in the disclosure, including technical and scientific terms, have meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. By means of further guidance, term definitions are included for better understanding of the present disclosure.

As used herein, the singular forms ‘a’, ‘an’ and ‘the’ include both singular and plural referents unless the context clearly dictates otherwise.

The term ‘comprising’, ‘comprises’ or ‘comprised of’ as used herein are synonymous with ‘including’, ‘includes’, ‘containing’ or ‘contains’ and are inclusive or open-ended and do not exclude additional, non-recited members, elements or method steps.

The recitation of numerical ranges by endpoints includes all numbers and fractions subsumed within the respective ranges, as well as the recited endpoints.

The term ‘about’ as used herein when referring to a measurable value such as a parameter, an amount, a temporal duration, and the like, is meant to encompass variations of ±10% or less, preferably ±5% or less, more preferably ±1% or less and still more preferably ±0.1% or less of and from the specified value, insofar such variations are appropriate to perform the present disclosure. It is to be understood that the value to which the modifier ‘about’ refers is itself also specifically, and preferably disclosed.
The term ‘ASTM D3359’ as used herein refers to a test method for measuring adhesion by tape test. The test assesses the adhesion of film coatings on metallic substrates by applying and removing pressure-sensitive tape over cuts made in the film. ASTM D3359 comprises two distinct test methods- Method-A and Method-B.
In Method-A- an ‘X’ is cut through the film and a prescribed pressure-sensitive tape is applied over the cut and then removed. The adhesion is evaluated on a 0 to 5 scale (0A to 5A scale).
In Method-B- a perpendicular lattice pattern with either six or eleven cuts in each direction is made through the film and a prescribed pressure-sensitive tape is applied over the lattice and then removed. The adhesion is then evaluated by comparison with descriptions and illustrates. The adhesion is evaluated on a 0 to 5 scale (0B to 5B scale), wherein- 0B means flaking and detachment worse than classification; 1B means the coating has flaked along the edges of cuts in large ribbons and whole squares have detached. The area affected is 35 to 65% lattice; 2B means the coating has flaked along the edges and on parts of the squares. The area affected is 15 to 35% of the lattice; 3B means small flakes of the coating are detached along edges and at intersections of cuts. The area affected is 5 to 15%; 4B means small flakes of the coating are detached at intersections, less than 5% of the area is affected; and 5B means the edges of the cuts are completely smooth and none of the squares of the lattice is detached.

The term ‘Formability’ as used herein refers to ability of the coated substrate to undergo plastic deformation without being damaged and “Deep drawing” is a sheet metal formability where shape transformation occurs with retention of material retention.

The term ‘ISO 1520:2006’ as used herein refers to empirical test procedure for assessing the resistance of coating the composition to cracking and/or detachment from a substrate when subjected to gradual deformation by indentation under standard conditions.

The term ‘corrosion resistance’ or ‘salt resistance’ as used herein refers to ability of the coated substrate or the article comprising the composition, to prevent environmental deterioration by chemical or electro-chemical reaction.

The present disclosure relates to a simple and effective composition, particularly to a coating composition that provides for improved formability and improved corrosion resistance.

In some embodiments of the present disclosure, the composition comprises combination of- aminopolysiloxane sol, phosphorylated titania sol, sulfopolyester and additive.

In some embodiments of the present disclosure, the aminopolysiloxane sol is a combination of epoxy silane and aminoalkyl trialkoxy silane.

In some embodiments of the present disclosure, the epoxy silane is selected from a group comprising ethyl ethoxy tetra epoxy silane, butyl butoxy tetra epoxy silane and combinations thereof.

In some embodiments of the present disclosure, the aminoalkyl trialkoxy silane is selected from a group comprising 3-(N-ethyl aminoisobutyl) tributoxy silane, 3(-N-isopropyl aminoisobutyl)mono ethyl di-propyl silane and combinations thereof.

In some embodiments of the present disclosure, the epoxy silane is in an amount ranging from about 0.8 wt% to 5 wt%.

In some embodiments of the present disclosure, the epoxy silane is in an amount of about 0.8 wt%, about 1.0 wt%, about 1.2 wt%, about 1.4 wt%, about 1.6 wt%, about 1.8 wt%, about 2.0 wt%, about 2.2 wt%, about 2.4 wt% ,about 2.6 wt%, about 2.8 wt%, about 3.0 wt%, about 3.2 wt%, about 3.4 wt%, about 3.6 wt%, about 3.8 wt%, about 4.0 wt%, about 4.2 wt%, about 4.4 wt%, about 4.6 wt%, about 4.8 wt% or about 5.0 wt%.

In some embodiments of the present disclosure, the aminoalkyl trialkoxy silane is in an amount ranging from about 0.5 wt% to 2.0 wt%.

In some embodiments of the present disclosure, the aminoalkyl trialkoxy silane is in an amount of about 0.5 wt%, about 0.6 wt%, about 0.7 wt%, about 0.8 wt%, about 0.9 wt%, about 1.0 wt% about 1.1 wt%, about 1.2 wt%, about 1.3 wt%, about 1.5 wt%, about 1.6 wt%, about 1.7 wt%, about 1.8 wt%, about 1.9 wt% or about 2.0 wt%.

In some embodiments of the present disclosure, the phosphorylated titania sol is a combination of titanium alkoxide, chelating agent, phosphoric acid and solvent.

In some embodiments of the present disclosure, the titanium alkoxide is selected from a group comprising triethanolamine titanate, titanium isoporpoxide, tetra-n-butyl titanate and combinations thereof.

In some embodiments of the present disclosure, the chelating agent is selected from a group comprising lactic acid, 3-hydroxybutyric acid, 3-hydroxypentanoic acid and combinations thereof.

In some embodiments of the present disclosure, the chelating agent is selected from a combination comprising- combination of lactic acid and 3-hydroxybutric acid in a ratio of about 1:1; combination of lactic acid and 3-hydropentanoic acid in a ratio of about 1:1 and combination of 3-hydrobutyric acid and 3-hydroxypentanoic acid in a ratio of about 1:1.

In some embodiments of the present disclosure, the chelating agent is in an amount ranging from about 1 wt% to 2.5 wt%.

In some embodiments of the present disclosure, the chelating agent is in an amount of about 1 wt%, about 1.2 wt%, about 1.3 wt%, about 1.4 wt%, about 1.5 wt%, about 1.6 wt%, about 1.7 wt%, about 1.8 wt%, about 1.9 wt%, about 2.0 wt%, about 2.1 wt%, about 2.2 wt%, about 2.3 wt%, about 2.4 wt% or about 2.5 wt%.

In some embodiments of the present disclosure, the solvent includes but is not limited to demineralized water.

In some embodiments of the present disclosure, the solvent is in an amount ranging from about 63 wt% to 90 wt%.

In some embodiments of the present disclosure, the solvent is in an amount of about 63 wt%, about 65 wt%, about 70 wt%, about 75 wt%, about 80 wt%, about 85 wt% or about 90 wt%.

In some embodiments of the present disclosure, the phosphoric acid is in an amount ranging from about 1 wt% to 3 wt%.

In some embodiments of the present disclosure, the phosphoric acid is in an amount of about 1 wt%, about 1.1 wt%, about 1.2 wt%, about 1.3 wt%, about 1.4 wt%, about 1.5 wt%, about 1.6 wt%, about 1.7 wt%, about 1.8 wt%, about 1.9 wt%, about 2.0 wt%, about 2.1 wt%, about 2.2 wt%, about 2.3 wt%, about 2.4 wt%, about 2.5 wt%, about 2.6 wt%, about 2.7 wt%, about 2.8 wt%, about 2.9 wt% or about 3 wt%.
In some embodiments of the present disclosure, the sulfopolyester is in an amount ranging from about 2 wt% to 10 wt%.

In some embodiments of the present disclosure, the sulfopolyester is in an amount of about 2 wt%, about 2.2 wt%, about 2.4 wt%, about 2.6 wt%, about 2.8 wt%, about 3 wt%, about 3.2 wt%, about 3.4 wt%, about 3.6 wt%, about 3.8 wt%, about 4 wt%, about 4.2 wt%, about 4.4 wt%, about 4.6 wt%, about 4.8 wt%, about 5 wt%, about 5.2 wt%, about 5.4 wt%, about 5.6 wt%, about 5.8 wt%, about 6 wt%, about 6.2 wt%, about 6.4 wt%, about 6.6 wt%, about 6.8 wt% ,about 7.0 wt%, about 7.2 wt%, about 7.4 wt%, about 7.6 wt%, about 7.8 wt%, about 8.0 wt%, about 8.2 wt% ,about 8.4 wt%, about 8.6 wt%, about 8.8 wt%, about 9.0 wt%, 9.2 wt%, about 9.4 wt%, about 9.6 wt%, about 9.8 wt% or about 10 wt%.

In some embodiments of the present disclosure, the additive is selected from a group comprising lubricant, flexibilizer, surface tension reducer (surfactant), corrosion inhibitor and combinations thereof.

In some embodiments of the present disclosure, the lubricant includes but is not limited to polypropylene wax.

In some embodiments of the present disclosure, the lubricant is in an amount ranging from about 0.5 wt% to 3 wt%.

In some embodiments of the present disclosure, the lubricant is in an amount of about 0.5 wt%, about 0.6 wt%, about 0.7 wt%, about 0.8 wt%, 0.9 wt%, about 1.0 wt%, about 1.1 wt%, about 1.2 wt%, about 1.3 wt%, about 1.4 wt%, about 1.5 wt%, about 1.6 wt%, about 1.7 wt%, about 1.8 wt%, about 1.9 wt%, about 2.0 wt%, about 2.1 wt%, about 2.2 wt%, about 2.3 wt%, about 2.4 wt%, about 2.5 wt%, about 2.6 wt%, about 2.7 wt%, about 2.8 wt%, about 2.9 wt%, or about 3.0 wt%.

In some embodiments of the present disclosure, the polypropylene wax is processed polypropylene wax, wherein processing of the polypropylene wax is carried out by heating to a temperature ranging from about 150 ºC to 160 ºC followed by cooling to a temperature ranging from about 27 ºC to 30 ºC, wherein the cooling is carried out in a desiccator. Processing of the polypropylene wax minimizes the greasy nature of the wax and provides improved lubricity property.

In some embodiments of the present disclosure, the flexibilizer is selected from a group comprising hexylene glycol, propylene glycol, ethylene glycol and combinations thereof.

In some embodiments of the present disclosure, the flexibilizer is in an amount ranging from about 2 wt% to 4 wt%.

In some embodiments of the present disclosure, the flexibilizer is in an amount of about 2 wt%, about 2.1 wt%, about 2.2 wt%, about 2.3 wt%, about 2.4 wt%, about 2.5 wt%, about 2.6 wt%, about 2.7 wt%, about 2.8 wt%, about 2.9 wt%, about 3 wt %, about 3.1 wt%, about 3.2 wt%, about 3.3 wt%, about 3.4 wt%, about 3.5 wt%, about 3.6 wt%, about 3.7 wt%, about 3.8 wt%, about 3.9 wt% or about 4 wt%.

In some embodiments of the present disclosure, the surfactant includes but is not limited to non-foaming silicon.

In some embodiments of the present disclosure, the surfactant is in an amount ranging from about 0.1 wt% to 0.5 wt%.

In some embodiments of the present disclosure, the surfactant is in an amount of about 0.1 wt%, about 0.2 wt%, about 0.3 wt%, about 0.4 wt% or about 0.5 wt%.

In some embodiments of the present disclosure, the corrosion inhibitor includes but is not limited to magnesium sulfate.

In some embodiments of the present disclosure, the corrosion inhibitor is in an amount ranging from about 0.3 wt% to 2 wt%.

In some embodiments of the present disclosure, the corrosion inhibitor is in an amount of about 0.3 wt%, about 0.4 wt%, about 0.5 wt%, about 0.6 wt%, about 0.7 wt%, about 0.8 wt% about 0.9 wt%, about 1.0 wt%, about 1.1 wt%, about 1.2 wt%, about 1.3 wt%, about 1.4 wt%, about 1.5 wt%, about 1.6 wt%, about 1.7 wt%, about 1.8 wt%, about 1.9 wt% or about 2.0 wt%.

In some embodiments of the present disclosure, the composition comprises combination of aminopolysiloxane sol, phosphorylated titania sol, sulfopolyester, lubricant, flexibilizer, surfactant and corrosion inhibitor.

In some embodiments of the present disclosure, the composition provides improved forming and improved corrosion resistance to metallic substrates including but not limited to galvannealed substrate and galvanized substrate.

In some embodiments of the present disclosure, the aminopolysiloxane sol comprising combination of epoxy silane and aminoalkyl trialkoxy silane provides for improved corrosion resistance property. The improved corrosion resistance property by aminopolysiloxane sol is achieved due to effective crosslinking of aminoalkyl trialkoxy silane with epoxy silane. Additionally, the aminopolysiloxane sol provides for improved scrub resistance.

In some embodiments of the present disclosure, in the composition, the aminopolysiloxane sol (APS) and phosphorylated titania sol (PTS) is grafted with the sulfopolyester. Grafting of APS and PTS with sulfopolyester is illustrated in Figure 4.

In some embodiments of the present disclosure, sulfopolyester present in the composition provides for efficient film formation of the composition on a substrate and prevent deposition of the composition on the rollers while roll coating of the composition on a substrate. Further, the available active sites of the sulfopolyester leads to chemisorption onto the substrate.

The present disclosure further relates to method of preparing the composition described above.

In some embodiments of the present disclosure, the method of preparing the composition comprises- mixing aminopolysiloxane sol, phosphorylated titania sol, sulfopolyester and additive to obtain the composition.

In some embodiments of the present disclosure, the method of preparing the composition comprises mixing aminopolysiloxane sol where aminopolysiloxane is having 0.8 wt. % to 5 wt. % of oligomeric epoxy silane and 0.5 wt% to 2 wt, % of aminoalkyl trialkoxy silane, phosphorylated titania sol where phosphorylated titania sol is having 2 wt% to 5 wt. % of Triethanolamine titanate /Titanium isopropoxide/Tetra-n-butyl titanate, 63 wt% to 90 wt. % of DM water, 1wt % to 2.5 wt. % of Lactic acid/3 hydroxybutyric acid/3 hydroxy pentanoic acid, 1wt % to 3 wt. % of phosphoric acid and about 2 wt% to 10 wt % of sulfopolyester, wherein grafting of aminopolysiloxane sol (APS) and the phosphorylated titania sol (PTS) with sulfopolyester occurs. Grafting of APS and PTS with sulfopolyester is illustrated in Figure 4.
In some embodiments of the present disclosure, the method of preparing the composition comprises:
- preparing the aminopolysiloxane sol;
- preparing the phosphorylated titania sol;
- mixing the aminopolysiloxane sol and the phosphorylated titania sol to obtain mixture-A;
- mixing the sulfopolyester and the mixture-A to obtain mixture-B;
- mixing the additive comprising the corrosion inhibitor, the flexibilizer and the surface tension reducer (surfactant) and the mixture-B to obtain mixture-C; and
- mixing the additive comprising the lubricant and the mixture-C to obtain the composition.

In some embodiments of the present disclosure, preparing the aminopolysiloxane sol comprises mixing the epoxy silane and the amioalkyl trialkyoxy silane at a speed ranging from about 600 rpm to 800 rpm for a duration ranging from about 1 hour to 2 hours to obtain the aminopolysiloxane sol.

In some embodiments of the present disclosure, the preparing the aminopolysiloxane sol comprises mixing about 0.8 wt % to 5 wt% of epoxy silane and about 0.5 wt% to 2 wt% of aminoalkyl trialkoxy silane at a speed of about 600 rpm, about 620 rpm, about 640 rpm, about 660 rpm, about 680 rpm, about 700 rpm, about 720 rpm, about 740 rpm, about 760 rpm, about 780 rpm or about 800 rpm for a duration ranging from about 1 hour, about 1.1 hour, about 1.2 hour, about 1.3 hour, about 1.4 hour, about 1.5 hour, about 1.6 hour, about 1.7 hour, about 1.8 hour, about 1.9 or about 2 hours. The figure 2 illustrates scheme of preparation of the aminopolysiloxane sol.

In some embodiments of the present disclosure, preparing the phosphorylated titania sol comprises:
- mixing about 2 wt% to 5 wt. % of the titanium alkoxide and about 2 wt% to 5 wt. % of chelating agent, followed by heating;
- adding about 66 wt% to 93 wt. % of the diluted phosphoric acid wherein dilution of phosphoric acid is made by demineralized water which is in the range of about 63 wt% to 90 wt% and phosphoric acid in range of 1 wt% to 3 wt. % and mixing to obtain solution; and
- adding the demineralized water and holding the solution to obtain phosphorylated titania sol.
In some embodiments of the present disclosure, the mixture of titanium alkoxide and the chelating agent is subjected to heating at a temperature ranging from about 60 ºC to 70 ºC for a duration ranging from about 15 minutes to 20 minutes.
In some embodiments of the present disclosure, the mixture of titanium alkoxide and the chelating agent is subjected to heating to a temperature of about 60 ºC, about 61 ºC, about 62 ºC, about 63 ºC, about 64 ºC, about 65 ºC, about 66 ºC, about 67 ºC, about 68 ºC, about 69 ºC or about 70 ºC for a duration of about 15 minutes, about 16 minutes, about 17 minutes, about 18 minutes, about 19 minutes or about 20 minutes.

In some embodiments of the present disclosure, the chelating comprising the combination of lactic acid and 3-hydroxybutyric acid in a ratio of about 1:1, combination of lactic acid and 3-hydroxypentanoic acid in a ratio of about 1:1 or combination of 3-hydroxybutyric acid and 3-hydroxypentanoic acid in a ratio of about 1:1 upon mixing with the titanium alkoxide, suppresses active site of titanium alkoxide, which prevents the precipitation of the titanium alkoxide.

In some embodiments of the present disclosure, the phosphoric acid having concentration ranging from about 1 wt% to 3 wt % is added to the mixture of chelating agent and titanium alkoxide, followed by mixing. Further, demineralized water ranging from about 63 wt% to 90 wt% is added and subjected to mixing for a duration ranging from about 6 hours to 7 hours to obtain a white solution. Subsequently, white solution is subjected to holding time ranging from about 24 hours to 48 hours and holding temperature is ranging from about 15 ºC to 30 ºC to obtain transparent solution/clear solution of phosphorylated titania sol.

In some embodiments of the present disclosure, the demineralized water of about 63 wt%, about 65 wt%, about 70 wt%, about 75 wt%, about 80 wt%, about 85 wt% or about 90 wt% is added to the mixture of chelating agent and titanium alkoxide under mixing for a duration of about 6 hours, about 6.1 hours, about 6.2 hours, about 6.3 hours, about 6.4 hours, about 6.5 hours, about 6.6 hours, about 6.7 hours, about 6.8 hours, about 6.9 hours or about 7 hours. Subsequently, the white solution is subjected to holding time of about 24hours, about 26 hours, about 28 hours, about 30 hours, about 32 hours, about 34 hours, about 36 hours, about 38 hours, about 40 hours, about 42 hours, about 44 hours, about 46 hours or about 48 hours to obtain transparent solution/clear solution of phosphorylated titania sol.

In an embodiment of the present disclosure, figure 1 illustrates the schematics of the preparation of the phosphorylated titania sol.

In some embodiments of the present disclosure, the mixing of the aminopolysiloxane sol and the phosphorylated titania sol is carried out at a speed ranging from about 600 rpm to 800 rpm for a duration ranging from about 1 hour to 2 hours to obtain mixture-A.

In some embodiments of the present disclosure, the mixing of the aminopolysiloxane sol and the phosphorylated titania sol is carried out at a speed of about 600 rpm, about 620 rpm, about 640 rpm, about 660rpm, about 680 rpm, about 700 rpm, about 720 rpm, about 740 rpm, about 760 rpm, about 780 rpm or about 800 rpm for a duration of about 1 hour, about 1.1 hours, about 1.2 hours, about 1.3 hours, about 1.4 hours, about 1.5 hours, about 1.6 hours, about 1.7 hours, about 1.8 hours, about 1.9 hours or about 2 hours to obtain mixture-A.

In an embodiment of the present disclosure, figure 3 illustrates the schematics of mixing of the aminopolysiloxane sol and the phosphorylated titania sol and formation of mixture-A.

In some embodiments of the present disclosure, the mixing of the mixture-A and the sulfopolyester is carried out in low shear mixer at a speed ranging from about 400 rpm to 600 rpm for a duration ranging from about 15 minutes to 20 minutes, in presence of acid catalyst including but not limited to acetic acid and phosphoric acid to obtain mixture-B, wherein the sulfopolyester is in an amount ranging from 2 wt% to 10 wt%.

In some embodiments of the present disclosure, the mixing of the mixture-A and the sulfopolyester is carried out in low shear mixer at a speed of about 400 rpm, about 420 rpm, about 440 rpm, about 460 rpm, about 480 rpm, about 500 rpm, about 520 rpm, about 540 rpm, about 560 rpm, about 580 rpm or about 600 rpm for a duration of about 15 minutes, about 16 minutes, about 17 minutes, about 18 minutes, about 19 minutes or about 20 minutes, in presence of acid catalyst including but not limited to phosphoric acid to obtain mixture-B.

In an embodiment of the present disclosure, figure 4 illustrates the grafting of the mixture-A comprising aminopolysiloxane sol and phosphorylated titania sol with sulfpolyester to obtain mixture-B.

In some embodiments of the present disclosure, the additive comprising the corrosion inhibitor, the flexibilizer and the surfactant are mixed with the mixture-B at a speed ranging from about 600 rpm to 800 rpm to obtain mixture-C.

In some embodiments of the present disclosure, the corrosion inhibitor in an amount ranging from about 0.3 wt% to 2 wt%, the flexibilizer in an amount ranging from about 2 wt% to 4 wt% and the surfactant in an amount ranging from about 0.1 wt% to 0.5 wt% are mixed with the mixture B at a speed ranging from about 600 rpm to 800 rpm to obtain mixture-C.

In some embodiments of the present disclosure, the additive and the mixture-B are mixed at a speed of about 600 rpm, about 620 rpm, about 640 rpm, about 660 rpm, about 680 rpm, about 700 rpm, about 720 rpm, about 740 rpm, about 760 rpm, about 780 rpm or about 800 rpm to obtain mixture-C.

In some embodiments of the present disclosure, the lubricant including but not limited to polypropylene wax is mixed with mixture-C to obtain the composition described above, wherein the polypropylene wax is processed polypropylene wax/pretreated polypropylene wax.

In some embodiments of the present disclosure processing/pretreatment of the lubricant including but not limited to polypropylene wax is carried out by heating the lubricant at a temperature ranging from about 150 ºC to 160 ºC, followed by cooling to a temperature ranging from 27 ºC to 30 ºC, wherein the cooling is carried out in a desiccator. The processing/pretreatment of the lubricant minimizes the greasy nature of the lubricant and provides for improved lubricity property.

In some embodiments of the present disclosure, about 0.5 wt% to 3 wt% of the processed/pretreated lubricant including but not limited to polypropylene is added to mixture-C and mixing is carried out in high shear mixer at a speed ranging from about 1200 rpm to 1500 rpm for a duration ranging from about 1 hour to 2 hours to obtain the composition.

In some embodiments of the present invention, the processed/pretreated lubricant including but not limited to polypropylene and mixture-C is mixed in high shear mixer at a speed of about 1200 rpm, about 1220 rpm, about 1240 rpm, about 1260 rpm, about 1280 rpm, about 1300 rpm, about 1320 rpm, about 1340 rpm, about 1360 rpm, about 1380 rpm, about 1400 rpm, about 1420 rpm ,about 1440 rpm, about 1460 rpm, about 1480 rpm or about 1500 rpm for a duration of about 1 hour, about 1.1 hour, about 1.2 hour, about 1.3 hour, about 1.4 hour, about 1.5 hour, about 1.6 hour, about 1.7 hour, about 1.8 hour, about 1.9 hour or about 2.0 hour to obtain the composition.

The present disclosure further relates to an article comprising the composition described above.

In some embodiments of the present disclosure, the composition is in a form of film on surface of the article, wherein the thickness of the composition is ranging from about 0.5nm to 3000 nm, including all values or ranges derivable therefrom.

In some embodiments of the present disclosure, the composition has highest level of adhesion with the article, having ASTM class ranging from about 4B to 5B according to American standard test method (ASTM).

In some embodiments of the present disclosure, the composition has highest level of adhesion with the article, having ASTM class of about 4B according to American standard test method (ASTM).
In some embodiments of the present disclosure, the composition has highest level of adhesion with the article, having ASTM class of about 5B according to American standard test method (ASTM).

In some embodiments of the present disclosure, the article has corrosion resistance ranging from about 200 hours to 250 hours according to salt spray test, ASTM B117.

The present disclosure further relates to a method of producing the article described above.

In some embodiments of the present disclosure, the method of producing the article comprises- coating a substrate with the composition as claimed in claim 1, followed by curing to obtain the article.

In some embodiments of the present disclosure, coating of the composition on the substrate is carried out by technique including but not limited to spray coating, dip coating, roll coating and wiping method.

In some embodiments of the present disclosure, the curing upon coating of the composition is carried out at a temperature ranging from about 90 ºC to 100 ºC for a duration ranging from about 2 seconds to 3 seconds.

In some embodiments of the present disclosure, the curing upon coating of the composition is carried out at a temperature of about 90 ºC, about 91 ºC, about 92 ºC, about 93 ºC, about 94 ºC, about 95 ºC, about 96 ºC, about 97 ºC, about 98 ºC, about 99 ºC or about 100 ºC for a duration of about 2 seconds or about 3 seconds.

The present disclosure further relates to a method of coating a substrate with the composition described above for improving corrosion resistance of the substrate.

In some embodiments of the present disclosure, the method of coating the substrate with the composition described above for improving corrosion resistance of the substrate, wherein the coating is carried out by a technique including but not limited to spray coating, dip coating, roll coating and wiping method.

In some embodiments of the present disclosure, upon coating the composition, the substrate is subjected to curing at a temperature ranging from about 90 ºC to 100 ºC for a duration ranging from about 2 seconds to 3 seconds.

In some embodiments of the present disclosure, upon coating the composition, the substrate is subjected curing at a temperature of about 90 ºC, about 91 ºC, about 92 ºC, about 93 ºC, about 94 ºC, about 95 ºC, about 96 ºC, about 97 ºC, about 98 ºC, about 99 ºC or about 100 ºC for a duration of about 2 seconds or about 3 seconds.

In some embodiments of the present disclosure, the coated substrate has corrosion resistance ranging from about 200 hours to 250 hours according to salt spray test, ASTM B 117.

In some embodiments of the present disclosure, the coated substrate comprises the composition in form of a film, having highest level of adhesion ranging from about 4B to 5B, according to American standard test method (ASTM).

In some embodiments of the present disclosure, the coated substrate having the composition in the form of film has highest level of adhesion of about 4B according to American standard test method (ASTM).

In some embodiments of the present disclosure, the coated substrate having the composition in the form of film has highest level of adhesion of about 5B according to American standard test method (ASTM).

In some embodiments of the present disclosure, the substrate includes but not limited to bare metal, bare alloy, galvannealed metals, galvannealed alloy, galvanized metal and galvanized alloy.

It is to be understood that the foregoing description is illustrative not a limitation. While considerable emphasis has been placed herein on particular features of this disclosure, it will be appreciated that various modifications can be made, and that many changes can be made in the preferred embodiments without departing from the principles of the disclosure. Those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the embodiments as described herein. Similarly, additional embodiments and features of the present disclosure will be apparent to one of ordinary skill in art based upon description provided herein.

Descriptions of well-known/conventional methods/steps and techniques are omitted so as to not unnecessarily obscure the embodiments herein. Further, the disclosure herein provides for examples illustrating the above-described embodiments, and in order to illustrate the embodiments of the present disclosure, certain aspects have been employed. The examples used herein for such illustration are intended merely to facilitate an understanding of ways in which the embodiments may be practiced and to further enable those of skill in the art to practice the embodiments. Accordingly, following examples should not be construed as limiting the scope of the embodiments herein.

EXAMPLE

Example 1: Preparation of the composition
a) Preparation of Aminopolysiloxane sol
About 3 wt% of 3–(N-ethyl aminoisobutyl) tributoxy silane and about 1.25 wt% of ethyl ethoxy epoxy silane oligomer was stirred together for about 2 hours at about 800 rpm to prevent the sedimentation and get the transparent solution of aminopolysiloxane sol. Figure 2 provides schematics of the formation of aminopolysiloxane sol.

b) Preparation of phosphorylated titania sol:
About 5 wt% of Triethanolamine titanate and about 2 wt% of combination of lactic acid and 3-hydroxybutyric acid in a ratio of 1:1 were mixed and heated to a temperature ranging from about 70ºC constantly in reactor while purging nitrogen for about 15 minutes, followed by adding about 2 wt% of diluted phosphoric acid. Further, about 74.55 wt% of demineralized water was added and stirred for about 6 hours. The obtained solution is subjected to holding time of about 48 hours without stirring to obtain transparent solution of phosphorylated titania sol from white solution. Figure 1 provides schematics of the formation of phosphorylated titania sol.

c) Preparation of mixture-A (combination of aminpolysiloxane sol and phosphorylated titania sol)
About 4.25 wt% of aminopolysiloxane sol and about 83.55 wt % of phosphorylated titania sol was stirred in a reaction vessel for about 1 hour at a speed ranging from about 600 rpm to 800 rpm using mechanical stirrer to obtain mixture-A comprising combination of aminopolysiloxane and phosphorylated titania sol. Figure 3 provides schematics of the formation of mixture-A.

d) Preparation of mixture-B (combination of mixture-A and sulfopolyester)
About 87.80 wt% of mixture-A and about 7 wt% of sulfopolyester were mixed and stirred for about 15 minutes in a reaction vessel at low shear mixing in presence of phosphoric acid to obtain mixture-B (combination of mixture-A and sulfopolyester), wherein aminpolysiloxane sol and phosphorylated titania sol of mixture-A are grafted with sulfopolyester. Figure 4 illustrates grafting of the aminopolysiloxane sol and the phosphorylated titania sol with sulfopolyester.

Additive comprising- about 1 wt% of magnesium sulfate, about 2 wt% of hexylene glycol and about 0.2 wt% of non-foaming silicon are mixed with the mixture-B and stirred in a reaction vessel for about 2 hours at 600 rpm to 800 rpm using mechanical stirrer to obtain mixture-C.

Pre-treatment/processing of Polypropylene wax was carried out by heating up to about 150 ºC and then cooling it down in a desiccator. About 2 wt% of processed polypropylene wax was added to the mixture-C and stirred up to about 2 hours under high shear mixing to obtain the composition.

Example 2: Application of the Composition to a substrate
The composition prepared under Example 1 was applied by either roll coating or wiping method on to a substrate. The coated substrate was subjected to curing at about 90 ºC peak metal temperature for about 2 seconds to obtain a dense film of the composition on the substrate. The film (of the composition) on the substrate provides for an adherent film, exhibiting excellent forming and improved resistance to corrosion.

The composition coated substrate was subjected to- i. salt spray test (ASTM B 117); ii. Cross hatch adhesion test (ASTM D 3359-09); and iii. Deep drawing cup test (Formability: ISO 1520-2006).

i. Salt spray test:
The coated substrate was cut into 8/4 inch and edges were covered. The cut coated substrate was placed in fog chamber having about 5 wt% of NaCl. No rusting was observed/occurred on the coated substrate even after about 200 hours, indicating that the coating of the composition on the substrate provides for improved corrosion resistance.

ii. Cross hatch adhesion test:
Cross-hatch adhesion test kit was employed to perform the test. The coated substrate was cut into 6/4 inch, followed by brushing diagonally about five times in each direction. A special tape for testing adhesion was applied on the substrate and removed quickly by pulling the tape back of the substrate and the substrate was visually compared to ASTM standard D 3359-09. It was observed that the coated substrate exhibited 5B adhesion parameter. Thus, it was concluded that the composition prepared under Example 1 showed very good adherence of coating over the substrate.

iii. Deep drawing cup test
The coated substrate was cut into 100 mm of diameter and pressed by mechanical punch force using servo-hydraulic forming machine. Figure 5 demonstrates that the coated substrate with oil and without oil show lower punch force at each blank holding force as compared to the oiled and non-oiled uncoated substrates (galvannealed substrate). It was observed that coated substrate (galvannealed substrate coated by the composition) requires very low punch force to be drawn at each blank holding force, thus exhibiting excellent drawability when compared to uncoated samples or oiled samples.
Results:
Fracture point of non-oiled uncoated substrate- 15 KN
Fracture point of oil uncoated substrate- 25 KN
Fracture point of non-oiled coated substrate- 45 KN
Fracture point of oiled coated substrate- 65 KN

Observation:
- Improvement of fracture point in non-oil coated substrate when compared to non-oiled uncoated substrate was 30 KN.
- Improvement of fracture point in non-oiled coated substrate when compared to oiled uncoated substrate was 20 KN.
- Improvement of fracture point in oiled coated substrate when compared to oiled uncoated substrate was 40 KN.
- Improvement of fracture point in oiled coated substrate when compared to non-oiled uncoated GA was 50 KN.

Example 3: Preparation of the composition
a) Preparation of Aminopolysiloxane sol
About 5 wt% of 3–(N-ethyl aminoisobutyl) tributoxy silane and about 2 wt% of ethyl ethoxy epoxy silane oligomer was stirred together for about 2 hours at about 800 rpm to prevent the sedimentation and get the transparent solution of aminopolysiloxane sol. Figure 2 provides schematics of the formation of aminopolysiloxane sol.

b) Preparation of phosphorylated titania sol:
About 3 wt% of Triethanolamine titanate and about 2 wt% of combination of lactic acid and 3-hydropentanoic acid in a ratio of 1:1 were mixed and heated to a temperature ranging from about 70ºC constantly in reactor while purging nitrogen for about 15 minutes, followed by adding about 2 wt% of diluted phosphoric acid. Further, about 75.8 wt% of demineralized water was added and stirred for about 6hours. The obtained solution is subjected to holding time of about 48 hours without stirring to obtain transparent solution of phosphorylated titania sol from white solution. Figure 1 provides schematics of the formation of phosphorylated titania sol.

c) Preparation of mixture-A (combination of aminpolysiloxane sol and phosphorylated titania sol)
About 7 wt% of aminopolysiloxane sol and about 82.8 wt % of phosphorylated titania sol was stirred in a reaction vessel for about 1 hour at a speed ranging from about 600 rpm to 800 rpm using mechanical stirrer to obtain mixture-A comprising combination of aminopolysiloxane and phosphorylated titania sol. Figure 3 provides schematics of the formation of mixture-A.
d) Preparation of mixture-B (combination of mixture-A and sulfopolyester)
About 89.8 wt% of mixture-A and about 7 wt% of sulfopolyester were mixed and stirred for about 15 minutes in a reaction vessel at low shear mixing in presence of phosphoric acid to obtain mixture-B (combination of mixture-A and sulfopolyester), wherein aminpolysiloxane sol and phosphorylated titania sol of mixture-A are grafted with sulfopolyester. Figure 4 illustrates grafting of the aminopolysiloxane sol and the phosphorylated titania sol with sulfopolyester.

Additive comprising- about 1 wt% of magnesium sulfate, about 2 wt% of hexylene glycol and about 0.2 wt% of non-foaming silicon are mixed with mixture-B and stirred in a reaction vessel for about 2 hours at 600 rpm to 800 rpm using mechanical stirrer to obtain mixture-C.

Pre-treatment/processing of Polypropylene wax was carried out by heating up to about 150 ºC and then cooling it down in a desiccator. About 2 wt% of processed polypropylene wax was added to the mixture-C and stirred up to about 2 hours under high shear mixing to obtain the composition.

Example 4: Application of the Composition to a substrate
The composition prepared under Example 2 was applied by either roll coating or wiping method on to a substrate. The coated substrate was subjected to curing at about 100 ºC peak metal temperature for about 2 seconds to obtain a dense film of the composition on the substrate. The film (of the composition) on the substrate provides for an adherent film, exhibiting excellent forming and improved resistance to corrosion.

The composition coated substrate was subjected to- i. salt spray test (ASTM B 117); ii. Cross hatch adhesion test (ASTM D 3359-09); and iii. Deep drawing cup test (Formability: ISO 1520-2006).

iv. Salt spray test:
The coated substrate was cut into 8/4 inch and edges were covered. The cut coated substrate was placed in fog chamber having about 5 wt% of NaCl. No rusting was observed/occurred on the coated substrate even after about 200 hours, indicating that the coating of the composition on the substrate provides for improved corrosion resistance.
v. Cross hatch adhesion test:
Cross-hatch adhesion test kit was employed to perform the test. The coated substrate was cut into 6/4 inch, followed by brushing diagonally about five times in each direction. A special tape for testing adhesion was applied on the substrate and removed quickly by pulling the tape back of the substrate and the substrate was visually compared to ASTM standard D 3359-09. It was observed that the coated substrate exhibited 5B adhesion parameter. Thus, it was concluded that the composition prepared under Example 1 showed very good adherence of coating over the substrate.

vi. Deep drawing cup test
The coated substrate was cut into about 100 mm of diameter and pressed by mechanical punch force using servo-hydraulic forming machine. Figure 6 demonstrates that the coated substrate with oil and without oil show lower punch force at each blank holding force as compared to the oiled and non-oiled uncoated substrates (Galvanized substrate). It was observed that coated substrate (Galvanized substrate coated by the composition) requires very low punch force to be drawn at each blank holding force, thus exhibiting excellent drawability when compared to uncoated samples or oiled samples.
Results:
Fracture point of non-oiled uncoated substrate- 35 KN
Fracture point of oil uncoated substrate- 40 KN
Fracture point of non-oiled coated substrate- 90 KN
Fracture point of oiled coated substrate- 90 KN

Observation:
- Improvement of fracture point in non-oil coated substrate when compared to non-oiled uncoated substrate was 55 KN.
- Improvement of fracture point in non-oiled coated substrate when compared to oiled uncoated substrate was 50 KN.
- Improvement of fracture point in oiled coated substrate when compared to oiled uncoated substrate was 50 KN.
- Improvement of fracture point in oiled coated substrate when compared to non-oiled uncoated GA was 55 KN.

Documents

Application Documents

# Name Date
1 202131014272-STATEMENT OF UNDERTAKING (FORM 3) [30-03-2021(online)].pdf 2021-03-30
2 202131014272-REQUEST FOR EXAMINATION (FORM-18) [30-03-2021(online)].pdf 2021-03-30
3 202131014272-POWER OF AUTHORITY [30-03-2021(online)].pdf 2021-03-30
4 202131014272-FORM-8 [30-03-2021(online)].pdf 2021-03-30
5 202131014272-FORM 18 [30-03-2021(online)].pdf 2021-03-30
6 202131014272-FORM 1 [30-03-2021(online)].pdf 2021-03-30
7 202131014272-DRAWINGS [30-03-2021(online)].pdf 2021-03-30
8 202131014272-DECLARATION OF INVENTORSHIP (FORM 5) [30-03-2021(online)].pdf 2021-03-30
9 202131014272-COMPLETE SPECIFICATION [30-03-2021(online)].pdf 2021-03-30
10 202131014272-FORM-26 [22-07-2021(online)].pdf 2021-07-22
11 202131014272-Proof of Right [29-09-2021(online)].pdf 2021-09-29
12 202131014272-FER.pdf 2022-12-01
13 202131014272-OTHERS [23-05-2023(online)].pdf 2023-05-23
14 202131014272-FER_SER_REPLY [23-05-2023(online)].pdf 2023-05-23
15 202131014272-CLAIMS [23-05-2023(online)].pdf 2023-05-23
16 202131014272-US(14)-HearingNotice-(HearingDate-25-09-2023).pdf 2023-08-28
17 202131014272-Correspondence to notify the Controller [22-09-2023(online)].pdf 2023-09-22
18 202131014272-Written submissions and relevant documents [09-10-2023(online)].pdf 2023-10-09
19 202131014272-PatentCertificate10-10-2023.pdf 2023-10-10
20 202131014272-IntimationOfGrant10-10-2023.pdf 2023-10-10

Search Strategy

1 202131014272_searchstrategyE_28-11-2022.pdf

ERegister / Renewals

3rd: 04 Jan 2024

From 30/03/2023 - To 30/03/2024

4th: 04 Jan 2024

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5th: 12 Feb 2025

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