CN112080330A - Nano rhenium-molybdenum alloy-graphene composite lubricating oil additive - Google Patents

Nano rhenium-molybdenum alloy-graphene composite lubricating oil additive Download PDF

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CN112080330A
CN112080330A CN202011014700.8A CN202011014700A CN112080330A CN 112080330 A CN112080330 A CN 112080330A CN 202011014700 A CN202011014700 A CN 202011014700A CN 112080330 A CN112080330 A CN 112080330A
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rhenium
molybdenum alloy
graphene
alloy powder
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曾军堂
陈庆
司文彬
李钧
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Chengdu New Keli Chemical Science Co Ltd
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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
    • C10M141/00Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
    • C10M141/08Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic sulfur-, selenium- or tellurium-containing compound
    • 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
    • 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
    • C10M2201/05Metals; Alloys
    • 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
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06Thio-acids; Thiocyanates; Derivatives thereof
    • C10M2219/062Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
    • C10M2219/066Thiocarbamic type compounds
    • C10M2219/068Thiocarbamate metal salts

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The invention provides a nano rhenium-molybdenum alloy-graphene composite lubricating oil additive, which is prepared by wetting nano rhenium-molybdenum alloy powder by using a hydrogen peroxide solution, adding the nano rhenium-molybdenum alloy powder with defects on the surface and a surfactant into an ethanol dispersion liquid of graphene oxide for uniform ultrasonic dispersion, heating to reduce the graphene oxide into graphene and coating the graphene oxide with the graphene oxide, homogenizing, dispersing, spray drying, and uniformly dispersing with dithiocarbamate, bisphenol antioxidant and phosphate. The nano rhenium-molybdenum alloy-graphene provided by the invention has good lubricity and wear resistance, and the graphene is spread on the surface of a metal piece under high load to protect the metal surface and repair micro defects of the metal piece, and meanwhile, the nano rhenium-molybdenum alloy and the graphene can form a protective layer with excellent wear resistance on the metal surface.

Description

Nano rhenium-molybdenum alloy-graphene composite lubricating oil additive
Technical Field
The invention relates to the technical field of lubricating oil additives, in particular to a nano rhenium-molybdenum alloy-graphene composite lubricating oil additive.
Background
With the rapid development of the automobile industry and the mechanical industry, the requirements for high-load and high-speed operation are higher and higher, frictional wear is a ubiquitous natural phenomenon, the wear is a main cause of equipment damage in the mechanical operation, and lubricating oil plays an important role in high-performance machinery as the most effective technical means for reducing friction and wear. The role of lubricating oils is therefore becoming increasingly important for safety and performance requirements.
With the development of the lubricating oil industry, the harsh conditions of high pressure, high temperature and the like of lubricating oil used in the aspects of industrial machinery and the like put better demands on the lubricating oil, the performance of the basic lubricating oil reaches the technical bottleneck, the abrasion resistance, the friction reduction and the self-repairing performance of the lubricating oil are further improved, and the lubricating oil additive depending on functionality is needed. The nano particles as an additive show special and excellent tribological properties in lubricating oil, have great application prospects, and are the key point of the current high-performance lubricating oil research. The nano material technology is applied to the lubricating oil, and has great significance for increasing the wear resistance and the antifriction property of the lubricating oil. Various nano metals, nano oxides and nano sulfides are applied to the lubricating oil additive.
In recent years, in order to further advance the application of nanoparticles to lubricating oils and to promote the dispersion of nanoparticles, nanoparticles having an organically modified and coated shell-core structure have appeared. The nano particles with the shell-core structure are generally high polymer/inorganic nano shell-core type composite nano microspheres, not only have good wear resistance and friction reduction, but also are easy to repair worn parts. For example, at higher loads, the shell of the polymer melts and spreads to form an effective polymer lubricating film to repair the worn part. However, the nano inorganic particles modified by high polymer are used for wear resistance, friction reduction and repair of lubricating oil, and the lubricating film is easy to damage, which causes a problem of affecting the service life of the lubricating oil, so that research on lubricating oil additives with durability becomes a hot point.
Chinese patent application No. 201910970902.0 discloses a nano graphitized carbon ball lubricating oil additive with corrosion resistance, and a preparation method and application thereof, in the method, firstly, limited interfacial free radical copolymerization is realized through a surfactant and a monomer under the action of an initiator to obtain polymer nanospheres, then the polymer nanospheres are carbonized at high temperature to form porous hollow nano graphitized carbon balls, based on the fact that the porous hollow carbon balls are hollow porous structures, a corrosion inhibitor is loaded through a physical adsorption means, and then the porous hollow nano graphitized carbon balls are dispersed into lubricating oil and used as the lubricating oil additive. Chinese invention patent application No. 201711383769.6 discloses a lubricating oil additive of functionalized graphene loaded with natural montmorillonite, a preparation method and application thereof, firstly, graphene oxide is modified by a silane coupling agent to obtain functionalized graphene oxide; and then, mixing the functionalized graphene oxide with natural montmorillonite nano powder, and carrying out water (or solvent) thermal reaction to obtain the montmorillonite-loaded functionalized graphene composite material additive.
In order to improve the durability of the lubricating film and the repairing film formed during the high-load work of the lubricating oil, a novel composite nano inorganic particle lubricating oil additive is needed to be provided, so that the long-term protection of the lubricating oil on metal parts is ensured.
Disclosure of Invention
Aiming at the problem that a lubricating film formed by the current lubricating oil additive in practical application is easy to age or damage under the condition of high load, the invention provides a nano rhenium-molybdenum alloy-graphene composite lubricating oil additive, so that the lubricating oil can form a durable lubricating film and a durable repairing film in high-load work.
In order to achieve the purpose, the invention adopts the following technical scheme:
a nano rhenium-molybdenum alloy-graphene composite lubricating oil additive is prepared by wetting nano rhenium-molybdenum alloy powder by using a hydrogen peroxide solution, adding the nano rhenium-molybdenum alloy powder with defects on the surface and a surfactant into an ethanol dispersion liquid of graphene oxide for uniform ultrasonic dispersion, heating to reduce the graphene oxide into graphene and coat the nano rhenium-molybdenum alloy powder, homogenizing and dispersing, spray drying, and uniformly dispersing with dithiocarbamate, bisphenol antioxidant and phosphate ester; the preparation process comprises the following steps:
(1) adding graphene oxide into ethanol, and uniformly dispersing to obtain an ethanol dispersion solution of the graphene oxide;
(2) spraying a hydrogen peroxide solution on the surface of the nano rhenium-molybdenum alloy powder to slightly wet the nano rhenium-molybdenum alloy powder, and then standing to enable the surface of the nano rhenium-molybdenum alloy powder to have defects so as to obtain nano rhenium-molybdenum alloy powder with surface defects;
(3) adding the nano rhenium-molybdenum alloy powder with surface defects into an ethanol dispersion liquid of graphene oxide, then adding a surfactant, performing ultrasonic dispersion to disperse the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder, heating the dispersion liquid to generate ethanol steam while performing ultrasonic dispersion to gradually reduce the graphene oxide into graphene, and coating the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder to obtain a treated material;
(4) adding the treated material into a homogenizer for homogenizing and dispersing, and then spraying and drying to obtain graphene-coated nano rhenium-molybdenum alloy powder;
(5) and uniformly dispersing the nano rhenium and molybdenum alloy powder coated with the graphene, dithiocarbamate, bisphenol antioxidant and phosphate to obtain the nano rhenium and molybdenum alloy-graphene composite lubricating oil additive.
Preferably, the surfactant is sodium dodecyl benzene sulfonate.
Preferably, the dithiocarbamate is one of copper dithiocarbamate, zinc dithiocarbamate and cadmium dithiocarbamate.
Preferably, the concentration of the ethanol dispersion of graphene oxide in the step (1) is 5-15%.
Preferably, the mass concentration of the hydrogen peroxide solution in the step (2) is 30-40%.
Further preferably, the amount of the hydrogen peroxide solution is 1-2% of the mass of the nano rhenium-molybdenum alloy powder.
Preferably, the standing time in the step (2) is 2-3 h.
Preferably, the power of the ultrasonic dispersion in the step (3) is 750-850W, the frequency is 20-30kHz, and the time is 20-30 min.
Preferably, in the preparation of the material treated in the step (3), the mass ratio of the ethanol dispersion liquid of the graphene oxide, the nano rhenium-molybdenum alloy powder with the surface defect and the surfactant is 100: 30-35: 1-3.
Preferably, the pressure for homogeneous dispersion in the step (4) is 10-20MPa, and the time is 1-3 h.
Preferably, in the preparation of the composite lubricating oil additive in the step (5), the mass ratio of the graphene-coated nano rhenium-molybdenum alloy powder, the dithiocarbamate, the bisphenol antioxidant to the phosphate is 20-30: 1-3: 1-4: 2-4.
It is known that the nanoparticle additive commonly used in lubricating oil has special and excellent tribological properties, and the high polymer modified nano inorganic particles studied and applied in recent years can obviously improve the anti-wear performance of liquid lubricating oil. However, the lubricating film and repairing film formed by the high polymer modified nano inorganic particles when the lubricating oil is used are aged or damaged along with the work and load increase of the lubricating oil, so that the metal part is difficult to be protected for a long time, and meanwhile, the repairing layer and the lubricating film formed by the high polymer are poor in combination permeability with the metal, so that the long-term protection is difficult to form. The invention creatively uses the nano rhenium-molybdenum alloy and the graphene as raw materials to prepare the composite lubricating oil additive, thereby effectively solving the problems.
The raw materials selected by the invention are graphene and nano rhenium-molybdenum alloy with excellent performance. Each carbon atom in graphene is represented by SP2The hybrid graphene has the advantages that a unique two-dimensional hexagonal honeycomb lattice structure is formed, the hybrid graphene has super-strong electric conduction, heat conduction, lubrication and corrosion resistance, the super-large specific surface area and single-layer structure enable graphene to easily enter a contact surface, direct contact of rough surfaces is reduced, the friction coefficient is extremely low, and meanwhile, the super-strong structure and the thermal stability enable a graphene product to keep the basic performance of the graphene product unchanged at high temperature, and especially under the environment of high temperature, the excellent lubricating property, the wear resistance and the oxidation resistance of the graphene product are well reflected in the use of lubricating oil. The nano rhenium-molybdenum alloy is a molybdenum alloy which takes molybdenum as a base and is added with 2-5% of rhenium, the plasticity of the molybdenum can be improved and the strength of the molybdenum can be improved by adding the molybdenum into the rhenium, and the nano rhenium-molybdenum alloy belongs to a solid solution strengthening type alloy, and has good tensile strength and ductility because the rhenium is soft.
Firstly, spraying a hydrogen peroxide solution on the surface of nano rhenium-molybdenum alloy powder to slightly wet the nano rhenium-molybdenum alloy powder and standing the nano rhenium-molybdenum alloy powder, so that the surface of the nano rhenium-molybdenum alloy powder has defects; the dosage of the hydrogen peroxide solution is strictly controlled to be 1-2% of the mass of the nano rhenium-molybdenum alloy powder in the spraying and wetting process, so that only certain defects are generated on the surface of the alloy powder, the coating of graphene oxide in the subsequent preparation process is facilitated, and the excessive dosage can cause the alloy damage of the nano rhenium-molybdenum alloy, and the wear-resistant and antifriction effects are influenced.
Further, adding the nano rhenium-molybdenum alloy powder with surface defects and a surfactant into an ethanol dispersion liquid of graphene oxide, ultrasonically dispersing to enable the graphene oxide to be dispersed on the surface of the nano rhenium-molybdenum alloy powder, heating the dispersion liquid to generate ethanol steam, gradually reducing the graphene oxide into graphene in an ethanol steam environment, further coating the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder, and dispersing and spray-drying the graphene oxide by using a homogenizer to obtain the nano rhenium-molybdenum alloy powder coated by the graphene.
Further, uniformly dispersing the nano rhenium and molybdenum alloy powder coated by the graphene, dithiocarbamate, bisphenol antioxidant and phosphate to obtain the nano rhenium and molybdenum alloy-graphene composite lubricating oil additive. The nano rhenium-molybdenum alloy-graphene composite lubricating oil additive obtained by the invention is different from the method that graphene is directly added in lubricating oil, the nano rhenium-molybdenum alloy is coated by the graphene, and the characteristics of soft texture and good ductility of rhenium are utilized, so that the graphene can be combined on the surface of a metal piece to form a firm lubricating film and a firm repairing film; meanwhile, the nano rhenium-molybdenum alloy has the stretching capacity under load, a protective layer with excellent wear resistance is easily formed on the metal surface together with graphene, and the nano rhenium-molybdenum alloy can be prevented from aging or being damaged under high-load and high-temperature conditions.
The existing lubricating oil is difficult to form a durable lubricating film and a durable repairing film in high-load work, and the application of the lubricating oil is limited. In view of the above, the invention provides a nano rhenium-molybdenum alloy-graphene composite lubricating oil additive, which is prepared by dispersing graphene oxide in ethanol to obtain an ethanol-water dispersion of the graphene oxide; spraying a hydrogen peroxide solution on the surface of the nano rhenium-molybdenum alloy powder to slightly wet the nano rhenium-molybdenum alloy powder, standing to enable the surface of the nano rhenium-molybdenum alloy powder to have defects, then adding an ethanol-water dispersion liquid of graphene oxide, adding a surfactant, and performing ultrasonic dispersion to enable the graphene oxide to be dispersed on the surface of the nano rhenium-molybdenum alloy powder; heating the dispersion liquid to generate ethanol steam while performing ultrasonic dispersion, and gradually reducing graphene oxide into graphene in the ethanol steam environment so as to coat the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder; dispersing the treated material by a homogenizer, and spray-drying to obtain graphene-coated nano rhenium and molybdenum alloy powder, and further adding dithiocarbamate, bisphenol antioxidant and phosphate to uniformly disperse to obtain the nano rhenium and molybdenum alloy-graphene composite lubricating oil additive. The nano rhenium-molybdenum alloy-graphene provided by the invention has good lubricity and wear resistance, and the graphene is spread on the surface of a metal piece under high load to protect the metal surface and repair micro defects of the metal piece, and meanwhile, the nano rhenium-molybdenum alloy and the graphene can form a protective layer with excellent wear resistance on the metal surface.
Compared with the prior art, the invention provides a nano rhenium-molybdenum alloy-graphene composite lubricating oil additive which has the outstanding characteristics and excellent effects that:
1. according to the nano rhenium-molybdenum alloy-graphene composite material obtained by the invention, graphene oxide is reduced and coated on the surface of the nano rhenium-molybdenum alloy to form a structure in which the rhenium-molybdenum alloy is coated by the graphene, so that the nano rhenium-molybdenum alloy-graphene composite material not only has good lubricity and wear resistance, but also has the advantages that the graphene is spread on the surface of a metal piece when a high load is applied, the metal surface is protected, and the micro defects of the metal piece are repaired.
2. When the nano rhenium-molybdenum alloy-graphene composite lubricating oil additive is used for lubricating oil, different from the method of directly adding graphene into the lubricating oil, the nano rhenium-molybdenum alloy is mainly coated by the graphene, and the rhenium is soft in texture, so that the graphene is combined on the surface of a metal piece to form a firm lubricating film and a firm repairing film. Meanwhile, the nano rhenium-molybdenum alloy has the stretching capacity under load, and a protective layer with excellent wear resistance is easily formed on the metal surface together with the graphene.
Drawings
FIG. 1: the structure schematic diagram of the nano rhenium-molybdenum alloy-graphene composite lubricating oil additive obtained by the invention; wherein: 1-a graphene layer; 2-nano rhenium-molybdenum alloy.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Adding graphene oxide into ethanol, and uniformly dispersing to obtain an ethanol dispersion solution of graphene oxide with the concentration of 10%;
(2) spraying a hydrogen peroxide solution with the mass concentration of 35% onto the surface of the nano rhenium-molybdenum alloy powder, wherein the dosage of the hydrogen peroxide solution is 1.5% of the mass of the nano rhenium-molybdenum alloy powder, so that the nano rhenium-molybdenum alloy powder is slightly wetted, and then standing for 2.5 hours, so that the surface of the nano rhenium-molybdenum alloy powder has defects, and thus obtaining nano rhenium-molybdenum alloy powder with surface defects;
(3) adding 32.5kg of nano rhenium-molybdenum alloy powder with surface defects into 100kg of ethanol dispersion liquid of graphene oxide, then adding 2kg of sodium dodecyl benzene sulfonate, carrying out ultrasonic dispersion at the power of 800W and the frequency of 25kHz for 25min to disperse the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder, heating the dispersion liquid to generate ethanol steam while carrying out ultrasonic dispersion to gradually reduce the graphene oxide into graphene, and coating the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder to obtain a treated material;
(4) homogenizing the treated material, homogenizing and dispersing for 2h under the pressure of 15MPa, and then spraying and drying to obtain graphene-coated nano rhenium-molybdenum alloy powder;
(5) and uniformly dispersing 25kg of graphene-coated nano rhenium and molybdenum alloy powder, 2kg of copper dithiocarbamate, 2.5kg of bisphenol antioxidant and 3kg of phosphate to obtain the nano rhenium and molybdenum alloy-graphene composite lubricating oil additive.
Example 2
(1) Adding graphene oxide into ethanol, and uniformly dispersing to obtain an ethanol dispersion liquid of graphene oxide with the concentration of 8%;
(2) spraying a hydrogen peroxide solution with the mass concentration of 32% onto the surface of the nano rhenium-molybdenum alloy powder, wherein the dosage of the hydrogen peroxide solution is 1.2% of the mass of the nano rhenium-molybdenum alloy powder, so that the nano rhenium-molybdenum alloy powder is slightly wetted, and then standing for 2 hours to enable the surface of the nano rhenium-molybdenum alloy powder to have defects, so as to obtain nano rhenium-molybdenum alloy powder with surface defects;
(3) adding 31kg of nano rhenium-molybdenum alloy powder with surface defects into 100kg of ethanol dispersion liquid of graphene oxide, then adding 1.5kg of sodium dodecyl benzene sulfonate, ultrasonically dispersing for 28min at the power of 760W and the frequency of 22kHz to disperse the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder, heating the dispersion liquid to generate ethanol steam while ultrasonically dispersing to gradually reduce the graphene oxide into graphene, and coating the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder to obtain a treated material;
(4) adding the treated material into the mixture for homogenization, carrying out homogenization dispersion for 2.5h under the pressure of 12MPa, and then carrying out spray drying to obtain graphene-coated nano rhenium-molybdenum alloy powder;
(5) and uniformly dispersing 23kg of graphene-coated nano rhenium and molybdenum alloy powder, 2.5kg of zinc dithiocarbamate, 3kg of bisphenol antioxidant and 3.5kg of phosphate to obtain the nano rhenium and molybdenum alloy-graphene composite lubricating oil additive.
Example 3
(1) Adding graphene oxide into ethanol, and uniformly dispersing to obtain an ethanol dispersion solution of graphene oxide with the concentration of 12%;
(2) spraying a hydrogen peroxide solution with the mass concentration of 38% onto the surface of the nano rhenium-molybdenum alloy powder, wherein the dosage of the hydrogen peroxide solution is 1.8% of the mass of the nano rhenium-molybdenum alloy powder, so that the nano rhenium-molybdenum alloy powder is slightly wetted, and then standing for 3 hours to enable the surface of the nano rhenium-molybdenum alloy powder to have defects, so as to obtain nano rhenium-molybdenum alloy powder with surface defects;
(3) adding 34kg of nano rhenium-molybdenum alloy powder with surface defects into 100kg of ethanol dispersion liquid of graphene oxide, then adding 2.5kg of sodium dodecyl benzene sulfonate, ultrasonically dispersing for 22min at the power of 840W and the frequency of 28kHz to disperse the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder, heating the dispersion liquid to generate ethanol steam while ultrasonically dispersing to gradually reduce the graphene oxide into graphene, and coating the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder to obtain a treated material;
(4) adding the treated material into the mixture for homogenization, carrying out homogenization dispersion for 1.5h under the pressure of 18MPa, and then carrying out spray drying to obtain graphene-coated nano rhenium-molybdenum alloy powder;
(5) and uniformly dispersing 28kg of graphene-coated nano rhenium and molybdenum alloy powder, 1.5kg of cadmium dithiocarbamate, 2kg of bisphenol antioxidant and 3.5kg of phosphate to obtain the nano rhenium and molybdenum alloy-graphene composite lubricating oil additive.
Example 4
(1) Adding graphene oxide into ethanol, and uniformly dispersing to obtain 5% graphene oxide ethanol dispersion liquid;
(2) spraying a hydrogen peroxide solution with the mass concentration of 30% onto the surface of the nano rhenium-molybdenum alloy powder, wherein the dosage of the hydrogen peroxide solution is 1% of the mass of the nano rhenium-molybdenum alloy powder, so that the nano rhenium-molybdenum alloy powder is slightly wetted, and then standing for 2 hours to enable the surface of the nano rhenium-molybdenum alloy powder to have defects, so as to obtain nano rhenium-molybdenum alloy powder with surface defects;
(3) adding 30kg of nano rhenium-molybdenum alloy powder with surface defects into 100kg of ethanol dispersion liquid of graphene oxide, then adding 1kg of sodium dodecyl benzene sulfonate, carrying out ultrasonic dispersion for 30min at the power of 750W and the frequency of 20kHz, so that the graphene oxide is dispersed on the surface of the nano rhenium-molybdenum alloy powder, heating the dispersion liquid to generate ethanol steam while carrying out ultrasonic dispersion, so that the graphene oxide is gradually reduced into graphene and is coated on the surface of the nano rhenium-molybdenum alloy powder, and thus a treated material is obtained;
(4) homogenizing the treated material, homogenizing and dispersing for 3h under the pressure of 10MPa, and then spraying and drying to obtain nano rhenium-molybdenum alloy powder coated with graphene;
(5) and uniformly dispersing 20kg of graphene-coated nano rhenium and molybdenum alloy powder, 3kg of copper dithiocarbamate, 4kg of bisphenol antioxidant and 4kg of phosphate to obtain the nano rhenium and molybdenum alloy-graphene composite lubricating oil additive.
Example 5
(1) Adding graphene oxide into ethanol, and uniformly dispersing to obtain an ethanol dispersion solution of graphene oxide with the concentration of 15%;
(2) spraying a hydrogen peroxide solution with the mass concentration of 40% onto the surface of the nano rhenium-molybdenum alloy powder, wherein the dosage of the hydrogen peroxide solution is 2% of the mass of the nano rhenium-molybdenum alloy powder, so that the nano rhenium-molybdenum alloy powder is slightly wetted, and then standing for 3 hours to enable the surface of the nano rhenium-molybdenum alloy powder to have defects, so as to obtain nano rhenium-molybdenum alloy powder with surface defects;
(3) adding 35kg of nano rhenium-molybdenum alloy powder with surface defects into 100kg of ethanol dispersion liquid of graphene oxide, then adding 3kg of sodium dodecyl benzene sulfonate, carrying out ultrasonic dispersion for 20min at the power of 850W and the frequency of 30kHz to disperse the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder, heating the dispersion liquid to generate ethanol steam while carrying out ultrasonic dispersion to gradually reduce the graphene oxide into graphene, and coating the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder to obtain a treated material;
(4) homogenizing the treated material, homogenizing and dispersing for 1h under the pressure of 20MPa, and then spraying and drying to obtain nano rhenium-molybdenum alloy powder coated with graphene;
(5) and uniformly dispersing 30kg of graphene-coated nano rhenium and molybdenum alloy powder, 1kg of zinc dithiocarbamate, 1kg of bisphenol antioxidant and 2kg of phosphate to obtain the nano rhenium and molybdenum alloy-graphene composite lubricating oil additive.
Comparative example 1
Compared with the embodiment 1, the comparative example 1 directly adopts the nano rhenium-molybdenum alloy powder and the graphene in a mass ratio of 10: 3 composite, the others are completely consistent with example 1.
The test method comprises the following steps:
testing the bearing capacity of the lubricant: the compound lubricating oil additives prepared in the examples 1-5 and the comparative example 1 of the invention are prepared into lubricating oil according to the following formula (mass percent): 150SN 50%, 500SN 44%, OCP 5.5%, lubricant additive 0.5%, and base without lubricant additiveThe base oil is a reference sample; the lubricating oil prepared by the lubricating oil additives of the examples and the comparative examples and the lubricating oil of the reference sample are subjected to a four-ball friction grinding test according to the standard of the determination method of the bearing capacity of the lubricating oil (GB/T3142-2019), and the maximum non-seizure load P of the lubricating oil is testedBAnd sintering load PDThe value is obtained. The test results are shown in table 1.
Table 1:
performance index PB(N) PD(N)
Example 1 790 2680
Example 2 785 2670
Example 3 795 2685
Example 4 775 2660
Example 5 800 2700
Comparative example 1 550 2010
Reference sample 420 1600
As can be seen from Table 1, the lubricating oils formulated with the lubricating oil additives of examples 1-5 of the present invention exhibited better wear resistance, lubricity and durability when subjected to the four-ball friction wear test, with the maximum non-seizure load and sintering load being higher than those of comparative example 1. The lubricating oil additive of the comparative example 1 is simple composition of nano rhenium-molybdenum alloy powder and graphene, and has poor binding property, so that the lubricating oil additive cannot effectively play a role in durable lubrication and wear resistance. The reference sample had no additives added, and thus had the worst lubricity and abrasion resistance.

Claims (9)

1. The nano rhenium-molybdenum alloy-graphene composite lubricating oil additive is characterized in that a hydrogen peroxide solution is used for wetting nano rhenium-molybdenum alloy powder, then the nano rhenium-molybdenum alloy powder with defects on the surface and a surfactant are added into an ethanol dispersion liquid of graphene oxide for uniform ultrasonic dispersion, then the mixture is heated to reduce the graphene oxide into graphene and coat the nano rhenium-molybdenum alloy powder, and then the graphene oxide is homogenized, dispersed, sprayed and dried and then uniformly dispersed with dithiocarbamate, bisphenol antioxidant and phosphate to prepare the nano rhenium-molybdenum alloy composite lubricating oil additive; the preparation process comprises the following steps:
(1) adding graphene oxide into ethanol, and uniformly dispersing to obtain an ethanol dispersion solution of the graphene oxide;
(2) spraying a hydrogen peroxide solution on the surface of the nano rhenium-molybdenum alloy powder to slightly wet the nano rhenium-molybdenum alloy powder, and then standing to enable the surface of the nano rhenium-molybdenum alloy powder to have defects so as to obtain nano rhenium-molybdenum alloy powder with surface defects;
(3) adding the nano rhenium-molybdenum alloy powder with surface defects into an ethanol dispersion liquid of graphene oxide, then adding a surfactant, performing ultrasonic dispersion to disperse the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder, heating the dispersion liquid to generate ethanol steam while performing ultrasonic dispersion to gradually reduce the graphene oxide into graphene, and coating the graphene oxide on the surface of the nano rhenium-molybdenum alloy powder to obtain a treated material;
(4) adding the treated material into a homogenizer for homogenizing and dispersing, and then spraying and drying to obtain graphene-coated nano rhenium-molybdenum alloy powder;
(5) and uniformly dispersing the nano rhenium and molybdenum alloy powder coated with the graphene, dithiocarbamate, bisphenol antioxidant and phosphate to obtain the nano rhenium and molybdenum alloy-graphene composite lubricating oil additive.
2. The nano rhenium and molybdenum alloy-graphene composite lubricating oil additive as claimed in claim 1, which is characterized in that,
the surfactant is sodium dodecyl benzene sulfonate;
the dithiocarbamate is one of copper dithiocarbamate, zinc dithiocarbamate and cadmium dithiocarbamate.
3. The nano rhenium and molybdenum alloy-graphene composite lubricating oil additive as claimed in claim 1, wherein the concentration of the ethanol dispersion liquid of the graphene oxide in the step (1) is 5-15%.
4. The nano rhenium-molybdenum alloy-graphene composite lubricating oil additive as claimed in claim 1, wherein the mass concentration of the hydrogen peroxide solution in the step (2) is 30-40%, and the amount of the hydrogen peroxide solution is 1-2% of the mass of the nano rhenium-molybdenum alloy powder.
5. The nano rhenium and molybdenum alloy-graphene composite lubricating oil additive as claimed in claim 1, wherein the standing time in the step (2) is 2-3 hours.
6. The nano rhenium and molybdenum alloy-graphene composite lubricating oil additive as claimed in claim 1, wherein the power of ultrasonic dispersion in the step (3) is 750-850W, the frequency is 20-30kHz, and the time is 20-30 min.
7. The nano rhenium and molybdenum alloy-graphene composite lubricating oil additive as claimed in claim 1, wherein in the preparation of the material treated in the step (3), the mass ratio of the ethanol dispersion liquid of graphene oxide, the nano rhenium and molybdenum alloy powder with surface defects and the surfactant is 100: 30-35: 1-3.
8. The nano rhenium and molybdenum alloy-graphene composite lubricating oil additive as claimed in claim 1, wherein the pressure of homogeneous dispersion in the step (4) is 10-20MPa, and the time is 1-3 h.
9. The nano rhenium and molybdenum alloy-graphene composite lubricating oil additive as claimed in claim 1, wherein in the preparation of the composite lubricating oil additive in step (5), the mass ratio of the graphene-coated nano rhenium and molybdenum alloy powder, the dithiocarbamate, the bisphenol antioxidant and the phosphate is 20-30: 1-3: 1-4: 2-4.
CN202011014700.8A 2020-09-24 2020-09-24 Nano rhenium-molybdenum alloy-graphene composite lubricating oil additive Withdrawn CN112080330A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113798535A (en) * 2021-10-21 2021-12-17 安徽军明机械制造有限公司 Drilling device with efficient self-lubricating function
CN115873648A (en) * 2022-12-26 2023-03-31 吉诺润滑技术(苏州)有限公司 Composite additive for lubricating oil

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113798535A (en) * 2021-10-21 2021-12-17 安徽军明机械制造有限公司 Drilling device with efficient self-lubricating function
CN115873648A (en) * 2022-12-26 2023-03-31 吉诺润滑技术(苏州)有限公司 Composite additive for lubricating oil
CN115873648B (en) * 2022-12-26 2024-06-04 吉诺润滑技术(苏州)有限公司 Composite additive for lubricating oil

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Application publication date: 20201215