CN104169404A - Grease and method for softening grease - Google Patents

Grease and method for softening grease Download PDF

Info

Publication number
CN104169404A
CN104169404A CN201380010619.4A CN201380010619A CN104169404A CN 104169404 A CN104169404 A CN 104169404A CN 201380010619 A CN201380010619 A CN 201380010619A CN 104169404 A CN104169404 A CN 104169404A
Authority
CN
China
Prior art keywords
lubricating grease
mole
grease
cycloalkyl
base oil
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.)
Pending
Application number
CN201380010619.4A
Other languages
Chinese (zh)
Inventor
关口浩纪
香村健太郎
末次义幸
中西祐辅
藤浪行敏
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.)
Idemitsu Kosan Co Ltd
Original Assignee
Idemitsu Kosan Co Ltd
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 Idemitsu Kosan Co Ltd filed Critical Idemitsu Kosan Co Ltd
Publication of CN104169404A publication Critical patent/CN104169404A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M133/00Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
    • C10M133/02Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
    • C10M133/16Amides; Imides
    • C10M133/18Amides; Imides of carbonic or haloformic acids
    • C10M133/20Ureas; Semicarbazides; Allophanates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M115/00Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
    • C10M115/08Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating 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
    • C10M169/02Mixtures of base-materials and thickeners
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M177/00Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/028Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
    • C10M2205/0285Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/10Amides of carbonic or haloformic acids
    • C10M2215/102Ureas; Semicarbazides; Allophanates
    • C10M2215/1026Ureas; Semicarbazides; Allophanates used as thickening material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01Physico-chemical properties
    • C10N2020/02Viscosity; Viscosity index
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/30Anti-misting
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/02Bearings
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/06Instruments or other precision apparatus, e.g. damping fluids
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2070/00Specific manufacturing methods for lubricant compositions

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The grease of the present invention is obtained by blending 15 to 25 mass% of diurea represented by the following formula as a thickener in a hydrocarbon-containing base oil based on the total amount of the composition, and the penetration after stirring of the grease is 170 to 295. R1NHCONHR2NHCONHR3(1)。R1、R3Different from each other, a hydrocarbon group having 6 to 18 carbon atoms. R2Is a divalent aromatic hydrocarbon group having 6 to 13 carbon atoms.

Description

The softening method of lubricating grease and lubricating grease
Technical field
The present invention relates to the softening method of lubricating grease and lubricating grease, in particular to low the dirt lubricating grease using with by the further softening method of this lubricating grease in clean room etc.
Background technology
The precision electronic device such as semiconductor-fabricating device or liquid crystal mfg. apparatus manufacturing installation requires very clean environment, thereby is arranged in clean room.In addition, in food mfg factory or medicine manufacturing works etc., for fear of impurity, sneak into product, also require clean environment.In the mechanism using, there is various bearings or sliding part, junction surface under these environment, in its lubricated part, use low dirt lubricating grease.
As low dirt lubricating grease, use for example fluorenone.But fluorenone is conventionally expensive, and oilness is not enough, thereby the torque of the bearing of sometimes filling can increase.In addition,, in the manufacture of precise electronic parts, sneaking into of halogenic ingredient is not preferred.And then low dirt is also far from being fully.As not halogen-containing low dirt lubricating grease, also use Lithium soap grease or lithium complex soap grease.For example, a kind of lubricating grease has been proposed, it has coordinated, and to account for 15~30% the Li salt as lipid acid of composition in its entirety and length and diameter be that fibrous material below 2 μ m is used as thickening material, and the carbonatoms of the Li salt of described lipid acid is more than 10 and does not have hydroxyl (with reference to patent documentation 1).Because it contains metal-salt, thereby for semiconductor-fabricating device, if lubricant splashes, may cause that product is bad.And then its low dirt is also far from being fully.
Owing to there being the problems referred to above, thereby also use urea grease.For example, disclose a kind of lubricating grease, it contains ester oil as base oil more than 50%, and contains aliphatics allophanamide thickening material more than 20%, and its stir after penetration degree be that 220~300(is with reference to patent documentation 2).Owing to containing in a large number ester oil, thereby hydrolytic resistance is troubling, and the life-span now also can shorten.In addition, its low dirt is also far from being fully.
As urea grease, also exist to have used not contain the report example of the base oil of ester.(with reference to patent documentation 3).After the stirring of this lubricating grease, the range of application of penetration degree is that 190~230(is harder), thereby be difficult to easily coat and make use, worry in addition the increase of torque or the reduction of lubricity.And then this lubricating grease low dirt that is also far from being is abundant.
Prior art document
Patent documentation
Patent documentation 1: TOHKEMY 2004-352953
Patent documentation 2: TOHKEMY 2005-272764
Patent documentation 3: Japanese kokai publication hei 11-166191.
Summary of the invention
The technical problem that invention will solve
As mentioned above, urea grease is in the past difficult to suppress powder amount under suitable denseness.
The present invention is in view of above-mentioned prior art, and its object is to provide a lower lubricating grease of dirt.In addition, during lubricating grease deliquescing, (when denseness uprises) conventionally sent out dirt and also risen, while thereby the present invention also aims to provide and improve denseness and reduce the method for sending out dirt.
Means for technical solution problem
In order to solve above-mentioned problem, the invention provides lubricating grease shown below and the softening method of lubricating grease.
(1) lubricating grease, is characterized in that, it is in containing the base oil of hydrocarbon, take total composition as benchmark, coordinates the allophanamide shown in the above and following formula as thickening material below 25 quality % (1) of 15 quality % to form,
After the stirring of this lubricating grease, penetration degree is more than 170 and below 295,
     R 1NHCONHR 2NHCONHR 3     (1)
R 1, R 3mutually different, be the alkyl of carbonatoms 6 to 18.R 2for the divalence aromatic hydrocarbyl of carbonatoms more than 6 and below 13.
(2) lubricating grease of the present invention, is characterized in that, after stirring, penetration degree is more than 230 and below 265.
(3) lubricating grease of the present invention, is characterized in that, described alkyl is saturated hydrocarbyl.
(4) lubricating grease of the present invention, is characterized in that, described saturated hydrocarbyl is alkyl or cycloalkyl.
(5) lubricating grease of the present invention, is characterized in that, described cycloalkyl is cyclohexyl.
(6) lubricating grease of the present invention, is characterized in that, described R 1, R 3for octyl group or cyclohexyl.
(7) lubricating grease of the present invention, is characterized in that, the total amount of alkyl and cycloalkyl Zhe Liangzhong functional group of take is benchmark, the average proportions of the cycloalkyl in described allophanamide be 85 % by mole following and more than 15 % by mole.
(8) lubricating grease of the present invention, is characterized in that, the average proportions of described cycloalkyl is below 50 % by mole and more than 15 % by mole.
(9) lubricating grease of the present invention, is characterized in that, the average proportions of described cycloalkyl is below 85 % by mole and more than 75 % by mole.
(10) lubricating grease of the present invention, is characterized in that, take base oil total amount as benchmark, and described hydrocarbon is more than 90 quality %.
(11) lubricating grease of the present invention, is characterized in that, described hydrocarbon is poly-alpha olefins.
(12) lubricating grease of the present invention, is characterized in that, 40 ℃ of kinematic viscosity of base oil are 400mm 2below/s.
(13) softening method of lubricating grease, is characterized in that, of the present invention lubricating grease applied to centrifugal force on one side stir on one side.
The allophanamide of the ad hoc structure of lubricating grease use specified amount of the present invention is as thickening material, thereby powder amount is considerably less, and the mechanism that is particularly suitable for using in clean room is used.In addition, during lubricating grease deliquescing, (when denseness uprises) common powder amount can increase, on one side by lubricating grease of the present invention being applied to centrifugal force on one side, stir, higher although denseness becomes, but also can form, send out the lower lubricating grease of dirt.
Embodiment
Lubricating grease of the present invention (following, also referred to as " this lubricating grease ") is in comprising the base oil of hydrocarbon, to coordinate the allophanamide of ad hoc structure to form as thickening material.
Below, be elaborated.
(base oil)
For the manufacture of this grease base plinth oil, contain hydrocarbon as principal constituent.When base oil is the ether oil of alkyl diphenyl base ether and so on or ester oil, sending out dirt can uprise, therefore not preferred.And then, if use these base oils with polar group, can produce hydrolysis, also may damage the function as lubricating grease.Therefore, preferably avoid as far as possible sneaking into these oily kinds, base oil preferably contains hydrocarbon more than 90 quality %, most preferably only contains hydrocarbon.
As the hydrocarbon that can be used as base oil, the viewpoint from low dirt, is preferably poly-alpha olefins.
40 ℃ of kinematic viscosity of base oil are preferably 400mm 2below/s.If 40 ℃ of kinematic viscosity surpass 400mm 2/ s, stirs resistance and increases, thereby moment of torsion excessively increases, wearability variation.Particularly fretting wear may increase.Therefore, 40 of base oil ℃ of kinematic viscosity are preferably 100mm 2/ s is following, 50mm more preferably 2below/s.
On the other hand, if 40 ℃ of kinematic viscosity of base oil are less than 10mm 2/ s, volatility uprises, and in addition, resistance to loading performance likely reduces.
If 40 ℃ of kinematic viscosity 10mm of base oil 2above and the 50mm of/s 2below/s, volatility is also fully low, and can reduce moment of torsion, thereby favourable while using lubricating grease under the little condition of loading.Should illustrate, 40 ℃ of kinematic viscosity of base oil can be measured according to JIS K 2283.
(thickening material)
The thickening material that can be used for manufacturing this lubricating grease is the allophanamide shown in following formula (1). 
     R 1NHCONHR 2NHCONHR 3     (1)。
Here, R 1, R 3be the alkyl of carbonatoms 6 to 18 independently.The R of the allophanamide of formula (1) 1, R 3mutually different.The allophanamide of formula (1) is used usually used as mixture.In addition, difference represents R mutually 1, R 3100 % by mole of the equal less thaies of average proportions of saturated hydrocarbyl.If 100 % by mole of the average proportions of arbitrary functional group, likely cannot take into account penetration degree and low dirt after preferred stirring.
Especially, from the viewpoint of low dirt, the more preferably average proportions of the cycloalkyl in aforementioned allophanamide, the total amount of alkyl and cycloalkyl Zhe Liangzhong functional group of take is benchmark, cycloalkyl be 85 % by mole following and more than 15 % by mole.
In addition, also the average proportions of preferred aforementioned cycloalkyl is below 50 % by mole and more than 15 % by mole, or the average proportions of aforementioned cycloalkyl is below 85 % by mole and more than 75 % by mole.
Here, the alkyl of carbonatoms 6 to 18 has saturated and unsaturated, and saturated hydrocarbyl has alkyl, cycloalkyl.Unsaturated alkyl has thiazolinyl.Alkyl is preferably linear chain structure.From the viewpoint of low dirt, alkyl is preferably octyl group, the viewpoint of the balance of penetration degree and low dirt from stirring, and cycloalkyl is preferably cyclohexyl.Thiazolinyl has oleyl etc.
R particularly preferably 1, R 3for octyl group and cyclohexyl.
R 2for the divalence aromatic hydrocarbyl of carbonatoms more than 6 and below 13.For example can enumerate: 4,4 '-diphenyl methyl or tolyl.
The allophanamide of above-mentioned formula (1) can easily be manufactured with reacting of monoamine by aromatic diisocyanate.As aromatic diisocyanate, can enumerate: ditan-4,4 '-vulcabond or tolylene diisocyanate.As monoamine, can enumerate: octyl amine or cyclo-hexylamine etc.
(this lubricating grease)
Lubricating grease of the present invention is in above-mentioned base oil, to coordinate above-mentioned thickening material, to make to stir rear penetration degree be more than 175 and 295 following, be preferably more than 180 and 275 following, more preferably more than 180 and 265 below, more preferably more than 230 and 265 following forming.
Here, the use level of thickening material be take total composition need to be more than 15 quality % and below 25 quality % as benchmark, are preferably 15 quality % above and below 20 quality %.If the use level of thickening material is few, can form and stir the rear too high lubricating grease of penetration degree, powder amount increases.On the other hand, if the use level of thickening material is too much, after stirring, penetration degree reduces and can form hard grease.Although powder amount is now few, to the Interventional of surface of friction (easily accessibility) deficiency, and likely cause insufficient lubrication.
Should illustrate, while mixing to manufacture lubricating grease with base oil when equivalent mixing vulcabond is manufactured thickening material with amine, the use level of thickening material is the use level as vulcabond and the amine in its source.
Lubricating grease of the present invention is like this owing to using the allophanamide of the ad hoc structure of specified amount to be used as thickening material, thereby it is very low and because base oil is hydrocarbon to send out dirt, thereby hydrolytic resistance is also excellent.Especially, it is characterized in that, even penetration degree is more than 230 softness and the region of use sense excellence after stirring, send out dirt also low.In addition due to can not halogen-containing and metal-salt, thereby suitablely as precision electronic device, use.
(the softening processing of this lubricating grease)
This lubricating grease, by under centrifugal force stirring, makes to stir rear penetration degree and rises, and sends out dirt simultaneously and reduces.Conventionally, if make consistency of grease increase, sending out dirt can uprise, thereby the lubricating grease that forms above-mentioned proterties is worth dated especially.
Preferred centrifugal force is more than 200G, more preferably more than 300G.
In this lubricating grease, can, in realizing the scope of the object of the invention, coordinate as required the additives such as antioxidant, rust-preventive agent, solid lubricant, weighting agent, oiliness improver and metal passivator.
As antioxidant, can enumerate such as: the amine such as alkylation diphenylamine, phenyl-α-naphthylamine, alkylation-Alpha-Naphthyl amine are antioxidant, 2,6-di-tert-butyl-4-methy phenol, 4,4 '-methylene-bis (2,6-DI-tert-butylphenol compounds) etc. phenol is antioxidant etc., and their ratios above in 0.05 quality % and the following degree of 2 quality % are used.
As rust-preventive agent, can enumerate: Sodium Nitrite, sulfonated petro-leum, dehydrating sorbitol monooleate, fatty acid soaps, amine compound etc.
As solid lubricant, can enumerate: polyimide, PTFE, graphite, metal oxide, boron nitride, melamine cyanurate (MCA), molybdenumdisulphide etc.
Above-described various additive can be separately or several combinations coordinate.
Embodiment
Then, enumerate embodiment and comparative example is described in more detail the present invention, but the present invention is not subject to any restriction of their record content.
Particularly, by aftermentioned method, manufacture various lubricating grease, characteristic is compared to evaluation.Each characteristic of lubricating grease according under show that method obtains.
(1) penetration degree after the stirring of lubricating grease
According to JIS K 2220.7, measure.
(2) powder amount (sending out dirt test)
Use is arranged at ball screw evaluation in clean room's (ISO14644-1 defined 2 grades) from the degree of sending out dirt of lubricating grease.Particularly, the lubricating grease at the integral-filled 10g of screw rod face of ball screw (diameter 16mm, pitch 8mm) carries out the running of 50 hours under the condition of ball-nut speed 100mm/s, stroke 150mm.From being arranged near the suction opening screw rod of reciprocal central part, gather air (pumping velocity 3L/min), by micropartical more than alpha counter (KC-03B processed of RION Co., Ltd.) instrumentation 0.3 μ m and as a dirt number.With total instrumentation number of the unit representation test period (50 hours) of individual/10L, and evaluate with following benchmark.
A:0/10L~500/10L
B:501/10L~1500/10L
C:1501/more than 10L.
(embodiment 1)
Manufacture lubricating grease as described below.Should illustrate, also identical in other embodiment and comparative example as the poly-alpha olefins of base oil, its proterties is as described below. 
40 ℃ of kinematic viscosity: 46mm 2/ s
100 ℃ of kinematic viscosity: 7.7mm 2/ s
   VI:137
15 ℃ of density: 0.83g/cm 3.
(manufacture of lubricating grease)
In separated flask (separate flask), add poly-alpha olefins 100g and ditan-4 as base oil, 4'-vulcabond (MDI, Mitsui Chemicals COSMONATE PH processed) 24.8g, put into after agitating vane, under nitrogen gas stream, under 60 ℃, 250rpm, carry out heated and stirred.After MDI dissolves (after approximately 15 minutes), slowly add the mixed amine (octyl amine 4.96g, cyclo-hexylamine 15.3g) being dissolved in base oil 50g, with the degree vigorous stirring of overall flow, once make its homogenizing.In addition, the container of mixed amine is cleaned with remaining base oil 5.0g, add in separated flask, again vigorous stirring.
Then, reaction solution is warming up to 160 ℃, reaches after top temperature, keep 1 hour (during maintenance with the degree vigorous stirring of 15 minutes 1 time so that whole homogenizing).Then, the heating of stopped reaction liquid, Slow cooling.Be cooled to after room temperature, use three-roll mill to carry out 2 precision work and process, obtain lubricating grease.
(the softening processing of lubricating grease)
With respect to the lubricating grease obtaining by aforesaid method, with automatic revolution formula stirrer (MAZERUSTAR processed of KURABO company), apply the centrifugal force of 400G, stir until denseness becomes No. 2 from No. 2.5 simultaneously.Composition and the evaluation result of this lubricating grease are shown in table 1.
(embodiment 2)
Except making to add reagent amount, be MDI18.9g, octyl amine 11.3g, cyclo-hexylamine 5.80g, manufacture in the same manner lubricating grease with embodiment 1, soften under the same conditions processing.Composition and the evaluation result of this lubricating grease are shown in table 1.
(embodiment 3)
Except making to add reagent amount, be MDI27.7g, octyl amine 22.3g, cyclo-hexylamine 4.01g, manufacture in the same manner lubricating grease with embodiment 1, soften under the same conditions processing.Composition and the evaluation result of this lubricating grease are shown in table 1.
(embodiment 4)
Except making to add reagent amount, be MDI27.7g, octyl amine 22.3g, cyclo-hexylamine 4.01g, and make beyond the speed of rotation of the agitating vane in grease manufacture changes into 400rpm from 250rpm, to manufacture in the same manner lubricating grease with embodiment 1.Wherein, do not carry out the softening processing of gained lubricating grease.Composition and the evaluation result of this lubricating grease are shown in table 1.
(embodiment 5)
Except making to add reagent amount, be MDI27.7g, octyl amine 22.3g, cyclo-hexylamine 4.01g, manufacture in the same manner lubricating grease with embodiment 1.Wherein, do not carry out the softening processing of gained lubricating grease.Composition and the evaluation result of this lubricating grease are shown in table 1.
(comparative example 1)
Except making to add reagent amount, be that MDI21.3g, octyl amine 21.3g(are not used cyclo-hexylamine), manufacture in the same manner lubricating grease with embodiment 1, soften under the same conditions processing.Composition and the evaluation result of this lubricating grease are shown in table 1.
(comparative example 2)
Except making to add reagent amount, be that MDI30.5g, cyclo-hexylamine 23.4g(are not used octyl amine), manufacture in the same manner lubricating grease with embodiment 1, soften under the same conditions processing.Composition and the evaluation result of this lubricating grease are shown in table 1.
(comparative example 3)
Except making to add reagent amount, be MDI12.3g, n-octylamine 9.84g, cyclo-hexylamine 1.89g, manufacture in the same manner lubricating grease with embodiment 1.Wherein, do not carry out the softening processing of gained lubricating grease.Composition and the evaluation result of this lubricating grease are shown in table 1.
(comparative example 4)
Except making to add reagent, be that MDI11.6g, Octadecane base amine 24.4g(are not used cyclo-hexylamine, octyl amine), lubricating grease manufactured in the same manner with embodiment 1.Wherein, do not carry out the softening processing of gained lubricating grease.Composition and the evaluation result of this lubricating grease are shown in table 1.
(reference example)
The evaluation result of low commercially available dirt lubricating grease (AFE-CA processed of THK company) is shown in table 1.
[table 1]
(evaluation result)
The lubricating grease of embodiment 1~5 is compared with the lubricating grease of reference example (commercially available) with comparative example 1~4, and known dirt is all extremely low.On the other hand, comparative example 1,3 is because the use level of thickening material when manufacturing lubricating grease is few, even thereby after stirring penetration degree be preferred value, powder amount is also many.Comparative example 2 is because penetration degree after stirring surpasses scope given to this invention, thereby powder amount is many.Comparative example 4 is because amounts of thickener is few, even thereby after stirring penetration degree be preferred value, powder amount is also slightly many.
Should illustrate, as shown in embodiment 4~5, even if do not utilize the aftertreatment (softening processing) of MAZERUSTAR, powder amount is also fully reduced.

Claims (13)

1. lubricating grease, is characterized in that, it is in containing the base oil of hydrocarbon, take total composition as benchmark, coordinates the allophanamide shown in the above and following formula as thickening material below 25 quality % (1) of 15 quality % to form,
     R 1NHCONHR 2NHCONHR 3     (1)
R 1, R 3mutually different, be the alkyl of carbonatoms 6 to 18; R 2for the divalence aromatic hydrocarbyl of carbonatoms more than 6 and below 13;
After the stirring of this lubricating grease, penetration degree is more than 170 and below 295.
2. lubricating grease claimed in claim 1, is characterized in that,
After the stirring of this lubricating grease, penetration degree is more than 230 and below 265.
3. the lubricating grease described in claim 1 or 2, is characterized in that,
Described alkyl is saturated hydrocarbyl.
4. lubricating grease claimed in claim 3, is characterized in that,
Described saturated hydrocarbyl is alkyl or cycloalkyl.
5. lubricating grease claimed in claim 4, is characterized in that,
Described cycloalkyl is cyclohexyl.
6. the lubricating grease described in claim 4 or 5, is characterized in that,
Described R 1, R 3for octyl group or cyclohexyl.
7. the lubricating grease described in any one in claim 4 to 6, is characterized in that,
The total amount of alkyl and cycloalkyl Zhe Liangzhong functional group of take is benchmark, the average proportions of the cycloalkyl in described allophanamide be 85 % by mole following and more than 15 % by mole.
8. lubricating grease claimed in claim 7, is characterized in that,
The average proportions of described cycloalkyl is below 50 % by mole and more than 15 % by mole.
9. lubricating grease claimed in claim 7, is characterized in that,
The average proportions of described cycloalkyl is below 85 % by mole and more than 75 % by mole.
10. the lubricating grease described in any one in claim 1 to 9, is characterized in that,
Take base oil total amount as benchmark, and described hydrocarbon is more than 90 quality %.
Lubricating grease in 11. claims 1 to 10 described in any one, is characterized in that,
Described hydrocarbon is poly-alpha olefins.
Lubricating grease in 12. claims 1 to 11 described in any one, is characterized in that,
40 ℃ of kinematic viscosity of base oil are 400mm 2below/s.
The softening method of 13. lubricating grease, is characterized in that, Yi Bian the lubricating grease described in any one in claim 1 to 12 is applied to centrifugal force, Yi Bian stir.
CN201380010619.4A 2012-02-24 2013-02-19 Grease and method for softening grease Pending CN104169404A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2012039214 2012-02-24
JP2012-039214 2012-02-24
PCT/JP2013/053959 WO2013125510A1 (en) 2012-02-24 2013-02-19 Grease and method for softening grease

Publications (1)

Publication Number Publication Date
CN104169404A true CN104169404A (en) 2014-11-26

Family

ID=49005695

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201380010619.4A Pending CN104169404A (en) 2012-02-24 2013-02-19 Grease and method for softening grease

Country Status (7)

Country Link
US (1) US20150045273A1 (en)
EP (1) EP2821465A4 (en)
JP (1) JPWO2013125510A1 (en)
KR (1) KR20140127241A (en)
CN (1) CN104169404A (en)
TW (1) TW201336983A (en)
WO (1) WO2013125510A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110546245A (en) * 2017-05-01 2019-12-06 出光兴产株式会社 Grease composition

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6618017B2 (en) * 2014-05-27 2019-12-11 出光興産株式会社 Urea grease
CN109937249A (en) * 2016-11-16 2019-06-25 出光兴产株式会社 Grease composition for machine having automatic grease supply device and method for manufacturing the same
EP3936590A4 (en) * 2019-03-05 2022-11-30 Idemitsu Kosan Co., Ltd. Grease composition, and lubrication method and device for sliding mechanism, using said grease composition
US11952549B2 (en) 2019-09-24 2024-04-09 Jtekt Corporation Grease composition and rolling bearing
JP2023151691A (en) * 2022-03-31 2023-10-16 出光興産株式会社 grease composition

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006029473A (en) * 2004-07-16 2006-02-02 Nsk Ltd Angular ball bearing and machine tool

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5511156B2 (en) * 1972-11-14 1980-03-22
JP2979274B2 (en) * 1992-06-29 1999-11-15 日本精工株式会社 Grease composition for high-speed rolling bearings
JPH0959661A (en) * 1995-08-21 1997-03-04 Nippon Seiko Kk Grease composition
US20030040442A1 (en) * 1997-07-02 2003-02-27 Nsk Ltd. Rolling bearing
JP4021532B2 (en) 1997-12-02 2007-12-12 日本精工株式会社 Grease and rolling device
JP2000192973A (en) * 1998-12-25 2000-07-11 Ntn Corp Low dusting rolling bearing
JP2003119485A (en) * 2001-10-16 2003-04-23 Nsk Ltd Method for producing grease
JP2004352953A (en) 2003-05-30 2004-12-16 Nsk Ltd Grease composition and rolling device
JP2005105025A (en) * 2003-09-29 2005-04-21 Nsk Ltd Grease composition and rolling bearing
JP4662118B2 (en) 2004-03-26 2011-03-30 協同油脂株式会社 Low dust generation grease composition
JP4461000B2 (en) * 2004-11-25 2010-05-12 本田技研工業株式会社 Grease composition for constant velocity joint and constant velocity joint
JP4843260B2 (en) * 2005-06-10 2011-12-21 Ntn株式会社 One-way clutch built-in type rotation transmission device
US8703678B2 (en) * 2006-10-06 2014-04-22 Idemitsu Kosan Co., Ltd. Grease

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006029473A (en) * 2004-07-16 2006-02-02 Nsk Ltd Angular ball bearing and machine tool

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刁立福: "《汽车性能与使用技术》", 31 January 2010, 中国水利水电出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110546245A (en) * 2017-05-01 2019-12-06 出光兴产株式会社 Grease composition
US11198834B2 (en) 2017-05-01 2021-12-14 Idemitsu Kosan Co., Ltd. Grease composition

Also Published As

Publication number Publication date
EP2821465A4 (en) 2015-11-25
KR20140127241A (en) 2014-11-03
TW201336983A (en) 2013-09-16
WO2013125510A1 (en) 2013-08-29
US20150045273A1 (en) 2015-02-12
EP2821465A1 (en) 2015-01-07
JPWO2013125510A1 (en) 2015-07-30

Similar Documents

Publication Publication Date Title
CN104169404A (en) Grease and method for softening grease
EP2785821B1 (en) Grease composition
JP6072532B2 (en) Grease composition
EP2489721B1 (en) Use of a grease composition for bearing of wind power generator
EP1930400B1 (en) Lubricant composition
CN103732729B (en) EV, HEV drive bearing of motor lubricant composition and EV, HEV to drive bearing of motor
JP2011178824A (en) Grease composition for hub unit bearing equipped with angular contact ball bearing, and hub unit bearing
CN105008503A (en) Grease composition for bearing
WO2012115141A1 (en) Grease composition
JP2014105252A (en) Grease composition
EP3692121A1 (en) Grease composition
CN102888271A (en) Rolling bearing lubricating grease composition and preparation method thereof
JP6826651B2 (en) Grease composition
CN102925258A (en) Lubricating grease composition and preparation method thereof
JP2020204015A (en) Grease composition and rolling bearing
CN104927984A (en) Rust-proof oil composition
CN1016514B (en) Composite lithium-base grease
CN107384558B (en) Lubricating grease with intercalation type layered magnesium phosphate as solid lubricating additive and preparation method thereof
JP3921061B2 (en) Grease composition
JP6919848B2 (en) Grease composition
CN105441164B (en) Chain lubricating oil and preparation method thereof
CN109825348A (en) A kind of low temperature resistant lubricating grease and preparation method thereof
CN107382927A (en) One kind lubrication oiliness improver and its synthetic method and application
JPS63312397A (en) Lubricant composition
JP2789044B2 (en) lubricant

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20141126