EP3060635B1 - Use of calcium salicylate to improve roll stability in a grease composition - Google Patents

Use of calcium salicylate to improve roll stability in a grease composition Download PDF

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Publication number
EP3060635B1
EP3060635B1 EP14786932.5A EP14786932A EP3060635B1 EP 3060635 B1 EP3060635 B1 EP 3060635B1 EP 14786932 A EP14786932 A EP 14786932A EP 3060635 B1 EP3060635 B1 EP 3060635B1
Authority
EP
European Patent Office
Prior art keywords
roll stability
grease composition
calcium salicylate
thickener
calcium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
EP14786932.5A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP3060635A1 (en
Inventor
Edward Alexander WORTHINGTON
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shell Internationale Research Maatschappij BV
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Shell Internationale Research Maatschappij BV
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Publication date
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Priority to EP14786932.5A priority Critical patent/EP3060635B1/en
Publication of EP3060635A1 publication Critical patent/EP3060635A1/en
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Classifications

    • 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
    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26—Carboxylic acids; Salts thereof
    • C10M129/48—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring
    • C10M129/54—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring containing hydroxy groups
    • 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
    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26—Carboxylic acids; Salts thereof
    • 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
    • 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
    • C10M2203/102—Aliphatic fractions
    • 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
    • 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
    • C10M2207/125—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
    • C10M2207/126—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 monocarboxylic
    • 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
    • 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
    • C10M2207/125—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
    • 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
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/144—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings containing hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/68—Shear stability
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy

Definitions

  • This invention relates to a grease composition having improved roll stability.
  • Roll stability is a measure of the stability of a grease when subjected to mechanical shearing.
  • ASTM D 1831 grease is placed in a cylinder containing a steel roller and the cylinder is rotated. The penetration of the grease is measured before and after the test, and the difference in penetration values indicates the roll stability.
  • US4719023 discloses the use of magnesium and calcium salts of C5-C50-alkyl salicylates in greases. The present inventors have sought to provide grease compositions having improved roll stability.
  • the present inventors have surprisingly found that adding calcium salicylate to grease compositions can improve roll stability. Accordingly the present invention provides the use of calcium salicylate to improve roll stability in a grease composition comprising a base oil and a fatty acid salt of lithium and/or calcium, wherein the roll stability is measured according to ASTM D 1831.
  • the present invention provides the use of calcium salicylate to improve roll stability in a grease composition.
  • the method for measuring roll stability is defined in ASTM D 1831.
  • the duration of the cylinder rotation may be varied but is preferably from 1 to 200 hours, more preferably from 10 to 50 hours and most preferably is 18 hours.
  • the temperature during the cylinder rotation may be varied, e.g. from room temperature to 100°C, but is preferably 65°C.
  • Suitably water is mixed with the grease before the roll stability is measured, e.g. 10wt% water based upon the weight of the grease composition.
  • the roll stability is determined by the difference in penetration before and after the roll stability test. Penetration is suitably measured by the method defined in ASTM D 1403 and is typically reported in 0.1mm. A small difference in penetration (particularly below 100 0.1mm) is indicative of good roll stability, whereas a large difference in penetration (particularly above 100 0.1mm) is indicative of poor roll stability.
  • calcium salicylate is incorporated in a grease composition to improve roll stability.
  • the roll stability of the grease composition is better than the roll stability of an otherwise identical grease composition that does not contain calcium salicylate (i.e. the penetration difference is lower for the grease composition than for an otherwise identical grease composition that does not contain calcium salicylate).
  • the amount of calcium salicylate that is suitably incorporated into the grease composition to improve roll stability is suitably from 0.3 to 0.6wt% based upon the weight of the grease composition.
  • the inventors have found that using less than 0.3wt% calcium salicylate does not give the desired improvement in roll stability and using more than 0.6wt% provides no further improvement.
  • the calcium salicylate is suitably overbased calcium salicylate.
  • the base oil in the grease composition is one which may ordinarily be used as the base oil of a grease composition and there are no special restrictions.
  • the base oil is suitably chosen from mineral oils, synthetic oils, animal and plant oils, and mixtures thereof.
  • base oils which belong to Group I, Group II, Group III, Group IV and so on of the API (American Petroleum Institute) base oil categories.
  • Group I base oils include, for example, paraffinic mineral oils obtained by a suitable combination of refining processes such as solvent refining, hydrorefining, and dewaxing in respect of lubricating oil fractions obtained by atmospheric distillation of crude oil.
  • Group II base oils include, for example, paraffinic mineral oils obtained by a suitable combination of refining processes such as hydrorefining and dewaxing in respect of lubricating oil fractions obtained by atmospheric distillation of crude oil.
  • Group III base oils and Group II+ base oils include paraffinic mineral oils manufactured by a high degree of hydrorefining in respect of lubricating oil fractions obtained by atmospheric distillation of crude oil, base oils refined by the Isodewax process which dewaxes and substitutes the wax produced by the dewaxing process with isoparaffins, and base oils refined by the Mobil wax isomerisation process.
  • synthetic oils include polyolefins, polyoxyalkylene glycols such as polyethylene glycol or polypropylene glycol, esters such as di-2-ethylhexyl sebacate or di-2-ethylhexyl adipate, polyol esters such as trimethylolpropane esters or pentaerythritol esters, perfluoroalkyl ethers, silicone oils and polyphenyl ethers.
  • Polyolefins include polymers of various olefins or hydrides thereof. Any olefin may be used, and as examples mention may be made of ethylene, propylene, butene and ⁇ -olefins with five or more carbons. In the manufacture of polyolefins, olefins may be used singly or two or more kinds may be used in combination. Particularly suitable are the polyolefins called poly- ⁇ -olefins (PAO). These are base oils of Group IV.
  • PAO poly- ⁇ -olefins
  • GTL (gas to liquid) base oils synthesised by the Fischer-Tropsch method of converting natural gas to liquid fuel have a very low sulphur content and aromatic content compared with mineral oil base oils refined from crude oil and have a very high paraffin constituent ratio, and so have excellent oxidative stability.
  • the various base oils may be used singly or in mixtures.
  • the thickener in the grease composition is a fatty acid salt of lithium and/or calcium.
  • the fatty acid is suitably a C 13 -C 21 fatty acid.
  • the thickener is a fatty acid salt of lithium and preferably the thickener is lithium-12-hydroxystearate.
  • the grease composition suitably comprises from 2 to 20wt% of fatty acid salt of lithium and/or calcium, based upon the weight of the grease composition.
  • the grease composition may also comprise anti-oxidants, rust preventatives, oiliness agents, extreme pressure additives, anti-wear agents, solid lubricants, metal deactivators, polymers and other additives.
  • the anti-oxidants include, for example, 2,6-di-t-butyl-4-methylphenol, 2,6-di-t-butyl-paracresol, P,P'-dioctyldiphenylamine, N-phenyl- ⁇ -naphthylamine and phenothiazines.
  • the rust preventatives include paraffin oxide, carboxylic acid metal salts, sulphonic acid metal salts, carboxylic acid esters, sulphonic acid esters, succinic acid esters, sorbitan esters and various amine salts.
  • the oiliness agents, extreme pressure additives and anti-wear agents include, for example, sulphurised zinc dialkyl dithiophosphates, sulphurised zinc diaryl dithiophosphates, sulphurised zinc dialkyl dithiocarbamates, sulphurised zinc diaryl dithiocarbamates, sulphurised molybdenum dialkyl dithiophosphates, sulphurised molybdenum diaryl dithiophosphates, sulphurised molybdenum dialkyl dithiocarbamates, sulphurised molybdenum diaryl dithiocarbamates, organic molybdenum complexes, sulphurised olefins, triphenylphosphates, triphenylphosphorothionates, tricresylphosphates, other phosphate esters and sulphurised fats and oils.
  • the solid lubricants include, for example, molybdenum disulphide, graphite, boron nitride, melamine cyanurate, PTFE (polytetrafluoroethylene), tungsten disulphide, mica, graphite fluoride and so on.
  • the metal deactivators include, for example, N,N'-disalicylidene-1,2-diaminopropane, benzotriazole, benzoimidazole, benzothiazole and thiadiazole.
  • the grease compositions may be manufactured using standard grease manufacturing routes.
  • the calcium salicylate is the first additive added to the reacted combination of thickener and base oil.
  • the grease compositions may be used for general industrial lubrication, including use in heavy duty bearings. They may also be used in heavy duty plain and rolling element bearings operating under harsh conditions including shock loading in wet environments. Furthermore they may be used in automotive applications such as wheel bearings (taper and rolling), chassis points, universal steering, suspension and transmission joints, water pump and generating bearings, and shackles and linkages.
  • Greases were prepared by combining 12-hydroxystearate with base oil in a kettle and heating to 90°C (heat rate of 3°C/min) whilst stirring at 150rpm. A mixture of base oil, water and lithium hydroxide was prepared and was heated to 60°C with stirring. The lithium hydroxide mixture was added to the kettle at 90°C and the kettle was closed. The kettle was then heated to 200°C (heat rate of 3°C/min) and the mixture was stirred at 200rpm. When the temperature reached 200°C, the kettle was vented and stirring rate was reduced to 100rpm. After venting the kettle was heated to 215°C (heat rate of 4°C/min) and the mixture was stirred at 150rpm.
  • the mixture was then cooled to 160°C (heat rate of 3°C/min) with stirring at 200rpm.
  • 160°C further preheated base oil was added by pump, and then the kettle was stirred at 150rpm for 15 minutes.
  • the kettle was cooled to 100°C (heat rate of 5°C/min) with stirring at 100rpm.
  • calcium salicylate was added and then an additive package was added after 10 minutes stirring. Further base oil was added, followed by stirring at 150rpm.
  • the product was mixed and de-aerated for 20 minutes, filtered, homogenised and de-aerated.
  • Example 1 Li-12-hydroxystearate (wt%) Calcium salicylate (wt%) Additive Package (wt%) Base Oil (wt%)
  • Example 1 10.30 0.50 6.25 82.95
  • Example 2 10.30 0.38 3.50 85.82
  • Example 3 10.30 0.38 4.00 85.32
  • Comparative Example 1 10.30 0 6.25 83.45 Comparative Example 2 10.30 0 3.50 86.20 Comparative Example 3 10.30 0 4.00 85.70 Comparative Example 4 10.30 0 4.00 85.70
  • Example 4 is a repeat of Example 3, and Comparative Example 4 is a repeat of Comparative Example 3.
  • the additive package is a standard package of grease additives and was the same in all examples and comparative examples.
  • the base oil was a paraffinic base oil with a viscosity of 220cSt.
  • Roll stability tests were carried out according to ASTM D 1831. In a first series of tests, the cylinder was rotated for 18 hours at 65°C. In a second series of tests, the cylinder was rotated for 100 hours at 65°C. Scanning electron microscope pictures were taken after the Roll Stability tests. The pictures were assessed to determine whether the thickener remained intact (fibre-like structures are visible) or had been destroyed (fibre-like structures are generally not visible).
  • the examples of the invention (all containing calcium salicylate) exhibited significantly improved roll stability compared to the comparative examples (not containing calcium salicylate).

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
EP14786932.5A 2013-10-24 2014-10-22 Use of calcium salicylate to improve roll stability in a grease composition Active EP3060635B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP14786932.5A EP3060635B1 (en) 2013-10-24 2014-10-22 Use of calcium salicylate to improve roll stability in a grease composition

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP13190038 2013-10-24
EP14786932.5A EP3060635B1 (en) 2013-10-24 2014-10-22 Use of calcium salicylate to improve roll stability in a grease composition
PCT/EP2014/072624 WO2015059181A1 (en) 2013-10-24 2014-10-22 Improved roll stability in a grease composition

Publications (2)

Publication Number Publication Date
EP3060635A1 EP3060635A1 (en) 2016-08-31
EP3060635B1 true EP3060635B1 (en) 2017-12-06

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Application Number Title Priority Date Filing Date
EP14786932.5A Active EP3060635B1 (en) 2013-10-24 2014-10-22 Use of calcium salicylate to improve roll stability in a grease composition

Country Status (7)

Country Link
US (1) US20160362627A1 (zh)
EP (1) EP3060635B1 (zh)
JP (1) JP6448638B2 (zh)
CN (1) CN105705621B (zh)
BR (1) BR112016008754B1 (zh)
RU (1) RU2673067C2 (zh)
WO (1) WO2015059181A1 (zh)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10734696B2 (en) * 2017-05-16 2020-08-04 Rigetti & Co, Inc. Connecting electrical circuitry in a quantum computing system
JP6895863B2 (ja) * 2017-10-02 2021-06-30 シェルルブリカンツジャパン株式会社 グリース組成物

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58125794A (ja) * 1982-01-21 1983-07-26 Showa Shell Sekiyu Kk 音響特性が改善された高滴点リチウムコンプレツクスグリ−ス組成物
JPS58125795A (ja) * 1982-01-21 1983-07-26 Showa Shell Sekiyu Kk 高滴点リチウムコンプレツクスグリ−ス組成物
GB8531626D0 (en) * 1985-12-23 1986-02-05 Shell Int Research Grease composition
JP4634585B2 (ja) * 2000-08-10 2011-02-16 昭和シェル石油株式会社 防錆性および耐摩耗性が改良されたグリース組成物
US7009072B2 (en) * 2002-10-31 2006-03-07 Crompton Corporation Method for producing lubricant detergents
JP5067761B2 (ja) * 2008-04-16 2012-11-07 住鉱潤滑剤株式会社 金属石鹸グリース組成物
FR2942627B1 (fr) * 2009-02-27 2011-05-06 Total Raffinage Marketing Composition de graisse
JP5643634B2 (ja) * 2010-02-15 2014-12-17 昭和シェル石油株式会社 グリース組成物

Also Published As

Publication number Publication date
BR112016008754B1 (pt) 2021-11-23
CN105705621A (zh) 2016-06-22
EP3060635A1 (en) 2016-08-31
BR112016008754A2 (pt) 2020-05-19
US20160362627A1 (en) 2016-12-15
JP6448638B2 (ja) 2019-01-09
RU2016119816A (ru) 2017-11-27
CN105705621B (zh) 2019-03-15
RU2016119816A3 (zh) 2018-06-27
JP2016534175A (ja) 2016-11-04
RU2673067C2 (ru) 2018-11-22
WO2015059181A1 (en) 2015-04-30

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