A ternary composite functional agent, a preparation method and application thereof

CN122609290APending Publication Date: 2026-08-21RUNYE FENGYUAN (TIANJIN) TECHNOLOGY DEVELOPMENT CO LTD
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Patent Information

Application Number
CN202610750796.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-05-28
Publication Date
2026-08-21

AI Technical Summary

Technical Problem

然而,现有技术体系仍面临四大共性瓶颈亟待突破:一是、功能表现的局限性:传统功能材料如润滑油添加剂、防伪油墨等,普遍存在功能单一化问题,且缺乏对自身状态变化及外部环境刺激的主动反馈与预警机制,导致相关系统长期处于“黑箱操作”状态,运行安全性与可控性不足

Benefits of technology

本发明所述三元复合功能剂通过在润滑油中构建“感知-响应-修复”一体化智能系统,实现对摩擦表面的动态调控;其修复作用呈现多维度协同特性,通过物理填充、化学催化与能量场介导的三重机制,形成由表及里、从宏观到微观的智能化修复体系,改善了传统润滑油的被动防护模式。

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Abstract

The application provides a ternary composite functional agent and a preparation method and application thereof, and relates to the technical field of advanced functional materials.The ternary composite functional agent comprises surface-modified nanometer cerium oxide, surface-modified niobium diselenide nanosheet and organic molybdenum.The ternary composite functional agent has an integrated action mechanism of energy transfer-electron transition-catalytic repair-fluorescence monitoring;wherein, through a triple mechanism of physical filling, chemical catalysis and energy field mediation, an intelligent and efficient repair system from the surface to the inside and from the macroscopic to the microscopic is formed.Meanwhile, based on the composite fluorescence characteristics of the surface-modified nanometer cerium oxide and the surface-modified niobium diselenide nanosheet, a monitoring system is constructed, and the ternary composite functional agent can also realize fluorescence monitoring.
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Description

Technical Field

[0001] This invention relates to the field of advanced functional materials technology, and in particular to a ternary composite functional agent, its preparation method, and its application. Background Technology

[0002] Currently, the demand for functional materials in the industrial sector is undergoing profound changes, rapidly evolving from traditional single-performance requirements to intelligent and multifunctional integration. However, the existing technological system still faces four common bottlenecks that urgently need to be overcome: First, the limitations of functional performance: Traditional functional materials, such as lubricant additives and anti-counterfeiting inks, generally suffer from single-function problems and lack proactive feedback and early warning mechanisms for changes in their own state and external environmental stimuli, resulting in related systems operating in a "black box" state for a long time, with insufficient operational safety and controllability. Second, the lack of intelligent sensing capabilities: Current material state monitoring mainly relies on external sensors, which not only increases system complexity and deployment costs but also makes it difficult to achieve full-domain, real-time, and accurate monitoring; the industry urgently needs to develop intrinsic sensing and tracing technologies built into the molecular structure of materials to build self-diagnostic capabilities for materials. Third, the technical barriers to the application of nanomaterials: The dispersion stability problem of nanofunctional materials in polymer matrices and oil-phase systems has not been effectively solved, and they are prone to aggregation, which seriously restricts the development of large-scale production processes and the promotion of practical engineering applications. Fourth, there is a contradiction between environmental performance and application efficiency: the high performance of traditional functional materials often comes at the cost of environmental friendliness, and the use of harmful elements such as sulfur, phosphorus, and chlorine is common, making it difficult to meet the increasingly stringent ecological and environmental protection regulations, and green development faces severe challenges.

[0003] In addition, various types of engines, including fuel oil, natural gas, methanol ethanol fuel, and hybrid power, all have significant technical pain points related to fuel characteristics and operating conditions in practical applications: (1) Fuel oil engines: Traditional fuel oil engines face carbon deposit problems during long-term operation, which directly leads to a decrease in combustion efficiency and affects the stability of power output; the wear of key friction pairs such as piston rings and cylinder liners is aggravated, which not only shortens the service life of the engine, but also increases maintenance costs; and the failure of the lubrication system will lead to an increase in the difficulty of controlling exhaust pollutant emissions, carbon particulate matter (PM), nitrogen oxides (NOx) x(1) Emissions of harmful substances such as carbon monoxide (CO) and hydrocarbons (HC) remain high. (2) Gas engines (including natural gas, liquefied gas and hydrogen engines): They have the advantage of clean combustion, but have unique lubrication problems. Natural gas engines are a typical example. Their "dry combustion" characteristics lead to insufficient lubrication of key components such as valves and valve seats, resulting in significant abnormal wear. At the same time, the tendency of engine knocking increases under high temperature conditions, which not only affects combustion efficiency but also accelerates the oxidation and deterioration of engine oil. High temperature environment further causes corrosion problems of parts, which puts forward higher requirements for the thermal stability and corrosion resistance of lubricating oil. (3) Alcohol fuel engines: Alcohol fuels such as methanol and ethanol are highly corrosive, which damage metal parts and sealing materials and affect the integrity of the lubrication system. Insufficient low temperature starting performance leads to untimely lubrication during the cold start stage, which aggravates instantaneous wear. Unconventional pollutants such as aldehydes produced during combustion are easy to react chemically with lubricating oil, leading to problems such as oil emulsification and acidification, which significantly reduces lubrication efficiency and service life. (4) Hybrid engines: The special working mode of hybrid engines brings complex lubrication challenges. Frequent start-stop cycles cause the engine to operate under insufficient lubrication conditions, resulting in significant instantaneous wear. The complex electric field environment generated by the motor system requires the lubricating oil to have good electrical insulation properties and chemical stability. Frequent switching of operating modes leads to large fluctuations in engine operating conditions, placing more stringent requirements on the viscosity adaptability, oxidation resistance, and durability of the lubricating oil.

[0004] Meanwhile, there are three core pain points in the field of intelligent lubrication and health management of industrial equipment: First, the lubrication status lacks real-time perception, which easily leads to maintenance delays or over-maintenance; Second, traditional anti-wear extreme pressure additives contain harmful components such as sulfur, phosphorus, and chlorine, which do not meet environmental protection requirements; Third, sudden lubrication failures can easily lead to shutdowns, resulting in high maintenance costs and significant losses. The specific pain points of each industry are as follows: Power plants: Gas turbines and other equipment operate at high temperatures for long periods, requiring extremely high lubrication reliability and resulting in huge losses from shutdowns; (1) Steel plants: Rolling mills and other equipment face extreme pressure, high temperature, and water spray conditions, which exacerbate component wear and corrosion; (2) Mines: Excavators and other equipment operate under extremely heavy loads and high dust environments, resulting in severe equipment wear and high maintenance costs; (3) Wind power generation: High-altitude gearboxes are difficult to maintain and costly, requiring ultra-long life oils; (4) Railway locomotives: Engines and other equipment operate under high vibration and high power density conditions, and lubrication reliability is related to safety. (5) Engineering / Agricultural machinery: harsh working conditions and untimely maintenance directly affect the uptime rate of lubrication durability; (6) Military equipment: needs to adapt to a wide temperature range of -40~180℃, and requires extreme reliability, rapid maintenance and anti-counterfeiting; (7) High precision equipment: CNC centers and the like have extreme requirements for vibration and precision, and lubrication fluctuations affect the processing quality; (8) Green metal processing fluid: traditional extreme pressure agents are not environmentally friendly, concentration control is difficult, and it affects the processing stability; (9) Intelligent anti-counterfeiting: existing technologies are easy to imitate, and inferior products may cause equipment failure.

[0005] In view of this, the present invention is hereby proposed. Summary of the Invention

[0006] The purpose of this invention is to provide a ternary composite functional agent, its preparation method, and its application. The ternary composite functional agent has dual functions of energy field catalytic repair and intelligent fluorescence ratio monitoring, so as to at least solve one of the technical problems existing in the prior art.

[0007] In order to achieve the above-mentioned objectives of the present invention, the following technical solution is adopted: In a first aspect, the present invention provides a ternary composite functional agent, the ternary composite functional agent comprising: surface-modified cerium oxide nanoparticles, surface-modified niobium diselenide nanosheets, and organic molybdenum.

[0008] Furthermore, the mass ratio of the surface-modified cerium oxide nanosheets, the surface-modified niobium diselenide nanosheets, and the organic molybdenum is (1~3):(0.2~1):(0.5~2).

[0009] Furthermore, the surface-modified nano-cerium oxide is nano-cerium oxide modified with long-chain fatty amines and / or long-chain fatty acids.

[0010] Furthermore, the long-chain fatty amine modified on the surface of the nano-cerium oxide is selected from C12~C22 long-chain fatty amines, preferably C14~C20 long-chain fatty amines, and more preferably C16~C18 long-chain fatty amines.

[0011] Furthermore, the long-chain fatty acid modified on the surface of the nano-cerium oxide is selected from C12~C22 long-chain fatty acids, preferably C14~C20 long-chain fatty acids, and more preferably C16~C18 long-chain fatty acids.

[0012] Furthermore, the molar ratio of the long-chain fatty amine to cerium is (1.5~3):1.

[0013] Furthermore, the molar ratio of the long-chain fatty acid to cerium is (1.5~3):1.

[0014] Furthermore, the particle size of the surface-modified cerium oxide nanoparticles is ≤50 nm.

[0015] Furthermore, the surface-modified niobium diselenide nanosheets are niobium diselenide nanosheets modified with long-chain fatty amines and / or long-chain fatty acids.

[0016] Furthermore, the long-chain fatty amine modified on the surface of the niobium diselenide nanosheets is selected from C12~C22 long-chain fatty amines, preferably C14~C20 long-chain fatty amines, and more preferably C16~C18 long-chain fatty amines.

[0017] Furthermore, the long-chain fatty acids used to modify the surface of the niobium diselenide nanosheets are selected from C12-C22 long-chain fatty acids, preferably C14-C20 long-chain fatty acids, and more preferably C16-C18 long-chain fatty acids.

[0018] Furthermore, the molar ratio of the long-chain fatty amine to niobium diselenide is (5~20):1.

[0019] Furthermore, the molar ratio of the long-chain fatty acid to niobium diselenide is (5~20):1.

[0020] Furthermore, the thickness of the surface-modified niobium diselenide nanosheets is <5 nm.

[0021] Furthermore, the organic molybdenum includes phosphorus-containing organic molybdenum and / or non-phosphorus organic molybdenum, preferably non-phosphorus organic molybdenum.

[0022] Furthermore, the organic molybdenum is selected from any one or a combination of at least two of the following: molybdenum dithiophosphate complexes, aryl molybdenum dithiophosphate complexes, molybdenum dithiosalicylate complexes, molybdenum dithiocarbamate complexes, organic molybdenum complexes of organic amides, and polyether amino molybdenum complexes.

[0023] In a second aspect, the present invention provides a method for preparing a ternary composite functional agent as described in the first aspect, the method comprising: Surface-modified cerium oxide precursor and niobium diselenide nanosheets were prepared by surface modification to obtain surface-modified cerium oxide nanosheets and surface-modified niobium diselenide nanosheets; then, the surface-modified cerium oxide nanosheets, surface-modified niobium diselenide nanosheets and organic molybdenum were mixed to obtain the ternary composite functional agent.

[0024] Furthermore, the surface-modified cerium oxide nanoparticles are prepared by the following steps: The cerium source and alkaline solution are mixed to carry out a precipitation reaction, resulting in a suspension containing the cerium hydroxide precursor. Long-chain fatty amines and / or long-chain fatty acids are added dropwise to the suspension containing the cerium hydroxide precursor to carry out an in-situ modification reaction, thereby obtaining a suspension containing the surface-modified precursor. Oxygen-containing gas is introduced into the suspension containing the surface-modified precursor to carry out an oxidation reaction, thereby obtaining surface-modified nano-cerium oxide.

[0025] Furthermore, the cerium source is selected from any one or a combination of at least two of cerium ammonium nitrate, cerium nitrate, and cerium oxide.

[0026] Furthermore, the molar ratio of the cerium source to the alkaline solute in the alkaline solution is 1:(4~12).

[0027] Furthermore, the alkaline solution is an aqueous solution of an alkali metal hydroxide, preferably an aqueous solution of sodium hydroxide.

[0028] Furthermore, the solid content of the alkaline solution is 10~30 wt%.

[0029] Furthermore, the precipitation reaction temperature is 55~65℃, and the precipitation reaction time is 0.5~5 h; the pH of the system needs to be controlled at 9.0~9.5 during the precipitation reaction.

[0030] Furthermore, the molar ratio of the long-chain fatty amine to cerium is (1.5~3):1.

[0031] Furthermore, the molar ratio of the long-chain fatty acid to cerium is (1.5~3):1.

[0032] Furthermore, the dropping time is controlled within 30 minutes; the temperature of the in-situ modification reaction is 75~85℃, and the time of the in-situ modification reaction is 2~6 hours.

[0033] Furthermore, the oxidation reaction is carried out at a temperature of 100-120°C for 2-6 hours.

[0034] Furthermore, the oxidation reaction is followed by the following post-processing steps: The suspension obtained after the oxidation reaction is mixed with an organic solvent and extracted to collect the organic phase. The organic phase is then concentrated and dispersed using an oil solvent. After shearing, a dispersion of surface-modified nano-cerium oxide is obtained.

[0035] Furthermore, in the process of preparing the dispersion of the surface-modified nano-cerium oxide, the organic solvent is cyclohexane.

[0036] Furthermore, in the process of preparing the dispersion of the surface-modified nano-cerium oxide, the oil solvent is selected from any one or a combination of at least two of PAO2 base oil, PAO4 base oil, PAO6 base oil, 4cst base oil, 6cst base oil, GTL base oil, and cycloalkyl mineral oil.

[0037] Furthermore, in the process of preparing the dispersion of the surface-modified nano-cerium oxide, the concentration is carried out by vacuum distillation at a temperature of 70~80℃ and a pressure of -0.10~-0.05 MPa.

[0038] Furthermore, in the process of preparing the dispersion of the surface-modified nano-cerium oxide, the shearing treatment is carried out using any one of the following devices: a high-shear emulsifier, a homogenizer, or a colloid mill.

[0039] Furthermore, during the preparation of the surface-modified nano-cerium oxide dispersion, the rotation speed of the shearing treatment is 1000~3000 rpm, and the shearing treatment time is 0.5~2 h.

[0040] Furthermore, in the dispersion of the surface-modified nano-cerium oxide, the particle size D50 of the nano-cerium oxide is ≤50nm; the solid content of the nano-cerium oxide is 30~50 wt%.

[0041] Furthermore, the surface-modified niobium diselenide nanosheets are prepared by the following steps: Long-chain fatty amines and / or long-chain fatty acids, along with niobium diselenide nanosheets, are mixed and modified to obtain surface-modified niobium diselenide nanosheets.

[0042] Furthermore, the molar ratio of the long-chain fatty amine to niobium diselenide is (5~20):1; the molar ratio of the long-chain fatty acid to niobium diselenide is (5~20):1.

[0043] Furthermore, the temperature of the modification reaction is 170~190℃, the pressure of the modification reaction is 0.8~1.0 MPa, and the time of the modification reaction is 12~36 h.

[0044] Furthermore, the modification reaction is followed by the following post-processing steps: The reaction slurry obtained from the modification reaction was centrifuged and the supernatant was collected. The supernatant was mixed with an azeotropic agent, concentrated, and then dispersed using an oil solvent. After shearing, a dispersion of surface-modified niobium diselenide nanosheets was obtained.

[0045] Furthermore, the centrifugation speed is 7000~9000 rpm.

[0046] Furthermore, the azeotropic agent includes any one or a combination of at least two of toluene, methylcyclohexane, cyclohexane, and n-heptane.

[0047] Furthermore, the mass ratio of the supernatant to the azeotropic agent is 1:(0.5~5).

[0048] Furthermore, in the process of preparing the dispersion of the surface-modified niobium diselenide nanosheets, the oil solvent is selected from any one or a combination of at least two of PAO2 base oil, PAO4 base oil, PAO6 base oil, 4cst base oil, 6cst base oil, GTL base oil, and cycloalkyl mineral oil.

[0049] Furthermore, in the process of preparing the dispersion of the surface-modified niobium diselenide nanosheets, the concentration is carried out by vacuum distillation at a temperature of 70~110℃ and a pressure of -0.10~-0.05MPa.

[0050] Furthermore, the rotational speed of the shearing process is 8000~12000 rpm, and the shearing time is 0.5~2 h.

[0051] Furthermore, in the dispersion of the surface-modified niobium diselenide nanosheets, the sheet thickness of the niobium diselenide nanosheets is <5 nm; the solid content of the niobium diselenide nanosheets is 5~20 wt%.

[0052] Thirdly, the present invention provides the application of the ternary composite functional agent as described in the first aspect in the preparation of lubricating media, greases and semi-solid lubricants, metal processing and forming media, lubricating preparations for assembly-anti-jamming and maintenance, dry film lubrication and functional coatings, industrial condition monitoring and predictive maintenance products, leak tracing and fault location products, oil authenticity identification and supply chain traceability products, anti-counterfeiting materials and ink products, smart packaging and quality indicators, and self-lubrication and wear resistance enhancement of polymers and composite materials.

[0053] As an optional implementation, the ternary composite functional agent is used in the preparation of industrial lubricating materials, automotive lubricating materials, metal processing lubricating materials, military equipment lubricating materials, anti-counterfeiting materials, and smart packaging.

[0054] Fourthly, the present invention provides a lubricating oil comprising the ternary composite functional agent as described in the first aspect.

[0055] Furthermore, the amount of the ternary composite functional agent added is 0.1 to 10.0% of the total mass of the lubricating oil, preferably 1.7 to 6.0%.

[0056] Compared with the prior art, the present invention has the following beneficial effects: The ternary composite functional agent of this invention achieves dynamic regulation of friction surfaces by constructing an integrated intelligent system of "sensing-response-repair" in lubricating oil. Its repair effect exhibits multi-dimensional synergistic characteristics. Through a triple mechanism of physical filling, chemical catalysis and energy field mediation, it forms an intelligent repair system from the surface to the interior and from the macro to the micro, improving the passive protection mode of traditional lubricating oil.

[0057] (1) Physical filling repair: The mechanism of the ternary composite functional agent is characterized by instantaneous response. It rapidly fills the micro-pits and scratches on the friction surface through nano-sized particles, which can quickly reduce surface roughness, optimize contact stress distribution, and effectively inhibit the expansion of defects into severe wear. This process is equivalent to building a "nano-scale repair substrate" for the friction interface, which not only improves the friction conditions in time, but also creates a smooth reaction interface for subsequent chemical repair, laying the foundation for long-term protection.

[0058] (2) Chemical catalytic repair: The ternary composite functional agent forms a protective film for a long time through chemical catalysis, that is, a non-stoichiometric, disordered amorphous nano-ceramic composite film is generated in situ on the friction surface. The film is mainly composed of elements such as Ce-O-Mo-Se-C, which are firmly bonded to the metal matrix through strong chemical bonds (such as Ce-O-Mo). It has both extremely high hardness (to resist wear) and extremely low shear strength (to reduce friction), thereby achieving the purpose of long-lasting anti-wear and friction reduction.

[0059] (3) Energy field-mediated intelligent directional repair: First, the ternary composite functional agent achieves intelligent directional repair. The wear area generates a stronger energy field due to the increased friction intensity, which promotes the directional enrichment of the active components of the functional agent and achieves the adaptive intelligent effect of "the more severe the wear, the more priority the repair", which greatly improves the repair efficiency and additive utilization rate. Second, the ternary composite functional agent can achieve efficient catalysis, which transforms the harmful frictional dissipation energy into a beneficial repair driving force, significantly improving the chemical film formation reaction rate and achieving rapid repair. Detailed Implementation

[0060] Unless otherwise defined herein, the scientific and technical terms used in conjunction with this invention shall have the meanings commonly understood by one of ordinary skill in the art. The meaning and scope of terms shall be clear; however, in any case of potential ambiguity, the definitions provided herein shall prevail over any dictionary or foreign definitions. In this application, unless otherwise stated, the use of "or" means "and / or". Furthermore, the use of the term "comprising" and other forms is non-limiting.

[0061] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0062] In a first aspect, the present invention provides a ternary composite functional agent, the ternary composite functional agent comprising: surface-modified cerium oxide nanoparticles, surface-modified niobium diselenide nanosheets, and organic molybdenum.

[0063] In this invention, the ternary composite functional agent is a ternary composite functional agent with surface-modified cerium oxide (CeO2) nanosheets and surface-modified niobium diselenide (NbSe2) nanosheets as the core, supplemented by organic molybdenum. This functional agent constructs an integrated mechanism of "energy transfer-electronic transition-catalytic repair-fluorescence monitoring", and innovatively develops an industrial preparation process for the core components to overcome the bottleneck of nano-rare earth material applications, and provides intelligent application solutions in multiple fields; wherein, surface-modified cerium oxide (CeO2) nanosheets serve as the 4f electron transition and catalytic repair center, surface-modified niobium diselenide (NbSe2) nanosheets serve as the quantum energy antenna and superlubricating framework, and organic molybdenum serves as a synergistic friction-reducing and catalytic component.

[0064] In this invention, the repair effect of the ternary composite functional agent exhibits multi-dimensional synergistic characteristics. Through a triple mechanism of physical filling, chemical catalysis, and energy field mediation, it forms an intelligent repair system that extends from the surface to the interior and from the macroscopic to the microscopic level, improving the passive protection mode of traditional lubricating oil. The specific repair mechanisms and their effects are as follows: First layer, physical filling and repair (instantaneous effect): Surface-modified cerium oxide (CeO2) nanoparticles (≤50 nm) and surface-modified niobium diselenide (NbSe2) nanosheets (<5 nm thickness), thanks to their ultra-fine nanoscale effect, penetrate with lubricating oil to microscopic scratches, pits, and other damage defects on the friction pair surface. Through physical adsorption and van der Waals forces, they directly "intercalate" and "fill" these defects. Characterized by instantaneous response, the nanoscale particles rapidly fill the microscopic pits and scratches on the friction surface, quickly reducing surface roughness, optimizing contact stress distribution, and effectively inhibiting the expansion of defects into severe wear. This process is equivalent to constructing a "nanoscale repair substrate" for the friction interface, not only immediately improving friction conditions but also creating a smooth reaction interface for subsequent chemical repair, laying the foundation for long-term protection.

[0065] Second stage, chemical catalytic repair (fundamental function): Under the high temperature and pressure environment generated by friction, the oxygen vacancies on the surface of surface-modified nano-cerium oxide (CeO2) act as highly efficient catalytic active centers, which are activated. These vacancies catalyze the breaking of C-C and CH bonds in base oil molecules and additive molecules adsorbed on the metal surface, generating active free radical fragments. Under the catalysis of CeO2 and friction, these fragments undergo cross-linking, polymerization, and recombination reactions with the decomposition products of organic molybdenum (such as MoO3 or MoS2) and the decomposition products of surface-modified niobium diselenide (NbSe2) (such as Se). This results in a durable protective film formed through chemical catalysis, namely, the in-situ generation of a non-stoichiometric, disordered, amorphous nano-ceramic composite film on the friction surface. This film is mainly composed of elements such as Ce-O-Mo-Se-C, and is firmly bonded to the metal matrix through strong chemical bonds (such as Ce-O-Mo). It possesses both extremely high hardness (to resist wear) and extremely low shear strength (to reduce friction), thereby achieving the purpose of durable anti-wear and friction reduction.

[0066] The third level, energy field-mediated intelligent targeted repair (core repair): First, the ternary composite functional agent achieves energy capture: the dispersed waste energy (thermal energy, vibrational energy, phonons) generated during friction is efficiently captured by niobium diselenide (NbSe2) nanosheets due to their quantum confinement effect (when their size is extremely small, the band structure changes, exhibiting unique physical properties). Second, the ternary composite functional agent achieves energy transfer: the NbSe2 nanosheets act as "quantum energy antennas," "regulating" the captured random energy and then directionally and efficiently transferring it to adjacent cerium oxide (CeO2) nanoparticles through resonant energy transfer (RET) or electronic coupling mechanisms. Finally, the ternary composite functional agent achieves 4f electron transitions and energy release: the transferred energy precisely excites Ce in CeO2. 3+ The 4f orbital electrons of the ions undergo a transition; when the electron falls back from the excited state to the ground state, the released energy is not wasted as useless heat, but is precisely used to significantly reduce the activation energy of the chemical film-forming reaction in the "second stage" of repair. This enables the ternary composite functional agent to achieve intelligent directional repair. The increased friction intensity in the worn area generates a stronger energy field, promoting the directional enrichment of the active components of the functional agent, achieving an adaptive intelligent effect of "the more severe the wear, the higher the priority for repair," greatly improving repair efficiency and additive utilization. Simultaneously, the ternary composite functional agent can achieve highly efficient catalysis, converting harmful frictional dissipation energy into beneficial repair driving force, significantly increasing the rate of chemical film-forming reaction and achieving rapid repair.

[0067] In summary, the triple repair mechanism of the ternary composite functional agent described in this invention effectively couples physical energy capture, chemical film-forming reaction, and intelligent directional regulation through the core hub of 4f electron transition, realizing the "turning waste into treasure" of frictional energy. This technology breaks through the limitations of traditional passive protection of lubricating oils, pioneering a new intelligent lubrication path of "active sensing-energy conversion-targeted repair," providing key technical support for the long-life and high-efficiency operation of high-end equipment. The discovery of its 4f electron regulation mechanism further lays the theoretical foundation for energy-driven intelligent materials in the field of tribochemistry.

[0068] It should be noted that the following descriptions of energy transfer, 4f electron transition, resonant energy transfer, and film formation pathway are intended to help understand the possible mechanism of action of the present invention and are not intended to limit the scope of protection of the present invention; the actual action pathway may differ under different substrates, carriers, and operating conditions.

[0069] In particular, it is necessary to explain the mechanism and role of the 4f electron transition: (1) Mechanism: The electron configuration of rare earth element cerium (Ce) has its own characteristics, and its valence electron is located in the 4f orbital ([Xe]4f). 1 5d 1 6s 2 ); the 4f orbital is surrounded by the outer 5s 2 5p 6 The shielding of the orbitals minimizes the influence of the external environment on the electrons, yet allows for a sensitive response to the internal chemical environment. The process by which an electron, after absorbing external energy, "jumps" from a lower energy level orbital (ground state) to a higher energy level orbital (excited state) is called a transition. Therefore, in the system of the aforementioned ternary composite functional agent, energy is transferred from the NbSe2 nanosheets to CeO2, and the CeO2 lattice contains Ce... 3+ When an ion absorbs this energy, one of its electrons in the 4f orbital is excited to a higher energy level (5d orbital). This process is called the 4f electron transition. This excited state is extremely unstable, and the electron will quickly fall back to the ground state (4f orbital).

[0070] (2) Function: The energy released during the electron fall-off process is transformed through two key pathways, bringing significant value to the performance improvement of functional agents. First, the core pathway is chemical energy conversion. The released energy can be precisely applied to the breaking and reconstruction of chemical bonds, directly driving the formation reaction of the amorphous nano-ceramic composite film in the "second layer" repair mechanism, which is equivalent to providing directional energy supply for the repair process. This pathway has three major advantages: First, it is highly efficient and accelerated. By reducing the activation energy barrier of the chemical reaction, the formation rate of the repair film is increased by several orders of magnitude, achieving "instant repair" efficiency. Second, it saves energy and reduces consumption. By recycling the heat energy originally dissipated during the friction process, the consumption of functional agents is significantly reduced while achieving the same or even better repair effect, thus improving economic efficiency. Third, it is intelligently adapted. The energy can be precisely applied to the worn parts, so that the repair behavior and the degree of damage are dynamically matched, greatly improving the level of intelligence. Second, the additional pathway is light energy conversion and monitoring function. Some energy is released in the form of photons and generates fluorescence, which constitutes the physical basis for the fluorescence monitoring function of functional agents. By monitoring changes in fluorescence intensity and ratio, the efficiency of 4f electron transition and the real-time consumption status of functional agents can be indirectly reflected, providing key technical support for the visualization and controllability of the repair process.

[0071] In summary, the triple repair mechanism of the ternary composite functional agent described in this invention is a manifestation of its powerful and intelligent function. The 4f electron transition is an important energy conversion hub, which can perfectly couple physical energy capture and transfer with chemical film-forming reactions, turning harmful frictional energy into valuable resources and realizing the technology from "passive protection" to "active intelligent repair".

[0072] Furthermore, it should be noted that the ternary composite functional agent described in this invention can also achieve fluorescence monitoring. A monitoring system is constructed based on the composite fluorescence properties of CeO2 and NbSe2 nanosheets: CeO2 emits approximately 450 nm blue fluorescence under 365 nm ultraviolet light excitation, while NbSe2 nanosheets produce approximately 550 nm yellow-green fluorescence. The two form an intrinsic fluorescence ratio signal (defined as R=I). 550 / 450In some embodiments, the R value is measured under conditions of 25°C, 365 nm excitation, same optical path, same sample concentration, and same integration time. This ratio signal is highly sensitive to key state parameters such as material consumption, ambient temperature, and mechanical stress, and can meet monitoring needs in multiple scenarios through portable ultraviolet light sources or professional spectral analysis equipment. The monitoring method is divided into a two-level application system: First, rapid on-site screening: using a portable ultraviolet flashlight to illuminate the dipstick or observation window of the equipment, and qualitative judgment is achieved by observing changes in fluorescence color. New oil appears bright yellow-green due to its high ratio value; as the active ingredients are consumed during use, the fluorescence gradually tends to white; when the oil is ineffective, the ratio value drops significantly, appearing as a dull blue. This method is simple to operate, responds quickly, and is suitable for daily equipment inspection and maintenance. Secondly, precise laboratory quantification: Utilizing a fluorescence spectrometer to accurately determine the ratio value R of oil samples, and combining this with chemometrics methods to establish a mathematical model of the R value and key oil indicators (such as acid value, kinematic viscosity, and content of metal wear elements), quantitative assessment of oil degradation and accurate prediction of remaining life can be achieved, providing data support for optimizing equipment maintenance cycles. Thirdly, in terms of functional expansion, this fluorescence characteristic can be further extended to the field of oil quality control: by comparing the fluorescence spectral characteristics of standard samples and test samples, rapid identification of genuine and counterfeit oil can be achieved; in industrial scenarios, using ultraviolet light to track the fluorescence trajectory of leaking oil can accurately locate leaks in hydraulic or lubrication systems, effectively improving troubleshooting efficiency. Therefore, the ternary composite functional agent system described in this invention possesses both qualitative and quantitative analytical capabilities, achieving full-chain coverage from on-site equipment monitoring to precise laboratory analysis, providing an innovative solution for industrial oil condition monitoring and equipment health management.

[0073] As an optional implementation, the mass ratio of the surface-modified cerium oxide nanosheets, the surface-modified niobium diselenide nanosheets, and the organic molybdenum is (1~3):(0.2~1):(0.5~2); Among them, "1~3" can be, for example, 1, 1.2, 1.4, 1.6, 1.8, 2, 2.2, 2.4, 2.6, 2.8, 3, etc.; Among them, "0.2~1" can be, for example, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, etc.; Among them, "0.5~2" can be, for example, 0.5, 0.6, 0.8, 1, 1.2, 1.4, 1.6, 1.8, 2, etc.

[0074] As an optional implementation, the surface-modified nano-cerium oxide is nano-cerium oxide modified with long-chain fatty amines and / or long-chain fatty acids.

[0075] It should be noted that ordinary nano-cerium oxide powder has extremely high surface energy, making it prone to irreversible hard agglomeration and difficult to disperse stably in the oil phase. This not only results in the loss of nano-effects but may also clog oil passages. Furthermore, its catalytic active sites (oxygen vacancies) are easily coated, leading to low catalytic efficiency, and it lacks state feedback functionality. In contrast, this invention preferably uses nano-cerium oxide modified with long-chain fatty amines and / or long-chain fatty acids to achieve organic coating of the nano-cerium oxide particle surface. This significantly reduces particle surface energy, effectively inhibits irreversible hard agglomeration, achieves stable dispersion in the oil phase, avoids clogging oil passages, and fully preserves the nano-effects. The modification layer precisely coats the particle surface rather than the catalytic active sites (oxygen vacancies), ensuring full exposure of active sites and significantly improving catalytic efficiency. Simultaneously, the organic modification layer enhances compatibility with the oil phase and can leverage the characteristics of organic groups to build a foundation for subsequent state feedback functionality, significantly improving its reliability and adaptability in applications such as lubrication.

[0076] As an optional implementation, the long-chain fatty amine modified on the surface of the nano-cerium oxide is selected from C12~C22 long-chain fatty amines.

[0077] As an optional implementation, the long-chain fatty amine modified on the surface of the nano-cerium oxide is selected from any one or a combination of at least two of laurylamine, myristamine, palmitamine, palmeneamine, stearamine, oleamine, linoleic acidamine, arachidamine, arachideneamine, erucic acidamine, mustardamine, behenamine, and beheneneamine.

[0078] In a preferred embodiment, the long-chain fatty amine modified on the surface of the nano-cerium oxide is selected from C14~C20 long-chain fatty amines.

[0079] As a more preferred embodiment, the long-chain fatty amine modified on the surface of the nano-cerium oxide is selected from C16~C18 long-chain fatty amines.

[0080] As an optional implementation, the long-chain fatty acid amine modified on the surface of the nano-cerium oxide is selected from C12~C22 long-chain fatty acids.

[0081] As an optional implementation, the long-chain fatty acids modified on the surface of the nano-cerium oxide are selected from any one or a combination of at least two of the following: lauric acid, myristic acid, palmitic acid, palmitic acid, stearic acid, oleic acid, trans oleic acid, linoleic acid, α-linolenic acid, γ-linolenic acid, arachidonic acid, arachidonic acid, and erucic acid.

[0082] In a preferred embodiment, the long-chain fatty acid amine modified on the surface of the nano-cerium oxide is selected from C14~C20 long-chain fatty acids.

[0083] As a more preferred embodiment, the long-chain fatty acid amine modified on the surface of the nano-cerium oxide is selected from C16~C18 long-chain fatty acids.

[0084] As an optional implementation, the molar ratio of the long-chain fatty amine to cerium is (1.5~3):1, for example, it can be 1.5:1, 1.6:1, 1.8:1, 2:1, 2.2:1, 2.4:1, 2.6:1, 2.8:1, 3:1, etc.

[0085] As an optional implementation, the molar ratio of the long-chain fatty acid to cerium is (1.5~3):1, for example, it can be 1.5:1, 1.6:1, 1.8:1, 2:1, 2.2:1, 2.4:1, 2.6:1, 2.8:1, 3:1, etc.

[0086] As an optional implementation, the particle size of the surface-modified nano-cerium oxide is ≤50 nm, for example, it can be 50 nm, 45 nm, 40 nm, 35 nm, 30 nm, 25 nm, 20 nm, 15 nm, 10 nm, 5 nm, 1 nm, etc.

[0087] As an optional implementation, the surface-modified niobium diselenide nanosheets are niobium diselenide nanosheets modified with long-chain fatty amines and / or long-chain fatty acids.

[0088] It should be noted that bulk niobium diselenide lacks quantum effects, while laboratory-prepared few-layer niobium diselenide nanosheets are extremely expensive, have very poor stability, and are prone to oxidation and aggregation, making them unsuitable for large-scale commercial applications. This invention preferably uses niobium diselenide nanosheets modified with long-chain fatty amines and / or long-chain fatty acids, which effectively retains the quantum effects of the few-layer structure, compensating for the performance shortcomings of bulk materials. The modification layer isolates the nanosheets from air, inhibits oxidation, and reduces particle surface energy, preventing aggregation and significantly improving stability. It also reduces the difficulty and cost of large-scale preparation, overcoming the bottleneck of commercializing laboratory samples. Furthermore, the organic modification layer enhances its compatibility with oil phases, polymers, and other matrices, laying the foundation for subsequent large-scale applications in lubrication, catalysis, and other fields.

[0089] As an optional implementation, the long-chain fatty amines that modify the surface of the niobium diselenide nanosheets are selected from C12~C22 long-chain fatty amines.

[0090] As an optional implementation, the long-chain fatty amines used to modify the surface of the niobium diselenide nanosheets are selected from any one or a combination of at least two of laurylamine, myristicamine, palmitamine, palmeneamine, stearylamine, oleylamine, linoleylamine, linolenic acidamine, arachidamine, arachideneamine, erucic acidamine, mustardamine, behenamine, and beheneneamine.

[0091] In a preferred embodiment, the long-chain fatty amines that modify the surface of the niobium diselenide nanosheets are selected from C14~C20 long-chain fatty amines.

[0092] As a more preferred embodiment, the long-chain fatty amine modified on the surface of the niobium diselenide nanosheets is selected from C16~C18 long-chain fatty amines.

[0093] As an optional implementation, the long-chain fatty acids used to modify the surface of the niobium diselenide nanosheets are selected from C12~C22 long-chain fatty acids.

[0094] As an optional implementation, the long-chain fatty acids used to modify the surface of the niobium diselenide nanosheets are selected from any one or a combination of at least two of the following: lauric acid, myristic acid, palmitic acid, palmitic acid, stearic acid, oleic acid, trans oleic acid, linoleic acid, α-linolenic acid, γ-linolenic acid, arachidonic acid, arachidonic acid, and erucic acid.

[0095] In a preferred embodiment, the long-chain fatty acids used to modify the surface of the niobium diselenide nanosheets are selected from C14 to C20 long-chain fatty acids.

[0096] As a more preferred embodiment, the long-chain fatty acid used to modify the surface of the niobium diselenide nanosheets is selected from C16-C18 long-chain fatty acids.

[0097] As an optional implementation, the molar ratio of the long-chain fatty amine and niobium diselenide is (5~20):1, for example, it can be 5:1, 6:1, 8:1, 10:1, 12:1, 14:1, 16:1, 18:1, 20:1, etc.

[0098] As an optional implementation, the molar ratio of the long-chain fatty acid to niobium diselenide is (5~20):1, for example, it can be 5:1, 6:1, 8:1, 10:1, 12:1, 14:1, 16:1, 18:1, 20:1, etc.

[0099] As an optional implementation, the thickness of the surface-modified niobium diselenide nanosheets is <5 nm, for example, it can be 4.9 nm, 4.5 nm, 4 nm, 3.5 nm, 3 nm, 2.5 nm, 2 nm, 1.5 nm, 1 nm, etc.

[0100] As an optional implementation, the organic molybdenum includes phosphorus-containing organic molybdenum and / or non-phosphorus organic molybdenum.

[0101] In a preferred embodiment, the organic molybdenum is a non-phosphorus organic molybdenum.

[0102] As an optional implementation, the organic molybdenum is selected from any one or a combination of at least two of the following: molybdenum dithiophosphate complexes, aryl molybdenum dithiophosphate complexes, thiophosphate esters, molybdenum dithiosalicylate complexes, molybdenum dithiocarbamate complexes, organic molybdenum complexes of organic amides, and polyether amino molybdenum complexes.

[0103] In a preferred embodiment, the organic molybdenum is Molyvan 855.

[0104] It should be noted that the preferred non-phosphorus organic molybdenum Molyvan 855 in this invention is a sulfur-free and phosphorus-free organic molybdenum ester / amide complex. Its environmental friendliness stems from its sulfur-free phosphorus component, avoiding the sulfide pollution and catalyst poisoning problems caused by traditional sulfur-containing phosphorus organic molybdenum. It also reduces the risk of eutrophication of water bodies caused by phosphorus. Molybdenum is easily biodegradable, extending lubricant life and reducing waste oil emissions. The product's excellent compatibility relies on its unique molecular structure, possessing both lipophilic alkyl chains and polar ester / amide groups. It is completely miscible with various base oils such as mineral oil, PAO, and ester oils, and works synergistically with detergents, dispersants, and other additives without antagonism. In liquid form, it can be stably dispersed without special processes, making it suitable for various lubrication scenarios. Therefore, it is more environmentally friendly and has good compatibility with different lubricants.

[0105] In a second aspect, the present invention provides a method for preparing a ternary composite functional agent as described in the first aspect, the method comprising: Cerium oxide and niobium diselenide nanosheets were surface-modified separately to prepare surface-modified cerium oxide nanosheets and surface-modified niobium diselenide nanosheets; then, the surface-modified cerium oxide nanosheets, surface-modified niobium diselenide nanosheets and organic molybdenum were mixed to obtain the ternary composite functional agent.

[0106] As an optional implementation, the surface-modified nano-cerium oxide is prepared by the following steps: (A) The cerium source and alkaline solution are mixed and a precipitation reaction is carried out to obtain a suspension containing cerium hydroxide precursor (which can be regarded as hydrated cerium oxide); (B) Add long-chain fatty amines and / or long-chain fatty acids dropwise to the suspension containing the cerium hydroxide precursor to carry out an in-situ modification reaction, thereby obtaining a suspension containing the surface-modified precursor; (C) Introduce oxygen-containing gas into the suspension containing the surface-modified precursor to carry out an oxidation reaction and obtain surface-modified nano-cerium oxide.

[0107] As an optional implementation, in step (A), the cerium source is selected from any one or a combination of at least two of cerium ammonium nitrate, cerium nitrate, and cerium oxide.

[0108] In a preferred embodiment, in step (A), the cerium source is selected from cerium ammonium nitrate.

[0109] As an optional implementation, in step (A), the molar ratio of the cerium source and the alkaline solute in the alkaline solution is 1:(4~12), for example, it can be 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, etc.

[0110] As an optional implementation, in step (A), the alkaline solution is an aqueous solution of an alkali metal hydroxide.

[0111] As an optional implementation, in step (A), the alkaline solution is an aqueous solution of sodium hydroxide.

[0112] As an optional implementation, in step (A), the solid content of the alkaline solution (i.e., the mass fraction of the alkaline solute in the alkaline solution) is 10~30 wt%, for example, it can be 10 wt%, 12 wt%, 14 wt%, 16 wt%, 18 wt%, 20 wt%, 22 wt%, 24 wt%, 26 wt%, 28 wt%, 30 wt%, etc.

[0113] As an optional implementation, in step (A), the temperature of the precipitation reaction is 55~65℃, for example, it can be 55℃, 56℃, 58℃, 60℃, 62℃, 64℃, 65℃, etc.

[0114] As an optional implementation, in step (A), the precipitation reaction time is 0.5 to 5 h, for example, it can be 0.5 h, 1 h, 1.5 h, 2 h, 2.5 h, 3 h, 3.5 h, 4 h, 4.5 h, 5 h, etc.

[0115] In a preferred embodiment, the precipitation reaction in step (A) takes 0.8 to 2 hours.

[0116] In a more preferred embodiment, in step (A), the precipitation reaction time is 1 to 1.5 h.

[0117] As an optional implementation, in step (A), the pH of the system needs to be controlled at 9.0~9.5 during the precipitation reaction process, for example, it can be 9.0, 9.1, 9.2, 9.3, 9.4, 9.5, etc.

[0118] As an optional implementation, in step (B), the molar ratio of the long-chain fatty amine to cerium is (1.5~3):1, for example, it can be 1.5:1, 1.6:1, 1.8:1, 2:1, 2.2:1, 2.4:1, 2.6:1, 2.8:1, 3:1, etc.

[0119] As an optional implementation, in step (B), the molar ratio of the long-chain fatty acid to cerium is (1.5~3):1, for example, it can be 1.5:1, 1.6:1, 1.8:1, 2:1, 2.2:1, 2.4:1, 2.6:1, 2.8:1, 3:1, etc.

[0120] As an optional implementation, in step (B), the dripping time is controlled within 30 minutes, for example, it can be 30 minutes, 29 minutes, 28 minutes, 27 minutes, 26 minutes, 25 minutes, 24 minutes, 23 minutes, 22 minutes, 21 minutes, 20 minutes, etc.

[0121] As an optional implementation, in step (B), the temperature of the in-situ modification reaction is 75~85℃, for example, it can be 75℃, 76℃, 78℃, 80℃, 82℃, 84℃, 85℃, etc.

[0122] As an optional implementation, in step (B), the in-situ modification reaction time is 2 to 6 hours, for example, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours, 6 hours, etc.

[0123] In a preferred embodiment, the in-situ modification reaction in step (B) takes 3 to 4 hours.

[0124] As an optional implementation, in step (C), the oxygen-containing gas is air.

[0125] As an optional implementation, in step (C), the temperature of the oxidation reaction is 100~120℃, for example, it can be 100℃, 102℃, 104℃, 106℃, 108℃, 110℃, 112℃, 114℃, 116℃, 118℃, 120℃, etc.

[0126] As an optional implementation, in step (C), the oxidation reaction time is 2 to 6 hours, for example, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours, 6 hours, etc.

[0127] In a preferred embodiment, the oxidation reaction in step (C) takes 3 to 4 hours.

[0128] As an optional implementation, the oxidation reaction further includes the following post-processing steps: The suspension obtained after the oxidation reaction is mixed with an organic solvent and extracted to collect the organic phase. The organic phase is then concentrated and dispersed using an oil solvent. After shearing, a dispersion of surface-modified nano-cerium oxide is obtained.

[0129] As an optional implementation, in the process of preparing the dispersion of the surface-modified nano-cerium oxide, the organic solvent is cyclohexane.

[0130] As an optional implementation, in the process of preparing the dispersion of the surface-modified nano-cerium oxide, the oil solvent is selected from any one or a combination of at least two of PAO2 base oil, PAO4 base oil, PAO6 base oil, 4cst base oil, 6cst base oil, GTL base oil, and cycloalkyl mineral oil.

[0131] As an optional implementation, in the process of preparing the dispersion of the surface-modified nano-cerium oxide, the concentration is carried out by vacuum distillation. The temperature of the vacuum distillation is 70~80℃, for example, 70℃, 72℃, 74℃, 76℃, 78℃, 80℃, etc., and the pressure of the vacuum distillation is (gauge pressure) -0.10~-0.05 MPa, for example, -0.10 MPa, -0.09 MPa, -0.08 MPa, -0.07 MPa, -0.06 MPa, -0.05 MPa, etc.

[0132] As an optional implementation, during the preparation of the surface-modified nano-cerium oxide dispersion, vacuum distillation is performed until the distillate is substantially solvent-free.

[0133] As an optional implementation, during the preparation of the surface-modified nano-cerium oxide dispersion, solvent-free distillation is carried out and the moisture content of the distilled material (Karl Fischer method) is ≤2000 ppm.

[0134] In a preferred embodiment, during the preparation of the surface-modified nano-cerium oxide dispersion, solvent-free distillation is carried out and the moisture content of the distilled material (Karl Fischer method) is ≤1000 ppm.

[0135] As a more preferred embodiment, during the preparation of the surface-modified nano-cerium oxide dispersion, solvent-free distillation is carried out and the moisture content of the distilled material (Karl Fischer method) is ≤500 ppm.

[0136] As an optional implementation, in the process of preparing the dispersion of the surface-modified nano-cerium oxide, the shearing treatment is carried out using any one of the following devices: a high-shear emulsifier, a homogenizer, or a colloid mill.

[0137] As an optional implementation, during the preparation of the surface-modified nano-cerium oxide dispersion, the rotation speed of the shearing treatment is 1000~3000 rpm, for example, 1000 rpm, 1200 rpm, 1400 rpm, 1600 rpm, 1800 rpm, 2000 rpm, 2200 rpm, 2400 rpm, 2600 rpm, 2800 rpm, 3000 rpm, etc., and the shearing treatment time is 0.5~2 h, for example, 0.5 h, 0.6 h, 0.8 h, 1 h, 1.2 h, 1.4 h, 1.6 h, 1.8 h, 2 h, etc.

[0138] As an optional implementation, in the dispersion of surface-modified nano-cerium oxide, the particle size D50 of the nano-cerium oxide is ≤50 nm, for example, it can be 50 nm, 45 nm, 40 nm, 35 nm, 30 nm, 25 nm, 20 nm, 15 nm, 10 nm, 5 nm, 1 nm, etc.; the solid content of the nano-cerium oxide is 30~50 wt%, for example, it can be 30 wt%, 32 wt%, 34 wt%, 36 wt%, 38 wt%, 40 wt%, 42 wt%, 44 wt%, 46 wt%, 48 wt%, 50 wt%, etc.

[0139] As an optional implementation, the particle size D50 of the surface-modified nano-cerium oxide dispersion is measured by a laser particle size analyzer or dynamic light scattering after the dispersion is diluted in a certain proportion and pre-dispersed by ultrasonic / shear.

[0140] As an optional implementation, the surface-modified niobium diselenide nanosheets are prepared by the following steps: Long-chain fatty amines and / or long-chain fatty acids, along with niobium diselenide nanosheets, are mixed and modified to obtain surface-modified niobium diselenide nanosheets.

[0141] As an optional implementation, the niobium diselenide nanosheets are exfoliated before the modification reaction.

[0142] It should be noted that the core of the pre-modification exfoliation of niobium diselenide nanosheets is to break the interlayer van der Waals forces, reduce the multilayer / bulk material to a few layers / single layer, expose more edge and basal active sites, increase the specific surface area, and allow the modifying reagent to fully contact and react uniformly. As a typical layered two-dimensional metal chalcogenide, niobium diselenide (NbSe2) is most commonly exfoliated using three methods: mechanical exfoliation, liquid phase exfoliation, and intercalation-assisted exfoliation.

[0143] As an optional implementation method, the mechanical exfoliation method is the most classic and commonly used. It involves using adhesive tape to peel off NbSe2 blocks and then using external force to obtain few-layer / single-layer nanosheets. This method is simple to operate, produces highly crystalline sheets with few defects, and is suitable for small-scale laboratory preparation and high-performance device development.

[0144] As an optional implementation method, the liquid phase exfoliation method involves dispersing bulk NbSe2 in a suitable solvent (such as NMP or a water-based dispersion), and then performing interlayer exfoliation by ultrasonication and / or ball milling. This method is simple to operate, can be used for batch preparation, has good dispersibility, and is suitable for subsequent solution phase modification and composite material preparation.

[0145] As an optional implementation method, the intercalation-assisted exfoliation method involves inserting a chemical intercalating agent (such as an alkali metal or an organic amine) into the NbSe2 interlayer to expand the interlayer spacing and weaken van der Waals forces, followed by exfoliation via ultrasound and / or centrifugation. This method has high exfoliation efficiency and high sheet yield, making it suitable for large-scale preparation of few-layer nanosheets.

[0146] As an optional implementation, the molar ratio of the long-chain fatty amine to niobium diselenide (calculated as NbSe2) is (5~20):1, for example, it can be 5:1, 6:1, 8:1, 10:1, 12:1, 14:1, 16:1, 18:1, 20:1, etc.

[0147] In a preferred embodiment, the molar ratio of the long-chain fatty amine to niobium diselenide (calculated as NbSe2) is (8~15):1.

[0148] As a more preferred embodiment, the molar ratio of the long-chain fatty amine to niobium diselenide (calculated as NbSe2) is (9~12):1.

[0149] As an optional implementation, the molar ratio of the long-chain fatty acid to niobium diselenide (calculated as NbSe2) is (5~20):1, for example, it can be 5:1, 6:1, 8:1, 10:1, 12:1, 14:1, 16:1, 18:1, 20:1, etc.

[0150] In a preferred embodiment, the molar ratio of the long-chain fatty acid to niobium diselenide (calculated as NbSe2) is (8~15):1.

[0151] As a more preferred embodiment, the molar ratio of the long-chain fatty acid to niobium diselenide (calculated as NbSe2) is (8~15):1.

[0152] As an optional implementation, the temperature of the modification reaction is 170~190℃, for example, it can be 170℃, 172℃, 174℃, 176℃, 178℃, 180℃, 182℃, 184℃, 186℃, 188℃, 190℃, etc.

[0153] As an optional implementation, the pressure of the modification reaction is 0.8~1.0 MPa, for example, it can be 0.8 MPa, 0.85 MPa, 0.9 MPa, 0.95 MPa, 1.0 MPa, etc.

[0154] As an optional implementation, the modification reaction time is 12 to 36 hours, for example, 12 hours, 14 hours, 16 hours, 18 hours, 20 hours, 22 hours, 24 hours, 26 hours, 28 hours, 30 hours, 32 hours, 34 hours, 36 hours, etc.

[0155] As an optional implementation, the following post-processing steps are further included after the modification reaction is completed: The reaction slurry obtained from the modification reaction was centrifuged and the supernatant was collected. The supernatant was mixed with an azeotropic agent, concentrated, and then dispersed using an oil solvent. After shearing, a dispersion of surface-modified niobium diselenide nanosheets was obtained.

[0156] As an optional implementation, the centrifugation speed is 7000~9000 rpm, for example, it can be 7000 rpm, 7200 rpm, 7400 rpm, 7600 rpm, 7800 rpm, 8000 rpm, 8200 rpm, 8400 rpm, 8600 rpm, 8800 rpm, 9000 rpm, etc.

[0157] As an optional implementation, the azeotropic agent includes any one or a combination of at least two of toluene, methylcyclohexane, cyclohexane, and n-heptane.

[0158] As an optional implementation, the mass ratio of the supernatant to the azeotropic agent is 1:(0.5~5), for example, it can be 1:0.5, 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5, 1:5, etc.

[0159] As an optional implementation, in the process of preparing the dispersion of the surface-modified niobium diselenide nanosheets, the oil solvent is selected from any one or a combination of at least two of PAO2 base oil, PAO4 base oil, PAO6 base oil, 4cst base oil, 6cst base oil, GTL base oil, and cycloalkyl mineral oil.

[0160] As an optional implementation, in the process of preparing the dispersion of the surface-modified niobium diselenide nanosheets, the concentration is carried out by vacuum distillation. The temperature of the vacuum distillation is 70~110℃, for example, 70℃, 75℃, 80℃, 85℃, 90℃, 95℃, 100℃, 105℃, 110℃, etc., and the pressure of the vacuum distillation is -0.10~-0.05 MPa, for example, -0.1 MPa, -0.09 MPa, -0.08 MPa, -0.07 MPa, -0.06 MPa, -0.05 MPa, etc.

[0161] As an optional implementation, during the preparation of the dispersion of the surface-modified niobium diselenide nanosheets, the rotation speed of the shearing treatment is 8000~12000 rpm, for example, 8000 rpm, 8500 rpm, 9000 rpm, 9500 rpm, 10000 rpm, 11000 rpm, 12000 rpm, etc., and the shearing treatment time is 0.5~2 h, for example, 0.5 h, 0.6 h, 0.8 h, 1 h, 1.2 h, 1.4 h, 1.5 h, 1.6 h, 1.8 h, 2 h, etc.

[0162] As an optional implementation, in the dispersion of the surface-modified niobium diselenide nanosheets, the sheet thickness of the niobium diselenide nanosheets is <5 nm, for example, it can be 4.9 nm, 4.5 nm, 4 nm, 3.5 nm, 3 nm, 2.5 nm, 2 nm, 1.5 nm, 1 nm, etc.; the solid content of the niobium diselenide nanosheets is 5~20 wt%, for example, it can be 5 wt%, 6 wt%, 8 wt%, 10 wt%, 12 wt%, 14 wt%, 16 wt%, 18 wt%, 20 wt%, etc.

[0163] Thirdly, the present invention provides the application of the ternary composite functional agent as described in the first aspect in the preparation of lubricating media, greases and semi-solid lubricants, metal processing and forming media, lubricating preparations for assembly-anti-jamming and maintenance, dry film lubrication and functional coatings, industrial condition monitoring and predictive maintenance products, leak tracing and fault location products, oil authenticity identification and supply chain traceability products, anti-counterfeiting materials and ink products, smart packaging and quality indicators, and self-lubrication and wear resistance enhancement of polymers and composite materials.

[0164] It should be noted that the ternary composite functional agent described in this invention can be used not only in lubricating oil systems, but also in the following scenarios (not limited to these): (1) Full spectrum expansion of lubricating media: It can be used for various industrial and transportation fluids other than engine oil, including but not limited to: industrial gear oil, wind power gearbox oil, hydraulic oil, circulating oil, turbine oil, compressor oil, vacuum pump oil, slideway oil, chain oil, open gear jet lubricant, wire rope lubricant, etc.

[0165] (2) Greases and semi-solid lubricants: It can be used for high-temperature grease, heavy-duty bearing grease, gear grease, steel plant water spray grease, mining heavy-duty grease, wind power pitch / yaw grease, construction machinery pin grease, railway and military wide-temperature grease, etc., to achieve anti-wear and friction reduction, extreme pressure bearing and long-term stable dispersion, and facilitate quick identification and maintenance on site.

[0166] (3) Metal processing and forming media: It can be used as an extreme pressure anti-wear and friction-reducing additive in various metal processing and forming lubrication systems, including but not limited to: cutting oil, grinding oil, tapping oil, drawing oil, stamping oil, rolling oil, cold heading / extrusion forming lubricant, forging lubricant, etc.; it can also be used in water-based processing fluids (emulsified, semi-synthetic, fully synthetic) to improve boundary lubrication and extreme pressure performance, and support rapid identification and management of concentration / ratio.

[0167] (4) Lubricants for assembly, anti-jamming, and maintenance: It can be used in thread anti-seize paste, assembly lubricant, guide rail anti-creep lubricant, seal assembly lubricant, industrial maintenance spray, etc., to achieve anti-seize, anti-wear and surface repair under heavy-load contact and boundary lubrication conditions, and can realize visual identification and inspection.

[0168] (5) Dry film lubrication and functional coatings: It can be used as a wear-resistant and friction-reducing functional component in dry film lubricants, sliding coatings, wear-resistant coatings, anti-scratch varnishes, mold lubrication / release coatings, and tool / mold surface friction-reducing coatings to form a low shear strength protective layer and provide visual recognition capabilities.

[0169] (6) Industrial condition monitoring and predictive maintenance products: It can be used for equipment oil / grease condition monitoring and maintenance decision-making, including but not limited to: oil change / grease replenishment cycle determination, additive consumption trend judgment, early warning of abnormal wear, and identification of deterioration of operating conditions; it is suitable for scenarios that require rapid inspection and reliable maintenance, such as centralized lubrication stations, wind turbine nacelles, heavy-duty mining equipment, steel mill rolling mills, railway locomotives, and military equipment.

[0170] (7) Leakage tracing and fault location products: It can be used for rapid leak location, pollution source tracking and cleaning confirmation in scenarios such as hydraulic systems, circulating oil systems, gearboxes, ship engine rooms, and construction machinery, improving maintenance efficiency and reducing downtime losses.

[0171] (8) Oil product authenticity identification and supply chain traceability products: It can be used for batch identification of high-value lubricants, specialty oils and greases, channel anti-counterfeiting, verification and sampling inspection and traceability management, forming a "formula-level fingerprint" for quality management and brand protection.

[0172] (9) Anti-counterfeiting materials and inks: It can be used for anti-counterfeiting inks, anti-counterfeiting coatings, anti-counterfeiting labels / seals, tamper-evident markings, etc., and is suitable for industrial spare parts, military products, certificates, anti-counterfeiting packaging and high-value products. It supports rapid identification and high-security level recognition.

[0173] (10) Smart packaging and quality indication products: It can be used for indication and acceptance sampling inspection of the transportation process of barrelled / boxed oil products and high-value components, such as heat, pressure and vibration, to achieve visualized quality control in the warehousing / delivery process.

[0174] (11) Self-lubricating and wear-resistant reinforcement of polymers and composite materials: It can be used in self-lubricating engineering plastics, rubber sealing materials, resin-based composite materials and other systems, as a functional filler for wear resistance, friction reduction and visual identification, serving sliding parts, bushings, guide rails, seals and other components.

[0175] (12) Other scalable directions It can be used as a multifunctional nano-friction-reducing / catalytic / tracer component in special adhesives, wear-resistant repair agents, industrial maintenance composites and other systems to provide friction reduction, wear resistance and identifiable features.

[0176] As an optional implementation, the ternary composite functional agent is used in the preparation of industrial lubricating materials, automotive lubricating materials, metal processing lubricating materials, military equipment lubricating materials, anti-counterfeiting materials, and smart packaging.

[0177] As an optional implementation, the application of the ternary composite functional agent in the preparation of engine oil for fuel engines is to add the ternary composite functional agent to the engine oil of the fuel engine.

[0178] It should be noted that after adding the aforementioned ternary composite functional agent to the engine oil of the fuel engine, its nano-components penetrate into the combustion chamber periphery along with the lubricating oil. Nano-cerium oxide (CeO2), with its unique oxygen vacancy effect and catalytic activity, significantly promotes the oxidation and combustion of soot particles at high temperatures, effectively reducing the activation energy of the combustion reaction, thereby reducing carbon deposits and particulate matter formation at the source. Simultaneously, niobium diselenide (NbSe2) nanosheets synergistically work with organic molybdenum to form an extremely tough, low-shear-strength protective film on the surface of the friction pairs inside the engine, significantly reducing the coefficient of friction and wear. This improves fuel economy, helps enhance power output stability, and contributes to improved emissions performance. Furthermore, its built-in fluorescence monitoring function provides an intuitive and scientific basis for quality-based oil changes through color changes (yellow-green for new oil, blue for degraded oil).

[0179] As an optional implementation, the application of the ternary composite functional agent in the preparation of engine oil for gas (natural gas, liquefied gas, hydrogen) engines involves adding the ternary composite functional agent to the engine oil of the gas (natural gas, liquefied gas, hydrogen) engine.

[0180] It should be noted that after adding the aforementioned ternary composite functional agent to the engine oil of the gas engine, its nanomaterials can form a robust lubricating film on the friction surface under high loads, greatly alleviating the wear problem of the valve system unique to gas engines. The excellent thermal stability and antioxidant properties of nano-cerium oxide (CeO2) can effectively inhibit the oxidative deterioration of the engine oil at high temperatures, delaying oil degradation and potentially extending the oil change interval. More importantly, its fluorescence monitoring characteristics provide a powerful tool for predictive engine maintenance, allowing for rapid assessment of the engine oil condition using a UV lamp without disassembly, ensuring operational safety. Furthermore, its built-in fluorescence monitoring function provides an intuitive and scientific basis for quality-based oil changes through color changes (yellow-green for new oil, blue for degraded oil).

[0181] As an optional implementation, the application of the ternary composite functional agent in the preparation of engine oil for methanol / ethanol engines is to add the ternary composite functional agent to the engine oil for methanol / ethanol engines.

[0182] It should be noted that after adding the aforementioned ternary composite functional agent to the engine oil of the methanol / ethanol engine, its nano-cerium oxide (CeO2) can efficiently catalyze the combustion process of methanol / ethanol, making it more complete and thorough, thereby significantly reducing the generation of unburned alcohol fuel and harmful emissions such as formaldehyde. Its alkaline surface can also effectively neutralize acidic substances produced during combustion, fundamentally slowing down corrosion inside the engine. After application, it not only improves the engine's low-temperature starting performance but also effectively protects the engine from fuel corrosion, inhibits early acidification and emulsification of the engine oil, and ensures the engine's durability under harsh fuel conditions. Furthermore, its built-in fluorescent monitoring function provides an intuitive and scientific basis for quality-based oil changes through color changes (yellow-green for new oil, blue for degraded oil).

[0183] As an optional implementation, the application of the ternary composite functional agent in the preparation of engine oil for hybrid engines is to add the ternary composite functional agent to the engine oil of the hybrid engine.

[0184] It should be noted that after adding the aforementioned ternary composite functional agent to the engine oil of the hybrid engine, its nanomaterials can provide instantaneous anti-wear protection against frequent start-stop cycles, acting immediately upon startup to greatly reduce wear during this phase. The strong antioxidant properties of nano-cerium oxide (CeO2) help maintain the oil's performance stability throughout its long lifespan, adapting to the complex operating environment of the hybrid system. Its unique fluorescence ratio monitoring function can accurately track the oil's performance degradation process, providing reliable data support for scientific, condition-based predictive maintenance under complex operating conditions, a key technology for achieving long-life, high-reliability operation of hybrid vehicles. Furthermore, its built-in fluorescence monitoring function provides an intuitive and scientific basis for quality-based oil changes through color changes (yellow-green for new oil, blue for degraded oil).

[0185] Thirdly, the present invention provides a lubricating oil comprising the ternary composite functional agent as described in the first aspect.

[0186] As an optional implementation, the amount of the ternary composite functional agent added is 0.1% to 10.0% of the total mass of the lubricating oil, for example, it can be 0.1%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5%, 5.0%, 5.5%, 6.0%, 6.5%, 7.0%, 7.5%, 8.0%, 8.5%, 9.0%, 9.5%, 10.0%, etc.

[0187] In a preferred embodiment, the amount of the ternary composite functional agent added is 1.7 to 6.0% of the total mass of the lubricating oil.

[0188] As an optional implementation, the lubricating oil, based on its total mass of 100%, comprises: 1-3% surface-modified nano-cerium oxide (e.g., 1%, 1.2%, 1.4%, 1.6%, 1.8%, 2%, 2.2%, 2.4%, 2.6%, 2.8%, 3%, etc.), 0.2-1% surface-modified niobium diselenide nanosheets (e.g., 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, etc.), 0.5-2% organic molybdenum (e.g., 0.5%, 0.6%, 0.8%, 1%, 1.2%, 1.4%, 1.6%, 1.8%, 2%, etc.), with the balance being oil solvent.

[0189] As an optional implementation, the oil solvent in the lubricating oil is selected from any one or a combination of at least two of PAO2 base oil, PAO4 base oil, PAO6 base oil, 4cst base oil, 6cst base oil, GTL base oil, and naphthenic mineral oil.

[0190] The present invention will be further illustrated by the following examples. Unless otherwise specified, the materials in the examples are prepared according to existing methods or purchased directly from the market.

[0191] It is understood that the ternary composite functional agent provided by this invention can be tested for its performance using a "fluorescent" product (application number: 202610570553.3).

[0192] Example 1 This embodiment provides a ternary composite functional agent and a lubricating oil containing the same, wherein the ternary composite functional agent and the lubricating oil containing the same are prepared by the following steps: The surface-modified cerium oxide nanoparticles are prepared by the following steps: (A) Precipitation reaction: In a reaction vessel, 10 wt% aqueous solution of cerium ammonium nitrate and 20 wt% aqueous solution of NaOH (molar ratio of cerium ammonium nitrate and NaOH is 1:8) are mixed and reacted at 60±2℃ for 1 h. The pH is strictly controlled at 9.0~9.5 to generate cerium hydroxide precursor precipitate and obtain a suspension containing cerium hydroxide precursor. (B) In-situ modification: The oleylamine was added dropwise to the suspension of the cerium hydroxide precursor obtained in step (A) within 30 min at a molar ratio of oleylamine to cerium of 2:1. The mixture was stirred at 80±2℃ and 120 rpm for 4 h to complete the organic coating of the precursor particles and obtain a suspension of the surface-modified precursor. (C) Oxidation and solvent replacement: The temperature of the suspension containing the surface-modified precursor obtained in step (B) is raised to 110±2℃, and purified air is introduced for oxidation for 6 h until the material turns bright yellow, indicating that it has been completely converted into cerium oxide; after cooling, cyclohexane is added for liquid-liquid extraction, and the organic phase containing oleylamine-modified nano-cerium oxide is collected. (D) Concentration and blending: The organic phase obtained in step (C) was distilled under reduced pressure at 75°C and -0.08 MPa to completely remove cyclohexane and water; then, it was blended and dispersed with PAO4 base oil and subjected to high shear (2000 rpm, 1 h) to obtain a stable dispersion of oil-containing amine-modified nano-cerium oxide with a solid content of 40wt%.

[0193] Quality inspection standard: The surface-modified nano-cerium oxide has a D50 ≤ 50 nm (laser particle size analyzer, referring to the particle size after dispersion); no precipitation occurs after standing at room temperature for 30 days.

[0194] The surface-modified niobium diselenide nanosheets are prepared by the following steps: (a) Liquid phase exfoliation and modification: Niobium diselenide powder and ethanol aqueous solution at a mass ratio of 1:20 (V 乙醇 :V 去离子水 The mixture (niobium diselenide powder, ... (b) Centrifugal purification: After cooling the reaction slurry obtained in step (a), centrifuge it at 8000 rpm using a tubular centrifuge to remove the unpeeled thick-layer particles and collect the supernatant rich in surface-modified niobium diselenide nanosheets. (c) Solvent replacement and concentration: An azeotropic agent (toluene) was added to the supernatant obtained in step (b), and free alkylamines and water were completely removed by vacuum distillation at 90°C and -0.08 MPa; the mixture was then prepared with PAO4 base oil and homogenized by high-shear emulsification at 10,000 rpm to obtain a uniform gray-black dispersion of niobium diselenide nanosheets with a solid content of 10 wt%.

[0195] The lubricating oil is prepared by the following steps: A stable dispersion of cerium nano-oxide modified with 40 wt% oleylamine, a uniform gray-black dispersion of niobium diselenide nanosheets modified with 10 wt% oleylamine, and organic molybdenum Molyvan 855 were added to PAO6 base oil to obtain a lubricating oil containing the ternary composite functional agent. The lubricating oil containing the ternary composite functional agent comprises: 2% surface-modified cerium nano-oxide, 0.6% surface-modified niobium diselenide nanosheets, 1.4% organic molybdenum Molyvan 855, and the balance being PAO6 base oil.

[0196] Example 2 This embodiment provides a ternary composite functional agent and a lubricating oil containing the same. The only difference from Embodiment 1 is that the lubricating oil containing the ternary composite functional agent includes: 1.5% surface-modified nano-cerium oxide, 0.3% surface-modified niobium diselenide nanosheets, 0.8% organic molybdenum Molyvan 855, and the balance being PAO6 base oil. The other steps are the same as in Embodiment 1.

[0197] Example 3 This embodiment provides a ternary composite functional agent and a lubricating oil containing the same. The only difference from Embodiment 1 is that the lubricating oil containing the ternary composite functional agent includes: 2.5% surface-modified nano-cerium oxide, 1.0% surface-modified niobium diselenide nanosheets, 1.5% organic molybdenum Molyvan 855, and the balance is PAO6 base oil. The other steps are the same as in Embodiment 1.

[0198] Example 4 This embodiment provides a ternary composite functional agent and a lubricating oil containing it. The only difference from Example 1 is that the oleamine selected in the preparation process of the surface-modified cerium oxide nanosheets and the surface-modified niobium diselenide nanosheets is replaced with laurylamine. The other steps are the same as in Example 1.

[0199] Example 5 This embodiment provides a ternary composite functional agent and a lubricating oil containing it. The only difference from Example 1 is that the oleamine selected in the preparation process of the surface-modified cerium oxide nanosheets and the surface-modified niobium diselenide nanosheets is replaced with erucic acid amine. The other steps are the same as in Example 1.

[0200] Example 6 This embodiment provides a ternary composite functional agent and a lubricating oil containing it. The only difference from Example 1 is that the modifier selected in the preparation process of surface-modified cerium oxide nanosheets and surface-modified niobium diselenide nanosheets is replaced by myristic acid (as a long-chain fatty acid modifier) ​​instead of oleylamine. The other steps are the same as in Example 1.

[0201] Example 7 This embodiment provides a ternary composite functional agent and a lubricating oil containing it. The only difference from Example 1 is that the modifier selected in the preparation process of surface-modified cerium oxide nanosheets and surface-modified niobium diselenide nanosheets is replaced by arachidonic acid (as a long-chain fatty acid modifier) ​​instead of oleylamine. The other steps are the same as in Example 1.

[0202] Comparative Example 1 This comparative example provides a 100% PAO6 base oil.

[0203] Comparative Example 2 This comparative example provides a lubricating oil comprising: 2% unmodified cerium oxide, 0.6% unmodified niobium diselenide, 1.4% organic molybdenum Molyvan 855, and the balance being PAO6 base oil.

[0204] Comparative Example 3 This comparative example provides a lubricating oil comprising: 1.6% surface-modified niobium diselenide nanosheets prepared in Example 1, 2.4% organic molybdenum Molyvan 855, and the balance being PAO6 base oil.

[0205] Comparative Example 4 This comparative example provides a lubricating oil comprising: 2.3% surface-modified nano-cerium oxide prepared in Example 1, 1.7% organic molybdenum Molyvan 855, and the balance being PAO6 base oil.

[0206] Comparative Example 5 This comparative example provides a lubricating oil comprising: 2.7% surface-modified nano-cerium oxide prepared in Example 1, 1.3% surface-modified niobium diselenide nanosheets prepared in Example 1, and the balance being PAO6 base oil.

[0207] Test Example 1 Test samples: Lubricating oils provided in Examples 1-7 and Comparative Examples 1-5; The test characteristics and test results are shown in Table 1 below: Table 1

[0208] As shown by the exemplary theoretical data in Table 1, the friction coefficient and wear scar diameter of the lubricating oil after adding the ternary composite functional agent described in this invention are significantly reduced, which can reduce the wear of key friction pairs of equipment and extend its service life. The maximum non-seize load (PB value) and sintering load (PD value) are significantly improved. The significant increase in PB value and PD value enhances the extreme pressure bearing capacity, making it suitable for heavy loads and extreme working conditions, and avoiding seize and sintering failures. At the same time, the ternary composite functional agent can display strong yellow-green fluorescence with stable ratios, which can realize the quantitative assessment of the degree of oil deterioration and the accurate prediction of remaining life, providing data support for the optimization of equipment maintenance cycles. This fluorescence characteristic can be further extended to the field of oil quality control: by comparing the fluorescence spectral characteristics of standard samples and test samples, the authenticity of oil can be quickly identified.

[0209] As shown in Table 1, compared with Comparative Examples 1-5, the lubricating oils containing the ternary composite functional agent of the present invention described in Examples 1-7 exhibit superior overall performance in terms of friction coefficient, wear scar diameter, maximum non-seizure load (PB value), and sintering load (PD value). Specifically, the friction coefficient of Examples 1-7 is 0.043-0.049, significantly lower than the 0.055-0.110 of Comparative Examples 1-5; the wear scar diameter is 0.32-0.36 mm, significantly smaller than the 0.38-0.62 mm of Comparative Examples 1-5; the PB value is 1180-1300 N, and the PD value is ≥2350-2600 N, both higher than those of Comparative Examples 1-5. This indicates that the ternary composite functional agent of the present invention can effectively reduce friction and wear, and improve extreme pressure bearing capacity, thereby helping to reduce wear on key friction pairs of equipment and extend service life.

[0210] As can be seen from the comparison between Example 1 and Comparative Examples 3, 4 and 5, under the condition of consistent lubricating oil matrix, when any of the following components are missing from the formulation: surface-modified nano-cerium oxide, surface-modified niobium diselenide nanosheets or organic molybdenum, the lubrication performance and fluorescence interpretation stability decrease to varying degrees. Specifically, compared to Comparative Example 3, the coefficient of friction in Example 1 decreased from 0.060 to 0.043, the wear scar diameter decreased from 0.40 mm to 0.32 mm, the maximum non-seize load (PB value) increased from 1050 N to 1250 N, and the sintering load (PD value) increased from 2200 N to ≥2500 N; compared to Comparative Example 4, the coefficient of friction in Example 1 decreased from 0.065 to 0.043, the wear scar diameter decreased from 0.42 mm to 0.32 mm, the maximum non-seize load (PB value) increased from 980 N to 1250 N, and the sintering load (PD value) increased from 2100 N to ≥2500 N; compared to Comparative Example 5, the coefficient of friction in Example 1 decreased from 0.055 to 0.043, the wear scar diameter decreased from 0.38 mm to 0.32 mm, the maximum non-seize load (PB value) increased from 1120 N to 1250 N, and the sintering load (PD value) increased from 2300 N to ≥2500 N. N is increased to ≥2500 N.

[0211] The above results indicate that when surface-modified cerium oxide nanosheets, surface-modified niobium diselenide nanosheets, and organic molybdenum are used in combination, they can achieve better overall effects in terms of friction reduction and wear resistance, extreme pressure bearing capacity, and fluorescence ratio signal stability, indicating that the three have a synergistic improvement effect.

[0212] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A ternary composite functional agent, characterized in that, The ternary composite functional agent includes: surface-modified cerium oxide nanoparticles, surface-modified niobium diselenide nanosheets, and organic molybdenum.

2. The ternary composite functional agent according to claim 1, characterized in that, The mass ratio of the surface-modified cerium oxide nanosheets, the surface-modified niobium diselenide nanosheets, and the organic molybdenum is (1~3):(0.2~1):(0.5~2).

3. The ternary composite functional agent according to claim 1 or 2, characterized in that, The surface-modified nano-cerium oxide is nano-cerium oxide modified with long-chain fatty amines and / or long-chain fatty acids. Preferably, the long-chain fatty amine is selected from C12-C22 long-chain fatty amines, more preferably C14-C20 long-chain fatty amines, and even more preferably C16-C18 long-chain fatty amines; Preferably, the long-chain fatty acid is selected from C12-C22 long-chain fatty acids, more preferably C14-C20 long-chain fatty acids, and even more preferably C16-C18 long-chain fatty acids; Preferably, the molar ratio of the long-chain fatty amine to cerium is (1.5~3):1; the molar ratio of the long-chain fatty acid to cerium is (1.5~3):

1. Preferably, the particle size of the surface-modified cerium oxide nanoparticles is ≤50 nm.

4. The ternary composite functional agent according to claim 1 or 2, characterized in that, The surface-modified niobium diselenide nanosheets are niobium diselenide nanosheets modified with long-chain fatty amines and / or long-chain fatty acids. Preferably, the long-chain fatty amine is selected from C12-C22 long-chain fatty amines, more preferably C14-C20 long-chain fatty amines, and even more preferably C16-C18 long-chain fatty amines; Preferably, the long-chain fatty acid is selected from C12-C22 long-chain fatty acids, more preferably C14-C20 long-chain fatty acids, and even more preferably C16-C18 long-chain fatty acids; Preferably, the molar ratio of the long-chain fatty amine to niobium diselenide is (5~20):1; the molar ratio of the long-chain fatty acid to niobium diselenide is (5~20):

1. Preferably, the thickness of the surface-modified niobium diselenide nanosheets is <5 nm.

5. The ternary composite functional agent according to claim 1 or 2, characterized in that, The organic molybdenum includes phosphorus-containing organic molybdenum and / or non-phosphorus organic molybdenum; Preferably, the organic molybdenum is selected from any one or a combination of at least two of the following: molybdenum dithiophosphate complexes, aryl molybdenum dithiophosphate complexes, molybdenum dithiosalicylate complexes, molybdenum dithiocarbamate complexes, organic molybdenum complexes of organic amides, and polyether amino molybdenum complexes.

6. A method for preparing a ternary composite functional agent according to any one of claims 1 to 5, characterized in that, The preparation method includes: Surface-modified cerium oxide precursor and niobium diselenide nanosheets were prepared by surface modification to obtain surface-modified cerium oxide nanosheets and surface-modified niobium diselenide nanosheets; then, the surface-modified cerium oxide nanosheets, surface-modified niobium diselenide nanosheets and organic molybdenum were mixed to obtain the ternary composite functional agent.

7. The preparation method of the ternary composite functional agent according to claim 6, characterized in that, The surface-modified cerium oxide nanoparticles are prepared by the following steps: The cerium source and alkaline solution are mixed to carry out a precipitation reaction, resulting in a suspension containing the cerium hydroxide precursor. Long-chain fatty amines and / or long-chain fatty acids are added dropwise to the suspension containing the cerium hydroxide precursor to carry out an in-situ modification reaction, thereby obtaining a suspension containing the surface-modified precursor. An oxygen-containing gas is introduced into the suspension containing the surface-modified precursor to carry out an oxidation reaction, thereby obtaining surface-modified nano-cerium oxide. Preferably, the cerium source is selected from any one or a combination of at least two of cerium ammonium nitrate, cerium nitrate, and cerium oxide; Preferably, the molar ratio of the cerium source to the alkaline solute in the alkaline solution is 1:(4~12); Preferably, the alkaline solution is an aqueous solution of an alkali metal hydroxide, and more preferably an aqueous solution of sodium hydroxide; Preferably, the solid content of the alkaline solution is 10-30 wt%; Preferably, the precipitation reaction temperature is 55~65℃, and the precipitation reaction time is 0.5~5 h; the pH of the system needs to be controlled at 9.0~9.5 during the precipitation reaction. Preferably, the molar ratio of the long-chain fatty amine to cerium is (1.5~3):1; the molar ratio of the long-chain fatty acid to cerium is (1.5~3):

1. Preferably, the dropping time is controlled within 30 minutes; the temperature of the in-situ modification reaction is 75~85℃, and the time of the in-situ modification reaction is 2~6 hours. Preferably, the oxidation reaction is carried out at a temperature of 100-120°C for 2-6 hours. Preferably, the oxidation reaction further includes the following post-processing steps: The suspension obtained after the oxidation reaction was mixed with an organic solvent and extracted to collect the organic phase. The organic phase was then concentrated and dispersed using an oil solvent. After shearing, a dispersion of surface-modified nano-cerium oxide was obtained. Preferably, the organic solvent is cyclohexane; Preferably, the oil solvent is selected from any one or a combination of at least two of PAO2 base oil, PAO4 base oil, PAO6 base oil, 4cst base oil, 6cst base oil, GTL base oil, and naphthenic mineral oil; Preferably, the concentration is carried out by vacuum distillation, the temperature of which is 70~80℃ and the pressure of which is -0.10~-0.05 MPa; Preferably, the shearing process is carried out using any one of a high-shear emulsifier, a homogenizer, or a colloid mill. Preferably, the rotational speed of the shearing process is 1000~3000 rpm, and the shearing time is 0.5~2 h; Preferably, in the dispersion of the surface-modified nano-cerium oxide, the particle size D50 of the nano-cerium oxide is ≤50 nm; and the solid content of the nano-cerium oxide is 30~50 wt%.

8. The preparation method of the ternary composite functional agent according to claim 6, characterized in that, The surface-modified niobium diselenide nanosheets were prepared by the following steps: Long-chain fatty amines and / or long-chain fatty acids, along with niobium diselenide nanosheets, are mixed and modified to obtain surface-modified niobium diselenide nanosheets. Preferably, the molar ratio of the long-chain fatty amine to niobium diselenide, calculated as NbSe2, is (5~20):1; the molar ratio of the long-chain fatty acid to niobium diselenide, calculated as NbSe2, is (5~20):

1. Preferably, the temperature of the modification reaction is 170~190℃, the pressure of the modification reaction is 0.8~1.0 MPa, and the time of the modification reaction is 12~36 h; Preferably, the modification reaction further includes the following post-processing steps: The reaction slurry obtained from the modification reaction was centrifuged and the supernatant was collected. The supernatant was mixed with an azeotropic agent, concentrated, and then dispersed using an oil solvent. After shearing, a dispersion of surface-modified niobium diselenide nanosheets was obtained. Preferably, the centrifugation speed is 7000~9000 rpm; Preferably, the azeotropic agent includes any one or a combination of at least two of toluene, methylcyclohexane, cyclohexane, and n-heptane; Preferably, the mass ratio of the supernatant to the azeotropic agent is 1:(0.5~5); Preferably, the oil solvent is selected from any one or a combination of at least two of PAO2 base oil, PAO4 base oil, PAO6 base oil, 4cst base oil, 6cst base oil, GTL base oil, and naphthenic mineral oil; Preferably, the concentration is carried out by vacuum distillation, wherein the temperature of vacuum distillation is 70~110℃ and the pressure of vacuum distillation is -0.10~-0.05 MPa; Preferably, the rotational speed of the shearing process is 8000~12000 rpm, and the shearing time is 0.5~2 h; Preferably, in the dispersion of the surface-modified niobium diselenide nanosheets, the thickness of the niobium diselenide nanosheets is <5 nm; and the solid content of the niobium diselenide nanosheets is 5~20 wt%.

9. The application of a ternary composite functional agent according to any one of claims 1 to 5 in the preparation of lubricating media, greases and semi-solid lubricants, metal processing and forming media, lubricating preparations for assembly-anti-jamming and maintenance, dry film lubrication and functional coatings, industrial condition monitoring and predictive maintenance products, leak tracing and fault location products, oil authenticity identification and supply chain traceability products, anti-counterfeiting materials and ink products, smart packaging and quality indicators, and self-lubrication and wear resistance enhancement of polymers and composite materials.

10. A lubricating oil, characterized in that, The lubricating oil includes a ternary composite functional agent as described in any one of claims 1 to 5; Preferably, the amount of the ternary composite functional agent added is 0.1 to 10.0% of the total mass of the lubricating oil.

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