CN106350153A - Modified graphene oxide, engine lubricating oil and application thereof - Google Patents

Modified graphene oxide, engine lubricating oil and application thereof Download PDF

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Publication number
CN106350153A
CN106350153A CN201610723166.5A CN201610723166A CN106350153A CN 106350153 A CN106350153 A CN 106350153A CN 201610723166 A CN201610723166 A CN 201610723166A CN 106350153 A CN106350153 A CN 106350153A
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graphene oxide
oil
modified graphene
lubricating oil
base oil
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CN106350153B (en
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唐果东
张宇
宫明军
严守洋
姚常青
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Jiangsu Hi Tech Co Ltd
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Jiangsu Hi Tech Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
    • C10M141/06—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic nitrogen-containing compound
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
    • C10M141/12—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic compound containing atoms of elements not provided for in groups C10M141/02 - C10M141/10
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    • 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
    • C10M169/04—Mixtures of base-materials and additives
    • C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
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    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/087—Boron oxides, acids or salts
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/281—Esters of (cyclo)aliphatic monocarboxylic acids
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/283—Esters of polyhydroxy compounds
    • C10M2207/2835—Esters of polyhydroxy compounds used as base material
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
    • C10M2209/084—Acrylate; Methacrylate
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    • 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
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/086—Imides
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/046—Overbasedsulfonic acid salts
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • 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
    • C—CHEMISTRY; METALLURGY
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    • 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
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    • 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
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • 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
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/12—Groups 6 or 16
    • C—CHEMISTRY; METALLURGY
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/02—Viscosity; Viscosity index
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/72—Extended drain
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/25—Internal-combustion engines

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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)

Abstract

The invention discloses a graphene oxide modifying method and application thereof in engine lubricating oil. The method comprises the following steps: firstly preparing graphene oxide (GO) by adopting an improved Hummers process, and modifying the graphene oxide with long-chain fatty amine and organic silicon to obtain modified graphene derivative; and secondly, taking the modified graphene oxide as A), and compounding a friction modifier with a metal cleaning agent B), a metal corrosion inhibitor C), a complex antioxidant, an anti-foaming agent, a viscosity index improver, synthetic ester base oil and base oil, so that the engine lubricating oil added with the graphene oxide modifying agent is obtained. The method disclosed by the invention has the advantages that abrasion of an engine is greatly reduced by adding the graphene oxide modifying agent, so that oil draining period of automobile engine oil is prolonged to 50000 kilometers from 5000 kilometers, and fuel oil can be saved by 7-10% in the aspect of fuel economy.

Description

A kind of modified graphene oxide, engine lubricating oil and its application
Technical field
The present invention relates to a kind of modified graphene oxide, engine lubricating oil and its application, belong to technical field of lubricating oil.
Background technology
Electromotor is automobile and the heart of many industrial equipments, and the consumption of its lubricating oil accounts for lubricating oil total amount about 50%, is profit Lubricating oil industry is paid close attention to most, is also the fastest kind that updates.Engine oil plays lubrication, cooling, close as the blood of electromotor Envelope, cleaning are kept a public place clean and the effect such as antirust, anti-corrosive, are to maintain the functional liquid of engine long life-span, Effec-tive Function.
Manufacture with electromotor is more and more accurate, and the requirement to lubricating oil is more and more harsher, lube oil additive for Improve lubricants performance most important.In current Lube Oil Market, conventional lubrication oil still occupies leading position, but due to it Lubricating ability is limited and conventional lubrication oily in the sulfur-bearing that adds, phosphorus, the additive of the element such as chlorine severe contamination is caused to environment, Work requirements now cannot be met.Therefore, the research of novel lubricating oil additive is subject to the extensive pass of lot of domestic and foreign scholar Note.
Carbon nano lubricating oil additive instead of traditional additive containing elements such as sulfur, phosphorus, chlorine, solves it to friction Corrosion and environmental problem that subband comes；Nanometer additive particle diameter is little simultaneously, is uniformly dispersed it is possible to fill friction in base oil The cut of secondary surface, plays repair；And nano-particle is dispersed in oil in the form of colloid, it is difficult to form blocking.
Graphene, due to molecular structure, itself possesses self-lubricating property so as to can be used for preparing Graphene lubrication Film.Research shows, for more exposed Copper Foil, the Copper thin film of Graphene deposition has higher contact angle and lower friction system Number, can be used as high-performance lubricating film.But make it can not be molten because Graphene has each other stronger model ylid bloom action power Stable dispersion in agent, also bad with the compatibility of other materials, easily stacked together again be difficult to open, this be restriction graphite Alkene research and a major obstacle of application.Therefore, Graphene is modified with improve its dispersibility in a solvent and with The compatibility of other materials, has highly important theoretical and realistic meaning.
Content of the invention
The purpose of the present invention is: provides a kind of Graphene of modification, and this modified graphene exists as additive Application in lubricating oil.
Technical scheme is:
A kind of modified graphene oxide, is using graphene oxide as raw material, then passes through surface long-chain fat race amine and/or silicon Alkane coupling agent obtains after modifying.
Graphene oxide refers to prepare using hummers method.
The preparation method of described modified graphene oxide, comprises the steps:
Long-chain fat amine is dissolved in ethanol, after mix homogeneously, is poured into containing in graphene oxide (go) aqueous solution, heats Reaction, naturally cools to room temperature afterwards, reaction solidss is leached, uses washing with alcohol solidss, filtration cakes torrefaction, finally obtain and change The graphene oxide of property.
Described long-chain fat amine is selected from lauryl amine, tetradecylamine, hexadecylamine or octadecylamine.
When being dissolved in long-chain fat amine in ethanol, silane coupler wherein can also be added.
Described silane coupler is selected from kh-550, kh-560 or kh-570.
The application in lubricating oil as friction improver of above-mentioned modified graphene oxide.
A kind of engine lubricating oil, includes following component by weight percentage:
A) friction improver 1.0～2.2%
B) metal detergent 0.5～1.1%
C) metal corrosion inhibitor 0.2～1.2%
D) antioxidant 2.0～2.5%
E) defoamer 0.05～0.1%
F) dispersant 1～1.2%
G) viscosity index improver 8～10%
H) synthesizing ester base oil 8～10%
I) base oil surplus；
Wherein, include above-mentioned modified graphene oxide in described friction improver.
Described friction improver also can also include molybdenum dialkyldithiocarbamacompositions, nano boric acid salt or receive One or more of rice boric acid；More preferably molybdenum dialkyldithiocarbamacompositions, nano boric acid salt, nano boric acid, modification Graphene oxide according to weight than 11:6:2:1 compound form.
Described metal detergent is alkyl benzene calcium sulfonate between 500～600mgkoh/g for the base number；Described alkyl Benzenesulfonic acid calcium is the sulfonic acid calcium salt that carbon number is straight or branched alkyl between c10～c20.
Metal corrosion inhibitor be one of zinc dialkyl dithiophosphate or dialkyl dithio amidocarbonic acid zinc or Two kinds of mixture.
Antioxidant is phenolic ester kind antioxidant, amine antioxidants, dialkyl dithio amino formate aid anti-oxidants compound and Become.
Defoamer is preferably acrylic ester type non-silicon defoaming agent.
Dispersant is preferably the mixing of one of mono butonediimide or Ramulus Uncariae Cum Uncis imidodicarbonic diamide or two kinds.
Viscosity index improver is selected from one of polyethylene propylene copolymer, polymethacrylates or polyisobutylene Or multiple mixing.
Synthesizing ester base oil is preferably pentaerythritol ester, and viscosity grade is 100 °, and viscosity is in 8～10mm2/s.
Hydrogenated base oil is selected from two class hydrogenated base oil 500sn, two class hydrogenated base oil 500n, three class hydrogenated base oils One of 500sn or three class hydrogenated base oil 500n or several mixing.
Beneficial effect
The present invention passes through to add compound friction improving agent to reduce coefficient of friction, greatly reduces the abrasion of electromotor, simultaneously Graphene Modifying agent, the addition of organic-molybdenum friction modifiers can replace phosphor-included additive, can reduce the phosphorus content in lubricating oil component, Reduce the impact to vehicle exhaust three-way catalytic apparatus, add substantial amounts of antioxidant with friction modifiers compounding use energy greatly Extend the oil draining period, make the automobile engine oil oil draining period extend to 50,000 kilometers from 5000 kilometers, fuel economy aspect, Ke Yijie Save fuel oil 7～10%.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail.But those skilled in the art will manage Solution, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Unreceipted concrete skill in embodiment Art or condition person, are carried out according to the technology described by document in the art or condition or according to product description.Examination used Agent or the unreceipted production firm person of instrument, be can by city available from conventional products.
Using the value of range format expression should be interpreted as in a flexible way not only including clearly including as scope The numerical value of limit value, but also include covering all single numbers within the range or subinterval, just as each numerical value and sub-district Between be expressly recited out.For example, the concentration range of " about 0.1% to about 5% " should be understood to not only to include clearly to include The concentration of about 0.1% to about 5%, also includes single concentration (e.g., 1%, 2%, 3% and 4%) and the subinterval (example in the range of alluding to As 0.1% to 0.5%, 1% to 2.2%, 3.3% to 4.4%).Heretofore described percentage ratio no illustrate in the case of, Refer to percentage by weight.
" embodiment ", " another embodiment ", " embodiment " of being addressed in this manual etc., refers to In conjunction with this embodiment description specific features, structure or include the application generality description at least one embodiment in. Multiple local appearance statement of the same race in the description is not necessarily to refer to same embodiment.Furthermore, it is understood that combining arbitrary When embodiment describes specific features, structure or feature, to be advocated is to realize this spy with reference to other embodiment Levy, structure or feature also fall in the application scope of the claimed.
The present invention is by being modified to graphene oxide, and is applied in lube oil additive, improves lubrication Oiliness energy.
The preparation method of this modified graphene oxide, mainly adopts the graphite oxide of improved hummer method preparation Alkene is precursor, by solvent-thermal method, with long-chain fat race amine under different reaction conditions, the modified graphene such as organosilicon, Lauryl amine, tetradecy lamine, cetylamine, octadecylamine (oda), hexadecyl trimethoxy silane, γ-methyl is adopted in the present invention Acryloxypropyl trimethoxy silane (kh-570) etc. is modified to graphene oxide, is prepared for functionalization graphite oxide Alkene.
Heretofore described improvement hummers method prepares graphene oxide can be using the side disclosed in known technology Method is prepared, and is exemplified below: 1) by 1g native graphite, dense h2so4、h3po4Three is placed in there-necked flask, and dense h2so4With h3po4Volume ratio be 9: 1, and by several times add 6g potassium permanganate, ice-water bath stir 1h.2) temperature rises to 50 DEG C, and insulation is anti- Answer 12h.3) products therefrom is poured in frozen water, add appropriate hydrogen peroxide while stirring, until solution colour is changed into golden yellow, so After filter, and be 5% with hcl(volume fraction) and distilled water product is washed till ph value close to 7.Finally, gained graphite oxide is divided It is dispersed in water, ultrasonic 8h, be placed in drying for standby in vacuum drying oven.
After having obtained modified graphene oxide, can be as additive application in lubricating oil.
The lubricating oil that the present invention provides can be made up of following component by weight percentage:
A) friction improver 1.0～2.2%
B) metal detergent 0.5～1.1%
C) metal corrosion inhibitor 0.2～1.2%
D) antioxidant 2.0～2.5%
E) defoamer 0.05～0.1%
F) dispersant 1～1.2%
G) viscosity index improver 8～10%
H) synthesizing ester base oil 8～10%
I) base oil surplus.
Friction improver in described component a), at least needs to include the graphene oxide of above-mentioned modification, in addition yet may be used To include one or more of molybdenum dialkyldithiocarbamacompositions, nano boric acid salt or nano boric acid；It is preferably two Alkyl molybdenum dithiocarbamate, nano boric acid salt, nano boric acid, modified graphene oxide are more multiple than 11:6:2:1 according to weight Join and form.
In described component b), metal detergent is alkyl benzene calcium sulfonate between 500～600mgkoh/g for the base number, described Alkyl benzene calcium sulfonate be the sulfonic acid calcium salt that carbon number is straight or branched alkyl between c10～c20, for example: base number is 500 Octadecyl benzenesulfonic acid calcium between～600mgkoh/g.
Metal corrosion inhibitor in described component c) is zinc dialkyl dithiophosphate or dialkyl dithio amido first The mixture of one of sour zinc or two kinds.
Antioxidant in described component d) be preferably t508(phenolic ester kind antioxidant), t557(amine antioxidants), t323(bis- Alkyl dithiocarbamate aid anti-oxidants) form according to weight is more compounding than 2:2:1.
In described component e), defoamer is preferably acrylic ester type non-silicon defoaming agent.
In described component f), dispersant is preferably one of mono butonediimide or Ramulus Uncariae Cum Uncis imidodicarbonic diamide or two kinds Mixing.
In described component g), viscosity index improver is selected from polyethylene propylene copolymer, polymethacrylates or gathers different The mixing of one or more of butylene.
In described component h), synthesizing ester base oil is preferably pentaerythritol ester, and viscosity grade is 100 ° of viscosity 8～ 10mm2/s.
Hydrogenated base oil described in described component i) is selected from two class hydrogenated base oil 500sn, two class hydrogenated base oils One of 500n, three class hydrogenated base oil 500sn or three class hydrogenated base oil 500n or several mixing.
Above lubricating oil can be prepared in the way of conventional heating mixing.For example: by the basis of component h) and 1/3 It is warming up to 50 DEG C in oil addition reactor, sequentially add component b), component c), component f), component d), component a), stir 30 points Clock, the base oil adding 1/3 is warming up to 70 DEG C, adds component g), stirs 30 minutes, adds remaining 1/3 basis Oil stirring 2 hours, adds component e) while stirring, and filtration gets product.
Prepared by embodiment 1 long-chain fat amine modified graphene
Respectively by the different long-chain fat amine (lauryl amine, tetradecylamine, hexadecylamine, octadecylamine) of 500g It is dissolved in the 95v/v% ethanol of 50l, ultrasonic disperse 1 hour, is made into uniform solution, it is poured rapidly into the 10mg/ml containing 50l Graphene oxide (go) aqueous solution carry teflon-lined stainless steel cauldron in, 100 DEG C heating, react 2h, it After naturally cool to room temperature, by reaction solidss leach, mixed with solidss with ethanol as solvent, by product in 9000r/min Lower centrifugation 30min, repeated centrifugation three times, remove unreacted organic amine, vacuum filtration product, and use a large amount of deionized water rinsings Three times, filter cake is dried overnight at 30 DEG C of vacuum, finally obtains the modified graphene oxide of light/dark balance powder long-chain fat amine.
The product that different organic amines obtain must be measured:
Embodiment 2
Difference with embodiment 1 is: in graphene oxide modification, is also added into silane coupler γ-methacryloxypropyl Propyl trimethoxy silicane (kh-570).
The octadecylamine of 500g and 50g kh570 are dissolved in the 95v/v% ethanol of 50l, ultrasonic disperse 1 hour, are made into Uniform solution, graphene oxide (go) aqueous solution it being poured rapidly into the 10mg/ml containing 50l carries polytetrafluoroethyllining lining Stainless steel cauldron in, 100 DEG C heating, react 2h, naturally cool to room temperature afterwards, by reaction solidss leach, use ethanol Make solvent to mix with solidss, product is centrifuged under 9000r/min 30min, repeated centrifugation three times, removes unreacted organic Amine, vacuum filtration product, and with a large amount of deionized water rinsing three times, filter cake is dried overnight at 30 DEG C of vacuum, finally obtains The modified graphene oxide of light/dark balance powder octadecylamine.
The preparation of embodiment 3 diesel lubrication oil
A) friction improver (molybdenum dialkyldithiocarbamacompositions, nano boric acid salt, nano boric acid, modified graphene oxide Compound than 11:6:2:1 according to weight and form) 1.1%, modified graphene oxide here is respectively adopted 4 obtain in embodiment 1 Plant the modified graphene oxide obtaining in the modified graphene oxide of long-chain fat amine and embodiment 2.
B) metal detergent (octadecyl benzenesulfonic acid calcium between 500～600mgkoh/g for the base number) 0.5%
C) metal corrosion inhibitor (zinc dialkyl dithiophosphate) 0.3%
D) antioxidant (t508(phenolic ester kind antioxidant), t557(amine antioxidants), t323(dialkyl dithio amino formate Aid anti-oxidants) form according to weight is more compounding than 2:2:1) 2.1%
E) defoamer (acrylic ester type non-silicon defoaming agent) 0.05%
F) dispersant (mono butonediimide) 1%
G) viscosity index improver (polymethacrylates) 8%
H) (pentaerythritol ester, viscosity grade is 100 ° of viscosity in 8～10mm to synthesizing ester base oil2/s) 8%
I) base oil (two class hydrogenated base oil 500sn) surplus.
Its preparation method is: the base oil of component h) and 1/3 is added in reactor and is warming up to 50 DEG C, sequentially add component B), component c), component f), component d), component a), stirs 30 minutes, the base oil adding 1/3 is warming up to 70 DEG C, adds Component g), stirs 30 minutes, and the base oil adding remaining 1/3 stirs 2 hours, adds component e) while stirring, filtration is Obtain finished product.
Reference examples 1
Difference with embodiment 3 is: is provided without the graphene oxide of modification, but directly prepared by hummers method oxidation stone Black alkene is as friction improver.
Oil property is tested
In tests below, sample 1～5 is to refer to 5 kinds of lubricating oil sample that embodiment 2 and embodiment 3 obtain successively respectively, in addition will The lubricating oil of reference examples 1 is as control sample.
As can be seen from the above table, the lubricating oil that the present invention provides has preferable wearability and dispersibility, sample 1～4 For control sample, after having carried out fatty amino modified to graphene oxide, wearability is made to be improved； In addition, sample 5 is for sample 4, during long-chain fat amine modified graphene oxide, add kh570 can have Effect the cleaning dispersibility in oil field is made to be improved, deposit significantly reduces.
Every trade is entered using the lubricating oil (the modified graphene oxide of octadecylamine is as additive) obtaining in embodiment 1 Car is tested.
1st, road performance test [extending the oil draining period]
It is used as the just charge of oil that dispatches from the factory by the engine lubricating oil of a collection of new car actual interpolation present invention to certain automaker, so Afterwards after same test conditions downward driving, machine oil is detected, the contrast standard of changing oil decides whether to reach the oil draining period.Following table Result shows that being added with the automobile of lubricating oil of the present invention can also continue to use in 50,000 kilometers of actual driving rear engine oil, Also do not arrive the standard of changing oil, the automobile without adding the present invention can not be further continued for using in 5000 kilometers of rear engine oil of traveling, Must change oil, indicate the oil draining period that inventive engine lubricating oil substantially prolongs automobile.
Present invention driving oil draining period test data
2nd, road performance test [fuel economy]
By to a collection of new car different commercially available cj-4 level usual diesel fuel machine oil of interpolation of certain automaker and starting of the present invention Machine oil, then carries out the driving fuel economy test under 500-5000 kilometer the same terms respectively.The data display of following table, adds Automobile added with the engine lubricating oil of the present invention can save fuel 7-10% in the different tests stage.
The driving fuel economy test data of lubricating oil of the present invention
It is believed that the engine lubricating oil of the present invention can greatly prolong the engine oil change phase after above-mentioned analysis of experiments, save combustion Material, reduces discharge, and environmental pollution is little, has wide market value and development prospect.

Claims (10)

1. a kind of modified graphene oxide is it is characterised in that be using graphene oxide as raw material, then by surface long-chain fat Obtain after fat race amine and/or silane coupler modification.
2. modified graphene oxide according to claim 1 is it is characterised in that graphene oxide refers to adopt hummers Method prepares.
3. the preparation method of the modified graphene oxide described in claim 1 is it is characterised in that comprise the steps: long-chain Fatty amine is dissolved in ethanol, after mix homogeneously, is poured into containing in graphene oxide (go) aqueous solution, reacting by heating, afterwards Naturally cool to room temperature, reaction solidss are leached, uses washing with alcohol solidss, filtration cakes torrefaction, finally obtain the oxidation of modification Graphene.
4. the preparation method of modified graphene oxide according to claim 3 is it is characterised in that described long-chain fat amine Selected from c12～c18 alkylamine；Preferably lauryl amine, tetradecylamine, hexadecylamine or octadecylamine.
5. the preparation method of modified graphene oxide according to claim 3 is it is characterised in that will be molten for long-chain fat amine When in ethanol, wherein can also add silane coupler；Described silane coupler is selected from kh-550, kh-560 or kh- 570.
6. the application in lubricating oil as friction improver of the modified graphene oxide described in claim 1.
7. a kind of engine lubricating oil, includes following component by weight percentage:
A) friction improver 1.0～2.2%
B) metal detergent 0.5～1.1%
C) metal corrosion inhibitor 0.2～1.2%
D) antioxidant 2.0～2.5%
E) defoamer 0.05～0.1%
F) dispersant 1～1.2%
G) viscosity index improver 8～10%
H) synthesizing ester base oil 8～10%
I) base oil surplus；
It is characterized in that, include the modified graphene oxide described in claim 1 in described friction improver.
8. engine lubricating oil according to claim 7 is it is characterised in that described friction improver also can also comprise There are one or more of molybdenum dialkyldithiocarbamacompositions, nano boric acid salt or nano boric acid；More preferably dialkyl group Molybdenum dithiocarbamate, nano boric acid salt, nano boric acid, modified graphene oxide compound than 11:6:2:1 according to weight and Become；Described metal detergent is alkyl benzene calcium sulfonate between 500～600mgkoh/g for the base number；Described alkyl benzene sulphonate Calcium is the sulfonic acid calcium salt that carbon number is straight or branched alkyl between c10～c20；Metal corrosion inhibitor is dialkyl disulfides Mixture for one of zinc phosphate or dialkyl dithio amidocarbonic acid zinc or two kinds.
9. engine lubricating oil according to claim 7 it is characterised in that antioxidant be phenolic ester kind antioxidant, amine resist Oxygen agent, dialkyl dithio amino formate aid anti-oxidants compound and form；Defoamer is preferably acrylic ester type non-silicon defoaming agent； Dispersant is preferably the mixing of one of mono butonediimide or Ramulus Uncariae Cum Uncis imidodicarbonic diamide or two kinds.
10. engine lubricating oil according to claim 7 is it is characterised in that viscosity index improver is selected from polyethylene third The mixing of one or more of alkene copolymer, polymethacrylates or polyisobutylene；Synthesizing ester base oil is preferably Pentaerythritol ester, viscosity grade is 100 °, and viscosity is in 8～10mm2/s；Hydrogenated base oil be selected from two class hydrogenated base oil 500sn, One of two class hydrogenated base oil 500n, three class hydrogenated base oil 500sn or three class hydrogenated base oil 500n or several Mixing.
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