EP1570034A1 - Harnstoffschmierfettzusammensetzung - Google Patents

Harnstoffschmierfettzusammensetzung

Info

Publication number
EP1570034A1
EP1570034A1 EP03799554A EP03799554A EP1570034A1 EP 1570034 A1 EP1570034 A1 EP 1570034A1 EP 03799554 A EP03799554 A EP 03799554A EP 03799554 A EP03799554 A EP 03799554A EP 1570034 A1 EP1570034 A1 EP 1570034A1
Authority
EP
European Patent Office
Prior art keywords
compound
molybdenum
grease composition
urea grease
grease
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.)
Granted
Application number
EP03799554A
Other languages
English (en)
French (fr)
Other versions
EP1570034B1 (de
Inventor
Kouichi Numazawa
Kazushige Ohmura
Takahiro Ozaki
Keiji Tanaka
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
Original Assignee
Shell Internationale Research Maatschappij BV
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shell Internationale Research Maatschappij BV filed Critical Shell Internationale Research Maatschappij BV
Publication of EP1570034A1 publication Critical patent/EP1570034A1/de
Application granted granted Critical
Publication of EP1570034B1 publication Critical patent/EP1570034B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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
    • C10M115/00—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
    • C10M115/08—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof containing nitrogen
    • 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
    • C10M169/06—Mixtures of thickeners and additives
    • 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
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064—Di- and triaryl amines
    • 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
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
    • C10M2215/10—Amides of carbonic or haloformic acids
    • C10M2215/102—Ureas; Semicarbazides; Allophanates
    • C10M2215/1026—Ureas; Semicarbazides; Allophanates used as thickening material
    • 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
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/221—Six-membered rings containing nitrogen and carbon only
    • C10M2215/222—Triazines
    • 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
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
    • C10M2219/066—Thiocarbamic type compounds
    • C10M2219/068—Thiocarbamate metal salts
    • 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
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/045—Metal containing thio derivatives
    • 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
    • C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/09—Complexes with metals
    • 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
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • C10N2040/046—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives for traction drives
    • 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—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy

Definitions

  • the present invention relates to a urea grease composition.
  • urea grease is known as heat-resistant grease because it generally has a higher dropping point and superior thermal stability than general-purpose lithium- soap grease containing lithium soap as a thickening agent .
  • urea grease has superior wear resistance and lubricating properties than greases in which various metal soap and inorganic materials have been used as thickening agents. It is thought that the superior wear resistance is because urea grease can form both a urea film and an oxide film on lubricated sliding surfaces.
  • Urea grease has achieved rapid growth as grease which may be conveniently applied to typical grease- lubricated locations, including a wide variety of bearings for vehicle constant-velocity joints, ball joints, wheel bearings, alternators and cooling fans, ball screws and linear guides of machine tools, a wide variety of sliding areas of construction equipment, and bearings and gears in steel equipment and various other industrial mechanical facilities.
  • urea grease has been rising steadily in particular applications, such as various kinds of vehicle parts including CVJs (constant-velocity joints) where there is a strong demand for durability and reduced friction and wear in sliding areas in response to the trend of the present times toward miniaturisation, weight reduction and a hostile use environment, and in steel equipment which requires highly heat-resistant, wear- resistant lubricating grease.
  • CVJs constant-velocity joints
  • Examples of lubricated parts of vehicles include various kinds of bearings, such as cooling fan bearings of a radiator, compressor bearings of an air conditioner and alternator bearings, constant-velocity joints, universal joints of a propeller shaft, gears and bearings of a steering unit, ball screws, sliding areas of rack guides, and ball joints.
  • bearings such as cooling fan bearings of a radiator, compressor bearings of an air conditioner and alternator bearings, constant-velocity joints, universal joints of a propeller shaft, gears and bearings of a steering unit, ball screws, sliding areas of rack guides, and ball joints.
  • examples of parts to be lubricated in other industries which are limited in direct low-noise requirements as compared with vehicles, domestic electric appliances and office automation equipment, include a wide variety of bearings of auto- assembly robots, ball screws and linear guides of machine tools, various sliding areas of construction equipment, and various bearings of steel facilities.
  • the low-noise properties of greases are further explained by taking a bearing as an example.
  • the lubricating mechanism of a grease on a rolling- element bearing is such that the grease which has been packed in the bearing is temporarily swung and scattered by revolution, and thereafter a trace amount of grease or oil is fed to a sliding area as churning and channeling are repeated, thereby lubricating the sliding area.
  • a sound caused by vibrations occurring between a tumbling element- of the bearing and a rolling surface appears as a bearing noise.
  • urea compounds which have been obtained by reacting amine and isocyanate are used as thickening agents and these are dispersed in the oil and maintain the grease state.
  • Urea grease is generally superior to soap grease in abrasion resistance because the urea compound (s) used therein as a thickening agent are likely to adsorb to metal surfaces.
  • many of the urea compounds obtained by the afore-mentioned reaction between amine and isocyanate are in a hard granular state, thereby impairing the sound characteristics and having an adverse effect on smooth lubrication.
  • JP-A-1-139696, JP-A-2-77494 and JP-A-6-17080 concern the acoustic properties of urea grease.
  • JP-A-1-139696 discloses a thickening agent containing a mixture of diurea compounds (a) and (b) represented by the following formulae (a) and (b) , respectively:
  • R NHCONHR5NHCONHR 6 wherein R2 is a diphenylmethane group, R]_ and R3 each represents a C8 linear or branched saturated alkyl group, R5 represents a tolylene group or a bitolylene group, and R4 and Rg each represents an alkyl-substituted aromatic group or a halogen-substituted aromatic group.
  • JP-A-2-77494 discloses a thickening agent containing a mixture of diurea compounds (a) and (b) represented by the foregoing formulae (a) and (b) wherein, however, R2 represents a bitolylene group, R]_ and R3 each represent a
  • R5 represents a diphenylmethane group
  • R4 and R ⁇ represent C8 linear or branched saturated alkyl groups.
  • JP-A-6-17080 discloses a thickening agent containing a mixture of diurea compounds (a) and (b) represented by the foregoing formulae (a) and (b) wherein, however, R2 represents a tolylene group, RQ_ and R3 represent C16-18 linear or branched saturated alkyl groups or unsaturated alkyl groups, R5 represents a diphenylmethane group, and R4 and Rg represent C8 linear or branched saturated alkyl groups .
  • JP-A-3-28299 discloses a grease composition wherein the base oil containing an alkyldiphenyl ether oil as an essential component is mixed with a thickening agent which is a diurea compound represented by the foregoing formula (a) wherein, however, 2 represents a C6-15 aromatic hydrocarbon group, and R ⁇ and R3 represent C8-18 linear alkyl groups, provided that the proportion of C8 alkyl groups in the combination of R]_ and R3 is from 60 to 100 mole %.
  • JP-A-2-80493 discloses a composition for circular conical roller bearings which is prepared by admixing urea grease with 0.5 to 5 % by weight of oxidation-modified polyolefin and/or acid- modified polyolefin, and further discloses in Table 2 the urea thickening agents prepared from C8 octylamine, C18 stearylamine (octadecylamine) and MDI (diphenylmethane- 4, 4' -diisocyanate) and demonstrates that these agents produce beneficial effects on machine stability, wet shear stability and pressure transferability.
  • JP-A-3-243696 discloses a diurea compound represented by the foregoing formula (a) wherein, however, R2 is a 3, 3' -dimethyl-4, ' -biphenylene group and
  • R ] _ and R3 are mixtures of C8-18 alkyl groups with an oleyl group.
  • the art disclosed in this document has defects that the consistency yield is so low that grease having a consistency of about 250 cannot be obtained without increasing the amount of the thickening agent and the degree of oil separation under high temperature conditions is great.
  • JP-A-58-185693 discloses a diurea grease improved by incorporating therein one or more of an additive selected from alkenylsuccinic acid i ides, metal salts of alkylbenzenesulfonic acids, or metal salts of petroleum sulfonic acid.
  • the document further discloses the use of diisocyanate and monoamines for the diurea grease, and recites aliphatic amines, such as stearylamine and oleylamine, and aromatic amines, such as cyclohexylamine, as examples of those monoamines. Said document indicates that the sound characteristics of said grease were favourable.
  • JP-A-2-4895 discloses a urea grease preparation method enabling improvement in sound characteristics, wherein an isocyanate and an amine are added to a base oil and reacted with each other at a temperature of 60 to 120°C, and then the mixture of a urea compound produced and the base oil is subjected to dispersion treatment by use of a kneading apparatus and further heated up to 160 to 180°C at a temperature-rising speed of 0.5 to 2°C per minute.
  • JP-A-3-190996 discloses a method of preparing greases which are said to have good sound characteristics, wherein the isocyanate-dissolved or dispersed base oil and the amine-dissolved or dispersed base oil are mixed through collisions by pressurizing them in a reaction vessel to cause reaction with each other, or they are pressurized and introduced to an revolving impeller, thereby causing reaction with each other.
  • JP-A-3-231993 discloses a method of preparing low-noise urea grease, which includes the first step of heating the mixture constituted of 2 to 30 % by weight of a urea compound represented by the foregoing formula (a) , wherein R_ and R3 are C8-18 saturated alkyl groups and R2 is a tolylene group, a diphenylmethane group or a dimethylbiphenylene group, and 98 to 70 % by weight of a base oil up to 170 to 230°C to thoroughly dissolve the urea compound into the base oil, and the second step of cooling the solution obtained in the first step at a speed of at least 5°C per second.
  • a urea compound represented by the foregoing formula (a) wherein R_ and R3 are C8-18 saturated alkyl groups and R2 is a tolylene group, a diphenylmethane group or a dimethylbiphenylene group, and 98 to 70 % by weight of
  • the agglomeration of urea compounds is avoided by using kneading apparatus, performing the reaction in a high- pressure vessel, or dissolving two or more kinds of grease by heating and then mixing them.
  • urea grease compositions having a satisfactory consistency yield, with little oil separation at high temperature and with outstanding sound properties and lubricating properties.
  • said urea grease compositions may be produced in conventional grease-making facilities without the need for specialised equipment such as high-pressure kettles or kneading machines in order to disperse the thickening agent.
  • the urea grease compositions of the present invention have good lubrication capabilities and can easily spread on and are strongly adsorbed to friction surfaces.
  • the intervened thickening function of the urea compounds in said grease composition is not an obstacle therein as extraneous matter. Therefore, the urea grease composition of the present invention causes no noise, and, in addition, can enhance the strength of oil film by its viscoelasticity and can form more effective lubrication film on sliding surfaces under a synergy with additives.
  • favourable grease lubrication can be attained.
  • a urea grease composition comprising a lubricating base oil and from 2 to 30 wt.% of a thickening agent, with respect to the total weight of the urea grease composition and wherein said thickening agent is selected from: (1) a mixture comprising a compound (a) and a compound (b) , containing compound (a) at 20 to 80 mol%, relative to the total amount of compound (a) and compound (b) ; (2) a mixture formed by mixing a compound (c) with a mixture (1) ; or
  • R NHCONHR 2 NHCONHR 3 R NHCONHR 2 NHCONHR 3 , and wherein R2 is a diphenylmethane group, R_ is a C6-10 saturated alkyl group and R3 is a C14-20 saturated and/or unsaturated alkyl group, wherein unsaturated alkyl groups constitute at least 20 mol% of the R3 alkyl group.
  • unsaturated alkyl groups constitute at least 25 mol%, more preferably at least 30 mol% of the R3 alkyl group.
  • R ] _ is a saturated C8 alkyl group and/or R3 is a C14-20 saturated and/or unsaturated alkyl group wherein unsaturated alkyl groups constituting at least 20 mol% of the R3 alkyl group are oleyl groups.
  • a urea grease composition comprising a lubricating base oil and from 2 to 30 wt.% of a thickening agent, with respect to the total weight of the urea grease composition and wherein said thickening agent is selected from:
  • R 1 NHCONHR2NHCONHR3 , and wherein R2 is a diphenylmethane group, R ⁇ is a C8 saturated alkyl group, R3 is a C14-20 saturated and/or unsaturated alkyl group, with the alkyl groups being such that this constituent includes at least 20 mol% of an oleyl constituent.
  • a urea grease having outstanding characteristics and performance is obtained when a thickening agent as described above is incorporated into a lubricating base oil in an amount of from 2 to 30 wt%, preferably from 5 to 20 wt% with respect to the total weight of the urea grease composition.
  • a thickening agent as described above is incorporated into a lubricating base oil in an amount of from 2 to 30 wt%, preferably from 5 to 20 wt% with respect to the total weight of the urea grease composition.
  • the content of urea compounds as thickening agent is less than 2 wt%, the thickening effect is small and it is impossible to form a grease.
  • the content of urea compounds as thickening agent exceeds 30 wt%, the grease becomes too stiff and no lubricating effect is obtained.
  • the lubricating base oil used in the urea grease composition of the present invention may conveniently be one or more of a vegetable oil, a mineral oil, and/or a synthetic oil.
  • Base oils of mineral origin may be mineral oils, for example those produced by solvent refining or hydroprocessing.
  • Base oils of synthetic origin may typically be hydocarbon oils such as hydrocarbon polymers, for example liquid polymers of alpha-olefins (poly ( ⁇ -olefin) ) , ester type synthetic oils, silicone oils and/or ether type synthetic oils. They may also be a mixture of these oils.
  • mineral oils that may conveniently be used include those sold by member companies of the Royal Dutch/Shell Group under the designations "HVI", “MVIN”, or HMVIP"- Polyalphaolefins and base oils of the type manufactured by the hydroisoi ⁇ ierisation of wax, such as those sold by member companies of the Royal Dutch/Shell Group under the designation N XHVI" (trade mark) , may also be used.
  • the urea grease composition of the present invention further includes a zinc compound as an additive.
  • zinc dithiophosphates include zinc diethyldithiophosphate, zinc dipropyldithio- phosphate, zinc dibutyldithiophosphate, zinc dipentyl- dithiophosphate, zinc dihexyldithiophosphate, zinc didecyldithiophosphate, zinc diisobutyldithiophosphate, - zinc di (2-ethylhexyl) dithiophosphate, zinc diamyldithio- phosphate, zinc dilauryldithiophosphate, zinc distearyl- dithiophosphate, zinc diphenyldithiophosphate, zinc ditolyldithiophosphate, zinc dixylyldithiophosphate, zinc diethylphenyldithiophosphate, zinc dipropylphenyldithio'- phosphate, zinc dibutylphenyldithiophosphate, zinc dipentylpheny
  • the metallic elements such as S or P in these organometallic zinc compounds react with iron in frictional surfaces to form extreme pressure films of iron phosphide or iron sulphide, etc.; and the additive itself breaks down and inter-reacts with other additives to form a protective film.
  • the urea grease compositions of the present invention exhibit outstanding lubricating properties due to synergistic effects of such S-P type additives with the urea thickening agents of the present invention, which have outstanding penetration into the interface and adsorption.
  • the urea grease composition of the present invention may advantageously include a molybdenum compound therein as an additive.
  • molybdenum compounds readily adsorb positively to the metal surfaces which constitute sliding surfaces, and are decomposed by the heat produced at the frictional surfaces to produce 0O3 and M0S 2 , and this MoS 2 component diffuses into the metal and has a mechanism of action which protects the frictional surfaces.
  • the urea grease compositions of the present invention exhibit outstanding lubricating properties due to synergistic effects of the chemical properties of these molybdenum compounds and physical and chemical properties such as adsorption and penetration of the urea thickening agents of the present invention .
  • antioxidants including alkylphenol, hindered phenol, alkylamine, diphenylamine and triazine antioxidants
  • anticorrosion agents include calcium sulphonate, sodium sulphonate, barium sulphonate and amino derivatives or metal salts of carboxylic acids
  • extreme pressure agents including sulphurized oils or fats, sulphurized olefins, phosphoric acid esters, tricresyl phosphate, trialkyl thiophosphates and triphenyl phosphorothionates may be conveniently used.
  • Lubricants for bearing use may advantageously comprise the urea grease composition of the present invention .
  • the present invention further provides a method of lubricating a bearing comprising packing the .bearing with the urea grease composition of the present invention.
  • lubricants for application to a sliding surface of a machine in a relative motion may advantageously comprise the urea grease composition of the present invention.
  • the present invention further provides a method of lubricating the sliding surface of a machine in a relative motion comprising lubricating said sliding surface with the urea grese composition of the present invention.
  • the present invention further provides the use of the urea grease composition of the present invention as a noise-reducing grease composition and, in particular, the use of said grease composition to reduce noise in bearing applications.
  • MDI diphenylmethane-4,4'-diisocyanate
  • base oil 60 parts by weight of base oil were introduced into a grease kettle and heated to approximately 50°C; and after dissolving the MDI, octylamine dispersed in 20 parts by weight of the base oil was slowly added with brisk stirring. After approximately 10 minutes, oleylamine dispersed in 20 parts by weight of the base oil was added and stirring was continued.
  • MDI in the compounding proportions indicated in Table 1 and 60 parts by weight of base oil were introduced into a grease kettle and heated to approximately 50°C, and after dissolving the MDI, a mixture of octylamine and oleylamine dissolved in 40 parts by weight of the base oil was slowly added to the solution and the mixture was stirred vigorously.
  • the contents of the grease kettle were heated to 168 °C and held at this temperature for approximately 30 minutes to complete the reaction, and then cooled to room temperature and treated with a triple roll mill to obtain grease. Examples 8-10
  • the compounding proportions are shown in Table 2. 50 parts by weight of the grease of Example 1 and 50 parts by weight of grease of Example 6 were mixed uniformly with a spatula to give the grease of Example 8. 50 parts by weight of the grease of Example 2 and 50 parts by weight of grease of Example 6 were mixed uniformly with a spatula to give the grease of Example 9. 50 parts by weight of the grease of Example 3 and 50 parts by weight of grease of Example 6 were mixed uniformly with a spatula to give the grease of Example 10. Examples 11-16
  • MDI diphenylmethane-4, 4' -diisocyanate
  • base oil 20 parts by weight of octylamine dissolved in the base oil was slowly added with brisk stirring. After approximately 10 minutes, the amines other than octylamine mixed in the composition shown in Table 3 with 20 parts by weight of base oil were added and stirring was continued.
  • Diisocyanates in the compounding proportions indicated in Tables 5-7 and 60 parts by weight of base oil were put into a grease kettle and after dissolving the diisocyanates at the temperatures below, amines dispersed in 40 parts by weight of the base oil were slowly added with brisk stirring.
  • the contents of the grease kettle were heated to 168°C and held at this temperature for approximately 30 minutes to complete the reaction, and then cooled to room temperature and treated with a triple roll mill to obtain grease.
  • MDI is diphenylmethane-4, 4' -diisocyanate; heating temperature approximately 50°C TDI is 2,4/2,6 (80%/20%) trilene-4, 4' -diisocyanate; heating temperature approximately 30°C TODI is 3, 3' -bitrilene-4, 4' -diisocyanate; heating temperature approximately 75°C.
  • the viscosity at 100°C of the oils shown in the examples and comparative examples was 10.12 mm ⁇ /s for mineral oil, 12.69 mm ⁇ /s for alkyl diphenyl ether oil and 12.70 mm ⁇ /s for poly ( ⁇ -olefin) oil.
  • Additive A is a primary Zn-DTP (primary zinc dithiophosphate) with C4 and C5 alkyl groups
  • Additive B is secondary Zn-DTP (secondary zinc dithiophosphate) with C3 and C6 alkyl groups
  • Additive C is Zn-DTC (zinc dithiocarbamate) with C5 alkyl groups
  • Additive D is Mo-DTC (molybdenum dithiocarbamate) with mainly C8 alkyl groups
  • Additive E is a molybdenum complex compound as described in JP 5-66435 Bl
  • Additive F is Mo-DTP (molybdenum dithiophosphate) with predominantly C8 alkyl groups ;
  • Additive G is a slurry formed by compounding 2,4-bis(n- octylthio) -6- (4-hydroxy-3, 5-di-t-butylamine) -1, 3, 5- triazine and octyldiphenylamine in a ratio 1:2 at a concentration of 50% with mineral oil.
  • Oil separation The JIS K2220 method was performed under -the conditions of 150 °C temperature for 24 hours.
  • Noise test Bearing noise was measured for each grease using an NSK Noise Tester (available from NSK Ltd) as described in JP 53 2357 Bl .
  • Bowden friction test The coefficient of friction was measured using a device with the specifications below, which evaluated friction in a frictional surface between a reciprocating bed and a pin receiving a load vertical to a plate fitted to the bed, having a mechanism applying a load vertical to the bed.
  • Test piece Fixed side: steel sphere or rod
  • the urea grease of the present invention has a high dropping point and does not show oil separation at high temperatures.

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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)
EP03799554.5A 2002-12-10 2003-12-10 Harnstoffschmierfettzusammensetzung Expired - Lifetime EP1570034B1 (de)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
JP2002358152 2002-12-10
JP2002358152 2002-12-10
JP2003284529 2003-07-31
JP2003284529A JP4405202B2 (ja) 2002-12-10 2003-07-31 ウレアグリース組成物
PCT/EP2003/050980 WO2004053032A1 (en) 2002-12-10 2003-12-10 Urea grease composition

Publications (2)

Publication Number Publication Date
EP1570034A1 true EP1570034A1 (de) 2005-09-07
EP1570034B1 EP1570034B1 (de) 2016-02-17

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Family Applications (1)

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EP03799554.5A Expired - Lifetime EP1570034B1 (de) 2002-12-10 2003-12-10 Harnstoffschmierfettzusammensetzung

Country Status (9)

Country Link
US (1) US20040224859A1 (de)
EP (1) EP1570034B1 (de)
JP (1) JP4405202B2 (de)
KR (1) KR20050085578A (de)
AU (1) AU2003299220B2 (de)
BR (1) BR0317109B1 (de)
CA (1) CA2509235A1 (de)
PL (1) PL375721A1 (de)
WO (1) WO2004053032A1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016125859A1 (ja) 2015-02-05 2016-08-11 出光興産株式会社 グリースおよびグリースの製造方法

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EP1570034B1 (de) 2016-02-17
US20040224859A1 (en) 2004-11-11
BR0317109A (pt) 2005-10-25
JP2004204218A (ja) 2004-07-22
PL375721A1 (en) 2005-12-12
BR0317109B1 (pt) 2014-05-27
KR20050085578A (ko) 2005-08-29
WO2004053032A1 (en) 2004-06-24
JP4405202B2 (ja) 2010-01-27
CA2509235A1 (en) 2004-06-24
AU2003299220A1 (en) 2004-06-30
AU2003299220B2 (en) 2007-03-22

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