CN118126762A - Antiwear fullerene lubricant and preparation method thereof - Google Patents

Antiwear fullerene lubricant and preparation method thereof Download PDF

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Publication number
CN118126762A
CN118126762A CN202410241114.9A CN202410241114A CN118126762A CN 118126762 A CN118126762 A CN 118126762A CN 202410241114 A CN202410241114 A CN 202410241114A CN 118126762 A CN118126762 A CN 118126762A
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fullerene
antiwear
parts
lubricant
graphene oxide
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苏桂珍
叶皓堂
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Guangdong Qiwei Lubricating Materials Co ltd
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Guangdong Qiwei Lubricating Materials 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
    • 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
    • C10M169/044Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and 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
    • 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
    • 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
    • C10M2201/06Metal compounds
    • C10M2201/065Sulfides; Selenides; Tellurides
    • 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
    • C10M2201/14Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic 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
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/18Natural waxes, e.g. ceresin, ozocerite, bees wax, carnauba; Degras
    • 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
    • C10M2207/40Fatty vegetable or animal oils
    • 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
    • C10M2227/061Esters derived from boron
    • 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
    • C10N2030/04Detergent property or dispersant property
    • 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
    • C10N2030/64Environmental friendly compositions

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

Abstract

The invention relates to the technical field of lubricants, and particularly discloses an antiwear fullerene lubricant and a preparation method thereof. The antiwear fullerene lubricant comprises the following raw material components in parts by weight: 5-10 parts of modified fullerene, 2.5-5 parts of graphene oxide-tungsten disulfide composite nano particles, 4-8 parts of vegetable wax and 65-80 parts of base oil; wherein the modified fullerene is prepared by modifying Fe/onion-shaped fullerene by stearic acid; the graphene oxide-tungsten disulfide composite nano particles are prepared from graphite oxide and ammonium dithiotungstate serving as raw materials by a spray drying-solid phase thermal decomposition method. The antiwear fullerene lubricant provided by the invention has good stability and dispersibility, and has antiwear antifriction synergistic effect among the components, so that the antiwear fullerene lubricant is energy-saving and environment-friendly.

Description

Antiwear fullerene lubricant and preparation method thereof
Technical Field
The invention relates to the technical field of lubricants, in particular to an antiwear fullerene lubricant and a preparation method thereof.
Background
Frictional wear is a major cause of high energy consumption and is also a key technical problem affecting the service life of mechanical equipment. Statistics show that about one third of the world's primary energy is consumed by frictional wear, and most of the mechanical part failures and more than half of the mechanical equipment malignancies are caused by lubrication failure or excessive wear. Lubrication failure of mechanical parts becomes one of main reasons for restricting service life of equipment, and direct economic loss of China caused by friction and abrasion is up to trillion yuan.
The most effective method for controlling or reducing frictional wear is to use lubricating oil, and various additives are added to improve the performance of lubricating oil, such as conventional additives of chlorinated paraffin, sulfurized isobutylene, zinc dialkyldithiophosphate and the like, and can generate a sacrificial friction film under the action of friction side reaction to prevent surface wear. However, conventional additives contain various elements or chemical groups (such as phosphorus, chlorine or metals in organic complexes), and toxic compounds or greenhouse gases are released after degradation, severely polluting the environment. Therefore, it is of great importance to develop an environmentally friendly lubricating oil additive with excellent antifriction and antiwear properties.
Disclosure of Invention
In view of the above, the invention provides an antiwear fullerene lubricant which has good stability and dispersibility, and has antiwear antifriction synergistic effect among the components, and is energy-saving and environment-friendly.
In a first aspect, the invention provides an antiwear fullerene lubricant, which comprises the following raw material components in parts by weight:
5 to 10 parts of modified fullerene, 2.5 to 5 parts of graphene oxide-tungsten disulfide composite nano particles, 4 to 8 parts of vegetable wax and 65 to 80 parts of base oil;
Wherein the modified fullerene is prepared by modifying Fe/onion-shaped fullerene by stearic acid; the graphene oxide-tungsten disulfide composite nano particles are prepared from graphite oxide and ammonium dithiotungstate serving as raw materials by a spray drying-solid phase thermal decomposition method.
The nano tungsten disulfide not only has good impact resistance and chemical inertness, but also has excellent lubricating and wear-resistant effects, and can improve friction shearing through rolling, deformation and stripping. However, the nano tungsten disulfide has large specific surface area, strong adsorption effect and strong instability, is easy to agglomerate in base oil, and greatly limits popularization and application. The graphene oxide has amphipathy and can be well self-dispersed in lubricating oil, the graphene oxide and the ammonium dithiotungstate are used as raw materials, and the interaction of more electronegative functional groups on the surface of the graphene oxide and ions in the ammonium dithiotungstate is utilized to prepare the graphene oxide-tungsten disulfide composite nano particles, so that the graphene oxide-tungsten disulfide composite nano particles have good dispersion stability and thermal stability and excellent wear resistance in a wide temperature range. When the load is higher and the friction is aggravated, the graphene oxide-tungsten disulfide composite nano particles can be adsorbed on the surface of the friction pair to generate a low-shear force physical adsorption lubricating film consisting of graphene oxide and tungsten disulfide; meanwhile, part of particles can also undergo a tribochemical reaction on the surface of the friction pair to form a tribochemical reaction film consisting of tungsten oxide, ferrous sulfate and ferric oxide, so that the wear resistance and antifriction performance of the base oil are greatly improved.
The Fe/onion-shaped fullerene has good mechanical properties, and the onion-shaped fullerene has excellent self-lubricating property due to the toughness and a unique hexagonal structure similar to a graphite structure, a layer of graphite coating similar to a micro-bearing can be formed between friction pairs to replace a broken oil film for lubricating, and iron elements play a role in repairing to a certain extent, and pits filled on the surfaces of the friction pairs play a role in reducing surface roughness. According to the invention, the Fe/onion-shaped fullerene is modified by the stearic acid, so that the surface energy of the nano onion-shaped fullerene can be reduced, and a single-molecule adsorption layer can be formed, so that fullerene particles have lipophilicity, and the dispersibility and stability of the fullerene particles in lubricating oil are improved.
According to the invention, the modified fullerene and the graphene oxide-tungsten disulfide composite nano particles are compounded, and have excellent anti-wear antifriction synergistic effect, the fullerene can form rolling friction between friction surfaces to improve lubrication due to a unique structure, a layered structure of the graphene oxide can form a stable friction interface to reduce contact pressure between materials, meanwhile, the tungsten disulfide and iron elements in the modified fullerene can be deposited on the worn part of the friction surfaces to play a role of packing and repairing, and can also form a ferrous sulfide film with a lower melting point with a metal matrix to effectively reduce contact between friction pairs, so that the wear is reduced, and the synergistic lubrication effect is achieved from multiple aspects of a physical lubrication film and a chemical reaction film. On the other hand, stearic acid can form a steric hindrance layer in the lubricating oil, and can prevent the aggregation and precipitation of onion-like fullerene and tungsten disulfide composite nano particles, so that a stable dispersion system is formed in the lubricating oil.
The invention is also added with vegetable wax, contains acid, alcohol and ester macromolecular organic matters, has the characteristics of biodegradability and environmental friendliness, can form a lubricating oil film with high bearing capacity on the friction surface, and reduces mechanical abrasion.
Optionally, the preparation method of the modified fullerene comprises the following steps: ferrocene is used as a catalyst, acetylene is used as a carbon source, argon is used as a carrier gas, the reaction is carried out at 800-1200 ℃, cooling and acid washing are carried out, fe/onion-shaped fullerene is obtained, and then the mass ratio is 1: mixing Fe/onion-shaped fullerene and stearic acid according to a proportion of 5-6, adding the mixture into sulfuric acid solution for ultrasonic dispersion, refluxing, filtering, washing to be neutral, and drying in vacuum to obtain the modified fullerene.
Further alternatively, the concentration of the sulfuric acid solution is 2mol/L.
Further alternatively, the temperature of the reflux is 80-100 ℃, and the time of the reflux is 2-3 hours.
Further alternatively, the temperature of the vacuum drying is 60-80 ℃, and the time of the vacuum drying is 6-12 h.
Optionally, the preparation method of the graphene oxide-tungsten disulfide composite nano-particles comprises the following steps: adding ammonium dithiotungstate into the graphite oxide solution, carrying out ultrasonic stripping, spray drying and granulating, and calcining the obtained product in an argon atmosphere at 390-410 ℃ and 440-460 ℃ for 1h respectively to obtain the graphene oxide-tungsten disulfide composite nano particles.
Further optionally, the mass fraction of the graphite oxide ink solution is 1% -1.5%.
Further alternatively, the ammonium dithiotungstate is added in an amount of 0.05 g/mL to 0.15g/mL.
Further alternatively, the spray-drying outlet temperature is 200 ℃ to 240 ℃.
Further alternatively, the time of ultrasonic stripping is 30 min-45 min.
Optionally, the plant wax is skin wax of any plant selected from sugarcane, cinnamomum camphora and Ginkgo biloba.
Optionally, the base oil comprises at least one of methyl borate, gasoline, olive oil, or palm oil.
In a second aspect, the present invention also provides a method for preparing the above antiwear fullerene lubricant, comprising the steps of:
Weighing the components according to the proportion, uniformly mixing the modified fullerene, the graphene oxide-tungsten disulfide composite nano particles and the base oil at the temperature of between 35 and 60 ℃, adding vegetable wax, heating and uniformly stirring to obtain the antiwear fullerene lubricant.
Optionally, the heating temperature is 65-75 ℃, and the stirring rotating speed is 100-150 r/min.
Compared with the prior art, the invention has the following beneficial effects:
The modified fullerene, the graphene oxide-tungsten disulfide composite nano particles and the vegetable wax in the antiwear fullerene lubricant provided by the invention are mutually cooperated, so that a physical lubricating film and a chemical friction reaction film can be formed on the friction surface, the direct contact between friction pairs is effectively reduced, the mechanical abrasion is reduced, the content of additives in lubricating oil is reduced, the antiwear and antifriction performances of the oil are greatly improved, the energy is saved, the environment is protected, and the antiwear fullerene lubricant can be widely used as additives of lubricating oil, hydraulic oil or lubricating grease for various vehicle engines and large-scale mechanical equipment.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the following examples. Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention. The various reagents and materials used in the present invention are commercially available or may be prepared by known methods unless otherwise specified. The graphene oxide used in the invention is prepared by a low-temperature oxidation intercalation method, the specific surface area is 200m 2/g~500m2/g, and the sheet diameter is 200 nm-500 nm.
In order to better illustrate the present invention, the following examples are provided for further illustration.
Example 1
The embodiment provides an antiwear fullerene lubricant, which comprises the following raw material components in parts by weight: 7 parts of modified fullerene, 3.5 parts of graphene oxide-tungsten disulfide composite nano particles, 6 parts of sugarcane epidermis wax and 73 parts of palm oil.
The preparation method of the modified fullerene comprises the following steps: preparing Fe/onion-shaped fullerene by adopting Chemical Vapor Deposition (CVD), firstly taking ferrocene as a catalyst, acetylene as a carbon source and argon as a carrier gas, carrying out catalytic reaction at 1000 ℃, cooling, and collecting a sample at an air outlet to obtain a Fe/onion-shaped fullerene crude product. And heating and refluxing the crude product with 1mol/L dilute hydrochloric acid at 90 ℃ for 3 hours, ball-milling for 4 hours at a high speed, and centrifugally washing with deionized water to be neutral to obtain the Fe/onion-shaped fullerene. Then, the mass is 1:5.5 mixing ball-milled Fe/onion-shaped fullerene and stearic acid, adding the mixture into 2mol/L sulfuric acid solution for ultrasonic dispersion, adding the product into concentrated sulfuric acid, heating and refluxing for 3 hours at 90 ℃, filtering, washing with deionized water to be neutral, and vacuum drying for 9 hours at 70 ℃ to obtain the modified fullerene.
The preparation method of the graphene oxide-tungsten disulfide composite nano particles comprises the following steps:
(1) Dissolving tungsten trioxide in an ammonium sulfide aqueous solution, stirring for 1h at 0 ℃, standing and crystallizing for 24h at 0 ℃ after the reaction is finished, collecting by adopting a filtering method, and purifying for 3 times by using ice water and ice ethanol to obtain the ammonium dithiotungstate.
(2) Taking an aqueous solution of graphite oxide with the mass fraction of 1.25%, adding ammonium dithiotungstate according to the proportion of 0.1g/mL, carrying out ultrasonic stripping for 35min, carrying out spray drying granulation on the mixed solution, and carrying out spray drying at the outlet temperature of 220 ℃. And then calcining the obtained intermediate product in argon atmosphere at 400 ℃ and 450 ℃ for 1h respectively to obtain the graphene oxide-tungsten disulfide composite nano particles.
The embodiment also provides a preparation method of the antiwear fullerene lubricant, which comprises the following steps: weighing the components according to the proportion, uniformly mixing the modified fullerene, the graphene oxide-tungsten disulfide composite nano particles and the base oil at 50 ℃, then adding the vegetable wax, and uniformly stirring at the speed of 125r/min at 70 ℃ to obtain the antiwear fullerene lubricant.
Example 2
The embodiment provides an antiwear fullerene lubricant, which comprises the following raw material components in parts by weight: 5 parts of modified fullerene, 2.5 parts of graphene oxide-tungsten disulfide composite nano particles, 4 parts of sugarcane epidermis wax and 65 parts of palm oil.
The preparation method of the modified fullerene comprises the following steps: preparing Fe/onion-shaped fullerene by adopting Chemical Vapor Deposition (CVD), firstly taking ferrocene as a catalyst, acetylene as a carbon source and argon as a carrier gas, carrying out catalytic reaction at 800 ℃, cooling, and collecting a sample at an air outlet to obtain a Fe/onion-shaped fullerene crude product. And heating and refluxing the crude product with 1mol/L dilute hydrochloric acid at 90 ℃ for 3 hours, ball-milling for 4 hours at a high speed, and centrifugally washing with deionized water to be neutral to obtain the Fe/onion-shaped fullerene. Then, the mass is 1:5, mixing the ball-milled Fe/onion-shaped fullerene and stearic acid, adding the mixture into 2mol/L sulfuric acid solution for ultrasonic dispersion, adding the product into concentrated sulfuric acid, heating and refluxing for 3 hours at 90 ℃, filtering, washing with deionized water to be neutral, and vacuum drying for 6 hours at 60 ℃ to obtain the modified fullerene.
The preparation method of the graphene oxide-tungsten disulfide composite nano particles comprises the following steps:
(1) Dissolving tungsten trioxide in an ammonium sulfide aqueous solution, stirring for 1h at 0 ℃, standing and crystallizing for 24h at 0 ℃ after the reaction is finished, collecting by adopting a filtering method, and purifying for 3 times by using ice water and ice ethanol to obtain the ammonium dithiotungstate.
(2) Taking an aqueous solution of graphite oxide with the mass fraction of 1%, adding ammonium dithiotungstate according to the proportion of 0.05g/mL, carrying out ultrasonic stripping for 30min, carrying out spray drying granulation on the mixed solution, and carrying out spray drying at the outlet temperature of 200 ℃. And then calcining the obtained intermediate product in argon atmosphere at 390 ℃ and 440 ℃ for 1h respectively to obtain the graphene oxide-tungsten disulfide composite nano particles.
The embodiment also provides a preparation method of the antiwear fullerene lubricant, which comprises the following steps: weighing the components according to the proportion, uniformly mixing the modified fullerene, the graphene oxide-tungsten disulfide composite nano particles and the base oil at 35 ℃, then adding the vegetable wax, and uniformly stirring at the speed of 100r/min at 65 ℃ to obtain the antiwear fullerene lubricant.
Example 3
The embodiment provides an antiwear fullerene lubricant, which comprises the following raw material components in parts by weight: 10 parts of modified fullerene, 5 parts of graphene oxide-tungsten disulfide composite nano particles, 8 parts of sugarcane epidermis wax, 20 parts of methyl borate, 15 parts of olive oil and 45 parts of palm oil.
The preparation method of the modified fullerene comprises the following steps: preparing Fe/onion-shaped fullerene by adopting Chemical Vapor Deposition (CVD), firstly taking ferrocene as a catalyst, acetylene as a carbon source and argon as a carrier gas, carrying out catalytic reaction at 1200 ℃, cooling, and collecting a sample at an air outlet to obtain a Fe/onion-shaped fullerene crude product. And heating and refluxing the crude product with 1mol/L dilute hydrochloric acid at 90 ℃ for 3 hours, ball-milling for 4 hours at a high speed, and centrifugally washing with deionized water to be neutral to obtain the Fe/onion-shaped fullerene. Then, the mass is 1:6, mixing the ball-milled Fe/onion-shaped fullerene and stearic acid, adding the mixture into 2mol/L sulfuric acid solution for ultrasonic dispersion, adding the product into concentrated sulfuric acid, heating and refluxing for 3 hours at 90 ℃, filtering, washing with deionized water to be neutral, and vacuum drying for 12 hours at 80 ℃ to obtain the modified fullerene.
The preparation method of the graphene oxide-tungsten disulfide composite nano particles comprises the following steps:
(1) Dissolving tungsten trioxide in an ammonium sulfide aqueous solution, stirring for 1h at 0 ℃, standing and crystallizing for 24h at 0 ℃ after the reaction is finished, collecting by adopting a filtering method, and purifying for 3 times by using ice water and ice ethanol to obtain the ammonium dithiotungstate.
(2) Taking an aqueous solution of graphite oxide with the mass fraction of 1.5%, adding ammonium dithiotungstate according to the proportion of 0.15g/mL, carrying out ultrasonic stripping for 40min, carrying out spray drying granulation on the mixed solution, and carrying out spray drying at the outlet temperature of 240 ℃. And then calcining the obtained intermediate product in an argon atmosphere at 410 ℃ and 460 ℃ for 1h respectively to obtain the graphene oxide-tungsten disulfide composite nano particles.
The embodiment also provides a preparation method of the antiwear fullerene lubricant, which comprises the following steps: weighing the components according to the proportion, uniformly mixing the modified fullerene, the graphene oxide-tungsten disulfide composite nano particles and the base oil at 60 ℃, then adding the vegetable wax, and uniformly stirring at the speed of 150r/min at 75 ℃ to obtain the antiwear fullerene lubricant.
Comparative example 1
This comparative example provides an antiwear fullerene lubricant prepared in exactly the same manner as in example 1, except that the modified fullerene was replaced with an equivalent amount of fullerene C60.
Comparative example 2
The comparative example provides an antiwear fullerene lubricant, which is prepared in the same process as in example 1, except that the graphene oxide-tungsten disulfide composite nanoparticles are replaced by equivalent amounts of nano tungsten disulfide, and the average particle size is 50-90 nm.
Comparative example 3
This comparative example provides an antiwear fullerene lubricant, which was prepared in exactly the same manner as in example 1, except that the graphene oxide-tungsten disulfide composite nanoparticles were replaced with the same amount of graphene oxide.
Performance testing
The lubricants prepared in examples 1 to 3 and comparative examples 1 to 3 were examined for their respective properties, and the results are shown in Table 1 below.
Dispersion stability: after dispersion and standing sedimentation by ultrasonic heating, the transparency of the mixed solution is observed to distinguish the quality of dispersion stability, and the test conditions are as follows: the ultrasonic power is 800W, the ultrasonic frequency is 22KHz, the ultrasonic temperature is 40 ℃, the ultrasonic stirring time is 30min, the heating temperature is 50 ℃, and the standing time is 60d.
Coefficient of friction: referring to SH0762-2005, the conditions are: the MRS-10B four-ball friction and wear testing machine comprises GCr15 steel balls, the rotating speed is 1450r/min, the room temperature is high, the long grinding time is 60min, and the load is 392N.
Biodegradability: reference is made to CEC-L-33-A-93.
Emission reduction experiment: the antiwear fullerene lubricant prepared in example 1 was prepared by mixing 1:9, adding the mixture into piston engine lubricating oil in a volume ratio, heating to 120 ℃, sealing, mixing, stirring until no water is contained, adjusting the pH value to be neutral, and naturally cooling to obtain the lubricating oil. When the oil is used in a piston type gasoline engine, compared with the piston type engine lubricating oil which does not contain antiwear fullerene lubricant, the oil can be obviously saved by 29%, the exhaust emission after combustion is reduced by 35%, the noise is reduced by 8 db, and the engine temperature is reduced by 8 ℃.
Table 1 test results
From the results, the antiwear fullerene lubricant provided by the invention has good stability and dispersibility, and has antiwear antifriction synergistic effect among the components, so that the antiwear fullerene lubricant is energy-saving and environment-friendly.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.

Claims (10)

1. The antiwear fullerene lubricant is characterized by comprising the following raw material components in parts by weight:
5-10 parts of modified fullerene, 2.5-5 parts of graphene oxide-tungsten disulfide composite nano particles, 4-8 parts of vegetable wax and 65-80 parts of base oil;
Wherein the modified fullerene is prepared by modifying Fe/onion-shaped fullerene by stearic acid; the graphene oxide-tungsten disulfide composite nano particles are prepared from graphite oxide and ammonium dithiotungstate serving as raw materials by a spray drying-solid phase thermal decomposition method.
2. The antiwear fullerene lubricant according to claim 1, wherein the preparation method of the modified fullerene comprises the following steps:
Ferrocene is used as a catalyst, acetylene is used as a carbon source, argon is used as a carrier gas, the reaction is carried out at 800-1200 ℃, cooling and acid washing are carried out, fe/onion-shaped fullerene is obtained, and then the mass ratio is 1: and 5-6, mixing Fe/onion-shaped fullerene and stearic acid, adding the mixture into sulfuric acid solution for ultrasonic dispersion, refluxing, filtering, washing to be neutral, and drying in vacuum to obtain the modified fullerene.
3. The antiwear fullerene lubricant of claim 1, wherein the concentration of the sulfuric acid solution is 2mol/L; and/or
The temperature of the reflow is 80-100 ℃, and the reflow time is 2-3 hours; and/or
The temperature of the vacuum drying is 60-80 ℃, and the time of the vacuum drying is 6-12 hours.
4. The antiwear fullerene lubricant according to claim 1, wherein the preparation method of the graphene oxide-tungsten disulfide composite nano particles comprises the following steps:
Adding ammonium dithiotungstate into the graphite oxide solution, carrying out ultrasonic stripping, spray drying and granulating, and calcining the obtained product in an argon atmosphere at 390-410 ℃ and 440-460 ℃ for 1h respectively to obtain the graphene oxide-tungsten disulfide composite nano particles.
5. The antiwear fullerene lubricant according to claim 4, wherein the mass fraction of the graphite oxide solution is 1% -1.5%; and/or
The addition amount of the ammonium dithiotungstate is 0.05 g-0.15 g/mL.
6. The antiwear fullerene lubricant according to claim 4, wherein the outlet temperature of the spray drying is 200 ℃ -240 ℃; and/or
The ultrasonic stripping time is 30-45 min.
7. The antiwear fullerene lubricant according to claim 1, wherein the plant wax is a skin wax of any one of sugarcane, camphor, ginkgo.
8. The antiwear fullerene lubricant of claim 1, wherein the base oil comprises at least one of methyl borate, gasoline, olive oil, or palm oil.
9. The preparation method of the antiwear fullerene lubricant is characterized by comprising the following steps of:
weighing the components according to the proportion, uniformly mixing the modified fullerene, the graphene oxide-tungsten disulfide composite nano particles and the base oil at 35-60 ℃, adding vegetable wax, heating and uniformly stirring to obtain the antiwear fullerene lubricant.
10. The method according to claim 9, wherein the heating temperature is 65 ℃ to 75 ℃, and the stirring speed is 100r/min to 150r/min.
CN202410241114.9A 2024-03-04 2024-03-04 Antiwear fullerene lubricant and preparation method thereof Pending CN118126762A (en)

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