CN108485753B - Graphene-based nano borate lubricating oil and preparation method thereof - Google Patents

Graphene-based nano borate lubricating oil and preparation method thereof Download PDF

Info

Publication number
CN108485753B
CN108485753B CN201810480598.7A CN201810480598A CN108485753B CN 108485753 B CN108485753 B CN 108485753B CN 201810480598 A CN201810480598 A CN 201810480598A CN 108485753 B CN108485753 B CN 108485753B
Authority
CN
China
Prior art keywords
graphene
based nano
borate
lubricating oil
parts
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201810480598.7A
Other languages
Chinese (zh)
Other versions
CN108485753A (en
Inventor
陈文志
陈艺勇
林志峰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xiamen 6c Technology Co ltd
Original Assignee
Xiamen 6c Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xiamen 6c Technology Co ltd filed Critical Xiamen 6c Technology Co ltd
Priority to CN201810480598.7A priority Critical patent/CN108485753B/en
Publication of CN108485753A publication Critical patent/CN108485753A/en
Application granted granted Critical
Publication of CN108485753B publication Critical patent/CN108485753B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • C10M139/00Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing atoms of elements not provided for in groups C10M127/00 - C10M137/00
    • 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
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04Mixtures of base-materials and additives
    • C10M169/045Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution and non-macromolecular compounds
    • 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
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
    • 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
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102Aliphatic fractions
    • C10M2203/1025Aliphatic fractions used as base material
    • 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/287Partial esters
    • C10M2207/289Partial esters containing free hydroxy groups
    • 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
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/08Amides
    • 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
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/086Imides
    • 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
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
    • 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
    • C10M2227/00Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/06Organic compounds derived from inorganic acids or metal salts
    • 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
    • C10M2227/00Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/06Organic compounds derived from inorganic acids or metal salts
    • C10M2227/066Organic compounds derived from inorganic acids or metal salts derived from Mo or W
    • 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
    • C10N2030/02Pour-point; Viscosity index
    • 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
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/10Inhibition of oxidation, e.g. anti-oxidants
    • 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
    • C10N2030/64Environmental friendly compositions

Abstract

The invention provides graphene-based nano borate lubricating oil and a preparation method thereof, and relates to the technical field of lubricating oil. The preparation method comprises the steps of mixing and dispersing one or more of graphene-based calcium hexadecylborate, graphene-based nano lanthanum borate and graphene-based nano cerium borate with base oil to obtain a first mixture. Then, the ashless dispersant, the succinimide, the amine antioxidant and the amide solvent are added and mixed to obtain a second mixture. And then heating to 70-80 ℃, stirring for 2-4 h, then sequentially adding a viscosity index improver, a composite additive and a defoaming agent, continuing to heat and stir for 2-4 h after the addition is finished, and then performing ultrasonic dispersion and filtration to obtain the graphene-based nano borate lubricating oil. The preparation method is simple and the reaction temperature is low. The prepared lubricating oil has low friction coefficient, long service life, controllable product and strong wear resistance.

Description

Graphene-based nano borate lubricating oil and preparation method thereof
Technical Field
The invention relates to the technical field of lubricating oil, and particularly relates to graphene-based nano borate lubricating oil and a preparation method thereof.
Background
Lubricating oil is an indispensable material for machine operation, and plays a very important role in maintaining the operation of a mechanism and improving the machine life. With the development of science and technology, the requirements on the service life and the operating environment of a mechanism are more and more strict, and lubricating oil is required to have excellent comprehensive performance, such as strong dynamic property, energy conservation, environmental protection and good lubricating coefficient.
In recent years, researches on graphene and composite materials thereof become hot spots, the special structure of the graphene determines that the graphene has good mechanical property, wear resistance and pressure resistance, high specific surface area and the like, and the two-dimensional structure of the graphene and corresponding nano materials can be used for preparing high-performance lubricating oil.
Disclosure of Invention
The invention aims to provide a preparation method of graphene-based nano borate lubricating oil, which is simple, reacts at a lower temperature, is energy-saving and environment-friendly, and is suitable for industrial large-scale production.
The invention also aims to provide the graphene-based nano borate lubricating oil which takes the graphene-based nano borate as a basic substance of an antiwear agent material and has excellent performance.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of graphene-based nano borate lubricating oil, which comprises the following steps:
s1, mixing and dispersing graphene-based nano borate and base oil to obtain a first mixture, wherein the graphene-based nano borate is selected from one or more of graphene-based hexadecyl calcium borate, graphene-based nano lanthanum borate and graphene-based nano cerium borate;
s2, adding an ashless dispersant, succinimide, an amine antioxidant and an amide solvent into the first mixture, and mixing to obtain a second mixture;
s3, heating the second mixture to 70-80 ℃, stirring for 2-4 hours, then sequentially adding the viscosity index improver, the composite additive and the defoaming agent, continuing heating and stirring for 2-4 hours after the addition is finished, and then performing ultrasonic dispersion and filtration to obtain the graphene-based nano borate lubricating oil.
The invention provides graphene-based nano borate lubricating oil which is prepared by the preparation method.
The graphene-based nano borate lubricating oil and the preparation method thereof have the beneficial effects that:
according to the invention, the graphene-based nano borate is used as an anti-wear material of the lubricating oil, the nano borate particles have very strong anti-wear performance, the graphene and the nano borate are compounded to obtain the graphene-based nano borate, and borate groups are introduced to the graphene, so that the dispersion of the graphene and the improvement of the anti-wear performance are facilitated. Meanwhile, the graphene-based nano borate is used as an anti-wear and anti-pressure material, so that the use of traditional anti-wear agents such as sulfur, phosphorus and the like can be reduced, corrosion to friction pair materials and the like can not occur, and the service life is long. In the production process, the production of waste water, waste gas and the like is reduced, and the environment is protected.
During the preparation, the different additions are added in steps. Proper amount of dispersant, amine antioxidant, etc. are added and mixed to ensure the dispersing effect of graphene base nanometer borate and raise the antiwear, antioxidant and other performance of lubricating oil. And other additives such as a viscosity index improver and the like are added, so that the viscosity of the lubricating oil is increased, and the dispersion stability of the graphene-based nano borate is facilitated. Various additives are compounded with the graphene-based nano borate for use, so that the performance of the lubricating oil is further improved. In the preparation process, the reaction temperature is low, various parameters are easy to control, and the product is controllable.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a process flow diagram of a preparation method of graphene-based nano borate lubricating oil according to an embodiment of the present invention;
fig. 2 is a diagram of an apparatus for preparing the graphene-based nano borate lubricant according to the present embodiment.
Icon: 1-an electric stirrer; 2-reflux condenser tube; 3-reaction flask; 4-heating device.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The graphene-based nano borate lubricating oil and the preparation method thereof according to the embodiments of the present invention will be specifically described below.
The embodiment of the invention provides a preparation method of graphene-based nano borate lubricating oil, which comprises the following steps:
and S1, mixing and dispersing the graphene-based nano borate and the base oil to obtain a first mixture. The graphene-based nano borate is selected from one or more of graphene-based hexadecyl calcium borate, graphene-based nano lanthanum borate and graphene-based nano cerium borate.
Further, in a preferred embodiment of the present invention, the graphene nano borate is 0.002 to 0.1 part by weight, and the base oil is 80 to 90 parts by weight. Further preferably, the graphene nano borate is 0.005-0.035 parts.
It is understood that, in the present embodiment, the base oil may be one or more selected from mineral oils, hydrocarbon-based synthetic oils, ester-based oils, and ether-based oils. Preferably, in this embodiment, the base oil is commercially available API group ii base oil, which has few impurities and good thermal stability and oxidation resistance.
Further, in the embodiment, the graphene-based nano borate comprises, by weight, 0.001 to 0.01 parts of graphene-based hexadecyl calcium borate, 0.002 to 0.005 parts of graphene-based nano lanthanum borate, and 0.001 to 0.03 parts of graphene-based nano cerium borate. The inventor researches and discovers that the friction coefficient of the lubricating oil can be controlled by adjusting the dosage ratio of the graphene-based nano borate. When 0.01 part of graphene-based hexadecyl calcium borate, 0.005 part of graphene-based nano lanthanum borate and 0.001 part of graphene-based nano cerium borate are used, the wear resistance of the lubricating oil is optimal.
Further, in the embodiment of the invention, the graphene-based nano borate is obtained by a low-temperature plasma method. For example, the graphene-based nano borate is prepared by the following preparation method:
(1) providing a chemical vapor deposition device with a radio frequency matcher, andthe substrate is placed in the reaction chamber of the apparatus and evacuated to 2 x 10-4Pa, and keeping for 30 min. Then heating to 400 ℃, and introducing H2Keeping for 40 min;
(2) starting the radio frequency matcher with the power of 200W and the voltage of 1.2KV, and then introducing carbon source gas (CH)4CO, etc.) 100sccm and Ar gas 50sccm, and reacting for 15 min;
(3) stopping heating, closing the radio frequency matcher, and taking out the substrate with the graphene deposited on the surface after the temperature is reduced to room temperature under the protection of Ar gas;
(4) annealing the substrate in the step (3) in a vacuum tube furnace, wherein the annealing temperature is 380 ℃ and the time is 20min, and after cooling to room temperature, scraping out the film powder on the substrate to obtain graphene;
(5) dispersing 10 parts by weight of graphene in 100 parts by weight of N, N-dimethylformamide, adding 0.1 part by weight of 3-aminopropyltriethoxysilane and 50 parts by weight of hexadecyl nano calcium borate or nano cerium borate or nano lanthanum borate, and stirring and mixing to obtain a mixed solution;
(6) and heating the mixed solution to 180 ℃ in a heating reflux reaction device, carrying out reflux reaction for 6 hours, filtering and drying to obtain the graphene-based calcium hexadecylborate or the graphene-based nano cerium borate or the graphene-based nano lanthanum borate.
The graphene-based nano borate is obtained by adopting a low-temperature plasma method, is simple, efficient and energy-saving, and can improve the crystal quality and the dispersion performance of graphene through annealing treatment. Graphene and nano borate are compounded to obtain graphene-based nano borate, so that the lubricating oil has good dispersibility and can greatly improve the wear resistance and compression resistance of the lubricating oil.
Further, in the preferred embodiment of the present invention, in step S1, the mixing and dispersing process of the graphene-based nano borate and the base oil is as follows: stirring for 1-5 h under the condition of heat preservation at 70-90 ℃, and then ultrasonically dispersing for 1-3 h.
After obtaining the first mixture, the following steps are performed:
and S2, adding the ashless dispersant, the succinimide, the amine antioxidant and the amide solvent into the first mixture, and mixing to obtain a second mixture.
Further, the mixing process of the step is as follows: stirring for 1-5 h, and then ultrasonically dispersing for 1-3 h.
Further, the composition comprises, by weight, 1-2 parts of an ashless dispersant, 1-3 parts of succinimide, 1-2 parts of an amine antioxidant and 1-2 parts of an amide solvent.
The ashless dispersant can be selected from a commercial ashless dispersant T154 which is used as a dispersant of lubricating oil together with succinimide to prevent insoluble substances from suspending in the use process of oil products. The amine antioxidant can be selected from diphenylamine compounds (dioctyl diphenylamine, butyl octyl diphenylamine), p-diphenylamine compounds, etc. In this embodiment, the amide solvent is N, N-dimethylformamide or N, N-dimethylacetamide.
After obtaining the second mixture, the following steps are performed:
s3, heating the second mixture to 70-80 ℃, stirring for 2-4 hours, then sequentially adding the viscosity index improver, the composite additive and the defoaming agent, continuing heating and stirring for 2-4 hours after the addition is finished, and then performing ultrasonic dispersion and filtration to obtain the graphene-based nano borate lubricating oil.
In this example, the viscosity index improver and the defoaming agent were commercially available products. The viscosity index improver can improve the viscosity-temperature performance and the like of the lubricating oil, and in this embodiment, the viscosity index improver can be a commercially available viscosity index improver OCP or a viscosity index improver HSD.
Further, the viscosity index improver is 1-2 parts by weight, the composite additive is 1-5 parts by weight, and the defoaming agent is 1-2 parts by weight. The addition of the above additives to the lubricating oil can further improve the properties of the lubricating oil and further increase the sol stability.
Further, in the embodiment, the composite additive comprises, by weight, 80-90% of base oil, 3-8% of a corrosion inhibitor, 1-4% of a metal deactivator, 1-4% of an extreme pressure additive, 1-4% of a demulsifier, and 1-4% of copper oxide powder. Preferably, the composition of the base oil is the same as the base oil composition in step S1.
Furthermore, the corrosion inhibitor is selected from a sulfonate corrosion inhibitor or an ester corrosion inhibitor. The sulfonate realizes the corrosion inhibition effect through the adsorption and solubilization effects, and the ester compound can form an adsorption film with high hydrophobicity due to the cohesive force between lipophilic groups. In the embodiment, the preferable mass ratio of the petroleum sulfonate to the sorbitan oleate monoester is 1:2, and the petroleum sulfonate and the sorbitol oleate monoester are compounded to have good corrosion inhibition effect.
Further, the metal deactivator is a commercially available T551 or T552 metal deactivator; the extreme pressure additive may be selected from molybdate ester, organic borate ester, etc., preferably, in this embodiment, the extreme pressure additive is selected from molybdate ester, which has a very good antioxidant synergistic effect with amine antioxidant. The demulsifier is selected from commercially available Tl001, DL-32, KR-12, etc. The copper oxide powder is preferably nano copper oxide powder, and the addition of the nano copper oxide powder can improve the tribological performance under high-temperature and vibration conditions, increase the lubricity and reduce the abrasion.
Further, the preparation method of the composite additive comprises the following steps:
mixing base oil and copper oxide powder, performing ultrasonic treatment for 30min, sequentially adding a corrosion inhibitor, a metal deactivator and an extreme pressure additive, and performing ball milling for 1 h. And finally, adding the demulsifying agent, heating to 60 ℃, and stirring for 1.5 hours to obtain the composite additive.
The composite additive takes the base oil as a basic component, and then is added with other additive components such as a rust inhibitor, a metal deactivator and the like, so that the dispersion and mixing of various additives can be facilitated, and the integral stability of the lubricating oil can be facilitated after the composite additive is mixed with other components.
Further, the heating and stirring process of step S3 is carried out in a reflux reaction device with a stirrer, the stirring speed is 1000-4000 r/min, and the heating circulating reflux speed is 1-400 ml/h. More preferably, the stirring speed is 1500-2000 r/min, and the heating circulating reflux speed is 150-200 ml/h.
Further, in step S3, the filtering step is to filter out particles of 350 mesh or larger.
The embodiment of the invention also provides graphene-based nano borate lubricating oil which is prepared by the preparation method.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The graphene-based nano borate lubricating oil provided by the embodiment is prepared by the following steps:
(1) mixing 0.01 part of graphene-based calcium hexadecylborate, 0.005 part of graphene-based nano lanthanum borate, 0.001 part of graphene-based nano cerium borate and 85 parts of API II base oil, stirring at the temperature of 80 ℃ for 4 hours, and then ultrasonically dispersing for 2 hours to form a mixed solution.
(2) And (2) adding 1.5 parts of ashless dispersant, 2 parts of succinimide, 1.5 parts of amine antioxidant and 2 parts of N, N-dimethylformamide into the mixed solution obtained in the step (1), stirring for 3 hours, and then carrying out ultrasonic dispersion for 2 hours to form a mixed solution.
(3) The mixture obtained in (2) was placed in a reflux reaction apparatus (shown in FIG. 2) equipped with a stirrer, heated to 75 ℃ and stirred and heated for 2 hours. And sequentially adding 1.5 parts of viscosity index improver, 4 parts of composite additive and 1.5 parts of defoaming agent in the stirring process, continuing heating and stirring for 2 hours after the addition is finished, and then ultrasonically dispersing for 3 hours, and filtering to remove particles of more than 350 meshes to obtain the graphene-based nano borate lubricating oil. In the process, the heating and stirring speed is 1300r/min, and the heating circulating reflux speed is controlled to be about 180 ml/h.
The composite additive is prepared by the following method:
proportioning: 86% of API group II base oil, rust inhibitor: 6% of petroleum sulfonate and oleic acid sorbitol monoester, 2% of metal deactivator, 2% of extreme pressure additive, and the mass ratio of petroleum sulfonate to oleic acid sorbitol monoester is 1: 2: 2% of molybdate, 2% of demulsifier and 2% of nano copper oxide powder.
Mixing base oil and nano copper oxide powder, performing ultrasonic treatment for 30min, sequentially adding a corrosion inhibitor, a metal deactivator and an extreme pressure additive, and performing ball milling for 1 h. And finally, adding the demulsifying agent, heating to 60 ℃, and stirring for 1.5 hours to obtain the composite additive.
Example 2
The graphene-based nano borate lubricating oil provided in this example is different from that in example 1 in that:
(1) 0.001 part of graphene-based calcium hexadecylborate, 0.005 part of graphene-based nano lanthanum borate, 0.03 part of graphene-based nano cerium borate and 85 parts of API II base oil are mixed.
Example 3
The graphene-based nano borate lubricating oil provided in this example is different from that in example 1 in that:
(1) 0.001 part of graphene-based calcium hexadecylborate, 0.003 part of graphene-based nano cerium borate and 85 parts of API II base oil are mixed.
Example 4
The graphene-based nano borate lubricating oil provided in this example is different from that in example 1 in that:
the composite additive is prepared by the following method:
proportioning: 86% of API group II base oil, rust inhibitor: 6% of petroleum sulfonate and oleic acid sorbitol monoester, 2% of metal deactivator, 2% of extreme pressure additive, and the mass ratio of petroleum sulfonate to oleic acid sorbitol monoester is 1: 2: 2% of molybdate, 2% of demulsifier and 2% of nano copper oxide powder.
And (3) mixing the base oil with the nano copper oxide powder, the corrosion inhibitor, the metal deactivator and the extreme pressure additive, and stirring for 2 hours to obtain the composite additive.
Comparative example 1
The graphene-based nano borate lubricating oil provided by the comparative example is prepared according to the following steps:
0.001 part of graphene-based hexadecyl calcium borate, 0.003 part of graphene-based nano cerium borate, 1.5 parts of ashless dispersant, 2 parts of succinimide, 1.5 parts of amine antioxidant, 2 parts of N, N-dimethylformamide, 1.5 parts of viscosity index improver, 4 parts of composite additive (provided in example 1) and 1.5 parts of defoaming agent are mixed with 85 parts of API II base oil, heated to 75 ℃, and heated and stirred for 10 hours. And ultrasonically dispersing for 6h, and filtering to remove particles with the particle size of more than 350 meshes to obtain the graphene-based nano borate lubricating oil.
Application example 1
The graphene-based nano borate lubricating oils obtained in examples 1 to 4 and comparative example 1 were used for the wear-leveling diameter and maximum seizure-free load performance tests, and the anti-wear and anti-friction properties of the lubricating oils were characterized, and the results are shown in table 1.
TABLE 1
Figure BDA0001665726100000091
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (9)

1. A preparation method of graphene-based nano borate lubricating oil is characterized by comprising the following steps:
s1, mixing and dispersing graphene-based nano borate and base oil to obtain a first mixture, wherein the graphene-based nano borate is selected from one or more of graphene-based hexadecyl calcium borate, graphene-based nano lanthanum borate and graphene-based nano cerium borate;
s2, adding an ashless dispersant, succinimide, an amine antioxidant and an amide solvent into the first mixture, and mixing to obtain a second mixture;
s3, heating the second mixture to 70-80 ℃, stirring for 2-4 hours, then sequentially adding a viscosity index improver, a composite additive and a defoaming agent, continuing heating and stirring for 2-4 hours after the addition is finished, and then performing ultrasonic dispersion and filtration to obtain the graphene-based nano borate lubricating oil;
the composite additive comprises 80-90% of base oil, 3-8% of rust inhibitor, 1-4% of metal deactivator, 1-4% of extreme pressure additive, 1-4% of demulsifier and 1-4% of copper oxide powder;
the preparation method of the composite additive comprises the following steps:
mixing base oil and copper oxide powder, performing ultrasonic treatment for 30min, sequentially adding a corrosion inhibitor, a metal deactivator and an extreme pressure additive, and performing ball milling for 1 h; and finally, adding the demulsifying agent, heating to 60 ℃, and stirring for 1.5 hours to obtain the composite additive.
2. The method for preparing the graphene-based nano borate lubricating oil according to claim 1, wherein in step S1, the graphene nano borate is 0.002-0.1 parts by weight, and the base oil is 80-90 parts by weight.
3. The method for preparing the graphene-based nano borate lubricating oil according to claim 1, wherein in step S2, the ashless dispersant is 1 to 2 parts, the succinimide is 1 to 3 parts, the amine antioxidant is 1 to 2 parts, and the amide solvent is 1 to 2 parts by weight.
4. The method for preparing the graphene-based nano borate lubricating oil according to claim 1, wherein in step S3, the viscosity index improver, the composite additive and the defoamer are respectively in an amount of 1 to 2 parts by weight, 1 to 5 parts by weight and 1 to 2 parts by weight, respectively.
5. The method for preparing the graphene-based nano borate lubricating oil according to claim 1, wherein in step S1, the mixing and dispersing process of the graphene-based nano borate and the base oil is as follows: stirring for 1-5 h under the condition of heat preservation at 70-90 ℃, and then ultrasonically dispersing for 1-3 h.
6. The method for preparing the graphene-based nano borate lubricating oil according to claim 1, wherein in step S2, the mixing process is as follows: stirring for 1-5 h, and then ultrasonically dispersing for 1-3 h.
7. The preparation method of the graphene-based nano borate lubricating oil according to claim 1, wherein in step S3, the stirring speed is 1000 to 4000r/min, and the heating circulation reflux speed is 1 to 400 ml/h.
8. The method for preparing the graphene-based nano borate lubricating oil according to claim 1, wherein the base oil is one or more selected from mineral oil, hydrocarbon-based synthetic oil, ester-based oil, and ether-based oil.
9. A graphene-based nano borate lubricating oil, characterized by being prepared by the preparation method of any one of claims 1 to 8.
CN201810480598.7A 2018-05-18 2018-05-18 Graphene-based nano borate lubricating oil and preparation method thereof Active CN108485753B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810480598.7A CN108485753B (en) 2018-05-18 2018-05-18 Graphene-based nano borate lubricating oil and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810480598.7A CN108485753B (en) 2018-05-18 2018-05-18 Graphene-based nano borate lubricating oil and preparation method thereof

Publications (2)

Publication Number Publication Date
CN108485753A CN108485753A (en) 2018-09-04
CN108485753B true CN108485753B (en) 2021-04-27

Family

ID=63352938

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810480598.7A Active CN108485753B (en) 2018-05-18 2018-05-18 Graphene-based nano borate lubricating oil and preparation method thereof

Country Status (1)

Country Link
CN (1) CN108485753B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110373251B (en) * 2019-07-18 2021-09-28 南京理工大学 Graphene/lanthanum borate/kaolin composite lubricating oil additive
CN110373247B (en) * 2019-07-18 2021-09-21 南京理工大学 Functional graphene/montmorillonite/lanthanum borate composite lubricating oil additive
CN114958452B (en) * 2022-06-11 2024-03-05 山东极热新材料科技有限公司 Preparation method and application of graphene composite material capable of being used for lubricating oil

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106811267B (en) * 2015-12-02 2019-10-01 中国科学院宁波材料技术与工程研究所 Graphene modified high molecular weight ashless dispersant, preparation method and application
CN105969478B (en) * 2016-05-17 2018-07-17 扬州大学 A kind of preparation method of the composite lubricated material of line borate/stannic oxide/graphene nano
CN107312599A (en) * 2017-07-06 2017-11-03 广西柳工机械股份有限公司 Nano-graphene compounded lubricating oil
CN107460021B (en) * 2017-08-07 2021-07-30 泉州师范学院 Preparation method of low-temperature graphene-based nano borate composite material

Also Published As

Publication number Publication date
CN108485753A (en) 2018-09-04

Similar Documents

Publication Publication Date Title
CN108485753B (en) Graphene-based nano borate lubricating oil and preparation method thereof
CN112534027B (en) Conductive lubricant
Gusain et al. Ultrasound assisted shape regulation of CuO nanorods in ionic liquids and their use as energy efficient lubricant additives
CN106367170B (en) Compound machine oil of the plant of containing graphene and preparation method thereof
CN111247233B (en) Lubricating oil composition and method for producing same
CN107338100B (en) Lubricating oil
CN105886001B (en) Lubricating oil based on nitrogen-containing surface modifier modified graphene and preparation method thereof
CN110760361B (en) Perfluoropolyether lubricating grease and preparation method thereof
CN108130172B (en) Biodegradable environment-friendly lubricating oil
CN107057813B (en) Graphene lubricating oil additive, preparation method and application thereof, and lubricating oil containing graphene lubricating oil additive
CN115353922B (en) Carbon nitride quantum dot-based polyethylene glycol lubricating additive and preparation method thereof
CN113817530B (en) Drawing oil containing nano-particle additive
CN111808660B (en) Low-friction-coefficient composite calcium sulfonate lubricating grease composition and preparation method thereof
CN110373246B (en) Montmorillonite-titanium nitride-functional graphene composite lubricating oil additive
CN104560313A (en) Composite lithium-calcium based lubricating grease and preparation method thereof
CN113652286A (en) Refrigerating machine oil composition and preparation method thereof
CN110437910A (en) Graphene lubricating oil and preparation method thereof
Gondolini et al. Easy preparation method of stable copper‐based nanoparticle suspensions in lubricant engine oil
CN110373247B (en) Functional graphene/montmorillonite/lanthanum borate composite lubricating oil additive
CN111676085B (en) Graphene lubricating oil for robot and preparation method and application thereof
CN110305712B (en) Layered silicate loaded graphene lubricating oil additive and preparation method thereof
CN111892982A (en) Preparation method of nitrogen-doped nano lubricating material
CN114517118B (en) Graphite alkyne lubricating oil composition and preparation method thereof
CN113186017B (en) Graphene lithium-based lubricating grease for high extreme pressure condition and preparation method thereof
CN115011395B (en) Cylinder lubricating oil composition with high oxidation stability

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant