Title of Invention

THE NOVEL PROCESS FOR THE COMPLEXING OF LITHIUM GREASE

Abstract The Lithium complex greases are prepared by reacting the Hydrogenated Castor oil or the 12-Hydroxy Stearic Acid with the lithium Hydroxide and in addition with the mono or the dicarboxylic organic acids/esters of acids/inorganic acids like boric acid, acetic acid by co-crystallization. Such processes involve the multi components addition, in which there is a possibility of omission of the ingredients or the change in sequence of the addition of ingredients as a result failure of the product. In order to simply the complexing of the lithium soap greases, a new approach of complexing is invented. In the invention under consideration, first a simple lithium soap grease is prepared in the conventional method by reacting the 12-Hydroxy stearic with the aqueous slurry of the Lithium hydroxide in the paraffinic base oil. The multifunctional additive package prepared by the combination of the special ZDDP with the tri butyl borate ester (self complexing agent). This additive is incorporated in this simple lithium grease after getting the desired NLGI consistency grease below 80°C. The developed grease when tested for all the parameters vis-a-vis with the lithium complex grease prepared by the conventional method. The properties of grease prepared with new method are having the better structural and mechanical stability, comparable drop point and all the other characteristics of the lithium complex grease made in the conventional method.
Full Text FORM-2
THE PATENTS ACT, 1970
(39 of 1970)
AND
THE PATENTS RULES, 2003 COMPLETE SPECIFICATION
(See Section 10; Rule 13)
1. TITLE OF THE INVENTION:
"THE NOVEL PROCESS FOR THE COMPLEXING OF LITHIUM GREASE."
2. APPLICANTS:
i)
(a) NAME: HINDUSTAN PETROLEUM CORPORATION LIMITED.
(b) NATIONALITY: INDIAN COMPANY.
(c) ADDRESS: RESEARCH & DEVELOPMENT CENTRE,
PLOT D-500, TTC AREA OF MIDC, NAVI MUMBAI-400 705, MAHARASHTRA, INDIA.
The follo.wing specification describes the nature of the invention and the manner in which it is to be performed: -
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THE NOVEL PROCESS FOR THE COMPLEXING OF THE LITHIUM GREASE
3. PREAMBLE TO THE DESCRIPTION Field of Invention
The present invention relates to the novel process for the complexing of lithium grease.
Background of the Invention & the Related Art
The conventional Lithium soap based greases are prepared by reacting 12-Hydroxy Stearic Acid or Hydrogenated Castor oil with aqueous lithium hydroxide slurry in the suitable base oil. These lithium soap greases have the acceptable characteristics like drop point, thermal stability, water wash out characteristics and reasonable
load carrying properties, but maximum working limit is upto 120°C only. In order to increase high temperature working limit and the performance at high temperature, the complexing of the conventional lithium soap grease is essential.
The complexing of lithium soap greases involves co-crystallization of two or more components i.e. saponification of two dissimilar acids, acid/ester with the lithium hydroxide. This involves an addition of multi-components and a special precaution is required while adding various components, as the change in the sequence of components and the omission of ingredients may cause failure of the product.
Additionally, the high inventory to be maintained for various raw materials is also a constraint. Considering all these factors a new approach (method) of complexing of conventional lithium soap grease is sought, which may eliminate the multicomponents addition and reduction in inventory of various raw materials.
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Summary of the Invention
The lithium soap grease was prepared by the conventional method i.e. by using 12-Hydroxy Stearic and lithium hydroxide in paraffmic mineral oil of ISO VG 100. The mixture of naphthenic oil and paraffinic oil can also be taken for making the grease. After the achievement of the desired NLGI, consistency the performed
additive package, which contains self complexing agent, is added below 80°C. The performed additive package contains rust inhibitor, antioxidants and extreme pressure agent and a self complexing component.
4. DESCRIPTION OF THE INVENTION
This invention describes the preparation of lithium complex grease with an enhanced high temperature thermal/oxidation stability, good shear and mechanical stability, high drop point and load carrying capacity.
For an extended lubrication life, the structure/shear stability and the mechanical stability of the grease is very essential at high temperature. The Performance of the grease was bench marked with respect to the structure/shear stability by the worked penetration at an extended hour working intervals i.e. 100,000X, 200,000X, 400,000X and 500,000X strokes. If the structure stability of the grease is poor, a very rapid thermal or oxidative degradation takes place at the temperature much below the drop point due to depletion of an additive from the gel structure of grease. The mechanical stability of grease was tested by the roll
stability test at an ambient temperature and 82°C for 16 hours and 48 hours respectively. The mechanical stability is its resistance to the hardening or the softening as it is worked. An unstable greases whose characteristics changes drastically in the service can result in poor the lubrication.
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The grease was tested for the drop point. The dropping point is the temperature at which the grease turns from semisolid to the liquid state. It is significant only in when an operating temperature above the dropping point may cause the permanent thickener separation or the alteration of grease properties. It is not necessary a measure of the upper working temperature limit of grease. The serious EP testes were performed of the grease i.e. the load wear index, the four ball weld point, the four ball wear scar diameter and the Timken OK load. The developed grease was also tested for various other required properties of the lithium complex grease.
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The properties of developed grease are mentioned in the table 1. Table 1: The Test Results of the prepared grease-

Characteristics Results Targets Test Method
NLGI Grade NLGI 3 NLGI 3 NLGI
[email protected]°C Worked, 60X Worked, 100,000X Worked, 200,000X Worked, 400,000X Worked, 500,000X 245 240 235 240 244 250 ± 10 of 60X 220 - 250 ASTM D 217
Drop Point, °C 268 >250 ASTM D 566
Copper corrosion, @100°C, 24 hrs. la Pass ASTM D 130
Thermal stability, @ 100°C, 30 hours 1.98 >5.0 IS 1448 P:89
Wheel bearing test, Leakage by mass Slump test 1.23 pass 5.0 Pass ASTM D 1263
Water washout @80°C, % loss wt. 2.46 Roll stability test, % change [email protected] ambient, after 16 [email protected], 82°C, after 48 hours 6 14 10 20 ASTM D 1831
Oxidation stability, @100°C Drop in pressure, @ 100 hrs. Drop in pressure, @ 500 hrs. 37 1025 ASTM D 942
Emcor rust test, rating 0,0 0,0 IP 220
EP properties Load wear Index, kg Four ball weld load, kg Four ball wear scar dia, mm Timken OK load, lb 52 315 0.4155 40 min280 min0.5045 ASTM D 2596 ASTM D 2596 ASTM D 2266 ASTM D 2509
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Conclusions
The lithium complex grease prepared by new approach has better structure/shear stability and mechanical stability as evidenced by extended worked penetration and roll stability tests respectively. The grease has high drop point which is comparable with other lithium complex greases. The series of four ball EP tests and Timken OK load test reveal the load carrying capacity of prepared grease.
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5. WE CLAIM:
1. The novel process for the complexing of lithium grease, used in making a
lithium complex grease with the high mechanical/shear stability and the
high drop point prepared by using an approach, involving a direct addition
of the performance additive package containing self the complexing agent,
comprising of:
(i) the preparation of the complexing agent, by reacting the boric acid
and the butyl alcohol by esterification. (ii) the preparation of ZDDP. (iii) the mixing of the components mentioned above to get the
performance enhancing additive further adding this package in the simple lithium soap grease below 80°C after getting the desired NLGI consistency.
2. The novel process for the complexing of lithium grease as claimed in claim 1 above, wherein the complex lithium soap thickener comprising of a mixture of the special ZDDP, the rust and the corrosion inhibitor and the borate ester and the ithium stearate.
3. The novel process for the complexing of lithium grease as claimed in claim 1 and 2 above, the total amount of the lithium salt components present ranging from about 10 to 15% by wt based on finished grease.
Dated this 20th day of November, 2006.
I Sanjeev Niphadkar,
Agents for the Applicants,
Hindustan Petroleum Corporation Limited.
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7.
ABSTRACT
The Lithium complex greases are prepared by reacting the Hydrogenated Castor oil or the 12-Hydroxy Stearic Acid with the lithium Hydroxide and in addition with the mono or the dicarboxylic organic acids/esters of acids/inorganic acids like
boric acid, acetic acid by co-crystallization. Such processes involve the multi components addition, in which there is a possibility of omission of the ingredients or the change in sequence of the addition of ingredients as a result failure of the product. In order to simply the complexing of the lithium soap greases, a new approach of complexing is invented. In the invention under consideration, first a simple lithium soap grease is prepared in the conventional method by reacting the 12-Hydroxy stearic with the aqueous slurry of the Lithium hydroxide in the paraffinic base oil. The multifunctional additive package prepared by the combination of the special ZDDP with the tri butyl borate ester (self complexing agent). This additive is incorporated in this simple lithium grease after getting the
desired NLGI consistency grease below 80°C. The developed grease when tested for all the parameters vis-a-vis with the lithium complex grease prepared by the conventional method. The properties of grease prepared with new method are having the better structural and mechanical stability, comparable drop point and all the other characteristics of the lithium complex grease made in the conventional method.

Documents:

1912-MUM-2006-ABSTRACT(16-3-2011).pdf

1912-MUM-2006-ABSTRACT(20-11-2006).pdf

1912-MUM-2006-ABSTRACT(GRANTED)-(31-5-2011).pdf

1912-mum-2006-abstract.doc

1912-mum-2006-abstract.pdf

1912-MUM-2006-CANCELLED PAGES(29-4-2011).pdf

1912-MUM-2006-CLAIMS(20-11-2006).pdf

1912-MUM-2006-CLAIMS(AMENDED)-(16-3-2011).pdf

1912-MUM-2006-CLAIMS(AMENDED)-(25-11-2009).pdf

1912-MUM-2006-CLAIMS(GRANTED)-(31-5-2011).pdf

1912-mum-2006-claims.pdf

1912-mum-2006-correspondance-received.pdf

1912-MUM-2006-CORRESPONDENCE(01-09-2010).pdf

1912-MUM-2006-CORRESPONDENCE(IPO)-(31-5-2011).pdf

1912-mum-2006-description (complete).pdf

1912-MUM-2006-DESCRIPTION(COMPLETE)-(20-11-2006).pdf

1912-MUM-2006-DESCRIPTION(GRANTED)-(31-5-2011).pdf

1912-MUM-2006-FORM 18(17-12-2007).pdf

1912-MUM-2006-FORM 2(COMPLETE)-(20-11-2006).pdf

1912-MUM-2006-FORM 2(GRANTED)-(31-5-2011).pdf

1912-MUM-2006-FORM 2(TITLE PAGE)-(16-3-2011).pdf

1912-MUM-2006-FORM 2(TITLE PAGE)-(20-11-2006).pdf

1912-MUM-2006-FORM 2(TITLE PAGE)-(GRANTED)-(31-5-2011).pdf

1912-MUM-2006-FORM 26(25-11-2009).pdf

1912-mum-2006-form-1.pdf

1912-mum-2006-form-2.doc

1912-mum-2006-form-2.pdf

1912-MUM-2006-REPLY TO EXAMINATION REPORT(25-11-2009).pdf

1912-MUM-2006-REPLY TO HEARING(16-3-2011).pdf

1912-MUM-2006-REPLY TO HEARING(29-4-2011).pdf

1912-MUM-2006-SPECIFICATION(AMENDED)-(16-3-2011).pdf

1912-MUM-2006-SPECIFICATION(AMENDED)-(29-4-2011).pdf


Patent Number 247896
Indian Patent Application Number 1912/MUM/2006
PG Journal Number 22/2011
Publication Date 03-Jun-2011
Grant Date 31-May-2011
Date of Filing 20-Nov-2006
Name of Patentee HINDUSTAN PETROLEUM CORPORATION LIMITED.
Applicant Address RESEARCH & DEVELOPMENT CENTRE, PLOT D-500, TTC AREA OF MIDC, NAVI MUMBAI – 400 705,
Inventors:
# Inventor's Name Inventor's Address
1 B. S. NAGARKOTI. B-205, SUN HILL VIEW APARTMENT, HIMALAYA SOCIETY, ASALPHA, GHATKOPAR (WEST), MUMBAI - 400 084,
2 AMITABH KUMAR JAIN. 27/202, HP Nagar (E) Vashi Naka, chembur, Mumbai 400 074
3 B. RAMESWAR. 34/602, HP Nagar (E), Vashi Naka Chembur, Mumbai 400 074
4 G. BASKARAN. Banglow No. 8C, HP Nagar (E) Vashi Naka Chembur, Mumbai 400 074
5 C. S. KRISHNASWAMY. Flat No. B-802, BPCL CHS Plot No. 3, Sector 46 A, Nerul, Navi Mumbai 400 706
PCT International Classification Number C10M117/04
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA