CN108102763A - Serpentine/functionalization graphene lube oil additive, preparation method and applications - Google Patents
Serpentine/functionalization graphene lube oil additive, preparation method and applications Download PDFInfo
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- CN108102763A CN108102763A CN201711432605.8A CN201711432605A CN108102763A CN 108102763 A CN108102763 A CN 108102763A CN 201711432605 A CN201711432605 A CN 201711432605A CN 108102763 A CN108102763 A CN 108102763A
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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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/26—Compounds containing silicon or boron, e.g. silica, sand
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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
- C10M177/00—Special 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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- 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
- C10M2201/10—Compounds containing silicon
- C10M2201/102—Silicates
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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- 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
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a kind of serpentine/functionalization graphene lube oil additive, preparation method and applications.Its step is：Functional graphene oxide is obtained with silane coupler modified processing graphene oxide；Functional graphene oxide is mixed with serpentine nano-powder, water (or solvent) thermal response obtains the nanocomposite of serpentine/functionalization graphene；Frictional wear experiment is carried out after the composite additives and lubricating oil are mixed in a certain ratio, few additive amount has effects that excellent antiwear and antifriction and intelligence are repaired with regard to that can achieve the effect that coefficient of friction is substantially reduced.The additive agent powder of the present invention has excellent stability and dispersiveness in lubricating oil, and simple for process, cost-effective, and raw material is easy to get；Its excellent surface property, heat-conducting effect and stability etc. can generate beneficial effect to lubricating oil.
Description
Technical field
The present invention relates to a kind of serpentine/functionalization graphene lube oil additive, preparation method and applications, belong to profit
Lubricating oil technical field.
Background technology
As mechanized equipment constantly develops to directions such as high speed, heavy duty, high-precision, integrated and long-lives, thereupon
Wear problem influence it is more and more extensive, therefore resist fretting wear technology requirement it is higher and higher.Although conventional lubrication is oily
Still in occupation of the leading position in current lubricating oil field and market, but it is in harshnesses such as high-mechanic, high speed, long-plays
The limitation shown under working condition can not be ignored.At present, domestic and international researcher uses different types of additive, such as
Nano metal simple substance powder, hydroxide, oxide, sulphur compound, borate, silicate and high-molecular compound etc. improve
The lubricant effect of lubricating oil, and play positive effect in lubricating oil (fat).But some characteristics of these particles are sometimes
It can be limited in the dispersiveness of lubricating oil or the performance of self-repair function.Therefore, the research and development of new lubricant are subject to state
The extensive concern of inside and outside tribology scientific research personnel.
Serpentine main component is hydroxyl magnesium silicate Mg6[Si4O10](OH)8, it is a kind of In Natural Silicate solonchak, there is heat surely
Qualitative good, the of low cost and free of contamination advantage of use.Some researches show that natural serpentine micro-nano powder has preferably
Anti-wear and wear-resistant performance and self-repair function [it soars, Xu Yi, Xu Binshi, Zhang Baosen, Zhang Bo, the natural serpentine powders of history pendant capital
The self-healing properties of lube oil additive and reconditioning layer formation mechanism study tribology journals, 2011,31 (05):431-
438.] ；But nano-powder is unstable, is easily settled in reunion or oil.
Graphene is with sp by carbon atom2Hybrid form formed it is cellular, only there are one carbon atomic layer thickness two dimension
Material, have certain lubricity, but due between graphene stronger Van der Waals force make its in a solvent be difficult to stablize point
It is also bad to dissipate the compatibility of presence and other materials, is easily stacked accumulation again and is difficult to open.And graphene oxide not only has
Most of excellent specific properties of graphene, while there is abundant oxygen-containing functional group as hydroxyl, carboxyl, epoxy group in its sheet surfaces
Deng.These functional groups can not only mitigate the Van der Waals force between graphene sheet layer, at the same for its with other materials is compound provides
It may.Although graphene oxide and graphene have certain greasy property and mechanical performance [patent No. CN 101812351
A], but there is no the abilities that selfreparing is generated during mechanical friction.
The content of the invention
It is an object of the invention to provide a kind of serpentine/functionalization graphene lube oil additive, preparation method and its
Using the additive is in lubricating oil by the way that friction mechanics and/or physical reaction occur in process of friction and wear in friction surface
A kind of selfreparing film is formed, so as to improve the service life of the greasy property of lubricating oil and machinery.
The technical solution adopted by the present invention is as follows to achieve these goals：
A kind of serpentine/functionalization graphene lube oil additive changes graphene oxide using amino silicane coupling agent
Property be made functional graphene oxide, then serpentine be bonded by chemical method obtain the serpentine/functionalization graphene and moisten
Oil additive.
Wherein, any one in amino silicane coupling agent A-1100, A-1110, A-1120, KBM-602.
Further, the mass ratio of graphene oxide and serpentine is 1:0.5-8.
The preparation method of above-mentioned lube oil additive carries out as follows：
(1) graphene oxide prepared using improved Hummers methods is prepared the dispersion liquid of graphene oxide, added as raw material
Entering silane coupling agent, stir 0.5-2 h at room temperature, heating reaction 1-3 h, are cooled to room temperature at 60-95 DEG C, centrifuge,
Functional graphene oxide is obtained after cleaning；
(2) a certain amount of serpentine is weighed, is dissolved in functional graphene oxide dispersion liquid, 30-90 min are stirred, in 100-
180 DEG C of heating reaction 0.5-2 h, stand cooling；It centrifuges, serpentine/functionalization graphene lubricating oil is obtained after cleaning and is added
Add agent.
In step (1), the additive amount of silane coupling agent corresponds to every gram of graphene oxide for 25-200 mL silane coupling agents；
Dispersant in the dispersion liquid of graphene oxide is water or ethyl alcohol；Mode of heating can be water-bath reflux, hydro-thermal or solvent
Heat.
In step (2), the dispersant in the dispersion liquid of functional graphene oxide is water or ethyl alcohol；Mode of heating is water
Heat or solvent heat.
The lube oil additive of above-mentioned function serpentine/functionalization graphene is in use, additive matter in lubricating oil
Amount percentage is 0.01 %-0.5 %.The lubricating oil can be the lubricating oil of arbitrary brand, as the Kunlun scorpio F5000,
SF15W-40 types lubricating oil and Great Wall SJ10W-40 lubricating oil etc.；It can also be base oil as mineral base oil or synthesize basis
Oil.
Compared with prior art, it is an advantage of the invention that：（1）The system of serpentine/functionalization graphene lube oil additive
Standby process is easy to operate, and raw material is easy to get, and cost is relatively low；（2）By chemically composited mode, serpentine nano-particle is anchored on
On graphene sheet layer, such compound system has high diffusivity and self-diffusion ability, and the additive is made in the oil may be used
Uniformly dispersed for a long time without settling；（3）By the positive coupling of serpentine and two component of functional graphene, the addition
Agent is in use, few additive amount can just achieve the effect that coefficient of friction is substantially reduced, during friction-wear test
A kind of selfreparing film is formed in wear surface by the way that friction mechanics and/or physical reaction occurs, plays self-repair function, so as to
Improve the greasy property of lubricating oil and the service life of machinery.
Description of the drawings
Fig. 1 is example one, functional graphene oxide and graphene oxide infrared light is obtained by the reaction in five different solvents of example
Spectrogram.
Fig. 2 is the infrared of serpentine/functionalization graphene composite material after the mixing of one simple physical of example and 120 DEG C of hydro-thermals
Spectrogram.
Fig. 3 schemes for the SEM of lower sample after friction and wear test, and flat portion is the polishing scratch area after selfreparing in box.
Specific embodiment
The detailed description carried out below for specific implementation example to the present invention, but embodiment does not do any shape to the present invention
The restriction of formula.
The present invention uses chemically composited means, functionalization graphene is passed through with serpentine nano-powder silane coupled
Agent is anchored together, obtains stable serpentine/functionalization graphene lube oil additive, which can integrate two kinds of materials
Expect the advantages of respective, largely improve the greasy property of lubricating oil, play the role of excellent antiwear and antifriction, while have bright
Aobvious intelligent repairing effect.
Embodiment one
(1) it is using graphene oxide prepared by improved Hummers methods as raw material, obtained graphene oxide is even with silane
Join agent modification.First, 1.6 g of graphene oxide water solution of 2.5 wt% is weighed, adds 150 mL deionized waters dilution ultrasound
It is uniformly dispersed.Then, the silane coupling agent (A-1100) of 6 mL is added dropwise, at room temperature 1 h of magnetic agitation.Finally it is transferred to flask
In, 80 DEG C of 2 h of water-bath.Cooling is stood, is centrifuged, appropriate amount of deionized water is added in after washing and obtains functionalization graphite oxide
Alkene dispersion liquid.Fig. 1 is graphene oxide and functional graphene oxide infrared spectrogram, by spectrogram it can be seen that work(is successfully made
Graphene oxide can be changed.
(2) the serpentine nano-powder of 0.08 g is weighed, is dissolved in above-mentioned functional graphene oxide dispersion liquid；Magnetic force stirs
Mix 60 min；120 DEG C of 1 h of hydro-thermal reaction in reaction kettle are transferred to, stand cooling；It centrifuges, is washed respectively with water and ethyl alcohol,
It is dried to obtain serpentine/functionalization graphene lube oil additive powder.Fig. 2 mixes (before) and 120 DEG C for simple physical
The infrared spectrogram of (after) serpentine/functionalization graphene composite material after hydro-thermal, by spectrogram it can be seen that successfully preparing snake
Line stone/functionalization graphene composite material.
(3) tribological property is evaluated
Serpentine obtained/functionalization graphene lube oil additive and the Kunlun scorpio F5000 lubricating oil are mixed in varing proportions
It closes.Utilize HT-1000 high temperature friction and wear testing machines, test condition：1000 g of load, 3 mm of friction radius, motor speed 336
R/min, 120 min of test period.Friction is secondary using ball-disk contact form, and upper sample isΦThe GCr15 steel balls of 6 mm, hardness
770 HV；Lower sample is sizeΦ45 steel of the mm of 25 mm × 8, hardness are 250 ~ 300 HV.Serpentine/functionalization in this example
Fretting wear data are shown in Table 1 to graphene lube oil additive under various concentration in lubricating oil, by the coefficient of friction of various concentration
It can be seen that additive obtained has significant antiwear and antifriction effect；The oil sample for being wherein 2.5 mg/mL for addition concentration carries out
For a long time（320 min）Friction and wear test its data be shown in Table 1；Fig. 3 schemes for worn-out surface SEM after fretting wear, box
Interior flat portion is the polishing scratch area after selfreparing, and wear scar width is about 450 μm as seen from the figure, and worn-out surface ratio
It is apparent smooth that part is not ground on side, it is seen that the material intelligent repair to wear surface in itself.
Embodiment two
(1) it is using graphene oxide prepared by improved Hummers methods as raw material, obtained graphene oxide is even with silane
Join agent modification.First, 1.6 g of graphene oxide water solution of 2.5 wt% is weighed, adds 150 mL deionized waters dilution ultrasound
It is uniformly dispersed.Then, the silane coupling agent (KBM-602) of 3 mL is added dropwise, at room temperature 1 h of magnetic agitation.Finally it is transferred to flask
In, 80 DEG C of 2 h of water-bath.Cooling is stood, is centrifuged, appropriate amount of deionized water is added in after washing and obtains functionalization graphite oxide
Alkene dispersion liquid.
(2) the serpentine nano-powder of 0.08 g is weighed, is dissolved in above-mentioned functional graphene oxide dispersion liquid；Magnetic force stirs
Mix 60 min；120 DEG C of 1 h of hydro-thermal reaction in reaction kettle are transferred to, stand cooling；It centrifuges, is washed respectively with water and ethyl alcohol,
It is dried to obtain serpentine/functionalization graphene lube oil additive powder.
(3) tribological property is evaluated
Serpentine obtained/functionalization graphene lube oil additive is mixed with the Kunlun scorpio F5000 lubricating oil with certain proportion
It closes.Utilize HT-1000 high temperature friction and wear testing machines, test condition：1000 g of load, 3 mm of friction radius, motor speed 336
R/min, 120 min of test period.Friction is secondary using ball-disk contact form, and upper sample isΦThe GCr15 steel balls of 6 mm, hardness
770 HV；Lower sample is sizeΦ45 steel of the mm of 25 mm × 8, hardness are 250 ~ 300 HV.Its fretting wear data is shown in Table 1.
Embodiment three
(1) it is using graphene oxide prepared by improved Hummers methods as raw material, obtained graphene oxide is even with silane
Join agent modification.First, 1.6 g of graphene oxide water solution of 2.5 wt% is weighed, adds 150 mL deionized waters dilution ultrasound
It is uniformly dispersed.Then, the silane coupling agent (A-1110) of 8 mL is added dropwise, at room temperature 0.5 h of magnetic agitation.Finally it is transferred to flask
In, 60 DEG C of 1 h of water-bath stand cooling；It centrifuges, appropriate absolute ethyl alcohol is added in after washing and obtains functionalization graphite oxide
Alkene dispersion liquid.
(2) the serpentine nano-powder of 0.32 g is weighed, is dissolved in above-mentioned functional graphene oxide dispersion liquid；Magnetic force stirs
Mix 30 min；It is transferred to 100 DEG C of solvents in reaction kettle（Ethyl alcohol）0.5 h of thermal response stands cooling；It centrifuges, uses water respectively
It is washed with ethyl alcohol, is dried to obtain serpentine/functionalization graphene lube oil additive powder.
(3) tribological property is evaluated
Serpentine obtained/functionalization graphene lube oil additive is mixed with the Kunlun scorpio F5000 lubricating oil with certain proportion
It closes.Utilize HT-1000 high temperature friction and wear testing machines, test condition：1000 g of load, 3 mm of friction radius, motor speed 336
R/min, 120 min of test period.Friction is secondary using ball-disk contact form, and upper sample isΦThe GCr15 steel balls of 6 mm, hardness
770 HV；Lower sample is sizeΦ45 steel of the mm of 25 mm × 8, hardness are 250 ~ 300 HV.Its fretting wear data is shown in Table 1.
Embodiment four
(1) it is using graphene oxide prepared by improved Hummers methods as raw material, obtained graphene oxide is even with silane
Join agent modification.First, 1.6 g of graphene oxide water solution of 2.5 wt% is weighed, adds 150mL absolute ethyl alcohols dilution ultrasound
It is uniformly dispersed.Then, the silane coupling agent of 1mL is added dropwise（A-1120）, 2 h of magnetic agitation at room temperature.Finally it is transferred to reaction kettle
In, 95 DEG C of 3 h of solvent thermal reaction stand cooling；It centrifuges, alcohol adds in appropriate absolute ethyl alcohol and obtains functionalization oxidation stone after washing
Black alkene dispersion liquid.
(2) the serpentine nano-powder of 0.02 g is weighed, is dissolved in above-mentioned functional graphene oxide dispersion liquid；Magnetic force stirs
Mix 90 min；It is transferred to 140 DEG C of solvents in reaction kettle（Ethyl alcohol）2 h of thermal response stands cooling；Centrifuge, respectively with water and
Ethyl alcohol is washed, and is dried to obtain serpentine/functionalization graphene lube oil additive powder.
(3) tribological property is evaluated
Serpentine obtained/functionalization graphene lube oil additive is mixed with the Kunlun scorpio F5000 lubricating oil with certain proportion
It closes.Utilize HT-1000 high temperature friction and wear testing machines, test condition：1000 g of load, 3 mm of friction radius, motor speed 336
R/min, 120 min of test period.Friction is secondary using ball-disk contact form, and upper sample isΦThe GCr15 steel balls of 6 mm, hardness
770 HV；Lower sample is sizeΦ45 steel of the mm of 25 mm × 8, hardness are 250 ~ 300 HV.Its fretting wear data is shown in Table 1.
Embodiment five
(1) it is using graphene oxide prepared by improved Hummers methods as raw material, obtained graphene oxide is even with silane
Join agent modification.First, 1.6 g of graphene oxide water solution of 2.5 wt% is weighed, adds 150 mL absolute ethyl alcohols dilution ultrasound
It is uniformly dispersed.Then, the silane coupling agent (A-1100) of 6 mL is added dropwise, at room temperature 1 h of magnetic agitation.Finally it is transferred to flask
In, 75 DEG C of 2 h of water-bath back flow reaction.Cooling is stood, is centrifuged, appropriate amount of deionized water is added in after washing and obtains functionalization oxidation
Graphene dispersing solution.Fig. 1 is graphene oxide and functional graphene oxide infrared spectrogram, by spectrogram it can be seen that successfully making
Obtain functional graphene oxide.
(2) the serpentine nano-powder of 0.16 g is weighed, is dissolved in above-mentioned functional graphene oxide dispersion liquid；Magnetic force stirs
Mix 60 min；180 DEG C of 1 h of hydro-thermal reaction in reaction kettle are transferred to, stand cooling；It centrifuges, is washed respectively with water and ethyl alcohol,
It is dried to obtain serpentine/functionalization graphene lube oil additive powder.
(3) tribological property is evaluated
Serpentine obtained/functionalization graphene lube oil additive is mixed with the Kunlun scorpio F5000 lubricating oil with certain proportion
It closes.Utilize HT-1000 high temperature friction and wear testing machines, test condition：1000 g of load, 3 mm of friction radius, motor speed 336
R/min, 120 min of test period.Friction is secondary using ball-disk contact form, and upper sample isΦThe GCr15 steel balls of 6 mm, hardness
770 HV；Lower sample is sizeΦ45 steel of the mm of 25 mm × 8, hardness are 250 ~ 300 HV.Its fretting wear data is shown in Table 1.
Lubricating oil fretting wear coefficient of the table 1 containing serpentine/functionalization graphene additive
Claims (10)
1. serpentine/functionalization graphene lube oil additive, which is characterized in that be coupled graphene oxide using amino silane
Agent is modified obtained functional graphene oxide, then is bonded serpentine by chemical method and obtains the serpentine/functionalization
Graphene lube oil additive.
2. lube oil additive as described in claim 1, which is characterized in that amino silicane coupling agent A-1100, A-1110,
Any one in A-1120, KBM-602.
3. lube oil additive as described in claim 1, which is characterized in that the mass ratio of graphene oxide and serpentine is 1:
0.5-8。
4. the preparation method of the lube oil additive as described in claim 1 ~ 3 is any, which is characterized in that as follows into
Row：
Using graphene oxide prepared by improved Hummers methods as raw material, the dispersion liquid of graphene oxide is prepared, adds in silicon
Alkane coupling agent stirs 0.5-2 h at room temperature, and heating reaction 1-3 h, are cooled to room temperature at 60-95 DEG C, centrifuge, cleaning
After obtain functional graphene oxide；
Serpentine is dissolved in functional graphene oxide dispersion liquid and is stirred, in 100-180 DEG C of heating reaction 0.5-2 h, is stood
Cooling；It centrifuges, serpentine/functionalization graphene lube oil additive is obtained after cleaning.
5. preparation method as claimed in claim 4, feature is being, in step (1), the additive amount of silane coupling agent is
25-200 mL silane coupling agents correspond to every gram of graphene oxide；Dispersant in the dispersion liquid of graphene oxide is water or second
Alcohol.
6. preparation method as claimed in claim 4, feature is being, in step (1), in step (2), and functionalization oxidation
Dispersant in the dispersion liquid of graphene is water or ethyl alcohol；Serpentine is dissolved in functional graphene oxide dispersion liquid and is stirred
30-90 min。
7. the application of serpentine/functionalization graphene lube oil additive as described in claim 1 ~ 3 is any.
8. the use as claimed in claim 7, which is characterized in that additive mass percent in lubricating oil is 0.01 %-
0.5 %。
9. the use as claimed in claim 7, which is characterized in that the lubricating oil is mineral base oil or synthetic base oil.
10. the use as claimed in claim 7, which is characterized in that the lubricating oil is the Kunlun scorpio F5000, SF15W-40 type
Lubricating oil or Great Wall SJ10W-40 lubricating oil.
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| CN110982586B (en) * | 2019-11-05 | 2021-10-29 | 四川碳世界科技有限公司 | High-wear-resistance and strong-restoration graphene turbine oil and preparation method thereof |
| CN111250708A (en) * | 2020-03-23 | 2020-06-09 | 广西科技大学 | Wear-resistant bushing for excavator and preparation method thereof |
| CN111250708B (en) * | 2020-03-23 | 2021-12-24 | 广西科技大学 | Wear-resistant bushing for excavator and preparation method thereof |
| WO2022058095A1 (en) | 2020-09-18 | 2022-03-24 | Evonik Operations Gmbh | Compositions comprising a graphene-based material as lubricant additives |
| CN115491248A (en) * | 2022-10-19 | 2022-12-20 | 陈梓昊 | Lubricating oil containing modified graphene material and preparation method thereof |
| CN116426329A (en) * | 2023-04-18 | 2023-07-14 | 河北金普石油科技有限公司 | Antiwear lubricating oil capable of enabling parts to form magnetic levitation state and preparation method thereof |
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