CN106883900A - The lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification, lubricating oil and application - Google Patents
The lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification, lubricating oil and application Download PDFInfo
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- CN106883900A CN106883900A CN201510906342.4A CN201510906342A CN106883900A CN 106883900 A CN106883900 A CN 106883900A CN 201510906342 A CN201510906342 A CN 201510906342A CN 106883900 A CN106883900 A CN 106883900A
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Abstract
The invention discloses a kind of lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification, lubricating oil and application.A kind of graphene oxide lube oil additive of nitrogenous surface modification, comprising the graphene oxide using nitrogenous surface modification, the thickness of the graphene oxide of the nitrogenous surface modification is 0.17 1.4nm, and piece footpath size is 10 1000nm, and the mass percent in lubricating oil is 0.01 0.9%.And lubricating oil and the application in lubricating oil of a kind of graphene oxide lube oil additive for adding nitrogenous surface modification.The method of the present invention is simple and easy to apply, and repetitive rate is high, is adapted to large-scale industrialization production.Lube oil additive of the invention has dispersiveness well, and can be effectively increased the abrasion resistance of lubricating oil can simultaneously reduce the loss of engine.
Description
Technical field
The present invention relates to lubricating oil field, especially a kind of lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification, lubricating oil and application.
Background technology
The performances such as the greasy property of engine and the safe and environment-friendly of automobile and energy-conservation are closely bound up, with the continuous improvement of engine performance, requirement in terms of to lubrication is increasingly sophisticated, harshness, in order to the lube oil additive for improving engine lubrication performance, realize anti-attrition energy-conservation, improve mechanical efficiency also arises at the historic moment.Conventional additive is divided into the oil soluble additive and the major class of solid additive two with special layer structure of polar functionalities at present.
Graphene oxide as a kind of carbonaceous new material with two-dimensional structure, with a series of excellent properties such as specific surface area higher, thermal conductivity and mechanical property.It is added to graphene oxide as solid additive in lubricating oil, obvious anti-attrition energy-saving effect can be played.But how to prevent graphene oxide additive from producing layering and deposited phenomenon in use, be the technical problem that researcher has to face.
The content of the invention
Regarding to the issue above, the present invention proposes a kind of graphene oxide lube oil additive of nitrogenous surface modification modification and preparation method thereof, to improve the dispersion stabilization of Graphene, improves the lubricity of engine.
As one aspect of the present invention, the invention provides a kind of lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification, graphene oxide containing nitrogen-containing compound surface modification, the thickness of the graphene oxide of the nitrogen-containing compound surface modification is 0.17-1.4 nm, piece footpath size is 10-1000nm, mass percent in lubricating oil is 0.01-0.9 %, is more preferably 0.1-0.6 %.
Wherein, the reagent for performing the nitrogen-containing compound surface modification is selected from the chain alkyl amine that carbon number is 4-16, and the compound with amide groups, imide, glucose amido, pyrrole radicals or pyridine radicals.
Wherein, the reagent for performing the nitrogen-containing compound surface modification is ethylenediamine, hexamethylene diamine, acetamide, galactosamine, preferably ethylenediamine or hexamethylene diamine.Wherein, the lubricating oil is automobile oil.
As another aspect of the present invention, the invention provides a kind of lubricating oil of the graphene oxide based on nitrogen-containing compound surface modification, include the lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification described in as above any one.
As another aspect of the invention, present invention also offers a kind of application of the lube oil additive in automobile oil of the graphene oxide based on nitrogen-containing compound surface modification described in as above any one.
The present invention realizes that surface of graphene oxide is processed using two phase process, prepares oil-soluble graphene oxide.The method is simple and easy to apply, and repetitive rate is high, is adapted to large-scale industrialization production.Lube oil additive of the invention, with good dispersiveness, the use of traditional dispersant is avoided, the abrasion resistance for effectively increasing lubricating oil and can reduce the loss of engine, layering and deposited phenomenon that graphene oxide additive is produced in use can be prevented.
Brief description of the drawings
Fig. 1 is the flow chart of the preparation method of lubricating oil of the invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention become more apparent, below in conjunction with specific embodiment, and referring to the drawings, the present invention is described in further detail.
Lubricating oil; it is used in all kinds automobile, plant equipment reducing friction; the liquid or semisolid lubricants of protection machinery and workpiece; it is main to play lubrication, cooling, antirust, cleaning, sealing and buffering etc.; divide animal oil, vegetable oil, petroleum oil and the major class of synthetic lubricant fluid four by its source.The lubricating oil used in the present invention is all types of automobile oils of commercialization.
The nitrogenous coating material for performing nitrogen-containing compound surface modification includes but is not limited to the chain alkyl amine and the compound with groups such as amide groups, imide, glucose amido, pyrrole radicals or pyridine radicals that carbon number is 4-16, such as ethylenediamine, hexamethylene diamine, acetamide, galactosamine etc., wherein preferably ethylenediamine, hexamethylene diamine.
Graphene oxide used in the present invention, can be various known Graphenes, the Graphene of the methods such as method, chemical oxidization method, crystal epitaxy method, chemical vapour deposition technique, organic synthesis method and CNT stripping method preparation is for example by mechanically pulling off by being processed further treatment, such as the Graphene after oxidation processes, can also be the graphene oxide for obtaining graphite oxide partial reduction, the graphene oxide for for example being prepared by Hummer methods.Big the neglecting of the thickness of the graphene oxide and piece footpath is actually needed selection, and preferred thickness is 0.17-1.4 nm, and piece footpath size is 10-1000nm.
The invention discloses a kind of lube oil additive of the graphene oxide based on the modification of nitrogenous coating material, wherein contain the graphene oxide of nitrogen-containing compound surface modification, the mass percent that the graphene oxide of the nitrogen-containing compound surface modification is shared in lubricating oil is 0.01-0.9%, preferably 0.1-0.6 %.
Lubricating oil can be various types of lubricating oil, preferably automobile oil, and various known lube oil additives, such as antioxidant, dispersant, viscosity index improver can also be added in lubricating oil.
The invention also discloses a kind of preparation method of lube oil additive, the lube oil additive is based on the graphene oxide of nitrogen-containing compound surface modification, as shown in figure 1, comprising the following steps：
Graphene oxide is dissolved in ultra-pure water, ultrasonic disperse prepares graphene oxide（GO）Weak solution；
Choose nitrogenous coating material to be dissolved in organic solution, prepared composition powder, the organic solvent can be toluene or hexamethylene；
The graphene oxide that will be prepared（GO）Weak solution and the organic solution containing nitrogenous coating material（Dispersant）Mixing, forms two-phase, is warmed up to 60-90 DEG C, is stirred vigorously lower reaction 3-12 hours；
Washed with the mixed solutions for many times of first alcohol and water, wherein methyl alcohol and water volume ratio are, for example, 3：7, it is centrifugally separating to obtain target product.
And the lubricating oil of the graphene oxide based on nitrogen-containing compound surface modification is obtained, it is only necessary to the lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification obtained above is directly appended to lubricating oil（Base oil）In, it is uniformly mixed and obtains final product target product（GORHY lubricating oil）.
In above-mentioned preparation method, graphene oxide thickness is 0.17-1.4 nm, and piece footpath size is 10-1000nm.The lube oil additive of the graphene oxide based on the modification of nitrogenous coating material obtained above, i.e. mass percent of the graphene oxide of nitrogen-containing compound surface modification in lubricating oil are 0.01-0.9 %, preferably 0.1-0.6 %.
The present invention is illustrated in more detail with reference to specific embodiment.
Embodiment
1
The preparation of graphite oxide：Using Hummer methods, 2g crystalline flake graphite powder is added in a beaker of 250 mL, 1g NaNO are added thereto under conditions of ice-water bath3The H of 46mL 98% is added afterwards2SO4And it is sufficiently stirred for；Be slowly added to 6g KMnO4, keep solution temperature is more than 20 DEG C and keeps this condition 5 minutes, then remove ice-water bath and be heated to 35 DEG C, keep this condition 30 minutes；The water of 92 mL is added, is stirred for 15 minutes, temperature will be increased to about 98 DEG C；60 DEG C 3% of 80 mL of hydrogen peroxide is continuously added, the liquid after above-mentioned treatment in 30 minutes is centrifuged under 7200 turns with centrifuge；Residue is cleaned with hot water until the pH of upper strata suspension is about 7；The powder for obtaining is dispersed back into ultrasound 45 minutes in water, a kind of homogeneous suspension is obtained after having filtered black residue；Graphite oxide is obtained after suspension is freezed（Alkene）.
The graphite oxide that 1 g is obtained（Alkene）Powder is dissolved in deionized water, ultrasonic disperse 2 hours, add the ethylenediamine toluene solution that 5.3 g concentration are 0.25 mol/L, it is warming up to 80 DEG C, it is heated to reflux, the graphene oxide that ethylenediamine is surface-treated is obtained by two phase process, the graphene oxide powder of ethylenediamine surface modification is filtered and is dried to obtain in cleaning.The graphene oxide of the ethylenediamine surface modification that mass percent is 0.15 % is added in lubricating oil, a hour is stirred, the lubricating oil of the graphene oxide based on ethylenediamine surface modification is obtained.
It is above-mentioned the step of graphite oxide is dissolved in into water in, the addition of graphite oxide powder can be adjusted with visual response degree, for example, can add 250-500g deionized waters with 1 ~ 1.5g graphite oxide powder.
Embodiment
2
, with embodiment 1, differ only in addition is the ethylenediamine toluene solution that 5.3 g concentration are 0.5 mol/L for reaction raw materials and condition.
Embodiment
3
, with embodiment 1, it is the graphite oxide for obtaining 1.5 g to differ only in for reaction raw materials and condition（Alkene）Powder is dissolved in 100ml deionized waters, adds the galactosamine toluene solution that 1.4 g concentration are 0.25 mol/L.
Embodiment
4
Reaction raw materials and condition differ only in and the Graphene of the ethylenediamine surface modification that mass percent is 0.01 % are added in lubricating oil with embodiment 1, stir a hour.
Embodiment
5
Reaction raw materials and condition differ only in and the Graphene of the ethylenediamine surface modification that mass percent is 0.9 % are added in lubricating oil with embodiment 1, stir a hour.
Embodiment
6
Reaction raw materials and condition differ only in and the Graphene of the galactosamine surface modification that mass percent is 0.30 % are added in lubricating oil with embodiment 3, stir a hour.
Comparative example
1-2
The method of graphene powder is prepared with embodiment 1, differ only in be added without nitrogenous coating material carry out two phase process reaction graphene oxide powder is surface-treated.
Respectively be 0.01 % by mass percent and the graphene oxide powder of the non-surface modification of 0.9 % is added in lubricating oil, stirs a hour.
Storage stability is tested
Obtained target product is stood 15 days, 30 days, the situation of object observing product.
By experiment, by after 15 days, obvious layering of reuniting is occurred in that in the lubricating oil that with the addition of the Graphene lube oil additive being surface-treated, and with the addition of the lubricating oil of surface treated Graphene lube oil additive, even across 30 days afterwards, still can not observe and substantially reunite or be layered with stable dispersion.
The embodiment 1-6 of table 1 and comparative example's 1-2 storage stability performance tables
Anti-attrition energy-conservation performance test
By four-ball tester and gear testing machine come the anti-attrition energy-efficient performance of test target product.
As shown in table 2, found by experiment, when the mass percent of surface-treated Graphene is 0.1-0.6 %, the anti-attrition energy-saving effect of lubricating oil is best.
Table 2
Particular embodiments described above; the purpose of the present invention, technical scheme and beneficial effect are further described; it should be understood that; the foregoing is only specific embodiment of the invention; it is not intended to limit the invention; all any modification, equivalent substitution and improvements within the spirit and principles in the present invention, done etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification, graphene oxide containing nitrogen-containing compound surface modification, the thickness of the graphene oxide of the nitrogen-containing compound surface modification is 0.17-1.4 nm, piece footpath size is 10-1000nm, and the mass percent in lubricating oil is 0.01-0.9 %.
2. the lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification according to claim 1, wherein mass percent of the Graphene of the nitrogen-containing compound surface modification in the lubricating oil is 0.1-0.6 %.
3. the lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification according to claim 1, the reagent for wherein performing the nitrogen-containing compound surface modification is selected from the chain alkyl amine that carbon number is 4-16, and the compound with amide groups, imide, glucose amido, pyrrole radicals or pyridine radicals.
4. the lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification according to claim 1, wherein the reagent for performing the nitrogen-containing compound surface modification is ethylenediamine, hexamethylene diamine, acetamide or galactosamine.
5. the lube oil additive of the graphene oxide based on nitrogen-containing compound surface modification according to claim 1, wherein the lubricating oil is automobile oil.
6. a kind of lubricating oil of the graphene oxide based on nitrogen-containing compound surface modification, comprising the lube oil additive just like the graphene oxide based on nitrogen-containing compound surface modification described in claim 1 to 5 any one.
7. application of the lube oil additive of a kind of graphene oxide based on nitrogen-containing compound surface modification as described in claim 1 to 5 any one in automobile oil.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107706431A (en) * | 2017-09-26 | 2018-02-16 | 西南大学 | Preparation method of graphene support Pt nano-particle catalysts and products thereof and application |
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| CN101812351A (en) * | 2010-04-01 | 2010-08-25 | 江苏工业学院 | Lubricating oil additive based on single-layer or more-layer graphene |
| CN103450967A (en) * | 2013-08-16 | 2013-12-18 | 上海应用技术学院 | Oil-soluble nano-graphite and preparation method and application thereof |
| CN104031716A (en) * | 2013-03-06 | 2014-09-10 | 安炬科技股份有限公司 | Graphene-containing lubricating oil |
| CN104109569A (en) * | 2013-04-22 | 2014-10-22 | 安炬科技股份有限公司 | Graphite nanosheet-containing lubricating oil |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101812351A (en) * | 2010-04-01 | 2010-08-25 | 江苏工业学院 | Lubricating oil additive based on single-layer or more-layer graphene |
| CN104031716A (en) * | 2013-03-06 | 2014-09-10 | 安炬科技股份有限公司 | Graphene-containing lubricating oil |
| CN104109569A (en) * | 2013-04-22 | 2014-10-22 | 安炬科技股份有限公司 | Graphite nanosheet-containing lubricating oil |
| CN103450967A (en) * | 2013-08-16 | 2013-12-18 | 上海应用技术学院 | Oil-soluble nano-graphite and preparation method and application thereof |
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| CN107706431A (en) * | 2017-09-26 | 2018-02-16 | 西南大学 | Preparation method of graphene support Pt nano-particle catalysts and products thereof and application |
| CN107706431B (en) * | 2017-09-26 | 2020-04-14 | 西南大学 | Preparation method of graphene supported Pt nanoparticle catalyst, product and application thereof |
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