CN109971527A - Modified graphene material, lubricating oil containing modified graphene material and preparation method thereof - Google Patents
Modified graphene material, lubricating oil containing modified graphene material and preparation method thereof Download PDFInfo
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- CN109971527A CN109971527A CN201910319583.7A CN201910319583A CN109971527A CN 109971527 A CN109971527 A CN 109971527A CN 201910319583 A CN201910319583 A CN 201910319583A CN 109971527 A CN109971527 A CN 109971527A
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- graphene
- phenyl ring
- small molecule
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- acid solution
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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
- C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
- C10M103/02—Carbon; Graphite
-
- 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
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—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
Abstract
The invention discloses a kind of modified graphene materials, the lubricating oil containing modified graphene material and preparation method thereof, including will contain phenyl ring small molecule and graphene mixing after, ground, obtain uniformly mixed mixture, mixture is pressed into mixture；The mixture is electrochemically reacted in acid solution, obtains the electrolyte of the link graphene of small molecule containing phenyl ring；The electrolyte of the small molecule containing phenyl ring link graphene is subjected to ultrasound by ultrasonic machine, removal acid solution graphene is then centrifuged by centrifuge, obtains the small molecule containing phenyl ring being linked on the graphene.
Description
Technical field
The present invention relates to technical field of graphene more particularly to a kind of modified graphene material, contain modified graphene material
Lubricating oil of material and preparation method thereof.
Background technique
Fretting wear is prevalent in nature, and world's non-renewable energy loss late is caused to reach 50% because of fretting wear
More than, therefore one of the main reason for fretting wear is material and equipment scrapping.In industrial production and daily life, it will usually
The fretting wear in material or equipment is reduced using lubricating oil.
In order to increase the anti-wear and wear-resistant performance of lubricating oil, lubricating oil service performance is improved, it will usually be added in lubricating oil
Graphene enhances its abrasion resistance.Currently, in order to allow graphene to disperse inside lubricating oil, often using in graphene
The mode of surface attachment activity agent, to improve dispersion effect of the graphene in lubricating oil.When in actual use, with friction
Between extend, graphene surface attachment activating agent it is vulnerable, to influence the overall performance of lubricating oil.
Summary of the invention
The present invention provides a kind of modified graphene material, lubricating oil containing modified graphene material and preparation method thereof,
Modified graphene material stable structure therein, applies and is able to ascend the overall performance of lubricating oil in lubricating oil.
One aspect of the present invention provides a kind of modified graphene material, including graphene and is linked at containing on the graphene
Phenyl ring small molecule.
In a kind of embodiment, the small molecule containing phenyl ring is to contain hydroxyl at least one substituent group on phenyl ring
Or the small molecule of carboxyl.
In a kind of embodiment, the small molecule containing phenyl ring is preferably phenol or mellitic acid.
In a kind of embodiment, the graphene is preferably small lamella graphene；The piece of the small lamella graphene
Diameter is 1-10 microns, with a thickness of 0.33-3 nanometers.
Another aspect of the present invention provides a kind of preparation method of modified graphene material, comprising: will contain phenyl ring small molecule and
After graphene mixing, is ground, obtain uniformly mixed mixture, mixture is pressed into mixture；By the mixture
It is electrochemically reacted in acid solution, obtains the electrolyte of the link graphene of small molecule containing phenyl ring；It will the small molecule containing phenyl ring
The electrolyte for linking graphene carries out ultrasound by ultrasonic machine, is then centrifuged removal acid solution by centrifuge.
It is described to be electrochemically reacted the mixture in acid solution in a kind of embodiment, comprising: will be described
Mixture is connected to positive pole, and inert material is connected to power cathode；Acid solution is heated to 35-70 DEG C, by mixture and
Inert material immerses in acid solution；Startup power supply, control voltage strength are 5-20V, make mixture and inert material in the acid solution
Middle reaction 20-40min.
In a kind of embodiment, the electrolyte by the small molecule containing phenyl ring link graphene passes through ultrasonic machine
Ultrasound is carried out, removal acid solution is then centrifuged by centrifuge, comprising: by the electrolyte of the small molecule containing phenyl ring link graphene
Electrolyte by ultrasonic machine ultrasound 5-30 minutes, after obtaining ultrasound；Electrolyte after the ultrasound is added in centrifuge, if
Setting revolving speed is that 800-1500r/min is centrifuged 8-15 minutes, and separation removal supernatant liquid obtains deposit；In the deposit
Any one of water, ethyl alcohol or ethanol water is added, is uniformly mixed, obtains dispersion liquid；Centrifuge is added in the dispersion liquid
In, setting revolving speed is that 800-1500r/min is centrifuged 25-45 minutes, separation removal supernatant liquid, the modified graphite after being washed
Alkene material.
In a kind of embodiment, the preparation method is after being centrifuged removal acid solution by centrifuge, further includes: will
Modified graphene material after the washing is dried in vacuo, and modified graphene material is obtained.
Another aspect of the present invention provides a kind of lubricating oil, including base oil and as described in any one of above-mentioned embodiment
Modified graphene material.
Another aspect of the present invention provides a kind of preparation method of lubricating oil, comprising: will be as described in above-mentioned embodiment
Described in any item modified graphene materials are dispersed in base oil, obtain the lubricating oil containing modified graphene material.
Modified graphene material stable structure provided by the invention has anti-friction, reparation, reduces wear resistance；It should
Grapheme material is applied in lubricating oil, is able to ascend the overall performance of lubricating oil, is dispersed in lubricating oil steadily in the long term, drop
Low friction repairs abrasion, extends the service life of lubricating oil.
Detailed description of the invention
Fig. 1 shows the structural schematic diagram of modified graphene material of the embodiment of the present invention；
Fig. 2 shows the structural schematic diagrams of one of which of embodiment of the present invention small molecule containing phenyl ring；
Fig. 3 shows the structural schematic diagram of the small lamella graphene of the embodiment of the present invention；
Fig. 4 shows the structural schematic diagram of the small lamella graphene of edge of embodiment of the present invention weak oxide；
Fig. 5 shows the flow diagram of modified graphene material preparation method of the embodiment of the present invention.
Specific embodiment
To keep the purpose of the present invention, feature, advantage more obvious and understandable, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
It is only a part of the embodiment of the present invention, and not all embodiments.Based on the embodiments of the present invention, those skilled in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
Fig. 1 shows the structural schematic diagram of modified graphene material of the embodiment of the present invention.
Referring to Fig. 1, the embodiment of the present invention provides a kind of modified graphene material, including graphene and is linked on graphene
Small molecule containing phenyl ring.
Modified graphene material provided by the invention links small molecule containing phenyl ring on graphene.Graphene is mono-layer graphite
The two-dimentional carbon nano-structured material that piece is constituted has ultralow coefficient of friction, high thermal conductivity, big specific surface area, strong change
Learn stability.Studies have shown that graphene has excellent lubrication and abrasion resistance, and graphene can rub what frictional interface was formed
Adsorbed film and antithesis transfer membrane are wiped, excellent mechanical performance and chemical inertness inhibit directly contacting and grinding for friction pair surface
Damage.
The molecular weight of the small molecule containing phenyl ring is not easy to reunite less than 500, is easy dispersion, and have scalability, structure can be with
It is changed with the increase of CONTACT WITH FRICTION.After graphene is linked with small molecule containing phenyl ring, graphene sheet layer and lamella it
Between can directly lean on small molecule containing phenyl ring link, the steady chemical structure that small molecule containing phenyl ring is bonded with graphene, in the structure
Under, modified graphene material is able to bear the high pressure of 200 DEG C of high temperature and GPa ranks below, under the high temperature and pressure of the condition,
Disengaging will not be decomposed between small molecule containing phenyl ring and graphene.The link structure of small molecule containing phenyl ring and graphene can also appoint
Meaning distortion, advantageously forms super lubrication system, keeps the Wear vesistance of modified graphene material more excellent.It can be according to using ring
The difference in border links different number, different types of small molecule containing phenyl ring on graphene, contains benzene according to what is linked on graphene
The adjustment of the value volume and range of product of ring small molecule makes the anti-friction of modified graphene material, reparation, reduces wear resistance.
Fig. 2 shows the structural schematic diagrams of one of which of embodiment of the present invention small molecule containing phenyl ring.
Referring to fig. 2, in embodiments of the present invention, small molecule containing phenyl ring is to contain hydroxyl at least one substituent group on phenyl ring
The small molecule of base or carboxyl.
Hydroxy or carboxy is linked on an at least substituent group on phenyl ring, phenyl ring can be made to activate, and there is orientation effect,
Small molecule containing phenyl ring can expand the chip architecture of graphene, have modified graphene material provided in an embodiment of the present invention more
Perfect reparation structure, to make the lubricating oil added with the modified graphene material that there is repair function.Small point of phenyl ring will be contained
The designated position of son is linked on graphene, is advantageously formed super lubrication system, is being moistened when applying the modified graphene material
When in lubricating oil, the Wear vesistance of lubricating oil can be made more excellent.Further, in embodiments of the present invention, contain small point of phenyl ring
Son is preferably phenol or mellitic acid.
Fig. 3 shows the structural schematic diagram of the small lamella graphene of the embodiment of the present invention.
Referring to Fig. 3, in embodiments of the present invention, graphene is preferably small lamella graphene；The piece diameter of small lamella graphene
It is 1-10 microns, with a thickness of 0.33-3 nanometers.
The main acquiring technology means of the small lamella graphene of the embodiment of the present invention can use mechanical stripping method, chemical oxygen
Change method, crystal epitaxy method, chemical vapour deposition technique, organic synthesis method and CNT stripping method it is any.
Compared to the big lamella graphene that piece diameter is greater than 10 microns, small lamella graphene is more easier to contain its edge
The link of phenyl ring small molecule is handled, and small lamella graphene, because of feature small in size, curling is less likely to occur, connects for its own
It connects, avoids due to graphene itself curling, connects caused graphene agglomeration.By modification provided in an embodiment of the present invention
When grapheme material is applied in lubricating oil, can eliminate abrasion bring graphene for a long time makes from the negative effect reunited
Modified graphene material can be dispersed in lubricating oil steadily in the long term, can further decrease friction, repair abrasion, extend profit
The service life of lubricating oil.
Fig. 4 shows the structural schematic diagram of the small lamella graphene of edge of embodiment of the present invention weak oxide；Fig. 5 shows this
The flow diagram of inventive embodiments modified graphene material preparation method.
Referring to fig. 4 and Fig. 5, the embodiment of the present invention also provide a kind of preparation method of modified graphene material, comprising: step
101, after phenyl ring small molecule and graphene mixing will be contained, is ground, obtain uniformly mixed mixture, mixture is pressed into
Mixture；Step 102, mixture is electrochemically reacted in acid solution, obtains the electricity of the link graphene of small molecule containing phenyl ring
Solve liquid；Step 103, the electrolyte of the link graphene of small molecule containing phenyl ring is subjected to ultrasound by ultrasonic machine, then passes through centrifugation
Machine centrifugation removal acid solution, obtains modified graphene material.
Modified graphene material provided in an embodiment of the present invention during the preparation process, firstly, by graphene with containing phenyl ring it is small
Molecule is mixed, and mixing can carry out in any vessel.In order to keep graphene evenly dispersed with small molecule containing phenyl ring,
After mixing, it is also necessary to be ground to graphene and the mixture of the small molecule containing phenyl ring, grinder progress can be used in grinding, can also
With grinding rod hand lapping, it is ground to small molecule containing phenyl ring and is dispersed in graphene.For the ease of electrochemical in next step
The progress for learning reaction, after small molecule containing phenyl ring is dispersed in graphene, it is also necessary to by graphene and containing small point of phenyl ring
The mixture of son is pressed into mixture, and compacting can be suppressed by mold, and according to the needs of electrochemical reaction, mixture can be with
It is bar-like, sheet, bulk or any other irregular shape.
After the compacting for completing mixture, mixture is connected to power supply, by electrochemical reaction, to graphene and contains benzene
Ring small molecule is handled, and it is a large amount of that when carrying out edge weak oxide to graphene graphene sheet layer will not generate electrochemical process
Defect, can guarantee the integrality of graphene sheet layer, thus make modified graphene material obtained in friction process, graphene
Lamella will not be damaged easily, avoids since graphene sheet layer breakage influences the performance of modified graphene material.
While carrying out edge weak oxide to small lamella graphene using electrochemical reaction, acid solution being capable of catalytic graphite alkene
Edge oxide group is reacted with the group of the small molecule containing phenyl ring, is bonded graphene with small molecule containing phenyl ring, and is formed stable
Chemical structure is not easily decomposed under the high pressure of 200 DEG C of high temperature and GPa ranks below, manufactured modified graphene material is added
Steady in a long-term, extension Working Life of Lubricating Oil can be played the role of by being added in lubricating oil.Acid solution of the embodiment of the present invention can be dense
Sulfuric acid or mixed acid including the concentrated sulfuric acid.
Finally, removing acid solution after by ultrasound and centrifugation, the modified graphene material that chain is connected to the small molecule containing phenyl ring can be obtained
Material.Acid solution can be recycled, so that acid solution be avoided to pollute environment.
Thus obtained modified graphene material by electrochemical reaction stable structure, be easy dispersion, anti-friction performance it is good,
Recovery dynatron effect is good, it is good to reduce abrasive effect.
In embodiments of the present invention, in step 102, mixture is electrochemically reacted in acid solution, comprising: firstly,
Mixture is connected to positive pole, inert material is connected to power cathode；Then, acid solution is heated to 35-70 DEG C, will mixed
Fit and inert material immerses in acid solution；Finally, startup power supply, control voltage strength is 5-20V, makes mixture and inert material
20-40min is reacted in acid solution.
Mixture is connected to positive pole by conducting wire, makes mixture as anode；Inert material is connected by conducting wire
It connects in power cathode, makes inert material as cathode；Wherein inert material can be platinum electrode or other do not occur instead with acid solution
The metal material answered, and rodlike, sheet or other desired shape can be made in inert material, the embodiment of the present invention is not to inertia
The shape of material is defined.
In order to enable acid solution to be heated evenly, acid solution can be heated by the way of heating water bath, and is controlled acid solution and stablized
It is maintained between 35-70 DEG C.When acid solution is warming up between 35-70 DEG C, mixture and inert material are immersed in acid solution simultaneously,
And it controls the spacing between mixture and inert material and is maintained at 2-10cm.Startup power supply, power supply export direct current, control voltage
Intensity is between 5-20V, preferably 10V.After power supply is powered, electrochemical reaction occurs in acid solution for mixture and inert material,
While graphene carries out edge weak oxide, acid solution catalytic graphite alkene edge oxide group and the group of the small molecule containing phenyl ring are anti-
It answers, forms the modified graphene material that chain is connected to the small molecule containing phenyl ring.The modified graphene material of formation is dispersed in acid solution, shape
At the electrolyte of the link graphene of small molecule containing phenyl ring.
In embodiments of the present invention, by step 103, the electrolyte of the link graphene of small molecule containing phenyl ring is passed through into ultrasound
Machine carries out ultrasound, is then centrifuged removal acid solution by centrifuge, comprising: firstly, by the electricity of the link graphene of small molecule containing phenyl ring
It solves liquid to pass through ultrasonic machine ultrasound 5-30 minutes, the electrolyte after obtaining ultrasound；Then, centrifuge is added in the electrolyte after ultrasound
In, setting revolving speed is that 800-1500r/min is centrifuged 8-15 minutes, and separation removal supernatant liquid obtains deposit；After again, heavy
Any one of water, ethyl alcohol or ethanol water is added in product object, is uniformly mixed, obtains dispersion liquid；Finally, dispersion liquid is added
In centrifuge, setting revolving speed is that 800-1500r/min is centrifuged 25-45 minutes, separation removal supernatant liquid, changing after being washed
Property grapheme material.
In order to separate modified graphene material from the electrolyte of the link graphene of small molecule containing phenyl ring, by super
It is centrifuged after sound and removes most of acid solution first, obtain deposit, deposit includes the link graphene of small molecule containing phenyl ring and acid
Liquid；In order to further remove the acid solution of the link graphene surface attachment of small molecule containing phenyl ring, by the way that water, second are added in deposit
Any one of alcohol or ethanol water play the purpose of dissolved dilution acid solution, are then centrifuged again, to remove containing the molten of acid solution
Liquid；This step is 1-5 times repeatable, after repeatedly dissolving centrifugation, is reaching the removal link graphene surface of small molecule containing phenyl ring
Acid solution purpose.
In embodiments of the present invention, after being centrifuged removal acid solution by centrifuge, further includes: by the modification stone after washing
Black alkene material is dried in vacuo, and modified graphene material is obtained.Modified graphene material after washing is gone by vacuum drying
Except liquid remained on surface, dry modified graphene material is obtained.
The embodiment of the present invention also provides a kind of lubricating oil, including base oil and such as the modification stone of any one of above-described embodiment
Black alkene material.
Base oil is mixed with modified graphene material provided in an embodiment of the present invention, graphene modified material can be significant
Improve the carrying of lubricating oil and the abrasion-resistance that friction is secondary；The high heat conductance of graphene modified material can also be to the cold of lubricating oil
But performance brings promotion.Modified graphene material can effectively promote the formation of lubricating oil film, thus play good antifriction,
Wear-resistant and extreme pressure property, and then improve quality, using effect and the service life of lubricating oil.
Moreover, the lubricating oil of addition modified graphene material can show superior viscosity-temperature characteristics, further promoted
Quality, using effect and the service life of lubricating oil.Modified graphene material in lubricating oil have high dispersion, stability, no
It is easy to reunite, it is easily adsorbed in surface of friction pair and forms one layer of coherent film, effectively enhance the anti-wear and wear-resistant performance of lubricating oil.In machine height
Speed operating, easily formation hot-spot, and the modified graphene material added in lubricating oil can make Temperature Distribution more uniform,
To extend friction member service life.
The embodiment of the present invention also provides a kind of preparation method of lubricating oil, comprising: by the modification of any one of such as embodiment
Grapheme material is dispersed in base oil, obtains the lubricating oil containing modified graphene material.
Dispersion means herein can only be needed by ultrasonic disperse, emulsion dispersion, grinding distribution or other dispersing methods
It is uniformly mixed base oil with modified graphene material.
In order to be further explained explanation, two kinds of specific embodiments also provided below to the embodiments of the present invention.
Embodiment one
Step 201, it is mellitic acid: small lamella graphene=1 according to mass ratio by mellitic acid and small lamella graphene:
50 ratio is uniformly mixed in the agate mortar, is then ground 10 minutes by grinding rod in the agate mortar, is made mellitic acid
It is dispersed in small lamella graphene, obtains mixture.
Step 202,0.5g mixture is weighed, is pressed into mixture under 10MPa pressure using infrared tablet press machine, is mixed
Body is thin slice.
Step 203, thin slice is connected to the anode of power supply by conducting wire, platinized platinum is connected to the cathode of power supply by conducting wire,
The 80mL concentrated sulfuric acid is added in 100mL flask, by concentrated sulfuric acid heating water bath to 35-40 DEG C.It inserts again by thin slice is parallel with platinized platinum
Enter in the concentrated sulfuric acid, keep two electrode spacing 3cm, power supply is the DC voltage of 10V, startup power supply, and keeps the concentrated sulfuric acid temperature to be
35-40 DEG C, sustained response 30min, remaining thin slice and platinized platinum are taken out, links the electrolysis of graphene in flask for small molecule containing phenyl ring
Liquid.
Step 204, by small molecule containing phenyl ring link graphene electrolyte in ultrasonic cleaner sonic oscillation 5min,
It is then transferred to centrifuge tube, revolving speed 1000r/min is controlled by supercentrifuge and is centrifuged 10 minutes, the dense of centrifuge tube upper layer is recycled
Sulfuric acid.
Step 205, the sediment into centrifuge tube is mixed with water, and centrifuge tube is put into supercentrifuge, to turn
Fast 10000r/min is centrifuged 30 minutes, removes the aqueous solution on centrifuge tube upper layer.
Step 206, the sediment addition ethyl alcohol continued into centrifuge tube is uniformly mixed, and centrifuge tube is put into supercentrifuge
In, with revolving speed 10000r/min centrifugation 30 minutes, the ethyl alcohol on the upper layer of falling centrifuge tube is removed, the modified graphene material after being washed
Material.
Step 207, the modified graphene material after washing is obtained into dry modified graphene in 60 DEG C of vacuum drying 4h
Material.
Step 208,1g modified graphene material is taken, 100g base oil is uniformly mixed, and ultrasound 30 minutes is sanded 30 minutes,
Obtain lube oil additive.
It step 209, is lube oil additive: lubricating oil=1:50 according to mass ratio by lube oil additive and lubricating oil
Ratio is uniformly mixed, and obtains lubricating oil one.
Embodiment two
It step 301, is phenol according to according to mass ratio by phenol and small lamella graphene: small lamella graphene=1:50's
Ratio is uniformly mixed in the agate mortar, is placed in grinding distribution 10 minutes in agate mortar, is obtained mixture.
Step 302,0.5g mixture is weighed, is pressed into mixture under 10MPa pressure using infrared tablet press machine, is mixed
Body is thin slice.
Step 303, thin slice is connected to the anode of power supply by conducting wire, platinized platinum is connected to the cathode of power supply by conducting wire,
The 80mL concentrated sulfuric acid is added in 100mL flask, by concentrated sulfuric acid heating water bath to 55-60 DEG C.It inserts again by thin slice is parallel with platinized platinum
Enter in the concentrated sulfuric acid, keep two electrode spacing 3cm, power supply is the DC voltage of 10V, startup power supply, and keeps the concentrated sulfuric acid temperature to be
55-66 DEG C, sustained response 30min, remaining thin slice and platinized platinum are taken out, links the electrolysis of graphene in flask for small molecule containing phenyl ring
Liquid.
Step 204, by small molecule containing phenyl ring link graphene electrolyte in ultrasonic cleaner sonic oscillation 5min,
It is then transferred to centrifuge tube, revolving speed 1000r/min is controlled by supercentrifuge and is centrifuged 10 minutes, the dense of centrifuge tube upper layer is recycled
Sulfuric acid.
Step 205, the sediment into centrifuge tube is mixed with water, and centrifuge tube is put into supercentrifuge, to turn
Fast 10000r/min is centrifuged 30 minutes, removes the aqueous solution on centrifuge tube upper layer.
Step 207, the modified graphene material after washing is obtained into dry modified graphene in 60 DEG C of vacuum drying 4h
Material.
Step 208,1g modified graphene material is taken, 100g base oil is uniformly mixed, and ultrasound 30 minutes is sanded 30 minutes,
Obtain lube oil additive.
It step 209, is lube oil additive: lubricating oil=1:50 according to mass ratio by lube oil additive and lubricating oil
Ratio is uniformly mixed, and obtains lubricating oil two.
It should be noted that the lubricating oil in lubricating oil and embodiment two in embodiment one is the lubrication of same kind
Oil.The frictional behaviour of lubricating oil one and lubricating oil two is tested by four-ball tester.
And lubricating oil identical with embodiment one and embodiment two is selected, under the premise of not adding lube oil additive,
The test of frictional behaviour is carried out as blank control.
Test result is as follows table:
To sum up, lubricating oil one and lubricating oil two provided in an embodiment of the present invention apply the feelings of identical friction pressure in four-ball tester
Under condition, coefficient of friction and wear scar diameter have this to be decreased obviously compared to the plain oil for not adding lube oil additive.Into
One step, when small molecule containing phenyl ring of the embodiment of the present invention is mellitic acid, the ability of the reduction coefficient of friction of lubricating oil is mentioned
It rises larger；It is larger to the capability improving for reducing wear scar diameter when small molecule containing phenyl ring of the embodiment of the present invention is phenol.According to upper
It states as a result, the graphene of different small molecules containing phenyl ring link is different to lubricants performance improvement, for different frictions
Environment can graft different types of small molecule containing phenyl ring, to play anti-friction, reparation, reduce the different effects such as abrasion
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.Moreover, particular features, structures, materials, or characteristics described
It may be combined in any suitable manner in any one or more of the embodiments or examples.In addition, without conflicting with each other, this
The technical staff in field can be by the spy of different embodiments or examples described in this specification and different embodiments or examples
Sign is combined.
In addition, term " first ", " second " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance
Or implicitly indicate the quantity of indicated technical characteristic." first " is defined as a result, the feature of " second " can be expressed or hidden
It include at least one this feature containing ground.In the description of the present invention, the meaning of " plurality " is two or more, unless otherwise
Clear specific restriction.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. a kind of modified graphene material, which is characterized in that including graphene and be linked at small containing phenyl ring on the graphene
Molecule.
2. material according to claim 1, which is characterized in that the small molecule containing phenyl ring is that at least one takes on phenyl ring
The upper small molecule containing hydroxy or carboxy of Dai Ji.
3. material according to claim 1, which is characterized in that the small molecule containing phenyl ring is preferably phenol or benzene pregnancy
Acid.
4. material according to claim 1, which is characterized in that the graphene is preferably small lamella graphene；It is described small
The piece diameter of Sheet Graphite alkene is 1-10 microns, with a thickness of 0.33-3 nanometers.
5. a kind of preparation method of modified graphene material characterized by comprising
After phenyl ring small molecule and graphene mixing will be contained, is ground, obtain uniformly mixed mixture, mixture is pressed into
Mixture；
The mixture is electrochemically reacted in acid solution, obtains the electrolyte of the link graphene of small molecule containing phenyl ring；
The electrolyte of the small molecule containing phenyl ring link graphene is subjected to ultrasound by ultrasonic machine, is then centrifuged by centrifuge
Remove acid solution.
6. preparation method according to claim 5, which is characterized in that described that the mixture is carried out to electrification in acid solution
Learn reaction, comprising:
The mixture is connected to positive pole, inert material is connected to power cathode；
Acid solution is heated to 35-70 DEG C, mixture and inert material are immersed in acid solution；
Startup power supply, control voltage strength are 5-20V, and mixture and inert material is made to react 20-40min in the acid solution.
7. preparation method according to claim 6, which is characterized in that described that the small molecule containing phenyl ring is linked graphene
Electrolyte by ultrasonic machine carry out ultrasound, then by centrifuge centrifugation remove acid solution, comprising:
Electricity by the electrolyte of the small molecule containing phenyl ring link graphene by ultrasonic machine ultrasound 5-30 minutes, after obtaining ultrasound
Solve liquid；
Electrolyte after the ultrasound is added in centrifuge, setting revolving speed is that 800-1500r/min is centrifuged 8-15 minutes, separation
Supernatant liquid is removed, deposit is obtained；
Any one of water, ethyl alcohol or ethanol water are added in the deposit, is uniformly mixed, obtains dispersion liquid；
The dispersion liquid is added in centrifuge, setting revolving speed is that 800-1500r/min is centrifuged 25-45 minutes, in separation removal
Layer liquid, the modified graphene material after being washed.
8. preparation method according to claim 7, which is characterized in that the preparation method is being centrifuged removal by centrifuge
After acid solution, further includes:
Modified graphene material after the washing is dried in vacuo, modified graphene material is obtained.
9. a kind of lubricating oil, which is characterized in that including base oil and modified graphene material according to any one of claims 1-4
Material.
10. a kind of preparation method of lubricating oil characterized by comprising by modified stone according to any one of claims 1-4
Black alkene material is dispersed in base oil, obtains the lubricating oil containing modified graphene material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910319583.7A CN109971527B (en) | 2019-04-19 | 2019-04-19 | Modified graphene material, lubricating oil containing modified graphene material and preparation method of lubricating oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910319583.7A CN109971527B (en) | 2019-04-19 | 2019-04-19 | Modified graphene material, lubricating oil containing modified graphene material and preparation method of lubricating oil |
Publications (2)
| Publication Number | Publication Date |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009134707A2 (en) * | 2008-04-27 | 2009-11-05 | Board Of Regents, The University Of Texas System | Ultracapacitors and methods of making and using |
| CN102745666A (en) * | 2012-05-29 | 2012-10-24 | 大连理工大学 | Porous carbon with high-volumetric-specific-capacitance composite graphene, preparation method thereof, and application thereof |
| CN104831307A (en) * | 2015-05-13 | 2015-08-12 | 东南大学 | Preparation method of micro/nano graphene sheet |
| CN106221863A (en) * | 2016-07-07 | 2016-12-14 | 重庆德领科技有限公司 | Modified graphene lubricating oil that a kind of dispersive property is good and preparation method thereof |
| CN108517238A (en) * | 2018-04-04 | 2018-09-11 | 中国科学院宁波材料技术与工程研究所 | Protein modification redox graphene water lubrication additive, its preparation method and application |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009134707A2 (en) * | 2008-04-27 | 2009-11-05 | Board Of Regents, The University Of Texas System | Ultracapacitors and methods of making and using |
| CN102745666A (en) * | 2012-05-29 | 2012-10-24 | 大连理工大学 | Porous carbon with high-volumetric-specific-capacitance composite graphene, preparation method thereof, and application thereof |
| CN104831307A (en) * | 2015-05-13 | 2015-08-12 | 东南大学 | Preparation method of micro/nano graphene sheet |
| CN106221863A (en) * | 2016-07-07 | 2016-12-14 | 重庆德领科技有限公司 | Modified graphene lubricating oil that a kind of dispersive property is good and preparation method thereof |
| CN108517238A (en) * | 2018-04-04 | 2018-09-11 | 中国科学院宁波材料技术与工程研究所 | Protein modification redox graphene water lubrication additive, its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| MARYAM JAHAN ET AL.: "Structure-Directing Role of Graphene in the Synthesis of", 《AMERICAN CHEMICAL SOCIETY》 * |
| 安雅娟等: "石墨烯带-苯环-石墨烯带结构的电子输运", 《江西师范大学学报（自然科学版）》 * |
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