Title of Invention

COMPOSITION OF OIL FOR THIN GAUGE STEEL ROLLING

Abstract The invention relates to a composition of oil for thin gauge steel rolling comprising of natural fats / oils, synthetic esters, high viscosity mineral oil and other performance additives such as extreme pressure, antiwear, emulsifiers, antioxidants, antifoam etc. The composition forms oil-in-water milky meta-stable emulsion with water. The said composition is suitable for thin gauge steel rolling. It has excellent lubricity and burn off characteristics. It also has very good hard water compatibility.
Full Text FORM 2
THE PATENTS ACT, 1970
(39 of 1970)
&
THE PATENTS RULES, 2003
COMPLETE SPECIFICATION
(See Section 10; rule 13)
"COMPOSITION OF OIL FOR THIN GAUGE STEEL ROLLING"
INDIAN OIL CORPORATION LIMITED of the address: G-9, Ali Yavar Jung Marg, Bandra (East), Mumbai-400051, India.
The following specification particularly describes and ascertains the nature of this invention and the manner in which it has to be performed:

Field of Invention
The present invention relates to a steel cold rolling oil composition comprising of natural fats / oils, synthetic ester, fatty acid, antioxidant, extreme pressure, antiwear, antifoam, emulsifiers and high viscosity index mineral oil. The composition described in present invention relates to the composition of an oil, which forms metastable milky emulsion with water and is quite useful for steel cold rolling and particularly thin gauge rolling in 4-Hi and 6-Hi rolling mills.
Prior Art
Rolling oil prepared by adding emulsifier and dispersing agents to the mixtures obtained by adding oiliness improvers, extreme pressure and antiwear additives, antioxidants, antifoam, animal fat or vegetable fat such as tallow, palm, coconut, various synthetic ester and base mineral oil or the mixture of oils thereof. In rolling, a liquid obtained by emulsifying and dispersing rolling oil in a suitable concentration (coolant liquid) by means of mechanical agitation in a tank is sprayed on work rolls for cooling and lubrication at roll bite. The coolant liquid is circulated continuously to remove the iron fines and debris generated during rolling operation.
Formulation of the rolling oil depends on the customer requirement and is mill specific. The plant may be slow, medium or high speed. Depending upon the mill speed, load, quality of water, stirring rate of the coolant, the formulation of the rolling oil also changed to a great extent. The formulation variation observed in terms of saponification value/fat and synthetic ester content, extreme pressure additives, quantity and quality of emulsifier, antifoam etc. The lubrication requirement also changes from mill to mill.
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The lubricity and surface cleanliness property seems to be the most important characteristics of a cold rolling oil formulation. The lubrication property of cold rolling oil can be assesses by measurement of the load carrying ability of the oil and low friction coefficient. The lubricity property of a cold rolling oil formulation is dependent probably on two parameters e.g. the lubricating additives selected and the metastability of the emulsion. The lubrication property is also dependent on the plate out characteristics of the cold rolling oil. The plate out characteristics basically an adhesion_property of the cold rolling oil to the metal surface. The metastability and plate out characteristics is highly correlated and a linear correlation exists between them. But they are measured in different scale. A less amount of plate-out / metastability brings about insufficient lubrication. Although plate out /metastability are the desirable properties, the extreme value of these properties are also not desired as these leads to the unstable emulsion as well as high oil consumption during rolling. So an optimum quantity of plate out / metastability is required for a good cold rolling oil. In this patent we have measured the metastability as it is better to define and also a measurement of hard water tolerance of rolling oil. The cold rolling oil is generally used as an emulsion where a certain quantity of cold rolling oil is added to the water. Now the quality and hardness of the water changes from customer to customer. Thus the stability and hard water tolerance of the cold rolling oil emulsion is also another criteria. The emulsion (coolant) must not be unstable in hard water. The cold rolling oil emulsion may be a tight emulsion without much oil separation. This is not a desirable characteristic for lubrication. Actually a cold rolling oil emulsion required a "metastable" emulsion (loose emulsion with to some extent oil separation characteristics). The metastable emulsion separates oil to some extent at the roll bite and the separated oil takes care of the lubrication property and just after the rolling operation the oil and water mix together to form the emulsion again which is possible as the separated oil also contains emulsifiers. Thus the
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measurement of emulsion stability for hard water tolerance and metastability is an important criterion for rolling oil emulsion.
The surface cleanliness of the rolled sheet before and after rolling is another important criterion for good cold rolling oil. In actual customer site, the surface cleanliness property and iron pick up mark of cold rolling oil is assessed by visual observation and tape test. The burn off characteristics is the laboratory measured property which correlates with the good surface cleanliness property of the rolled sheet. The burn off characteristics can be assessed by the Thermo gravimetric analysis (TGA). Trace to very low residue is considered to be cold rolling oil with excellent burn off characteristics. In addition to the lubrication and load carrying capacity, excellent burn off characteristics of cold rolling oil is considered to be one of the basic requirements. This signifies good surface cleanliness properties after annealing of the cold rolling process.
U.S Pat No 4693839 describes a rolling oil composition with specific type of water soluble cationic or amphoteric polymer compounds. U.S Pat No 4746448 discloses cold rolling oil for steels which contain monoester, dimmer acid, polyester, a polymer compound having a nitrogen atom. Pat. No WO 2005017078 describes a rolling oil formulation with polyol ester with hydroxyl value between 20-50 mg KOH/g and level of polyunsaturation of between 0.01 to 8 % by weight. Pat No. WO 2004078893 present a invention where a polar liquid ( fatty alcohol fatty ester) with boiling point between 25 °C and 500 °C. Patent No. JP2003301191 discloses a cold rolling composition comprises palm oil and/or beef tallow, cationic polymeric compound and a nonionic surfactant and/or a high molecular-weight polymer. Patent No. JP 2002167595 discloses a cold rolling oil formulation containing base oil, modified fat, a synthetic saturated fatty acid ester and a
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combination of nonionic emulsifiers. Patent no. CN 1653166 describes a cold rolling oil formulation comprising a base oil containing 0.5 to 30 % wt diester and 0.01- 5 % wt phosphorous compound. The author claims excellent anti- heat-scratching and gloss irregularity of rolled plate. Pat. No. JP2000017284 describes a rolling mill lubricant which describes phenolic, aminic antioxidant and the rust preventive. Pat No JP2000219890 describes a cold rolling oil composition containing base stock, natural fat and synthetic base oil, phospholipids, phosphite. Pat No JP 11222598 describes the cold rolling oil composition which has a high rolling lubricity and generates little scum. The composition contains one base oil chosen from animal or vegetable fats, alkyl phosphate and emulsifiers. JP 11061167 discloses cold rolling oil formulation base oil, cationic emulsifier, nonionic high molecular compound and a higher aliphatic alcohol. Pat No JP 9208984 discloses a cold rolling oil formulation comprises a mineral oil with 5

JP 62011799 discloses a cold rolling oil formulation containing fats, fatty acid ester, mineral oil and a high polymer dispersant. Patent KR9004507 describes cold rolling oil composition for steel sheet comprises cold rolling oil and cationic high molecular wt compound and 0.1%-5% of nonionic surfactant of HLB value 12 or more, as an emulsifying and dispersing agent. The invention JP60023490 discloses a lubricating oil composition for cold rolling obtained by adding a dispersant composed of phytic acid as an essential component to the main lubrication component and capable of dispersing the scum produced by the rolling process. The Patent No. GB982363 a cold rolling oil formulation containing mineral lubricating oil, emulsifier and 20-30% of lard oil. In the invention of cold rolling of steel ( Pat No US 5122288) the formulation containing two nonionic emulsifiers (one of them is high molecular weight) as emulsifying and dispersing agent. This invention also claimed the adverse effect of iron power can be avoided by the addition of acetylene glycol.
Whereas numerous cold rolling oil lubricants based on different additive system have been developed, there is a continuing need for new products. This is particularly so where the new products present economic advantages and/or performance advantages. Performance advantages can include greater latitude in the ability to effectively formulate the lubricant. It can also include improvement in one or more of the properties of the lubricant. It is particularly effective if these improvements are achieved without adversely affecting the other essential properties of the lubricant.
Several disadvantages are associated and recognized with the known compositions based on the above patents. The formulations are based on either the advantage of emulsifier systems or on the advantages of one or few additives separately. One
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such disadvantage is that the formulations are based on part of the total additives of cold rolling oil formulation. Yet another disadvantage is that the formulations do not possess superior lubrication properties on the overall additive system. Further burn off characteristics of the cold rolling oil composition also not covered on the overall composition based on emulsifiers and additive system. Still further, the composition does not cover both the lubrication as well as surface cleanliness property on the overall formulations. Still further the formulations do not describe property the entire practical range of the diluted version of the cold rolling oil lubricant formulation containing the above advantage of superior lubrication as well as surface cleanliness property. Further none of the diluted lubricant formulation describes the metastability characteristics of the coolant (emulsion). Further disadvantages of the formulations are that the none of the formulations are available which shows good lubrication property, burn off characteristics and metastability. Another disadvantage in the above patents is the hard water compatibility of the diluted cold rolling oil formulation.
Background of the Invention
This invention relates to the development of a composition of oil suitable for thin gauge steel rolling.
In this era of rapidly increasing lubricant costs and the ever present possibility of critical shortages, it is mandatory that users obtain maximum utilization of each lubricant. Cold rolling oil for steel is a prime example which is being used in significant volumes by steel mills. Its performance is critical to the proper rolling of steel, maintaining good shape of steel sheet and high strip surface cleanliness. The oil residue left on the steel sheet after rolling is converted into black powdery material during annealing treatment and it poses difficulties in next operations like
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coating, painting, etc. Now-a-days steel industry demands rolling oils that leave no or minimal residue after annealing treatment to produce mirror finish steel strip and boost the brand image of their products.
In the rolling process, the thickness of the strip is reduced by the action of stretching from side and loading in normal direction. The coefficient of friction existing in the zone of contact between the roll and strip has a pronounced effect on the roll separating force required to achieve a given reduction in thickness. The theoretical relationship between these forces and the coefficient of friction is complex and based on many assumptions. However, it is reported that the lower coefficient of friction, the lower the rolling load and the greater the reduction that can be taken. There is also a minimum level below which friction must not be reduced or the grip required to keep the strip moving through the roll bite will be lost, producing skidding. The rolling oil performs the functions of reducing the coefficient of friction at roll bite and cooling of work roll / strip to avoid heat marks.
Formulations of rolling oils are quite complex. The performance or nonperformance of rolling oil becomes quickly evident during its use in rolling mills. The performance of water-soluble rolling oils is dependent on the water quality and handling practices adopted at the mill site also. A defect in the rolling oil formulation will unveil in a couple of days if not earlier and will require corrective action. The factors affecting the performance of rolling oils are multi-faceted and require special attentions of the formulator as well as user. Performance of the same oil may vary significantly from one use to other depending upon the application, metallurgy and maintenance practices.
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Keeping in view of all the above properties of rolling oil composition, a developmental program was initiated at authors' laboratory. A large number of chemical additives were used in the development of rolling oil composition and described in the present invention. The present invention is a synergistic combination of a set of ingredients to achieve the desired out put. Whereas, all prior art compositions were based on the concentrations of one/ two ingredients of the total composition and their benefits. It differentiate the present invention with prior art.
Summary of the Invention
The composition of oil suitable for thin gauge steel sheet rolling disclosed in the present invention is an optimized combination of natural fats / oils, synthetic esters, high viscosity mineral oil and other performance additives such as extreme pressure, antiwear, emulsifiers, antioxidants, antifoam etc.
The oil composition of the present invention forms metastable milky oil-in-water emulsion when mixed with water using proper agitation. The emulsion so formed provides adequate lubricity and cooling during rolling of thin gauge steel sheets. This emulsion also depicts very good hard water compatibility, required for longer useful life The emulsion also exhibited superior burn off characteristics as no coolant patches were observed after annealing treatment of rolled steel coils.
Detailed Description
In cold rolling of steel sheets, a fluid dispersion is prepared by emulsifying and dispersing a cold rolling oil in hot water ( 50-60 °C ) at a concentration of 0.5 % -10% by stirring and supplying the lubricating oil to the rolling rolls and steel sheets.
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The cold rolling oil composition is prepared by incorporating extreme pressure and antiwear additives, antioxidant, polar oiliness improver, friction reducing and lubricity agent, antifoam, if required, emulsifier in basic ingredient animal fat, or vegetable fat or synthetic ester and/ or base stock, and/or mixture of base oils, if required.
According to this invention there is provided a cold rolling oil composition for use as a lubricant with lubrication, burn off characteristics and a cold rolling oil emulsion with additional metastability and hard water compatibility in cold rolling of metals especially steel comprising 10 to 90 % by weight of natural fats , oils . 5 to 30% by weight of synthetic esters, 0 to 20 % by weight of fatty acid or mixture of fatty acids , 0.01 to 5 % by weight of antioxidant or mixtures of antioxidants, 0.5 to 15 % by weigh of S or P or zinc based extreme pressure and antiwear additives or mixtures thereof, nil to 1 % by weight of antifoam agents, 0.5 to 10% by weight of minimum one emulsifier or surface active agent and mineral base oil may present as nil to 30% by weight.
The natural fat used in the present invention is based on the vegetable and /or animal based and mixture thereof and selected from fatty acid ester of C-8 to C-22 fatty acid, preferably C-12,C-14,C-T6,C18, C-22,its mixture and /or its isomers. The saponification value of the natural fats/oils used in the present invention is 150 to 300_mg KOH/g. The Kinematic viscosity of the oil varies between 30 cSt to 250 cSt at 40 °C and flash point typically higher than 160 °C. Examples of vegetable fats are palm oil, coconut oil, rape seed oil, Soybean oil, Sulphurised oil/ fat, Sunflower oil, groundnut oil, linseed oil, jojoba oil etc., and the like. Animal fat is generally Lard oil, tallow etc.
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The synthetic ester used as an additive in the present invention based on fatty acid ester of C12 to CI8, its isomers and mixtures including complex and self emulsifying esters.
The Kinematic viscosity of the synthetic ester varies between 5 cSt to 60 cSt, preferably 30 to 50 cSt at 40 °C having flash point more than 160 °C.
Synthetic Esters used in the present invention:-

S.No. Synthetic Esters Examples
1. Mono Esters Oleate ester of methyl, isopropyl, isobutyl, n-butyl, 2-ethyl hexyl etc. Stearate ester of n-butyl,, 2-ethyl-hexyl, isobutyl, isooctyl etc. Laurate ester of methyl, 2-ethyl hexyl etc. Isopropyl myristate/palmitate.
2. Unsaturated Polyol Esters Trimethylol propane (TMP) ester/trioleate, pentaerythritol (PE) terra oleate/dioleate, neopentyl glycol (NPG) dioleate etc.
3. Saturated Polyol Esters Glycerol monooleate/dioleate, propylene glycol dioleate, glycerol trioleate, propylene glycol 400 dioleate etc.
4. Fatty Acid amide Ester, phthalate esters etc. —
The fatty acid used in the additive of the present invention is selected from C-12 to C-22 fatty acids, preferably C-16-C-18 fatty acids and /or its isomers thereof.
The natural fats and ester have a tendency to decompose to fatty acid with time, heating and hydrolyze during use in the cold rolling operation. Antioxidant used to prevent the conversion of ester to the fatty acid. The antioxidants used in the present invention are amine type and /or hindered phenolic based their mixtures and isomers thereof. The amine type antioxidants used in the invention are such as
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phenyl naphthyl amines( alpha and/or beta), diphenyl amines, including alkylated diphenyl amines. Commercially available examples of such antioxidants are Irganox L-57, Vanlube SL,_Irganox L 67, etc. The phenolic type antioxidants used in the invention are such as 2, 6-di-tert-butylphenol, liquid mixtures of tertiary butylated phenols, 2, 6-di- tert-butyl-4-methyl phenol, 4,4'-methylenebis(2.6-di-tert-butylphenol), 2, 2'-methylenebis(4-methyl-6-tert-butyl-phenol), mixed methylene-bridged polyalkyl phenols and 4,4'-thiobis(2-methyl-6-tert-butyl phenol). Commercially available examples of such phenolic type antioxidants are Irganox L 115, Irganox L-l 18 and Irganox 135 etc.
Extreme pressure and antiwear additives are also required to take care the load during the actual process of rolling and reduction in the mill. The additives selected and used in the present invention are based on sulphur, phosphorous, and Zinc as single component or mixture of components of above. Examples of extreme-pressure and anti-wear agents are dilauryl phosphate, didodecyl phosphite, trialkylphosphate such as tri(2-ethylhexyl)phosphate, tricresylphosphate (TCP), zinc dialkyl(or diaryl)dithiophosphates (ZDDP), phospho-sulphurized fatty oils, zinc dialkyldithiocarbamate), mercaptobenzothiazole, sulphurized fatty oils, sulphurized terpenes, sulphurized oleic acid, alkyl and aryl polysulphides, sulphurized sperm oil, sulphurized mineral oil, chlornaphta xanthate, chlorinated paraffinic oils, chlorinated paraffin wax, and zinc dialkyl(or diaryl)dithiophosphates (ZDDP), tricresylphosphate (TCP), trixylylphosphate (TXP), dilauryl phosphate, respectively.
Antifoam is required to prevent the foam and frothing characteristics of the oil in the presence of water during use. Sometimes the formulation it self is enough to take care of the antifoaming characteristics. Hence the formulation may or may not
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contain antifoam. The antifoam selected in the formulation is silicone based antifoam. Examples of anti-foaming agents are Polyoxyalkylenamine, Branched Polyamines, Succinic Anhydride Derivatives, Siloxanes e.g. methylpolysiloxanes, amino-substituted organopolysiloxanes etc., Commercial antifoams are Foam blast 2 and foam blast 5 available at Lubrizol. Other commercial sample is Foamban MS 455-3A
The emulsifier and surfactant are required for the emulsion formation, the stability of the formulation as a lubricant and surface cleaning agent. The emulsifiers used are nonionic, cationic, and anionic as individual or the mixtures of all thereof. The emulsifiers may be ethylene oxide, propylene oxide or its condensate, amine ethoxylate, alcohol ethoxilate, sulphonate etc. The molecular weigh of the nonionic emulsifier/surfactant is 1000 - 20000 with an HLB value 4- 16, typically 7-12.
An example of the nonionic surfactants having a molecular weight of 1000-20000 and an HLB value of 4-9 includes Sorbitan Monooleate, copolymers of propylene glycol and ethylene glycol, as well as esters or polyesters prepared from fatty acids, polyfatty acids or polycondensed fatty acids and alcohols such as ethylene glycol, glycerin, sorbitol, sorbitan and the like or polyalcohols.. Examples of nonionic surfactants having an HLB value of 10-16 include Sorbitan Esters, e.g. Sorbitan Monooleate, Ethyoxylated Sorbitan Ester e.g., Polyoxyethylene (20) Sorbitan Trioleate, Polyoxyethylene Sorbitan Monooleate, Alcohol Ethoxylates, Alkanol amides, Ethoxylated alkanolamides, Ethylene Oxide/Propylene Oxide copolymers, Fatty acid ethoxylatges e.g. PEG (400) monolaurate, Polyoxyethylene nonylphenol/Alkyl phenol ethoxylates, Polyoxyethylene alcohol, polyoxyethylene alcohol ether, polyoxyethylene nonylphenyl ether, polyoxyethylene fatty ester, polyoxyethylene sorbitan ester, polyoxyethylene sorbitol ester and the like.
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The cationic emulsifiers used in the present invention are Tallow amine e.g. PEG-10 Tallow amine, PEG-15 Tallow Amine, Quaternary ammonium salt, amine, imidazoline and their derivatives. Examples of commercially available cationic emulsifiers- Rhodameen S 20, Rhodameen S25 etc.
The base stock oil can be paraffinic or naphthenic, hydrocracked and all possible isomers or mixture thereof. The base stocks are belonged to API group I and II oils.
The base oil typically has a viscosity from 5 to 60 cSt at 40.degree. C. and preferably from 12 to 58 cSt at 40 °C. Viscosity of the formulation can be adjusted by mixing adequate quantity of the required different base oils. The flash point of the base oil should be greater than 150 °C and typically 200 °C.
The base oil and/ fat, ester heated to 45-50 °C with stirring. The cold rolling oil phase was prepared by adding the extreme pressure and / antiwear additives, emulsifiers, antioxidant etc to the base oil or the mixture of base oil, fat and ester one by one under stirring condition. Reasonable time (5-10 minutes for each additive) was given to dissolve one additive before addition of the next additive. The final (after addition of the final additive) rolling oil blend stirred for another 30 minutes with stirring and heating. Ordinary Remi stirrer used for the stirring and dissolving the additives to the base stock. Precaution taken for avoiding excessive heating (> 60 °C) of the oil phase. Thus the cold rolling oil formulation finalized. The water used for making the emulsion was either D.M water with a pH of 6.5-7.5 and hardness 14

addition of cold rolling oil phase of required quantity to the water phase ( 45-50 C) and stirring the emulsion under high shear @ 11000 rpm for 5 minutes with a special homogenizer ( ULTRA TURRAX T-25 basic unit with dispersing tool spindle No : S 25 N-25 F of IKA LABORTECHNIK, GmbH, Staufen). The total emulsion prepared was 100 ml. The condition of the emulsion (oil separation and stability) was checked time to time for 24 hrs keeping the emulsion ( 100 ml in a measuring cylinder with stopper) in a preset 50 °C air oven. The emulsion stability and metastabilty of the emulsion then assessed by the separation of the amount of cream and oil.
The lubrication property of the formulations can be evaluated in terms of friction coefficient and Falex Jaw Load ( Load Carrying Capacity of the rolling Oil). This is carried out as per ASTM D-6425 (friction coefficient) and ASTM- D 3233 ( Falex Jaw Load). The concentrated and diluted emulsions (coolants) were evaluated for the friction coefficient and Falex Jaw Load respectively. The burn off characteristics is evaluated by the thermo gravimetric analysis (TGA) in inert gas e.g. Argon atmosphere. The evaluation is carried out by heating the sample from the room temperature to the to the specified temperature. We have selected the final temperature to 550 °C. Then the residue left is measured.
Experimental Description
In order to establish the suitability of the developed oil composition, a number of compositions using various components comprising natural fats / oils, synthetic esters, high viscosity mineral oil and other performance additives such as extreme pressure, antiwear, emulsifiers, antioxidants, antifoam etc. were prepared and evaluated for emulsion stability, hard water compatibility, burn off characteristics, lubricity etc.
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It can be appreciated that only combination of emulsifiers and natural fats / oils is not sufficient for making good quality steel cold rolling oil. Therefore, an optimized combination of emulsifiers and other performance additives was selected based on the chemistry and nature of the emulsifiers to get a composition of rolling oil suitable for thin gauge steel sheet rolling.
The compositions and results of various experiments carried out are compiled as follows:
Example -1
A blend of 40 % wt of coconut oil, 40% wt of palm oil, 10% wt of TMP trioleate, 4.5 %wt of oleic acid, 0. 5 % wt hindered phenol based antioxidant, 1% wt of phosphorous based extreme pressure additive, 3% wt nonionic emulsifier-1 ( HLB value = 11), 1% wt nonionic emulsifier-2 (HLB value = 10).
Example -2
A similar composition of blend-1 where 5% wt of TMP trioleate replaced by 5% wt of base stock where paraffin is the major ingredient.
Example -3
A similar composition of blend -1 where 1% wt of nonionic emulsifier-2 replaced by 1% wt of amine ethoxylate.
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Example - 4
A similar composition of blend -1 where 0.5% wt of hindered phenol has been replaced by mixed antioxidants 0.4% wt of hindered phenol and 0.1 %wt of amine type antioxidant.
Example - 5
A similar composition of blend -2 where 100 ppm antifoam is present replacing 100 ppm base oil.
Example - 6
A similar composition of blend -2 where the 1% wt of nonionic emulsifier-2 replaced by amine ethoxylate and 1% phosphorous based extreme pressure additive replaced by 0.5% phosphorous and 0.5%wt of sulphur based extreme pressure additive.
Example -7
A similar composition of blend -1 where 40 % wt of palm oil replaced by 40 % wt ofrapeseedoil.
Example - 8
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A similar composition of blend - 7 where 10 % wt of coconut oil, 10% wt of rapeseed oil and 5% wt of TMP trioleate are replaced by 25 % wt of similar base stock as the composition of the blend -2.
Example - 9
A dilution of blend -3 which contain 2% of blend -3 and 98 % of DM water.
Example -10
A dilution of blend - 8 which contain 3.5% of blend -8 and 96.5 % wt of 100 ppm hardness (as CaC03) water.
Example-11
Example No 1 with 0.1% wt. of nonionic emulsifier-1 and 0.1% wt of nonionic emulsifier-2 in place of 3 % wt of nonionic emulsifier-1 and 1% wt of nonionic emulsifier-2 respectively.
Example -12
Example No. 2 with 11% wt. of Polyoxyethylene Sorbitan trioleate and 1% wt. of Proprietary amine ethoxylate emulsifier
Example -13
A blend of 5% wt. Rapeseed oil, 3% wt. of Pentaerythritol dioleate, 1% wt of oleic acid, 0.3% wt of hindered phenol based antioxidant, 0.2% sulfurised fat, 2% nonyl
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phenol ethylene oxide condensate, 0.5% imidazoline emulsifier and 8% wt of paraffinic (major) base Stock.
Example-14
A blend of 5% of Rapeseed oil and 88% wt of base stock in example- 13 is replaced by 50% rapeseed, 20% wt of castor oil and 23% wt of coconut oil.
The above stated examples are only illustrative of the present invention but the scope of the present invention is not limited to that only.
Test Results
The results obtained on various blends explained above are compiled in the following tables based on the studies carried out on particular characteristics:
Table -1. Lubrication Data and Burn off characteristics ( Concentrated Neat
Oil)

s.No. Example No. Friction of Coefficient(300N,50 Hz.,lmm,50-150°C, 1 Hr.) Thermo gravimetricAnalysis (TGA ) @550 °C, inertatmosphere,Residue Left, % wt
1. Example No. 1 0.10 2 Example No. 2 0.12 3 Example No. 3 0.10 4 Example No. 4 0.10 5 Example No. 6 0.11 6. Example No. 13 0.22
7. Example No. 14 — 0.20
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TabIe-2 Lubrication Data and Burn Off Characteristics (Water diluted
Product)

S.No Example No. Falex Jaw Load, lbs Thermo gravimetricAnalysis (TGA) @550 °C, inertatmosphere,Residue Left, % wt
1. 2%v/v oil of Example No 1 in DM water 2800 2 2%v/v oil of Example No 9 in DM water 2700 3 2%v/v oil of Example No 10 in DM water 2400 4. 2% v/v oil of Example No. 13 in DM water 1300
5. 2% v/v oil of Example No. 14 in DM water 0.20
Table-3 Metastability Characteristics
Conditions: Temperature : 50±1 °C , Shear Mixing Rate = 11,000 rpm,
Mixing Time = 5 minutes.

s.No Example No Cream, % VafterInitiaI/lHr/24Hrs Oil, % VafterInitial/lHr/24Hrs Metastability
1. 2 % v/v oil of Example No 1 in DM water Nil/Trace /Nil Nil /Trace/ 1.0 Yes
2. 2 % v/v oil of Example No. 2 in DM water Nil/Trace / Nil Nil/Nil /1.0 Yes
3. 2%v/v oil of Example No 3 Trace/
in 100 ppm (as CaC03) Hard water
4. 2% v/v oil of Example No. 11 in DM as well as 200 ppm (as CaCo3) hard water - - No (Complete separation)
Table 4 : Hard Water Compatibility Data Conditions: Temperature : 50±1 °C , Shear Mixing Rate = 11,000 rpm ,
Mixing Time = 5 minutes

s.No Example No Cream / Oil, % V (after 24 Hrs) Emulsion Stability
1. 2%v/v oil of Example No 1 in 100 ppm (as CaC03) Hardness water Trace / 1.0 Satisfactory
2. 2%v/v oil of Example No 4 in 200 ppm (as CaC03) Hardness water 3. 2%v/v oil of Example No 10 in 200 ppm (as CaC03) Hardness water 1.0/1.5 Satisfactory
4. 2% v/v oil of Example No. 11 in 100 and 400 ppm (as CaC03) Hardness water Complete separation
The above test results describe the lubricity, burn off, emulsion stability and hard water compatibility characteristics of the oil composition claimed in the present invention.
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We claim:-
1. A rolling oil composition which forms a metastable oil-in-water emulsion after dilution with water and having hard water tolerance, good burn off characteristics and good lubrication properties comprising 10 to 90% by weight of natural fats/oils, 5 to 30% by weight of synthetic esters, 0-20% by weight of fatty acids or mixtures thereof, 0.01-5% by weight of antioxidants or mixtures thereof, 0.5 to 15% by weight of extreme pressure and antiwear additives or mixtures thereof, 0 to 1% by weight of antifoam agents. 0.5 to 10% by weight of minimum one emulsifier or surface active agent and mixtures thereof and 0 to 30% by weight of high viscosity mineral base oil.
2. A rolling oil composition as claimed in claim 1, wherein the said natural fats or oils are based on the vegetable or animal fats or mixture thereof; and selected from fatty acid esters of C-8 TO C-22 preferably C-12, C-14r C-16. C-l 8 and C-22, their mixtures and their isomers.
3. A rolling oil composition as claimed in claim 1, wherein the said fatty acids having saponificaiton value of 150 to 300 mgKOH/g, having Kinematic viscosity of 30cst to 250cst 40°C and having flash point higher than 160° C .
4. A rolling oil composition as claimed in claim 1, wherein the said synthetic ester selected from fatty acid esters of C-12 to C-l8, their isomers, complexes, mixtures thereof and self emulsifying esters.
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A rolling oil composition as claimed in claim 1, wherein the said synthetic esters having kinematic viscosity of 5 est to 60 est, preferably 30 to 50 est at 40° C and having flash point more than 160°.
A rolling oil composition as claimed in claim 1, wherein said fatty acids are selected from C-12 to C-22 fatty acids, preferably C-16 to C-18 fatty acids and isomers thereof.
A rolling oil composition as claimed in claim 1, wherein said antioxidants are amine type or/ and hindered phenol type including their isomers and mixtures thereof.
A rolling oil composition as claimed in claim 1, wherein said extreme pressure and antiwear additives are based on sulphur, phosphorous. Zinc and mixtures thereof.
A rolling oil composition as claimed in claim 1, wherein said antifoam agents are selected from polyoxyalkylenamine, branched polyamines, succinic anhydride derivatives, siloxanes and mixtures thereof.
A rolling oil composition as claimed in claim 1, wherein said emulsifiers or surface active agents are non-ionic, cationic, anionic and their mixtures thereof.
A rolling oil composition as claimed in claim 10, wherein said non-ionic emulsifiers or surface active agents having HLB value of 4-16, preferably 7-12, with molecular weight of 1000-20000.
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12. A rolling oil composition as claimed in claim 10, wherein said cationic emulsifiers or surface active agents are nitrogen based.
13. A rolling oil composition as claimed in claim 1, wherein said mineral base oil is selected from paraffinic, naphthenic, hydrocracked oils and mixture thereof. These base stocks belongs to API group I and II base oils.
14. A rolling oil composition as claimed in claim 1, wherein said mineral base oil having kinematic viscosity of 5 to 60 Cst at 40° C, preferably 12 to 58 Cst at 40° C and having flash point higher than 150° C.
15. A rolling oil composition as claimed in claim 1 to 14 having friction coefficient between 0.05-0.20.
16. A rolling oil composition as claimed in claim 1 to 15 having superior burn off characteristics (TGA@550° C 17. A rolling oil composition substantially as herein described with foregoing description and accompanying tables and examples.
SHARAD VADEHRA
FOR KAN-AND KRISHME ATTORNEY FOR THE APPLICANTS
Dated this 27th day of June 2006
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ABSTRACT
"Composition of oil for thin gauge steel rolling"
The invention relates to a composition of oil for thin gauge steel rolling comprising of natural fats / oils, synthetic esters, high viscosity mineral oil and other performance additives such as extreme pressure, antiwear, emulsifiers, antioxidants, antifoam etc. The composition forms oil-in-water milky meta-stable emulsion with water. The said composition is suitable for thin gauge steel rolling. It has excellent lubricity and burn off characteristics. It also has very good hard water compatibility.
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Documents:

1007-mum-2006-abstract.doc

1007-mum-2006-abstract.pdf

1007-MUM-2006-CLAIMS(AMENDED)-(26-3-2013).pdf

1007-MUM-2006-CLAIMS(AMENDED)-(29-1-2014).pdf

1007-MUM-2006-CLAIMS(MARKED COPY)-(26-3-2013).pdf

1007-MUM-2006-CLAIMS(MARKED COPY)-(29-1-2014).pdf

1007-mum-2006-claims.pdf

1007-mum-2006-correspondance-recieved.pdf

1007-MUM-2006-CORRESPONDENCE(19-05-2010).pdf

1007-MUM-2006-CORRESPONDENCE(5-8-2013).pdf

1007-MUM-2006-CORRESPONDENCE(IPO)-(27-6-2006).pdf

1007-mum-2006-description (complete).pdf

1007-MUM-2006-FORM 18(19-05-2010).pdf

1007-MUM-2006-FORM 2(TITLE PAGE)-(27-6-2006).pdf

1007-mum-2006-form-1.pdf

1007-mum-2006-form-2.doc

1007-mum-2006-form-2.pdf

1007-mum-2006-form-26.pdf

1007-mum-2006-form-3.pdf

1007-mum-2006-form-5.pdf

1007-MUM-2006-POWER OF ATTORNEY(27-6-2006).pdf

1007-MUM-2006-POWER OF ATTORNEY(29-1-2014).pdf

1007-MUM-2006-REPLY TO EXAMINATION REPORT(26-3-2013).pdf

1007-MUM-2006-REPLY TO HEARING(29-1-2014).pdf


Patent Number 259470
Indian Patent Application Number 1007/MUM/2006
PG Journal Number 12/2014
Publication Date 21-Mar-2014
Grant Date 13-Mar-2014
Date of Filing 27-Jun-2006
Name of Patentee INDIAN OIL CORPORATION LIMITED
Applicant Address G-9, ALI TAVAR JUNG MARG, BANDRA (EAST), MUMBAI
Inventors:
# Inventor's Name Inventor's Address
1 DEEPAK SAXENA C/O INDIAN OIL CORPORATION LIMITED, G-9, ALI YAVAR JUNG MARG, BANDRA (EAST), MUMBAI-400051,
2 SUBINOY PAUL C/O INDIAN OIL CORPORATION LIMITED, G-9, ALI YAVAR JUNG MARG, BANDRA (EAST), MUMBAI-400051,
3 ARUNAGIRI SAMY C/O INDIAN OIL CORPORATION LIMITED, G-9, ALI YAVAR JUNG MARG, BANDRA (EAST), MUMBAI-400051,
4 KANDISSERIL CHELLAPPAN JAYAPRAKASH C/O INDIAN OIL CORPORATION LIMITED, G-9, ALI YAVAR JUNG MARG, BANDRA (EAST), MUMBAI-400051,
5 UMISH SRIVASTAVA C/O INDIAN OIL CORPORATION LIMITED, G-9, ALI YAVAR JUNG MARG, BANDRA (EAST), MUMBAI-400051,
6 RAJENDRA MAHAPATRA C/O INDIAN OIL CORPORATION LIMITED, G-9, ALI YAVAR JUNG MARG, BANDRA (EAST), MUMBAI-400051,
7 AJAY KUMAR HARINARAIN C/O INDIAN OIL CORPORATION LIMITED, G-9, ALI YAVAR JUNG MARG, BANDRA (EAST), MUMBAI-400051,
8 VEENA RANI BANSAL C/O INDIAN OIL CORPORATION LIMITED, G-9, ALI YAVAR JUNG MARG, BANDRA (EAST), MUMBAI-400051,
9 BABU RAM TYAGI C/O INDIAN OIL CORPORATION LIMITED, G-9, ALI YAVAR JUNG MARG, BANDRA (EAST), MUMBAI-400051,
10 RAVINDER KUMAR MALHOTRA C/O INDIAN OIL CORPORATION LIMITED, G-9, ALI YAVAR JUNG MARG, BANDRA (EAST), MUMBAI-400051,
11 RAM PRAKASH VERMA C/O INDIAN OIL CORPORATION LIMITED, G-9, ALI YAVAR JUNG MARG, BANDRA (EAST), MUMBAI-400051,
PCT International Classification Number C10M143/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA