CN108117913B - Preparation method and application of spherical graphene lubricating additive - Google Patents

Preparation method and application of spherical graphene lubricating additive Download PDF

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CN108117913B
CN108117913B CN201611065350.1A CN201611065350A CN108117913B CN 108117913 B CN108117913 B CN 108117913B CN 201611065350 A CN201611065350 A CN 201611065350A CN 108117913 B CN108117913 B CN 108117913B
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graphene
spherical
spherical graphene
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CN108117913A (en
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曾尤
王函
薛伟海
佟钰
英哲
张藤心
成会明
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Institute of Metal Research of CAS
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/02Carbon; Graphite
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/16Solid spheres
    • C08K7/18Solid spheres inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/08Ingredients agglomerated by treatment with a binding agent
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04Elements
    • C10M2201/041Carbon; Graphite; Carbon black
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2070/00Specific manufacturing methods for lubricant compositions

Abstract

The invention relates to the application field of graphene materials, in particular to a preparation method and application of a spherical graphene lubricating additive. Graphene or graphene oxide is used as a raw material, a graphene solution dispersion system with excellent dispersion stability is obtained through mechanical crushing or ultrasonic shearing and a centrifugal separation process, spherical graphene is obtained through a spray drying method, and reduced graphene oxide spheres are obtained through reduction treatment of graphene spheres prepared from graphene oxide. The spherical graphene can be used as a lubricating additive to be directly dispersed in lubricating oil, lubricating grease or a polymer matrix, and a high-performance graphene modified lubricating product can be obtained through simple mechanical stirring or manual oscillation. Therefore, the graphene lubricating oil/grease or graphene modified polymer composite material with good dispersion stability can be obtained by adding the spherical graphene, and the tribological performance of the graphene modified polymer composite material can be obviously improved by adding the spherical graphene.

Description

Preparation method and application of spherical graphene lubricating additive
Technical Field
The invention relates to the application field of graphene materials, in particular to a preparation method and application of a spherical graphene lubricating additive.
Background
Graphene, as a novel carbon material, has received extensive attention from the scientific and industrial fields since its unique planar two-dimensional structure and excellent physicochemical properties. The graphene has extremely high mechanical strength (the strength is as high as 1TPa), excellent interlayer shear slip performance, stable chemical properties and good environmental inertness, and is an ideal lubricating material. The wear-resistant and antifriction performance of the material can be remarkably improved by adding the graphene into the lubricating oil/grease or polymer composite material.
In recent years, based on the excellent tribological characteristics of graphene, a novel graphene-based lubricating material has become a research focus of people's attention, and a large number of graphene lubricating products are produced accordingly. However, graphene does not exhibit a very outstanding wear-resistant antifriction modifying effect in these lubricating systems (lubricating oils/greases, polymer composites, etc.). This is mainly due to the large specific surface area, large aspect ratio, high surface energy, high tendency to agglomerate, and the fact that graphene cannot exist in a fully extended two-dimensional lamellar structure in a lubricant/grease or polymer matrix, but rather exists in the form of irregular agglomerates. The irregular morphology of graphene in the lubricating oil/grease or polymer matrix affects the dispersion stability of graphene in the lubricating oil matrix or the dispersion uniformity of the lubricating grease and the polymer matrix, and seriously affects the comprehensive tribological performance of the graphene/lubricating oil (grease) or graphene/polymer composite material due to the existence of the irregular morphology. Therefore, graphene as a lubricating additive cannot fully show excellent tribological properties of the graphene in the using process, the wear-resisting and friction-reducing properties of the corresponding graphene modified lubricating oil/grease or graphene modified polymer composite material are not remarkably improved, and the quality stability of the corresponding related product is greatly influenced, so that the industrial production application of the graphene as the lubricating additive is restricted.
The morphological structure of graphene in a lubricating oil/grease or polymer matrix directly influences the tribological properties of graphene modified lubricating grease and graphene modified polymer composite materials. In order to improve the dispersion stability of graphene in a lubricating oil/grease or polymer matrix and the tribological performance of graphene as a lubricating additive, graphene is usually chemically or physically modified, and an alkane chain is grafted on the surface of the graphene to improve the compatibility of the graphene in the lubricating oil/grease, so that a graphene/lubricating oil (grease) system with good dispersion stability is obtained. Or, the chemical surface treatment is carried out on the graphene to improve the compatibility of the graphene and the polymer matrix, so that the graphene is more easily dispersed in the polymer matrix. However, although the compatibility of graphene and a composite matrix can be improved to a certain extent by a chemical modification method, the problems that the graphene structure is easily damaged and the tribological performance of graphene is affected, the treatment method is complex and difficult to realize industrial application, and the chemical reagent volatilizes to cause environmental pollution exist. Therefore, how to improve the compatibility of the graphene with a lubricating medium by regulating the morphological structure and the surface property of the graphene is a technical key for obtaining the graphene lubricating additive with a uniform dispersion system and excellent wear-resistant and antifriction properties.
Disclosure of Invention
The invention aims to provide a preparation method and application of a spherical graphene lubricating additive which is suitable for lubricating oil/grease or polymer composite materials and can obviously improve the wear-resisting and friction-reducing performance of the materials.
In order to achieve the technical aim, the technical scheme provided by the invention is as follows:
a preparation method of a spherical graphene lubricant additive comprises the following steps:
(1) taking graphene or graphene oxide as a raw material, and carrying out particle size adjustment on the graphene raw material through a mechanical crushing or ultrasonic shearing and centrifugal separation process;
(2) adding a surfactant and stirring to obtain a solution system with stable dispersion;
(3) and obtaining the spherical graphene powder material or the spherical graphene oxide powder material by a spray drying method.
In the preparation method of the spherical graphene lubricant additive, in the step (1), the graphene is prepared by a catalytic intercalation expansion stripping method, a graphite oxidation reduction method, a chemical vapor deposition method, an epitaxial growth method and a mechanical stripping method.
According to the preparation method of the spherical graphene lubricant additive, in the step (1), when mechanical crushing equipment is adopted for particle size adjustment, a moving part is in a paddle shape, the operating speed is 5000-25000 rpm, and the processing time is 30-120 min.
In the preparation method of the spherical graphene lubricant additive, in the step (1), when an ultrasonic shearing device is adopted for particle size adjustment, a dispersion medium is water or an ethanol solution with the concentration of 10 wt% -100 wt%, the dispersion concentration of graphene is 0.1 mg/ml-15 mg/ml, the dispersion concentration of graphene oxide is 0.1 mg/ml-3 mg/ml, the operating power is 500-1500W, and the working time is 10-180 min.
The preparation method of the spherical graphene lubricant additive comprises the step (1), wherein a high-speed centrifuge is adopted for centrifugal separation, the rotating speed is 1000-12000 rpm, the working time is 30-180 min, the size of the obtained separated graphene is 0.1-20 mu m, and the number of layers is 1-10.
The preparation method of the spherical graphene lubricant additive comprises the step (2), wherein the obtained solution system with stable dispersion is obtained, the dispersion medium is water or an ethanol solution with the concentration of 0.1-10 wt%, the dispersion concentration of graphene is 0.05-12 mg/ml, the dispersion concentration of graphene oxide is 0.05-3 mg/ml, the dispersing agent is N-methyl-pyrrole compounds, sodium dodecyl benzene sulfonate, polyvinylpyrrolidone or a surfactant capable of dispersing graphene in a polar solvent, and the dosage of the dispersing agent is 0-2%.
In the step (3), the spherical graphene or spherical graphene oxide powder material is obtained by a spray drying method, the inlet temperature of a dryer is controlled to be 90-220 ℃, the outlet temperature is controlled to be 60-100 ℃, the drying rate is 10-1000 ml/h, the fan strength is controlled to be 50-100, and the particle size of the obtained spherical graphene or spherical graphene oxide is 500-15 mu m.
The application of the spherical graphene lubricating additive prepared by the method is as follows:
(1) reducing a spherical graphene oxide powder material prepared by taking graphene oxide as a raw material to obtain a reduced graphene oxide ball;
(2) and dispersing the spherical graphene powder material in a lubricating oil/grease or polymer matrix to obtain the spherical graphene modified lubricating oil/grease or spherical graphene modified polymer composite material.
The application of the spherical graphene lubricant additive is that spherical graphene oxide powder materials obtained by spray drying of graphene oxide serving as a raw material are reduced in a heat treatment mode, the high-temperature treatment temperature is 300-1000 ℃, and the treatment time is 1-5 hours.
The application of the spherical graphene lubricating additive is that spherical graphene powder materials are directly dispersed in lubricating oil base oil/grease or finished oil/grease; or, dispersing the spherical graphene powder material in the lubricating oil base oil/grease or finished product oil/grease by adding a surfactant, wherein the addition content of the surfactant is 0-30%; or, the spherical graphene powder material is directly dispersed in the polymer matrix;
the preparation method of the composite material is a melt blending method or a solution method, and the addition amount of the spherical graphene powder material is 0.1-3 wt%.
The design idea of the invention is as follows:
based on the defects of the traditional graphene lubricating additive, such as: the dispersion stability of the graphene is poor, the structural morphology of the graphene in a matrix is irregular and uncontrollable, the tribological performance of the graphene is not remarkable, and the like. The invention provides a preparation method of a high-performance graphene lubricant additive, which is characterized in that a graphene solution with uniform and controllable size and particle size distribution is obtained by technical means of mechanical crushing, ultrasonic shearing, ultrasonic dispersion and centrifugal classification, a graphene solution dispersion system with excellent dispersion stability is obtained by adding a dispersing agent such as a surfactant, and spherical graphene is obtained by a spray drying or atomization drying method. The spherical graphene can be uniformly dispersed in a lubricating oil/grease and polymer composite material matrix, has good chemical stability, and can play a role in resisting wear and reducing friction in a rolling and elastic deformation mode in a friction process. The spherical graphene and the flake graphene are different from the traditional flake graphene lubricating additive, are not easy to be adhered together, and are easy to be dispersed in a lubricating oil/grease or polymer matrix. In addition, the spherical graphene lubricating additive plays a friction reducing role in a rolling friction mode initially in the friction process, and can greatly reduce the friction coefficient of the lubricating oil/grease or polymer composite material. And then under the action of a large external load (for lubricating oil/grease, under an extreme pressure environment), the spherical graphene has good elastic deformation capacity, and the anti-wear and anti-wear effects of the material can be further improved. When the shearing force is too large, the spherical graphene is subjected to sheet peeling, and acts in a lubrication mode of the flaky nano graphene sheet. By adding the spherical graphene lubricating additive, the friction coefficient of the lubricating oil can be reduced by 80%, the diameter of the wear-resistant spot can be reduced by 50%, and the wear-resistant and antifriction properties of the lubricating oil/grease or polymer composite material can be remarkably improved. In addition, the preparation method of the spherical graphene lubricant additive has the technical characteristics of simple process, good repeatability, obvious application effect and the like, and is suitable for large-scale industrial production.
The invention has the advantages and beneficial effects that:
1. the invention provides a preparation method of a high-performance graphene lubricant additive, which is characterized in that a graphene solution with uniform and controllable size and particle size distribution is obtained by technical means of mechanical crushing, ultrasonic shearing, ultrasonic dispersion and centrifugal classification, a graphene solution dispersion system with excellent dispersion stability is obtained by adding a dispersing agent such as a surfactant, and spherical graphene is obtained by a spray drying or atomization drying method.
2. The invention provides a design idea that graphene has a spherical structure and plays a role in wear resistance and friction reduction in a lubricating medium by regulating and controlling the structural form of the graphene. The spherical graphene can be uniformly dispersed in a lubricating oil/grease and polymer composite material matrix, has good chemical stability, and can play a role in resisting wear and reducing friction in a rolling and elastic deformation mode in a friction process. The spherical graphene lubricating additive is remarkably different from the traditional flaky graphene lubricating additive, and the spherical graphene lubricating additive plays a friction reducing role in a rolling friction mode initially in the friction process, so that the friction coefficient of lubricating oil/grease or polymer composite material can be greatly reduced. And then under the action of a large external load (for lubricating oil/grease, under an extreme pressure environment), the spherical graphene has good elastic deformation capacity, and the anti-wear and anti-wear effects of the material can be further improved. When the shearing force is too large, the spherical graphene is subjected to lamellar exfoliation, and the spherical graphene acts in a lubrication mode of the flaky nano graphene sheet.
Drawings
Fig. 1 is a scanning electron micrograph of a spherical graphene lubricant additive.
FIG. 2 is a photograph of a friction coefficient curve of a spherical graphene lubricant additive added to a lubricant base oil, wherein the content of the added graphene is 0.1 mg/ml. In the figure, 1-Base oil represents a lubricant Base oil; 2-pristine graphene/oil represents graphene raw material/base oil; 3-Graphene ball/oil stands for spherical Graphene/base oil. The abscissa Time is the Time(s) and the ordinate frictioning coefficient is the coefficient of Friction.
Detailed Description
In the specific implementation process, the preparation method and the application of the spherical graphene lubricant additive are as follows:
(1) the method comprises the steps of carrying out particle size adjustment on a graphene raw material through a mechanical crushing or ultrasonic shearing and centrifugal separation process, wherein when mechanical crushing equipment is adopted for particle size adjustment, a moving part is in a paddle shape, the operating speed is 5000-25000 rpm, and the processing time is 30-120 min. When an ultrasonic shearing device is adopted for particle size adjustment, a graphene dispersion medium is water or an ethanol solution with the concentration of 10 wt% -100 wt%, the graphene dispersion concentration is 0.1 mg/ml-15 mg/ml, the graphene oxide dispersion concentration is 0.1 mg/ml-3 mg/ml, the operation power is 500-1500W, and the effective working time is 10-180 min. When a centrifugal separation device is adopted for particle size adjustment, the rotating speed is 1000-12000 rpm, the working time is 30-180 min, the size of the obtained separated graphene sheet layer is 0.1-20 mu m, and the number of the obtained graphene sheets is 1-10.
(2) A solution system with stable graphene dispersion is obtained by adding a surfactant and stirring, wherein a dispersion medium is water or an ethanol solution with the concentration of 0.1-10 wt%, the dispersion concentration of graphene is 0.05-12 mg/ml, the dispersion concentration of graphene oxide is 0.05-3 mg/ml, a dispersing agent is N-methyl-pyrrole compound (ketonic), sodium dodecyl benzene sulfonate, polyvinylpyrrolidone or a common anionic surfactant and the like which can be used for dispersing graphene in a polar solvent, and the dosage of the dispersing agent is 0-2%.
(3) Obtaining a spherical graphene powder material by a spray drying method; the inlet temperature of the dryer is controlled to be 90-220 ℃, the outlet temperature is controlled to be 60-100 ℃, the drying rate is 10-1000 ml/h, and the strength of the fan is controlled to be 50-100.
(4) Reducing spherical graphene prepared by taking graphene oxide as a raw material to obtain reduced graphene oxide spheres, wherein the high-temperature treatment temperature is 300-1000 ℃, and the treatment time is 1-5 hours.
(5) The method comprises the steps of dispersing spherical graphene in a lubricating oil/grease or polymer matrix to obtain a spherical graphene modified lubricating oil/grease or spherical graphene modified polymer composite material, wherein the spherical graphene can be directly dispersed in lubricating oil base oil/grease or finished oil/grease, or can be dispersed in the lubricating oil base oil/grease or finished oil/grease by adding surfactants such as oleic acid and span80, the addition content of the surfactants is more than 0-30%, the spherical graphene can be directly dispersed in the polymer matrix, and the preparation method of the graphene/polymer composite material can be a melt blending method or a solution method.
The invention is further illustrated, but is not limited, by the following examples:
example 1
In this embodiment, the specific process and process parameters for preparing the spherical graphene lubricant additive are as follows:
(1) graphene prepared by a redox method is selected as a raw material, and is crushed by a universal mechanical crusher at the rotating speed of 9000rpm for 60 min. Dispersing the crushed graphene into water with the concentration of 2mg/ml, and performing ultrasonic dispersion and crushing treatment on the graphene solution by using a cell crushing ultrasonic machine with the operation power of 1000W for 120 min. And (3) carrying out centrifugal separation treatment on the solution after ultrasonic treatment, wherein the rotating speed of a centrifugal machine is 9000rpm, the working time is 30min, and selecting the graphene solution with the lamella size of 8-15 microns after separation.
(2) And carrying out surfactant modification water dispersion treatment on the graphene solution system, selecting polyvinylpyrrolidone (PVP) as a surfactant, adding the PVP into the graphene solution, and preparing the graphene aqueous solution with the PVP addition of 0.1 wt% and the graphene concentration of 0.1mg/ml and good dispersion stability.
(3) The spherical graphene powder material is obtained by a spray drying method, the inlet temperature of a dryer is controlled at 90 ℃, the outlet temperature of the dryer is controlled at 70 ℃, the drying rate is 100ml/h, and the strength of a fan is controlled at 80.
As shown in fig. 1, it can be seen from the scanning electron micrograph of the graphene lubricant additive that spherical graphene with a diameter of 1 μm can be obtained by spray drying, and the spherical graphene has the characteristics of smooth and round surface and uniform size distribution.
(4) And dispersing the spherical graphene in the lubricating oil base oil to obtain the spherical graphene modified lubricating oil, wherein the addition amount of the spherical graphene is 0.1 mg/ml. Through tribology tests, the friction coefficient of the modified lubricating oil is reduced by 70% compared with that of the base oil, and the diameter of the wear scar is reduced by 47.6%, as shown in figure 2.
Example 2
The difference from embodiment 1 is that, in this embodiment, the specific process and process parameters for preparing the spherical graphene lubricant additive are as follows:
(1) graphene prepared by a redox method is selected as a raw material, and is crushed by a universal mechanical crusher at the rotation speed of 10000rpm for 45 min. Dispersing the crushed graphene into water with the concentration of 4mg/ml, and performing ultrasonic dispersion and crushing treatment on the graphene solution by using a cell crushing ultrasonic machine with the operation power of 1200W for 150 min. And (3) carrying out centrifugal separation treatment on the solution after ultrasonic treatment, wherein the rotating speed of a centrifugal machine is 9000rpm, the working time is 60min, and selecting the graphene solution with the lamella size of 10-12 microns after separation.
(2) And carrying out surfactant modification water dispersion treatment on the graphene solution system, selecting PVP (polyvinyl pyrrolidone) as a surfactant, adding the PVP into the graphene solution, and preparing the graphene aqueous solution with the PVP addition of 0.2 wt% and the graphene concentration of 0.2mg/ml and good dispersion stability.
(3) The spherical graphene powder material is obtained by a spray drying method, the inlet temperature of a dryer is controlled at 100 ℃, the outlet temperature of the dryer is controlled at 80 ℃, the drying rate is 50ml/h, and the strength of a fan is controlled at 100.
(4) And dispersing the spherical graphene in the lubricating grease to obtain the spherical graphene modified lubricating grease, wherein the addition amount of the spherical graphene is 0.1 mg/ml. Through tribology tests, the friction coefficient of the modified lubricating grease can be reduced by 50% compared with that of the base grease, and the diameter of the wear scar can be reduced by 30%, as shown in figure 2.
The embodiment result shows that the spherical graphene lubricating additive obtained by the spray drying method has the characteristics of good dispersibility and remarkable wear-resistant and friction-reducing effects, can be directly added into lubricating oil/grease or polymer composite materials when in use, and can be used for obtaining a graphene modified product with excellent wear-resistant and friction-reducing properties through a simple mechanical mixing mode. According to the invention, the graphene lubricating oil/grease or graphene modified polymer composite material with good dispersion stability can be obtained by adding the spherical graphene, and the addition of the spherical graphene can obviously improve the tribological performance of the lubricating oil/grease or graphene modified polymer composite material. The preparation method of the spherical graphene additive provided by the invention has the technical characteristics of simple process, good repeatability, obvious application effect and the like.

Claims (5)

1. A preparation method of a spherical graphene lubricant additive is characterized by comprising the following steps:
(1) taking graphene or graphene oxide as a raw material, and carrying out particle size adjustment on the graphene raw material through a mechanical crushing or ultrasonic shearing and centrifugal separation process;
in the step (1), a high-speed centrifuge is adopted for centrifugal separation, the rotating speed is 1000-12000 rpm, the working time is 30-180 min, the size of the obtained separated graphene is 0.1-20 mu m, and the number of layers is 1-10;
(2) adding a surfactant and stirring to obtain a solution system with stable dispersion;
(3) obtaining a spherical graphene powder material or a spherical graphene oxide powder material by a spray drying method;
in the step (3), the spherical graphene or spherical graphene oxide powder material is obtained by a spray drying method, the inlet temperature of a dryer is controlled to be 90-220 ℃, the outlet temperature is controlled to be 60-100 ℃, the drying rate is 10-1000 ml/h, the fan intensity is controlled to be 50-100, and the particle size of the obtained spherical graphene or spherical graphene oxide is 500 nm-15 mu m.
2. The method for preparing the spherical graphene lubricant additive according to claim 1, wherein in the step (1), the graphene is prepared by a catalytic intercalation expansion exfoliation method, a graphite oxidation reduction method, a chemical vapor deposition method, an epitaxial growth method and a mechanical exfoliation method.
3. The preparation method of the spherical graphene lubricant additive according to claim 1, wherein in the step (1), when mechanical crushing equipment is adopted for particle size adjustment, the moving part is in a paddle shape, the operating speed is 5000-25000 rpm, and the processing time is 30-120 min.
4. The preparation method of the spherical graphene lubricant additive according to claim 1, wherein in the step (1), when an ultrasonic shearing device is adopted for particle size adjustment, the dispersion medium is water or an ethanol solution with a concentration of 10 wt% -100 wt%, the dispersion concentration of graphene is 0.1 mg/ml-15 mg/ml, the dispersion concentration of graphene oxide is 0.1 mg/ml-3 mg/ml, the operation power is 500-1500W, and the working time is 10-180 min.
5. The method for preparing a spherical graphene lubricant additive according to claim 1, wherein in the step (2), the dispersion-stable solution system is obtained, the dispersion medium is water or an ethanol solution with a concentration of 0.1 wt% to 10 wt%, the graphene dispersion concentration is 0.05mg/ml to 12mg/ml, the graphene oxide dispersion concentration is 0.05mg/ml to 3mg/ml, the surfactant is an N-methyl-pyrrole compound, sodium dodecylbenzene sulfonate or polyvinylpyrrolidone, and the amount of the surfactant is more than 0 and not more than 2 wt%.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101993065A (en) * 2010-12-17 2011-03-30 中国科学院上海微***与信息技术研究所 Method for preparing graphene powder
CN104009205A (en) * 2014-06-12 2014-08-27 上海中聚佳华电池科技有限公司 Hollow graphene ball and preparation method and application thereof
WO2014189065A1 (en) * 2013-05-20 2014-11-27 国立大学法人岡山大学 Water-based lubricant
CN104342236A (en) * 2014-09-29 2015-02-11 广东东莞市天润电子材料有限公司 Graphene-containing frictional regulator and preparation method thereof
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
CN105217622A (en) * 2015-11-13 2016-01-06 武汉大学 A kind of preparation method of controlled three-dimensional grapheme microballoon

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101993065A (en) * 2010-12-17 2011-03-30 中国科学院上海微***与信息技术研究所 Method for preparing graphene powder
WO2014189065A1 (en) * 2013-05-20 2014-11-27 国立大学法人岡山大学 Water-based lubricant
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
CN104009205A (en) * 2014-06-12 2014-08-27 上海中聚佳华电池科技有限公司 Hollow graphene ball and preparation method and application thereof
CN104342236A (en) * 2014-09-29 2015-02-11 广东东莞市天润电子材料有限公司 Graphene-containing frictional regulator and preparation method thereof
CN105217622A (en) * 2015-11-13 2016-01-06 武汉大学 A kind of preparation method of controlled three-dimensional grapheme microballoon

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Self-dispersed crumpled graphene balls in oil for friction and wear reduction;Xuan Dou et al.;《PANS》;20160209;第113卷(第6期);第1528-1533页 *
Size distribution-controlled preparation of graphene oxide nanosheets with different C/O ratios;Jianli Chen et al.;《Materials Chemistry and Physics》;20131231;第139卷;第8-11页 *

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