CN112322370A - Preparation method of nano lubricating oil additive with double-layer hollow composite shell structure - Google Patents

Preparation method of nano lubricating oil additive with double-layer hollow composite shell structure Download PDF

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CN112322370A
CN112322370A CN202011090213.XA CN202011090213A CN112322370A CN 112322370 A CN112322370 A CN 112322370A CN 202011090213 A CN202011090213 A CN 202011090213A CN 112322370 A CN112322370 A CN 112322370A
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particles
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pah
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任柏静
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Changchun Faway Tong Yang Automobile Plastic Components Co Ltd
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Changchun Faway Tong Yang Automobile Plastic Components Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C01P2004/34—Spheres hollow
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C10M2201/066—Molybdenum sulfide
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds

Abstract

A preparation method of a double-layer hollow composite shell structure nano lubricating oil additive comprises the following steps: (1) mixing Na2MoO4·H2Dispersing O and KSCN in deionized water, stirring, and adding C16H36BrN, adding HCL solution to enable the pH of the mixed solution to be less than 1, stirring, transferring the mixed solution into a polytetrafluoroethylene reaction kettle for sealing, and carrying out hydrothermal reaction for 24 hours at the temperature of 200 ℃ to obtain expected nanoparticles; (2) polyallylamine is reacted withPreparing the hydrochloride PAH particles into a clear aqueous solution of 1g/L, and taking MoS2The nanometer particles are immersed into PAH solution and stirred to obtain the MoS modified by PAH2The particles are put into the graphene oxide solution and stirred; and pouring the mixed solution into a polytetrafluoroethylene reaction kettle after stirring, sealing, carrying out hydrothermal reduction at the temperature of 180 ℃ for 20 hours, filtering, centrifuging and washing a reaction product until the pH value is 7, and finally carrying out freeze drying to obtain the molybdenum disulfide @ graphene particles with the double-layer hollow composite shell structure. The composite particle prepared by the invention can comprehensively improve the tribological performance of the composite particle.

Description

Preparation method of nano lubricating oil additive with double-layer hollow composite shell structure
Technical Field
The invention belongs to the technical field of lubricating oil additives, and particularly relates to a preparation method of a double-layer hollow composite shell structure nano lubricating oil additive.
Background
Statistically, the economic loss of mechanical parts due to frictional wear accounts for a considerable proportion of the total value of national production every year. The development of lubricating oil can change the current situation and reduce the economic loss caused by friction and abrasion.
With the continuous development of nano technology, the research and application range of nano materials is also expanding continuously. The nano material has the characteristics of large specific surface area, high diffusivity, easy sintering property, low melting point, high hardness and the like, so that the nano particles serving as the additive are applied to the lubricating oil to play a role in reducing friction and resisting wear in a mode different from that of the traditional additive. The novel lubricating material can form a layer of easily-sheared film on the friction surface to reduce the friction factor, and can also fill and repair the friction surface to a certain extent to play a self-repairing role. Therefore, the nano lubricating oil additive has outstanding extreme pressure resistance, excellent wear resistance and better lubricating property, and is suitable for working under heavy load, low speed and high temperature.
Molybdenum disulfide (MoS)2) The lubricant has the characteristics of high dispersibility, high extreme pressure property and the like, is originally used for the lubricant due to the unique layered structure, and is called as a super lubricant due to the excellent properties of low friction coefficient and hardness, excellent adhesion, corrosion resistance, pressure resistance, thermal stability and the like. The graphene has a good lamellar structure, the friction coefficient is close to zero, and the antifriction property of the additive can be improved through surface sliding friction. Chinese patent CN 108517239A discloses a preparation method of a graphene-based nano molybdenum disulfide lubricant additive, which adopts a hydrothermal method to compound graphene and molybdenum disulfide, so that nano molybdenum disulfide can be well dispersed on graphene, and the friction coefficient is reduced; however, the friction-reducing and wear-resisting properties of the lubricating oil additive still need to be improved.
Disclosure of Invention
In view of the above technical problems and disadvantages, an object of the present invention is to provide a method for preparing a nano-lubricant additive with a double-layer hollow composite shell structure, which develops a novel composite nano-particle structure with a double-layer hollow composite shell structure based on a molybdenum disulfide hollow shell as a framework, wherein the composite particles with such a structure can fully exert the composite effect and the multivariate synergetic mechanism thereof in a lubricating system, thereby fully improving the tribological properties of the composite particles.
In order to realize the purpose, the invention is realized by adopting the following technical scheme:
a preparation method of a double-layer hollow composite shell structure nano lubricating oil additive comprises the following steps:
(1) preparing hollow spherical molybdenum disulfide: mixing Na2MoO4·H2O and KSCN is calculated at a ratio of 1: 3 in deionized water, magnetically stirring until the solution is clear, adding C in the same proportion as KSCN16H36BrN, then slowly adding HCL solution to enable the pH of the mixed solution to be less than 1, stirring for 1.5h, transferring the mixed solution into a polytetrafluoroethylene reaction kettle for sealing, and carrying out hydrothermal reaction for 24h at the temperature of 200 ℃; then, after filtering and centrifuging the reaction product, washing the reaction product by using ethanol and deionized water to remove ions remained on the surface of the reaction product until the pH value is 7; finally, the white substance obtained by synthesis is dried in vacuum for 24 hours at the temperature of 60 ℃ to obtain the expected nano particles;
(2) and (3) synthesizing molybdenum disulfide @ graphene particles: first, the polyallylamine hydrochloride PAH fine particles were prepared as a clear aqueous solution of 1g/L, and MoS was collected2The nanometer particles are immersed in PAH solution, magnetically stirred for 1 hour, and the PAH solution is used for MoS2Performing amino modification on the surface of the particle; secondly, centrifuging the mixed solution to obtain the MoS modified by PAH2The particles are put into the graphene oxide solution and stirred for 5 hours by magnetic force; pouring the mixed solution into a polytetrafluoroethylene reaction kettle after stirring, sealing, and carrying out hydrothermal reduction for 20 hours at the temperature of 180 ℃; and then, filtering and centrifuging the reaction product, washing the reaction product with ethanol and deionized water, removing ions remained on the surface of the substance until the pH value is 7, and finally, freeze-drying the substance to obtain the molybdenum disulfide @ graphene particles with the double-layer hollow composite shell structure.
The invention has the advantages and beneficial effects that:
(1) the nano lubricating oil additive provided by the invention is a double-layer hollow composite shellStructure of the additive passing through MoS2The synergistic effect between the two hollow nanoshells of the @ graphene particle enables the particle to repair a worn surface more easily in the process of wear, enhances the wear resistance of the nano composite particle, and enables the prepared composite lubricating oil additive to have stronger friction-reducing and wear-resisting properties.
(2) The preparation method of the nano lubricating oil additive provided by the invention has the advantages of simple preparation process of the composite particles and high environmental friendliness.
Drawings
FIG. 1 is a diagram of the friction mechanism of the nano lubricating oil additive of the present invention.
Detailed Description
The present invention is described in further detail with reference to the following detailed description, but the present invention is not limited thereto, and those skilled in the art can make various modifications and substitutions based on the basic idea of the present invention without departing from the basic idea of the present invention.
Example 1
A preparation method of a double-layer hollow composite shell structure nano lubricating oil additive comprises the following steps:
(1) preparing hollow spherical molybdenum disulfide: mixing Na2MoO4·H2O and KSCN is calculated at a ratio of 1: 3 in deionized water, magnetically stirring until the solution is clear, adding C in the same proportion as KSCN16H36BrN, then slowly adding HCL solution to enable the pH of the mixed solution to be less than 1, stirring for 1.5h, transferring the mixed solution into a polytetrafluoroethylene reaction kettle for sealing, and carrying out hydrothermal reaction for 24h at the temperature of 200 ℃; then, after filtering and centrifuging the reaction product, washing the reaction product by using ethanol and deionized water to remove ions remained on the surface of the reaction product until the pH value is 7; finally, the white substance obtained by synthesis is dried in vacuum for 24 hours at the temperature of 60 ℃ to obtain the expected nano particles;
(2) and (3) synthesizing molybdenum disulfide @ graphene particles: the obtained MoS2Preparing MoS from nano particles and graphene oxide solution in a ratio of 1:12@ graphene microparticles; first, particles of polyallylamine hydrochloride (PAH) were preparedPreparing the hydrochloride into 1g/L clear aqueous solution, and taking MoS2The nanometer particles are immersed in PAH solution, magnetically stirred for 1 hour, and the PAH solution is used for MoS2Performing amino modification on the surface of the particle; secondly, centrifuging the mixed solution to obtain the MoS modified by PAH2The particles are put into a graphene oxide solution (deionized water with the concentration of 5mg/ml solvent) and are magnetically stirred for 5 hours; pouring the mixed solution into a polytetrafluoroethylene reaction kettle after stirring, sealing, and carrying out hydrothermal reduction for 20 hours at the temperature of 180 ℃; and then, filtering and centrifuging the reaction product, washing the reaction product with ethanol and deionized water, removing ions remained on the surface of the substance until the pH value is 7, and finally, freeze-drying the substance to obtain the molybdenum disulfide @ graphene particles with the double-layer hollow composite shell structure.
Example 2
(1) Preparing hollow spherical molybdenum disulfide: mixing Na2MoO4·H2O and KSCN is calculated at a ratio of 1: 3 in deionized water, magnetically stirring until the solution is clear, adding C in the same proportion as KSCN16H36BrN, then slowly adding HCL solution to enable the pH of the mixed solution to be less than 1, stirring for 1.5h, transferring the mixed solution into a polytetrafluoroethylene reaction kettle for sealing, and carrying out hydrothermal reaction for 24h at the temperature of 200 ℃; then, after filtering and centrifuging the reaction product, washing the reaction product by using ethanol and deionized water to remove ions remained on the surface of the reaction product until the pH value is 7; finally, the white substance obtained by synthesis is dried in vacuum for 24 hours at the temperature of 60 ℃ to obtain the expected nano particles;
(2) and (3) synthesizing molybdenum disulfide @ graphene particles: the obtained MoS2Preparing MoS from the nano particles and the graphene oxide solution in the ratio of 1:2 in the manner2@ graphene microparticles.
Referring to fig. 1, the antifriction and antiwear mechanism of the nano lubricating oil additive of the present invention is:
the composite nano particles with the double-layer hollow structure have a spherical structure, when lubricating oil flows, the composite nano particles are attached to the interface of the friction pair and roll on a wear surface under pressure, and the core-shell structure plays a role of a ball bearing and can improve the wear resistance of the friction pair at the initial stage of wear; followed byWith the increase of the wear time, the graphene with the hollow shell can be torn into graphene fragments with smaller sizes, and pits and gullies on the surface are repaired along with the fact that lubricating oil enters the damaged wear surface, so that the exposed nano MoS is exposed2The particles can also be redeposited on the wear surface to form nano-MoS2Physical deposition of films of particles due to nano-MoS2The particles are also in a hollow sphere structure, so the particles can slide along with the interlayer structure and are crushed into fine fragments again, the fine fragments enter the damaged wear surface, pits and gullies on the wear surface are repaired, and the self-repairing function of the nano particles is realized; in the later stage of abrasion, friction heat is generated in the lubricating oil due to abrasion, so that the temperature of the lubricating oil between friction pair interfaces is increased, and chemical reaction among components in a lubricating system is caused; the chemical reaction film formed by the frictional heat can further repair gullies on the worn surface, so that the surface is smooth; thus, graphene and MoS2The self-repairing and the chemical reaction of the lubricating oil jointly form a synergistic lubricating oil system, and the tribological performance of the composite nano lubricating oil can be effectively improved.

Claims (1)

1. A preparation method of a double-layer hollow composite shell structure nano lubricating oil additive is characterized by comprising the following steps:
(1) preparing hollow spherical molybdenum disulfide: mixing Na2MoO4·H2O and KSCN is calculated at a ratio of 1: 3 in deionized water, magnetically stirring until the solution is clear, adding C in the same proportion as KSCN16H36BrN, then slowly adding HCL solution to enable the pH of the mixed solution to be less than 1, stirring for 1.5h, transferring the mixed solution into a polytetrafluoroethylene reaction kettle for sealing, and carrying out hydrothermal reaction for 24h at the temperature of 200 ℃; then, after filtering and centrifuging the reaction product, washing the reaction product by using ethanol and deionized water to remove ions remained on the surface of the reaction product until the pH value is 7; finally, the white substance obtained by synthesis is dried in vacuum for 24 hours at the temperature of 60 ℃ to obtain the expected nano particles;
(2) and (3) synthesizing molybdenum disulfide @ graphene particles: first, the polyallylamine hydrochloride PAH fine particles were prepared as a 1g/L clear aqueous solution,get MoS2The nanometer particles are immersed in PAH solution, magnetically stirred for 1 hour, and the PAH solution is used for MoS2Performing amino modification on the surface of the particle; secondly, centrifuging the mixed solution to obtain the MoS modified by PAH2The particles are put into the graphene oxide solution and stirred for 5 hours by magnetic force; pouring the mixed solution into a polytetrafluoroethylene reaction kettle after stirring, sealing, and carrying out hydrothermal reduction for 20 hours at the temperature of 180 ℃; and then, filtering and centrifuging the reaction product, washing the reaction product with ethanol and deionized water, removing ions remained on the surface of the substance until the pH value is 7, and finally, freeze-drying the substance to obtain the molybdenum disulfide @ graphene particles with the double-layer hollow composite shell structure.
CN202011090213.XA 2020-10-13 2020-10-13 Preparation method of nano lubricating oil additive with double-layer hollow composite shell structure Pending CN112322370A (en)

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Publication number Priority date Publication date Assignee Title
CN108517239A (en) * 2018-05-25 2018-09-11 北京航科航天科技有限公司 A kind of preparation method of graphene-based nano molybdenum disulfide lube oil additive
CN109904397A (en) * 2017-12-08 2019-06-18 中国石油化工股份有限公司 A kind of molybdenum disulfide/C/ graphene composite material
US10669498B1 (en) * 2017-06-12 2020-06-02 U.S.A. as Represented by the Administrator of the National Aeronautics and S pace Administration MOS2- or WS2-filled hollow ZnS hexagonal nanotubes as core-shell structured solid lubricants and lubricant modifiers for space mechanisms
CN111575087A (en) * 2020-06-04 2020-08-25 青岛理工大学 Super-lubricating water lubricating additive, super-lubricating water lubricant, preparation method and application
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US10669498B1 (en) * 2017-06-12 2020-06-02 U.S.A. as Represented by the Administrator of the National Aeronautics and S pace Administration MOS2- or WS2-filled hollow ZnS hexagonal nanotubes as core-shell structured solid lubricants and lubricant modifiers for space mechanisms
CN109904397A (en) * 2017-12-08 2019-06-18 中国石油化工股份有限公司 A kind of molybdenum disulfide/C/ graphene composite material
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CN111575087A (en) * 2020-06-04 2020-08-25 青岛理工大学 Super-lubricating water lubricating additive, super-lubricating water lubricant, preparation method and application
CN111704950A (en) * 2020-07-07 2020-09-25 长春工业大学 Preparation method of soft shell-hard core shell composite structure nano lubricating oil additive

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Application publication date: 20210205