Abstract: The present invention provides a new biodegradable base stock composition based on nonedible seed oil Jatropha, Pongamia, Salvadora, Mahua. High performance neat cutting oil resulted from Pongamia oil ester exhibited excellent oxidation stability, excellent load bearing and antiwear properties, along with corrosion inhibiting characteristics, higher flash point , reduced ash content, and low TAN. The neat cutting oil so developed is a new potential candidate, for cutting operations under lubricated conditions, for single point and multi point cutting operations and a replacement for currently being used mineral based products which are toxic and non-biodegradable. The invention base oil meets specified properties as such for Neat cutting oil, IS: 3065-1985 (Non Staining, Type II Grade I & Grade II).
FIELD OF THE INVENTION
The present invention relates to biodegradable base stock as neat cutting oil.
Particularly, the present invention provides a biodegradable base stock
composition based on non-edible seed oil Jatropha, Pongamia (Karanja) ,
Salvadora, Mahua. High performance neat cutting oil resulted from Pongamia
(karanja) oil ester exhibited excellent oxidation stability, excellent load bearing
and antiwear properties, along with corrosion inhibiting characteristics. Higher
flash point and reduced ash content, and Total Acid Number (TAN) are also
reported. More particularly, present invention relates to a process for the
development of biodegradable base stock as neat cutting oil useful in modern
day cutting operations of turning, milling, drilling and tapping.
BACKGROUND OF THE INVENTION
Machining processes have a distinct, remarkable impact in the manufacturing
industry. The cost effectiveness of machining processes is a function of
parameters associated with machining operations viz. cutting speed, feed rate
and depth along with appropriate selection of cutting tools, work piece material
and the cutting fluid combination. During the machining process, friction
between work piece cutting tool and cutting tool-chip interfaces cause high
temperature on cutting tool. The effect of this generated heat decreases tool
life, increases surface roughness and decreases the dimensional sensitiveness
of work material. The cutting oil at the interface acts as a lubricant minimizing
the friction between the tool- work piece interface and reducing the
wear of the tool; dispensing medium - carry away the frictional heat from the
tool - work piece interface thereby protecting the tool and work piece surface
from the thermal distress; and finally cleaning medium: carry away chip and
debris away from the interface and allowing desired length of the chips. The
most significant task performed by the cutting oil is that of lubrication. The
cutting oil penetrates into the chip tool contact area and reduces the contact
length and decreases the forces, heat generation, temperatures and tool wear.
Its ability to improve surface finish is attributed to the fact that it can lubricate
the rake face and avoid formation of built-up edge by minimizing adherence.
Most of the conventional cutting oils in use are mineral based and blended with
chemical compounds in the form of additives imparting desired characteristic
properties to the cutting oil. The mineral based cutting oils are costly due to
the petroleum origin. These products are poor in environment friendliness and
are not bio-degradable. Moreover the used of additive package imparts toxicity
to the product thereby proving them to be carcinogenic in many of the cases.
Bio-based cutting oil derived from the non-edible oils can prove best
replacement to the mineral based cutting oils with improved friction and wear
behavior. It is in this context neat cutting oil is invented based on the nonedible
karanj oil ester. The composition of vegetable oil can be exploited for use
as a base stock for neat cutting oil formulation.
Reference may be made to US patent No. 1,367,428 by Pressell et aI, wherein a
base for the metal cutting compounds and process of preparing the same has
been reported. The product can be used either in the form of a concentrated
base or mixed in proportions with a mineral oil to be used as cutting oil. The
ingredients comprise of wool fat (distilled wool grease), sulfur, lard oil and
paraffin oil mixed together and brought to a temperature of approximately
350°F, at which temperature the sulfur completely dissolves and combines
with the other constituents. The oleaginous product cools the metal and
conduces to a clean cut and lengthens the life of the cutting tool.
Reference may be made to the US patent No. 2,388,439 by Raymond et aI,
wherein cutting oil consisting principally of mineral oil, naphthenic acid and
small proportion of metallic naphthenate dissolved or colloid ally dispersed.
The invention provides a highly effective lubricating and protective film on both
the work and the tool and does not require the use of animal or vegetable oil or
the addition of sulphur.
Reference may be made to the US patent No. 2,393,927 by Myers et aI, wherein
cutting oil compositions consisting essentially of mineral oil but characterized
by their ability to emulsify with water. The cutting oil base consisting of rosin
soap of an alkali metal and a fatty acid mono ester of a poly or dihydric alcohol
is capable of giving desired results. A typical cutting oil base of the invention
consists of potassium rosin soap (45 parts by weight), glyceryl mono oleate (35
parts by weight), red oil soap (5 parts by weight) and water (7.5%).
Reference may be made to the US patent No. 2,406,671 by Diamond et aI,
wherein cutting oil with foam reducing additives is exemplified by soluble
cutting oils which contain emulsifying agents and which spontaneously
emulsify when diluted with water. The foam inhibiting characteristics are
achieved with the use of saturated alkyl silicon oxides or esters. For the said
purpose those silicones in which the two R's are of about the same molecular
weight and particularly those in which each R is a saturated alkyl radical
containing about 14 to 24 carbon atom are preferred. Illustrative examples are
tetra decyl, pentadecyl, hexadecyl, heptadecyl, Octadecyl, nonadecyl, eicosyl,
heneicosyl, docosyl, tricosyl, tetracosyl and the like.
Reference may be made to the US patent No. 2,421,159 by Myers et aI, wherein
the cutting oil bases to be added to ordinary mineral oils to endow them with
emulsifying characteristics. The cutting oil base essentially consists of rosin
soap of an alkali metal and a fatty acid monoester of a poly or dihydric alcohol.
The preferred cutting oil base contain from 40-50 parts by weight of a rosin
soap such as potash rosin soap, 30-40 parts by weight of a monoester of a fatty
acid containing 16-18 carbon atoms in chain length with a di or polyhydric
alcohol, for example glyceryl monooleate, a small quantity up to 5 parts of an
alkali metal soap of oleic acid such as potassium oleate and small quantities of
water approximately 5-10 parts by weight thereof.
Reference may be made to the US patent No. 2,466,645 by Myers et aI, wherein
cutting oil composition, consisting essentially of mineral oil but characterized
by their ability to emulsify with water. The cutting oil base essentially consists
of rosin soap of an alkali metal and a fatty acid monoester of a poly or dihydric
alcohol. A typical base of the invention consists of substantially 1 part of fatty
acid mono ester to each 1 to 2 parts of rosin soap. A typical cutting oil base of
the invention consists of potassium rosin soap (45 parts by weight), glyceryl
mono oleate (35 parts by weight), red oil soap (5 parts by weight) and water
(7.5%).
Reference may be made to the US patent No. 2,673,183 by Hughes et aI,
wherein novel neutralized, oxidized oil suitable for use as a cutting oil or as an
additive to a cutting oil base stock and to a process of preparing the same. The
composition of the said oil is obtained by first oxidizing refined oil and then
neutralizing it with a strong base. The neutralized oil is then treated with
elemental sulfur to affect a solution of sulfur in the oil.
Reference may be made to the US patent No. 2,790,772 by Hughes et aI,
wherein cutting oil concentrate characterized by a combination of superior
cutting ability and absence of the formation of disagreeable odors when in use.
The method of invention comprises reacting one or more alkylbenzyl halides
containing ten carbon atoms and therefore including trimethyl-, methyl-ethyl-,
proply- and isopropylbenzyl halides with an excess of alkali-metal polysulfide
and elemental sulfur at an elevated temperature. These polysulfides are highly
useful as cutting oil concentrates but are then preferably reacted with
elemental sulfur to form alkyl-substituted benzyl polysulfides containing an
average of between four and five and preferably close to five sulfur atoms per
molecule.
Reference may be made to the US patent No. 2,918,432 by Feng et aI, wherein
transparent cutting oil having superior performance characteristics by virtue of
the presence of a highly effective additive. The cutting oil essentially consists of
transparent lubricating oil and monochloro-phenyl dimethyl phosphorothionate
(0.5 to 15 percent by weight). The phosphorus additive in actual cutting
operations imparts greatly superior performance characteristics to the base oil.
The base oil is preferably mineral lubricating oil (naphthenic).
Reference may be made to the US patent No. 3,799,875 by Rohde et aI, wherein
cutting oil composition of improved high load performance of a hydrogenated
butadiene/styrene copolymer to a conventional cutting oil formulation. The
composition of the invention consists of (i) a mineral base oil, (ii) a
hydrogenated butadiene / styrene copolymer, (iii)a sulfur-containing
multifunctional additive, and (iv)a chlorine-containing multifunctional additive.
The mineral oil base stock amounts to about 99.9 - 72 weight percent of the
total mix. The hydrogenated butadiene/styrene copolymer contains sulfur
containing multifunctional additive as essential ingredients.
Reference may be made to the US patent No. 3,919,098 by Altgelt et al wherein
metal working fluid composition having improved low fog properties. The
composition comprises of a major portion of hydrocarbon oil and a minor
amount of an antifog additive selected from polyisobutene, poly-n-butene and
mixtures thereof, and having molecular weight in the range of 0.3 to 10 million.
The cutting oil can comprise a mineral oil or synthetic hydrocarbon oil with the
viscosity ranging from 50 to 500 SUS at 38°C. In addition to the polybutene
antifog agent, other additives may be present within the cutting oil
composition.
Reference may be made to the US patent No. 3,929,652 by Seni et aI, wherein
a dual purpose cutting oil which serves as a heavy duty cutting oil and a
machine lubricant. The oil comprises a base oil, an extreme pressure agent
comprising primarily Bis (f3-chlorophenethyl) disulfine afld a C01Jper eurrosion
inhibitor comprising an alkyl derivative of 2,5-di-mercapto 1, 3, 4-thiadiazole.
The base oil is a paraffinic oil of the form about 100 to 170 SUS/100 0 F
viscosities.
Reference may be made to the US patent No. 4,210,544 by Burton et aI,
wherein a dual purpose cutting oil which serves as heavy duty cutting oil and
machine lubricant in automatic screw machines. The oil comprises of a base
oil, extreme pressure agents (primarily a di-tertiary alkyl polysulfide),
chlorinated paraffin, and a copper corrosion inhibitor comprising a sulfur
scavenger such as a 2, 5-bis (n-alkyldithio)-thiadiazole. The base oil is low
dielectric constant oil which is inert to the additives essentially a paraffinic or
intermediate base mineral oil.
Reference may be made to the US patent No. 4,416,788 by Apikos, wherein an
improved transparent lubricating oil composition useful as high severity metal
cutting oil. The composition comprises a major amount of mineral/ synthetic oil
and a minor effective amount of at least one sulfur-containing compound and
sulfur. The combination of sulfur-containing compounds and elemental sulfur
is present in an amount effective to improve the extreme pressure properties of
the composition. The composition is applicable when the lubricating oil
contains at least about 30% by weight, more preferably, at least about 40% by
weight, of substantially paraffinic hydrocarbons.
Reference may be made to the US patent No. 5,534,172 by Perry et aI, wherein
an aqueous-based cutting fluid for machining photoreceptor substrates
consisting of: (a) at least one antioxidant, (b) one or more surfactants, at least
one of which is a polysiloxane surfactant, (c) at least one lubricant and (d)
water. The cutting fluid exhibits excellent water-break properties and is
environmentally safe, non-toxic and biodegradable. Furthermore, it poses no
fire risk, provides a uniform coverage of a transparent protective coating
allowing inspection of the machined part and excellent lubricity. The
antioxidant preferably is an amine or carboxylic acid salt, most preferably the
triethanolamine. The surfactant can be a mixture of one or more surfactants
preferably polysiloxane compound having an HLB of 14 to 16. The additional
surfactant used IS preferably octylphenoxy polyethoxy ethanol,
propyleneoxide/ ethyleneoxide copolymer or polyoxyethylene glycol sorbitant
monolaurate. The lubricant preferably IS a polyhydric alcohol including
dihydric alcohols, e.g, glycol such as ethylene glycol, propylene glycol, trimethylene
glycol, and neopentyl glycol.
Reference may be made to the US patent No. 6,448,207 B1 by Fukutani et aI,
wherein a metal working fluid, having excellent properties, contains a metal
stearate, a carbonate, a hydrogencarbonate, and a surfactant. The metal
working fluid may further contain ethyleneglycol and a rust inhibitor. More
particularly, the invention relates to a water soluble metal-working fluid, which
can be used as a substitute for cutting oil. The composition is environmentfriendly
and possesses excellent lubricity and cooling properties.
Reference may be made to the US patent No. 2008/0026967 Al by Suda et aI,
wherein metal working fluid comprising of an ester oil and a hydrocarbon oil
with a kinematic viscosity of 1-20 mm2/s at 40°C. The hydrocarbon oil is
preferably one or more types selected from among white oils and polyolefins or
their hydrogenated forms. Another composition for the metal working fluid
employs ester oil as the base oil and has a moisture content of 200-20000ppm.
Both the compositions of the metal working fluid have excellent properties as
water insoluble oils for non-ferrous metal working and as oils for cutting and
grinding in a minimum quantity lubrication system, and can therefore achieve
improved working efficiency and extended tool life.
Reference may be made to the US patent No. 2009/0018039 Al by Goto et aI,
wherein a metal working oil composition which is used for a very small
amount of oil-feeding type metal working methods compnsmg a base oil
selected from the group consisting of natural fats, derivatives thereof and
synthetic ester oils, and a phospholipid. The metal working oil composition has
good lubricating properties and is suitable for processing metallic materials
such as cast irons, steel, stainless steel and the like by the very small amount
of oil-feeding type metal working method. The phospholipid comprises at least
one selected from the group consisting of egg-yolk lecithin, soybean lecithin
and the like. The phospholipid contains a mixture of phosphatidylcholine,
phosphatidylethanolamine and phosphatidylinositol.
Reference may be made to the US patent No. 2010/0077817 Al by Goto et aI,
wherein metal working fluid composition which comprises a morpholine
compound and an isothiazoline compound and a metal working method which
makes use of the metal working fluid composition. The composition relates to a
water soluble metal working fluid which is excellent in antiseptic properties
and can widely be applied to metal working techniques such as cutting,
grinding, form rolling, press working and plastic working techniques.
From the patent search it can be concluded that, hither to, no literature
information is available on neat cutting oil formulation having non-edible seed
oil Jatropha, Salvadora, Mohua & Pongamia oil as base oil which is
biodegradable, have been used as neat cutting oil base stock.
OBJECTIVE OF THE INVENTION
Main object of the present invention is to provide biodegradable base stock as
neat cutting oil using nonedible seed oils.
Another object of the present invention is to provide a method for the synthesis
of new biodegradable base stock as neat cutting oil for cutting operations in
manufacturing sector.
Still another objective of the present invention is to utilize the non-edible
vegetable oil as starting material in place of conventional mineral oil which is
toxic and non- biodegradable.
Yet another objective of the present invention is to synthesize a product that
reduces tool wear and the friction between the tools - work piece interface
when compared to or better than the existing conventional mineral oil base
cutting oil.
Still another objective of the present invention is to make use of the same base
stock for the turning, facing, milling, drilling and tapping operations.
Yet another objective of the present invention is to synthesize eco friendly neat
cutting oil with renewable base meeting the requirements of International
specifications for cutting oils.
SUMMARY OF THE INVENTION
Accordingly, present invention provides a process for preparation of
biodegradable base stock comprising the steps of:
1. refluxing non-edible oil with alcoholic NaOH for a period in the
range of 3 to 7 h at temperature in the range of 80 to 85°C to
obtain saponified mixture;
11. cooling the saponified mixture as obtained In step (i) at
temperature in the range of 20 to 30°C followed by acidifying with
HCI to pH 2 to 3 to obtain CI2-CIS carbon range fatty acid mixture;
111. esterifying the fatty acid mixture as obtained in step (ii) with
alcohol (CIS) in the ratio of 1: 1 in the presence of 20-30% catalyst
at a maximum operating temperature of 150°C and solvent,
followed by stirring, refluxing to obtain 76 to 98% neat cutting oil
composition.
In an embodiment of the present invention, non edible oil is selected from the
group consisting of Jatropha, Karanja, Mahua or Salvadora preferably karanja
oil.
In another embodiment of the present invention, alcohol used is selected from
saturated streyl alcohol and unsaturated oleyl alcohol.
In yet another embodiment of the present invention, catalyst used is a cationic
ion exchange resin of macro porous cross linked poly styrene.
In yet another embodiment of the present invention, solvent used IS selected
from toluene or xylene.
In yet another embodiment of the present invention, alcoholic NaOH preferable
may be solution of NaOH and Isopropyl alcohol.
In yet another embodiment, present invention provides an ecofriendly
biodegradable base stock as neat cutting oil prepared by the process as
claimed in claim 1 having the following characteristics:
1. Biodegradable as per ASTM D-5864-95
11. viscosity of 15.90 CSt at 40°C;
lll. Ash % by mass is 0.014;
IV. acid value 0.20mgKOHj gm;
v. flash point 2040C, copper strip corrosion <1;
VI. wear scar diameter 0.62 mm and load bearing capacity greater
than 145Kgf.
In yet another embodiment of the present invention, said base stock is useful
for the modern day manufacturing (metal cutting) operations of turning,
milling, drilling and tapping, where the cutting oil performs the function of
cleaning and dispensing along with the cooling characteristics.
DETAIL DISCRIPTION OF THE INVENTION
Cutting oil is a new potential candidate, for cutting operations under
lubricated conditions, for single point and multi point cutting operations and a
replacement for currently being used mineral based products which are toxic
and non-biodegradable.
Present invention provides a method for the development of ecofriendly
biodegradable base stock as neat cutting oil which comprises sponification of
non edible oils by refluxing with 1.1 M alcoholic (isopropoyl) NaOH for a
duration of 3-7 hrs depending upon the oil used, the said saponified mixture is
cooled down at room temperature i.e.20 to 30°C, acidified with O.IN HCI to pH2
of mixture. Fatty acids precipitated out of the solution, washed 2-4 times
with cold water.
The acid value of the fatty acid mixture (202-214mgKOHjg) was determined to
check the complete conversion of the vegetable oils to fatty acid mixture.
The said fatty acids mixture (carbon range of CI2-CI8) is esterified with one
mole of CI8 saturated (streyl alcohol) & unsaturated (oleyl alcohol) alcohol in
presence of ion exchange resin catalyst, a cationic ion exchange resin of macro
porous cross linked poly styrene (H+ ion 4.8 minimum dry) at a maximum
operating temperature of 150aC in presence of 200 ml azeotropic solvent such
as toluene or xylene, the said contents are stirred and refluxed, water is
collected as against a 100% (theoretical) up to 6 hrs. After the removal of water
the contents cooled, filtered and solvent (toluene, xylene) recovered. The yield
of the product was 76.4-98% depending on the oil used.
Non edible oils used are selected from Jatropha oil, Karanja oil, Mahua oil,
Salvadora oil.
Neat cutting oil of the present invention is useful for the modern day
manufacturing (metal cutting) operations of turning, milling, drilling and
tapping, where the cutting oil performs the function of cleaning and dispensing
along with the cooling characteristics.
Base Stock meets specified properties as such for Neat cutting oil, IS: 30651985
(Non Staining, Type II Grade I & Grade II). The product has excellent load
bearing capacity.
Base Stock obtained by this invention can be used as neat cutting oil which is
completely eco friendly, biodegradable as per ASTM D 5864-95 method where
as hitherto conventional mineral based neat and soluble cutting oils are not
biodegradable.
EXAMPLES
The following examples are gIven by way of illustration and therefore should
not be construed to limit the scope of present invention.
EXAMPLE 1
100 gms Jatropha oil was saponified by refluxing with alcoholic (Isopropoyl)
NaOH (1.1 M) for 5 hrs at 820C. The saponified mixture was cooled to room
temperature i.e. 200C, acidified with O.IN HCI to pH-2, Fatty acids precipitated
out of the solution, washed 3 times with cold water. Acid value of the fatty acid
mixture is 214mgKOHjg. (- 90 gms fatty acid mixture).
282gms of Jatropha fatty acid (1 mole) was esterified with 284gms of saturated
alcohol ( Steryl alcohol, CIS, 1 mole) in presence of 20wt% of macro porous
cross linked poly styrene (H+ ion 4.8 minimum dry) at 150°C maximum
operating temperature and 200 ml toluene. The contents were stirred by a
mechanical stirrer and refluxed at 111°C. Only 70% of water was collected as
against a 100% (theoretical) up to 6 hrs. After the removal of water the
contents were cooled, filtered and 190 ml of toluene was recovered with the
conversion of 76.4% only.
Example 2
Esterification was repeated under identical conditions as In example-l except
increasing the catalyst to 25 wt%. The reaction was complete in 4 hours by
collecting 100% of experimental water (theoretical) 195 ml of solvent (toluene)
recovered with the conversion of 98% to bioester. The performance evaluation
of the product has a load bearing capacity WL 172 kgf (kilogram-force) and
wear scar diameter (WSD) of 0.72 mm.
Example 3
Example-2 was repeated under identical conditions except increasing the
catalyst to 30 wt%. The reaction was complete in 4 hours by collecting 100% of
experimental water (theoretical) 195 ml of solvent (toluene) recovered with the
conversion of 98% to bioester.
Example 4
Example-2 was repeated under identical conditions except using oleyl alcohol
(282 gms,lmol.) The reaction was complete in 4 hours by collecting 100% of
experimental water (theoretical) 195 ml of solvent (toluene) recovered with the
conversion of 98% to bioester. The performance evaluation of the product has a
load bearing capacity WL 170 kgf (kilogram-force) and wear scar diameter
(WSD) of 0.62 mm.
EXAMPLES
100 gms Mahua oil was saponified by refluxing with alcoholic (Isopropoyl)
NaOH (1.1 M) for 5 hrs at 80°C. The saponified mixture was cooled to room
temperature i.e. 25°C, acidified with O.lm HCI to pH-2, Fatty acids precipitated
out of the solution, washed 3 times with cold water. Acid value of the fatty acid
mixture is 205mgKOH/g. (~ 90 gms fatty acid mixture).
284gms of Mahua fatty acid (1 mole) was esterified with 284 gms of saturated
alcohol (CI8, 1 mole) in presence of 25wt% cationic ion exchange resin of macro
porous cross linked poly styrene (H+ ion 4.8 minimum dry) at 150aC maximum
operating temperature and 200 ml toluene. The contents were stirred by a
mechanical stirrer and refluxed at 111°C The reaction was complete in 4 hours
by collecting 100% of experimental water (theoretical) 195 ml of solvent
(toluene) recovered with the conversion of 98% to bioester. The performance
evaluation of the product has a load bearing capacity WL 160 kgf (kilogramforce)
and wear scar diameter (WSD) of 0.62 mm.
Example 6
Esterification was repeated under identical conditions as In example-5 except
using oleyl alcohol.The product after usual work up gives bioester comprising
22.4 to 36.8 w/w % palmitic acid esters, 18.6 to 24.0 w/w % stearic acid
esters, 1.23 w/w % arachidic acid esters, 32.0 to 38.0 w/w % oleic acid esters
and 14.0 to 18.0 w/w % linoleic and traces of linolenic acid esters of oleyl
alcohol. The performance evaluation of the product has a load bearing capacity
WL 170 kgf (kilogram-force) and wear scar diameter (WSD) of 0.74 mm.
EXAMPLE 7
100 gms Salvadora oil was saponified by refluxing with alcoholic (Isopropoyl)
NaOH (1.1 M) for 5 hrs at 850C. The saponified mixture was cooled to room
temperature i.e. 200C, acidified with O.lm HCI to pH-2, Fatty acids precipitated
out of the solution, washed 3 times with cold water. Acid value of the fatty acid
mixture is 205mgKOH/g. (- 90 gms fatty acid mixture).
228gms of salvadora fatty acid (1 mole) was esterified with 284 gms of
saturated steryl alcohol (CI8, 1 mole) in presence of 25wt% cationic ion
exchange resin of macro porous cross linked poly styrene (H+ ion 4.8 minimum
dry) at 150aC maximum operating temperature and 200 ml toluene. The
reaction was complete in 4 hours by collecting 100% of experimental water
(theoretical) 195 ml of solvent (toluene) recovered with the conversion of 95% to
bioester. The contents were stirred by a mechanical stirrer and refluxed at
111°C. The performance evaluation of the product has a load bearing capacity
WL 160 kgf (kilogram-force) and wear scar diameter (WSD) of 0.56 mm.
Example 8
Esterification was repeated under identical conditions as In example-7 except
using oleyl alcohol.The product after usual work up gives bioester comprising
35.6 to 49.6 w/w % lauric acid esters, 26.4 to 50.8 w/w % myristic acid esters,
5.0 to 8.3 w/w % stearic acid esters, -2.0 w/w % oleic acid esters of oleyl
alcohol. The performance evaluation of the product has a load bearing capacity
WL 170 kgf (kilogram-force) and wear scar diameter (WSD) of 0.49 mm.
EXAMPLE 9
100 gms Karanja oil (Purchased from M/s Amrut Industrial Products, Anand
Bhawan, Princess Street, Mumbai-400002) was saponified by refluxing with
alcoholic (Isopropoyl) NaOH (1.1 M) for 5 hrs at 850C. The saponified mixture
was cooled to room temperature i.e. 22°C, acidified with O.lm HCI to pH-2,
Fatty acids precipitated out of the solution, washed 3 times with cold water.
Acid value of the fatty acid mixture IS 213mgKOH/g. (- 90 gms fatty acid
mixture).
280gms of karanja fatty acids (1 mole) was esterified with 284 gms of saturated
alcohol 1-0ctadecanollSteryl alcohol (C 18, 1 mole) in presence of 25wt%
cationic ion exchange resin of macro porous cross linked poly styrene (H+ ion
4.8 minimum dry) at 150aC maximum operating temperature and 200 ml
toluene. The contents were stirred by a mechanical stirrer and refluxed at
111°C. The reaction was complete in 6 hours by collecting 100% of
experimental water (theoretical) 195 ml of solvent (toluene) recovered with the
conversion of 97% to bioester. The performance evaluation of the product has
a load bearing capacity WL 170 kgf (kilogram-force) and wear scar diameter
(WSD) of 0.82 mm.
Example 10
280gms of karanja fatty acids (1 mole) was esterified with 282 gms of
unsaturated alcohol oleyl alcohol (CI8:1, 1 mole) in presence of 25wt% cationic
ion exchange resin of macro porous cross linked poly styrene (H+ ion 4.8
minimum dry) at 150aC maximum operating temperature and 200 ml toluene.
The contents were stirred by a mechanical stirrer and refluxed at 111°C. The
reaction was complete in 6 hours by collecting 100% of experimental water
(theoretical) 190 ml of solvent (toluene) recovered with the conversion of 97% to
bioester. Base oill bioester. The performance evaluation of the product has a
load bearing capacity WL 145 kgf (kilogram-force) and wear scar diameter
(WSD) of 0.62 mm.
Example 11
Example 10 was repeated under identical conditions except increasing the
reaction temperature to 138°C as xylene was used as solvent. The reaction was
complete in 4hrs and yield observed was 98%. On increasing reaction
temperature the reaction time and yield almost remains same. The
performance evaluation of the Base oil/ bioester has a load bearing capacity
WL 145 kgf, wear scar diameter (WSD) of 0.62 mm.
EXAMPLE 12
Example-10 was repeated under identical conditions for the synthesis of bulk
quantity of base oil(4Kg) for the performance evaluation of the base oil.
The performance characteristics of synthesized biolube as in example 10 are
given in Table 1.
SI. Characteristic Test Method Observations
No. s Synthesized Commercia Commercia
Ester 1 Oil A 1 Oil B
1. Wear (Four ASTM D- Avg. WSD Avg. WSD Avg. WSD
Ball Method) 2266 (Wear Scar (Wear Scar (Wear Scar
diameter)= diameter)= diameter)=
0.62 mm 0.89 mm 0.92 mm
2. E.P (Extreme IP - 239 Weld Load Weld Load Weld Load =
Pressure) (load bearing = 160 kgf 140 kgf
(Four Ball capacity) =
Method) 145 kgf
3. A. cidity . IS: 1448 (P:2) 0.20 10.68 4.66
Inorgamc (mg
of KOH/g)
4. Ash, % by IS: 1448 (P:4) 0.014 1.75 1.07
mass (Max.)
5. Copper strip IS: 1448 < 1 No.1 No.1
corrosion for 3 (P: 15)
h at 100°C
6. Flash point DC, IS: 1448 204 172 140
(P:21)
7. Kinematic IS: 1448 15.90 36.98 42.99
viscosity, at (P:25)
40°C, cSt
8. Saponifiable IS: 1448 9.0 -- --
matter, % by (P:55)
mass (Min.)
9. Thermal IS: 1448 Shall Pass -- --
stability test (P: 100) the test
10. Reactive IP155j177 nil -- --
sulphur at
100°C, % by
mass
EXAMPLE-13
Example-10 was repeated under identical conditions. The catalyst was recycled
three times without loss of activity, only reaction time increased. In the fourth
recycle even after 8.0 hrs, the reaction was not complete and yield observed
was only 30%. The performance evaluation of the product has a load bearing
capacity WL 170 kgf and wear scar diameter (WSD) of 0.74mm.
ADVANTAGES OF THE INVENTION
It will be possible to replace conventional mineral oil based commercial cutting
oils by chemical transformation of non edible vegetable oils Jatropha, Karanja,
Mahua, Salvadora, to high performance long service life environment friendly
lubricants as neat cutting oil.
Vegetable oil based esters, Mahua and Karanja, have high viscosity index, low
freezing points and favorable viscosity-temperature characteristics
Synthesized esters have viscosity of 15.90 and 16.2 CSt at 40°C
Synthesized esters have flash point of 204 and 216°C matching the
specification.
Synthesized esters also pass the thermal stability and copper strip corrOSIOn
test.
Ash percentage was found to be nil.
Same product can be used for turning, milling, drilling and tapping operations
with negligible tool wear.
Synthesized product have a good antiwear properties, excellent load bearing
capacity, very good shelf life due to the improved oxidation stability observed
for a period of 28 days at 85±2°C, good potential for use as such for Neat
Cutting oil, IS: 3065-1985 (Non Staining, Type II Grade I & Grade II).
Product synthesized is a new potential candidate, for cutting operations under
lubricated conditions, for single point and multi point cutting operations and a
replacement for currently being used mineral based products which are toxic
and non-biodegradable as such for Neat cutting oil, IS: 3065-1985 (Non
Staining, Type II Grade I & Grade II).
We claim
1. A process for preparation of biodegradable base stock comprising the
steps of:
1. refluxing non-edible oil with alcoholic NaOH for a period in the
range of 3 to 7 h at temperature in the range of 80 to 85°C to
obtain saponified mixture;
11. cooling the saponified mixture as obtained In step (i) at
temperature in the range of 20 to 30DC followed by acidifying with
HCI to pH 2 to 3 to obtain CI2-CIS carbon range fatty acid mixture;
111. esterifying the fatty acid mixture as obtained in step (ii) with
alcohol (C IS) in the ratio of 1: 1 in the presence of 20-30% catalyst
at a maximum operating temperature of 150aC and solvent,
followed by stirring, refluxing to obtain 76 to 98% neat cutting oil
composition.
2. The process as claimed in claim 1, wherein non edible oil is selected from
the group consisting of Jatropha, Karanja, Mahua or Salvadora
preferably karanja oil.
3. The process as claimed in claim 1, wherein alcohol used is selected from
saturated streyl alcohol and unsaturated oleyl alcohol.
4. The process as claimed in claim 1, wherein catalyst used is a cationic ion
exchange resin of macro porous cross linked poly styrene.
5. The process as claimed in claim 1, wherein solvent used is selected from
toluene or xylene.
6. The process as claimed In claim 1, wherein alcoholic NaOH preferable
may be solution of NaOH and Isopropyl alcohol.
7. An ecofriendly biodegradable base stock as neat cutting oil prepared by
the process as claimed in claim 1 having the following characteristics:
1. Biodegradable as per ASTM D-5864-95
11. viscosity of 15.90 CSt at 40°C;
111. Ash % by mass is 0.014;
IV. acid value 0.20mgKOHjgm;
v. flash point 2040C, copper strip corrosion < 1;
VI. wear scar diameter 0.62 mm and load bearing capacity greater
than145Kgf.
8. The base stock as claimed in claim 7, wherein said base stock is useful
for the modern day manufacturing (metal cutting) operations of turning,
milling, drilling and tapping, where the cutting oil performs the function
of cleaning and dispensing along with the cooling characteristics.
| Section | Controller | Decision Date |
|---|---|---|
| # | Name | Date |
|---|---|---|
| 1 | 3483-del-2012-Form-5.pdf | 2013-08-20 |
| 1 | 3483-DEL-2012-IntimationOfGrant30-08-2022.pdf | 2022-08-30 |
| 2 | 3483-del-2012-Form-3.pdf | 2013-08-20 |
| 2 | 3483-DEL-2012-PatentCertificate30-08-2022.pdf | 2022-08-30 |
| 3 | 3483-DEL-2012-Written submissions and relevant documents [25-08-2022(online)].pdf | 2022-08-25 |
| 3 | 3483-del-2012-Form-2.pdf | 2013-08-20 |
| 4 | 3483-del-2012-Form-1.pdf | 2013-08-20 |
| 4 | 3483-DEL-2012-Correspondence to notify the Controller [23-08-2022(online)].pdf | 2022-08-23 |
| 5 | 3483-DEL-2012-US(14)-HearingNotice-(HearingDate-25-08-2022).pdf | 2022-08-04 |
| 5 | 3483-del-2012-Description(Provisional).pdf | 2013-08-20 |
| 6 | 3483-DEL-2012-NBA Approval Submission [11-01-2022(online)].pdf | 2022-01-11 |
| 6 | 3483-del-2012-Correspondence-others.pdf | 2013-08-20 |
| 7 | 3483-DEL-2012-FER_SER_REPLY [13-09-2018(online)].pdf | 2018-09-13 |
| 7 | 3483-del-2012-Abstract.pdf | 2013-08-20 |
| 8 | 3483-del-2012-Form-5-(07-11-2013).pdf | 2013-11-07 |
| 8 | 3483-DEL-2012-FER.pdf | 2018-03-28 |
| 9 | 3483-del-2012-Correspondence Others-(25-03-2015).pdf | 2015-03-25 |
| 9 | 3483-del-2012-Form-3-(07-11-2013).pdf | 2013-11-07 |
| 10 | 3483-del-2012-Form-18-(25-03-2015).pdf | 2015-03-25 |
| 10 | 3483-del-2012-Form-2-(07-11-2013).pdf | 2013-11-07 |
| 11 | 3483-del-2012-Correspondence Others-(07-11-2013).pdf | 2013-11-07 |
| 12 | 3483-del-2012-Form-18-(25-03-2015).pdf | 2015-03-25 |
| 12 | 3483-del-2012-Form-2-(07-11-2013).pdf | 2013-11-07 |
| 13 | 3483-del-2012-Correspondence Others-(25-03-2015).pdf | 2015-03-25 |
| 13 | 3483-del-2012-Form-3-(07-11-2013).pdf | 2013-11-07 |
| 14 | 3483-DEL-2012-FER.pdf | 2018-03-28 |
| 14 | 3483-del-2012-Form-5-(07-11-2013).pdf | 2013-11-07 |
| 15 | 3483-del-2012-Abstract.pdf | 2013-08-20 |
| 15 | 3483-DEL-2012-FER_SER_REPLY [13-09-2018(online)].pdf | 2018-09-13 |
| 16 | 3483-del-2012-Correspondence-others.pdf | 2013-08-20 |
| 16 | 3483-DEL-2012-NBA Approval Submission [11-01-2022(online)].pdf | 2022-01-11 |
| 17 | 3483-del-2012-Description(Provisional).pdf | 2013-08-20 |
| 17 | 3483-DEL-2012-US(14)-HearingNotice-(HearingDate-25-08-2022).pdf | 2022-08-04 |
| 18 | 3483-DEL-2012-Correspondence to notify the Controller [23-08-2022(online)].pdf | 2022-08-23 |
| 18 | 3483-del-2012-Form-1.pdf | 2013-08-20 |
| 19 | 3483-DEL-2012-Written submissions and relevant documents [25-08-2022(online)].pdf | 2022-08-25 |
| 19 | 3483-del-2012-Form-2.pdf | 2013-08-20 |
| 20 | 3483-DEL-2012-PatentCertificate30-08-2022.pdf | 2022-08-30 |
| 20 | 3483-del-2012-Form-3.pdf | 2013-08-20 |
| 21 | 3483-DEL-2012-IntimationOfGrant30-08-2022.pdf | 2022-08-30 |
| 21 | 3483-del-2012-Form-5.pdf | 2013-08-20 |
| 1 | 3484_DEL_2012patseersearch_21-03-2018.pdf |