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Biobased/Vegetable Oil Based High Temperature Grease And Process For Preparation Thereof

Abstract: The present invention discloses a bio-based, biodegradable, non-toxic high temperature multipurpose grease formulation having high oxidative stability and process for preparation thereof. The process utilizes oxidatively stable palmolein oil and a vegetable oil as base fluids. The grease formulation of the present invention is usable in various segments including but not limited to industrial, agriculture/farming equipment, and forestry applications.

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Patent Information

Application #
Filing Date
11 July 2012
Publication Number
29/2014
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
Parent Application

Applicants

MINT AGRI RESEARCH & DEVELOPMENT PVT LTD
S NO 1073/1-2-3 MUTHA ROAD, PIRANGUT TALUKA-MULSHI, DISTRICT-PUNE PIN - 412 111

Inventors

1. YASHWANT GOPAL GHAISAS
S NO 1073/1-2-3 MUTHA ROAD, PIRANGUT TALUKA-MULSHI, DISTRICT-PUNE PIN - 412 111
2. RAHUL RAMCHANDRA GOKHALE
S NO 1073/1-2-3 MUTHA ROAD, PIRANGUT TALUKA-MULSHI, DISTRICT-PUNE PIN - 412 111
3. SHRIDHAR NARAYAN BENDKE
S NO 1073/1-2-3 MUTHA ROAD, PIRANGUT TALUKA-MULSHI, DISTRICT-PUNE PIN - 412 111

Specification

FORM 2
THE PATENT ACT 1970
& The Patents Rules, 2003
COMPLETE SPECIFICATION (See section 10 and rule 13)
1. TITLE OF THE INVENTION:
"Bio-Based/ Vegetable Oil Based High Temperature Grease and Process for Preparation Thereof'
2. APPLICANT
(a) NAME: Mint Agri Research & Development Pvt Lid
(b) NATIONALITY: Indian Company
(c) ADDRESS: S No 1073/1-2-3 Mutha road, Pirangut
"Taluka- Mulshi. District-Pune Pin - 412 111
3. PRREAMBLE TO THE DESCRIPTION
COMPLETE
The following specification particularly describes the invention and the manner in which it is to be performed.

Bio-Based/Vegetable Oil Based High Temperature Grease and Process for
Preparation Thereof
Field of the invention
The present invention relates to a high temperature grease, and more particularly, to a biodegradable, non-toxic, bio-based/vegetable oil based multi-purpose grease and process for preparation thereof.
Background of the invention
Presently available high temperature greases are made from mineral oil based or from synthetic materials. The mineral based oils have low flashpoint, low lubricity, low viscosity index and are non polar in nature. Also, ine mineral based oils are not biodegradable and are toxic. Hence, they are hazardos for disposal. The petroleum oils lubricity is derived from various additives in the formulation.
Synthetic materials exhibit somewhat better qualities in respect of lubricity, viscosity index and flash point. But they are also not necessarily biodegradable and non toxic.
Accordingly, there exists a need of a high temperature bio-based/vegetable oil based multi-purpose grease having high lubricity, polar nature, high viscosity index, high flash point, as well as biodegradability and non toxic nature.
Objects of the invention
An object of the present invention is to provide a high temperature bio-based/vegetable oil based multi-purpose grease forn-miation having high oxidative stability.

Another object of the present invention is to provide the multi-purpose grease having high lubricity, polar nature, high viscosity index, high flash point, and high oxidative stability as well as biodegradability and non toxic nature.
Yet another object of the present invention is to provide a process for preparation of bio-based/vegetable oil based, biodegradable, non-toxic, multi-purpose grease.
Summary of the invention
Accordingly, the present invention provides a bio-based high temperature grease formulation having high oxidative stability. The high temperature grease formulation comprises boric acid in a range of 0.5 % by weight to 1 % by weight, lithium hydroxide (monohydrate) in a range of 0.15 % by weight to 2.5 % by weight, a thickener in a range of 14 % by weight to 16 % by weight, vegetable oil in a range of 40 % by weight to 60 % by weight, palmolien in a range of 8 % by weight to 25 % by weight, tackifier in a range of 1 % by weight by 3 % by weight, an antioxidant in a range of 0.3 % by weight to 0.7 % by weight and balance quantity of an aqueous carrier.
In another aspect, the present invention provides a process of a preparation of bio-based vegetable oil grease having high oxidative stability.
Detailed description of the invention
The foregoing objects of the present invention are accomplished and the problems and shortcomings associated with the prior art. techniques and approaches are overcome by the present invention as described below in the preferred embodiments.
Accordingly, the present invention provides a bio-based/vegetable oil based, biodegradable, non-toxic, high temperature multi-purpose grease formulation having

high oxidative stability. The formulation of present invention is suitable for high temperature applications and has high lubricity, polar nature, high viscosity index, high flash point, and high oxidative stability as well as biodegradability and non toxic nature. The formulation of present invention is useful for industrial applications having surrounding temperature to the extent of 250 C. In another aspect, the present invention discloses a process for the preparation of bio-based grease formulation suitable for high temperature applications requiring high oxidative stability.
The bio-based/vegetable oil based high temperature grease formulation (hereinafter referred as "the high temperature grease formulation") comprises boric acid in a range of 0.5 % by weight to 1 % by weight. Further, the high temperature grease formulation comprises lithium hydroxide (monohydrate) in a range of 0.15 % by weight to 2.5 % by weight. Furthermore, the high temperature grease formulation comprises a thickener in a range of 14 % by weight to 16 % by weight. Specifically, the thickener is 12-hydoxy stearic acid. Moreover, the high temperature grease formulation comprises vegetable oil in a range of 40 % by weight to 60 % by weight.
The high temperature grease formulation also comprises palmolein in a range of 8 % by weight to 25 % by weight. Palmolein is the liquid fraction obtained b> fractionation of palm oil after crystallization at controlled temperatures. The physical characteristics of palmolein differ from those of palm oil. The major fatty acids ol^ palmolein are palmitic acid (35% by weight), oleic acid (45% by weight) and linoleic acid (13% by weight). This means major portion of palmolein consists of oleic acid (monosaturated) and palmitic acid (saturated), i.e. approximately 80% by weight part of palmolein is thermo-oxidative stable. Hence, palmolein oil is best suited lor manufacturing of bio-based lubricating greases. Vegetable oils have significant potential as a base fluid and a substitute for mineral oil for grease formulation.

% by weight to 3 % by weight. Specifically, the tacher is polvalphaolefins- 100. Furthermore, the high temperature grease formulation comprises an antioxidant in a range of 0.3 % by weight to 0.7 % by weight. Specially, the antioxidant is di-tert-butyl-p-cresol. The high temperature grease formulation comprises balance quantity of all aqueous carrier, for example water.
The bio-based/vegetable oil based high temperature grease formulation is prepared by a process (200) as illustrated in figure 1. The process (200) starts at (10).
At step (20), the process (200) includes preparing a boric acid liquid soap solution. Liquid soap of boric acid is prepared by dissolving boric acid in boiling water Further, lithium hydroxide (monohydrate) is dissolved in hot water. The lithium hydroxide solution is added to boric acid slowly niaintaining a temperature from about 60° to about 90° C to form boric acid liquid soaP- The soap is used for complex soap formation.
At step (30), the process (200) includes preparing an alkali solution by dissolving lithium hydroxide in de-mineralized hot water at a temperature in a range of about 70° to 90°C.
At Step (40), the process (200) includes melting a 12-hydroxy stearic acid (herein after referred as '12-HSA')in a preheated soap reactor 70° C to 90° C. The melted 12-HSA is stirred continuously.
At step (50), the process (200) includes adding alkali solution slowly to the soap reactor containing molten 12-HSA to form a mixture and maintaining the temperature of the mixture in a range of 70° to 90° C.

At step (60), the process (200) includes adding boric acid liquid soap solution slowly to the above mixture to form soap, and the temperature is maintained at about 70° to 90 C for about 25-35 minutes with continuous stirring of the mixture.
At step (70), the process (200) includes soap digestion and structure stabilization, wherein a vegetable oil is added to the grease reactor and heated. The examples of vegetable oil include palm oil and degummed karanj oil. The temperature is maintained at about 70° to 90° C. The soap from soap reactor is slowly added to the preheated vegetable oil at about 70 to 90 C to form a reaction mixture. The temperature of the reaction mixture is maintained at about 80 C for about 20 minutes. Thereafter, the reactor temperature is maintained at about 120 C for about 50-70 minutes. Further, the reactor temperature is maintained at about 220° C for about 2-4 hours, with continuous stirring.
At step (80), the process (200) includes quenching wherein the heating to the reactor is stopped and palmolein is added to the reaction mixture all at once thereby causing the sudden drop in temperature by about 30 C to about 40 C. known as shock cooling.
At step (90), the process (200) includes checking consistency of the reaction mixture wherein un-worked penetration should be in-between 220 mm to 260 mm. The reaction mixture is cooled to about 70 C to about 90° C with continuous stirring.
At step (100), the process (200) includes adding predefined quantity of polyalphaolefins- 100 (herein after 'PAO-100') and di-tert-butyl-p-cresol to the reaction mixture and cooling the reaction mixture at about 80° C.
At step (110), the process (200) includes milling and filling of the mixture. The process (200) ends at step (120).

Advantages of the invention
1. The bio-based/vegetable oil based grease formulation of (he present invention is highly lubricant and polar. Hence, provides almost friction less operations and energy saving compared to the present mineral oil based or synthetic greases.
2. Grease formulation of the present invention has much superior high temperature qualities, such as high viscosity index for the base oil and high flash point for safety. Thus the grease maintains its structure at high temperatures unlike mineral oil based greases.
3. The bio-based/vegetable oil based grease multi-purpose grease formulation of the present invention is biodegradable and non toxic as well as it has high oxidative stability. Also, the grease formulation of present the invention is environment friendly and also easy for composting and disposal and is renewable through nature's cycle.
4. The formulation of the present invention is most suitable for high temperature applications in the industry for equipments in ovens and furnaces up to temperature of about 250° C for the grease.
The foregoing descriptions of specific embodiments of the present invention have been presented for purposes of illustration and description. They are not intended to be exhaustive or to limit the present invention (o the precise forms disclosed, and obviously many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the present invention and its practical application, to thereby enable others skilled in the art to best utilize the present invention and various embodiments with various modifications as are suited to the particular use contemplated. It is

understood that various omission and substitutions of equivalents are contemplated as circumstance may suggest or render expedient, but such are intended to cover the application or implementation without departing from the spirit or scope of the present invention.

We Claim:
l.A bio-based/vegetable oil based high temperature grease formulation having high oxidative stability, the grease formulation comprising:
boric acid in a range of 0.5 % by weight to 1 % by weight;
lithium hydroxide (monohydrate) in a range of 0.15 % by weight to 2.5
% by weight;
stearic acid in a range of 14 % by weight to 16 % by weight:
vegetable oil in a range of 40 % by weight to 60 % by weight:
palmolien in a range of 8 % by weight to 25 % by weight;
tackifier in a range of 1 % by weight to 3 % by weight;
an antioxidant in a range of 0.3 % by weight to 0.7 % by weight: and
balance quantity of an aqueous carrier.
2. The grease formulation as claimed in claim 1. wherein the stearic acid is 12-hydroxy stearic acid.
3. The grease formulation as claimed in claim 1, wherein the vegetable oil is selected from any one of palm oil and degummed Karanj oil.
4. The grease formulation as claimed in claim 1, wherein the tackifier is selected from the group consisting of polyalphaolefins and polyalphaolefms-100.
5. The grease formulation as claimed in claim 1. wherein the antioxidant is di-tert-butyl-p-ci-esol.
6. A process for preparation of a bio-based/vegetable oil based high temperature grease formulation, the process comprising:

preparing a boric acid soap solution vising boric acid and lithium hydroxide (monohydrate);
preparing an alkali solution using lithium hydroxide;
melting a 12-hydroxy stearic acid in a preheated soap reactor at a temperature in a range of 70° C -90° C;
adding alkali solution of lithium hydroxide to a molten 12-hydroxy stearic acid to form a mixture;
adding boric acid soap solution slowly to the mixture to form a soap;
adding the soap to a preheated vegetable oil and heating at a temperature in a range of 70° to 90° C to form a reaction mixture;
maintaining the temperature of the reaction mixture at about 80° C for about 20 minute, at about 120oC for about 50-70 minutes and at about 220oC for about 2-4 hours;
quenching the soap reactor and adding a predefined quantity of a palmolein to the reaction mixture;
checking consistency of the mixture;
adding predefined quantity of a tackifier and an antioxidant to the reaction mixture and cooling the reaction mixture at a temperature in a range of 70° C to 90° C; and
milling and tilling of the cooled reaction mixture.
7. The process for preparation of grease formulation as claimed in claim 6, wherein the vegetable oil is selected from any one of palm oil and degummed Karanj oil.
8. The process for preparation of grease formulation as claimed in claim 6. wherein the tackifier is selected from the group consisting of polyalphaolelins and polyalphaolefins-100.

9. The process for preparation of" grease formulation as claimed in claim 6. wherein the antioxidant is di-tert-butyl-p-cresol.

Documents

Application Documents

# Name Date
1 1168-MUM-2012-FER.pdf 2020-07-29
1 Form 18 [11-07-2016(online)].pdf 2016-07-11
2 1168-MUM-2012-ABSTRACT(11-7-2013).pdf 2018-08-11
2 ABSTRACT1.jpg 2018-08-11
3 1168-MUM-2012-REQUEST FOR POST-DATING(10-4-2013).pdf 2018-08-11
3 1168-MUM-2012-CLAIMS(11-7-2013).pdf 2018-08-11
4 1168-MUM-2012-POWER OF AUTHORITY.pdf 2018-08-11
4 1168-MUM-2012-CORRESPONDENCE(11-7-2013).pdf 2018-08-11
5 1168-MUM-2012-GENERAL POWER OF ATTORNEY(11-7-2013).pdf 2018-08-11
5 1168-MUM-2012-DESCRIPTION(COMPLETE)-(11-7-2013).pdf 2018-08-11
6 1168-MUM-2012-FORM 5(11-7-2013).pdf 2018-08-11
6 1168-MUM-2012-DESCRIPTION(PROVISIONAL).pdf 2018-08-11
7 1168-MUM-2012-FORM 3(11-7-2013).pdf 2018-08-11
7 1168-MUM-2012-DRAWING(11-7-2013).pdf 2018-08-11
8 1168-MUM-2012-FORM 2.pdf 2018-08-11
8 1168-MUM-2012-FORM 1.pdf 2018-08-11
9 1168-MUM-2012-FORM 2(11-7-2013).pdf 2018-08-11
9 1168-MUM-2012-FORM 2(TITLE PAGE).pdf 2018-08-11
10 1168-MUM-2012-FORM 2(TITLE PAGE)-(11-7-2013).pdf 2018-08-11
11 1168-MUM-2012-FORM 2(11-7-2013).pdf 2018-08-11
11 1168-MUM-2012-FORM 2(TITLE PAGE).pdf 2018-08-11
12 1168-MUM-2012-FORM 1.pdf 2018-08-11
12 1168-MUM-2012-FORM 2.pdf 2018-08-11
13 1168-MUM-2012-DRAWING(11-7-2013).pdf 2018-08-11
13 1168-MUM-2012-FORM 3(11-7-2013).pdf 2018-08-11
14 1168-MUM-2012-DESCRIPTION(PROVISIONAL).pdf 2018-08-11
14 1168-MUM-2012-FORM 5(11-7-2013).pdf 2018-08-11
15 1168-MUM-2012-DESCRIPTION(COMPLETE)-(11-7-2013).pdf 2018-08-11
15 1168-MUM-2012-GENERAL POWER OF ATTORNEY(11-7-2013).pdf 2018-08-11
16 1168-MUM-2012-CORRESPONDENCE(11-7-2013).pdf 2018-08-11
16 1168-MUM-2012-POWER OF AUTHORITY.pdf 2018-08-11
17 1168-MUM-2012-CLAIMS(11-7-2013).pdf 2018-08-11
17 1168-MUM-2012-REQUEST FOR POST-DATING(10-4-2013).pdf 2018-08-11
18 1168-MUM-2012-ABSTRACT(11-7-2013).pdf 2018-08-11
18 ABSTRACT1.jpg 2018-08-11
19 Form 18 [11-07-2016(online)].pdf 2016-07-11
19 1168-MUM-2012-FER.pdf 2020-07-29

Search Strategy

1 2020-03-2618-59-05E_27-03-2020.pdf