Title of Invention

"A PROCESS FOR METAL WORKING FLUID FROM HEAVY ALKYLATE"

Abstract The process relates to composition of metalworking fluid and for its preparation based on heavy alkyl benzenes having 22 to 26 carbon atoms to replace mineral oil and process for the same. A process for heavy alkylate based less toxic metalworking fluid composition comprising of 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 comprising of removing of insoluble matter from the heavy 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.
Full Text A PROCESS FOR METALWORKING FLUID FROM HEAVY ALKYLATE
Field 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 carbon atoms to replace mineral oil
Background and Prior Art References.
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 byproducts 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 low cost which show equivalent or improved performance to mineral oil or synthetic lubricant 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 M/S Petresa, Madrid, Spain, (www petresa es) wherein they are marketing heavy alkylate under the brand name of 'PETRENE' to be use as thermal fluid, transformer oil, refrigerating oil, sulfonation feedstock and lubricating greases but not for metalworking fluids
Reference may be made to M/s Chevron, USA Inc , (San Ramon, CA) has US patent 6,187,981 "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 alkylbenzene sulfonates, which can be used as detergents
Chevron, USA Inc, (San Ramon, CA) has US patent 6,392,109 "Synthesis of alkylbenzenes and synlubes from Fischer-Tropsch products" which is for an integrated process for producing alkylbenzenes, sulfonated alkylbenzenes and/or alkylcyclohexanes from 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 is 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 tailoied to obtain a high performance product of consistent quality It is an additional benefit to the alkylate industry Objects of the Invention.
The main objective of the present invention is to provide a process for metalworking fluids from heavy alkylate
Another object of the present invention is to pro\ ide heavy alkylate based less toxic lubricant component metalwoi king fluids
Still another object of the present invention is to provide a new application to the byproduct heavy alkylate
Yet another object of the present invention is to provide new composition of metalworking fluid for the benefit of metalworking and alkylate manufactunng industries
Summary 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 carbon atoms to replace mineral oil
The 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 at 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 and 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 general machining process where Cooling, Lubrication, Cleaning and extreme pressure characteristics are essential requirements Detailed description.
Accordingly the present invention provides a process for metalworking fluid from heavy alkylate, which comprises ,
(a) residual fraction having C20 to C22 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 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 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 C10-C14 olefin with benzene results in side reactions to give dialkyl benzenes and alkylated condensed ring derivatives These products aie generally in the range of 5 to 15 percent of the total alkylates 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 olefimc compounds are present in the heavy alkylates These heavy alkylates have been acquired fiom the Indian market
Table -1 Typical Relative Content of Alkyl Benzenes and Alkyl Napthalenes

(Table Removed)

Table – 2 Typical Characteristics of Heavy Alkyl Benzenes

(Table Removed)


In an embodiment of the present invention the oil component is a heavy alkvl benzene
having C20 - C22 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 >et another embodiment of the present invention the emulsifier component is a heavy
alkylate sodium sulfonates, sodium carboxylate, sodium oleate, Tnethalonoamine oleate,
Diethalonoamine 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
In still another embodiment of the present invention the extreme pressure additive
component is an organic sulfide or phosphosulfunztd metal salt selected from dibenzyl
disulphide, sulfunzed vegetable oil, phosphosulfunzed 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 tnazole
or sulfonate selected from 1 H-benzotnazole, ditertiary butylated 1 H-Benzotnazole,
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 tn 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 sulfonates (molecular weight less than 350) selected from hgno 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 of the soluble oil may be prepared by mixing the concentrate in water with vigorous agitation for 1 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 metalworking 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 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 hgno sulfonate as coupling agent in concentration of 5 weight percent of the fluid, 2,6, ditertiary butyl 4 methyl phenol 100 ppm as antioxidant, cresyhc acid 100 ppm as fungicide dibenzyl disulfide 100 ppm as extreme pressure additive, lH-benzotnazole 100 ppm as antirust additive and isobutanol 5 weight percent of the metalworking fluid as co-surfactant were added The mixture was further homogemzed 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
produce oil-water emulsion This emulsion was evaluated for its different characteristics, 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

(Table Removed)
Example - 2
The procedure of Example 1 was repeated with alkylate 60 weight percent except that Dodecyl Toluene Sodium Sulfonate 15 weight percent was taken as emulsifier in place of 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 cresyhc acid, phosphothio pentadecyl phenol as extreme pressure additive in place of dibenzyl disulphide The final composition (HA - II) 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 - III) 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
(Table Removed)
Table - 5 TYPICAL EVALUATION OF SOLUBLE OIL
(Table Removed)











We Claim :-
1. A metal working fluid composition from heavy alkylate, comprising,
(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) a vegetable oil which is selected from Karanja oil, rice bran oil, Mahua oil or
caster oil in the concentration of 2 to 10 parts (e) an antioxidant component is in the
concentration range of 50-500 ppm, (f) a fungicide component in the concentration range of
50-500 ppm, (g) an extreme pressure additive component in the concentration range of 50-
500 ppm (h) an antirust component in the concentration range of 50-500 ppm, (i) a co-
surfactant component in the range of 1-10 weight percent of metal working fluid, 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
2. A composition as claimed in claim 1, wherein the residual component of Alkyl Benzene is a oil component having heavy alkyl benzene of C20 - C22 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, Triethalonoamine oleate, Diethalonoamine oleate or Dodecyl Toluene sodium sulfonate or 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 or mixtures thereof
5. A composition as claimed in claim 1, wherein the antioxidant component is selected from the group consisting of an alkyl phenol aromatic amine, 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
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 cresyhc acid
7. A composition as claimed in claim 1, wherein the extreme pressure additive component is an organic sulfide or phosphosulfunzed metal salt selected from the group consisting of dibenzyl disulphide, sulfunzed vegetable oil, phosphosulfunzed decyl oleate molybdate and phosphothio pentadecyl phenol molybdate
8. A composition as claimed in claim 1, wherein the anti-rust component is a tnazole or sulfonate selected from the group consisting of 1 H-benzotnazole, ditertiary butylated 1 H-Benzotnazole, calcium petroleum sulfonate and calcium heavy alkylate sulfonate
9. A composition as claimed in claim 1, wherein the co-surfactant component is a alcohol selected from the group consisting of iso- propanol, n-butanol, iso-butanol, iso-amyl alcohol, 2 ethyl hexanol, mono & poly glycol selected from di ethylene glycol and tri ethylene

glycol.
10. A composition as claimed in claim 1, wherein the coupling agent component is a sulfonates (molecular weight less than 350) 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 a alkali and alkaline earth metal salt selected from the group consisting of sodium carbonate, sodium hydrogen carbonate, calcium carbonate and calcium oxide
12. A process for preparing metal working fluid as claimed in claim 1, the said process comprises the steps of
a) removing insoluble matter from the heavy alkylate followed by addition of emulsifier
and vegetable oil to obtain the mixture,
b) homogenizing the resultant mixture at a temperature in the range of
30 to 100°C for about one hour with stirring,
c) adding the antioxidant, fungicide, extreme pressure additives, anti trust component, cosurfactant, coupling agent, alkali, followed by addition of water to make up the quantity about 1kg, and
d) homogenizing the mixture for about 30 minutes, the pH of the solution was adjusted to 7-9 by addition of sodium carbonate and cooling the resultant metal working fluid at room temperature.

13. A process as claimed in claim 12, wherein the emulsifier is selected from the group consisting of heavy alkylate sodium sulfonates, sodium carboxylate, sodium oleate, Tnethalonoamine oleate, Diethalonoamine oleate or Dodecyl Toluene sodium sulfonate or mixtures thereof
14. A process as claimed in claim 12, wherein the concentration of emulsifier component is in the range of 10 to 40 weight percent of the metalworking fluid
15. A process as claimed in claim 12, wherein the concentration of vegetable oil component for lubricity boost is in the range of 2 to 10 weight percent of the metalworking fluid
16. A process as claimed in claim 12, wherein the antioxidant component is selected from the group consisting of an alkyl phenol, aromatic amine, 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
17. A process as claimed in claim 12, wherein the concentration of antioxidant component is in the range of 50 to 500 ppm
18. A process as claimed in claim 12, wherein the fungicide component is a phenol or phenolic acid selected from the group consisting of o-cresol, phenol, m-cresol and cresylic acid
19. A process as claimed in claim 12, wherein the concentration of fungicide component is

in the range of 50 to 500 ppm.
20. A process as claimed in claim 12, wherein the extreme pressure additive component is an organic sulfide or phosphosulfunzed metal salt selected from the group consisting of dibenzyl disulphide, sulfunzed vegetable oil, phosphosulfunzed decyl oleate molybdate and phosphothio pentadecyl phenol molybdate
21. A process as claimed in claim 12, wherein the concentration of extreme pressure additive component is in the range of 50 to 500 ppm
22. A process as claimed in claim 12, wherein the anti-rust component is a tnazole or sulfonate selected from the group consisting of 1 H-benzotnazole, ditertiary butylated 1 H-Benzotnazole, calcium petroleum sulfonate and calcium heavy alkylate sulfonate
23. A process as claimed in claim 12, wherein the concentration of anti-rust component is in the range of 50 to 500 ppm
24. A process as claimed in claim 12, wherein the co-surfactant component is a alcohol selected from the group consisting of isopropanol, n-butanol, iso-butanol, iso-amyl alcohol, 2 ethyl hexanol, mono & poly glycol such as di ethylene glycol and tri ethylene glycol
25. A process as claimed in claim 12, wherein the concentration of co-surfactant component is in the range of 1 to 10 weight percent of the metal working fluid 30 A process as claimed in claim 13, wherein the coupling agent component is a sulfonates (molecular weight less than 350) selected from the group consisting of ligno sulfonate, petroleum sulfonate, sodium dodecyl benzene sulfonate and sodium lauryl sulfate
26. A process as claimed in claim 12 wherein the concentration of coupling agent
component is in the range of 0 5 to 10 weight percent of the metalworking fluid
27. A process as claimed in claim 12, wherein the alkali component is a alkali and alkaline earth metal salt selected from the group consisting of sodium carbonate, sodium hydrogen carbonate, calcium carbonate, calcium oxide
28. A process for preparing metalworking fluid substantially as herein described with reference to the examples.

Documents:

666-del-2005-abstract.pdf

666-del-2005-Claims-(13-04-2011).pdf

666-del-2005-claims.pdf

666-del-2005-Correspondence Others-(13-04-2011).pdf

666-del-2005-correspondence-others.pdf

666-del-2005-description (complete).pdf

666-del-2005-form-1.pdf

666-del-2005-form-18.pdf

666-del-2005-form-2.pdf

666-del-2005-Form-3-(13-04-2011).pdf

666-del-2005-form-3.pdf

666-del-2005-form-5.pdf

666-del-2005-Petition-137-(13-04-2011).pdf


Patent Number 251864
Indian Patent Application Number 666/DEL/2005
PG Journal Number 16/2012
Publication Date 20-Apr-2012
Grant Date 12-Apr-2012
Date of Filing 28-Mar-2005
Name of Patentee COUNCIL OF SCIENTIFIC & INDUSTRIAL RESEARCH
Applicant Address ANUSANDHAN BHAWAN, RAFI MARG, NEW DELHI-110 001, INIDA.
Inventors:
# Inventor's Name Inventor's Address
1 SINGH ARUN KUMAR INDIAN INSTITUTE OF PETROLEUM, MOHKAMPUR, DEHRADUN 248005, UTTRANCHAL, INDIA.
2 GUPTA ASHOK KUMAR INDIAN INSTITUTE OF PETROLEUM, MOHKAMPUR, DEHRADUN 248005, UTTRANCHAL, INDIA.
3 ANAND ONKAR NATH INDIAN INSTITUTE OF PETROLEUM, MOHKAMPUR, DEHRADUN 248005, UTTRANCHAL, INDIA.
PCT International Classification Number C07C 2/16
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA 2004-03-26 U.S.A.