GB2215346A - Lithium complex lubricating grease - Google Patents

Lithium complex lubricating grease Download PDF

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Publication number
GB2215346A
GB2215346A GB8805551A GB8805551A GB2215346A GB 2215346 A GB2215346 A GB 2215346A GB 8805551 A GB8805551 A GB 8805551A GB 8805551 A GB8805551 A GB 8805551A GB 2215346 A GB2215346 A GB 2215346A
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Prior art keywords
acid
grease composition
grease
temperature
lithium
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GB8805551A
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GB2215346B (en
GB8805551D0 (en
Inventor
Lothar Endom
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ExxonMobil Technology and Engineering Co
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Exxon Research and Engineering Co
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Priority to GB8805551A priority Critical patent/GB2215346B/en
Publication of GB8805551D0 publication Critical patent/GB8805551D0/en
Priority to DE3907234A priority patent/DE3907234A1/en
Publication of GB2215346A publication Critical patent/GB2215346A/en
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M123/00—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential
    • C10M123/02—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential at least one of them being a non-macromolecular compound
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/063—Peroxides
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/087—Boron oxides, acids or salts
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    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
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    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102—Aliphatic fractions
    • C—CHEMISTRY; METALLURGY
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102—Aliphatic fractions
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/104—Aromatic fractions
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/106—Naphthenic fractions
    • C10M2203/1065—Naphthenic fractions used as base material
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    • C10M2203/108—Residual fractions, e.g. bright stocks
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    • C10M2207/02—Hydroxy compounds
    • C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/022—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups
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    • C10M2207/02—Hydroxy compounds
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/124—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof
    • C10M2207/1245—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof used as thickening agent
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    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
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    • C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
    • C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
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    • C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/141—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic
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    • C10M2207/141—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic
    • C10M2207/1415—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic used as thickening agent
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    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
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    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
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Description

Lubricating Grease The present invention relates to a lubricating grease,
in particular to a lithium complex grease composition which is suitable for use in hub units of passenger cars. For safety reasons more and more passenger cars are being equipped with double row angular contact ball bearings at the front axle instead of cone roller bearings. The double row angular contact ball bearings are combined with other parts in a so-called "Hub-Unit (of the second generation)", which is produced by bearing manufacturers. The units are delivered to the car industry grease-filled with a fill-for- life grease. However, hub-units suffer from the drawback that they tend to suffer from fretting corrosion (trough-like indentations) at the inner and outer rings when cars are transported over long distances by ship, rail or truck. These "standstill marks" cause noisy operation or even complete failure of the bearings. It is of German cars with hub-units estimated, for example, that about 104 are rejected by American customers due to fretting corrosion.
Attempts have been made by the ball bearings and automobile industries to find a remedy for this phenomenon. Changes in constructional design and/or in the materials employed have been proposed, but no satisfactory solution has yet been achieved.
An object of the present invention is to overcome this problem by providino an improved lubricating grease for use in such filled-for-life hub-units.
The basic performance requirements for suitable greases for hub-units are as follows:
T 1 a Operating range -40C to +150C, i.e.
(i) Low temperature torque at -40C (ASTM D 1478): pass (ii) High temperature test in bearing Rig FAG FE 9 (DIN 51821) at 150'C: L50 min 100 h (iii) Ambient temperature test in bearing Rig FAG FE 8: min 500 h a pass No fretting corrosion, i.e. BMW standstill vibration Rig:
a Effective corrosion protection i.e. Emcor corrosion test (DIN 51 802): rating max. 0 0 No considerable shrinking or swelling of seals i.e. seal compatibility with Neoprene: pass In accordance with one aspect of the invention there is provided a lithium complex grease composition containing a major proportion of mineral lubricating oil and from 12 to 22 mass 0%), preferably 13 to 18 mass 510, in total of a thickener comprising at least one lithium soap Of 8 12-14 hydroxy fatty acid, at least one lithium salt of boric acid, at least one lithium salt of a hydroxy benzoic acid, and at least one polyol grease structure modifier; the grease having a worked penetration in the range 280 to 330.
Preferably the hydroxy fatty acid will be a 16-2O such acid, and may be unsaturated or saturated. Monocarboxylic fatty acids are especially preferred. An hydroxy stearic acid is a preferred material, more especially 12-hyroxy stearic acid.
A T The hydroxybenzoic acid may be, for example, parahydroxybenzoic acid; salicylic acid; 2-hydroxy-4-hexylbenzoic acid; metahydroxybenzoic acid; 2, 5-dihydroxybenzoic acid (gentistic acid); 2,6-dihydroxybenzoic acid (gamma resorcyclic acid); or 4-hydroxy4-methoxybenzoic acid. Preferred are salicylic acid, and parahydroxybenzoic acid, more especially the former.
In accordance with an important feature of the invention instead of the free hydroxy acid of the latter type one can use a lower alcohol ester, e. g. the methyl, ethyl, or propyl, isopropyl, or sec-butyl ester of the acid, e.g. methyl salicylate, to give a better dispersion. A C1-3 such ester is preferred, especially the methyl ester.
The polyol grease structure modifier is suitably an aliphatic compound having from 2 to 6 hydroxy groups. Examples are 02-6 diols, polyalkylene glycols, and trihydric alcohols, especially glycerol.
The lithium borate present in the lithium complex grease of the invention may be, for example, metaborate, diborate, tetraborate or orthoborate such as monolithium orthoborate. A monolithium compound is preferred.
The lubricating oil of the complex grease is essentially one or more mineral lubricating oils. Such oil(s') will geneially have a viscosity of 95 to 120 mm2/s at 400C, and may be derived from paraffinic, naphthenic and mixed based crudes.
The greases of the invention may, of course, include one or more normal grease additives. For example, oxidation inhibitors, extreme-pressure additives, rust and corrosion inhibitors and dyestuffs. Such additives will be present in proportions conventional in lubricating greases.
i7 Preferred greases of the invention, without additives, have an alkalinity (ASTM D 128) of from 1.1 to 1.5 mass.1. NaOH, more especially 1.2 to 1.4. This enables dropping points of 290 to 350C to be achieved, more normally 290 to 340'C. Preferred greases of the invention have a 60-stroke worked penetration (ASTM D 217) of from 300 to 330 mm-1.
The accompanying Fig 1. illustrates the nature of relationship possible, in accordance with the invention, between dropping point and worked penetration on the one hand and alkalinity on the other.
The combination of (i) a worked penetration from 280 to 330, more especially 300 to 330, and (ii) a thickener content of 12 to 22 0, mass o, more especially 13 to 18, enables a grease of the present invention to meet the aforestated requirements of Operating range and fretting corrosion.
If the worked penetration is above 330 considerable leakage from a hub unit occurs at 15TC. If below 290 the low temperature (-40'C) torque and fretting corrosion prevention requirements are not met. A thickener content above 22 mass % results in unacceptable low temperature behaviour, and less than 12 mass 110 results in failure in the standstill vibration tests.
In accordance with another aspect of the invention there is provided a method of manufacturing the lithium complex grease composition hereinbefore defined, wherein the mineral oil and the components for forming the thickener are heated in a reactor, and the heating is conducted so that the maximum temperature of the bulk in the reactor lies in the range 190 to 205% and the wall temperature of the reactor is at a temperature in the range of 40 to 6TC, preferably 45 to 55% above the temperature of the bulk.
a Preferably the said temperature of the bulk lies in the range 190 to 20TC. There exists a relationship between the bulk temperature and the temperature gradient reactor (kettle) wall/grease bulk temperature on the one hand and the worked penetration on the other. Fig 1 illustrates this.
It has been unexpectedly found that close control on the bulk temperature and the said temperature gradient enables a grease to be produced having the properties required for a filled-for-life hub unit grease.
The following Table illustrates the proportions (mass '%) of components which may be employed:
12-Hydroxy-stearic acid Methyl salicylate Boric acid Glycerol Lithium hydroxide monolydrate Conventional additives Base Oil Mass "' M ass _ 151o 0 11. 5 to 18. 0 2.45 3.85 0.95 1.50 0.15 0.30 3.60 5.40 3.00 3.70 Example Mass % 13.5 2.88 1.10 0.22 3.80 3.05 Substantially wholly the remainder The following Example illustrates the preparation of one grease of the present invention:- 12 hydroxy-stearic acid and 2.88 M 100 13.5 M I'D methylsalicylate are dissolved in 50 m ',o Stanco Base 600. The thickening ingredients are heated and reacted with an aqueous solution consisting of boric acid (1.10 m %), glycerol (0.22) m 53b and lithium hydroxide (3.80 m 110) and hot water. This recipe results an alkalinity of 1.2 m % NaOH (referred to the total formulation). After the saponification, 15 m DD, base stock is added and the components are heated to a bulk temperature of 195C and a wall temperature of 235 to 255'C. After rapid cooling by base stock and kettle jacket cooling to 150% an oxidation inhibitor and zinc naphthenate are incorporated. Before consistency adjustment 0.5 m 11,0 Arquad-2c-Nit rite and dissolved Ebano 80 (10.4 m 0%) are added at about 7TC. The adjusted grease is milled, filtered and deaerated before packaging.
The grease thus prepared had the following properties:
Alkalinity m 110 NaOH Worked penetration Dropping Point 'C Water Washout Rating (DIN 51807) 1.20 320 >300 2 This grease was then compared with 7 commercially available greases of the types shown in Table 1. The comparison took the form of six tests. These tests and the results obtained are as shown in Table 2.
It wJLll be seen that only the grease of the present invention passes all requirements.
1:
11 TABLE 1
PERFORMANCE CHARACTERISTICS Low Temp Bearing Bearing Fretting Corrosion Seal Designation Type Tor ue Test FE 9 Test FE 8 (4) Corrosion Protection Compatibility -40 3 C (2) 150 0 C (3) BMW (5) Emcor (6) Neoprene (7) 1 Li-Soap pass 29 h (fail) n.t. fail Offl pass 2 Ca-Complex pass 69 h (fail) borderline fail Offl pass 3 Poly Urea fail 40 h (fail) fail pass M pass 4 Li-Complex fail 160 h (pass) pass fail Offl pass Ca-Complex fail 65 h (fail) borderline n.t. M pass 6 Li-Complex(l) paqs 260 h (pass) pass pass 0;0 fail 7 Bentonite + fail 198 h (pass) pass pass M pass Li-Complex The invention Modified pass 122 h (pass) pass pass M pass Li-Complex (1) Synthetic base stock; diester base fluid.
(2) ASTM D 1478 (3) DTN 51821 to (4) Described in "Gebrauchswertprufung von Schmierfetten f8r nochbeanspruchte WC'I'lzlager", E. Kleinlein and 11. Schemmel, Schmiertechnik und Tribologie, Vol 2, 1976, 23rd year.
(5) BMW Standstill Vibration Rig Test.
(6) DIN 51802 (7) Compatibility with Seal Material 7d/700 0 c Elastomer DIN 51538 S RE-NBR11.
Volume - Change max -1) DIN 53521 +5) n.t = not tested

Claims (11)

CLAIMS:
1. A lithium complex grease composition containing a major pro-portion of mineral lubricating oil and from 12 to 22 mass %, preferably 13 to 18 mass 14 in total of a thickener comprising at least one lithium soap Of a C12-14 hydroxy fatty acid, at least one lithium salt of boric acid, at least one lithium salt of a hydroxy benzoic acid, and at least one polyol grease structure modifier; the grease having a worked penetration in the range 280 to 330.
2. A grease composition as claimed in claim 1, wherein the hydroxy fatty acid is a C16-20 such acid.
3. A grease composition as claimed in claim 2, wherein the acid is a hydroxy stearic acid, preferably 12-hydroxy stearic acid.
4. A grease composition as claimed in any preceding claim wherein the hydroxy benzoic acid is salicylic acid.
5. A grease composition as claimed in any preceding claim, wherein the polyol is glycerol.
6. A grease composition as claimed in any preceding claim and having a dropping point of 290 to 35TC.
7. A grease composition as claimed in claim 1 and substantially described herein with or without reference to the accompanying drawings.
i 1 1 : 0.
k a. A method of manufacturing the lithium complex grease composition defined in any preceding claim, wherein the mineral oil and the components for forming the thickener are heated in a reactor, the heating being conducted such that the maximum temperature of the bulk in the reactor lies in the range 190 to 205% and the wall temperature of the reactor is at a temperature in the range of 40 to 60% preferably 45 to 55% above the temperature of the bulk.
9. A method as claimed in claim 8, wherein the temperature of the bulk is in the range 190 to 20TC.
10. A method as claimed in claim 8 or 9, wherein the amount of lithium hydroxide used in forming the thickener is from 1.2 to 1.4 mass % (calculated as sodium hydroxide) in excess of that required for neutralisation of the acids employed.
11. A method as claimed in any one of claims 8 to 1[), wherein a C1-3 alkyl ester, preferably the methylester, of the hydroxybenzoic acid is employed, partly or wholly in place of the free acid.
Published.1989 atThePatent OMoe, State House, 65,171 HI& Holborn, LondonWClR4TP. Further copies maybe obtained from The PatentOffice. Baas Branch, St Mary Cray, Orpington, Kent BR5 3RD. Printed by Multiplex techniques ltd, st Mary Cray, Kent, Con. 1/87 4
GB8805551A 1988-03-09 1988-03-09 Lubricating grease Expired - Lifetime GB2215346B (en)

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DE3907234A DE3907234A1 (en) 1988-03-09 1989-03-07 LUBRICATING GREASE COMPOSITION

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991013955A1 (en) * 1990-03-07 1991-09-19 Exxon Research And Engineering Company Lubricating grease composition
US6214778B1 (en) 1995-08-24 2001-04-10 The Lubrizol Corporation Polyurea-thickened grease composition
CN104164290A (en) * 2014-08-05 2014-11-26 中国石油化工股份有限公司 Crusher upper arm support shaft sleeve lubricating grease composition and preparation method
US9157045B2 (en) 2013-11-27 2015-10-13 Chevron U.S.A. Inc. Continuous lithium complex grease manufacturing process with a borated additive

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0084910A2 (en) * 1982-01-21 1983-08-03 Shell Internationale Researchmaatschappij B.V. High dropping-point lithium-complex grease having improved anti-noise properties
EP0096919A2 (en) * 1982-06-14 1983-12-28 Shell Internationale Researchmaatschappij B.V. High dropping-point lithium-complex grease composition having improved extreme pressure properties

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0084910A2 (en) * 1982-01-21 1983-08-03 Shell Internationale Researchmaatschappij B.V. High dropping-point lithium-complex grease having improved anti-noise properties
EP0096919A2 (en) * 1982-06-14 1983-12-28 Shell Internationale Researchmaatschappij B.V. High dropping-point lithium-complex grease composition having improved extreme pressure properties

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991013955A1 (en) * 1990-03-07 1991-09-19 Exxon Research And Engineering Company Lubricating grease composition
US6214778B1 (en) 1995-08-24 2001-04-10 The Lubrizol Corporation Polyurea-thickened grease composition
US9157045B2 (en) 2013-11-27 2015-10-13 Chevron U.S.A. Inc. Continuous lithium complex grease manufacturing process with a borated additive
CN104164290A (en) * 2014-08-05 2014-11-26 中国石油化工股份有限公司 Crusher upper arm support shaft sleeve lubricating grease composition and preparation method
CN104164290B (en) * 2014-08-05 2017-05-31 中国石油化工股份有限公司 Arm support shaft sleeve lubricating oil/fat composition and preparation method on disintegrating machine

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GB8805551D0 (en) 1988-04-07
DE3907234A1 (en) 1989-09-21

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