Form 2
THE PATENTS ACT 1970
(39 of 1970) COMPLETE SPECIFICATION
(SECTION 10, rule 13)

"A soluble cutting oil and soluble cutting oil additive composition"
Indian Oil Corporation Limited, an Indian company, ofG-9, All Yavar Jung Marg, Sandra (East), Mumbai - 400051, Maharashtra, India.

The following specification particularly describes and ascertains the nature of this invention and the manner in which it is to be performed

This invention relates to soluble cutting oil and soluble cutting oil additive for metal working applications.
Metal working oils in general constitute an area of lubrication technology where chemistry is very much in action in the whole application regime. The performance or non-performance of a metal working fluid becomes quickly evident during its use. Unlike other industrial oil lubricants, where the performance of the oil will be known only after some time, the performance of metalworking oil will become evident as soon as it is put into the machining operation. A defect in a soluble oil, for example cutting oil or rolling oil, will show up in a couple of days if not earlier and will call for quick corrective action. The factors affecting the performance of these oils are multi faceted; therefore, these oils require special attention 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 etc.'
Metal cutting fluids are traditionally classified according to their composition and are classified as neat oil, soluble oil, semi-synthetic fluid, or synthetic fluid. Soluble cutting oils do not contain appreciable amount of water and are provided to the end user as oil containing Specialty additives. Soluble cutting oil (or emulsifiable oil) is a combination of 30-85% of highly refined mineral oil, and tailor made additive systems. The emulsifier additives adsorb over oil globules and help in dispersing oil in water phase. The fluid concentrate usually includes other additives such as chlorinated or sulfurized mineral oils, fatty oils, or mixtures thereof, biocides, corrosion/rust inhibitors etc. to improve performance and lengthen the life of the fluid. Soluble cutting oil products are supplied as concentrates that are diluted with water to obtain the working fluid. Depending on the fluid and the application, the concentrate may be diluted one part concentrate to five parts of water or up to one part concentrate to forty parts of water (i.e. 17% to 2.4%). Soluble cutting oils provide good lubrication. In addition, they provide improved cooling as compared to straight oils. However, soluble cutting oils sometimes have poor corrosion control and sometimes leave the machine tool surface and nearby areas dirty because of the oil and difficult-to-remove product residues, may smoke, and may have poor mix stability or short sump life.
Consequently, a need exists for a metal working fluid (soluble oil), which provides longer
sump life, which is relatively inexpensive, and which is effective for reducing friction
generated during metal cutting operation and is able to provide effective cooling of the
work-piece and tool. There is also a need that soluble cutting oil should be less foaming
and providing corrosion protection.
Today, soluble type metal working fluids are made by two ways. First is by taking all the required ingredients i.e. base oil and additives one-by-one in one go and mixing/reacting

them to get the desired product. However, this procedure is tricky and requires careful blending of all the components. Second process is however, more economical and widely used in the industry. In this process a soluble cutting oil concentrate is prepared first and thereafter it is further diluted with required quantity of the base oil etc. to get the final product.
The present invention covers the composition and process of making soluble cutting oil and also a versatile soluble cutting oH additive(concentrate) for making soluble cutting oils.
PRIOR ART
A variety of chemicals, additives and surfactants have been used to formulate the soluble cutting oils. Some of the common ingredients are base oils, polyol esters, sodium petroleum sulphonates, salts of fatty acids, nonionic surfactants, mono ethanol amine, tri elfianol amine, sulphurised fatty material, iatiy acid esters, chlorinated paraffin, fatty alcohols, hindered phenols^bipcides, odorizing agent, azo dyes, alkali etc, The composition of soluble cutting oils is specific for each company or worker. No two compositions are identical and these compositions are specific to the application requirements. The compositions most recent to some of the oldest, as reported in literature are listed below:
An antibacterial water-soluble cutting fluids resistant to yeast-like fungi is patented by Masahiro Noda etal. of Yushiro Chemical Industry Co., Ltd., Japan (European Patent Appl. {1990), EP 388320 Al 19900919)^ comprises an amine or amine derivative, TrTa^dTGonto a mineral~oif Bnd/or fatty oil, an extreme-pressure additive and a surfactant. Suitable amines include anilinoamines and aralkylamines, e.g., 4-methoxy-2-methylaniline and p-benzylaminophenol.
Stable emulsions of soluble oil are disclosed by John R. Scheidker and Ford C. Teeter of Sinclair Research, Inc. (JUS 3296129p Emulsions which are stable even when prepared with H20 at 50 deg.F. ancTcontaihing 100 ppm hardness as CaC03 are obtained by first augmenting the normal H20 content of soluble oils (0.5-5%) by the addition of .apprx.l part by vol. H20/1. soluble oil. The soluble oils contain 60-98% of a medium-viscosity refined mineral lubricating oil, with 6-25% by weight of the oil of oil-soluble aromatic sulfonates prepared from sulfonic acids of av. mol. weight 400-500 as an emulsifying agent and 1-5% by weight of the oil of a glycol or alkyl ether glycol with 12 deg.C. atoms as a coupling agent; the soluble oil may also contain corrosion inhibitor(s), secondary emulsifying agents, bactericide(s) and (or) antifoam age'nt(si Jacob Faust and Ira Kukin of Sonneborn Chemical and Refining C6jro (US 309882^Wiave patented Soluble oil-base cutting oils prepared, by blending 72T5-parls by_ weight of a mixture containing 70% petroleum mahogany sulfonate, 19.5% K rosin soap, 4.5% diethylene glycol, and 6% water with 2.8 parts 45% KOH solution, 6.5 parts nonylphenol, and 18.2 parts of a naphthenic-based petroleum hydrocarbon distillate. Solution-type metal-cutting and grinding fluid are patented-by-^ohn-fcj^urray and Roy A Westlund Jr. of Esso Research and Engineering Co(US 3046^2^). The composition can be prepared by aqueous solution of NaNOZ and*Nalauroyl sarcosinate (I) in a weight ratio of 1:1 to 11:1,
3

with or without a compatible nonionic or anionic surface-active agent. NaN02 and I combine synergistically to give rust inhibition at low concentrations A buffer may also be included. The working fluid contains 0.2-0.5% NAN02, 0.02-0.05% I, and 0.20.5% surface-active agent. Stock solutions for diln. to working fluid may contain as much as 10% NaN02, with other components in proportion. E.g., a concentrated solution was prepared containing NaN02 10, Pluronic L-64 20, 30% aqueous solution of II 3.33, and water 66.07 parts. At -20:1 diln. this solution gave no rust on east iron in an 18-24-hr. test; 50:1 diln. gave only a trace of rust. Earl E.Fischer of Gulf Oil Corp. (US 2913410) has disclosed that soluble oil composition can be prepared, by blending 3-7% K soap of resin acids, 4-7% Na petroleum sulfonate having an av. mol. weight of 425-430, and a sufficient amount of coupling agent to produce a readily emulsifiable soluble oil with 80-95% mineral lubricating oil. He has further disclosed that the compositions are useful as cutting oils as well as for any of the other uses in which oils forming stable non-corrosive emulsions with H20 are used. For example, a soluble oil base was prepared by charging 59.5% by weight of Dresinate 95 (consisting of 80.5-82.0% K salts of tall oil acids, 11.0-13.0% H20, and 6.0-7.5% diethylene glycol as the coupling agent) to a mixing tank, heating to 100-130 deg.F., and stirring in 39.5% Bryton 430 sulfonate (consisting of 62-3% Na petroleum sulfonate having an av. mol. weight of 430 and the balance mineral oil). H20 (1%) was added to the tank, and the entire contents stirred at 120-130 deg.F. until mixed. The soluble oil base (18.0% by weight) was blended with 82.0% light lubricating oil (100/2 Texas oil) to form a soluble cutting oil having the following characteristics: A.P.I, gravity, 20.3 ; viscosity at 100 and 210 deg.F. , resp., of 285 and 50.1 Saybolt Seconds Universal; flash point, 320 deg.F.; ignition point, 360 deg.F; pour point, -35 F.; 0.46% S; 0.80% H20 by distn.; and 2.56% C residue (Conradson). Everett C Hughes and Harrison M. Stine of Standard Oil Co. (US 2852468) patented a soluble cutting oil composition consisting of 80-99% sulfurized mineral oil (I), 1-20% sorbitan mono- or trioleate, and 0.25-5% of an oil-soluble chlorinated org. compd. (II). The I include any oil of lubricating range viscosity containing 0.3-2% S. The II include chlorinated C10H8, biphenyl, diphenyl oxide, and paraffin wax. A typical composition consists of 29% I prepared from neutral oil having a viscosity of 100 Saybolt sec. at 100 F. and containing 0.8% S, 5% sorbitan mono.ovrddotoleate, and 3% chlorinated biphenyl containing 1.62% CI. John D. Oathout of Esso Research and Engineering Co. has disclosed (US 2802786) that emulsifiable cutting oils are produced from the "Napex" solution which is used for extn. of naphthenic acids from lubricating oil. Other sulfonates and soaps may be added. A typical oil was prepared as follows: a Coastal distillate was treated with 20 lb./bbl. of 98% black H2S04, and the sludge was removed; the remaining oil was extracted with 6 bbl. fresh Napex solution (I)/100 bbl. of oil, and the mixture was heated to 190 deg. F. by blowing with steam. The I is an aqueous solution of 20-30% toluene- or xylenesulfonates, 10-15% inorganic salts (principally Na2S04), 0.5-5% NaOH, and 50-70% H20. The spent I was allowed to settle out, the water layer was drawn off, and the org. layer was blown with air to remove the remaining water. About 12 bbl. of product were recovered per 100 bbl. of oil treated. The Napex was blended as follows: Napex 15.6, mineral lubricating (45 Saybolt Universl sec. viscosity at 210 deg.F.) 79.4, diethylene glycol 3.0, water 1.0, and triethanolamine 1.0% by weight Elliott S.Francis and Joseph H. Piatt of Gulf Research & Development Co (US 2818386) have disclosed soluble cutting-oil compositions comprises 15-40% by weight of an oil-in-water emulsifying agent (I) and 60-85% of a lubricating grease (II). I includes sulfonated

fatty materials, oleates and stearates of mono-, di-, or triethanolamines, polyoxyethylene sorbitan fatty acid esters, or Na mahogany sulfonates. II contains a water-insoluble soap of satd. fatty acids, such as a Ca soap of tallow, and is preferably formed before I is mixed with II.
CAN Paul M. Ruedrich of NOPCO Chemical Co. (US 2794000) has patented emulsifiers for soluble oils, cutting oils, and spray oils. He has disclosed that a mixture of 30.4% lauric acid, 25.4% oleic acid, 3.5% Mid-Continent oil (I), and 40.7% diethanolamine was introduced into a vented esterification kettle and heated to 325 deg.F. When titration showed an acid value equiv. to 12 mg. KOH/g., indicating consumption of 93% of the acid, the reaction was stopped by cooling to room temp.; a brown, viscous liquid was obtained, d. 8.4 lb./gal. at 85 Deg, F. To 95 parts by weight of a solvent-refined Coalinga crude oil fraction having a Saybolt Universal viscosity of about 100 at 100 deg.F., 5 parts by weight of the above liquid was added to give a clear solution which remained stable without precipitaion for several months. Ten parts by weight of this oil was added to 90 parts water to give an oil-in-water emulsion which remained stable for 24 hrs. and was satisfactory as a cutting-oil emulsion. A steel plate immersed in this emulsion did not rust in 24 hrs. Use of dipropanolamine and etnylbutanolamine is also claimed. Geo. R Cook etal. of Pure Oil Co. (US 2764549) have disclosed that stable oil-in-water emulsions with Mid-Continent oil (I) are prepared by addition to the oil of an equal amount of the ext. obtained when I is extracted with phenols, e.g. in the preparation of lubricating oils. To form the emulsion, 15% by weight emulsifying agent (II) is added to the oil-ext. mixture The II consists of mahogany sulfonate (III) 10.06, diethylene glycol (IV) 1.64, oleic acid 2.01, KOH 0.34, and water 0.95 parts by weight diluted with water in ratios of 1:10,1:15, or 1:20. Ill functions as an emulsifier; for economic reasons, part of it can be replaced by Na or K salts of processed rosins or resins. IV is a coupling agent soluble in both oil and water. The dispersibility of II in oil is controlled with oleic acid and KOH. A satisfactory emulsion useful as a cutting oil can also be prepared with residual ext. only, III, IV, and alkali, but without fatty acid or additional oil. John D. Oathout of Standard Oil Development Co. (US 2689222) has disclosed that performance of cutting oils is improved by the addition of 0.1-3% by weight of the partial fatty esters of sorbitan and the polyoxyethylene derivatives of such partial esters. David. Frazier of Standard Oil Co. (US 2653909) has reported that an emulsifiable lubricant or coolant for machining, cutting, or grinding of metals is made by oxidizing a solvent-extracted or white petroleum oil of 75-600 Saybolt Universal sec. viscosity at 100 deg. F. The product is neutralized with 5 times the calculated amount of base in the presence of 0.1 % by weight of solvent. The recommended concentration of oil in water is 1 to 40-80 parts. The oil thus prepared is very stable, has excellent chip-settling properties, and does not require an emulsifying agent when used in the form of a water emulsion. Bacteria grow very slowly in it, hence it has a long life. Ernst Laug of Socony-Vacuum Oil Co., Inc. (US 2625509) has disclosed that stable, rust-inhibiting, water-base cutting fluids are prepared in the following composition range: K soap of castor-oil fatty acids 17-20, triethanolamine soap of castor-oil fatty acids 2-5, triethanolamine phosphate 8-13, H20-soluble polyalkylene glycol 3-5, NaN02 1.5-2.5, Na mercaptobenzothiazole 0.75-1.5, phenol 1-1.5%, rest H20. The compns. are preferably dild. with 10-60 parts of H20 per part of the composition In compounding, castor oil is heated in an agitated, steam-jacketed kettle at 110-20 deg. F. KOH (50% aqueous solution) is then added slowly with
5

stirring and temp, rise to 180 deg. F. for 15 hrs. or until saponification is complete. With continuing agitation, triethanolamine is added, followed by polyalkylene glycols and phosphoric acid. After stirring 0.5 hr., the mixture is cooled to 120 deg.F., H20 added slowly, and stirring continued until the solution is clear. NaN02 is then dissolved in the solution, followed by Na mercaptobenzothiazole and phenol. The product was tested for its efficiency in tapping and drilling of steel and for its corrosivity to malleable Fe. Machining fluid are^catented by Franklin Veatch and John G. Partch of Standard Oil Co. (US 257886$),! He has described that a "soluble cutting oil" of high S content combining the-Jreaf removal qualities of emulsions with the surface finish qualifies of sulfurized cutting oils has been produced. Heretofore, sulfurized cutting oils for a good surface finish have been limited to a max. of about 5% S. For high speed cutting operations heat removal is the prime consideratipn and "soluble cutting oils" consisting of oil emulsions containing about 90% H20 are used. In such emulsions previous sulfurized oils have no advantage as regards surface finish. It has been found possible to prep, a S concentrate containing as much as 35-50% S in "motor polymer," which is made by nonselective polymerization of C3 and C4 olefins, and consists mainly of C8-C10 highly-branched olefins, with substantially no diolefins, aromatic, naphthenic, or paraffinic hydrocarbons. When properly prepared this concentrate has a "color suitability index" of 75 or less, giving light-colored emulsions. The machining fluid consists of an emulsifying agent, e.g. sulfonated mineral oil, and mineral oil if necessary to produce a stable emulsion. E.g., motor polymer 44 and S 36 lb. were heated in a closed vessel at 300 deg.F. for 5 hrs. with slight agitation. Unreacted S was removed, and 28.7% of the reaction product was removed by steam stripping as unreacted motor polymer. Two parts of I were mixed with 2 parts of straw oil having a viscosity of 75 Saybolt Universal seconds at 100 deg.F., and 1 part of sulfonated mineral oil to give a sulfurized "water soluble" cutting oil containing 17.9% S (II). Five parts of II were mixed with 95 parts H20 to give an emulsion which was used in a heavy machining test under controlled conditions. II gave a surface finish much better than the usual soluble oils. Thomas W. Dixon of Standard Oil Development Co (US 2563588) nks disclosed a nonfoaming, soluble cutting oil consists of petroleurAvSulfonate 10-50, ry reacting alkanolamine and fatty acid in situ.
The alkanolamine for the preparing amine oleate is selected from diethanol amine, monoethanol amine and tri ethanolamine, preferably tri ethanolamine and the fatty acid is oleic acid.
The co-solvent is lauryl alcohol-
The non-ionic emulsifier is selected from sorbitan monooleate, Tween 80 (Polyoxyethylene sorbitan monooleate) and Tween 85 (Polyoxyethylene sorbitan trioleate). More preferably non-ionic emulsifier is sorbitan monooleate.
More preferably potassium oleate is used.
The biocide in the soluble cutting oil composition is a triazine derivative.
The deodorant is selected from pine oil, eucalyptus oil and phenol preferably pine oil.
Evaluation Methodology
Tests for emulsion stability, cast iron corrosion, thermal stability and frothing tendencies were conducted on the developed compositions of soluble cutting oils. Generally, 20:1 and 5: 1 dilutions were used in the evaluation studies. The details of the test are given below:
• Emulsion Stability Test
A required dilution of the soluble cutting oil in known hardness of water is prepared. A calcium sulphate solution of total hardness equivalent to 400 + 10 ppm in term of calcium carbonate is used for making different dilutions. The dilutions are prepared by taking required hard water in a 500 ml conical flask and this is stirred with the help of magnetic stirrer and oil is quickly added to it and continuously stirred for 2 minutes after last drop addition of soluble cutting oil. The dilutions so prepared are poured in special flasks with graduated neck and allowed to stand for 24 hrs. at 40 ± 4 deg.C. in oven. At the end of 24 hours period neck of the flask is examined for separation of oil and separated material (Cream) and results are reported to the nearest of 0.1 ml of oil/cream separated as emulsion stability. (Reference: IS 1115 - P: 98 test method of IS 1448)
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• Cast Iron Corrosion Test Method
Soluble cutting oil emulsion of required dilution is prepared in accordance with the method given in Emulsion Stability Test procedure. 2 gm of steel millings is kept in the form of a layer on pre polished cast iron test plate. About 2 ml of the emulsion to be tested is poured on the millings so that they are thoroughly wetted. This test plate is kept in the test chamber maintained at 27 + 2 deg. C. and a humidity of 52 + 5% for 24 hours. After completion of the test cast iron plate is rated for number of pits, area of plate stained and intensity of staining. (Reference : IS 1115 Appendix-A test method)
• Thermal Stability Tests
In the thermal stability test method 75 ml each sample of soluble cutting oil is stored at 0 deg.C. and 50 deg.C, in separate stoppered bottles, in an air oven maintained at 50 ± 1 deg. C. and also in refrigerator maintained at 0 ± 1 deg.C. for 16 hours. At the end of test, bottles are removed from refrigerator and oven and allowed to stand undisturbed to attain a temperature of 27 ± 2 deg.C. for any sign of turbidity, gelling or separation reported as the thermal stability of the oil. (Reference: IS 1115 - P: 100 test method of IS 1448)
• Frothing Test
In order to determine the frothing tendency of a soluble cutting oil in a given dilution, the dilution of the soluble cutting oil is prepared in distilled water by dissolving known amount of calcium sulphate so as to give total hardness equivalent to 200 + 10 ppm in term of calcium carbonate. 100 ml of the emulsion is poured at once in a 250 ml capacity stoppered graduated cylinder and shaken vigorously for 15 seconds. After shaking, the cylinder is kept in vertical position and volume of froth is measured after elapse of 15 minutes. After 15 minutes amount of froth remaining in the cylinder is reported as froth. (Reference: IS 1115 - P: 99 test method of IS 1448)
• Bio-stability Test
To determine the biological stability of aqueous machining fluids, a given volume of dilution of the test product is circulated in a special apparatus. The following parameters are being fixed : volume, flow rate, temperature, concentration and dilution water. At regular intervals, the liquid is dosed with a special inoculum. Simultaneously, samples of the liquid are taken out to check the growth of bacterial population and also the pH and rust protection properties. (Reference: ISO/DTR 12927:1995(E))
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Experimental Description
In order to establish the efficacy of the developed soluble cutting oil and soluble cutting oil additive, a number of compositions using components given below were prepared and evaluated for the test listed above.
Components used for Development of Soluble Cutting Oil Composition
Following components were used for this study:

S.No. Components
1. Spindle oil
2. Heavy alkyl benzene
3. Oleic acid
4. Sodium petroleum sulphonate
5. Tnethanolamme
6. Sorbitan monooleate
7. Aqualox 232
8. Lauryl alcohol
9. Triazene derivative
10. Tween 85(Polyoxyethylene Sorbitan trioleate)
11. Tween 80 (Polyoxyethylene Sorbitan monooleate)
12. Water
13. KOH/NaOH solution (30 to 60% solution in distilled water)
14. Odorant (selected from pine oil, eucalyptus oil and phenol preferably pine oil)
Preparation of Amine Oleate-
In order to prepare blends containing oleic acid and triethanolamine, oleic acid and tri ethanolamine are mixed in 1:2 wt % ratio and allowed to react for 3 hours at 50° C and other ingredients are mixed there after. However, amine oleate can be prepared separately also by mixing oleic acid and triethanolamine in 1:2 wt % ratio and allow to react them at 50° C for 3 hours.
Preparation of Potassium Oleate -
After charging of aqueous solution of KOH to the blend components, the reaction is allowed to continue overnight at room temperature, for the complete neutralization of oleic acid, wherein formation of potassium oleate takes place. Oleic acid may also be reacted directly with KOH solution with mild heating to give a thick soap type paste.

\0

s.
No. Components Blend 1 Blend 2 Blend 3 Blend 4
Compositions in % wt
1 Spindle oil 83.5 81.5 79.5 77.5
2 Oleic Acid 7.0 7.0 7.0 7.0
3 Tri ethanol amine 2.5 2.5 2.5 2.5
4 Sodium Petroleum Sulphonate 4.0 6.0 8.0 10.0
5 Lauryl Alcohol 1.5 1.5 1.5 1.5
6 Triazine derivative 1.0 1.0 1.0 1.0
7 Aqualox 232 0.5 0.5 0.5 0.5
Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Clear Brown Liquid Clear Brown Liquid
2 Emulsion Stability -@ 40° C, for 24 hrs at
-20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml 0.3/0.2 0.2/0.5 Nil / 0.4 Nil / 0.5 0.1/0.3 Nil / 0.2 •Nil/0.4 Nil / 0.7
3 Thermal Stability for 16 hrs @ i) 50° C ii) 0° C Pass Pass Gelling Layering Pass Pass Hazy blend Two layers
Example 2
Compositions and properties of blends prepared by variation of water content in Blend 3 are complied in the following table -

s.
No. Components Blend 5 Blend 6 Blend 7 Blend 8
Compositions in % wt
1 Spindle oil 79.5 79.0 78.5 78.0
2 Oleic Acid fi'6\ 7.0 7.0 7.0
3 Tri ethanol amine (ii) 2.5 2.5 2.5
4 Sodium Petroleum Sulphonate u 8.0 8.0 8.0
5 Lauryl Alcohol 1.5 1.5 1.5 1.5
6 Triazine derivative 1.0 1.0 1.0 1.0
7 H20 0.5 1.5 3.0 5.0
U#

Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Clear Brown Liquid Hazy liquid
2 Emulsion Stability -@ 40° C, for 24 hrs at
-20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml 0.1/0.4 0.2/0.5 0.1/0.4 Nil / 0.5 0.1/0.3 Nil / 0.2 0.1/0.4 0.2 / 0.7
__j Thermal Stability for 16 hrs @
i) 50° C
ii)0°C Pass Pass Pass Pass Hazy blend Layering Hazy blend Two layers
The self-emulsifiability of these blends was poor.
Example 3
Compositions and properties of blend prepared using Tween 80 additive by varying its concentration from 0.3 % to 1.5% in blend 6 are given below:

s.
No. Components Blend 9 Blend 10 Blend 11 Blend 12
Compositions in % wt
1 Spindle oil 78.2 78.0 77.5 77.0
2 Oleic Acid 7.0 7.0 7.0 7.0
3 Tri ethanol amine 2.5 2.5 2.5 2.5
4 Sodium Petroleum Sulphonate 8.0 8.0 8.0 8.0
5 Lauryl Alcohol 1.5 1.5 1.5 1.5
6 Triazine derivative 1.0 1.0 1.0 1.0
7 H20 1.5 1.5 1.5 1.5
8 Tween 80 0.1 0.5 1.0 2,5
Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Clear Brown Liquid Clear Brown Liquid
The blends were having good thermal stability but emulsion stability as well as self-emulsibility of these blends was poor.
Example 4
Composition and properties of blends with Tween 85 additive by varying its concentration from 0.3 % to 1.5% in blend 6 are given below:
0 /2~

S.No. Components Blend 13 Blend 14 Blend 15 Blend 16
Compositions in % wt
1 Spindle oil 78.2 78.0 77.5 77.0
2 Oleic Acid 7.0 7.0 7.0 7.0
3 Tri ethanol amine 2.5 2.5 2.5 t 2-5
4 Sodium Petroleum Sulphonate 8.0 8.0 8.0 8.0
5 Lauryl Alcohol 1.5 1.5 1.5 1.5
6 Triazine derivative 1.0 1.0 1.0 1.0
7 H20 1.5 ■ 1.5 1.5 1.5
8 Tween 85 0.1 0.5 1.0 2.5
Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Clear
Brown
Liquid Clear Brown Liquid
The blends were having good thermal stability but emulsion stability as well as self-emulsifiability of these blends was poor.
Example 5
Compositions wim changing base oil concentration were also studied in the concentration range of 70% to 90% and increasing and decreasing the additive concentration in the base blend-6 accordingly as given below:

S.No. Components Blend 17 Blend 18 Blend 19
Compositions in % wt
1 Spindle oil 70 80 90
2 Oleic Acid 10.0 6.7 3.3
^
J Tri ethanol amine 3.6 2.4 1.2
4 Sodium Petroleum Sulphonate 11.4 7.6 3.8
5 Lauryl Alcohol 2.1 1.4 0.7
6 Triazine derivative 1.4 1.0 0.5
7 H20 1.4 1.0 0.5
Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Hazy blend
2 Emulsion Stability -@ 40° C, for 24 hrs at -20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml 0.1/0.2 0.1/0.2 0.1/0.2 Nil / 0.3 No emulsion formation
3 Thermal Stability for 16 hrs @ i) 50° C ii) 0° C Pass Slight Gelling Pass Pass -
%

Example 6
Compositions with different heavy alkyl benzene concentrations were also studied by changing its concentration from 1% to 5 % in blend 18 as given below.

S.No. Components Blend 20 Blend 21 Blend 22
Compositions in % wt
1 Spindle oil 79.0 77.0 75.0
2 Oleic Acid 6.7 6.7 6.7
3 Tri ethanol amine 2.4 2.4 2.4
4 Sodium Petroleum Sulphonate 7.6 7.6 7.6
5 Lauryl Alcohol 1.4 1.4 1.4
6 Triazine derivative 1.0 1.0 1.0
7 H20 1.0 1.0 1.0
8 HAB (Heavy alkyl benzene) 1.0 3.0 5.0
Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Clear Brown Liquid
2 Emulsion Stability -@ 40° C, for 24 hrs at -20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml 0.2/0.3 0.1/0.2 0.2 / 0.4 Nil / 0.3 0.3/0.4 0.2 / 0.3
3 Thermal Stability for 16 hrs @ i) 50° C ii) 0° C Pass Pass Pass Pass Pass Pass
Example 7
Compositions of blends prepared with variation concentration of oleic acid from 2-12% in blend 18 are given below.

S.No. Components Blend 23 Blend 24 Blend 25
Compositions in % wt
1 Spindle oil 84.5 79.5 74.5
2 Oleic Acid 2.0 7.0 12.0
3 Tri ethanol amine 2.4 2.4 2.4
4 Sodium Petroleum Sulphonate 7.6 7.6 7.6
5 Lauryl Alcohol 1.4 1.4 1.4
6 Triazine derivative 1.0 1.0 1.0
7 H20 1.0 1.0 1.0
1*

Properties
1 Appearance Hazy blend Clear Brown Liquid Layer in blend
2 Emulsion Stability -@ 40° C, for 24 hrs at -20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml - 0.1/0.2 Nil / 0.3 -
3 Thermal Stability for 16 hrs @ i) 50° C ii) 0° C . Pass Pass -
Example 8
Compositions of blends prepared with variation in concentration of triethanol amine from 2-12% in blend 24 are given below:

S.No. Components Blend 26 Blend 27 Blend 28
Compositions in % wt
1 Spindle oil 80.0 75.0 70.0
2 Oleic Acid 7.0 7.0 7.0
3 Tri ethanol amine 2.0 7.0 12.0
4 Sodium Petroleum Sulphonate 7.6 7.6 • 7.6
5 Lauryl Alcohol 1.4 1.4 1.4
6 Triazine derivative 1.0 1.0 1.0
7 H20 1.0 1.0 1.0
Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Layer
separation in
blend
2 Emulsion Stability test in water of 400 ppm hardness as CaC03 at -20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml 0.1/0.2 Nil / 0.3 - -
3 Thermal Stability for 16 hrs @ i) 50° C ii) 0° C Pass Pass Fail Fail -
4 Cast iron corrosion test of 20:1 dilution in water of 400 ppm hardness as CaC03 0/1-1 - -
Example 9
Compositions of blends prepared with variation in concentration of sorbitan monooleate 1-15% in blend 24 are given below:
15

S.No. Components Blend 29 Blend 30 Blend 31
Compositions in % wt
1 Spindle oil 78.6 72.1 64.6
2 Oleic Acid 7.0 7.0 7.0
3 Tri ethanol amine 2.4 2.4 2.4
4 Sodium Petroleum Sulphonate 7.6 7.6 7.6
5 Lauryl Alcohol 1.4 1.4 1.4
6 Triazine derivative 1.0 1.0 1.0
7 H20 1.0 1.0 1.0
8 Sorbitan monooleate 1.0 7.5 15.0
Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Clear Brown Liquid
2 Emulsion Stability test in water of 400 ppm hardness as CaC03 at -20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml 0.1/0.1 Nil / 0.2 No emulsion formation No emulsion formation
^ J Thermal Stability for 16 hrs @ i) 50° C ii) 0° C Pass Pass Pass Pass Pass Pass
4 Cast iron corrosion test of 20:1 dilution in water of 400 ppm hardness as CaC03 0/1-1 - -
5 Frothing test on 5:1 dilution in water of 200 ppm hardness as CaC03 Pass - -
Example 10
Compositions of blends prepared with variation in concentration of lauryl alcohol 0.5-5.0% in blend 29 are given below:

S.No. Components Blend 32 Blend 33 Blend 34
Compositions in % wt
1 Spindle oil 79.5 77.5 75.0
2 Oleic Acid 7.0 7.0 7.0
3 Tri ethanol amine 2.4 2.4 2.4
4 Sodium Petroleum Sulphonate 7.6 7.6 7.6
5 Lauryl Alcohol 0.5 2.5 5.0
6 Triazine derivative 1.0 1.0 1.0
7 H20 1.0 1.0 1.0
8 Sorbitan monooleate 1.0 1.0 1.0
i£

Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Clear Brown Liquid
2 Emulsion Stability test in water of 400 ppm hardness as CaC03 at -20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml 0.1/0.1 Nil/0.2 0.2/0.4 0.1/0.3 0.2/0.7 0.3/0.6
3 Thermal Stability for 16 hrs @ i) 50° C ii) 0° C Pass Fail Pass Pass Pass Pass
4 Cast iron corrosion test of 20:1 dilution in water of 400 ppm hardness as CaC03 0/1-1 0/3-1 0/3-2
5 Frothing test on 5:1 dilution in water of 200 ppm hardness as CaC03 Pass Pass Pass
Example 11
Compositions of blends prepared with variation in concentration of triazene derivative 0.5 to 4.0% in blend 29 are given below:

S.No. Components Blend 35 Blend 36 Blend 37
Compositions in % wt
1 Spindle oil 79.1 77.6 75.6
2 Oleic Acid 7.0 7.0 7.0
3 Tri ethanol amine 2.4 2.4 2.4
4 Sodium Petroleum Sulphonate 7.6 7.6 7.6
5 Lauryl Alcohol 1.4 1.4 1.4
6 Triazine derivative 0.5 2.0 4.0
7 H20 1.0 1.0 1.0
8 Sorbitan monooleate 1.0 1.0 1.0
Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Clear Brown Liquid
2 Emulsion Stability test in water of 400 ppm hardness as CaC03 at -20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml 0.1/0.1 Nil/0.1 0.1/0.1 0.1/0.3 0.2/0.3 0.2/0.2
3 Thermal Stability for 16 hrs @ i) 50° C ii) 0° C Pass Pass Pass Pass Pass Pass
4 Cast iron corrosion test of 20:1 dilution in water of 400 ppm hardness as CaC03 0/1-1 0/2-1 0/3-2
5 Frothing test on 5:1 dilution in water of 200 ppm hardness as CaC03 Pass Pass Pass
t*

Example 12
Compositons of blends prepared with variation in concentration of Aqualox 232 additive from 0.5-5% in blend 29.

S.No. Components Blend 38 Blend 39 Blend 40
• Compositions in % wt
1 Spindle oil 77.6 77.6 77.6
2 Oleic Acid 7.0 7.0 7.0
3 Tri ethanol amine 2.4 2.4 2.4
4 Sodium Petroleum Sulphonate 7.6 7.6 7.6
5 Lauryl Alcohol 1.4 1.4 1.4
6 Triazine derivative 2.0 2.0 2.0
7 H20 1.0 1.0 1.0
8 Sorbitan monooleate 1.0 1.0 1.0
9 Aqaulox 232 0.5 2.5 5.0
Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Clear Brown Liquid
2 Emulsion Stability test in water of 400 ppm hardness as CaC03 at -20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml 0.1/0.1 0.1/0.2 0.1/0.3 0.1/0.4 ' 0.2/0.5 0.2/0.4
3 Thermal Stability for 16 hrs @
i) 50° C
ii)0°C Pass Pass Pass Pass Pass Pass
4 Cast iron corrosion test of 20:1 dilution in water of 400 ppm hardness as CaC03 0/1-1 0/0-0 0/0-0
5 Frothing test on 5:1 dilution in water of 200 ppm hardness as CaC03 Pass Pass Pass
Example 13
In order to further improve the emulsion stability of the blends it was observed that if KOH or NaOH solution ( 30% to 60% wt in distilled water)is added to the soluble cutting oil blend in a balanced manner than emulsion stability and self emulsibility of the blends is improved substantially.
Compositions and results of 0.1, 2.5 and 5.5% alkali solution variation in blend 38 are given below:
!#

S.No. Components Blend 41 Blend 42 Blend 43
Compositions in % wt
1 Spindle oil 77 74.6 71.6
2 Oleic Acid 7.0 7.0 7.0
3 Tri ethanol amine 2.4 2.4 2.4
4 Sodium Petroleum Sulphonate 7.6 7.6 7.6
5 Lauryl Alcohol 1.4 1.4 1.4
6 Triazine derivative 2.0 2.0 2.0
7 H20 1.0 1.0 1.0
8 Sorbitan monooleate 1.0 1.0 1.0
9 Aqaulox 232 0.5 0.5 0.5
10 Alkali Solution 60% wt in DW 0.1 2.5 5.5
Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Brown Liquid
with gel
formation
2 Emulsion Stability test in water of 400 ppm hardness as CaC03 at -20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml Nil/0.1 Nil/0.2 0.1/0.3 0.1/0.4 0.4/0.7 0.5/1.5
3 Thermal Stability for 16 hrs @ i) 50° C ii) 0° C Pass Pass Pass Fail Fail Fail
4 Cast iron corrosion test of 20:1 dilution in water of 400 ppm hardness as CaC03 0/1-1 0/3-1 0/4-2
5 Frothing test on 5:1 dilution in water of 200 ppm hardness as CaC03 Pass Pass Fail
However, high concentration of the alkali solution may give poor quality cutting oil.
Example 14
Use of deodorant provides very good smell to the cutting oil and also to its emulsion without disturbing the performance properties of the cutting oil. However there is a need to adjust the components concentration to get the better results. Compositions and results of 0.1. 0.5 and 0.9% deodorant variation in blend 41 are given below :
* 19

S.No. Components Blend 44 Blend 45 Blend 46
Compositions in % wt
1 Spindle oil 76.9 76.5 76.1
2 Oleic Acid 7.0 7.0 7.0
3 Tri ethanol amine 2.4 2.4 2.4
4 Sodium Petroleum Sulphonate 7.6 7.6 7.6
5 Lauryl Alcohol 1.4 1.4 1.4
6 Triazine derivative 2.0 2.0 2.0
7 H20 1.0 1.0 1.0
8 Sorbitan monooleate 1.0 1.0 1.0
9 Aqaulox 232 0.5 0.5 0.5
10 Alkali Solution 60% wt in DW 0.1 0.1 0.1
11 Deodorant 0.1 0.5 0.9
Properties
1 Appearance Clear Brown Liquid Clear Brown Liquid Clear Brown Liquid
2 Emulsion Stability test in water of 400 ppm hardness as CaC03 at -20:1 dilution, Oil/Cream in ml -5:1 dilution, Oil/Cream in ml Nil/0.1 Nil/0.2 Nil/0.1 Nil/0.1 01/0.2 Nil/0.3
3 Thermal Stability for 16 hrs @ i) 50° C ii) 0° C Pass Pass Pass Pass Pass Pass
4 Cast iron corrosion test of 20:1 dilution in water of 400 ppm hardness as CaC03 0/1-1 0/1-1 0/1-1
5 Frothing test on 5:1 dilution in water of 200 ppm hardness as CaC03 Pass Pass Pass
It is evident form the example 1 to example 14 that a cutting oil formulation can be obtained, if additive concentrations are maintained in the ranges as given below:
•Jf>

Compositon-1: General Composition of Soluble Cutting Oil

S.No. Components Composition in % wt.
1. Spindle oil 70-90
2. Heavy alkyl benzene 1-5
3. Oleic acid 2-12
4. Sodium Sulphonate 4-10
5. Triethanolamine 2-12
6. Sorbitan mono oleate 1-15
7. Aqualox 232 0.5-5
8. Lauryl alcohol 0.5-5
9. Triazene Derivative 0.5-4
10. Tween 85 0.1-2.5
11. Tween 80 0.1-2.5
12. Water 0.5-5.0
13. KOH/NaOH Solution (30 to 60% solution in distilled water) 0.1-5.5
14. Deodorant 0.1-0.9
However, a high quality cutting oil meeting all the performance properties and also the BIS soluble cutting oil specification IS 1115 is obtained when additives concentrations are in the further narrow range as given below:
Compositon-2 : Composition of Soluble Cutting Oil

S.No. Components Composition in % wt.
1. Spindle oil 75- 85
2. Heavy alkyl benzene 0-2
3. Oleic acid 3-8
4. Sodium Sulphonate 4-8
5. Triethanolamine 2-7.5
6. Sorbitan mono oleate 2.1-9.5
7. Aqualox 232 0.0-1.5
8. Lauryl alcohol 0.5-3.2
9. Triazene Derivative 0.5-2.7
10. Tween 85 0.0-1.5
11. Tween 80 0.0-1.5
12. Water 0.5-3.5
13. KOH/NaOH Solution (30 to 60% solution in distilled water) 0.1-3.5
14. Deodorant 0.1-0.9
Soluble cutting oil thus obtained is meeting the requirements of IS 1115 specification for soluble cutting oils and also it is superior in bio-stability test conducted as per ISO/DTR 12927: 1995(E) test method when compared to commercially available soluble cutting oils. It has resistance to 700ppm or more hardness of water also.

As discussed earlier, in order to get ease of blending of soluble cutting oil. Soluble cutting oil composition was developed from this composition by minimizing the base oil and increasing the concentrate proportionately. A suitable package for making soluble cutting oil has following composition.
Compositon-3 : Composition of Soluble Cutting Oil Additive

S.No. Components Composition in % wt.
1. Spindle oil 5-25
2. Heavy alkyl benzene 0-8
3. Oleic acid 12-32
4. Sodium Sulphonate 16-32
5. Triethanolamine 8.0-30.0
6. Sorbitan mono oleate 8.4-38.0
7. Aqualox 232 0.0-6.0
8. Lauryl alcohol 2.0-12.8
9. Triazene Derivative 2.0-10.8
10. Tween 85 0.0-6.0
11. Tween 80 0.0-6.0
12. Water 2.0-14.0
13. KOH/NaOH Solution (30 to 60% solution in distilled water) 0.4-14.0 .
14. Deodorant 0.4-3.6
The procedure for making package is different from that for the soluble cutting oil Dreparation. The components were mixed for prolonged duration to homogenize the nixture. During the process temperature was maintained at 35 deg.C. to 60 deg.C. Once a homogeneous package is obtained it is mixed in base oil in the concentration range of 18 % to 40% to give various quality of soluble cutting oils. Package can be prepared at lab scale as well as commercial scale. The performance of cutting oil so obtained was excellent and meet all the specification requirements. Results are given in Example-15.
Example-15
Base oil was heated to around 40 deg.C. and to this Soluble Cutting Oil Package as per Composition -3 was added slowly as per the required concentration and allow to mix for 2-3 hours to give a soluble cutting oil meeting performance tests as well as tests as per IS 1115 specification requirements and also passing in bio-stability test for four weeks.
#22-

Compositon-2: Composition of Soluble Cutting Oil

S.No. Components Composition in % wt
1. Spindle oil 75-85
2. Heavy alkyl benzene 0-2
3. Oleic acid 3-8
4. Sodium petroleum sulphonate 4-8
5. Triethanolamine 2-7.5
6. Sorbitan mono oleate 2.1-9.5
7. Aqualox 232 0.0-1.5
8. Lauryl alcohol 0.5-3.2
9. Triazene Derivative 0.5-2.7
10. Tween 85 0.0-1.5
11. Tween 80 0.0-1.5
12. Water 0.5-3.5
13. KOH/NaOH Solution (30 to 60% solution in distilled water) 0.1-3.5
14. Deodorant 0.1-0.9
Soluble cutting oil thus obtained is meeting the requirements of IS 1115 specification for soluble cutting oils and also it is superior in bio-stability test conducted as per ISO/DTR 12927: 1995(E) test method when compared to commercially available soluble cutting oils. It has resistance to 700ppm or more hardness of water also.
As discussed earlier, in order to get ease of blending of soluble cutting oil. Soluble cutting oil composition was developed from this composition by minimizing the base oil and increasing the concentrate proportionately. A suitable package for making soluble cutting oil has following composition.
Compositon-3 : Composition of Soluble Cutting Oil

S.No. Components Composition in % wt.
1. Spindle oil 5-25
2. Heavy alkyl benzene 0-8
3. Oleic acid 12-32
4. Sodium Sulphonate 16-32
5. Triethanolamine 8.0-30.0
6. Sorbitan mono oleate 8.4-38.0
7. Aqualox 232 0.0-6.0
8. Lauryl alcohol 2.0-12.8
9. Triazene Derivative 2.0-10.8

We claim:
1. A soluble cutting oil composition comprising a high viscosity index (HVl) base oil 5-90% by wt, amine oleate 3-60% by wt, heavy alkyl benzene 0-8% by wt, biocide 0.5-10.8% by wt, co-solvent 0.5-12.8% by wt, deodorant 0.1-3.6%by wt, sodium petroleum sulphonate 4-32% by wt, non-ionic emulsifier 0-38.0% by wt, corrosion inhibitor 0-8% by wt, optionally / sodium oleate or potassium oleate, and water for metal working applications.
2. A soluble cutting oil composition as claimed in cJaim 1, wherein the amine oleate is prepared by reacting alkanolamine and fatty acid in situ.
3. A soluble cutting oil composition as claimed in claim 2 wherein the alkanolamine is selected from diethanol amine, monoethanol amine and tri ethanol amine, preferably tri ethanol amine.
4. A soluble cutting oil composition as claimed in claim 2, wherein fatty acid is oleic acid.
5. A soluble cutting oil composition as claimed in claim 1, wherein co-solvent is preferably lauryl alcohol.
6. A soluble cutting oil composition as claimed in claim 1, wherein the non-ionic emulsifier is selected from sorbitan monooleate, Tween 80 (Polyoxyethylene sorbitan monooleate) and Tween 85 (Polyoxyethylene sorbitan trioleate), preferably sorbitan monooleate.

7. A soluble cutting oil composition as claimed in claim 1, wherein the biocide is triazine derivative.
8. A soluble cutting oil composition as claimed in claim 1, wherein deodorant is selected from pine oil, eucalyptus oil or phenol preferably pine oil.
9. A soluble cutting oil composition as claimed in claim 1, wherein the
preferred concentration of base oil is 70 to 85% by wt, heavy alkyl
benzene concentration is 0 to 2.0 % by wt, concentration of amine oleate
is 4 to 15.5% by wt, concentration of sodium petroleum sulphonate is 4.0
to 8.0% by wt, concentration of non-ionic emulsifier is 0 to 9.5% by wt,
concentration of lauryl alcohol is 0.5 to 3.2% by wt, concentration of

triazine derivative type biocide is 0.5 to 2.7% by wt, concentration of Aqualox 232 additive is 0 to 1.5% by wt, concentration of deodorant is 0.1 to 0.9% by wt and concentration of potassium oleate is 3.0 to 18.8% by wt., and concentration of water in the final composition is 0.5 to 3.5% by wt respectively.
10. A soluble cutting oil composition as claimed in claim 1, wherein the preferred concentration of base oil is 5 to 25% by wt, heavy alkyl benzene concentration is 0 to 8.0 % by wt, concentration of amine oleate is 12 to 39.5% by wt, concentration of sodium petroleum sulphonate is 16.0 to 32.0% by wt, concentration of non-ionic emulsifier is 0 to 38.0% by wt, concentration of iauryl alcohol is 2.0 to 12.8% by wt, concentration of triazine derivative type biocide is 2.0 to 10.8% by wt, concentration of Aqualox 232 additive is 0 to 6.0% by wt, concentration of deodorant is 0.4 to 3.6% by wt and concentration of potassium oleate is 12.0 to 40.4% by wt., and concentration of water in the final composition is 2.0 to 14.0% by wt respectively.
11. A soluble cutting oil composition as herein described in claim 12 and claim 13 and with reference to the examples.

12.A soluble cutting oil composition substantially as herein described with reference to the foregoing examples.
Dated this 24th day of February, 2004