Indian Patents. 215826:"A SYNERGISTIC FORMULATION USEFUL AS AN EXTREME PRESSURE ANTIWEAR AND ANTIFRICTION ADDITIVE FOR AN INDUSTRIAL GEAR OILS"

Title of Invention	"A SYNERGISTIC FORMULATION USEFUL AS AN EXTREME PRESSURE ANTIWEAR AND ANTIFRICTION ADDITIVE FOR AN INDUSTRIAL GEAR OILS"
Abstract	and karanjia oil; 0.25 to 0.5% by weight of phosphosulfurised hydrogenated cardanol; 0.25 to 0.5% of The present invention provides a synergistic formulation useful as an extreme pressure antiwear and antifriction additive for an industrial gear oils which comprises 0.25 to 0.5% by weight of sulfurised non traditional vegetable oils such as neem oil, mohwa oil dibenzyl disulfide by weight.

Full Text	The present invention relates to a formulation useful as an extreme pressure, antiwear and antifriction additive for industrial gear oils. The present invention particularly relates to a formulation consisting of sulfurised derivatives of Neem Oil and phosphosulfurised derivatives of hydrogenated cardanols with low corrosivity to copper which in a synergistic combination with dibenzyl di sulfide gives energy efficient industrial gear oils meeting U.S. Steel 224 specifications "" ' ^ when blended in SAE-90 gear lubricant base stock. The additive formulation of the present invention in 3-6% concentration in SAE-90 gear lubricant base stock gives welding load more than 300 Kg., wear scar diameters less than 0.4mm and co-efficient of friction less than 0.085, passes 12th stage of FZG gear rating without scoring and Timken O.K load more than 45 Kg. The copper corrosion at 4% concentration is in the range of 1 at 100°C for 3 hours without the addition of metal passivators. Organic sulfides, sulfurised fatty oils, sulfurised defines and alkyl aryl phosphorothibates as a class of compounds whether alone or in admixtures with each other are being extensively employed as extreme pressure (e.p.^ antiwear and antifriction additives. Extensive published information, papers and patents is available on the mode and mechanism of action of these additives and formulations for various types of gear oils and metal working oils over past thirty years. • The currently markete commercial formulations of additives for industrial as well as automotive gear oils mainly contain sulfurised defines, fatty esters and alkyl phosphorothioates. Some recent formulations contain small quantities of molybdenum derivatives also such as in energy efficient low friction gear oils. But none of the formulations have so far used sulfurised non traditional vegetable oils and phosphosulfurised naturally occuring alkyl phenols as additive components and formulations for energy efficient industrial gear oils which meet performance requirements of U.S Steel 224 specifications. 'Most of the sulfurised olefines and alkyl aryl phosphorothioates used in e.p. formulations have relatively high toxicity and low biodegradability. These products usually have high corrosivity towards copper which is supressed by use of metal passivators which in turn depress their performance characteristics too. The wear and extreme pressure characteristics are satisfactory but the friction co-efficients usually are not reduced which cause higher energy cosnumption. The main object of the present invention is to provide a formulation useful as an extreme pressure, antiwear and antifriction additive for industrial gear oils which obviates the draw backs as detailed above. Another object of the present invention is to use sulfurised and phosphosulfurised derivatives of non traditional vegetable oils and naturally occuring alkyl phenols as extreme pressure, antiwear and antifriction additives. Still another object of the present invention is to provide a formulation useful as an additive for energy efficient industrial gear oils which meet performance characteristics of US Steel 224 specifications and the additive formulation can also be used for GL-5 type of energy efficient automotive gear oils. Another object of the present invention is to provide a formulation useful as a gear oil additive consisting of sulfurised non traditional vegetable oils such as mohwa oil, neem oil, karanja oil prepared by the process as described and claimed in our copending patent application no. Yet another object of the present invention is to provide a formulation useful as a gear oil additive consisting of phosphosulfurised hydrogenated cardanol prepared by the process as described and claimed in our copending patent application no. , Accordingly the present invention provides a formulation useful as an extreme pressure, antiwear and antifriction additive for industrial gear oils which comprises : i) 0.25 to 0.5% by weight of sulfurised non traditional vegetable oils such as neem oil, mohwa oil and karanja oil; ii) 0.25 to 0.5% by weight of phosphosulfurised hydrogenated cardanol; iii) 0.25 to 0.5% of dibenzyl disulfide 0.25 - 0.5% by weight. The sulfurised non traditional vegetable oil used may be such as sulfurised neem oil, mohwa oil, karanja oil prepared by a process as described and claimed our patent application number: . The phosphosulfurised hydrogenated cardanol used may be prepared by a process ^described and claimed in our patent application number: The dibenzyl disulfide used may be such that copper corrosion rating is not more than Ib at 100°C for 3 hours and sulfur content is not less than 25 percent by weight. The individual components of the formulation of the present invention is not a mere admixture but a blend having synergistic properties which are not a mere aggregation of the individual properties but results in a synergistic composition having properties different from that of the aggregated properties of the individual components. The characteristics of the formulation of the present invention, when blended in SAE-90 gear lubricant base stock and evaluated for performance is as follows: Weld load : 300 - 450 Kg. Mean Hertz Load : 71-105 Wear Scar dia mm. : 0.3 - 0.4 Co-efficient of friction : 0.09-0.08 FZG gear Rating : No scoring at 12th stage Sulfur content in the blend : 0.5-1.00% due to additive components Phosphorus content in the : 0.05 - 0.1% blend ~~""~ me louowing examples are given by way of illustration and should not be construed as a limitation to the present invention. Example 1 1.4 gm of powdered dibenzyl disulfide, sulfur content 25% by weight, is added to 0.875 gm. of the sulfurised neem oil, sulfur content 13% by weight, and stirred into a thick paste to which is added 1.225gm. of phospho sulfurised hydrogenated cardanol, sulfur content 9% by weight, phosphorus content 4% by weight. The contents are heated to 80°C with stirring and 96.5 gm. Of SAE-90 lubricant base stock is added to it. The mixture is stirred for one hour till it becomes completely homogenous. It is allowed to stand for two hours to ensure that it remains homogenous. The sample is taken in a tube in which a freshly polished copper strip is dipped and at 120°C for 3 hours. The copper strip corrosion value of Ib was obtained as per ASTM D-l 13 procedure. 1000 gm of the. sample prepared as stated above and tests were run on four ball e.p. tester and friction and wear testers as per ASTM. The FZG rating was carried on FZG gear testing rig by increasing the load to each succesive stage till the scoring was observed on the gear teath. The following results are obtained. Welding Load 400 kg. Mean Hertz Load 105 kg. Wear Scar diameter 0.344 mm. Co-efficient of friction 0.086 FZG Gear rating No scoring at 11th stage Example 2 1.5 gm of powdered dibenzyl disulfide, sulfur content 25% by weight, is added to 1.25 gm. of the sulfurised neem oil, sulfur content 13% by weight, and stirred into a thick paste to which is added 2.25gm. of phospho sulfurised hydrogenated cardanol, sulfur content 9% by weight, phosphorus content 4% by weight. The contents are mixed by vigrous stirring at 80°C and 95 gm of SAE 90 lubricating oil became completely homogenous. The blend was kept for two hours in order to ensure that it remained homogenous. 1000 gm of the sample is prepared with the above composition for performance characteristics as discussed in example 1. The following results are obtained. Copper Strip Corrosion 1 b Welding Load 420 Mean Hertz Load 85 Wear Scar diameter mm. 0.3 Co-efficient of friction 0.08 FZG gear rating No scoring at 12th stage. Example 3 1.2 gm of powdered dibenzyl disulfide, sulfur content 25% by weight, is added to 1.4 gm. of the sulfurised neem oil, sulfur content 13% by weight, and stirred into a thick paste to which is added 1.4gm. of phosphosulfurised hydrogenated cardanol, sulfur content 9% by weight, phosphorus content 4% by weight. The content are mixed by vigorous stirring at 80°C and 96 gm of SAE-90 lubricating oil base stock is added and mixture stirred till it becomes completely homogenous and allowed to stant for 2 hrs. to ensure that it remains homogenous. 1000 gm of the blend of above composition is prepared for evaluation of performance characteristics as described in example 1&2. The following are the characteristics : Copper Corrosion at 120°C for 3 hrs. lb Welding load, Kg. 380 Mean Hertz Load 75 Wear Scar diameter, mm 0.30 Co-efficient of friction 0.084 FZG gear rating No scoring at 11th Stage Example 4 1.8 gm of powdered dibenzyl disulfide is mixed with 2.1 gm of sulfurised neem oil and 2.1 gm of phosphosulfurised hydrogenated cardanol at 80°C with vigorous stirring and 94 gm of SAE-90 lubricant base stock is added. The mixture is stirred till it becomes completely homogenous as described above. 1000 gm of the blend of above composition is prepared for performance characteristics. The following are the characteristics. Copper Strip Corrosion at 120°C for 3 hours Ib Welding load Kg. 400 Mean Hertz Load 90 Wear Scar dia mm 0.3 Co-efficient of friction 0.08 FZG gear rating No scoring at 12th Stage The main advantages of the additive composition of the present invention are : 1. The composition leads to development of high performance energy efficient e.p. additive from naturally occuring starting materials from renewable resources which are cheaply priced. 2. The composition produced possess outstanding load carrying properties as well as lubricity characteristics such as low wear and lower friction as compared to many other commercial formulations. 3. The formulation has components which have higher biodegradability and lower toxicity than most of the components used currently. 4. The formulation shows better performance than most other additive formulations because it does not require any metal passivators which reduce the efficacy of e.p. additives. 5. The co-efficient of friction is reduced 1.4 times and weld load is increased by 2.7 times, wear scar diameter reduced 2.2 and anti scuffing properties as reflected by FZG gear rating increased by several stages as compared to base oil alone at 0.75% sulfur and 0.1% P concentration. We Claim: 1. A synergistic formulation useful as an extreme pressure antiwear and antifriction additive for an industrial gear oils which comprises: i) 0.25 to 0.5% by weight of sulfurised non traditional vegetable oils such as neem oil, mohwa oil and karanjia oil; ii) 0.25 to 0.5% by weight of phosphosulfurised hydrogenated cardanol; iii) 0.25 to 0.5% of dibenzyl disulfide by weight. 2. A formulation as claimed in claim 1, wherein in the sulfurised non traditional vegetable oil used is such as sulfurised neem oil, mohwa oil, karanjia oil as herein described. 3. A formulation as claimed in claims 1 to 2, wherein dibenzyl disulfide used is such that the copper corrosion is not more than Ib at 100°C for 3 hrs., and sulfur content not less than 25% by weight. 4. A synergistic formulation useful as an extreme pressure antiwear and antifriction additive for industrial gear oils substantially as herein described with reference to the examples.

Full Text

The present invention relates to a formulation useful as an extreme pressure, antiwear and antifriction additive for industrial gear oils.
The present invention particularly relates to a formulation consisting of sulfurised derivatives of Neem Oil and phosphosulfurised derivatives of hydrogenated cardanols with low corrosivity to copper which in a synergistic combination with dibenzyl di sulfide gives energy efficient industrial gear oils meeting U.S. Steel 224 specifications
"" ' ^
when blended in SAE-90 gear lubricant base stock.
The additive formulation of the present invention in 3-6% concentration in SAE-90 gear
lubricant base stock gives welding load more than 300 Kg., wear scar diameters less than
0.4mm and co-efficient of friction less than 0.085, passes 12th stage of FZG gear rating
without scoring and Timken O.K load more than 45 Kg. The copper corrosion at 4%
concentration is in the range of 1 at 100°C for 3 hours without the addition of metal
passivators.
Organic sulfides, sulfurised fatty oils, sulfurised defines and alkyl aryl phosphorothibates
as a class of compounds whether alone or in admixtures with each other are being
extensively employed as extreme pressure (e.p.^ antiwear and antifriction additives.
Extensive published information, papers and patents is available on the mode and
mechanism of action of these additives and formulations for various types of gear oils and
metal working oils over past thirty years. •
The currently markete commercial formulations of additives for industrial as well as

automotive gear oils mainly contain sulfurised defines, fatty esters and alkyl phosphorothioates. Some recent formulations contain small quantities of molybdenum derivatives also such as in energy efficient low friction gear oils.

But none of the formulations have so far used sulfurised non traditional vegetable oils
and phosphosulfurised naturally occuring alkyl phenols as additive components and
formulations for energy efficient industrial gear oils which meet performance
requirements of U.S Steel 224 specifications.
'Most of the sulfurised olefines and alkyl aryl phosphorothioates used in e.p. formulations
have relatively high toxicity and low biodegradability. These products usually have high
corrosivity towards copper which is supressed by use of metal passivators which in turn
depress their performance characteristics too. The wear and extreme pressure
characteristics are satisfactory but the friction co-efficients usually are not reduced which
cause higher energy cosnumption.
The main object of the present invention is to provide a formulation useful as an extreme
pressure, antiwear and antifriction additive for industrial gear oils which obviates the
draw backs as detailed above.
Another object of the present invention is to use sulfurised and phosphosulfurised
derivatives of non traditional vegetable oils and naturally occuring alkyl phenols as
extreme pressure, antiwear and antifriction additives.
Still another object of the present invention is to provide a formulation useful as an
additive for energy efficient industrial gear oils which meet performance characteristics
of US Steel 224 specifications and the additive formulation can also be used for GL-5
type of energy efficient automotive gear oils.
Another object of the present invention is to provide a formulation useful as a gear oil
additive consisting of sulfurised non traditional vegetable oils such as mohwa oil, neem

oil, karanja oil prepared by the process as described and claimed in our copending patent
application no.
Yet another object of the present invention is to provide a formulation useful as a gear oil
additive consisting of phosphosulfurised hydrogenated cardanol prepared by the process
as described and claimed in our copending patent application no. ,
Accordingly the present invention provides a formulation useful as an extreme pressure,
antiwear and antifriction additive for industrial gear oils which comprises :
i) 0.25 to 0.5% by weight of sulfurised non traditional vegetable oils such as neem
oil, mohwa oil and karanja oil;
ii) 0.25 to 0.5% by weight of phosphosulfurised hydrogenated cardanol; iii) 0.25 to 0.5% of dibenzyl disulfide 0.25 - 0.5% by weight. The sulfurised non traditional vegetable oil used may be such as sulfurised neem oil, mohwa oil, karanja oil prepared by a process as described and claimed our patent application number: .
The phosphosulfurised hydrogenated cardanol used may be prepared by a process ^described and claimed in our patent application number: The dibenzyl disulfide used may be such that copper corrosion rating is not more than Ib at 100°C for 3 hours and sulfur content is not less than 25 percent by weight. The individual components of the formulation of the present invention is not a mere admixture but a blend having synergistic properties which are not a mere aggregation of the individual properties but results in a synergistic composition having properties different from that of the aggregated properties of the individual components.
The characteristics of the formulation of the present invention, when blended in SAE-90
gear lubricant base stock and evaluated for performance is as follows:
Weld load : 300 - 450 Kg.
Mean Hertz Load : 71-105
Wear Scar dia mm. : 0.3 - 0.4
Co-efficient of friction : 0.09-0.08
FZG gear Rating : No scoring at 12th stage
Sulfur content in the blend : 0.5-1.00%
due to additive components
Phosphorus content in the : 0.05 - 0.1%
blend ~~""~
me louowing examples are given by way of illustration and should not be construed as a limitation to the present invention.
Example 1
1.4 gm of powdered dibenzyl disulfide, sulfur content 25% by weight, is added to 0.875 gm. of the sulfurised neem oil, sulfur content 13% by weight, and stirred into a thick paste to which is added 1.225gm. of phospho sulfurised hydrogenated cardanol, sulfur content 9% by weight, phosphorus content 4% by weight. The contents are heated to 80°C with stirring and 96.5 gm. Of SAE-90 lubricant base stock is added to it. The mixture is stirred for one hour till it becomes completely homogenous. It is allowed to stand for two hours to ensure that it remains homogenous. The sample is taken in a tube in which a freshly polished copper strip is dipped and at 120°C for 3 hours. The copper strip corrosion value of Ib was obtained as per ASTM D-l 13 procedure. 1000 gm of the.
sample prepared as stated above and tests were run on four ball e.p. tester and friction and
wear testers as per ASTM.
The FZG rating was carried on FZG gear testing rig by increasing the load to each
succesive stage till the scoring was observed on the gear teath. The following results are
obtained.
Welding Load 400 kg.
Mean Hertz Load 105 kg.
Wear Scar diameter 0.344 mm.
Co-efficient of friction 0.086
FZG Gear rating No scoring at 11th stage
Example 2
1.5 gm of powdered dibenzyl disulfide, sulfur content 25% by weight, is added to 1.25 gm. of the sulfurised neem oil, sulfur content 13% by weight, and stirred into a thick paste to which is added 2.25gm. of phospho sulfurised hydrogenated cardanol, sulfur content 9% by weight, phosphorus content 4% by weight. The contents are mixed by vigrous stirring at 80°C and 95 gm of SAE 90 lubricating oil became completely homogenous. The blend was kept for two hours in order to ensure that it remained homogenous. 1000 gm of the sample is prepared with the above composition for performance characteristics as discussed in example 1. The following results are obtained.
Copper Strip Corrosion 1 b
Welding Load 420
Mean Hertz Load 85
Wear Scar diameter mm. 0.3
Co-efficient of friction 0.08
FZG gear rating No scoring at 12th stage.
Example 3
1.2 gm of powdered dibenzyl disulfide, sulfur content 25% by weight, is added to 1.4 gm. of the sulfurised neem oil, sulfur content 13% by weight, and stirred into a thick paste to which is added 1.4gm. of phosphosulfurised hydrogenated cardanol, sulfur content 9% by weight, phosphorus content 4% by weight. The content are mixed by vigorous stirring at 80°C and 96 gm of SAE-90 lubricating oil base stock is added and mixture stirred till it becomes completely homogenous and allowed to stant for 2 hrs. to ensure that it remains homogenous. 1000 gm of the blend of above composition is prepared for evaluation of performance characteristics as described in example 1&2. The following are the characteristics :
Copper Corrosion at 120°C for 3 hrs. lb
Welding load, Kg. 380
Mean Hertz Load 75
Wear Scar diameter, mm 0.30
Co-efficient of friction 0.084
FZG gear rating No scoring at 11th Stage
Example 4
1.8 gm of powdered dibenzyl disulfide is mixed with 2.1 gm of sulfurised neem oil and
2.1 gm of phosphosulfurised hydrogenated cardanol at 80°C with vigorous stirring and 94
gm of SAE-90 lubricant base stock is added. The mixture is stirred till it becomes
completely homogenous as described above. 1000 gm of the blend of above composition
is prepared for performance characteristics. The following are the characteristics.
Copper Strip Corrosion at 120°C for 3 hours Ib
Welding load Kg. 400
Mean Hertz Load 90
Wear Scar dia mm 0.3
Co-efficient of friction 0.08
FZG gear rating No scoring at 12th Stage
The main advantages of the additive composition of the present invention are :
1. The composition leads to development of high performance energy efficient e.p.
additive from naturally occuring starting materials from renewable resources
which are cheaply priced.
2. The composition produced possess outstanding load carrying properties as well as
lubricity characteristics such as low wear and lower friction as compared to many
other commercial formulations.
3. The formulation has components which have higher biodegradability and lower
toxicity than most of the components used currently.
4. The formulation shows better performance than most other additive formulations
because it does not require any metal passivators which reduce the efficacy of e.p.
additives.
5. The co-efficient of friction is reduced 1.4 times and weld load is increased by 2.7
times, wear scar diameter reduced 2.2 and anti scuffing properties as reflected by
FZG gear rating increased by several stages as compared to base oil alone
at 0.75% sulfur and 0.1% P concentration.

We Claim:
1. A synergistic formulation useful as an extreme pressure antiwear and antifriction
additive for an industrial gear oils which comprises:
i) 0.25 to 0.5% by weight of sulfurised non traditional vegetable oils such as
neem oil, mohwa oil and karanjia oil;
ii) 0.25 to 0.5% by weight of phosphosulfurised hydrogenated cardanol; iii) 0.25 to 0.5% of dibenzyl disulfide by weight.
2. A formulation as claimed in claim 1, wherein in the sulfurised non traditional
vegetable oil used is such as sulfurised neem oil, mohwa oil, karanjia oil as herein
described.
3. A formulation as claimed in claims 1 to 2, wherein dibenzyl disulfide used is such
that the copper corrosion is not more than Ib at 100°C for 3 hrs., and sulfur
content not less than 25% by weight.
4. A synergistic formulation useful as an extreme pressure antiwear and antifriction
additive for industrial gear oils substantially as herein described with reference to
the examples.

Documents:

2521-del-1998-abstract.pdf

2521-del-1998-claims.pdf

2521-del-1998-correspondence-others.pdf

2521-del-1998-correspondence-po.pdf

2521-del-1998-description (complete).pdf

2521-del-1998-form-1.pdf

2521-del-1998-form-19.pdf

2521-del-1998-form-2.pdf

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Patent Number

215826

Indian Patent Application Number

2521/DEL/1998

PG Journal Number

12/2008

Publication Date

21-Mar-2008

Grant Date

04-Mar-2008

Date of Filing

26-Aug-1998

Name of Patentee

COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH

Applicant Address

RAFI MARG, NEW DELHI-110001, INDIA.

Inventors:

#	Inventor's Name	Inventor's Address
1	ONKAR NATH ANAND	INDIAN INSTITUTE OF PETROLEUM, DEHRADUN-248005, INDIA.
2	VIJAY KUMAR CHHIBBER	INDIAN INSTITUTE OF PETROLEUM, DEHRADUN-248005, INDIA.
3	KALYAN DUTT NEEMLA	INDIAN INSTITUTE OF PETROLEUM, DEHRADUN-248005, INDIA.
4	NAVAL KISHORE PANDEY	INDIAN INSTITUTE OF PETROLEUM, DEHRADUN-248005, INDIA.
5	RAJPAL SINGH BISHT	INDIAN INSTITUTE OF PETROLEUM, DEHRADUN-248005, INDIA.
6	ASHOK KUMAR GUPTA	INDIAN INSTITUTE OF PETROLEUM, DEHRADUN-248005, INDIA.

PCT International Classification Number

C10M 29/66

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA