AU5844298A - Titanium complex grease compositions having performance additives and to a process and compositions thereof - Google Patents

Description

-1- Regulation 3.2

AUSTRALIA

PATENTS ACT 1990 COMPLETE SPECIFICATION FOR A STANDARD PATENT

(ORIGINAL)

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a a a..

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a a~ Name of Applicant Actual Inventors Address for Service Indian Oil Corporation Limited Anoop KUMAR, Subhash Chandra NAGAR, Kanta Prasad NAITHANI, Madan Mohan RAI and Akhilesh Kumar BHATNAGAR DAVIES COLLISON CAVE, Patent Attorneys, 1 Little Collins Street, Melbourne, 3000 Titanium complex grease compositions having performance additives and to a process and compositions thereof 52072/93 Invention Title Details of Parent Application No: The following statement is a full description of this invention, including the best method of performing it known to us: FIELD OF INVENTION The present invention relates to titanium complex grease compositions having performance additives and to a process and compositions thereof. The additives envisaged by the present invention include anti-oxidants, extreme pressure and antiwear additives, rust inhibitors, friction modifiers, structural modifiers, polymers, solid lubricants, biodegradable additives/ashless additives, multifunctional additives etc.

PRIOR ART 0 In prior art, the concept of thickening oils by soaps for lubrication purpose is well known. The usage of metallic soaps or their complex soaps as thickeners still dominates in lubricating greases. These metallic or complex metallic soap tase greases are generally derived from metals such as lithium, calcium, sodium, barium, aluminium etc. Lithium base greases are mainly used, and probably for their better performance, -2easily availability and cost factors etc. Metallic soaps based on other metals have also been reported in prior art Boner.Ind.Eng.Chem,29, 59, 1937). However such metallic soaps did not have advantageous application in lubricating greases.

Such commercially used greases are associated with one or other disadvantages and are not able to meet fully the various requirements of modern machinery. For instance, most widely used lithium base greases use LioH but the restricted availability of lithium constitutes a disadvantage. Further, lithium has questionable toxicity (NLGI Spokesman, Apr 1994). These greases require addition of certain performance additives which are costly and many of them are environmentally unsafe. The manufacture of such greases require large quantities of vegetable fats, which otherwise could have been used for edible and other industrial applications.

OBJECTS OF THE INVENTION A primary object of this invention is to propose Ti-complex grease compositions incorporating certain performance additives and to a process for the preparation thereof.

Another object of this invention is to propose novel lubricating grease compositions with improved extreme pressure and anti wear properties.

oo *o *o Still to propos improved

A

propose rust and ee another object of this invention is lubricating grease compositions having antioxidant properties.

further object of this invention novel grease compositions with corrosion inhibition properties.

is to improved Yet another object of this invention is to propose novel lubricating grease compositions with improved frictional properties.

-4- Again further object of this invention is propose lubricating grease compositions improved structural stability.

DESCRIPTION OF INVENTION to with 0 According to this invention there is provided a lubricating grease composition comprising 2 to 20% by weight of titanium alkoxide, 2 to 20% by weight of carboxylic acid, to 35.0% by weight of fatty acids, 0.0 to 5.0% by weight of water and 20 to 90% by weight of mineral/synthetic oil and 0.01 to 50% of performance additives.

In accordance of this inventic composition 2 to alkoxide, 5 to 25% t by weight of c weight of water a mineral/synthetic additives.

with a preferred embodiment :n the lubricating grease 20% by weight of titanium y weight of fatty acid, 2 to :arboxylic acid, 0.0 to 5.0% by nd 20 to 90% by weight of oil, and said performance The performance additives are selected frcom the following additives and present singularly or in any combination.

TABLE I1 S.NO. CLASS OF ADITIVIES 1. Extreme pressure 2. Antiwear additives 3. Antioxidant Anti rust! corrosion inhibitors 5. Friction modifiers 6. Structure modifiers/tackifier 7. Solid lubricants a 8.Multifunctional additives 9. Biodegradable additives Further according to this invention there is provided a process for the preparation of lubricating grea-ie composition which comprises in -6the steps of forming in a first stage a mix by adding together 2 to 20% fatty acid, 2 to carboxylic acid and 20 to 90% by weight of mineral or synthetic oil stirring and heating such a mix to a temperature of 70 to 100'C, adding in a second 2 to 20% by weight of titanium alkoxide while maintaining said temperature, raising the temperature to 100' to 200'C to form a thickened grease product, cooling said product, and in a 10 third stage adding 0 to 5% by weight of water thereto, if required, and then subjecting the .mixture to the step of shearing, adding performance additives at 140-60'C while cooling followed by homogenising/milling to obtain said composition.

In accordance with this invention, a vessel equipped with a stirrer or rpm 0-150 in the first stage, is charged with 5 to 35% by weight of fatty acid, 2 to 20% by weight of carboxylic acid and 20 to 90% by weight of mineral or synthetic oil, based on the total weight of the final grease composition.

-7-

I

The mixture is stirred and heat is provided through a heating mantle to reach the temperature to 70-100'C. At the end of the first stage, 2 to 20% by weight of titanium alkoxide is added slowly based on the total weight of the final grease composition.

0 The mixture is continuously mixed and held at 70-100'C for 1-2 hour, temperature being raised very slowly to 100-200'C, duration of maintaining 10 at this temperature is 2-8 hours. During this period the product assumes grease structure and converts to a thickened mass. The product is then cooled with continuous stirring to 140-100'C at the end of this second stage, if desired up to by weight of water is added to the mixture, based on the total weight of the final grease composition. The mixture is further cooled to 80-60'C and sheared with the help of a colloid mill.

It is, however, possible to combine the first and second stages to provide an alternate route.

Thus, according to this invention there is -8provided an alternate process for the preparation of a lubricating grease composition which comprises in preparaing in the first stage a mix by adding together fatty acid, carboxylic acid, titanium alkoxide and mineral or synthetic oil in required proporitions, heating such a mixture to a temperature of 160 to 200'C adding said additives at a temperature of 140 to 160'C while cooling and then subjecting the composition to the step of 10 homogenization and milling.

*In accordance with the alternate process of this invention, the charge is stirred with simultaneous heating through a heating mantle.

The mixture is heated upto a temperature of 15 160-200'C in 2-8 hours. The resultant product is cooled to 140-80'C and water is added from 0.1 to This is further stirred for 5 minutes to 1 hour at this temperature and then further cooled to 80-50'C and sheared in a colloid mill.

Titanium alkoxide used in present invention is preferably titaiium alkoxide of C3 to C6 alcohol having titanium metal content of 17% by weight approximately and used in the amount 2-20% by weight of the final lubricating grease composition. The synthetic hydrocarbon lubricating oil used in the compositions of present invention is an oligomer of olefin such as polyalpha olefins, polybutenes, polyehteres, mineral base stocks are the neutral oils.

The sources of fatty acids employed in the grease composition are alkyl carboxylic acids from vegetable source which may have few double bonds in the structure. For instance, it includes stearic acid, hydroxystearic acid, oleic acid, mahuwa oil, etc. and present in an amount of 15 to 35% by weight of the final lubricating grease composition.

The carboxylic acids employed in this invention are, for example, mono-carboxylic acid ranging from acetic acid to BVC acid C2 to C10 carbor. chain dicarboxylic acids, hydroxydicarboxylic acids such as tartaric acid and citric acid, aromatic acids include mono and dicarboxylic acids both, as well as hydroxy mono carboxylic acid, for example, benzoic acid, salicylic acid, phthalic acid, terepthalic acid, (Table Inclusion of inorganic acids like boric and phosphoric is also the illustration of present invention. This is present in an amount to 20% by weight of the final lubricating grease.

10 The comprehensive range of additives employed in this invention is categorised in Table 2 hereinbelow. These type of additives include hindered phenols, aminic compounds, amino-phenol compounds, thiophosphates and carbamates of Zn, Mo, 15 Sb, Bi, Ti, Pb etc., ashless thiophosphates, benzotraizoles, benzothiqzolines, benzothiazolinethione derivates, phosphites, various substituted amines, oligomers of quinolines, phpenothiazine, organo metallic complexes of copper, thiadiazole derivatives, alkyl/aryl derivatives of phosphates, soluble Mo type additives, petroleum/synthetic -11sulfonates of Ba, Na, Ca, Zn, Li etc., cverbased metal sutlfonates, borated compounds, saroccasi nes, imidazolibes, mono/dimetallic salts of discarbcixyjic acids, diesters of sebacic acids, mercptobenzothiazoles, linear iscibutylirte polymers, mehcyaefntoaie methacrylate coupolymer, methacrylate-styrene copolymer, ethylene-prcipylene copolymer, styrene diene copolymers, Mos2, graphite, resins, fumed silica etc.

The antioxidants are present in the amount of 0.01 tco 5% by weight.

The extreme pressure, antiwear, rust inhibito~r, friction modifier, and structure **modifier are each present in the amount of 0.01 to 10% by weight.

The compcositicon contains at least a single solid lubricant and present in the amount of 0.1 to 50% by weight.

-12- Table2 1. Antioixidants: The antioxidants employed in the process of the present invention are selected from one or more oif the following: u Phenolic antioxr~idants hindered phenols amino 4 hydrcoxy benzyl phosphorcodithioate Cyclic hindered phenyl borates Di-Bu-2, 6-di--tert-butyl phenyl borates Dibenzyl phencolic compounds 4 Dihydrocarbyl-alpha-cyanomethyl phenols): Bis-2, 6-tert--butyl phenol their sulphur containing~ derivative Phenyl alpha naphtylamine and NN' dimet hy 1 tet ra lone-hydrozone N, NF, N''-tri substituted bis (Paminobenzyl anilines (Aminlry) alkylamines (d)J 4( -phenyl ethyl)-2-hydroxydiphenyl amine PP' dioctyl diphenyl amine Mixed alkyl diphenyl amine -13- 9 10 9.

(iii) Aminophenol Antioxidants: N-substituted hydroxypheylthicimethyl amine or urides Octylated diphenyl amines (iv) Thic-phosphate based Antioxidants: Zn dialkyl dithiophosphates Ashless thio-phosphates Reaction product of dithiophosphoric acid ester and aldehyde S-(hydrc'xylphenyl: thiophosphates Eis (dialkyl dithiophosphate) alkylene p01 yam ine Combination of Mo, Bis (p-tert-butylphenyl) bis (p-nonylphenyl) and dialkyiphenyldi thiophosphates 99 *994 99 99 9 9 9 9 99 99 99 9 99.9..

9 Other Antioxidants Combination of Mo complexes of base and didc'decyl sulphides N-tert--octyl benzotriazole 1-(di(2-ethylhexy:) amino benzotr iazole Benzothiazolines Benzothiazcoline -thione derivative Mf (Benzc.) triazole Alkyl resorcinol phosphite Manni ch methyl: -14-

S

S S

S.

955.

*5S

S

*9 5* S S *5

S

*9

S

S.

S

S

*SS.

S

S

S

thiobis (alkyl phenol) dithiobis (altk.ylphenol I: 2(3,5-di tert-buityl-4-hydroxypheyl benzl-4-thiozolidinone Compo'sition of para butylated and cctylated ortho-ethylated dipheylamines Butoxy carbonyl phenyl animo methyl thiobenzo t h ia z 1e Complex of copper with 2-hydroxy-3naphthemic arylamides (in) 3,7-di-tert-octyl phenothiazine Oligomers of trimethyldiphydroquinoline Table 3 Extreme Pressure and Antiwear Additives: The extreme pressure and antiwear additives are selected from one or more of the following: i) Heterocycl ic C~ompounds: thiirane derivatives with thiopho--sphate thiocarbamates Benzothiazc'line thione Substituted dimercapto-thiadiazo:le Imidazc'lidlne dimethylene bis pho:sphoro di thioiate Mf Derivatives of nvridine. Dvrazine.

2.

pyrimidine and pyridazine and their fused ring derivatives (ii) Phosphates: Triaryl phosphates, triphenyl phosphates, tri tolyiphosphate, tr ixylyl phosphates and mixed aryl phosphates.

(iii) Metal Complexes: Zn and Mo dithiophosphate Souble Mo type additivies Zn diisopropyl dithiophosphate tetramethylenediamine Zn dipropylglycolate dithiophosphate Product of tallow, dietholamine and ammonium molybdate O~rrX(f) Mo oxysulfide dithio.:arbamate Sulfur ized oxy Mo orciano phosphorothioate Lead diamyl dithio:carbamate Organo Pb-S additive Antimo:ny diallkyl dithiocarbamate Sb dialkyl dithiocarbamate Ba petroleum sulfonate/synthetic barium dinonylnaphthalene sulfonate f*4) (J~bber TS~pes: Triphenyl phosphorothionate -16- TABLE 4 3. Friction Modifiers: The friction modifiers used in the present invention are selected from one or more the following: M:-C:omplexes: Mo dithiophosphates and Mo-dithi:carbamates.

Reaction product of sulfurised dodecyl so phenol and alk.ylbenzene sulfonic acid.

10 (C Overbased Mo-alkylene earth metal sulfonates.

55..

(ii) Bo:ron Derivatives: 2, 6-di-tert-butyl--4-methyl phenyl-borate.

Eorated polyhydroxy-alkyl sulfides.

**56 Borated N-hydrucarbyl alkylene triamines.

Product of boric acid and cocosy1 sarcosene.

Prcduct of 1 ,2-hexadecanediol,C19-C1I5 alcohols and boric acid.

20 Zinc salts of partially bcrated and partially phcsphosulfurised penta or dipentaerythritol.

(iii) Amines/Amidus/Hetrocylic Compounds: N-oleylglycolamide -17- N-alkoxylakylene diamine diamide N-cocr formam ide Dialk:'>y alkyl po-lyoxYlatl'Yl amines Dialkoxylated alkylpolyox'y alkyl amine Product of 4,4 thjodipheno~l, formaldehyde and cioecsoamines Reaction products with F205 and sub, oxazolifles or sub imidazolines Reaction products of sub hydro"xylmethyl imidazoline and acyl sarocosifle Salts of imidazolifles.

Rust and Corroision Inhibitors The rust and corrosion inhibitors used in the present invention are selected fro'm one or more of the following: Benzotriazole type /chemical derivative of benzcotriazole containing more than one benzotriazole nuclei.

N

0 yl-phefloxy-acetic acid.

N-acyl derivatives of sarcosine (N-methyl glytE3d) High molecular weight substituted imidazoline Disodium salt of an aliphatic dicarboxylic acid -18- Diesters cif sebaci': acid (gi) Z ine-di-n-butyldi thiucarbamate Sodium mercapto benzothic-azole Z-mercapto benzothiazole (j3) Zn dianyldithicecarbamate Ba petroleum sulfonate Sodium dinonyl naphthalene sulfonate (in) Zn dinonyl naphthalene sulfonate Li dinonyl naphthalene sulfonate Table 6 Multifunctional additives used in the present invention are: Alkyl derivative of 2, 5-di-mercapato:-1,3,4thiadiazole.

Table 7 Structure modifiers: The structure modifiers used in the present invention are selected from one or more of the fol lowingi: Linear iscubutylene polymer.

(ii) Methacrylic polymer/functionalised methacrylate copolymer.

(iii) Methacrylate-styrene copolymer.

-19- (iv) Ethylenepropylene vinyl alkyl ketone polymer.

Ethylene-propylene copolymers grafted with glycidyl methacrylates.

(vi) Styrene -diene copolymers (vii) Ester modified styrene diene polymers.

These performance additives have been added in the grease composition as single component or more in combination to get synergistic or antagonestic effects. The effect of these additives on 10 lubricating grease properites has been systematically studied by suitable evaluation techniques as per ASTM/ IP test methods as described in Table 8.

The total quantity of these additives alone/or in combination ranges from 0.01 to 50%. by weight.

TABLE 8 ASTM/IP STANTDARDS USED IN THE EVALUATION OF NEW GENERATION HIGH PERFORMANCE TITANIUM COMPLEX GREASE 1. Cone penetration of lubricating greases ASTM D-217 2. Drop point of lubricating greases ASTM D-566/D-2265 3. Life performace of automotive wheel ASTM D-3527 bearing grease.

4. Corrosion preventive properties of ASTM D-1743 lubricating greases.

Determination of EP/AW properties IP 239 of lubricants.

ma 6. Wear preventive characteristics of ASTM D-2266 lubricating greases. Four ball method.

7. Oxidation stability of lubricating ASTM D- 942 by the oxygen bomb method.

8. Determination of corrosiveness to IP-112 copper of lubricating grease strip method.

In order to describe more fully the nature of the present invention, specific examples will be hereinafter be described. It should be understood, 10 however, that this is done solely by way of example and is intended neither to delineate nor limit the ambit of the appended claims.

EXAMPLE NO. 1 The lubricating grease composition was prepared containing the ingredients with 15 proportionss indicated as described hereinbelow and following the process as indicated above. Here fatty acid used is stearic acid 5.6% and titanium alkoxide is titanium tetraisopoppoxide, Table 9 exemplifies the various carboxylic acids tried in the preparation of the lubrication grease of the present invention.

I

TABLE 9 Carbox4ylic acids used in the inventions S.NO. Carboxic Structure ac: i d Acetic acid 2. acid 3. Oxalic acid 4. Malcinic acid Succinic acid 6. IGlutaric acid 7. Azelaic acid 8. Sebacic ac:id 9. Tartaric acid Citric acid 11. Bencozcic acid 12. Salicylic: acid 13. Phthalic acid (orth' benzene dlimarbcsxylic

.COOH

(CiH COOH 3 2 n

(COOH)

2 CH (COOH)

(C:OOH)

(CH) (COOH) 28 2 (CH (H):OOH) (CH COOH 1282

(CH(OH)COOH)

12 CH COOH C H COOH 6 CH 6 4 C H (COOH) 6 42 acid) 14. Terephtalic ac~id (para benzene dicarbc'xylic C H (COOH:) 6 4 acid) -22- Fumari.: acid C-H COOH 2 16. Maleim: acid C:H C:OOH) 2 17. Cinnamiscacid C H C:H=C*:H-C:OOH 6 EXAMPLE NO.2 The lubricating grease composition was prepared as describedd in example 1 with a difference *that antio:xidants such as hindered phenols, amino phenols, cyclic hindered phenyl borates, aminic compounds ashless and metallic thiophosphates, 1o benzothiazoles, Ti-DTC, Bi-DTC, phosphites, complexes of *copper, quinolines, carbamates of Zn, Sb, Mo, Zinc dialkyldithiophosphate, dibenzyl paracresol, butylated (Mono/di) phenyl amines etc. were added in the concentration 0.01 10 at the temperature 140-160'C while coocling. The mass was then homogenised/milled to get final structure. Thus obtained greases were tested for critical properties such as drop pcoint, penetration, oxidation stability as per D 942 etc.

It was illustrated in this invention that these additives substantially influence the prcoperties -23spec:ific:ally grease.

oxidaticon resistance of the formul1ated 5 N.a For instance, the lubric:ating grease composition has been prepared containing ingredients with properties as described hereinabove. The antioxidant ditert butyl paracresol (0.01 was added in the composition at 80 1201C before milling or homoagenisinig. Following physicci chemical properties were exhibited by formulated grease.

TABLE S.NO. PROPERTY METHOD RESULTS 1. Penetration at 25 deg C D-217 267 after 60 strokes 2. Drop po~int deg C D 2265 292 a 3. Copper corrosion at 1001C after 24 hrs 4. Oxidation stability at 991C pressure drcop after 100 hrs.

psi IP-1 12 D-942 Pass 1 -24- Addition of ditert parabutyl crescil reduced pressure drop after 100 hirs i n ASTM D--942 f rom to 1.0 thus improving antioxidant properties.

The effectiveness of lubricating grease composition described demcsstrates its improved oxidation stability while retaining drop point, corrosion resistance etc.

EXA~MPLE NO. 3 Lubricating greases compositions were prepared as described in Example 1. The performance additives in these coamposition are specifically extreme pressure and antiwear additives viz, *sulfurised fat, carbamates, phosphates, sulphurised isobutylene, dibenzyl disulphide, thiadiazoles, i derivatives of pyridine, pyrazine, pyrimidine and pyridazine and their fused ring derivatives etc.

Carbamates are generally alkyl carbamates of Zn, Sb, Mo, Pb etc:. and alkyl phosphates specially derived frcom Zn, Mo:, Bi, Ti etc.

A0 s a typical examples, zinc dialkyl dithicicarbamate is added in the Ti-complex girease in the process as indicated hereinabove. The dosage ranges from 0.01 to 10.0%. The resultant grease exhibited following physicci chemical c:harac:ter ist ics.

TABLE 11 S.NO. PROPERTY METHOD RESULTS 1. Penetration at 25 degi C D-217 280 after 60 strokes 2. Drop point deg C D 2265 290 3. Copper 'crrosio:n IP-112 Pass 4. Weld load, kg IP-239 400 Wear scar dia, min. D-2266 0.50 Zn dialkyldithiocarbamate in Ti-complex grease has increased weld load from 250 kg. to 400 kg.

thus improvingi extreme pressure properties. This composition retained high drop point, good corrosion resistance while, giving improved extreme pressure and antiwear properties.

-26- N NNNNM EXAMPLE NO. 4 This example illustrates the wide range of rust inhibitors generally used in conventional lubricants and greases have been used to make different grease compositions by method described hereinabove. The dosage added between temperature 140- 60 deg C varies from 0.01 to 10.0%.

The wide range of rust inhibitors envisaaged by the present invention are generally 10 imidazolines, chemical derivatives of benzotriazole, sarcosines, metallic derivatives of dicarboxylic acids e.g. disodium sebacate, borates, mercapto benzothiazoles, sulfonate, amines and their derivatives. For instance, in one of the embodiment 15 disodium sebacate was added in concentration of 1-10 during the processing of Ti- complex grease.

Following physico-chemical characteristics were obtained with this composition.

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TAB'LE 12 S. NO PROPERTY METHOD RESULTS 1. Penetration at 25 deg C D-217 280 after 60 strokes 2. Drop point deg C D 2265 29 3. Copper c:orrosion IP-1 12 Pass A.4. Rust preventive properties D-1743 Pass Emcor rating 0 Therefore, this composition has exhibited, good 10 corrosion resistance, high drop points, improved rust preventive characteristics.

EXAMPLE Various structure modifiers were added during manufacture of Ti-complex grease. The grease compositions prepared with different type of structure modifiers are polymers viz, ethylene propylene, copcolymer, styrene hydrogenated butadiene (SBR) copolymer, styrne-isiprene (SI block copolymers, pclyisobutylene (PIEO polymers, nonelasomeric polymethacrylate (PMA) polymers etc.

resins waxes, clays, fumed silica etc. The chemicals/ -28- N MMWMW compounds were added in lubricating grease co~mpositions at a temperature of between 25 -200 deg C or while cooling the total mass. The lubricating greases obtained were tested for physico chemical charac:teristics and it was fouind that these components signific:antly influence properties of Ti-ccmmplex grease.

In one cof the preferred compousition, the lubricating grease compositing was prepared with I- 10 cof ethylene propylene type cospolymer. The corresponding Ti- complex grease exhibited following physico-':hemical c:haracteristics.

TABLE 13 S. NO. PROPERTY METHOD RESULTS 1. Penetration at 25 deg C D-217 270 after 60 strokes 2. Drop point, deg C: D 2265 290 3. Lub. life, hrs D 3527 160 -29- The composition has improved long high temperature life, while retaining other properties.

Example 6 5 This example relates to the usage of more than one type of additives in lubricating Ticomplex grease. The single composition consists of general type additives such as Anti-oxidants, Extreme pressure, AW additives, Rust inhibitors, structure 10 modifiers and rust inhibitors and similar various other combinations.

This invention is more clear by the following specific example. The lubricating grease composition was prepared by addition of 0.1 10 zinc dialkyl dithiocarbamate and 0.1 -10% sulfurized fat in the normal Ti- complex grease processing method. This composition exhibited certain excellent physico chemical characteristics.

r TAB3LE 14 S.NO. PROPERTY METHOD RESULTS 1. Worked penetration D-217 275 2. Drop point, degi C D 2265 296 3. Copper crrosioin IP-112 Pass 4. Weld load, Kg- IP-239 620 745. Wear Scar dia, mm D-2266 0.

This combinatio~n of additives inc~reased weld C.load from 350 kg to 620 kg. This compomsi tion possesses excellent high drop point, good corrosion **resistance, remarkably enhanc:ed extreme pressure properties. Similarly other sets of combinations also showed goo~d encouraging results.

EXAMPLE NO. 7 Here lubricating grease compcositions has been prepared consisting ingredients with proportion hereinabove. The example has a variation of addition of so:lid lubricants such as MoS2, graphite etc. As an specific example, 1-50%. McsS2 was added to' the grease composition and the -31following physico-chemical characteristics o:btained as shown in Table were TABILE

C.

4-I a a a a a S. a a S. NO. PROPERTY METHOD

REISULTS

1. Worked Penetration at 25deg C D-217 265 2. Drop point, deg C D 2265 295 3. Copper cor rosion IP-1 12 Pass 4. Oxidation stability, Psi drop D-942 I.0 after 100) hrs.

Weld load, kg IP-239 620 6. Wear scar dia, mm D-2266 Addition of MoS2 enhanced weld load from 350 kg. to 620 kg. This composition has specifically improved extreme pressure and antiwear properties.

-32J- EXAMPLE NO. 8 This example relates to the addition of more than one solid lubricant in single grease formulatio~n. These additives were added in the range 1-30. by weight of total concentration.

S

*5 S 5 *5

S

5 S S S S S. S S. .5 S S 5

S

An graphite -80 deg c hem ical in Table specific example, and 40%. Mc'S2 was C while cooclingi.

c:haracter ist ics cof the addition of effected at between 160 The following physico were cobtained as shown 16.

TABLE 16 S.NO. PROPERTY METHOD RESULTS 1. Worked Penetration, 25 deg C: D-217 270 2. Drop point, deg C D 2265 290 3. Weld load, kg IP-239 700 4. Wear scar dia, mm D-2266 0.55 -33- T hi s weld load cosmpos'it ion~ Gnraphite lu bric:a tin g composition has specifically shown, high and excellent antiwear properties. This has also shown synrgisim of MoS2 co'mbinatio~n as in case of other greases.

S

*5 5* 9. 9 9 995*

S.

9 S p

S

-34-

Claims (4)

1. A lubricating grease composition compr is ing 2 to 20%. by weight of titanium alkoxide, 2 to 20%. by weight of carbox;ylic ac:id, to 35.0%. by weight of fatty acids, 0.0 to by weight of water and 20 to 907. by weight of mineral/synthetic: oil and 0.01 to 50%. o:f performance additives.

2. A lubricant grease composition as claimed in claim 1 wherein said additives are antioxidants and present in an amount of 0.01 to

57. by weight. 3. claimed extreme present A lubricating grease coa:mposition as in c:laim 1 wherein said additives are pressure and antiwear additives, each in an amount of 0.01 to 10%7 by weight. 4. A lubricating grease composition as claimed in claim I wherein said additives are rust inhibitors and present in an amount of 0.01 to by weight. A lubricating grease composition as claimed in claim 1 wherein said additives are friction modifiers and present in an amount of 0.01 to 10% by weight. C.. 6. A lubricating grease composition as claimed in claim 1 wherein said additives are structure modifiers and present in an amount of 0.01 to by weight. o 4*C 10 7. A lubricating grease composition as claimed in claim 1 containing at least a single solid lubricants and present in an amount of 0.1 to by weight. 8. A lubricating grease composition as claimed in claim 1 comprising a first and second solid lubricant and present in the ratio of 1:99 to 99:1. -36- 9. A process for the preparation of a lubricating grease composition which comprises in the steps of forming in a first stage a mix by adding together fatty acid, carboxylic acid and mineral or synthetic oil stirring and heating such a mix to a temperature of 70 to 100'C, adding in a second stage titanium dioxide while maintaining said temperature, raising the temperature to 100' to 200'C to form a thickened grease product, cooling S: 10 said product, and in a third stage adding water thereto, if required, and then subjecting the mixture to the step of shearing, adding performance additives at 140 to 60'C whle cooling followed by homogenizing/milling. o S 15 10. A process as claimed in claim 13 wherein 2 to 20% of titanium alkoxide is added. 11. A process as claimed in claim 9 wherein the mixture in the first stage is continuously mixed and held at 70-100'C for 1-2 hours and in the second stage at a temperature of 100 to -37- 200'C for a period of 2 to- 8 hours. 12. A process as claimed in claim 9 wherein the mix is cooled with continuous stirring to

140-100'C and 0-5% by wt. of water is addded. 5 13. A process for the preparation of a lubricating grease composition which comprises in preparing in the first stage a mix by adding together fatty acid, carboxylic acid, titanium alkoxide and mineral or synthetic oil, heating such a mixture to 10 a temperature of 160 to 200'C, cooling the resultant mix and in the second stage adding water, if required thereto, stirring the cooled mix and then further cooling said mix and adding additives thereto and 0* 0 subjecting it to the step of shearing. 14. A process as claimed in claim 13 wherein said mixture is cooled upto a temperature of 140 to 80'C in 2 to 8 hours. A process as claimed in claims 9 to 14 wherein said additives are antioxidants and present -38- P:\OPER\ADD\INDOIL.CLM 13/3/98 in an amount of 0.01 to 5% by weight. 16. A process as claimed in claims 9 to 14 wherein said additives are extreme pressure and antiwear additives, each present in an amount of 0.01 to 10% by weight. .17. A process as claimed in claims 9 to 14 wherein said additives are rust inhibitors and present in an amount of 0.01 to 10% by weight. 18. A process as claimed in claims 9 to 14 wherein said additives are friction modifiers and present in an amount of S0.01 to 10% by weight. 15 19. A process as claimed in claims 9 to 14 wherein said additives are structure modifiers and present in an amount of S. 0.01 to 10% by weight. A lubricating grease composition and/or a method of preparing same substantially as hereinbefore described with reference to the Examples. 21. The steps, features, compositions and compounds disclosed herein or referred to or indicated in the specification and/or claims of this application individually or collectively, and any and all combinations of any two or more of said steps or features. 39