CN107312599A - Nano-graphene compounded lubricating oil - Google Patents

Nano-graphene compounded lubricating oil Download PDF

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Publication number
CN107312599A
CN107312599A CN201710545140.0A CN201710545140A CN107312599A CN 107312599 A CN107312599 A CN 107312599A CN 201710545140 A CN201710545140 A CN 201710545140A CN 107312599 A CN107312599 A CN 107312599A
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China
Prior art keywords
nano
graphene
oil
lubricating oil
compounded lubricating
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CN201710545140.0A
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Chinese (zh)
Inventor
林博
朱斌强
梁浩
罗金琼
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Guangxi Liugong Machinery Co Ltd
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Guangxi Liugong Machinery Co Ltd
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Priority to CN201710545140.0A priority Critical patent/CN107312599A/en
Publication of CN107312599A publication Critical patent/CN107312599A/en
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    • 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
    • C10M169/04Mixtures of base-materials and additives
    • C10M169/044Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
    • 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
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04Elements
    • C10M2201/041Carbon; Graphite; Carbon black
    • 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
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
    • 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
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/065Sulfides; Selenides; Tellurides
    • C10M2201/066Molybdenum sulfide
    • 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
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006Petroleum or coal fractions, e.g. tars, solvents, bitumen 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
    • C10M2217/00Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/02Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/024Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an amido or imido group
    • 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
    • C10N2030/04Detergent property or dispersant property
    • 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
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure

Abstract

The present invention relates to lubrication technical field, and in particular to a kind of nano-graphene compounded lubricating oil.The nano-graphene compounded lubricating oil, in parts by weight, at least including following components, 100 parts of lubricating base oil;1~5 part of nano-graphene;1~5 part of nano-particle;8~25 parts of dispersant;1~10 part of antiwear additive.The preparation method of the nano-graphene compounded lubricating oil, at least comprises the following steps:(1) lubricating base oil, nano-graphene, nano-particle are added in high-speed mixer simultaneously, are warming up at 100~150 DEG C, homogeneous is stirred 1~5 hour, at 100 DEG C, be incubated 2 hours;(2) dispersant, the antiwear additive of corresponding parts by weight are added into step (1), 90~110 DEG C are warming up to, is mixed 5~30 minutes under 1300r/min speed, obtains nano-graphene compounded lubricating oil.

Description

Nano-graphene compounded lubricating oil
Technical field
The present invention relates to lubrication technical field, and in particular to a kind of nano-graphene compounded lubricating oil.
Background technology
Lubricating oil plays non-as the indispensable material of mechanical movement to maintaining the operation of mechanism and improving mechanical life Chang Guanjian effect.With the continuous progress of modern industry, the requirement more and more higher to mechanism service life, while running environment Also increasingly harsher, these, which are required to used lubricating oil, has more excellent combination property.
At present, lubricating oil is broadly divided into:(1) alkyl lubricating oil is synthesized:Synthesizing alkyl lubricating oil has than mineral lubricant The more excellent performance of oil, mainly includes PAO artificial oils and alkylated aromatic hydrocarbons etc..(2) synthetic ester lubricant:Synthetic ester lubricant be by Organic acid and Organic Alcohol obtained under catalyst action by dehydration esterification reaction by organising that ester functional groups constitute Compound.(3) perfluoro polyether oil:Fluorine containing lubricant is the syntholube containing fluorine element, it is most important have perfluorocarbon hydrocarbon, Chloro-fluorocarbon hydrocarbon and PFPE (PFPE).(4) mineral oil, alias paraffin oil, white oil, white oil, mineral oil is by essence obtained by oil The cycloalkane and alkane mixture of the mixture, predominantly saturation of liquid hydrocarbon are refined, crude oil is taken out through normal pressure and vacuum fractionation, solvent Carry and dewax, hydrofinishing and obtain.
Above-mentioned lubricating oil is difficult to the use requirement for meeting lubricity, thus, it is also very desirable to synthesize a new nanometer Graphene compounded lubricating oil.
Graphene has unique two-dimensional structure and excellent performance, such as Young's modulus (about 1100GPa), thermal conductivity, load Transport factor and specific surface area etc. are flowed higher, also with fractional quantum hall effect, quantum Hall ferromagnetism and exciton band The phenomenons such as gap.Exactly because graphene has these excellent performances and unique structure, extensive concern in recent years is become Focus, cause greatly study hotspot in the energy, material, electronics, biology, medicine and other fields.
Thus, graphene is added to the compounded lubricating oil obtained in lubricating oil huge practical value.
The content of the invention
In order to solve prior art problem, the first aspect of the present invention provides a kind of nano-graphene compounded lubricating oil, In parts by weight, at least including following components,
As a kind of preferred technical scheme of the present invention, the lubricating base oil is selected from:Mineral oil, hydrocarbon system artificial oil, ester It is any one in oil, ether system oil.
As a kind of preferred technical scheme of the present invention, kinematic viscosity of the lubricating base oil at 40 DEG C is 40~ 200mm2/s。
As a kind of preferred technical scheme of the present invention, the nano-graphene is nitrogen-doped graphene.
As a kind of preferred technical scheme of the present invention, the dispersant is selected from:Polyisobutene succinimide, acetone, Any one in propene carbonate.
As a kind of preferred technical scheme of the present invention, the antiwear additive is selected from:It is two thio Acidic phosphates zinc, two thio Dialkyl amido formic acid molybdenum, two thio dialkyl amido lead formates, molybdenum disulfide, polytetrafluoroethylene (PTFE), dibutyl dithio amino The mixing of any one or more in formic acid antimony, tungsten disulfide, selenium disulfide.
As a kind of preferred technical scheme of the present invention, the nano-particle is selected from:It is nano silicon, nano oxidized In aluminium, nanometer sulfoacid calcium, nano-calcium carbonate, nano molybdenum disulfide, nano aluminum nitride, nano titanium oxide any one or it is several The mixing planted.
As a kind of preferred technical scheme of the present invention, the nano silicon is silane coupler modified nano-silica SiClx.
As a kind of preferred technical scheme of the present invention, the nano-graphene compounded lubricating oil also include antioxidant, Appointing in antirust agent, oiliness improver, viscosity index improving agent, pour-point depressant, defoamer, emulsifying agent, matal deactivator, detergent-dispersant additive The mixing for one or more of anticipating.
The second aspect of the present invention provides the preparation method of the nano-graphene compounded lubricating oil, at least including following Step:
(1) lubricating base oil, nano-graphene, nano-particle are added in high-speed mixer simultaneously, it is warming up to 100~ At 150 DEG C, homogeneous is stirred 1~5 hour, at 100 DEG C, is incubated 2 hours;
(2) dispersant, the antiwear additive of corresponding parts by weight are added into step (1), 90~110 DEG C are warming up to, in 1300r/ Mixed 5~30 minutes under min speed, obtain nano-graphene compounded lubricating oil.
Embodiment
The participation in the election detailed description of the invention below for being preferable to carry out method and including embodiment this hair can be more easily understood Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with art of the present invention The identical implication that technical staff is generally understood that.When there is contradiction, the definition in this specification is defined.
As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ", " having ", " containing " or its any other deformation, it is intended that cover including for non-exclusionism.For example, the combination comprising listed elements Thing, step, method, product or device are not necessarily limited to those key elements, but can include not expressly listed other key elements or Such a composition, step, method, product or the intrinsic key element of device.
Conjunction " Consists of " excludes any key element do not pointed out, step or component.If be used in claim, this Phrase will make claim be closed, it is not included the material in addition to materials of those descriptions, but relative normal Except rule impurity.When being rather than immediately following in the clause that phrase " Consists of " appears in claim main body after theme, It is only limited to the key element described in the clause;Other key elements are not excluded outside as the overall claim.
Equivalent, concentration or other values or parameter are excellent with scope, preferred scope or a series of upper limit preferred values and lower limit During the Range Representation that choosing value is limited, this, which is appreciated that, specifically discloses by any range limit or preferred value and any scope All scopes that any pairing of lower limit or preferred value is formed, regardless of whether whether the scope separately discloses.For example, when open During scope " 1 to 5 ", described scope should be interpreted as including scope " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to 5 ", " 1 to 3 and 5 " etc..When number range is described herein, unless otherwise indicated, otherwise the scope is intended to include its end Value and all integers and fraction within the range.
Singulative includes plural number and object is discussed, unless the context clearly dictates otherwise." optional " or it is " any It is a kind of " refer to that the item or event that describe thereafter may or may not occur, and the description include situation that event occurs and The situation that event does not occur.
Approximate term in specification and claims is used for modifying quantity, represents that the present invention is not limited to this specific Quantity, includes the part of the amendment of the acceptable change without cause related basic function close to the quantity.Phase Answer, modify a numerical value with " about ", " about " etc., mean that the invention is not restricted to the exact numerical.In some examples, approximately Term likely corresponds to the precision of the instrument of measured value.In present specification and claims, scope is limited can be with Combine and/or exchange, these scopes include all subranges contained therebetween if not stated otherwise.
In addition, the indefinite article " one kind " and " one " before key element of the present invention or component are to key element or the quantitative requirement of component (i.e. occurrence number) unrestriction.Therefore " one " or " one kind " should be read as including one or at least one, and odd number The key element or component of form also include plural form, unless the obvious purport of the quantity refers to singulative.
In order to solve prior art problem, the first aspect of the present invention provides a kind of nano-graphene compounded lubricating oil, In parts by weight, at least including following components,
As a kind of preferred technical scheme of the present invention, the lubricating base oil is selected from:Mineral oil, hydrocarbon system artificial oil, ester It is any one in oil, ether system oil.
Described mineral oil, alias white oil, paraffin oil.From reducing in the angle of cost, the application, the mineral of selection Oil is industrial grade white oil.The trade mark that can be enumerated be 2# white oils, 3# white oils, 5# white oils, 10# white oils, 15# white oils, 26# white oils, 32# white oils, 46# white oils, 60# white oils, 90# white oils, 120# white oils, 150# white oils, 300# white oils, 500# white oils etc., wherein, # Representative number.
Described hydrocarbon system artificial oil, what can be enumerated has:Polyalphaolefin, specifically there are:Polybutene, polyisobutene, 1- are pungent Any one or a few mixing in alkene oligomer, 1- decylene oligomers, ethylene-propylene copolymer.
Described ester system oil, what can be enumerated has:Dibutyl sebacate, decanedioic acid two (2- ethylhexyls) ester, adipic acid The sour first of dioctyl ester, diisodecyl adipate (DIDA), adipic acid two (tridecyl) ester, glutaric acid two (tridecyl) ester, acetylricinoleate The diester oils such as ester;The aromatic ester oils such as trioctyl trimellitate (TOTM), tri trimellitate last of the ten Heavenly stems ester, tetraoctyl 1,2,4,5-benzenetetra-carboxylate;Trihydroxy methyl Propane caprylate, trimethylolpropane pelargonate, pentaerythrite -2 ethyl hexanoic acid ester, pentaerythrite pelargonate etc..
Described ether system oil, what can be enumerated has:Polyethylene glycol, polypropylene glycol, polyethylene glycol monoether, polypropyleneglycol monoether Deng polyethylene glycol;Alkyl diphenyl ether, dialkyl diphenyl ether, five phenyl ethers, tetraphenyl ether, monoalkyl tetraphenyl ether, dialkyl group The phenyl ether oil such as tetraphenyl ether.
As a kind of preferred technical scheme of the present invention, kinematic viscosity of the lubricating base oil at 40 DEG C is 40~ 200mm2/s。
Term " nano-graphene " refers to carbon atom with sp2The cellular flat film of hybrid form formation, is a kind of Have the quasi- two-dimensional material of an atomic layer level thickness, monoatomic layer graphite done so being called, carbon atom it is regular be arranged in it is cellular Among lattice structure unit.Each carbon atom in addition to being connected with three carbon atoms of σ keys and other, remaining pi-electron and its The pi-electron formation big pi bond of delocalization of his carbon atom, thus, graphene is acted on due to stronger π-π, and its dispersiveness is poor.
In the application, described nano-graphene obtains to be commercially available, is purchased from Suzhou Heng Qiu graphenes Co., Ltd.
As a kind of preferred technical scheme of the present invention, the nano-graphene is nitrogen-doped graphene.
In the application, described nitrogen-doped graphene obtains to be commercially available, is purchased from Suzhou Heng Qiu graphenes Co., Ltd.
As a kind of preferred technical scheme of the present invention, the nano-particle is selected from:It is nano silicon, nano oxidized In aluminium, nanometer sulfoacid calcium, nano-calcium carbonate, nano molybdenum disulfide, nano aluminum nitride, nano titanium oxide any one or it is several The mixing planted.
As a kind of preferred technical scheme of the present invention, the nano silicon is silane coupler modified nano-silica SiClx.
In a preferred embodiment, the nano aluminium oxide is nano-aluminium oxide.
In the application, the nano aluminium oxide obtains to be commercially available, is purchased from Xuancheng Jingrui New Material Co., Ltd..
The nano aluminium oxide is silane coupler modified nano aluminium oxide.
In a preferred embodiment, the preparation method of the silane coupler modified nano aluminium oxide is as follows:
N- (2- the aminoethyls) -3- aminopropyl trimethoxysilanes for weighing 0.10g add 5g deionized waters, and use glacial acetic acid Regulation is stirred at room temperature 2h, obtains silane coupler hydrolyzate to pH=4;
3g nano aluminium oxides are weighed, are dissolved in the ethanol solution that volume fraction is 60%, ultrasonic disperse 30min, then Silane coupler hydrolyzate is being added, 2h is heated to reflux at 60 DEG C, is being centrifuged after the completion of reaction, 2~3 are washed using ethanol It is secondary, obtain silane coupler modified nano aluminium oxide after drying.
As a kind of preferred technical scheme of the present invention, the nano silicon is silane coupler modified nano-silica SiClx.
The nano silicon is silane coupler modified nano silicon.
Term " silane coupler modified nano silicon " refers to N- (2- aminoethyls) -3- aminopropyl trimethoxy silicon Alkane, 3- Mercaptopropyltriethoxysilanes are modified to nano silicon simultaneously.
In a preferred embodiment, N- (2- the aminoethyls) -3- aminopropyl trimethoxysilanes, 3- sulfydryls third Weight ratio between ethyl triethoxy silicane alkane, nano silicon is 5:1:10.
In a preferred embodiment, the preparation method of the silane coupler modified nano silicon is at least wrapped Include following steps:
In the reactor, solvent 80ml toluene and 10g nano silicons, ultrasonic disperse 30min are added, 5g is sequentially added N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes, 1g 3- Mercaptopropyltriethoxysilanes, the back flow reaction at 100 DEG C 5h, filtering, ethanol is washed 3 times, and silane coupler modified nano silicon is obtained after drying.
As a kind of preferred technical scheme of the present invention, the nano-graphene compounded lubricating oil also include antioxidant, Appointing in antirust agent, oiliness improver, viscosity index improving agent, pour-point depressant, defoamer, emulsifying agent, matal deactivator, detergent-dispersant additive The mixing for one or more of anticipating.
As a kind of preferred technical scheme of the present invention, the dispersant is selected from:Polyisobutene succinimide, acetone, Any one in propene carbonate.
As a kind of preferred technical scheme of the present invention, the antiwear additive is selected from:It is two thio Acidic phosphates zinc, two thio Dialkyl amido formic acid molybdenum, two thio dialkyl amido lead formates, molybdenum disulfide, polytetrafluoroethylene (PTFE), dibutyl dithio amino The mixing of any one or more in formic acid antimony, tungsten disulfide, selenium disulfide.
As a kind of preferred technical scheme of the present invention, the antioxidant is selected from:Phenol antioxidant, sulphur system are anti-oxidant The mixing of any one or more in agent, phosphorous antioxidant, amine system antioxidant.
What the antioxidant can be enumerated has:Containing in sulphur ester antioxidant, phenolic antioxidant, phosphite ester kind antioxidant It is at least one.
It can be enumerated containing sulphur ester antioxidant:Dilauryl thiodipropionate, thio-2 acid 2 stearyl ester or thio Dipropionic acid two (octadecyl ester), β, β '-thio two butyric acid two (18) ester, thio-2 acid bay octadecyl ester, thio-2 acid two (13) ester, thio-2 acid two (14) ester etc..
Phenolic antioxidant can be enumerated:1- hydroxy-3-methyl -4- cumenes, 2,6- DI-tert-butylphenol compounds, the uncles of 2,6- bis- Butyl -4- ethyl -phenols, BHT, 2,6- di-t-butyl -4- normal-butyls phenol, 4- methylols -2,6- bis- Tert-butyl phenol, butylhydroxy anisole, 2- (1- methylcyclohexyls) -4,6- xylenols, the tertiary fourths of 2,4- dimethyl -6- Base phenol, 2- methyl -4,6- dinonyl phenol, 2,6- di-t-butyls-alpha, alpha-dimethyl amino-p-cresol, 2,4,6- tri-butyl benzenes Double (the octylsulfo) -1,3,5-triazines of phenol, 6- (4- hydroxyl -3,5- di-tert-butyls amido) -2,4-, 4,6- it is double (4- hydroxyl -3, 5- di-t-butyls phenoxy group) -2- n-octylthios -1,3,5-triazines, β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid first Ester, β-positive octadecanol ester of (4-hydroxyl-3,5-di-tert-butyl-phenyl) propionic acid, styrenated phenol, 4,4 '-dihydroxy connection Benzene, butylated octylated phenol, butylated stytrene cresols, 2,2 '-methylene bis (4- methyl-6-tert-butylphenols) or 2, 2 '-methylene bis (the 6- tert-butyl group -4- cresols), 2,2 '-methylene bis (4- ethyl -6- tert-butyl phenols), 2,2 '-methylene bis (4- first Base -6- cyclohexylphenols), 4,4 '-methylene bis (2,6- DI-tert-butylphenol compounds), 2, (6- α-methylbenzyls are to first for 2 '-methylene bis Phenol), 1,1- double (4- hydroxy benzenes) hexamethylene, 2,2 '-methylene bis (4- methyl -6- (Alpha-Methyl cyclohexyl) phenol) or 2,2 '-two Hydroxyl -3,3 '-two (Alpha-Methyl cyclohexyl) -5,5 '-dimethyl diphenylmethane, 1,3,5- trimethyls -2,4,6- tri- (3,5- bis- Tertiary butyl-4-hydroxy benzyl) benzene, 1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyls) butane, four (3- (3 ' 5 '-two uncles Butyl -4 '-hydroxy phenyl) propionic acid) pentaerythritol ester, 4,4 '-thiobis (the 6- tert-butyl group -3- methylphenols) or 4,4 '-thio Double (6- tert-butyl-m-cresols), 4,4 '-thiobis (2- methyl-6-tert-butylphenols) or 4,4 '-thiobis (6- tert-butyl o first Phenol), 2, the double (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid of 2 '-thiobis (4- methyl-6-tert-butylphenols), hexylene glycol Ester), 2,2 '-thiobis (3 ,-(3,5- di-tert-butyl-hydroxy phenyl) ethyl propionate), N, double (3,5- bis- uncles of N '-hexamethylene Butyl-4- hydroxyls hydrocinnamamide), 1,3,5- tri- (the 4- tert-butyl group-3- hydroxyls-2,6- dimethyl benzyls) 1,3,5-triazine-2,4, 6- (1H, 3H, 5H)-triketone, 1,3,5- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) guanamines, 4,6- (1H, 3H, 5H) three Ketone or isocyanuric acid three (3,5- di-tert-butyl-4-hydroxyl benzyl ester), [β-(3,5- di-t-butyl -4- hydroxy benzenes of isocyanuric acid three Base) propionyloxy ethyl ester], double [3,3- double (3 '-tert-butyl group -4 '-hydroxy phenyl) butyric acid] glycol esters, 1,1 '-thiobis (2- Naphthols), double (3,5- di-tert-butyl-4-hydroxyl benzyl) thioethers, 2,5- di-tert-butyl hydroquinones, the tertiary pentyls of 2,5- bis- are to benzene two Phenol, 3,5- di-tert-butyl-4-hydroxyl benzyls di(2-ethylhexyl)phosphate (18) ester, 3,5- di-tert-butyl-4-hydroxyl benzyls diethyl phosphate, three Double -3- (3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester, hydroquinone dibenzyl ethers of glycol etc..
Phosphite ester kind antioxidant can be enumerated:Triphenyl phosphite, phosphorous acid three (nonyl phenyl ester), phosphorous acid three are different pungent Ester, triisodecyl phosphite ester, the isodecyl ester of phosphorous acid benzene two, trilauryl trithiophosphite, trilauryl phosphite, phosphorous acid Three (octadecyl esters), the isodecyl ester of diphosphorous acid pentaerythrite two, diphosphorous acid pentaerythrite distearyl alcohol ester, 4,4 '-fourth fork are double (sub- Phosphoric acid (3- methyl-6-tert butyl phenyl) two (tridecyl) esters), isooctyl diphenyl phosphite, phosphorous acid benzene di-isooctyl, Asia Diphenyl octyl phosphate, phosphorous acid hexichol isodecyl ester, dioctyl phosphite, phosphorous acid dilauryl, dimethylphosphite, phosphorous acid Double 13 esters of two oleyl alcohol esters, didecyl phosphite, dibutyl phosphite, phosphorous acid, phosphorous acid double 14 esters, phosphorous triethylenetetraminehexaacetic acids Ester, tributyl phosphite, triisopropyl phosphite, the monooctyl ester of phosphorous acid three or phosphorous acid three (2- ethylhexyls), phosphorous acid-benzene are double (nonyl benzene) ester, phosphorous acid hexichol nonyl phenyl ester, phosphorous acid three (2,4- di-tert-butyl-phenyl) ester etc..
The second aspect of the present invention provides the preparation method of the nano-graphene compounded lubricating oil, at least including following Step:
(1) lubricating base oil, nano-graphene, nano-particle are added in high-speed mixer simultaneously, it is warming up to 100~ At 150 DEG C, homogeneous is stirred 1~5 hour, at 100 DEG C, is incubated 2 hours;
(2) dispersant, the antiwear additive of corresponding parts by weight are added into step (1), 90~110 DEG C are warming up to, in 1300r/ Mixed 5~30 minutes under min speed, obtain nano-graphene compounded lubricating oil.
The present invention is specifically described below by embodiment.It is necessarily pointed out that, following examples are only used In the invention will be further described, it is impossible to be interpreted as limiting the scope of the invention, professional and technical personnel in the field Some the nonessential modifications and adaptations made according to the content of the invention described above, still fall within protection scope of the present invention.
Embodiment 1
Embodiments herein 1 provides a kind of nano-graphene compounded lubricating oil, in parts by weight, at least including following Component,
Described lubricating base oil is mineral oil, and the mineral oil is 60# white oils;
Described nano-graphene is nitrogen-doped graphene, is purchased from Suzhou Heng Qiu graphenes Co., Ltd.
Described nano aluminium oxide is purchased from Xuancheng Jingrui New Material Co., Ltd..
Described dispersant is polyisobutene succinimide;
Described antiwear additive is molybdenum disulfide;
The preparation method of the nano-graphene compounded lubricating oil, at least comprises the following steps:
(1) lubricating base oil, nano-graphene, nano aluminium oxide are added in high-speed mixer simultaneously, is warming up to 150 DEG C Under, homogeneous is stirred 1 hour, at 100 DEG C, is incubated 2 hours;
(2) dispersant, the antiwear additive of corresponding parts by weight are added into step (1), 90 DEG C are warming up to, 1300r/min's Mixed 30 minutes under speed, obtain nano-graphene compounded lubricating oil.
Embodiment 2
Embodiments herein 2 provides a kind of nano-graphene compounded lubricating oil, in parts by weight, at least including following Component,
Described lubricating base oil is mineral oil, and the mineral oil is 60# white oils;
Described nano-graphene is nitrogen-doped graphene, is purchased from Suzhou Heng Qiu graphenes Co., Ltd.
Described nano aluminium oxide is purchased from Xuancheng Jingrui New Material Co., Ltd..
Described dispersant is polyisobutene succinimide;
Described antiwear additive is molybdenum disulfide;
The preparation method of the nano-graphene compounded lubricating oil, at least comprises the following steps:
(1) lubricating base oil, nano-graphene, nano aluminium oxide are added in high-speed mixer simultaneously, is warming up to 150 DEG C Under, homogeneous is stirred 1 hour, at 100 DEG C, is incubated 2 hours;
(2) dispersant, the antiwear additive of corresponding parts by weight are added into step (1), 90 DEG C are warming up to, 1300r/min's Mixed 30 minutes under speed, obtain nano-graphene compounded lubricating oil.
Embodiment 3
Embodiments herein 3 provides a kind of nano-graphene compounded lubricating oil, in parts by weight, at least including following Component,
Described lubricating base oil is mineral oil, and the mineral oil is 60# white oils;
Described nano-graphene is nitrogen-doped graphene, is purchased from Suzhou Heng Qiu graphenes Co., Ltd.
Described nano aluminium oxide is purchased from Xuancheng Jingrui New Material Co., Ltd..
Described dispersant is polyisobutene succinimide;
Described antiwear additive is molybdenum disulfide;
The preparation method of the nano-graphene compounded lubricating oil, at least comprises the following steps:
(1) lubricating base oil, nano-graphene, nano aluminium oxide are added in high-speed mixer simultaneously, is warming up to 150 DEG C Under, homogeneous is stirred 1 hour, at 100 DEG C, is incubated 2 hours;
(2) dispersant, the antiwear additive of corresponding parts by weight are added into step (1), 90 DEG C are warming up to, 1300r/min's Mixed 30 minutes under speed, obtain nano-graphene compounded lubricating oil.
Embodiment 4
Embodiments herein 4 provides a kind of nano-graphene compounded lubricating oil, in parts by weight, at least including following Component,
Described lubricating base oil is mineral oil, and the mineral oil is 60# white oils;
Described nano-graphene is nitrogen-doped graphene, is purchased from Suzhou Heng Qiu graphenes Co., Ltd;
The nano aluminium oxide is silane coupler modified nano aluminium oxide;
Described dispersant is polyisobutene succinimide;
Described antiwear additive is molybdenum disulfide;
The preparation method of the silane coupler modified nano aluminium oxide, at least comprises the following steps:
N- (2- the aminoethyls) -3- aminopropyl trimethoxysilanes for weighing 0.10g add 5g deionized waters, and use glacial acetic acid Regulation is stirred at room temperature 2h, obtains silane coupler hydrolyzate to pH=4;
3g nano aluminium oxides are weighed, are dissolved in the ethanol solution that volume fraction is 60%, ultrasonic disperse 30min, then Silane coupler hydrolyzate is being added, 2h is heated to reflux at 60 DEG C, is being centrifuged after the completion of reaction, is being washed 3 times using ethanol, Silane coupler modified nano aluminium oxide is obtained after drying.
The preparation method of the nano-graphene compounded lubricating oil, at least comprises the following steps:
(1) lubricating base oil, nano-graphene, nano aluminium oxide are added in high-speed mixer simultaneously, is warming up to 150 DEG C Under, homogeneous is stirred 1 hour, at 100 DEG C, is incubated 2 hours;
(2) dispersant, the antiwear additive of corresponding parts by weight are added into step (1), 90 DEG C are warming up to, 1300r/min's Mixed 30 minutes under speed, obtain nano-graphene compounded lubricating oil.
Embodiment 5
Embodiments herein 5 provides a kind of nano-graphene compounded lubricating oil, in parts by weight, at least including following Component,
Described lubricating base oil is mineral oil, and the mineral oil is 60# white oils;
Described nano-graphene is nitrogen-doped graphene, is purchased from Suzhou Heng Qiu graphenes Co., Ltd;
Described dispersant is polyisobutene succinimide;
Described antiwear additive is molybdenum disulfide;
The nano-particle is the mixture of nano aluminium oxide and nano silicon;
Weight ratio between nano aluminium oxide and nano silicon is 1:1;
The nano aluminium oxide is silane coupler modified nano aluminium oxide;
The nano silicon is silane coupler modified nano silicon;
The preparation method of the silane coupler modified nano aluminium oxide, at least comprises the following steps:
N- (2- the aminoethyls) -3- aminopropyl trimethoxysilanes for weighing 0.10g add 5g deionized waters, and use glacial acetic acid Regulation is stirred at room temperature 2h, obtains silane coupler hydrolyzate to pH=4;
3g nano aluminium oxides are weighed, are dissolved in the ethanol solution that volume fraction is 60%, ultrasonic disperse 30min, then Silane coupler hydrolyzate is being added, 2h is heated to reflux at 60 DEG C, is being centrifuged after the completion of reaction, is being washed 3 times using ethanol, Silane coupler modified nano aluminium oxide is obtained after drying.
The preparation method of silane coupler modified nano silicon is as follows:
In the reactor, solvent 80ml toluene and 10g nano silicons, ultrasonic disperse 30min are added, 5g is sequentially added N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes, 1g 3- Mercaptopropyltriethoxysilanes, the back flow reaction at 100 DEG C 5h, filtering, ethanol is washed 3 times, and silane coupler modified nano silicon is obtained after drying.
The preparation method of the nano-graphene compounded lubricating oil, at least comprises the following steps:
(1) lubricating base oil, nano-graphene, nano-particle are added in high-speed mixer simultaneously, is warming up to 150 DEG C Under, homogeneous is stirred 1 hour, at 100 DEG C, is incubated 2 hours;
(2) dispersant, the antiwear additive of corresponding parts by weight are added into step (1), 90 DEG C are warming up to, 1300r/min's Mixed 30 minutes under speed, obtain nano-graphene compounded lubricating oil.
Comparative example 1
The be the same as Example 3 of comparative example 1, difference is, not including nano aluminium oxide.
Comparative example 2
The be the same as Example 3 of comparative example 2, difference is, not including nano-graphene.
Comparative example 3
The be the same as Example 3 of comparative example 3, difference is, not including dispersant.
Comparative example 4
The be the same as Example 5 of comparative example 4, difference is, the silane coupler modified nano aluminium oxide is 3- (2,3- epoxies Third oxygen) propyl trimethoxy silicane modified nano-alumina.3- (2,3- the third oxygen of the epoxy) propyl trimethoxy silicane is modified The preparation method of nano aluminium oxide is as follows:
3- (2,3- the third oxygen of the epoxy) propyl trimethoxy silicane for weighing 0.10g adds 5g deionized waters, and uses glacial acetic acid Regulation is stirred at room temperature 2h, obtains silane coupler hydrolyzate to pH=4;
3g nano aluminium oxides are weighed, are dissolved in the ethanol solution that volume fraction is 60%, ultrasonic disperse 30min, then Silane coupler hydrolyzate is being added, 2h is heated to reflux at 60 DEG C, is being centrifuged after the completion of reaction, 2~3 are washed using ethanol It is secondary, obtain 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane modified nano-alumina after drying.
Comparative example 5
The be the same as Example 3 of comparative example 5, difference is, nitrogen-doped graphene is replaced with into graphene.
Comparative example 6
The be the same as Example 3 of comparative example 6, difference is, nitrogen-doped graphene is replaced with into graphene oxide.
Method of testing
1st, maximum nonseizure load PB:Maximum nonseizure load test is tested using GB/T 3142-1982 standards; This indicator measurements is higher, illustrates that oil lubrication performance is better.
2nd, sintering load PD:Sintering load test is using GB/T 3142-1982;Sintering load is higher, illustrates lubricating oil Extreme boundary lubrication performance is better.
3rd, wear scar diameter d:Wear scar diameter d tests are using SH/T 0189-1992 (292N, 60min, 75 DEG C, 1200r/ min);Wear scar diameter is smaller, illustrates the antiwear property of lubricating oil.
The performance test of table 1
From table 1 it follows that the nano-graphene compounded lubricating oil of the application has good greasy property.
Foregoing example is merely illustrative, some features of the feature for explaining the disclosure.Appended claim The scope as wide as possible for requiring to be contemplated that is intended to, and embodiments as presented herein is only according to all possible embodiment Combination selection embodiment explanation.Therefore, the purpose of applicant is appended claim not by the explanation present invention Feature example selectional restriction.And the progress in science and technology by formed language performance it is inaccurate due to and not The possible equivalent or son being presently considered are replaced, and these changes should also be interpreted by appended in the conceived case Claim is covered.

Claims (10)

1. a kind of nano-graphene compounded lubricating oil, it is characterised in that in parts by weight, at least including following components,
2. nano-graphene compounded lubricating oil as claimed in claim 1, it is characterised in that the lubricating base oil is selected from:Ore deposit Thing oil, hydrocarbon system artificial oil, ester system oil, ether system oil in any one.
3. nano-graphene compounded lubricating oil as claimed in claim 2, it is characterised in that the lubricating base oil is at 40 DEG C Kinematic viscosity be 40~200mm2/s。
4. nano-graphene compounded lubricating oil as claimed in claim 1, it is characterised in that the nano-graphene is N doping Graphene.
5. nano-graphene compounded lubricating oil as claimed in claim 1, it is characterised in that the dispersant is selected from:Poly- isobutyl Any one in alkene succimide, acetone, propene carbonate.
6. nano-graphene compounded lubricating oil as claimed in claim 1, it is characterised in that the antiwear additive is selected from:Two is thio Acidic phosphates zinc, two thio dialkyl amido formic acid molybdenums, two thio dialkyl amido lead formates, molybdenum disulfide, polytetrafluoroethyl-ne The mixing of any one or more in alkene, dibutyl dithiocaarbamate antimony, tungsten disulfide, selenium disulfide.
7. nano-graphene compounded lubricating oil as claimed in claim 1, it is characterised in that the nano-particle is selected from:Nanometer Silica, nano aluminium oxide, nanometer sulfoacid calcium, nano-calcium carbonate, nano molybdenum disulfide, nano aluminum nitride, nanometer titanium dioxide Any one or a few mixing in titanium.
8. nano-graphene compounded lubricating oil as claimed in claim 7, it is characterised in that the nano silicon is silane Coupling agent modified nano silicon.
9. nano-graphene compounded lubricating oil as claimed in claim 1, it is characterised in that the nano-graphene is composite lubricated Oil also includes antioxidant, antirust agent, oiliness improver, viscosity index improving agent, pour-point depressant, defoamer, emulsifying agent, metal passivation The mixing of any one or more in agent, detergent-dispersant additive.
10. the preparation method of the nano-graphene compounded lubricating oil as described in claim 1~9, it is characterised in that at least include Following steps:
(1) lubricating base oil, nano-graphene, nano-particle are added in high-speed mixer simultaneously, is warming up to 100~150 DEG C Under, homogeneous is stirred 1~5 hour, at 100 DEG C, is incubated 2 hours;
(2) dispersant, the antiwear additive of corresponding parts by weight are added into step (1), 90~110 DEG C are warming up to, 1300r/min's Mixed 5~30 minutes under speed, obtain nano-graphene compounded lubricating oil.
CN201710545140.0A 2017-07-06 2017-07-06 Nano-graphene compounded lubricating oil Pending CN107312599A (en)

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CN107880974A (en) * 2017-12-01 2018-04-06 苏州市宽道模具机械有限公司 A kind of lubricious oil additive based on modified nano-alumina and preparation method thereof
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CN110437918A (en) * 2019-08-26 2019-11-12 黄娟 A kind of antioxygen body self-restoring lubricating oil and preparation method thereof containing graphene oxide
CN110760365A (en) * 2018-07-27 2020-02-07 宝山钢铁股份有限公司 Graphene oxide/silicon dioxide-aluminum oxide nano composite water-based lubricant and preparation method thereof
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CN111040863A (en) * 2019-12-12 2020-04-21 贵安新区瑞诚生物工程有限公司 Preparation method of graphene lubricating oil, graphene lubricating oil and application
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CN111909751A (en) * 2020-08-25 2020-11-10 重庆石墨烯研究院有限公司 High-temperature extreme-pressure wear-resistant lubricating oil and preparation method thereof
CN113293045A (en) * 2021-05-27 2021-08-24 中国人民解放军空军勤务学院 Vulcanized nano-doped graphene anti-wear and anti-friction lubricating oil additive and preparation method and application thereof
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