CN108048170A - The lube oil additive of functionalization graphene load montmorillonite, preparation method and applications - Google Patents
The lube oil additive of functionalization graphene load montmorillonite, preparation method and applications Download PDFInfo
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- CN108048170A CN108048170A CN201711383769.6A CN201711383769A CN108048170A CN 108048170 A CN108048170 A CN 108048170A CN 201711383769 A CN201711383769 A CN 201711383769A CN 108048170 A CN108048170 A CN 108048170A
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- graphene oxide
- additive
- montmorillonite
- lubricating oil
- graphene
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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
- C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
- C10M159/12—Reaction products
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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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/042—Mixtures of base-materials and additives the additives being compounds of unknown or incompletely defined constitution only
-
- 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
-
- 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
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- 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
Abstract
Lube oil additive, preparation method and applications the invention discloses a kind of functionalization graphene load natural montmorillonite.First, functional graphene oxide is obtained with silane coupler modified processing graphene oxide;Then, functional graphene oxide is mixed with natural montmorillonite nano-powder, water (or solvent) thermal response obtains the functionalization graphene composite additives of load montmorillonite;Finally, frictional wear experiment is carried out after the composite material lube oil additive and lubricating oil are mixed in a certain ratio, few additive amount is with regard to that can achieve the effect that coefficient of friction is substantially reduced, have effects that excellent antiwear and antifriction and intelligence are repaired, highest can achieve the effect that reduce by 32% than friction coefficient of lubricating oil.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, and has good greasy property and high bearing capacity.
Description
Technical field
The present invention relates to a kind of lube oil additives of functionalization graphene load montmorillonite and preparation method thereof, belong to profit
Lubricating oil technical field.
Background technology
In today of world energy sources growing tension, how to improve existing metal friction part service life or to worn-out part into
Row is repaired to reach to save material, reduce energy consumption and shorten maintenance time seems particularly urgent and again to increase economic efficiency
It will.The research of self-repair type additive is worn to save material and energy consumption, realizes that environmentally protective production etc. provides one
Efficient and feasible approach, and have been achieved for some progress.In the research of this kind of additive, mainly with selectively transfer
It is emphasis direction with both nano-particles.Usually repair additive is added in lubricating oil, by lubricating oil in machine system
In cycling renovation agent component is transported to wear surface, under eroded area energy field and substance field action, renovation agent component
Power chemistry and friction chemical reaction occurs with metal filings and lubricating oil degradation product, there is wear-compensating in eroded area generation
3rd body of effect, to have the function that recover the mated condition and mechanical property of wear surface.
Montmorillonite is a kind of natural minerals of silicate, be bentonite ore essential mineral component, be one kind by nanometer thickness
The electronegative silicate lamella in surface of degree is packed together the earthy mineral of composition by the electrostatic interaction of interlayer, brilliant
Structure cell in body structure is made of one layer of alumina octahedral of folder among two layers of oxygen-octahedron.Some researches show that nano imvites
Particle can be used as lube oil additive, these particles are adsorbed on friction surface quickly during friction, form one layer and play antifriction and make
[red legend is auspicious, Zhou Yuankang, Yang Lv, and Zhu Chi nano imvite lube oil additives are to metallic rubbing pairs for physical absorption film
The influence nonmetallic ores of friction and wear behavior, 2012,35 (04): 79-81].Although the antifriction function of montmorillonite is apparent,
But as inorganic nano-particle, long-time stability in the oil are poor, are very easy to sedimentation and accumulate hardened, cause to use
Oil quality declines in the process.Compared with the inorganic metal compound such as montmorillonite, serpentine filler of traditional lubricating action,
Graphene has stronger mechanical property, and high intensity, high tensile energy, high elastic modulus can preferably improve rubbing for material
Polishing machine and mechanical property are wiped, but graphene or graphene oxide do not have the repair function of apparent wear surface.In addition,
Graphene has big specific surface area, can be used as carrier adsorption nano-particle, nano-particle is avoided to occur in use
Hydraulic performance decline caused by storing up;The presence of nano-particle can also prevent reassociating for graphene sheet layer simultaneously.
The content of the invention
It is an object of the invention to provide a kind of functionalization graphene load montmorillonite lube oil additive and its moistening
It is applied in lubricating oil.
The technical solution adopted by the present invention is as follows to achieve these goals:
A kind of lube oil additive of functionalization graphene load montmorillonite, by graphene oxide using amino silicane coupling agent into
The modified obtained functional graphene oxide of row, then montmorillonite is bonded by chemical method, heated reduction obtains the function fossil
Black alkene composite lube additive.
Wherein, any one in amino silicane coupling agent A-1100, A-1110, A-1120, KBM-602.
Further, graphene oxide and the mass ratio of montmorillonite are 1:0.5-8.
The preparation method and applications of above-mentioned lube oil additive carry 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 montmorillonite 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, the profit of functionalization graphene load montmorillonite is obtained after cleaning
Oil additive.
Step(1)In, 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.
Step(2)In, 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 application of the lube oil additive of above-mentioned functionalization graphene load montmorillonite, additive quality in lubricating oil
Percentage is 0.01 %-5 %;The lubricating oil can be the lubricating oil of arbitrary brand, as the Kunlun scorpio F5000, SF15W-40
Type lubricating oil and Great Wall SJ10W-40 lubricating oil etc. or base oil is as mineral base oil or synthetic base oil.
Compared with prior art, it is an advantage of the invention that:
1)Easy to operate, raw material is easy to get, and cost is relatively low.
2)Two components in additive are that chemical bonding is grown together, it is suppressed that aggregation during single use has excellent
Different dispersion stabilization and strong mutual synergistic effect.
3)In additive two components all have certain anti-friction effect, then by chemical bonding graphite olefinic constituent it is excellent
Elegant mechanical performance and thermal conductivity, which has excellent dispersiveness and stability in lubricating oil, and has
Significant antiwear and antifriction effect and the intelligent repair to wear surface.
Description of the drawings
Fig. 1 is graphene oxide and functional graphene oxide infrared spectrogram described in example one.
Fig. 2 is simple physical mixing and 120 DEG C of graphene-supported montmorillonite composite materials of hydro-thermal Post functionalization in example one
Infrared spectrogram.
The SEM figures of lower sample polishing scratch after one friction and wear test of Fig. 3 examples.
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.
Additive of the present invention, by the effect of coupling agent by graphene and montmorillonite-based nano chemistry of particles bonding system
It is standby to obtain.By the positive coupling of two components, additive is in lubricating oil by the way that friction mechanics and/or physical reaction occurs
A kind of selfreparing film is formed in wear surface, plays self-repair function, so as to improve the greasy property of lubricating oil and machinery
Service life.Meanwhile the compound additive of functionalization has excellent dispersion stabilization, it in the oil can for a long time uniformly
Disperse without settling.
Graphene and montmorillonite by silane coupling agent are combined with each other by chemical method and obtain high stable by the present invention
Property the nano combined additive of functionalization graphene, the advantages of can integrating two kinds of materials each largely improves lubrication
The greasy property of oil, plays the role of excellent antiwear and antifriction.Meanwhile by chemically composited mode, nano-particle is anchored on
On graphene sheet layer, such compound system has high diffusivity and self-diffusion ability.In friction process, two components
Synergistic effect so that compound particle can be formed by diffusion, osmosis in metal surface being oozed with good friction performance
Permeable layers and diffusion layer so as to further reduce the friction factor of metallic rubbing pairs, play good friction reducing effect, while have bright
Aobvious intelligent repairing effect.It is an advantage of the invention that:Easy to operate, raw material is easy to get, and cost is relatively low;Additive has in lubricating oil
There are excellent dispersiveness and stability, and with significant antiwear and antifriction effect and the intelligent repair to wear surface.
In use, additive mass percent in lubricating oil is 0.01 %-5 %.The lubricating oil can be arbitrary
The lubricating oil of brand, as the Kunlun scorpio F5000, SF15W-40 type lubricating oil and Great Wall SJ10W-40 lubricating oil etc.;Can also be
Base oil is as mineral base oil or synthetic base oil.
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 montmorillonite-based 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 the lube oil additive powder of functionalization graphene load montmorillonite.Fig. 2 for simple physical mix (before) and
The infrared spectrogram of (after) functionalization graphene load montmorillonite composite material after 120 DEG C of hydro-thermals, by spectrogram it can be seen that into
Work(prepares functionalization graphene load montmorillonite composite material.
(3) tribological property is evaluated
By the lube oil additive of functionalization graphene load montmorillonite obtained and the Kunlun scorpio F5000 lubricating oil with not year-on-year
Example mixing.Utilize HT-1000 high temperature friction and wear testing machines, test condition:1000 g of load, 3 mm of friction radius, motor turn
Speed 336 r/min, 2 h of test period.Friction is secondary using ball-disk contact form, and upper sample isΦThe GCr15 steel balls of 6 mm,
770 HV of hardness;Lower sample is sizeΦ45 steel of the mm of 25 mm × 8, hardness are 250 ~ 300 HV.Function fossil in this example
Fretting wear data are shown in Table 1 to the lube oil additive of black alkene load montmorillonite under various concentration in lubricating oil, by various concentration
The visible additive obtained of coefficient of friction there is significant antiwear and antifriction effect;Attached drawing 3 is worn-out surface SEM after fretting wear
Figure, wear scar width is about 200 μm as seen from the figure, and not grind part compared with side apparent smooth for worn-out surface, it is seen that material
Material is in itself to the intelligent repair to wear surface.
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 (A-1100) 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 montmorillonite-based 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 the lube oil additive powder of functionalization graphene load montmorillonite.
(3) tribological property is evaluated
By the lube oil additive of functionalization graphene load montmorillonite obtained with the Kunlun scorpio F5000 lubricating oil centainly to compare
Example mixing.Utilize HT-1000 high temperature friction and wear testing machines, test condition:1000 g of load, 3 mm of friction radius, motor turn
Speed 336 r/min, 2 h of test period.Friction is secondary using ball-disk contact form, and upper sample isΦThe GCr15 steel balls of 6 mm,
770 HV of hardness;Lower sample is sizeΦ45 steel of the mm of 25 mm × 8, hardness are 250 ~ 300 HV.Its fretting wear data is shown in
Subordinate list 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 montmorillonite-based 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 the lube oil additive powder of functionalization graphene load montmorillonite.
(3) tribological property is evaluated
By the lube oil additive of functionalization graphene load montmorillonite obtained with the Kunlun scorpio F5000 lubricating oil centainly to compare
Example mixing.Utilize HT-1000 high temperature friction and wear testing machines, test condition:1000 g of load, 3 mm of friction radius, motor turn
Speed 336 r/min, 2 h of test period.Friction is secondary using ball-disk contact form, and upper sample isΦThe GCr15 steel balls of 6 mm,
770 HV of hardness;Lower sample is sizeΦ45 steel of the mm of 25 mm × 8, hardness are 250 ~ 300 HV.Its fretting wear data is shown in
Subordinate list 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 montmorillonite-based 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 the lube oil additive powder of functionalization graphene load montmorillonite.
(3) tribological property is evaluated
By the lube oil additive of functionalization graphene load montmorillonite obtained with the Kunlun scorpio F5000 lubricating oil centainly to compare
Example mixing.Utilize HT-1000 high temperature friction and wear testing machines, test condition:1000 g of load, 3 mm of friction radius, motor turn
Speed 336 r/min, 2 h of test period.Friction is secondary using ball-disk contact form, and upper sample isΦThe GCr15 steel balls of 6 mm,
770 HV of hardness;Lower sample is sizeΦ45 steel of the mm of 25 mm × 8, hardness are 250 ~ 300 HV.Its fretting wear data is shown in
Subordinate list 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 (KBM-602) 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.
(2) the montmorillonite-based 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 the lube oil additive powder of functionalization graphene load montmorillonite.
(3) tribological property is evaluated
By the lube oil additive of functionalization graphene load montmorillonite obtained with the Kunlun scorpio F5000 lubricating oil centainly to compare
Example mixing.Utilize HT-1000 high temperature friction and wear testing machines, test condition:1000 g of load, 3 mm of friction radius, motor turn
Speed 336 r/min, 2 h of test period.Friction is secondary using ball-disk contact form, and upper sample isΦThe GCr15 steel balls of 6 mm,
770 HV of hardness;Lower sample is sizeΦ45 steel of the mm of 25 mm × 8, hardness are 250 ~ 300 HV.Its fretting wear data is shown in
Subordinate list 1.
The lube oil additive of 1 functionalization graphene load montmorillonite of table fretting wear system in lubricating oil
Claims (10)
1. the lube oil additive of functionalization graphene load montmorillonite, which is characterized in that graphene oxide is used into amino silicone
Alkane coupling agent is modified obtained functional graphene oxide, then is bonded montmorillonite by chemical method, and heated reduction obtains institute
State functionalization graphene composite lube additive.
2. additive as described in claim 1, which is characterized in that amino silicane coupling agent A-1100, A-1110, A-
1120th, any one in KBM-602.
3. additive as described in claim 1, which is characterized in that graphene oxide and the mass ratio of montmorillonite are 1:0.5-8.
4. the preparation method of the additive as described in claim 1 ~ 3 is any, which is characterized in that carry 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) montmorillonite is weighed, is dissolved in functional graphene oxide dispersion liquid, stirs 30-90 min, in 100-180 DEG C of heating
0.5-2 h are reacted, stand cooling;It centrifuges, the lube oil additive of functionalization graphene load montmorillonite is obtained after cleaning.
5. preparation method as claimed in claim 4, which is characterized in that step(1)In, 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 ethyl alcohol;
Mode of heating can be water-bath reflux, hydro-thermal or solvent heat.
6. preparation method as claimed in claim 4, which is characterized in that step(2)In, the dispersion liquid of functional graphene oxide
In dispersant be water or ethyl alcohol;Mode of heating is hydro-thermal or solvent heat.
7. the application of the lube oil additive of the functionalization graphene load montmorillonite 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 %-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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