CN106350151A - Lubricant additive based on surface modified oxidized graphene, lubricant based on surface modified oxidized graphene, and preparation methods of lubricant additive and lubricant - Google Patents
Lubricant additive based on surface modified oxidized graphene, lubricant based on surface modified oxidized graphene, and preparation methods of lubricant additive and lubricant Download PDFInfo
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- CN106350151A CN106350151A CN201510408831.7A CN201510408831A CN106350151A CN 106350151 A CN106350151 A CN 106350151A CN 201510408831 A CN201510408831 A CN 201510408831A CN 106350151 A CN106350151 A CN 106350151A
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Abstract
The invention discloses a lubricant additive based on a surface modified oxidized graphene. The lubricant additive comprises oxidized graphene, the surface of the oxidized graphene is treated by a bile salt or a derivative of the bile salt, and the mass percentage of the oxidized graphene in a lubricant is 0.01-0.9%. The invention further provides the lubricant based on the modified oxidized graphene and preparation methods of the lubricant additive and the lubricant. The method is simple and practicable, is high in repetitive rate, and is suitable for large-scale industrial production. The lubricant additive has an excellent dispersing property, effectively improves the abrasion resistance property of the lubricant, and reduces the loss of an engine.
Description
Technical field
The present invention relates to lubricating oil field, especially a kind of lubrication based on surface modification graphene oxide
Oil additive, lubricating oil and preparation method thereof.
Background technology
The greasy property of electromotor is closely bound up with performances such as the safe and environment-friendly of automobile and energy-conservations, with
The continuous improvement of engine performance, the requirement to lubrication aspect is increasingly sophisticated, harsh, in order to improve
Engine lubrication performance, realize anti-attrition energy-conservation, improve mechanical efficiency lube oil additive also meet the tendency and
Raw.How to select suitable nano-particle as additive, and improve its dispersibility and become and moisten in recent years
The focus of oil additive area research.
Graphene oxide, as a kind of carbonaceous new material with two-dimensional structure, has higher specific surface
Long-pending, a series of excellent performance such as heat conductivity and mechanical property.Graphene oxide is added as solid
Agent is added in lubricating oil, can play obvious anti-attrition energy-saving effect.But graphene oxide is both close
The property of water also oleophylic leads to graphene oxide additive easily to produce layering and heavy in use
How shallow lake phenomenon, give full play to the efficiency of graphene oxide, overcomes drawbacks described above to be exploitation based on oxidation
A difficult problem faced by the lubricant additive of grapheme material is necessary.
Content of the invention
For the problems referred to above, the present invention proposes a kind of lubricating oil based on surface modification graphene oxide
Additive, lubricating oil and preparation method thereof, to improve stably dispersing in lubricating oil for the graphene oxide
Property, improve the lubricity of electromotor.
As one aspect of the present invention, the invention provides a kind of be based on surface modification graphene oxide
Lube oil additive, comprise the graphene oxide of bile salt or derivatives thereof surface modification, described
The mass percent in lubricating oil for the graphene oxide of bile salt or derivatives thereof surface treatment is
0.01～0.9%, preferably 0.1～0.6%.
Wherein, described bile salt includes but is not limited to cholic acid, deoxycholic acid, chenodeoxy cholic acid, stone
Cholic acid, glycocholic acid, glycochenodeoxycholate, taurocholic acid, the sodium salt of Irish moss (chondrux) or
Person's potassium salt, preferably NaTDC.
Wherein, described lubricating oil is automobile oil.
Wherein, the graphene oxide of described bile salt or derivatives thereof surface modification is by aoxidizing
The aqueous solution of Graphene is added in the aqueous solution containing described bile salt or derivatives thereof, after reaction
The product obtaining.
Wherein, the thickness 0.17～1.4nm of described graphene oxide, piece footpath size is 0.1～100 μm.
As another aspect of the present invention, the invention provides a kind of be based on surface modification graphite oxide
The lubricating oil of alkene, includes the lubrication based on surface modification graphene oxide as above described in any one
Oil additive.
As another aspect of the invention, the invention provides a kind of be based on surface modification graphite oxide
The preparation method of the lube oil additive of alkene, comprises the following steps:
Prepare graphite oxide, be dispersed in organic solvent being prepared into graphite oxide weak solution；
Add the aqueous solvent of bile salt or derivatives thereof in the graphite oxide weak solution of preparation, acutely
After stirring, obtain target product.
Or
Prepare graphene oxide, be dispersed in water being prepared into graphene oxide weak solution；
Add the aqueous solvent of bile salt or derivatives thereof in the graphene oxide weak solution of preparation, rise
Temperature, to 60～80 DEG C, obtains target product after reaction.
Wherein, the thickness of the described surface modification graphene oxide obtaining is 0.17～1.4nm, and piece footpath is big
Little is 0.1～100 μm.
As another aspect of the invention, present invention also offers a kind of aoxidize stone based on surface modification
The preparation method of the lubricating oil of black alkene, comprises the following steps:
As above the profit based on surface modification graphene oxide that preparation method described in any one is obtained
Oil additive is directly appended in lubricating oil, and mix homogeneously obtains final product target product；
Wherein, the described prepared lube oil additive based on surface modification graphene oxide is in described profit
Mass percent in lubricating oil is 0.01～0.9%, preferably 0.1～0.6%.
The present invention realizes surface of graphene oxide using two phase process and processes, and prepares the oxidation of good dispersion
Graphene.The method is simple, and repetitive rate is high, is suitable for large-scale industrialization production.The present invention
Lube oil additive, there is good dispersibility, it is to avoid the use of traditional dispersant, effectively increase
Plus the anti-wear performance of lubricating oil reduce the loss of electromotor.By NaTDC etc. to oxidation stone
Black alkene is surface-treated, and preparation has the graphene oxide of fine dispersibility, avoids dispersion simultaneously
The interpolation of agent.
Brief description
Fig. 1 is the flow chart of the preparation method of lubricating oil of the present invention.
Specific embodiment
For making the object, technical solutions and advantages of the present invention become more apparent, below in conjunction with concrete reality
Apply example, and referring to the drawings, the present invention is described in further detail.
Lubricating oil, be used in all kinds automobile, in plant equipment to reduce friction, protection machinery and
The liquid of workpiece or semisolid lubricants, act primarily as lubrication, cooling, antirust, cleaning, sealing and
The effect such as buffering, by its source point animal oil, vegetable oil, petroleum oil and synthetic lubricant fluid four are big
Class.Used in the present invention, lubricating oil is all types of automobile oils of commercialization.
Bile acid, the general name of the acids secreted in bile.Bile acid (bile in normal human bile
Acid) two big class can be divided into by structure: a class is sequestered bile acid, including cholic acid (cholic acid),
Deoxycholic acid (deoxycholic acid), chenodeoxy cholic acid (chenodeoxy cholic acid) and few
The lithocholic acid (1itho chalic acid) of amount；Another kind of is above-mentioned free bile acid and glycine or cattle sulphur
The product of acid combination, title conjugated bile acidses, mainly include glycocholic acid, glycochenodeoxycholate,
Taurocholic acid and Irish moss (chondrux) etc..Bile salt, then be the salt of bile acid, such as sodium salt,
Potassium salt etc..The derivant of bile salt, then be hydrogen atom in bile salt or atomic group to be had him former
Son or atomic group replace and derivative product, such as UDCA, na- gallbladder acyl-(3-o- nitro
- d- serine) etc..
Graphene oxide used in the present invention, can be the various graphene oxide that oneself knows, for example logical
Cross mechanical stripping method, chemical oxidization method, crystal epitaxy method, chemical vapour deposition technique, You Jihe
The Graphene of the method such as one-tenth method and CNT stripping method preparation aoxidizes the oxidation of processed further
The graphene oxide that Graphene or graphite oxide reducing agent partial reduction obtain is for example logical
Cross hummer method, reducing agent used can be for example hydrazine hydrate, sodium borohydride or vitamin c.Institute
State the thickness of graphene oxide and piece footpath is neglected greatly and is actually needed selection, preferred thickness is 0.17～1.4
Nm, piece footpath size is 0.1～100 μm.
The invention discloses a kind of lube oil additive based on surface modification graphene oxide, wherein exist
With the addition of in lubricating oil bile salt or derivatives thereof process graphene oxide, described bile salt or
The shared mass percent in lubricating oil of its derivative modified graphene oxide is 0.01～0.9%,
It is preferably 0.1～0.6%.Wherein said bile salt or derivatives thereof is preferably NaTDC.
Described lubricating oil can be all types automobile oil of commercialization, in described lubricating oil
Can also add various known lube oil additives, for example antioxidant, dispersant, antiwear additive,
Viscosity index improver etc..
The invention also discloses a kind of system of the lube oil additive based on surface modification graphene oxide
Preparation Method, comprises the following steps:
Prepare graphite oxide, be dispersed in organic solvent being prepared into graphite oxide weak solution；
The aqueous solvent of bile salt or derivatives thereof, Deca is added in the graphite oxide weak solution of preparation
Reducing agent, obtains target product after reaction.
Or
Prepare graphene oxide, be dispersed in water being prepared into graphene oxide weak solution；
Add the aqueous solvent of bile salt or derivatives thereof in the graphene oxide weak solution of preparation, rise
Temperature, to 60～80 DEG C, obtains target product after reaction.
Wherein, described organic solvent can be toluene, dimethylbenzene, hexamethylene etc..
Wherein, the thickness of the described surface modification graphene oxide obtaining is 0.17～1.4nm, and piece footpath is big
Little is 0.1～100 μm.
The above-mentioned prepared lube oil additive based on surface modification graphene oxide, i.e. modified oxidized stone
Mass percent in lubricating oil for the black alkene is 0.01～0.9%, preferably 0.1～0.6%.
As a preferred embodiment, as shown in figure 1, the invention also discloses one kind is changed based on surface
The preparation method of the lube oil additive of property graphene oxide, comprises the following steps:
Prepare graphene oxide and be configured to graphene oxide (go) weak solution；
Choose bile salt or derivatives thereof, such as NaTDC stirring and dissolving (dispersion in water
Agent)；
Add deoxycholic acid sodium water solution in the graphene oxide weak solution of preparation, be warmed up to 60～90
DEG C, preferably 80 DEG C, reaction obtained target product after 12～24 hours.
And lubricating oil based on surface modification graphene oxide to be obtained it is only necessary to by above-mentioned prepared base
Lube oil additive in surface modification graphene oxide is directly appended in lubricating oil (base oil),
It is uniformly mixed, obtain final product target product (gorhy lubricating oil).
In above-mentioned preparation method, the graphene oxide thickness of surface modification is 0.17～1.4nm, and piece footpath is big
Little is 0.1～100 μm.The above-mentioned prepared lube oil additive based on surface modification graphene oxide,
I.e. mass percent in lubricating oil for the modified graphene oxide is 0.01～0.9%, preferably 0.1～0.6
%.
NaTDC is surface-treated in the preparation process of graphene oxide, the adding of graphene oxide powder
Dosage can be adjusted with visual response degree, for example, can add 250～500g with 1～1.5g graphene oxide powder
Deionized water.The concentration adding the aqueous solution of NaTDC can be selected between 0.25～0.5mol/l
Select.
With reference to specific embodiment, the present invention is illustrated in more detail.
Embodiment 1
The preparation of graphite oxide: using hummer method, add 2g in the beaker of a 250ml
Crystalline flake graphite powder, is added thereto to 1g nano under conditions of ice-water bath3Add 46ml 98% afterwards
H2so4And it is sufficiently stirred for；It is slowly added to 6g kmno4, keep solution temperature 20 DEG C with
Go up and keep this condition 5 minutes, then remove ice-water bath and be heated to 35 DEG C, keep this condition
30 minutes；Add the water of 92ml, be stirred for 15 minutes, temperature will be increased to about 98 DEG C；Continue
The hydrogen peroxide of continuous add 80ml 60 DEG C 3%, is centrifuged on 30 minutes under 7200 turns with centrifuge
State the liquid after process；Clean residue with hot water and be about 7 until the ph of upper strata suspension；Obtaining
Powder be dispersed back into ultrasonic 15 minutes in water, obtain a kind of homogeneous after having filtered black residue
Suspension；Obtain graphite oxide after suspension lyophilizing.
NaTDC is surface-treated the preparation of Graphene: the graphite oxide powder that 1g is obtained disperses
In toluene, microwave irradiation is disperseed, and adds the deoxycholic acid that 5.3g concentration is 0.5mol/l
The aqueous solution of sodium, is warming up to 80 DEG C, and reacts filtration after 24h with this understanding, by the product obtaining
Thing uses first alcohol and water to rinse repeatedly successively, and vacuum drying obtains the oxidation stone of NaTDC surface modification
Black alkene.
The graphene oxide of the NaTDC surface modification that mass percent is 0.1% is added to profit
In lubricating oil, it is uniformly mixed.
Embodiment 2
Preparation method, with embodiment 1, differs only in the deoxidation adding 5.3g concentration to be 0.25mol/l
The aqueous solution of sodium cholate, is warming up to 80 DEG C, is heated to reflux, and NaTDC table is obtained by two phase process
The graphene oxide that face is processed, cleaning, filter and be dried to obtain the oxidation of NaTDC surface treatment
Graphene powder.
The graphene powder of the NaTDC surface treatment that mass percent is 0.50% is added to
In lubricating oil, it is uniformly mixed.
Embodiment 3
The preparation such as embodiment 2 of the Graphene of NaTDC surface treatment.
The graphene powder of the lithocholic acid potassium surface treatment that mass percent is 0.01% is added to profit
In lubricating oil, stir mixing.
Embodiment 4
The preparation such as embodiment 2 of the Graphene of NaTDC surface treatment.
The graphene powder of the NaTDC surface treatment that mass percent is 0.9% is added to profit
In lubricating oil, stir mixing.
Embodiment 5
The preparation of graphite oxide: using hummer method, add 2g in the beaker of a 250ml
Crystalline flake graphite powder, is added thereto to 1g nano under conditions of ice-water bath3Add 46ml 98% afterwards
H2so4And it is sufficiently stirred for；It is slowly added to 6g kmno4, keep solution temperature 20 DEG C with
Go up and keep this condition 5 minutes, then remove ice-water bath and be heated to 35 DEG C, keep this condition
30 minutes；Add the water of 92ml, be stirred for 15 minutes, temperature will be increased to about 98 DEG C；Continue
The hydrogen peroxide of continuous add 80ml 60 DEG C 3%, is centrifuged on 30 minutes under 7200 turns with centrifuge
State the liquid after process；Clean residue with hot water and be about 7 until the ph of upper strata suspension；Obtaining
Powder be dispersed back into ultrasonic 15 minutes in water, obtain a kind of homogeneous after having filtered black residue
Suspension；Obtain graphite oxide after suspension lyophilizing.
The preparation of graphene oxide weak solution: the graphite oxide powder that 1g is obtained is in deionized water
Disperseed using microwave irradiation, be warming up to 80 DEG C, Deca 6～10ml hydrazine hydrate, and at this
Filter after reaction 24h under part, the product obtaining is used successively first alcohol and water rinse repeatedly, be redissolved in
The dilute aqueous solution of graphene oxide is obtained in deionized water.
NaTDC is surface-treated the preparation of graphene oxide: to containing 1g oxidation obtained above stone
Add the aqueous solution of the NaTDC that 5.3g concentration is 0.5mol/l in the aqueous solution of black alkene, heat up
To 80 DEG C, it is stirred vigorously, filters after reaction 24h, the product obtaining is used successively first alcohol and water rush
Wash repeatedly, vacuum drying obtains the graphene oxide of NaTDC surface modification.
The graphene oxide of the NaTDC surface modification that mass percent is 0.3% is added to profit
In lubricating oil, it is uniformly mixed.
Embodiment 6
The preparation such as embodiment 6 of the graphene oxide of sodium taurocholate surface treatment.
The graphene powder of the sodium taurocholate surface treatment that mass percent is 0.2% is added to profit
In lubricating oil, stir mixing.
Comparative example 1～2
The method preparing graphite oxide powder is same as Example 1, differs only in and is added without bile acid
Salt, but directly use hydrazine hydrate or sodium borohydride to graphite oxide powder reduction according to hummer method,
Obtain black oxidation graphene powder.
The graphene oxide powder being 0.01% and 0.9% non-surface modification by mass percent respectively adds
Enter in lubricating oil, be uniformly mixed.
Storage stability is tested
The target product being obtained is stood 15 days, 30 days, the situation of object observing product.
Through experiment, after 15 days, with the addition of the Graphene lubricating oil being surface-treated
Occur in that obvious layering of reuniting in the lubricating oil of additive, and with the addition of NaTDC surface treatment
Graphene lube oil additive lubricating oil, even across 30 days afterwards, still can stably divide
Dissipate, do not observe obvious reunion or layering.
Table 1 embodiment 1～6 and comparative example 1～2 storage stability list
Anti-attrition energy-conservation performance test
Anti-attrition energy-efficient performance by four-ball tester (gb/t 308) and gear testing machine test target product.
Find through experiment, when the mass percent of the graphene oxide of NaTDC surface treatment is
When 0.1～0.6%, the anti-attrition energy-saving effect of lubricating oil is best.
By experiment above, the oxidation processing through bile salt or derivatives thereof of the present invention
After Graphene is added in lubricating oil, preferably can disperse graphene oxide so that lubricating oil point
Scattered stability, and the lubricity of electromotor is all greatly improved.And without bile salt or its
The graphene oxide that derivant is processed is although can improve the profit of electromotor in the case of big addition
Slip, but because dispersion inequality also leads to the deterioration of other performances.
Although embodiment illustrate only bile salt or derivatives thereof changing to the surface of graphene oxide
Property, but this area is it is appreciated that by the inspiration of above-described embodiment, such scheme is equally applicable
Modification in other type graphite alkene.
Particular embodiments described above, is carried out to the purpose of the present invention, technical scheme and beneficial effect
Further describe it should be understood that the foregoing is only the specific embodiment of the present invention,
It is not limited to the present invention, all any modifications within the spirit and principles in the present invention, made,
Equivalent, improvement etc., should be included within the scope of the present invention.
Claims (11)
1. a kind of lube oil additive based on surface modification graphene oxide, includes bile salt
Or derivatives thereof surface modification graphene oxide, described bile salt or derivatives thereof surface treatment
Mass percent in lubricating oil for the graphene oxide is 0.01～0.9%.
2. the lube oil additive based on surface modification graphene oxide according to claim 1,
Quality in lubricating oil for the graphene oxide of wherein said bile salt or derivatives thereof surface modification
Percent is 0.1～0.6%.
3. the lube oil additive based on surface modification graphene oxide according to claim 1,
Wherein said bile salt include cholic acid, deoxycholic acid, chenodeoxy cholic acid, lithocholic acid, glycocholic acid,
Glycochenodeoxycholate, taurocholic acid, the sodium salt of Irish moss (chondrux) or potassium salt.
4. the lube oil additive based on surface modification graphene oxide according to claim 1,
Wherein said lubricating oil is automobile oil.
5. the lube oil additive based on surface modification graphene oxide according to claim 1,
The graphene oxide of wherein said bile salt or derivatives thereof surface treatment is by by graphite oxide
Aqueous solution be added in the aqueous solution containing described bile salt or derivatives thereof, obtain after reaction
Product.
6. the lube oil additive based on surface modification graphene oxide according to claim 1,
The thickness of wherein said graphene oxide is 0.17～1.4nm, and piece footpath size is 0.1～100 μm.
7. a kind of lubricating oil based on surface modification graphene oxide, comprises just like claim 1 to 6
The lube oil additive based on surface modification graphene oxide described in any one.
8. a kind of preparation method of the lube oil additive based on surface modification graphene oxide, including
The following step:
Prepare graphite oxide, be dispersed in organic solvent being prepared into graphite oxide weak solution；
The aqueous solvent of bile salt or derivatives thereof is added in the described graphite oxide weak solution of preparation,
Target product is obtained after reaction.
9. a kind of preparation method of the lube oil additive based on surface modification graphene oxide, including
The following step:
Prepare graphene oxide, be dispersed in water being prepared into graphene oxide weak solution；
Add the aqueous solvent of bile salt or derivatives thereof in the graphene oxide weak solution of preparation, rise
Temperature, to 60～80 DEG C, obtains target product after reaction.
10. being added based on the lubricating oil of surface modification graphene oxide according to claim 8 or claim 9
Plus the preparation method of agent, the thickness of the described surface modification graphene oxide wherein obtaining is 0.17～1.4
Nm, piece footpath size is 0.1～100 μm.
A kind of 11. preparation methoies of the lubricating oil based on surface modification graphene oxide, including following step
Rapid:
By prepared for the preparation method as described in claim 8 to 10 any one based on modified oxidized
The lube oil additive of grapheme material is added in lubricating oil, and mix homogeneously obtains final product target product；
Wherein, the described prepared lube oil additive based on surface modification graphene oxide is in described profit
Mass percent in lubricating oil is 0.01～0.9%, preferably 0.1～0.6%.
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| CN201510408831.7A CN106350151A (en) | 2015-07-14 | 2015-07-14 | Lubricant additive based on surface modified oxidized graphene, lubricant based on surface modified oxidized graphene, and preparation methods of lubricant additive and lubricant |
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| CN201510408831.7A CN106350151A (en) | 2015-07-14 | 2015-07-14 | Lubricant additive based on surface modified oxidized graphene, lubricant based on surface modified oxidized graphene, and preparation methods of lubricant additive and lubricant |
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| CN106867625A (en) * | 2015-12-10 | 2017-06-20 | 闫立群 | Lubricating oil and lube oil additive based on surface modified graphite alkene |
| CN107142132A (en) * | 2017-05-26 | 2017-09-08 | 北京碳世纪科技有限公司 | Lube oil additive, lubricating oil based on grapheme material 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 |
| CN108658066A (en) * | 2018-06-15 | 2018-10-16 | 集美大学 | A kind of preparation method and composite fuel of the compound Low Sulfur Fuel Oil of graphene oxide |
| CN109536240A (en) * | 2019-01-17 | 2019-03-29 | 常州碳孚新材料技术有限公司 | A kind of lube oil additive and preparation method thereof containing lipophilic graphene and carbonaceous mesophase spherules |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106867625A (en) * | 2015-12-10 | 2017-06-20 | 闫立群 | Lubricating oil and lube oil additive based on surface modified graphite alkene |
| CN107142132A (en) * | 2017-05-26 | 2017-09-08 | 北京碳世纪科技有限公司 | Lube oil additive, lubricating oil based on grapheme material and preparation method thereof |
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| CN109536240A (en) * | 2019-01-17 | 2019-03-29 | 常州碳孚新材料技术有限公司 | A kind of lube oil additive and preparation method thereof containing lipophilic graphene and carbonaceous mesophase spherules |
| CN109536240B (en) * | 2019-01-17 | 2021-06-22 | 常州碳孚新材料技术有限公司 | Lubricating oil additive containing lipophilic graphene and mesocarbon microbeads and preparation method thereof |
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