CN106221858B - A kind of polymolecularity and the modified graphene lubricating oil of high-affinity and preparation method thereof - Google Patents
A kind of polymolecularity and the modified graphene lubricating oil of high-affinity and preparation method thereof Download PDFInfo
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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- 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
- C10M141/02—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 oxygen-containing compound
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- C10M141/08—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 sulfur-, selenium- or tellurium-containing compound
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- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
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- 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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- 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
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
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Abstract
The invention discloses a kind of polymolecularities and the modified graphene lubricating oil of high-affinity and preparation method thereof, its modified graphene lubricating oil includes 0.3-1.5 parts of valence electron modified graphene, 0.05~0.5 part of dispersing agent, 0.05~1 part of affinity agent and 100 parts of base oil by weight, and described to remove valence electron modified graphene be one of fluorinated graphene, nitridation graphene, vulcanization graphene, boronized graphite alkene, phosphatization graphene, silicated graphite alkene.Preparation method is simple, is suitable for industrialized production, can effectively solve the problem of graphene is reunited, is conducive to dispersion of the graphene in lubricating oil.Lubricity with super strength and anti-attrition, are able to extend the service life of mechanical part after manufactured lubricating oil, now save fuel oil, reduce discharge, more environmentally-friendly.
Description
Technical field
The invention belongs to macromolecule and its application fields, are related to the modified graphene profit of a kind of polymolecularity and high-affinity
Lubricating oil further relates to the preparation method of the graphene lubricating oil.
Background technique
In recent years, the excellent frictional behaviour of graphene has caused people and has more and more paid close attention to, lamella sliding, friction
Abrasion mechanism and friction field application have many researchs and report.With the development of science and technology, especially in recent years
The promotion of graphene technology, graphene additive technology have been introduced into lubricating oil field.Application of the graphene as antiwear additive,
Low viscosity machine oil can be made more universal, to help automobile more energy-saving and environmental protection.However, graphene chemical stability is high, with
Other medium interactions are weaker, and interlayer has very big Van der Waals force, although lubricating oil can be improved to a certain degree
Greasy property, but lubrication oil-proofness made from improving is poor, will form aggregate after being long placed in drops the greasy property of lubricating oil
It is low, it is had caused great difficulties to the further application of graphene, it would therefore be highly desirable to which solving the problems, such as is how to realize that graphene is equal
It is even to be dispersed stably in oil product, to obtain a kind of stability, anti-attrition and the good graphene lubricating oil of mechanical protection performance.
Summary of the invention
In view of this, the purpose of the present invention is to provide the modified graphene lubricating oil of a kind of polymolecularity and high-affinity
And provide the preparation method of the graphene lubricating oil.
In order to achieve the above objectives, the invention provides the following technical scheme:
1, the modified graphene lubricating oil of a kind of polymolecularity and high-affinity includes following component: going by weight
0.3~1.5 part of valence electron modified graphene, 0.05~0.5 part of dispersing agent, 0.05~1 part of affinity agent and 100 parts of base oil.
Further, described that valence electron modified graphene is gone to be fluorinated graphene, nitridation graphene, vulcanize graphene, boronation
One of graphene, phosphatization graphene, silicated graphite alkene.
Further, the dispersing agent is in stearic acid, neopelex, fatty glyceride and quaternary ammonium compound
One or more, the affinity agent is the inorganic polymer and unsaturated organic acid and trivalent chromium of the low molecular weight containing zirconium aluminate
One of the metal chromium complex that ion is formed.
Preferably, go valence electron modified graphene that Bi is added to described2O3Or Sb2O3It is doped.
It is furthermore preferred that the Bi2O3Or Sb2O30.03-0.15 parts of additive amount.
Further, the base oil is one of mineral base oil, synthetic base oil and plant oil base oil or a variety of.
2, the preparation method of the modified graphene lubricating oil of a kind of polymolecularity and high-affinity, includes the following steps:
(1) valence electron modified graphene, dispersing agent, pour-point depressant will be gone to be added in base oil step by step according to the ratio, ultrasonic vibration,
Obtain mixture；
(2) affinity agent is added in mixture obtained by step (1) according to the ratio, carries out microwave treatment, obtains polymolecularity
With the lubricating oil of the modified graphene lubricating oil of high-affinity.
Further, by Bi before step (1)2O3Or Sb2O3Addition goes valence electron modified graphene to be doped.
Further, supersonic frequency described in step (1) is 20kHz~1MHz, and power is 30W~15kW, stirs at least 1h；
Microwave treatment temperature 50 C~95 DEG C described in step (2), the specific volume power of microwave radiation are 200W/L~6000W/L,
Handle time 1h~4h.
The beneficial effects of the present invention are: the invention discloses a kind of modified graphene of polymolecularity and high-affinity profits
Lubricating oil removes valence electron modified graphene by being added in base oil, due to going the graphene after valence electron to reduce graphene
The intermolecular force of interlayer reduces the stacking of lamella, changes the characteristic that graphene attracts each other, efficiently solves graphite
The problem of alkene is reunited, be conducive to dispersion of the graphene in lubricating oil, therefore there is good stability after lubricating oil is made.
Since graphene dispersion problem is resolved, lubricating oil obtained gets a promotion in greasy property, abrasion resistance
Excellent, simultaneously because also added amphipathic affinity agent, one end and metal adsorption, the other end and graphene are adsorbed, and are transported in machinery
Lubricating oil quickly can form one layer in graphene oil film in mechanical surface in dynamic, direct friction not generated, thus to movable machinery
Component plays a protective role, the service life of prolonged mechanical component, realizes and saves fuel oil, reduces discharge, more environmentally-friendly.
Use Bi2O3Or Sb2O3Metal oxide with high electron affinity carrys out doped graphene, and electronics is from graphene
Layer be transferred to metal oxide film, the interfacial charge transfer between graphene and metal oxide result in graphene not at
Formation to electronics, forms hole accumulation layer in graphene layer.The sucking action between ring graphene sheet layer is more broken, into
One step reduces the stacking of graphene film interlayer, and uses Bi2O3Or Sb2O3It is to protect to be doped with the graphite in excessive hole
Immature, the nondestructive means of graphene characteristic are held, metal oxide has fabulous thermostabilization in air and solution
Property and chemical stability, therefore include Bi2O3Or Sb2O3Graphene be suitable for the application in lubricating oil in harsh environment.
It is of the invention the invention also discloses the preparation method of polymolecularity and the modified graphene lubricating oil of high-affinity
Method first passes through the evenly dispersed of ultrasonic mechanism promotion graphene and auxiliary agent, then carries out microwave treatment again and reinforces lubrication
Interior atoms movement in oily each component, realizes the movement of internal dipole molecule high-frequency reciprocating, further increases modified graphene profit
The dispersion performance of lubricating oil, the preparation method is simple, is suitable for industrialized production.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
Fig. 1 is temperature comparisons' waveform diagram；
Fig. 2 is that coefficient of friction compares waveform diagram；
Fig. 3 is frictional resistance waveform diagram；
Fig. 4 is lubricating oil volatilization waveform diagram.
Specific embodiment
Below in conjunction with attached drawing, a preferred embodiment of the present invention will be described in detail.
Embodiment 1
A kind of modified graphene lubricating oil of polymolecularity and high-affinity includes following component by weight: fluorination
0.3 part of graphene, 0.05 part of stearic acid, 0.05 part of TL-1 aluminum-zirconium coupling agent and 100 parts of base oil.
A kind of preparation method for the modified graphene lubricating oil that dispersion performance is good, includes the following steps:
(1) fluorinated graphene and dispersing agent are added in base oil step by step according to the ratio, ultrasonic vibration obtains mixture.Ultrasound
Frequency is 1MHz, power 30W, stirs 1h.
(2) TL-1 aluminum-zirconium coupling agent is added in mixture obtained by step (1), carries out microwave treatment, obtains dispersibility
The lubricating oil of modified graphene lubricating oil that can be good.95 DEG C of microwave treatment temperature, the specific volume power of microwave radiation is 200W/
L handles time 4h.
Embodiment 2
A kind of modified graphene lubricating oil of polymolecularity and high-affinity includes following component by weight: nitridation
1 part of graphene, 0.3 part of fatty glyceride, 0.15 part of TL-2 aluminum-zirconium coupling agent and 100 parts of base oil.
A kind of preparation method for the modified graphene lubricating oil that dispersion performance is good, includes the following steps:
(1) first by 0.1 part of Sb2O3It is added in nitridation graphene and is doped.
(2) valence electron graphene and dispersing agent is gone to be added in base oil step by step according to the ratio by what step 1 obtained, ultrasound shake
It swings, obtains mixture.Supersonic frequency is 20kHz, power 15kW, stirs 1.2h.
(3) TL-2 aluminum-zirconium coupling agent is added in mixture obtained by step (2), carries out microwave treatment, obtains dispersibility
The lubricating oil of modified graphene lubricating oil that can be good.The specific volume power of microwave treatment temperature 50 C, microwave radiation is
6000W/L handles time 1h.
Embodiment 3
A kind of modified graphene lubricating oil of polymolecularity and high-affinity includes following component by weight: vulcanization
1.5 parts of graphene, 0.2 part of fatty glyceride, 0.2 part of polyacrylate, 0.5 part of TL-3 aluminum-zirconium coupling agent and base oil 100
Part.
A kind of preparation method for the modified graphene lubricating oil that dispersion performance is good, includes the following steps:
(1) first by 0.15 part of Bi2O3It is added in vulcanization graphene and is doped.
(2) valence electron graphene, dispersing agent is gone to be added in base oil step by step according to the ratio by what step 1 obtained, ultrasonic vibration,
Obtain mixture.Supersonic frequency is 20kHz, power 15kW, stirs 1.2h.
(3) TL-3 aluminum-zirconium coupling agent is added in mixture obtained by step (2), carries out microwave treatment, obtains dispersibility
The lubricating oil of modified graphene lubricating oil that can be good.The specific volume power of microwave treatment temperature 50 C, microwave radiation is
6000W/L handles time 1h.
Embodiment 4
A kind of modified graphene lubricating oil of polymolecularity and high-affinity includes following component: boronation by weight
1 part of graphene, 0.4 part of hard neopelex, 0.5 part of alkylnaphthalene, 0.3 part of methacrylic acid chromium complex and base
100 parts of plinth oil.
A kind of preparation method for the modified graphene lubricating oil that dispersion performance is good, includes the following steps:
(1) first by 0.1 part of Bi2O3It is added in boronized graphite alkene and is doped.
(2) valence electron graphene, dispersing agent is gone to be added in base oil step by step according to the ratio by what step 1 obtained, ultrasonic vibration,
Obtain mixture.Supersonic frequency is 20kHz, power 15kW, stirs 1.2h.
(3) methacrylic acid chromium complex is added in mixture obtained by step (2), carries out microwave treatment, obtains
The lubricating oil of the modified graphene lubricating oil good to dispersion performance.75 DEG C of microwave treatment temperature, the unit volume function of microwave radiation
Rate is 4500W/L, handles time 1h.
Embodiment 5
A kind of modified graphene lubricating oil of polymolecularity and high-affinity includes following component: phosphatization by weight
0.5 part of graphene, 0.1 part of stearic acid, 0.6 part of long chain alkylphenol, 0.1 part of methacrylic acid chromium complex and base oil
100 parts.
A kind of preparation method for the modified graphene lubricating oil that dispersion performance is good, includes the following steps:
(1) first by 0.05 part of Bi2O3It is added in phosphatization graphene and is doped.
(2) valence electron graphene, dispersing agent is gone to be added in base oil step by step according to the ratio by what step 1 obtained, ultrasonic vibration,
Obtain mixture.Supersonic frequency is 500kHz, power 5kW, stirs 1.5h.
(3) methacrylic acid chromium complex is added in mixture obtained by step (2), carries out microwave treatment, obtains
The lubricating oil of the modified graphene lubricating oil good to dispersion performance.90 DEG C of microwave treatment temperature, the unit volume function of microwave radiation
Rate is 3500W/L, handles time 1.1h.
The performance of Examples 1 to 5 and conventional graphite alkene lubricating oil (calling conventional lubrication oil in the following text) is compared.As a result as schemed
Shown in 1-4.
Interpretation of result: Fig. 1 temperature comparisons' figure is the temperature for embodying each time phase, and coefficient of friction is got in the detection process
Greatly, the temperature of generation is higher, and coefficient of friction is smaller, and the temperature of generation is lower, as seen from Figure 1, conventional lubrication oil 13 minutes
Just reach 150 degree of high temperature, and the modified graphene lubricating oil of the polymolecularity of embodiment 1-5 energy reached in 20 minutes most low energy
103 degree, up to 113.5 degree, it can be seen that, the greasy property of modified graphene lubricating oil is much higher than conventional lubrication oil.
It is to embody the coefficient of friction of each time phase, as shown in Figure 2, conventional lubrication that Fig. 2 coefficient of friction, which compares waveform diagram,
Polymolecularity of the coefficient of friction of oil much higher than embodiment 1-5 can modified graphene lubricating oil, regardless of engine cold-start and
In normal operation, the modified graphene lubricating oil of the polymolecularity energy of embodiment 1-5 is all much better than conventional lubrication oil, coefficient of friction
Bigger, the abrasion of engine is bigger, and service life is shorter, otherwise coefficient of friction is smaller, and service life is longer, it can be seen that, this
The frictional behaviour of the modified graphene lubricating oil of invention can significantly extend the service life of engine much higher than conventional lubrication oil.
Fig. 3 frictional resistance waveform diagram is intuitively to embody the resistance coefficients of each time phase, the lubricity of lubricating oil
Can be better, resistance is smaller, and HP, hp/litre is stronger, conversely, resistance is bigger, power per liter will be reduced, and power will subtract
Small, oil consumption just will increase.It can be seen from figure 3, the modified graphene lubricating oil machinery fortune of the polymolecularity energy of embodiment 1-5
Dynamic resistance is minimum, and energy saving is with the obvious advantage.
Fig. 4 lubricating oil volatilization waveform diagram is intuitively to embody the lubricating oil volatilization value of each time phase, can be seen by Fig. 4
Out, the modified graphene lubricating oil of polymolecularity energy of the volatilization value of conventional lubrication oil much higher than embodiment 1-5, lubricating oil are waved
Hair value is higher, and the mud carbon distribution that engine interior generates will be more, and the consumption of lubricating oil will be more.It can be seen that of the invention
Polymolecularity can modified graphene lubricating oil volatilization value it is low, mud carbon distribution is few, and energy saving is with the obvious advantage.
By Fig. 1-4 it can also be seen that using Bi2O3Or Sb2O3Metal oxide with high electron affinity adulterates
Greasy property made from graphene (embodiment 2-5) is better than lubricating oil (embodiment 1) made from undoped graphene.
The modified graphene lubricating oil of the energy of the polymolecularity made from the embodiment of the present invention 1~5 it can be seen from the above results
Greasy property much higher than conventional lubrication oil, and coefficient of friction is lower, can extend engine life, and mechanical resistance is small, section
Energy sexual clorminance is obvious.
Then graphene lubricating oil is moistened according to ASTM D92-12b GB/T 3536-2008 testing example 1~5 and tradition
Flash-point tests pour point according to ASTM D97-15, the results are shown in Table 1:
Table 1, pour point, flash-point statistical form
As shown in Table 1, lubricating oil pour point made from Examples 1 to 5 is below conventional lubrication oil pour point, shows using modification
Lubricating oil made from graphene has preferable mobility at relatively low temperature, can be suitable for lower temperature and use.From sudden strain of a muscle
From the point of view of point testing result, lubricating oil flash point made from Examples 1 to 5 is higher than conventional lubrication oil flash point, shows using modified graphite
Lubricating oil made from alkene is suitable for higher temperature.Therefore, suitable using modified graphene lubricating oil made from method of the invention
It is wider with temperature range.
Then the Zeta potential value of re-test Examples 1 to 5 and conventional lubrication oil, the results are shown in Table 2:
Table 2, Zeta potential Data-Statistics table
As shown in Table 2, the Zeta potential value that lubricating oil is made in Examples 1 to 5 is above the Zeta potential of conventional lubrication oil
Value, since Zeta potential value is the measurement to mutually exclusive between particle or attraction intensity, exists in Zeta potential absolute value
System is unstable under 10~30mV, after absolute value is higher than 30mV, as absolute value raising system is more stable.Therefore, the above results
Show that the lubrication oil systems obtained of the embodiment of the present invention 1~5 get over that stability is good, i.e., the dispersion performance of modified graphene is good.
Then the partial size of lubricating oil is made in detection Examples 1 to 5, as the result is shown the obtained lubricating oil of the embodiment of the present invention 1~5
Partial size is 60.55~101.2nm.Simultaneously using the lubricating oil without ultrasound and/or microwave treatment as control, the results show that
Do not use lubricating oil partial size made from ultrasound and microwave for 776.5~776.6nm, sonicated rear lubricating oil partial size is
448.7~461.2nm, lubricating oil partial size is 402.6~418.5nm after microwave treatment.As can be seen that using the method for the present invention
For lubricating oil obtained since partial size is within the scope of stable colloid, stability is more preferable.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (4)
1. the modified graphene lubricating oil of a kind of polymolecularity and high-affinity, which is characterized in that by weight include as follows
Component: 0.3 ~ 1.5 part of valence electron modified graphene, 0.05 ~ 0.5 part of dispersing agent, 0.05 ~ 1 part of affinity agent and base oil 100 are removed
Part；Go valence electron modified graphene that Bi is added to described2O3Or Sb2O3It is doped；The Bi2O3Or Sb2O3Additive amount
0.03-0.15 parts；It is described that valence electron modified graphene is gone to be fluorinated graphene, nitridation graphene, vulcanize graphene, boronized graphite
One of alkene, phosphatization graphene, silicated graphite alkene；The dispersing agent is that stearic acid, neopelex, fatty acid are sweet
One of grease and quaternary ammonium compound are a variety of, and the affinity agent is the inorganic polymer and not of the low molecular weight containing zirconium aluminate
One of the metal chromium complex that unsaturated organic acid and trivalent chromic ion are formed；A kind of polymolecularity and high-affinity
The preparation method of modified graphene lubricating oil, which comprises the steps of:
(1) valence electron modified graphene, dispersing agent will be gone to be added in base oil step by step according to the ratio, ultrasonic vibration obtains mixture；
(2) affinity agent is added in mixture obtained by step (1) according to the ratio, carries out microwave treatment, obtains polymolecularity and height
The modified graphene lubricating oil of compatibility；
By Bi before step (1)2O3Or Sb2O3Addition goes valence electron modified graphene to be doped.
2. the modified graphene lubricating oil of a kind of polymolecularity and high-affinity according to claim 1, it is characterised in that: institute
Stating base oil is one of mineral base oil, synthetic base oil and plant oil base oil or a variety of.
3. the preparation side of the modified graphene lubricating oil of a kind of any one of claims 1 or 2 polymolecularity and high-affinity
Method, which comprises the steps of:
(1) valence electron modified graphene, dispersing agent will be gone to be added in base oil step by step according to the ratio, ultrasonic vibration obtains mixture；
(2) affinity agent is added in mixture obtained by step (1) according to the ratio, carries out microwave treatment, obtains polymolecularity and height
The modified graphene lubricating oil of compatibility；
By Bi before step (1)2O3Or Sb2O3Addition goes valence electron modified graphene to be doped.
4. the preparation method of the modified graphene lubricating oil of a kind of polymolecularity and high-affinity according to claim 3,
Be characterized in that: supersonic frequency described in step (1) is 20kHz~1MHz, and power is 30W~15kW, shakes at least 1h；Step
(2) microwave treatment temperature 50 C~95 DEG C described in, the specific volume power of microwave radiation are 200W/L~6000W/L, processing
Time 1h~4h.
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| CN108641783B (en) * | 2018-03-26 | 2020-01-24 | 江苏大学 | CeO (CeO)2/FGO nano lubricating oil additive and bionic preparation method |
| CN109536240B (en) * | 2019-01-17 | 2021-06-22 | 常州碳孚新材料技术有限公司 | Lubricating oil additive containing lipophilic graphene and mesocarbon microbeads and preparation method thereof |
| CN110283642A (en) * | 2019-05-30 | 2019-09-27 | 辽宁兰晶科技有限公司 | A kind of quantum fluorinated graphene engine friction promotor and preparation method thereof |
| CN112877120A (en) * | 2021-03-02 | 2021-06-01 | 四川润连帮科技有限公司 | Graphene plant oil-based full-composite environment-friendly engine oil and preparation method thereof |
| CN115627557A (en) * | 2022-09-09 | 2023-01-20 | 罗莱生活科技股份有限公司 | Modified graphene fiber and preparation method and application thereof |
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