CN106167261B - Oil-soluble graphene screening technique - Google Patents
Oil-soluble graphene screening technique Download PDFInfo
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- CN106167261B CN106167261B CN201610532056.0A CN201610532056A CN106167261B CN 106167261 B CN106167261 B CN 106167261B CN 201610532056 A CN201610532056 A CN 201610532056A CN 106167261 B CN106167261 B CN 106167261B
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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
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- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention discloses a kind of oil-soluble graphene screening techniques, by graphene, base oil and dispersant into homogeneous solution, the solution then are placed in broken wall machining, the solution after processing is centrifuged removal hypostasis obtains suspension.It is more easy to remove the valence electron on its surface compared to the graphene to sink using the graphene in the suspension separated, i.e., more preferably realizes homodisperse with oil solvent.The oily fusibleness graphene that method disclosed by the invention filters out removable surface valence electron provides an important raw material preparatory process for graphene lubricating oil preparation field.
Description
Technical field
The invention belongs to graphene lubricating oil fields, and in particular to a kind of to be melted for producing the oil used in graphene lubricating oil
The screening technique of property graphene.
Background technology
Graphene is a kind of two-dimentional carbon material, is single-layer graphene, bilayer graphene and few layer (3~10 layers) graphene
It is referred to as.Graphene can firmly be attached to metal surface, graphene have almost fully transparent, nontoxic, chemical property is excellent,
The features such as excellent lubricating properties, mechanical strength are big, excellent thermal conductivity, extremely strong electric conductivity, makes graphene have in lubricating area
Huge application potential.
But due to its high-specific surface area of graphene and the strong model ylid bloom action of interlayer, they are very easy to reunite
Or graphite-structure is stacked into again, and graphene is difficult dissolving in usual vehicle.So graphene lubricating oil is real
It realizes, it is important to resolve the scattering problem in oil product, graphene is as lube oil additive, in friction process
In show good greasy property, it is appropriate not require nothing more than form and the number of plies and it is necessary to lubricating oil can be dispersed stably in
In.If being once separated, graphite is easy for being difficult to play its greasy property due to reunion.
By study find to realize that graphene uniform is dispersed stably in oil product, the first step tackle graphene surface into
Row is modified, and removes the valence electron of graphene surface, but through further research, it has been found that, not all graphene can be easier to
Removal graphene surface valence electron, so how to filter out the oily fusibleness graphene of removable surface valence electron for graphite
Alkene lubricating oil preparation field is very important research topic.
The content of the invention
In view of this, it is an object of the invention to provide a kind of method of oil-soluble graphene screening, sieved by this method
The removal surface valence electron that the graphene elected can be easier to, and help to ensure that the properties of product of later stage graphene lubricating oil.
To achieve the above object, the present invention specifically provides following technical solution：
Oil-soluble graphene screening technique, includes the following steps：By graphene, base oil and dispersant into uniformly it is molten
Then the solution is placed in wall-breaking machine or ball milling machines, the solution after processing is centrifuged to obtain suspension by liquid.
Preferably, the dispersant is stearic acid, in neopelex, fatty glyceride, quaternary ammonium compound
It is one or more of.
Preferably, the base oil is one or more of mineral base oil, synthetic base oil and plant base oil.
Preferably, count in mass ratio, the additive amount of the dispersant is 2.0~3.5wt% of solution.
Preferably, the additive amount of the graphene is equivalent to 10~20wt% of base oil.
It is furthermore preferred that the centrifugation is to centrifuge at least 15min under the conditions of speed is ten thousand revs/min of 6-8.
Preferably, the wall-breaking machine processing is to handle at least 5min in rotating speed for 25000 revs/min or more.
In the present invention, the graphene is single-layer graphene, bilayer graphene or 3~10 layer graphenes.
The beneficial effects of the present invention are：The invention discloses a kind of screening technique of oil-soluble graphene, by using
Then suitable dispersant after wall-breaking machine is handled, is then centrifuged, will be not easy to remove surface valence electron graphene removal, on
The removal surface valence electron being easier to is collected into clear liquid, so as to obtain the good graphene of dispersion performance, and it is used herein
Method is simple, suitable for industrialized production.
Description of the drawings
In order to make the purpose of the present invention, technical solution and advantageous effect clearer, the present invention provides drawings described below：
Fig. 1 shows the aspect graphs of mixed solution after centrifugation.
Specific embodiment
The preferred embodiment of the present invention is described in detail below.The experiment side of actual conditions is not specified in embodiment
Method, usually according to normal condition or according to the condition proposed by manufacturer.
Embodiment 1
Oil-soluble graphene is screened using following methods
By graphene, base oil and dispersant into homogeneous solution, the solution is then placed in broken wall and is machined into
Rotating speed handles 5min for 25000 revs/min or more, then by the solution after processing under the conditions of centrifugal speed is ten thousand revs/min of 6-8
15min is centrifuged, removal hypostasis collects upper strata suspension.Base oil uses mineral base oil in the present embodiment, and dispersant uses
Be stearic acid, dosage accounts for the 2.3wt% of base oil；Graphene uses 5 layer graphenes, and graphene additive amount accounts for base oil
10wt%.
As shown in Figure 1, wherein 1 represents to float over graphene above, 2 represent the graphite of sinking for state diagram after centrifugation
Alkene, as seen from Figure 1 solution two states are presented after centrifugation, 70% or so graphene is deposited in container bottom,
30% or so graphene suspends in the solution.And micro-analysis further is carried out to this two-part graphene, it finds to float over
Its number of plies of graphene above is smaller than the graphene number of plies of sedimentation.
Embodiment 2
Oil-soluble graphene is screened using following methods
By graphene, base oil and dispersant into homogeneous solution, the solution is then placed in broken wall and is machined into
Rotating speed handles 8min for 28000 revs/min or more, is then 6~80,000 revs/min of conditions in centrifugal speed by the solution after processing
Lower centrifugation 20min, removal hypostasis collect upper strata suspension.In the present embodiment, base oil uses synthetic base oil, and dispersant makes
It is neopelex, dosage accounts for the 2.5wt% of base oil, and graphene uses 3 layer graphenes, and dosage accounts for base oil
15%.
As shown in Figure 1, wherein 1 represents to float over graphene above, 2 represent the graphite of sinking for state diagram after centrifugation
Alkene, as seen from Figure 1 solution two states are presented after centrifugation, 65% or so graphene is deposited in container bottom,
35% or so graphene suspends in the solution.And micro-analysis further is carried out to this two-part graphene, it finds to float over
Its number of plies of graphene above is smaller than the graphene number of plies of sedimentation.
Embodiment 3
Oil-soluble graphene is screened using following methods
By graphene, base oil and dispersant into homogeneous solution, the solution is then placed in broken wall and is machined into
Rotating speed handles 6min for 30000 revs/min or more, is then 6~80,000 revs/min of conditions in centrifugal speed by the solution after processing
Lower centrifugation 18min, removal hypostasis collect upper strata suspension.In the present embodiment, base oil uses plant base oil, and dispersant makes
It is fatty glyceride, dosage accounts for the 3.0wt% of total solution, and graphene uses bilayer graphene, and dosage accounts for base oil
20%.
As shown in Figure 1, wherein 1 represents to float over graphene above, 2 represent the graphite of sinking for state diagram after centrifugation
Alkene, as seen from Figure 1 solution two states are presented after centrifugation, 70% or so graphene is deposited in container bottom,
30% or so graphene suspends in the solution.And micro-analysis further is carried out to this two-part graphene, it finds to float over
Its number of plies of graphene above is smaller than the graphene number of plies of sedimentation.
Embodiment 4
Oil-soluble graphene is screened using following methods
By graphene, base oil and dispersant into homogeneous solution, the solution is then placed in broken wall and is machined into
Rotating speed handles 10min for 25000 revs/min or more, is then 6~80,000 revs/min of conditions in centrifugal speed by the solution after processing
Lower centrifugation 25min, removal hypostasis collect upper strata suspension.Base oil uses plant base oil in the present embodiment, and dispersant makes
It is quaternary ammonium compound, dosage accounts for the 3.0wt% of total solution；Graphene uses single-layer graphene, and dosage accounts for base oil
18wt%.
As shown in Figure 1, wherein 1 represents to float over graphene above, 2 represent the graphite of sinking for state diagram after centrifugation
Alkene, as seen from Figure 1 solution two states are presented after centrifugation, 70% or so graphene is deposited in container bottom,
30% or so graphene suspends in the solution.And micro-analysis further is carried out to this two-part graphene, it finds to float over
Its number of plies of graphene above is smaller than the graphene number of plies of sedimentation.
The graphene for screening separated upper layer graphene and sedimentation to Examples 1 to 3 respectively again carries out surface valency electricity
Son experiment, i.e., be modified graphene surface, and experiment carries out as follows：Graphene is carried out by chemical oxidation method
Acidification obtains graphene oxide, then by graphene oxide and gamma-methyl allyl acyloxypropyl trimethoxysilane (KH-
570) reaction is prepared into functionalization graphene, then graphene is further detected to its dispersiveness in oil-based solvent.
Table 1 describes sedimentation graphene obtained by Examples 1 to 4 carries out products obtained therefrom after valence electron with the graphene to float respectively
Performance：
The separated graphene of table 1, Examples 1 to 4 carries out the dispersion performance after valence electron
Dispersed phase of the graphene screened as seen from the above table by the screening technique of the present invention in base oil
Its compared with exclusion is with obvious effects more preferable, and can also further be proved through apparent observation institute by surveying its Zeta potential value
Obtained result.
Comparative example
Surface valence electron experiment is carried out using common unscreened graphene, equally using the steps：It is logical
It crosses chemical oxidation method and graphene oxide is obtained to graphene progress acidification, then by graphene oxide and γ-methyl-prop
Alkene monomethacryloxypropyl trimethoxy silane (KH-570) reaction is prepared into functionalization graphene, is then further examined graphene
Survey its dispersiveness in oil-based solvent.It finds directly to carry out surface valence electron using unscreened graphene by verifying
The phenomenon that being re-dissolved in oil-based solvent being equally also easy to produce reunion.
It to sum up can be explained, ensure good dispersion of the graphene in oil-based solvent for preparing graphene lubricating oil, it is right
It is also very important in the preliminary screening of graphene, it is disclosed by the invention a kind of for producing the oil used in graphene lubricating oil
The screening technique of fusibleness graphene.The graphene screened using this method is easier to the removal of graphene surface valence electron i.e.
Graphene is modified and then prepares the more excellent graphene lube product of quality.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (5)
1. oil-soluble graphene screening technique, which is characterized in that include the following steps：Graphene, base oil and dispersant are mixed
Homogeneous solution is synthesized, the solution is then placed in wall-breaking machine or ball milling machines, then centrifuges the solution after processing
Removal hypostasis obtains suspension；The dispersant is stearic acid, neopelex, fatty glyceride, quaternary ammonium compound
One or more of；The centrifugation is to centrifuge at least 15min under the conditions of speed is ten thousand revs/min of 6-8；At the wall-breaking machine
Reason is to handle at least 5min in rotating speed for 25000 revs/min or more.
2. oil-soluble graphene screening technique according to claim 1, it is characterised in that：The base oil is mineral base
One or more of oil, synthetic base oil and plant base oil.
3. oil-soluble graphene screening technique according to claim 1, it is characterised in that：The additive amount of the dispersant is suitable
In 2.0 ~ 3.5wt% of base oil.
4. oil-soluble graphene screening technique according to claim 1, it is characterised in that：The additive amount of the graphene is suitable
In 10 ~ 20wt% of base oil.
5. according to any one of the claim 1 ~ 4 oil-soluble graphene screening technique, it is characterised in that：The graphene is single
Layer graphene, bilayer graphene or 3 ~ 10 layer graphenes.
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| CN106753693A (en) * | 2016-12-09 | 2017-05-31 | 王茹楠 | A kind of preparation method of the lube oil additive of ultra-low friction |
| CN112852523B (en) * | 2021-03-09 | 2022-12-06 | 山东莱克科技有限公司 | Renewable lubricating oil composition based on graphene modification |
| CN113479869B (en) * | 2021-06-30 | 2022-12-20 | 杭州烯鲸新材料科技有限公司 | Method for grading and screening particle size of graphene |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730631A (en) * | 2005-08-10 | 2006-02-08 | 湖南大学 | Preparation method of carbon nanotube compounded lubricating oil |
| CN105296053A (en) * | 2015-10-20 | 2016-02-03 | 唐山市烯润科技发展有限公司 | Method for preparing graphene lubricating oil additive |
| CN105670737A (en) * | 2016-02-29 | 2016-06-15 | 成都新柯力化工科技有限公司 | Preparation method of graphene lubricating additive |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730631A (en) * | 2005-08-10 | 2006-02-08 | 湖南大学 | Preparation method of carbon nanotube compounded lubricating oil |
| CN105296053A (en) * | 2015-10-20 | 2016-02-03 | 唐山市烯润科技发展有限公司 | Method for preparing graphene lubricating oil additive |
| CN105670737A (en) * | 2016-02-29 | 2016-06-15 | 成都新柯力化工科技有限公司 | Preparation method of graphene lubricating additive |
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