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Patent 2561351 Summary

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(12) Patent: (11) CA 2561351
(54) English Title: A PROCESS FOR MAKING METAL WORKING FLUID FROM HEAVY ALKYLATE
(54) French Title: PROCEDE DE FABRICATION D'UN FLUIDE DE TRANSFORMATION DE METAUX A PARTIR D'ALKYLATE LOURD
Status: Expired and beyond the Period of Reversal
Bibliographic Data
(51) International Patent Classification (IPC):
  • C10M 16/04 (2006.01)
  • C10M 10/08 (2006.01)
  • C10M 17/02 (2006.01)
(72) Inventors :
  • SINGH, ARUN KUMAR (India)
  • ANAND, ONKAR NATH (India)
  • GUPTA, ASHOK KUMAR (India)
(73) Owners :
  • COUNCIL OF SCIENTIFIC & INDUSTRIAL RESEARCH
(71) Applicants :
  • COUNCIL OF SCIENTIFIC & INDUSTRIAL RESEARCH (India)
(74) Agent: GOWLING WLG (CANADA) LLP
(74) Associate agent:
(45) Issued: 2011-10-11
(86) PCT Filing Date: 2005-02-21
(87) Open to Public Inspection: 2005-10-06
Examination requested: 2008-03-11
Availability of licence: N/A
Dedicated to the Public: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): Yes
(86) PCT Filing Number: PCT/IN2005/000053
(87) International Publication Number: IN2005000053
(85) National Entry: 2006-09-26

(30) Application Priority Data:
Application No. Country/Territory Date
10/810,387 (United States of America) 2004-03-26

Abstracts

English Abstract


The present invention relates to a process for heavy alkylate based less toxic
metalworking fluid composition comprising heavy alkyl benzene, one emulsifier
which is a sodium oleate, sulfonate or mixtures thereof, a vegetable oil as
lubricity booster, an antioxidant, a fungicide, an extreme pressure additive,
an antirust, a co-surfactant, a coupling agent and alkali component. The
process comprises removing of insoluble matter from the heave alkylate,
addition of emulsifier, additives, coupling agent and co-surfactant,
homogenizing the mixture at 20 - 120~C, followed by conditioning of the metal
working fluid concentrate which can be used as emulsion in water.


French Abstract

La présente invention concerne un procédé d'obtention d'une composition de fluide de transformation de métaux moins toxique à base d'alkylate lourd, contenant du benzène d'alkyle lourd, un émulsifiant constitué d'un oléate de sodium, d'un sulfonate de sodium ou de mélanges de ceux-ci, une huile végétale comme lubrifiant, un antioxydant, un fongicide, un additif extrême-pression, un antirouille, un cosurfactant, un agent de couplage et un composant alcali. Le procédé consiste à éliminer une matière insoluble de l'alkylate lourd, à ajouter l'émulsifiant, les additifs, l'agent de couplage et le cosurfactant, à homogénéiser le mélange à 20 - 120·C, puis à conditionner le concentré de fluide de transformation des métaux pouvant être utilisé comme une émulsion dans l'eau.

Claims

Note: Claims are shown in the official language in which they were submitted.


10
We Claim:
1. A metalworking fluid composition of heavy alkylate said composition
comprising
of:
(a) residual fraction having C20 to C22 alkyl carbon atom of detergent class
Alkyl
Benzene in the concentration range of 50 to 90 weight percent of the metal
working fluid, (b) at least one emulsifier in the range of 10 to 40 weight
percent
of the metalworking fluid, (c) at least one lubricity booster component in the
concentration range of 2-10 percent of the metalworking fluid, (d) an
antioxidant
component is in the concentration range: of 50-500 ppm, (e) a fungicide
component in the concentration range of 50-500 ppm, (f) an extreme pressure
additive component in the concentration range of 50-500 ppm (g) an anti-rust
component in the concentration range of 50-500 ppm, (h) a co-surfactant
component in the range of 1-10 weight percent of the metal working fluid, (i)
a
coupling agent in the range of 0.5 to 10 eight percent of the metal working
fluid,
(j) alkali component in the range of 8-10 weight percent of the metal working
fluid,
wherein said heavy alkylate is free from polyaromatic or olefinic compounds.
2. A composition as claimed in claim 1, wherein the residual component of
Alkyl
Benzene is an oil component having heavy alkyl benzene of C20 to C22 alkyl
carbon
number, a heavy fraction by-product separated from detergent class alkyl
benzene during
manufacture.
3. A composition as claimed in claim 1, wherein the emulsifier is selected
from the
group consisting of heavy alkylate sodium sulfonates, sodium carboxylate,
sodium oleate,
triethanolamine oleate, diethanolamine oleate or dodecyl toluene sodium
sulfonate, and
mixtures thereof.
4. A composition as claimed in claim 1, wherein the lubricity booster is a
vegetable
oil selected from the group consisting of karanja oil, neem oil, rice-bran
oil, castor oil,
and mixtures thereof.

11
5. A composition as claimed in claim 1, wherein the antioxidant component is
an
alkyl phenol or aromatic amine or substituted alkyl phenol selected from the
group
consisting of 2,6-ditertiary butyl phenol, 2,6-ditertiary p-cresol,
diphenylamine, tertiary
butyl phenol amino tetrazole, and 2,6-dioctyl phenylene-diamine.
6. A composition as claimed in claim 1, wherein the fungicide component is a
phenol or phenolic acid selected from the group consisting of o-cresol,
phenol, m-cresol,
and cresylic acid.
7. A composition as claimed in claim 1, wherein the extreme pressure additive
component is an organic sulfide or phosphosulfurized metal salt selected from
the group
consisting of dibenzyl disulphide, sulfurized vegetable oil, phosphosulfurized
decyl
oleate molybdate, and phosphothio pentadecyl phenol molybdate.
8. A composition as claimed in claim 1, wherein the anti-rust component is a
triazole
or sulfonate selected from the group consisting of 1H-benzotriazole,
ditertiary butylated
1H-Benzotriazole, calcium petroleum sulfonate, and calcium heavy alkylate
sulfonate.
9. A composition as claimed in claim 1, wherein the co-surfactant component is
an
alcohol selected from the group consisting of isopropanol, n-butanol, iso-
butanol, iso-
amyl alcohol, 2 ethyl hexanol, and mono and polyglycol.
10. A composition as claimed in claim 1, wherein the coupling agent component
is a
sulfonate selected from the group consisting of ligno sulfonate, petroleum
sulfonate,
sodium dodecyl benzene sulfonate, and sodium lauryl sulfate.
11. A composition as claimed in claim 1, wherein the alkali component is an
alkali
and alkaline earth metal salt selected from the group consisting of sodium
carbonate,
sodium hydrogen carbonate, calcium carbonate, and calcium oxide.
12. A composition as claimed in claim 1, wherein the composition is suitable
for use
as metal working fluid as admixture or emulsion with water in concentration
range from
20 to 80 weight percent.
13. A process for preparing the metalworking fluid composition as claimed in
claim
1, said process comprises the steps of;

12
a. removing of insoluble matter from the heavy alkylate followed by addition
of emulsifier and vegetable oil to obtain a mixture;
b. homogenizing the resultant mixture at a temperature in the range of
30° to
100° for about one hour with stirring;
c. adding the antioxidant, fungicide, extreme pressure additives, anti-rust
component, cosurfactant, coupling agent, alkali, followed by addition of water
to
make up the quantity about 1 kg, and
d. homogenizing the mixture for about 30 minutes, adjusting the pH of the
solution to 7-9 by addition of sodium carbonate and cooling the resultant
metal
working fluid at room temperature.
14. A process as claimed in claim 13, wherein the residual component of Alkyl
Benzene is a oil component having heavy alkyl benzene of C20 to C22 alkyl
carbon
number, a heavy fraction, by-product, separated from detergent class alkyl
benzene
during manufacture.
15. A process as claimed in claim 14, wherein the concentration of heavy alkyl
benzene component is in the range of 50 to 90 weight percent of the
metalworking fluid.
16. A process as claimed in claim 13, wherein the emulsifier is selected from
the
group consisting of heavy alkylate sodium sulfonates, sodium carboxylate,
sodium oleate,
triethanolamine oleate, diethanolamine oleate, dodecyl toluene sodium
sulfonate, and
mixtures thereof.
17. A process as claimed in claim 13, wherein the concentration of emulsifier
component is in the range of 10 to 40 weight percent or the metalworking
fluid.
18. A process as claimed in claim 13, wherein the vegetable oil component for
lubricity booster is selected from the group consisting of karanja oil, neem
oil, rice-bran
oil, castor oil, and mixtures thereof.
19. A process as claimed in claim 18, wherein the concentration of vegetable
oil
component for lubricity boost is in the range of 2 to 10 weight percent of the
metalworking fluid.

13
20. A process as claimed in claim 13, wherein the antioxidant component is an
alkyl
phenol or aromatic amine or substituted alkyl phenol selected from the group
consisting
of 2,6-ditertiary butyl phenol, 2,6-ditertiary p-cresol, diphenylamine,
tertiary butyl phenol
amino tetrazole, and 2,6-dioctyl phenylenediamine.
21. A process as claimed in claim 13, wherein the concentration of antioxidant
component is in the range of 50 to 500 ppm.
22. A process as claimed in claim 13, wherein the fungicide component is a
phenol or
phenolic acid selected from the group consisting of o-cresol, phenol. m-cresol
and
cresylic acid.
23. A process as claimed in claim 13, wherein the concentration of fungicide
component is in the range of 50 to 500 ppm.
24. A process as claimed in claim 13, wherein the extreme pressure additive
component is an organic sulfide or phosphosulfurized metal salt selected from
the group
consisting of dibenzyl disulphide, sulfurized vegetable oil, phosphosulfurized
decyl
oleate molybdate and phosphothio pentadecyl phenol molybdate.
25. A process as claimed in claim 13, wherein the concentration of extreme
pressure
additive component is in the range of 50 to 500 ppm.
26. A process as claimed in claim 13, wherein the anti-rust component is a
triazole or
sulfonate selected from the group consisting of 1H-benzotriazole, ditertiary
butylated,
1H-Benzotriazole calcium petroleum sulfonate and calcium heavy alkylate
sulfonate.
27. A process as claimed in claim 13, wherein the concentration of anti-rust
component is in the range of 50 to 500 ppm.
28. A process as claimed in claim 13, wherein the co-surfactant component is
an
alcohol selected from the group consisting of isopropanol, n-butanol, iso-
butanol, iso-
amyl alcohol, 2-ethyl-hexanol, and mono and polyglycol.
29. A process as claimed in claim 13, wherein the concentration of co-
surfactant
component is in the range of 1 to 10 weight percent of the metalworking fluid.

14
30. A process as claimed in claim 13, wherein the coupling agent component is
a
sulfonate selected from the group consisting of ligno sulfonate, petroleum
sulfonate,
sodium dodecyl benzene sulfonate, and sodium lauryl sulfate.
31. A process as claimed in claim 13, wherein the concentration of coupling
agent
component is in the range of 0.5 to 10 weight percent of the metalworking
fluid.
32. A process as claimed in claim 13, wherein the alkali component is an
alkali and
alkaline earth metal salt selected from the group consisting of sodium
carbonate, sodium
hydrogen carbonate, calcium carbonate, and calcium oxide.
33. A composition as claimed in claim 9, wherein the poly-glycol is selected
from the
group consisting of diethylene glycol and triethylene glycol.
34. A process as claimed in claim 28, wherein the poly-glycol is selected from
the
group consisting of diethylene glycol and triethylene glycol.
35. A composition as claimed in claim 10, wherein the sulfonate has a
molecular
weight less than 350.
36. A process as claimed in claim 30, wherein the sulfonate has a molecular
weight
less than 350.

Description

Note: Descriptions are shown in the official language in which they were submitted.


CA 02561351 2011-01-24
PROCESS FOR MAKING METAL WORKING FLUID FROM HEAVY ALKYLATE
b'IELD OF INVENTION:
The present invention relates to a process for metalworking fluids from heavy
alkylate.
More particularly this invention relates to composition of metalworking fluid
and process
for its preparation based on heavy alkyl benzenes having 22 to 26 alkyl carbon
atoms to
replace mineral oil.
BACKGROUND AND PRIOR ART OF THE INVENTION
Traditionally, the mineral oils and petroleum sulfonates have been the basic
source of
metalworking fluid formulations. The petroleum based lubricating oils and
sulfonates are
hydrocarbons of varying composition consisting of naphthenes, paraffins and
aromatics.
The sulfonates on the other hand formed by sulfonation of aromatic components
in these
lubricating oil streams act as oil/water emulsifiers. Besides these various
additives, which
are primarily chemicals of defined composition or structure, are added to the
soluble oils
to improve the physico-chemical properties and performance of metalworking
fluids.
Petroleum based soluble oils, generally suffer from many disadvantages such as
higher
toxicity to the environment, poor biodegradability and ever-changing
characteristics with
changes in crude oil composition. The other types of lubricants known as
synthetic
lubricants are designed for use in extreme conditions of temperature,
pressure, radiation
or chemical environment and have excellent lubricity and thermal stability.
The synthetic
lubricants are relatively costly as compared to petroleum based lubricants.
Poly-glycols,
polybutenes, dibasic acid esters, fluoropolymers, polyol esters, phosphate
esters,
silicones, poly-alpha olefins etc. are commonly used synthetic lubricants for
various
applications. Some of the synthetics are .also toxic to environment and are
not readily
biodegradable. Similar disadvantages are found with Petroleum sulfonates which
are by-
products of sulfonation of lubricating oils also suffer from inconsistent
emulsification and
compatibility characteristics due to everchanging composition of the
lubricating oils.
Keeping.in the view the environmental concerns and improved performance,
consistency
in structural and performance characteristics, there is a need to develop
alternative
lubricant and emulsifier component, for metalworking fluids, which are less
toxic and
1

CA 02561351 2011-01-24
!ow cost which show equivalent or improved performance to mineral oil or
synthetic
k bricant based metalworking fluids.
the use of Heavy alkyl benzene as lubricant is very limited. Recently, the
Heavy Alkyl
Benzene alkaline earth metal sulfonates are in use as detergent-dispersant-
anti rust
additive in various types of lubricants.
Reference may be made to MIS Petresa, Madrid, Spain, wherein they
:ire marketing heavy alkylate under the brand name of `PETRENE'M' to be used
as thermal
Iluid, transformer oil, refrigerating oil, sulfonation feedstock and
lubricating greases but
not for metalworking fluids.
o Rctcrcnce may be made to M/s Chevron, U.S.A. Inc., (San Ramon, CA) has US
patent
6,137,981 "Process for producing arylalkanes and arylalkanes sulfonates,
compositions
produced therefrom, and uses thereof'. Wherein this invention is a process for
producing
aryl-alkanes. This invention also provides process that to produce modified
allcylbenzene
3ulfonates, which can be used as detergents.
Chevron, U.S.A. Inc., (San Ramon, CA) has US patent 6,392,109 "Synthesis of
ilkylbenzenes and synlubes from Fischer-Tropsch products" which is for an
integrated
process for producing alkylbenzenes, sulfonated alkylbenzenes and/or
alkylcyclohexanes
1 om syngas and used as detergents and/or dispersants.
In view of the growing concern about the environment, there is a need for less-
toxic
lubricant component for metalworking soluble oil based on Heavy alkyl benzene,
which
i:~ a new application of the heavy alkylate. It will not only reduce the
toxicity of soluble
oil but also will be more cost effective than mineral oil because of improved
and
consistent performance because both the mineral oil component and the
sulfonates made
from these alkylates can be tailored to obtain a high performance product of
consistent
quality. It is an additional benefit to the alkylate industry.
SUMMARY OF INVENTION:
"lie present invention relates to a process for metalworking fluids from heavy
alkylate.
More particularly this invention relates to composition of metalworking fluid
and process
for its preparation based on heavy alkyl benzenes having 22 to 26 alkyl carbon
atoms to
rupiace mineral oil.
2

CA 02561351 2011-01-24
Flee speed of machining could be greatly increased if the cutting surface is
kept cool and
lubricated. Water can be regarded as the first cutting fluid because of its
high specific and
latent heats to give it unique potential cooling power and also it is
available everywhere
,it low cost. However, due to poor wetting efficiency, water alone can't cool
the metal
surface with its full ability. Another serious disadvantage is the formation
of rust on iron
;uid steel surfaces. Modern development has led to the introduction of
advanced water-oil
emulsion incorporating special chemicals, which considerably improve its
wettability,
lubrication, high cooling power, rust inhibiting and detergency properties.
These
concentrates and their emulsions in water are known as `Soluble Oil'. They are
ideal for
;Tcneral machining process where Cooling, Lubrication, Cleaning and extreme
pressure
characteristics are essential requirements.
One aspect of the present invention is to provide a process for metalworking
fluids from
heavy alkylate.
Another aspect of the present invention is to provide heavy alkylate based
less toxic
lubricant component metalworking fluids.
Still another aspect of the present invention is to provide a new application
to the by-
product heavy alkylate.
Yet another aspect of the present invention is to provide new composition of
metalworking fluid for the benefit of metalworking and alkylate manufacturing
industries.
DETAILED DESCRIPTION
Accordingly the present invention provides a process for metalworking fluid
from heavy
alkylate, which comprises ;
(a) residual fraction having C20 to C22 alkyl carbon atom of detergent class
Alkyl
Benzene in the concentration range of 50 to 90 weight percent of the metal
working fluid , (b) at least one emulsifier in the range of 10 to 40 weight
percent of the metalworking fluid, (c) at least one lubricity booster
component
in the concentration range of 2-10 percent of metal working fluid, (d) an
antioxidant component is in the concentration range of 50-500 ppm, (e) a
nungicide component in the concentration range of 50-500 ppm, (f) an extreme
3

CA 02561351 2010-08-05
pressure additive component in the concentration range of 50-500 ppm (g) an
antirust component in the concentration range of 50-500 ppm, (h) a co-
surfactant component in the range of 1-10 weight percent of metal working
fluid, (i) a coupling agent in the range of 0.5 to 10 weight percent of metal
working fluid, (j) alkali component in the range of 8-10 weight percent of
metal working fluid.
Heavy alkyl benzene is produced as by-products during the preparation of
linear alkyl
benzene sulfonates for detergent industry. The alkylation reaction of C)0-C14
olefin with
benzene results in side reactions to give dialkyl benzenes and alkylated
condensed ring
derivatives. These products are generally in the range of 5 to 15 percent of
the total
allcylates depending upon the reaction conditions and purity of reactants
employed.
Heavy alkyl benzene consists of substituted benzenes and Naphthalenes as
determined by
HPLC, UV, IR and RI analysis given in Table - 1. The typical properties such
as density,
kinetic viscosity, viscosity index, refractive index, pour point, molecular
weight and
distillation characteristics were given in Table - 2. No poly-aromatics or
olefinic
compounds are present in the heavy alkylates. These heavy alkylates have been
acquired
from the Indian market.
Table -1
Typical Relative Content of Alkyl Benzenes and Alkyl Napthalenes
Components HAB -I HAB - II
IR UV 254 IR UV 254
Alkyl Benzenes % by wt. 84 2 84 2 93 2 90 2
Alkyl Napthalenes % by wt. 15 2 16 2 7 2 10 2
Table - 2
Typical Characteristics of Heavy Alkyl Benzenes
Characteristics HAB - I HAB - II
Density at 15 C 0.8839 0.8813
K. Viscosity Cst at 40 C 28.95 26.93
K. Viscosity Cst at 100 C 4.50 4.31
Viscosity Index 37 32
4

CA 02561351 2011-01-24
Pour Point C (-) 27 (-) 25
Molecular wt. 365 5 361 5
Distillation range C (ASTM D1160) 225 - 440 226 -515
Refractive index at 20 C 1.4946 1.4916
In an embodiment of the present invention the oil component is a heavy alkyl
benzene
having C20-C22 alkyl carbon number, a heavy fraction, by-product, separated
from detergent
class alkyl benzene during manufacture.
In another embodiment of the present invention the concentration of heavy
alkyl benzene
component is in between 50 to 90 weight percent of the metalworking fluid.
In yet another embodiment of the present invention the emulsifier component is
a heavy
alkylate sodium sulfonates, sodium carboxylate, sodium oleate, triethanolamine
oleate,
diethanolamine oleate or dodecyl toluene sodium sulfonate or mixtures thereof.
In still another embodiment of the present invention the concentration of
emulsifier
component is in between 10 to 40 weight percent of the metalworking fluid.
In still another embodiment of the present invention the vegetable oil
component for
lubricity booster is a karanja oil, neem oil, rice-bran oil, castor oil or
mixtures thereof.
In still another embodiment of the present invention the concentration of
vegetable oil
component for lubricity boost is in between 2 to 10 weight percent of the
metalworking
fluid.
In still another embodiment of the present invention the antioxidant component
is an
alkyl phenol or aromatic amine or substituted alkyl phenol selected from 2,6-
ditertiary
butyl phenol, 2,6-ditertiary p-cresol, Diphenylamine, Tertiary butyl phenol
amino
tetrazole and 2,6-dioctyl phenylene diamine.
In still another embodiment of the present invention the concentration of
antioxidant
component is in between 50 to 500 ppm.
In still another embodiment of the present invention the fungicide component
is a phenol
or phenolic acid selected from o-cresol, phenol, m-cresol and cresylic acid.
In still another embodiment of the present invention the concentration of
fungicide
component is in between 50 to 500 ppm.
5

CA 02561351 2010-08-05
In still another embodiment of the present invention the extreme pressure
additive
component is an organic sulfide or phosphosulfurized metal salt selected from
dibenzyl
disulphide, sulfurized vegetable oil, phosphosulfiirized decyl oleate
molybdate and
phosphothio pentadecyl phenol molybdate.
In still another embodiment of the present invention the concentration of
extreme
pressure additive component is in between 50 to 500 ppm.
In still another embodiment of the present invention the anti-rust component
is a triazole
or sulfonate selected from 1H-benzotriazole, ditertiary butylated 1H-
Benzotriazole,
calcium petroleum sulfonate and calcium heavy alkylate sulfonate.
In still another embodiment of the present invention the concentration of ant-
rust
component is in between 50 to 500 ppm.
In still another embodiment of the present invention the co-surfactant
component is a
alcohol selected from isopropanol, n-butanol, iso-butanol, iso-amyl alcohol, 2
ethyl
hexanol, mono & poly glycol such as di ethylene glycol and tri ethylene
glycol.
In still another embodiment of the present invention the concentration of co-
surfactant
component is in between 1 to 10 weight percent of the metalworking fluid.
In still another embodiment of the present invention the coupling agent
component is a
sultonates (molecular weight less than 350) selected from ligno sulfonate,
petroleum
sulfonate, sodium dodecyl benzene sulfonate and sodium lauryl sulfate.
In still another embodiment of the present invention the concentration of
coupling agent
component is in between 0.5 to 10 weight percent of the metalworking fluid.
In still another embodiment of the present invention the alkali component is a
alkali and
alkaline earth metal salt selected from sodium carbonate, sodium hydrogen
carbonate,
calcium carbonate, calcium oxide.
In still another embodiment of the present invention the concentration of
alkali
component is in between 0.5 to 8 weight percent of the metalworking fluid.
In still another embodiment of the present invention the composition is
suitable for use as
metal working fluid and general emulsion as admixture with water in
concentration
ranging from 20 to 80 weight percent.
After the addition of all the components the mixture is homogenized. Then it
is
conditioned by keeping it at room temperature for 24 hours undisturbed. Dilute
emulsion
6

CA 02561351 2010-08-05
of the soluble oil may be prepared by mixing the concentrate in water with
vigorous
agitation for I to 5 minutes in the ratio of 20:80 to 80:20 as per
requirements of the metal
work and nature of metal.
It will be apparent from the foregoing that the present invention provides non-
toxic
lubricant component by using heavy alkyl benzene and useful for making
formulation for
weLalworking soluble oil. This invention further provides a suitable new
application for
heavy alkyl benzene as a by-product to increase its value.
The invention will now be further described by the following examples, which
are given
only for the purpose of illustration and not intended to limit the scope of
the invention.
Although the invention has been described in conjunction with examples and by
reference to the embodiments thereof, it is evident that many alternatives,
modifications
and variations will be apparent to those skilled in art in light of the
foregoing description,
accordingly it is intended in the invention to embrace these and all such
alternatives,
variations and modifications as may fall with in the sprit and scope of the
appended
'15 claims.
Example -1
After removal of insoluble matter, the heavy alkyl benzene in 65 weight
percent was
mixed with heavy alkyl benzene sodium sulfonate in 10 weight percent and
karanja oil 5
weight percent of metalworking fluid as component for lubricity. The mixture
was
homogenized at 30 to 100 C for one hour with stirring to obtain clear
solution. Then
ligno sulfonate as coupling agent.in concentration of 5 weight percent of the
fluid, 2,6,
ditertiary butyl 4 methyl phenol 100 ppm as antioxidant, cresylic acid 100 ppm
as
fungicide, dibenzyl disulfide 100 ppm as extreme pressure additive, 1H-
benzotriazole
100 ppm as antirust additive and isobutanol 5 weight percent of the
metalworking fluid as
co-surfactant were added. The mixture was further homogenized for 30 minutes.
Water
was added to make-up quantity to 1 kg and further homogenized for 30 minutes.
The pH
of the solution was adjusted to 7 - 9 by adding sodium carbonate. The solution
was
cooled down to room temperature with stirring. The final composition (HA - 1)
is given
in Table - 3. The neat soluble oil then mixed with water in 60:40 ratio and
shaken to
as produce oil-water emulsion. This emulsion was evaluated for its different
characteristics,
7

CA 02561351 2010-08-05
which are given in Table - 4 and 5. It was found that the characteristics of
the neat and
emulsion are at par with the specifications.
Table - 3
TYPICAL COMPOSITION OF SOLUBLE OIL
SN Constituents 1IA-I HA-II HA-III
I Heavy Alkyl Benzene % 65 60 75
2 Emulsifier % l0 15 10
3 Additives ppm 400 350 450
4 Co-surfactant % 6 5 7
5 Lubricity Additive 5 5 5
6 Coupling agent % .4 6 3
E S7 Alkali % 1 approx. 1 approx. 1 approx.
Water % 5 - 10 approx. 5 - 10 approx. 5 - 10 approx.
Example - 2
The procedure of Example I was repeated with alkylate 60 weight percent except
that
Dodecyl Toluene Sodium Sulfonate 15 weight percent was taken as emulsifier in
place of
'10 Heavy Alkyl Benzene Sodium Sulfonate, neem oil as component for lubricity
in place of
karanja oil, 2,6-dioctyl phenylene diamine as antioxidant in place of 2,6,-
ditertiary butyl
4-methyl phenol, m-cresol as fungicide in place of cresylic acid, phosphothio
pentadecyl
phenol as extreme pressure additive in place of dibenzyl disulphide. The final
composition (HA - 11) is given in Table - 3 and evaluation in Table-4 & 5.
Example - 3
The procedure of Example 1 was repeated with alkylate 75 weight percent except
that
Sodium Oleate 10 weight percent was taken as emulsifier in place of Heavy
Alkyl
Benzene Sodium Sulfonate. The final composition (HA - IIl) is given in Table -
3 and
evaluation in Table-4 & 5. It was found that the characteristics of the neat
and emulsion
are as per requirement.
Table - 4
TYPICAL CHARACTERISTICS OF SOLUBLE OIL
SN Formulation K.Viscosity Total Ash % Clarity Flash Reactable
40 C - Cst Acid No- Point C Sulfur at
8

CA 02561351 2010-08-05
mg KOH 100 C
I HA-I 23.3 NIL 0.009 Clear- 210 NIL
S 2IIA-II 26.2 NIL 0.008 Clear 215 NIL
3 IIA-III 24.5 NIL 0.006 Clear 213 NIL
Table - 5
TYPICAL EVALUATION OF SOLUBLE OIL
SN Formul Copper Deposit Emulsion Cast Saponificat Low temp Frothing
ation corrosion test stability iron rust ion value - Stability Test
mg KOH
11 IIA- I <1 NIL Pass Pass 4.8 Pass Pass
2 HA- II <1 NIL Pass Pass 4.5 Pass Pass
3 IIA- III < 1 NIL Pass Pass 4.6 Pass Pass
9

Representative Drawing

Sorry, the representative drawing for patent document number 2561351 was not found.

Administrative Status

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Event History

Description Date
Time Limit for Reversal Expired 2019-02-21
Letter Sent 2018-02-21
Change of Address or Method of Correspondence Request Received 2018-01-17
Grant by Issuance 2011-10-11
Inactive: Cover page published 2011-10-10
Inactive: Final fee received 2011-07-18
Pre-grant 2011-07-18
Notice of Allowance is Issued 2011-03-21
Letter Sent 2011-03-21
Notice of Allowance is Issued 2011-03-21
Inactive: Approved for allowance (AFA) 2011-03-17
Amendment Received - Voluntary Amendment 2011-01-24
Inactive: S.30(2) Rules - Examiner requisition 2010-09-30
Amendment Received - Voluntary Amendment 2010-08-05
Inactive: S.30(2) Rules - Examiner requisition 2010-02-05
Letter Sent 2008-05-13
Request for Examination Requirements Determined Compliant 2008-03-11
All Requirements for Examination Determined Compliant 2008-03-11
Request for Examination Received 2008-03-11
Inactive: IPRP received 2008-02-20
Letter Sent 2007-06-12
Inactive: Single transfer 2007-04-26
Inactive: Notice - National entry - No RFE 2006-12-06
Inactive: Courtesy letter - Evidence 2006-12-06
Inactive: Courtesy letter - Evidence 2006-11-28
Inactive: Cover page published 2006-11-24
Inactive: Notice - National entry - No RFE 2006-11-22
Inactive: IPRP received 2006-10-26
Application Received - PCT 2006-10-25
National Entry Requirements Determined Compliant 2006-09-26
Application Published (Open to Public Inspection) 2005-10-06

Abandonment History

There is no abandonment history.

Maintenance Fee

The last payment was received on 2010-12-03

Note : If the full payment has not been received on or before the date indicated, a further fee may be required which may be one of the following

  • the reinstatement fee;
  • the late payment fee; or
  • additional fee to reverse deemed expiry.

Patent fees are adjusted on the 1st of January every year. The amounts above are the current amounts if received by December 31 of the current year.
Please refer to the CIPO Patent Fees web page to see all current fee amounts.

Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
COUNCIL OF SCIENTIFIC & INDUSTRIAL RESEARCH
Past Owners on Record
ARUN KUMAR SINGH
ASHOK KUMAR GUPTA
ONKAR NATH ANAND
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
Documents

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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Description 2006-09-25 9 447
Abstract 2006-09-25 1 62
Claims 2006-09-25 6 233
Claims 2006-09-26 6 211
Description 2010-08-04 9 385
Claims 2010-08-04 5 205
Description 2011-01-23 9 382
Claims 2011-01-23 5 205
Reminder of maintenance fee due 2006-11-21 1 112
Notice of National Entry 2006-11-21 1 194
Notice of National Entry 2006-12-05 1 194
Courtesy - Certificate of registration (related document(s)) 2007-06-11 1 107
Acknowledgement of Request for Examination 2008-05-12 1 190
Commissioner's Notice - Application Found Allowable 2011-03-20 1 163
Maintenance Fee Notice 2018-04-03 1 180
PCT 2006-09-25 10 376
PCT 2006-09-26 13 505
Correspondence 2006-11-21 1 28
Correspondence 2006-12-05 1 28
Fees 2006-11-29 1 40
PCT 2006-09-26 12 520
Fees 2007-12-10 1 42
Fees 2009-02-05 1 50
Fees 2010-01-05 1 41
Fees 2010-12-02 1 41
Correspondence 2011-07-17 2 54