CN107325858A - A kind of preparation method of liquid-type graphene additive - Google Patents
A kind of preparation method of liquid-type graphene additive Download PDFInfo
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- CN107325858A CN107325858A CN201610279597.7A CN201610279597A CN107325858A CN 107325858 A CN107325858 A CN 107325858A CN 201610279597 A CN201610279597 A CN 201610279597A CN 107325858 A CN107325858 A CN 107325858A
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- graphene
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- additive
- type graphene
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Classifications
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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
- C10M125/02—Carbon; Graphite
-
- 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 present invention relates to the application field of graphene nano material, specially a kind of preparation method of liquid-type graphene additive.To be catalyzed the graphene of intercalation plavini or oxidation-reduction method production as raw material, oleic acid or base oil are decentralized medium, by mechanical crushing, ultrasonic shear, ultrasonic disperse, centrifugal classification multiple technologies means combination, obtain the strong liquid-type graphene additive of concentration height, good dispersion, suspending stabilized ability.The additive can be directly added in lubricant grease, and can obtain high performance graphene by simple mechanical agitation or artificial vibration is modified lubrication product.The preparation method of liquid-type graphene additive provided by the present invention has technique simple, reproducible, and application effect substantially waits technical characterstic.
Description
Technical field
The present invention relates to the application field of graphene nano material, specially a kind of liquid-type graphene additive
Preparation method.
Background technology
From the A.Geim and K.Novoselov of graceful Chester university of Britain in 2004 by special adhesive tape repeatedly
Paste and torn successfully from high starch breeding raw material since acquisition single-layer graphene, most frivolous but pole known to this
Caused for tough and tensile New Two Dimensional material with performances such as its peculiar and excellent mechanics, electricity, calorifics and magnetics
Worldwide extensive concern, it is contemplated that in high performance electronics, liquid crystal device, composite, Flied emission
The fields such as material, biomaterial, gas sensor and energy stores have huge application value and market latent
Power.
Graphene is combined between its lamellar structure with big pi bond, therefore is easily slid, and is suitable as
Used for lubriation material, can not only play the effect of antiwear and antifriction, lubricant grease antioxygen is improved while also having
Change ability, the effect for delaying or even preventing metallic article electrochemical corrosion.The science of U.S.'s Argonne National Laboratory
Family A.Sumant and A.Erdemir researchs find that the graphene sheet layer of steel surface absorption can make stainless steel rub
Wipe secondary coefficient of friction and be reduced to 0.15, wear rate then reduces 3~4 orders of magnitude.
In addition to independently forming lubricating film, graphene is also used as high-performance additives applied to lubricant grease
In, improve the performance particularly ability such as extreme pressure, heat conduction, anti-oxidant of lubrication product.It must be noted that
The surface of graphene sheet layer is in low pole, and the compatibility with oil medium is poor, may influence graphene in lubrication
The dispersion effect and long-time stability of grease.On the other hand, the thickness of graphene is small, radius-thickness ratio is big, surface energy
Height, easily reunites, and the operating method such as conventional stirring, vibration is to its dispersive property and stable suspersion ability
Improvement it is limited, and the laboratory technique such as ultrasonically treated can not then adapt to completely graphene be modified lubrication product
Industrialized production need.
Currently, the quality fluctuation of graphene commercially available prod is larger, and dispersiveness and stability are also relatively difficult to control,
It has impact on the development and application of graphene modification of lubricating oils product.
The content of the invention
It is an object of the invention to provide a kind of preparation side of the liquid-type graphene additive suitable for lubricant grease
Method, the favorable dispersibility of the additive, suspending power steady in a long-term is strong, easy to use, need to only be directly added to
Lubricant grease simultaneously suitably vibrates or stirred.
To realize above-mentioned technical goal, technical scheme proposed by the invention is：
A kind of preparation method of liquid-type graphene additive, comprises the following steps：
(1) granularity adjustment is carried out to graphene raw material by mechanical crushing or ultrasonic shear technique；
(2) graphene powder handled well is added into oil medium；
(3) lasting stirring makes graphene powder be sufficiently mixed with oil medium, when mixture is carried out into long in batches
Between ultrasonic disperse, 2~24 hours time；
(4) the outstanding mixed liquid of graphene after ultrasonically treated removes large scale present in outstanding mixed liquid by centrifugal treating
Particle, obtains graphene in the strong liquid-type graphene additive of good dispersion, suspending stabilized ability, additive
Volume is 2~20g/L.
In the preparation method of described liquid-type graphene additive, step (1), the piece of graphene after granularity adjustment
Layer size is not more than 2 μm.
In the preparation method of described liquid-type graphene additive, step (1), granularity adjustment uses mechanical crushing
During equipment, moving component is paddle-like, 10000~24000rpm of running speed, 10~120min of process time.
In the preparation method of described liquid-type graphene additive, step (1), granularity adjustment uses ultrasonic shear
During device, 600~1200W of operation power, 10~120min of effective time.
In the preparation method of described liquid-type graphene additive, step (2), oil medium uses oleic acid, base
The mixture of plinth oil or both, mixed proportion 0~100%.
In the preparation method of described liquid-type graphene additive, step (4), the centrifuge of centrifugal separation processes
2000~12000rpm of rotating speed, 0.5~4 hour working time.
The present invention basic fundamental thinking be：
Commercially available graphene (catalysis intercalation plavini or oxidation-reduction method production) is cut using mechanical crushing or ultrasound
The adjustment of row granularity is cut into, graphene adds into oil medium (oleic acid or mineral base oil) appropriate machine after processing
Tool is stirred, and long-time ultrasonic disperse is carried out in batches；The outstanding mixed liquid of graphene is placed in supercentrifuge after processing,
Using bulky grain that may be present in the outstanding mixed liquid of centrifugal classification effect removing, finally give and be uniformly dispersed, suspend surely
Qualitative good graphene additive slurry.In the present invention, graphene particles size is not more than 5 μm, in additive
Graphene volume is 2~20g/L.Graphene is scattered in oil medium in advance, the liquid-type graphite obtained
Alkene additive has good dispersed and steady in a long-term suspending power, and lubricant grease can be directly added to when using
In, it can obtain favorable dispersibility, suspending stabilized graphene using simple mechanical agitation or artificial vibration and change
Property lubricating oil.
Advantages of the present invention and beneficial effect are：
1st, the present invention can provide a kind of liquid-type graphene micron additive being modified for lubricant grease or nanometer adds
Plus agent, the additive is with good dispersed and steady in a long-term suspending power, and application process is easy.Only need by
Graphene additive is mixed into lubricating oil product in required ratio, is mechanically or manually stirred, vibration can obtain uniform
Scattered graphene modification of lubricating oils.
2nd, liquid-type graphene addictive preparation method proposed by the invention, is under the conditions of laboratory or workshop
Granularity to graphene is adjusted control, is further obtained by technological means such as ultrasonic disperse, centrifugations
The liquid-type graphene additive that concentration is high, dispersity is stable.
Brief description of the drawings
Fig. 1 is the optical photograph of liquid-type graphene nano additive, and graphene concentration is 5g/L.
Fig. 2 is the suspension stability that liquid-type graphene nano adds gained modification of lubricating oils after 100 times of dilution agent
Situation；Wherein, (a) time t=0, i.e., just mix；(b) after standing 30 days.
Embodiment
In specific implementation process, the preparation method of fluid present invention type graphene additive comprises the following steps：
(1) granularity adjustment, graphite after adjustment are carried out to graphene raw material by mechanical crushing or ultrasonic shear technique
The lamella size of alkene is not more than 2 μm, preferably 50~500nm.
(2) graphene powder handled well is added into oil medium, oil medium uses oleic acid, base oil
Or both mixture, oleic acid, base oil each 0~100wt% of ratio, preferably oleic acid, basis in mixture
The mass ratio of oil is 1:(20~50).
Base oil is the non-volatile grease that oil or ature of coal mineral extraction go out, and also can select fully synthetic artificial grease,
Such as：Polyolefin, saturated polyol fat, modified polyether or its mixture.
(3) lasting stirring makes graphene powder be sufficiently mixed with oil medium, when mixture is carried out into long in batches
Between ultrasonic disperse, using 50~500W of power, 2~24 hours processing times；
(4) the outstanding mixed liquid of graphene after ultrasonically treated removes large scale present in outstanding mixed liquid by centrifugal treating
Particle, you can the strong liquid-type graphene additive of favorable dispersibility, suspending stabilized ability is obtained, with quality hundred
Divide than metering, then graphene volume is 2~20g/L of oil medium quality.
The present invention is further illustrated with reference to embodiments, but the content of the invention is not limited solely to the reality
Apply example：
Embodiment 1
In the present embodiment, detailed process prepared by liquid-type graphene nano additive is with technological parameter：
(1) graphene prepared by catalysis intercalation plavini is chosen, 10min is processed using Universalpulverizer, crushed
Machine rotating speed 24000rpm, the lamella size of graphene is 800nm after adjustment；
(2) graphene after will be broken is added into oleic acid by 20g/L concentration, continues stirring until Graphene powder
End is well mixed with oil medium；
(3) 50mL graphene-oleic acid mixture is moved into 100mL beakers, is placed in ultrasonic disperse condition
Under, using 300W Power Processings 2 hours；
(4) the outstanding mixed liquid of the graphene after ultrasonic disperse is moved into supercentrifuge, is centrifuged with rotating speed 2000rpm
Handle 1h.
Gained liquid-type graphene nano additive concentration 5g/L, graphene particle size is not more than 2 μm, disperses
Property it is good, suspending stabilized ability is strong, as shown in Figure 1.The nanometer additive presses 1：100 mass ratios are mixed into profit
In sliding base oil, artificial vibration can obtain graphene modification of lubricating oils for several times, even if can still be protected after standing 30 days
Good scattered suspended state is held, as shown in Figure 2.
Embodiment 2
In the present embodiment, detailed process prepared by liquid-type graphene nano additive is with technological parameter：
(1) graphene prepared by catalysis intercalation plavini is chosen, 120min, powder are processed using Universalpulverizer
Broken machine rotating speed 10000rpm, the lamella size of graphene is 500nm after adjustment；
(2) graphene after will be broken is added to base oil (such as by 10g/L concentration：Mineral base oil) in,
Graphene powder is continued stirring until to be well mixed with oil medium；
(3) 100mL graphene-oleic acid mixture is moved into 200mL beakers, is placed in ultrasonic disperse bar
Under part, using 50W Power Processings 24 hours；
(4) the outstanding mixed liquid of the graphene after ultrasonic disperse is moved into supercentrifuge, is centrifuged with rotating speed 8000rpm
Handle 1h.
Gained liquid-type graphene nano additive concentration 7g/L, graphene particle size is not more than 1 μm, disperses
Property it is good, suspending stabilized ability is strong.
Embodiment 3
In the present embodiment, detailed process prepared by liquid-type graphene nano additive is with technological parameter：
(1) graphene prepared by oxidation-reduction method is chosen, by 1：100 mass ratios are mixed into absolute ethyl alcohol,
Using handled under the conditions of ultrasonic shears device 900W mixture after 30min, processing it is concentrated, filtering, dry
The lamella size for obtaining graphene after Ultrasonic Pulverization graphene, adjustment is 100nm；
(2) graphene of Ultrasonic Pulverization is added into oleic acid by 30g/L concentration, continues stirring until graphene
Powder is well mixed with oil medium；
(3) 50mL graphene-oleic acid mixture is moved into 100mL beakers, is placed in ultrasonically treated condition
Under, it is scattered 8 hours using 400W power ultrasonics；
(4) the outstanding mixed liquid of the graphene after ultrasonic disperse is moved into supercentrifuge, is centrifuged with rotating speed 20000rpm
Processing 0.5 hour.
Gained liquid-type graphene nano additive concentration 20g/L, graphene particle diameter is not more than 0.5 μm, point
Dissipate property good, suspending stabilized ability is strong.Four ball method Tribological Test shows, concentration dilution to 0.05g/L situations
Under, still there is graphene modification of lubricating oils good anti-attrition drop to damage performance, and compared with pure base oil, graphene changes
The coefficient of friction of property lubricating oil is reduced to 0.23, and wear scar diameter reduces 50%.
Embodiment 4
In the present embodiment, detailed process prepared by liquid-type graphene nano additive is with technological parameter：
(1) graphene prepared by oxidation-reduction method is chosen, by 1：100 mass ratios are mixed into absolute ethyl alcohol,
Using handled under the conditions of ultrasonic shears device 600W mixture after 120min, processing it is concentrated, filtering, dry
The lamella size for obtaining graphene after ultrasonic shear graphene, adjustment is 50nm；
(2) graphene of ultrasonic shear is added to oleic acid and base oil (such as by 10g/L concentration：It is fully synthetic
Base oil) mixture in, wherein the mass ratio of oleic acid and base oil be 1：9, continue stirring until graphene
Powder is well mixed with oil medium；
(3) 20mL graphene-oleic acid mixture is moved into 100mL beakers, is placed in ultrasonically treated condition
Under, it is scattered 8 hours using 50W power ultrasonics；
(4) the outstanding mixed liquid of the graphene after ultrasonic disperse is moved into supercentrifuge, is centrifuged with rotating speed 2000rpm
Processing 4 hours.
Gained liquid-type graphene nano additive concentration 18g/L, graphene particles size is not more than 2 μm, point
Dissipate property good, suspending stabilized ability is strong.
Embodiment result shows that the present invention is high, dispersed with concentration using oleic acid or base oil as decentralized medium
Well, the characteristics of suspending stabilized ability is strong, can be directly added in lubricant grease when using, and pass through simple machinery
Stirring or artificial vibration can obtain high performance graphene and be modified lubrication product.
Claims (6)
1. a kind of preparation method of liquid-type graphene additive, it is characterised in that comprise the following steps：
(1) granularity adjustment is carried out to graphene raw material by mechanical crushing or ultrasonic shear technique；
(2) graphene powder handled well is added into oil medium；
(3) lasting stirring makes graphene powder be sufficiently mixed with oil medium, when mixture is carried out into long in batches
Between ultrasonic disperse, 2~24 hours time；
(4) the outstanding mixed liquid of graphene after ultrasonically treated removes large scale present in outstanding mixed liquid by centrifugal treating
Particle, obtains graphene in the strong liquid-type graphene additive of good dispersion, suspending stabilized ability, additive
Volume is 2~20g/L.
2. according to the preparation method of the liquid-type graphene additive described in claim 1, it is characterised in that step
Suddenly in (1), the lamella size of graphene is not more than 2 μm after granularity adjustment.
3. according to the preparation method of the liquid-type graphene additive described in claim 1, it is characterised in that step
Suddenly in (1), when granularity adjustment is using mechanical crushing equipment, moving component is paddle-like, running speed 10000~
24000rpm, 10~120min of process time.
4. according to the preparation method of the liquid-type graphene additive described in claim 1, it is characterised in that step
Suddenly in (1), when granularity adjustment is using ultrasonic shears device, 600~1200W of operation power, effective time
10~120min.
5. according to the preparation method of the liquid-type graphene additive described in claim 1, it is characterised in that step
Suddenly in (2), oil medium is using the mixture of oleic acid, base oil or both, mixed proportion 0~100%.
6. according to the preparation method of the liquid-type graphene additive described in claim 1, it is characterised in that step
Suddenly in (4), 2000~12000rpm of centrifuge speed of centrifugal separation processes, 0.5~4 hour working time.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110509427A (en) * | 2019-07-09 | 2019-11-29 | 济南大学 | A kind of preparation method and application of graphene/cement dispersal device and the modified cement-based material of graphene |
| CN111117722A (en) * | 2020-01-09 | 2020-05-08 | 深圳市华胜隆科技有限公司 | Method for stably dispersing graphene powder in lubricating oil |
| CN111205903A (en) * | 2020-01-09 | 2020-05-29 | 深圳市华胜隆科技有限公司 | Method for stably dispersing graphene powder in gear box oil |
| CN113403125A (en) * | 2021-05-19 | 2021-09-17 | 兆丰(重庆)科技有限公司 | Preparation process of lubricating oil improver |
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| WO2015034340A1 (en) * | 2013-09-04 | 2015-03-12 | Instituto Tecnológico y de Estudios Superiores de Monterrey | Lubricating oil for automotive and industrial applications, containing decorated graphene |
| CN104593130A (en) * | 2014-12-29 | 2015-05-06 | 北京航空航天大学 | Method for preparing graphene water-based lubricating agent in situ |
| CN105176628A (en) * | 2015-10-20 | 2015-12-23 | 唐山建华科技发展有限责任公司 | Preparation method for lubricating oil of graphene loaded nanometer oxides |
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Patent Citations (4)
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| CN103589477A (en) * | 2012-08-13 | 2014-02-19 | 佛山市顺德宇红纳米科技有限公司 | Preparation method for stably dispersed composite metal nano-lubricating oil |
| WO2015034340A1 (en) * | 2013-09-04 | 2015-03-12 | Instituto Tecnológico y de Estudios Superiores de Monterrey | Lubricating oil for automotive and industrial applications, containing decorated graphene |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110509427A (en) * | 2019-07-09 | 2019-11-29 | 济南大学 | A kind of preparation method and application of graphene/cement dispersal device and the modified cement-based material of graphene |
| CN111117722A (en) * | 2020-01-09 | 2020-05-08 | 深圳市华胜隆科技有限公司 | Method for stably dispersing graphene powder in lubricating oil |
| CN111205903A (en) * | 2020-01-09 | 2020-05-29 | 深圳市华胜隆科技有限公司 | Method for stably dispersing graphene powder in gear box oil |
| CN113403125A (en) * | 2021-05-19 | 2021-09-17 | 兆丰(重庆)科技有限公司 | Preparation process of lubricating oil improver |
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Application publication date: 20171107 |