CN106244289A - Dispersibility and the good modified graphene lubricating oil of affinity and preparation method thereof - Google Patents

Dispersibility and the good modified graphene lubricating oil of affinity and preparation method thereof Download PDF

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CN106244289A
CN106244289A CN201610533724.1A CN201610533724A CN106244289A CN 106244289 A CN106244289 A CN 106244289A CN 201610533724 A CN201610533724 A CN 201610533724A CN 106244289 A CN106244289 A CN 106244289A
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lubricating oil
modified graphene
graphene
affinity
oil
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罗廷军
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CHONGQING DELING TECHNOLOGY Co Ltd
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CHONGQING DELING TECHNOLOGY Co Ltd
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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
    • C10M141/00Lubricating 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
    • C10M141/12Lubricating 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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    • 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
    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/02Carbon; Graphite
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    • 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
    • C10M139/00Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing atoms of elements not provided for in groups C10M127/00 - C10M137/00
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    • 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
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    • 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
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    • 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
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    • 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
    • C10M2201/14Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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    • 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
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    • 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/283Esters of polyhydroxy compounds
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    • 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/40Fatty vegetable or animal oils
    • C10M2207/401Fatty vegetable or animal oils used as base material
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    • 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
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
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    • 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
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
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    • 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
    • C10M2227/00Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/06Organic compounds derived from inorganic acids or metal salts
    • C10M2227/065Organic compounds derived from inorganic acids or metal salts derived from Ti or Zr
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    • 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
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • 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
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2060/00Chemical after-treatment of the constituents of the lubricating composition
    • C10N2060/09Treatment with nitrogen containing compounds
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10N2060/00Chemical after-treatment of the constituents of the lubricating composition
    • C10N2060/10Chemical after-treatment of the constituents of the lubricating composition by sulfur or a compound containing sulfur

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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)
  • Inorganic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The invention discloses dispersibility and the good modified graphene lubricating oil of affinity and preparation method thereof, described lubricating oil includes modified graphene, base oil, affinity agent, dispersant, the addition of described modified graphene is equivalent to the 3~15wt ‰ of base oil, the addition of described affinity agent is equivalent to the 0.1~2wt% of base oil, the addition of described dispersant is equivalent to the 0.5~1.0wt% of base oil, preferably, described lubricating oil also includes Stearate Modified TiO2Nanoparticle, the addition of described nanoparticle accounts for the 2~5wt% of base oil.The invention also discloses and use the mode of microwave to prepare lubricating oil.There is between its each component of modified graphene lubricating oil of the polymolecularity that the present invention provides dispersibility and the stability of excellence, which solve Graphene as additive long term stability problem in base oil.

Description

Dispersibility and the good modified graphene lubricating oil of affinity and preparation method thereof
Technical field
The invention belongs to lubricating oil field, be specifically related to a kind of dispersibility and the good modified graphene lubricating oil of affinity and Its preparation method.
Background technology
For component of machine, fretting wear is inevitable, and this not only brings a large amount of losses of material and the energy, also Cause the pollution of environment.Lubricating oil is effectively to slow down component of machine fretting wear, the important technical of reduction energy loss One of.Lubricating oil is modern industry and national defense industry operating blood, and it is made up of base oil and additive, modern industry at full speed Demand for development accelerates the upgrading of lubricating oil.Typically have following three kinds of modes can promote oil quality: 1) improve base oil Quality, 2) improve additive performance, 3) improve additive compounded technology.Profit contaminated product additive is various senior lubricants Marrow, and the core that the compounded technology of lube oil additive is lubricants performance to be achieved and key technology.
Graphene, because of its excellent greasy property, is prepared lubricating oil as additive and is more and more closed by Graphene Note, Graphene is as lube oil additive, to demonstrate good greasy property in friction process, do not require nothing more than form and The number of plies is wanted suitably and it is necessary to can be dispersed stably in lubricating oil.Once occurring to be separated, Graphene is easy for because of reunion It is difficult to play its greasy property.It would therefore be highly desirable to solve the Graphene dispersion problem as lube oil additive, thus obtain one Plant the Graphene lubricating oil that stability, anti-attrition and mechanical protection performance are good.
Summary of the invention
In view of this, an object of the present invention is to provide dispersibility and the good modified graphene lubricating oil of affinity, The two of the purpose of the present invention are to provide dispersibility and the preparation method of the good modified graphene lubricating oil of affinity.
For achieving the above object, the present invention provides following technical scheme:
1, dispersibility and the good modified graphene lubricating oil of affinity, described lubricating oil include modified graphene, base oil, Affinity agent, dispersant, the addition of described modified graphene is equivalent to the 3~15wt ‰ of base oil, the interpolation of described affinity agent Amount is equivalent to the 0.1~2wt% of base oil, and the addition of described dispersant is equivalent to the 0.5~1.0wt% of base oil.
Preferably, described modified graphene is the lipophilic graphene using covalent bond to modify.
Preferably, described modified graphene preparation method comprises the steps:
(1) Graphene is joined the H of 1~2mol/L2SO4In, at 80~100 DEG C, stirring reaction 6~10h, then enters one Step washing, vacuum lyophilization, prepare functionalization graphene;
(2) by Polyethylene Glycol, dodecylbenzene sodium sulfonate, polyene-based succimide, polyether-ether-ketone, polyvinylpyrrolidine Ketone, polythiophene, polyamide, poly-aspartic-acid, polyacetylene, during in polybutadiene, politef, at least one is with step (1) Described functionalization graphene with mass ratio be 2~3:2~5 in methanol be blended, mixed solution is at 80~100 DEG C of fierce ultrasound wave Shake 48~after 72h hour, with 250~300r/min stirring mixed solutions 4~8h under nitrogen protection, finally filter.
Preferably, described affinity agent is titanate ester.
Preferably, one or more during described base oil is mineral base oil, synthetic base oil and plant base oil.
Preferably, during described dispersant is stearic acid, dodecylbenzene sodium sulfonate, fatty glyceride, quaternary ammonium compound One or more.
Preferably, described lubricating oil also includes Stearate Modified TiO2Nanoparticle, the addition of described nanoparticle Account for the 2~5wt% of base oil.
2, described dispersibility and the preparation method of the good modified graphene lubricating oil of affinity, comprises the following steps:
(1) modified graphene, dispersant, affinity agent substep are added in base oil, stir, obtain mixed solution;
(2) step 1 gained mixed solution is stirred 20~30min under conditions of microwave irradiation.
Preferably, described microwave intensity is 500~700w.
Preferably, step (1) also includes adding Stearate Modified TiO2Nanoparticle.
The beneficial effects of the present invention is:
1) between the present invention provides dispersibility and the good each component of modified graphene lubricating oil of affinity, there is excellence Dispersibility and stability, which solve Graphene as additive long term stability problem in base oil, and lubricating oil In also added affinity agent, affinity agent one end and metal adsorption, the other end makes lubricating oil at mechanical part table with Graphene absorption Face forms one layer of ultra-thin Graphene oil film, and movable machinery surface is under the protection of Graphene oil film, and rubbing surface does not produce directly Friction, thus moving mechanical part is played a protective role, the service life of prolonged mechanical parts;Lubrication the most of the present invention Using less dispersant in oil, because dispersant is too much easily caused emulsifying, the present invention uses the less dispersant can also Realize the dispersed of Graphene;
2) present invention uses the mode of microwave irradiation to prepare dispersibility and the good modified graphene lubricating oil of affinity, in fact Show Graphene by the interior peptizaiton put in place, dispersed in base oil of Graphene additive has been had promotion property and makees With;
3) lubricating oil disclosed by the invention also added Stearate Modified TiO2Nanoparticle as another kind of additive, Research finds that itself and modified graphene have extraordinary synergism, because the TiO that organic group is modified2Nanoparticle has Excellent antiwear and antifriction ability, because of TiO2Nanoparticle and the small-size effect of modified graphene particle, skin effect cause firmly TiO modified by fat acid2Nanoparticle fusing point declines, sintering temperature declines.During friction temperature, surface local temperature is high, TiO2 Nanoparticle is in fusing, semi-molten or sintering state, forms one layer of nano ceramic film, and its toughness, bending strength are the biggest Big beyond general thin film, and nanoparticle has high diffusivity ability and self-diffusion ability, therefore nano-TiO2Particle pole can Can diffuse and penetrate in metallic matrix in friction process, and it is possible to generate Fe with metallic matrix2(TiO3)3, TiC etc. solid Solution, thus show the antiwear and friction reduction property of excellence, and because considerably less its of addition will not cause gold in lubricating oil Belong to the change of matrix macroscopic view, and now Graphene can preferably embody its greasy property on thin film.
4) the dispersion technology preparation that the present invention uses physics and chemical method to share has the modified graphene of polymolecularity Lubricating oil, can realize dispersed about 3~the modified graphene of 15wt ‰ in lubricating oil, this is not in general lubricating oil Can realize.
Accompanying drawing explanation
In order to make the purpose of the present invention, technical scheme and beneficial effect clearer, the present invention provides drawings described below:
Fig. 1 represents temperature comparisons's oscillogram;
Fig. 2 represents that coefficient of friction contrasts oscillogram;
Fig. 3 represents frictional resistance oscillogram;
Fig. 4 represents lubricating oil volatilization oscillogram.
Detailed description of the invention
Below the preferred embodiments of the present invention are described in detail.The experiment side of unreceipted actual conditions in embodiment Method, generally according to normal condition or according to the condition proposed by manufacturer.
Below the preferred embodiments of the present invention are described in detail.The experiment side of unreceipted actual conditions in embodiment Method, generally according to normal condition or according to the condition proposed by manufacturer.
Embodiment 1
The modified graphene lubricating oil of polymolecularity, described lubricating oil includes modified graphene, base oil, affinity agent, divides Powder, the addition of described modified graphene is equivalent to the 3wt ‰ of base oil, and the addition of described dispersant is equivalent to base oil 0.8wt%, the addition of described affinity agent is equivalent to the 2wt% of base oil.
Described modified graphene preparation method comprises the steps:
(1) Graphene is joined the H of 1mol/L2SO4In, at 80~100 DEG C, stirring reaction 6h, washs the most further, Vacuum lyophilization, prepares functionalization graphene;
(2) by functionalization graphene described in dodecylbenzene sodium sulfonate and step (1) with mass ratio for 1:1 in methanol Being blended, mixed solution is after 80~100 DEG C of fierce ultrasonic wave concussion 50h hour, with 250~300r/min stirrings under nitrogen protection Mixed solution 4~8h, finally filters.
Described base oil is mineral base oil, and described dispersant is dodecylbenzene sodium sulfonate, and described affinity agent is metatitanic acid Ester.
The preparation method of the modified graphene lubricating oil of polymolecularity, comprises the steps:
(1) modified graphene, dispersant, affinity agent substep are added in base oil, stir, obtain mixed solution;
(2) solution described in step 1 is stirred under conditions of microwave irradiation 30min.
Embodiment 2
The modified graphene lubricating oil of polymolecularity, described lubricating oil includes modified graphene, base oil, affinity agent, divides Powder, the addition of described modified graphene is equivalent to the 5wt ‰ of base oil, and the addition of described dispersant is equivalent to base oil 0.6wt%, the addition of described affinity agent is equivalent to the 1.5wt% of base oil.
Described modified graphene preparation method comprises the steps:
(1) Graphene is joined the H of 2mol/L2SO4In, at 80~100 DEG C, stirring reaction 8h, washs the most further, Vacuum lyophilization, prepares functionalization graphene;
(2) by functionalization graphene described in polyene-based succimide and step (1) with mass ratio for 2:3 in methanol Being blended, mixed solution is after 80~100 DEG C of fierce ultrasonic wave concussion 60 hours, with 250~300r/min stirrings under nitrogen protection Mixed solution 6h, finally filters.
Described base oil is plant base oil, and described dispersant is fatty glyceride, and described affinity agent is titanate esters.
The preparation method of the modified graphene lubricating oil of polymolecularity, comprises the steps:
(1) modified graphene, dispersant, affinity agent substep are added in base oil, stir, obtain mixed solution;
(2) solution described in step 1 is stirred under conditions of microwave irradiation 20min.
Embodiment 3
The modified graphene lubricating oil of polymolecularity, described lubricating oil includes modified graphene, base oil, affinity agent, divides Powder, the addition of described modified graphene is equivalent to the 8wt ‰ of base oil, and the addition of described dispersant is equivalent to base oil 0.7wt%, the addition of described affinity agent is equivalent to the 0.8wt% of base oil.
Described modified graphene preparation method comprises the steps:
(1) Graphene is joined the H of 1.5mol/L2SO4In, at 80~100 DEG C, stirring reaction 8h, washes the most further Wash, vacuum lyophilization, prepare functionalization graphene;
(2) polyvinylpyrrolidone is total in methanol for 1:1 with mass ratio with functionalization graphene described in step (1) Mixed, mixed solution is after 80~100 DEG C of fierce ultrasonic wave concussion 50 hours, mixed with 250~300r/min stirrings under nitrogen protection Close solution 4~8h, finally filter.
Described base oil is synthetic base oil, and described dispersant is quaternary ammonium compound, and described affinity agent is titanate esters.
The preparation method of the modified graphene lubricating oil of polymolecularity, comprises the steps:
(1) modified graphene, dispersant, affinity agent substep are added in base oil, stir, obtain mixed solution;
(2) solution described in step 1 is stirred under conditions of microwave irradiation 30min.
Embodiment 4
The modified graphene lubricating oil of polymolecularity, described lubricating oil includes modified graphene, base oil, affinity agent, divides Powder, Stearate Modified TiO2Nanoparticle, the addition of described modified graphene is equivalent to the 10wt ‰ of base oil, described point The addition of powder is equivalent to the 0.5wt% of base oil, and the addition of described nanoparticle accounts for the 2wt% of base oil, described parent The addition of mediating recipe is equivalent to the 0.5wt% of base oil.
Described modified graphene preparation method comprises the steps:
(1) Graphene is joined the H of 1.5mol/L2SO4In, at 80~100 DEG C, stirring reaction 8h, washes the most further Wash, vacuum lyophilization, prepare functionalization graphene;
(2) poly-aspartic-acid is total in methanol for 1:1 with mass ratio with functionalization graphene described in step (1) Mixed, mixed solution is after 80~100 DEG C of fierce ultrasonic wave concussion 50 hours, mixed with 250~300r/min stirrings under nitrogen protection Close solution 4~8h, finally filter.
Described base oil is mineral base oil, and described dispersant is dodecylbenzene sodium sulfonate, and described affinity agent is metatitanic acid Ester.
The preparation method of the modified graphene lubricating oil of polymolecularity, comprises the steps:
(1) modified graphene, dispersant, affinity agent substep are added in base oil, stir, obtain mixed solution;
(2) solution described in step 1 is stirred under conditions of microwave irradiation 30min.
Embodiment 5
The modified graphene lubricating oil of polymolecularity, described lubricating oil includes modified graphene, base oil, affinity agent, divides Powder, Stearate Modified TiO2Nanoparticle, the addition of described modified graphene is equivalent to the 15wt ‰ of base oil, described point The addition of powder is equivalent to the 2.5wt% of base oil, and the addition of described nanoparticle accounts for the 4wt% of base oil, described parent The addition of mediating recipe is equivalent to the 1.1wt% of base oil.
Described modified graphene preparation method comprises the steps:
(1) Graphene is joined the H of 1.5mol/L2SO4In, at 80~100 DEG C, stirring reaction 8h, washes the most further Wash, vacuum lyophilization, prepare functionalization graphene;
(2) poly-aspartic-acid is total in methanol for 1:1 with mass ratio with functionalization graphene described in step (1) Mixed, mixed solution is after 80~100 DEG C of fierce ultrasonic wave concussion 50 hours, mixed with 250~300r/min stirrings under nitrogen protection Close solution 4~8h, finally filter.
Described base oil is synthetic base oil, and described dispersant is quaternary ammonium compound, and described affinity agent is titanate esters.
The preparation method of the modified graphene lubricating oil of polymolecularity, comprises the steps:
(1) modified graphene, dispersant, affinity agent substep are added in base oil, stir, obtain mixed solution;
(2) solution described in step 1 is stirred under conditions of microwave irradiation 30min.
Comparative example 1
According to the method for embodiment 1, difference is to use conventional Graphene, then according to identical method makes graphite Alkene lubricating oil.
Comparative example 2
According to the method for embodiment 1, difference is in preparation process the mode not using microwave to stir, and uses mechanical agitation Replace.By embodiment 1~5 and the performance of Graphene lubricating oil for preparing of comparative example 1~2 compare.
By embodiment 1~5 and the performance of the Graphene lubricating oil for preparing of comparative example 1~2 and conventional lubrication oil enter Row compares.
Fig. 1 represents embodiment 1~5 and the Graphene lubricating oil of comparative example 1~2 preparation and the temperature of conventional lubrication oil Degree contrast oscillogram, temperature comparisons's oscillogram is to embody the temperature of each time phase.During detection, coefficient of friction is the biggest, The temperature produced is the highest;Coefficient of friction is the least, and the temperature of generation is the lowest.Conventional lubrication oil just reaches the high temperature of 150 degree for 13 minutes, And modified graphene lubricating oil is oily well below conventional lubrication compared to its temperature produced of conventional lubrication oil, and embodiment 1 ~5 is relatively low compared to its temperature produced of comparative example 1~2, Graphene that this explanation is conventional and preparation method for The performance of lubricating oil also has an impact.
Fig. 2 represents embodiment 1~5 and the rubbing of the Graphene lubricating oil of comparative example 1~2 preparation and conventional lubrication oil Wiping index contrast oscillogram, coefficient of friction contrast oscillogram is to embody the coefficient of friction of each time phase.As can be seen from Figure 2, Under room temperature and high temperature oil, the coefficient of friction of conventional lubrication oil is far above modified graphene lubricating oil, and embodiment 1~5 phase Less compared with its coefficient of friction of comparative example 1~2.
Fig. 3 represents embodiment 1~5 and the rubbing of the Graphene lubricating oil of comparative example 1~2 preparation and conventional lubrication oil Wiping resistance oscillogram, frictional resistance oscillogram is to embody the resistance coefficients of each time phase intuitively.The profit of lubricating oil Slip its resistance the best is the least, and HP, hp/litre will be the strongest;Otherwise resistance is the biggest, power per liter will reduce, and power will Reducing, oil consumption will increase, from figure 3, it can be seen that modified graphene lubricating oil mechanical movement drag minimization, its energy saving advantage is bright Aobvious.
Fig. 4 represents and executes example 1~5 and the Graphene lubricating oil of comparative example 1~2 preparation and the lubrication of conventional lubrication oil Oil volatilization oscillogram, lubricating oil volatilization oscillogram is to embody the lubricating oil volatilization value of each time phase intuitively.Can be seen by Fig. 4 Going out, the volatilization value of conventional lubrication oil is far above modified graphene lubricating oil.The volatilization value of lubricating oil is the highest, and engine interior produces Greasy filth carbon distribution will be the most, the consumption of lubricating oil will be the most.
By the above results it can also be seen that the greasy property of modified graphene lubricating oil for preparing of the embodiment of the present invention 1~5 The Graphene lubricating oil prepared far above comparative example 1 and 2, and coefficient of friction is lower, and mechanical resistance is little, and its energy saving is excellent Gesture is obvious.
By embodiment 1~5 and the Graphene lubricating oil for preparing of comparative example 1 and 2 use at mechanical surface and to find this The modified graphene lubricating oil that bright embodiment 1~5 prepares has fine stability, shows and stable under high/low temperature, and The phenomenons such as oxidation, emulsifying, rotten, volatilization will not be had to occur, performance colloid will not be shown at machinery, greasy filth, carbon distribution etc., and Can service life of prolonged mechanical parts.And there is modified graphene lubricating oil prepared by embodiment 4~5 compared to embodiment 1~3 its greasy properties are more preferable.This further illustrates modified graphene and Stearate Modified TiO in lubricating oil2Nanoparticle is worked in coordination with Act on and have the effect of promotion property for greasy property.
Embodiment 1 illustrates microwave irradiation with the performance detection data of the Graphene lubricating oil prepared by comparative example 2 Mode has the effect of promotion property to dispersed in base oil of Graphene additive.
Further the lubricating oil prepared by embodiment 1~5 and comparative example 1~2 is entered from pour point, flash-point, current potential Row detection (parallel three groups of experiments), obtains testing result as shown in table 1:
Table 1 each lubricants performance detection data
As seen from Table 1, modified graphene, dispersant, affinity agent is used to prepare by technical scheme disclosed by the invention The pour point of Graphene lower than traditional commerce lubricating oil, and can find that embodiment 4 and 5 is by adding Stearate Modified TiO2 Nanoparticle can realize the less pour point of lubricating oil, although the Graphene lubricating oil pour point ratio of comparative example 1~2 preparation passes System commercial lube oil is little, but its effect is not as good as embodiment 1~5.From the point of view of flash-point, the lubricating oil ratio of embodiment 1~5 preparation passes The flash-point of system commercial lube oil exceeds about 20 DEG C, and the lubricating oil of embodiment 1~5 preparation is prepared than comparative example 1~2 Lubricating oil flash point the highest.From the point of view of Zeta potential, the lubricating oil Zeta potential of embodiment 1~5 preparation has basically reached 100mv Above, its dispersion stabilization of lubricating oil of this explanation embodiment 1~5 preparation is fabulous, and embodiment 4~5 is hard by adding TiO modified by fat acid2Nanoparticle its also promote Zeta potential increase, and the Zeta potential of traditional commerce lubricating oil be just 20 left sides The right side, although comparative example 1~2 preparation lubricating oil stability better than conventional lubrication oil, but compared to embodiment 1~5 its Poor stability.
Finally illustrate, preferred embodiment above only in order to technical scheme to be described and unrestricted, although logical Cross above preferred embodiment the present invention to be described in detail, it is to be understood by those skilled in the art that can be In form and it is made various change, without departing from claims of the present invention limited range in details.

Claims (10)

1. dispersibility and the good modified graphene lubricating oil of affinity, it is characterised in that: described lubricating oil include modified graphene, Base oil, affinity agent, dispersant, the addition of described modified graphene is equivalent to the 3~15wt ‰ of base oil, described affinity agent Addition be equivalent to the 0.1~2wt% of base oil, the addition of described dispersant be equivalent to base oil 0.5~ 1.0wt%.
Dispersibility and the good modified graphene lubricating oil of affinity the most according to claim 1, it is characterised in that described modification Graphene is the lipophilic graphene using covalent bond to modify.
Dispersibility and the good modified graphene lubricating oil of affinity the most according to claim 1, it is characterised in that described modification Graphene preparation method comprises the steps:
(1) Graphene is joined the H of 1~2mol/L2SO4In, at 80~100 DEG C, stirring reaction 6~10h, washes the most further Wash, vacuum lyophilization, prepare functionalization graphene;
(2) by Polyethylene Glycol, dodecylbenzene sodium sulfonate, polyene-based succimide, polyether-ether-ketone, polyvinylpyrrolidone, Polythiophene, polyamide, poly-aspartic-acid, polyacetylene, institute during at least one is with step (1) in polybutadiene, politef State functionalization graphene with mass ratio be 2~3:2~5 in methanol be blended, mixed solution shakes at 80~100 DEG C of fierce ultrasound wave Swing 48~after 72h hour, with 250~300r/min stirring mixed solutions 4~8h under nitrogen protection, finally filter.
Dispersibility and the good modified graphene lubricating oil of affinity the most according to claim 1, it is characterised in that described affine Agent is titanate ester.
Dispersibility and the good modified graphene lubricating oil of affinity the most according to claim 1, it is characterised in that described basis Oil is one or more in mineral base oil, synthetic base oil and plant base oil.
Dispersibility and the good modified graphene lubricating oil of affinity the most according to claim 1, it is characterised in that described dispersion Agent is one or more in stearic acid, dodecylbenzene sodium sulfonate, fatty glyceride, quaternary ammonium compound.
Dispersibility and the good modified graphene lubricating oil of affinity the most according to claim 1, it is characterised in that described lubrication Oil also includes Stearate Modified TiO2Nanoparticle, the addition of described nanoparticle accounts for the 2~5wt% of base oil.
8. dispersibility described in any one of claim 1~7 and the preparation method of the good modified graphene lubricating oil of affinity, it is special Levy and be, comprise the following steps:
(1) modified graphene, dispersant, affinity agent substep are added in base oil, stir, obtain mixed solution;
(2) step 1 gained mixed solution is stirred 20~30min under conditions of microwave irradiation.
The preparation method of the modified graphene lubricating oil of polymolecularity the most according to claim 8, it is characterised in that described micro- Intensity of wave is 500~700w.
The preparation method of the modified graphene lubricating oil of polymolecularity the most according to claim 8, it is characterised in that step (1) also include adding Stearate Modified TiO2Nanoparticle.
CN201610533724.1A 2016-07-07 2016-07-07 Dispersibility and the good modified graphene lubricating oil of affinity and preparation method thereof Pending CN106244289A (en)

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CN106995740A (en) * 2017-05-02 2017-08-01 长乐净能新材料科技有限公司 A kind of lubricating oil preparation method material modified containing nano-graphene
CN107338086A (en) * 2017-08-03 2017-11-10 重庆华阳石墨烯科技有限公司 Lube oil additive of graphene doped and compounded dispersant and preparation method thereof
CN110437910A (en) * 2018-05-02 2019-11-12 新奥科技发展有限公司 Graphene lubricating oil and preparation method thereof
CN108822932A (en) * 2018-05-21 2018-11-16 上海利物盛企业集团有限公司 A kind of high speed extreme-pressure wear-resistant lubricating oil and its preparation method and application
CN108822932B (en) * 2018-05-21 2021-07-23 上海利物盛企业集团有限公司 High-speed extreme pressure wear-resistant lubricating oil and preparation method and application thereof
CN108559577A (en) * 2018-05-31 2018-09-21 烟台华恒节能科技有限公司 A kind of preparation method of diisocyanate modified graphene antiwear and energy-saving lubricant oil
CN108559577B (en) * 2018-05-31 2021-03-02 烟台华恒节能科技有限公司 Preparation method of diisocyanate modified graphene anti-wear energy-saving lubricating oil
CN110317665A (en) * 2019-06-10 2019-10-11 安徽华驰能源科技有限公司 A kind of graphene engine anti-wear renovation agent and preparation method thereof
CN110484338A (en) * 2019-09-19 2019-11-22 广东车三宝汽车科技有限公司 A kind of graphene machine oil that comprehensive performance is high and its preparation process
CN110484338B (en) * 2019-09-19 2021-10-08 广东车三宝汽车科技有限公司 Graphene engine oil with high comprehensive performance and preparation process thereof
CN111040844A (en) * 2019-11-15 2020-04-21 山东硕力新材料科技有限公司 Lipophilic nano material modified self-repairing engine oil
CN111676085A (en) * 2020-06-30 2020-09-18 佛山市南海区里水镇经济促进局 Graphene lubricating oil for robot and preparation method and application thereof

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