Industrial lubricating oil extreme pressure anti-wear agent containing self-repairing material and preparation method of industrial lubricating oil extreme pressure anti-wear agent
Microcapsules are prepared through polymetallic complexes and phosphate precursors, combined with functionalized MOF materials, and formed a self-healing lubricating film, which solves the wear problem of industrial lubricating oil under extreme conditions, achieves wear resistance and high temperature stability, and improves the comprehensive performance of the lubricant.
Patent Information
- Application Number
- CN202510550263.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-29
- Publication Date
- 2025-08-05
- Estimated Expiration
- 2045-04-29
AI Technical Summary
Existing industrial lubricants are difficult to effectively protect mechanical components under extreme conditions, resulting in wear and equipment failure, and cannot meet the needs of modern industry for high efficiency, long life and high reliability.
Microcapsules are prepared using polymetallic complexes and phosphate precursors, combined with functionalized MOF materials, and synergistically interact with metal-organic frame composite materials through the multifunctional microcapsule technology to form a self-healing lubricating film, providing anti-wear and high temperature stability.
In extreme pressure environments, the friction coefficient is significantly reduced, the service life of lubricant is extended, the wear resistance and high temperature stability of mechanical equipment are improved, and multi-layer lubricating protection is achieved.
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Figure CN120424696A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of lubricating oil additives and relates to an industrial lubricating oil extreme pressure anti-wear agent containing a self-repairing material and a preparation method thereof. Background Art
[0002] Industrial lubricants play a vital role in modern industry and are the core guarantee for the normal operation of mechanical equipment. Their main function is to reduce friction and wear between mechanical parts, extend the service life of equipment, and protect the stable operation of equipment under harsh working conditions such as high temperature, high pressure, heavy load, and high speed. However, relying solely on the basic lubrication properties of the lubricant itself is difficult to meet the needs of modern industry for high efficiency, long life and high reliability. Especially under extreme conditions, such as gear transmission systems, bearings, hydraulic equipment or metal processing scenarios, high loads, high temperatures and high speeds can lead to the rupture of the lubricating oil film and direct contact between metal surfaces, causing severe wear, seizure and even equipment failure. Therefore, in order to further improve the performance of lubricants and meet the stringent requirements of industrial equipment, extreme pressure anti-wear agents have emerged as important functional additives for lubricants.
[0003] The essential function of extreme pressure anti-wear agents is to impart anti-wear and anti-seizure properties to lubricants under extreme operating conditions. By forming a protective film on the metal surface, they effectively reduce the coefficient of friction, minimize direct contact between mechanical components, and prevent wear and plastic deformation of metal materials. Especially under high-load conditions, when the lubricating oil film ruptures due to immense pressure, the extreme pressure anti-wear agent interacts with the metal surface through physical adsorption or chemical reaction, forming a protective film with high shear strength, thereby continuing to protect the metal parts even in the event of lubricant failure. This protective film may be composed of metal sulfides, phosphates, borides, or oxides, and possesses high stability and low friction properties. This characteristic makes extreme pressure anti-wear agents an essential component of high-load industrial equipment and metalworking fluids.
[0004] In practical applications, extreme pressure anti-wear agents are widely used in a variety of lubricant products, including industrial gear oils, hydraulic oils, cutting fluids, and engine oils. For example, in gear transmission systems, extreme pressure anti-wear agents can effectively reduce wear at the gear meshing point and improve gear transmission efficiency. In hydraulic equipment, they can extend equipment life and reduce operating costs. In metalworking, extreme pressure anti-wear agents can reduce friction between tools and workpieces, improving machining accuracy and extending tool life. With the continuous advancement of industrial automation and equipment precision, the market demand for extreme pressure anti-wear agents continues to grow, placing higher demands on lubricant performance. Therefore, the research and development of extreme pressure anti-wear agents has important industrial value. Summary of the Invention
[0005] To address the shortcomings of the existing technology, the present invention aims to provide an extreme pressure anti-wear agent for industrial lubricants containing self-healing materials and a method for preparing the same. This method utilizes the synergistic effects of multifunctional microcapsule technology and metal-organic framework composites to enhance the anti-wear performance and high-temperature stability of lubricants. First, microcapsules are prepared using a multimetallic complex and a phosphate precursor via emulsification technology. The core contains the multimetallic active component and the outer shell is coated with a resin material to ensure its dispersibility and stability in the lubricant. Second, a functionalized MOF material is used to introduce active groups such as sulfur and phosphorus and a composite modifying component to prepare a MOF composite with enhanced lubricity and anti-wear properties. Finally, the microcapsules are mixed with the functionalized MOF composite to produce an extreme pressure anti-wear agent, thus meeting the needs of practical production.
[0006] To achieve this object, the present invention adopts the following technical solutions:
[0007] In a first aspect, the present invention provides a method for preparing an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material, the preparation method comprising:
[0008] A1. Disperse ammonium molybdate in the first portion of deionized water, sodium tungstate in the second portion of deionized water, and ammonium cerium nitrate in the third portion of deionized water. Add the ammonium molybdate solution to the sodium tungstate solution, then add the ammonium cerium nitrate solution, and add citric acid to adjust the pH to 6 to obtain a multi-metal complex solution.
[0009] A2, dispersing phosphoric acid and boric acid in deionized water, adjusting the temperature to 60°C and stirring to obtain a phosphate solution, then dispersing boron nitride in anhydrous ethanol and adding the solution to the phosphate solution, adjusting the pH to 7, to obtain a phosphate precursor;
[0010] S1, mixing a multi-metal complex solution, a phosphate precursor, butylated hydroxytoluene, and isopropyl alcohol, adjusting the temperature to a first temperature and stirring to obtain a core phase solution, dispersing urea and formaldehyde solution in deionized water, adjusting the pH to 7, heating to 70°C, adding benzaldehyde oxime and stirring to obtain a urea-formaldehyde resin precursor, dispersing the urea-formaldehyde resin precursor and melamine formaldehyde resin in deionized water, adding 1% by mass ammonium chloride solution and adjusting the pH to 4.5 to obtain a shell phase solution, then mixing the core phase solution and the shell phase solution with an emulsifier, adjusting the temperature to a second temperature and stirring, centrifuging, washing, and vacuum drying to obtain microcapsules;
[0011] S2, placing MOF at a third temperature for insulation to obtain an activated MOF, dispersing the activated MOF and 1,2-ethanedithiol in a first portion of DMF, allowing to stand at room temperature and then centrifugally drying to obtain an anti-wear component MOF, dispersing 1-ethyl-3-methylimidazoline bis(trifluoromethylsulfonyl)imide, bismaleimide and ammonium persulfate in a second portion of DMF, mixing evenly and then adding the anti-wear component MOF, adjusting the temperature to the second temperature under a nitrogen atmosphere and stirring, then adding the zinc ion solution and continuing to stir, after the reaction is completed, centrifugally washing and drying to obtain a MOF@PIL composite powder, mixing the microcapsules with the MOF@PIL composite powder to obtain an industrial lubricant extreme pressure anti-wear agent containing self-healing materials.
[0012] Ammonium molybdate and sodium tungstate are the core precursor substances in the present invention, which form molybdate and tungstate anions respectively after dissolution. These anions are the basic building blocks of polyoxometallic clusters. Molybdenum and tungsten are transition metals of the same family, and their chemical properties are highly similar, especially in solution, they can aggregate through oxygen bridges to form complex polyoxometallic clusters. The generation of these polyoxometallic clusters is a dynamic chemical process. By adjusting the pH of the system to 6, a weakly acidic environment is provided, which can both inhibit the dissociation of polyoxometallic clusters and promote their polymerization, thereby ensuring that molybdate and tungstate can form stable polyoxometallic clusters. The oxide skeleton of the polyoxometallic cluster has very high thermal stability, which is the basis for its role in extreme pressure and wear-resistant lubricants. Extreme pressure environments are usually accompanied by high temperature and high pressure. At local contact points on the metal surface, the temperature may instantly rise to hundreds of degrees Celsius or even higher. Under such extreme conditions, most organic lubricants will undergo thermal decomposition or oxidation. However, the oxide framework of polyoxometalates, due to the strong energy of the MO bond (M is molybdenum or tungsten) and the stability of the bridging oxygen structure, can withstand these extreme conditions well and ensure the continued performance of the lubricant. Furthermore, the oxygen cluster structure of polyoxometalates provides abundant active oxygen sites, especially bridging oxygen and surface boundary oxygen. These active oxygen species can chemically adsorb to the metal surface under friction conditions, forming an anti-wear protective film. The formation mechanism of this lubricating film is multifaceted: first, the polyoxometalates adhere to the metal surface through physical adsorption or chemical bonding, forming a boundary lubricating film. Second, under the influence of friction and high temperature, some of the metal oxides in the oxygen clusters chemically react with the metal surface, forming an in-situ metal oxide film with high hardness and lubricating properties. Furthermore, the unique molecular structure of polyoxometalates gives them a certain degree of dynamic adaptability. When the lubricating film is damaged by shear, the oxygen clusters can reform through intermolecular rearrangement to form a new protective film, achieving self-repair. This self-repairing property is particularly critical in extreme pressure and wear environments and can significantly extend the service life of the lubricant.
[0013] The addition of ammonium cerium nitrate further optimizes the chemical and lubricating properties of the polyoxometallic clusters. Ammonium cerium nitrate is a cerium-containing oxidant whose oxidizing properties stem from the unique redox properties of cerium ions. Cerium ions can interact with molybdate or tungstate to form a cerium-containing polyoxometallic cluster complex. The presence of this complex oxygen cluster enhances the chemical stability and adsorption capacity of the oxygen cluster. During friction, cerium ions can capture or release oxygen free radicals through redox cycles, acting as an antioxidant. Oxygen free radicals are the primary cause of lubricant degradation and oxidative damage to metal surfaces in lubrication systems. The presence of cerium ions effectively neutralizes these free radicals, thereby protecting the integrity of the lubricant and the stability of the metal surface. Furthermore, the introduction of cerium ions enhances the density and stability of the lubricating film. By coordinating with molybdate and tungstate, cerium ions form a denser composite film on the metal surface. This film not only exhibits excellent thermal stability but also maintains its integrity under high pressure, significantly reducing contact stress on the metal surface and extending the life of the lubricating film. Citric acid, a tricarboxylic acid molecule, forms multidentate coordination with the molybdenum, tungsten, and cerium ions in the polyoxometallic clusters through its carboxyl and hydroxyl groups. The introduction of citric acid further stabilizes the structure of the clusters, preventing them from dissociating or precipitating in aqueous solution. The multidentate coordination of citric acid enables the polyoxometallic clusters to form more stable complexes, which can better adhere to metal surfaces under friction conditions to form an anti-wear protective film. In addition, the carboxyl and hydroxyl groups of citric acid can be released and activated during the friction process, further enhancing the shear resistance of the lubricating film. Citric acid also has a certain buffering effect. By adjusting the pH value of the solution, the system is maintained in the weakly acidic range, thereby promoting the stabilization and uniform dispersion of the polyoxometallic clusters.
[0014] In the preparation of phosphate precursors, the synergistic effect of phosphoric acid and boric acid is the key to achieving a high-performance lubricating film. Phosphate is a highly chemically active anion that can react chemically with the metal surface under friction conditions to form an in-situ phosphate lubricating film with anti-wear properties. This lubricating film has remarkable high load stability and can maintain its integrity under high pressure conditions, thereby effectively reducing the contact stress on the metal surface. Another key characteristic of the phosphate film is its self-healing ability. Under high shear forces, the lubricating film may break or wear, but the phosphate ions in the system can be re-adsorbed onto the metal surface and repair the damaged film layer, thereby extending the effective service life of the lubricant.
[0015] Boric acid exists in solution as B(OH)3. Its unique chemical properties make it a crucial component in lubrication systems. Boric acid molecules reduce friction by forming slip planes (similar to a layered structure). These slip planes act as solid lubricants between rubbing surfaces, reducing the coefficient of friction. Furthermore, the synergistic effect of boric acid and phosphoric acid produces a denser, more wear-resistant composite lubricating film. The combination of phosphoric acid and boric acid not only improves the lubricating film's shear resistance but also enhances its thermal stability, enabling it to remain stable under extreme pressure. Boric acid also possesses a certain adsorption capacity, allowing its molecules to form weak chemical bonds or hydrogen bonds with metal surfaces, further enhancing the adhesion of the lubricating film. Boron nitride, a layered two-dimensional material, offers significant advantages in lubrication systems due to its chemical and physical properties. Its layered structure is similar to that of graphite, but with greater chemical stability, enabling it to maintain integrity under more severe friction conditions. In lubrication systems, boron nitride's layered structure forms a low-friction slip layer on metal surfaces. This slip layer significantly reduces the coefficient of friction under high-pressure conditions and minimizes direct contact between metal surfaces. In addition, the surface of boron nitride can adsorb phosphates, which further enhances the shear resistance of the lubricant. Boron nitride also has excellent high-temperature stability and can maintain its structural integrity in extreme pressure environments without failure due to thermal decomposition or chemical degradation.
[0016] The core phase solution primarily consists of a multimetallic complex and a phosphate precursor, which are key components in providing a lubricating film and anti-wear protection within the lubrication system. The multimetallic complex, through its redox properties and chemical adsorption of oxygen clusters, provides an antioxidant and lubricating protective film on the friction surface. The phosphate precursor chemically reacts with the metal surface to form a self-healing, wear-resistant film. Butylated hydroxytoluene, a commonly used antioxidant, is also incorporated into the core components to protect them from oxidative degradation in high-temperature and high-pressure environments, thereby extending the lubricant's useful life. The shell phase solution encapsulates and protects the core while enabling controlled release of the core components. The shell solution primarily consists of urea-formaldehyde resin and melamine-formaldehyde resin, two cross-linked polymers with high mechanical strength and heat resistance, capable of maintaining the integrity of the microcapsules under high-pressure conditions. Urea-formaldehyde resin exhibits excellent film-forming properties and chemical stability, making it suitable for use in high-temperature and high-pressure environments. Melamine-formaldehyde resin, with its higher hardness, enhances the mechanical strength of the microcapsules, preventing premature breakage during storage or use. The combination of these two forms a shell material that combines both flexibility and hardness, ensuring the microcapsules can withstand extreme pressure environments. Emulsifiers play a key role in the microencapsulation process. By reducing the interfacial tension between the core and shell solutions, the emulsifier promotes the formation of a uniform droplet structure. Under heating, the resin in the shell solution undergoes a cross-linking reaction, solidifying and encapsulating the core. The resulting microcapsules gradually release the core components during friction. This controlled release mechanism ensures that a lubricating film can rapidly form and repair wear under elevated pressure and temperature. Microencapsulation technology also extends the lubricant's service life by effectively protecting the core components during storage and use. The synergistic design of polymetallic oxide clusters, phosphates, and boron nitride provides multiple functionalities for extreme pressure and wear environments, including the formation of a lubricating protective film, a reduced coefficient of friction, and enhanced antioxidant properties. Furthermore, microencapsulation technology further optimizes the release behavior of these functional materials, ensuring that the core components are maximized under friction conditions.
[0017] MOFs are a class of porous materials with high surface area, tunable pores, and abundant active sites. Their structures are self-assembled from metal ions or metal clusters and organic ligands through coordination bonds. After synthesis, unreacted organic ligands or solvent molecules often remain within the MOF pores. These residues hinder the exposure of the MOF active sites, reducing their chemical reactivity and lubrication properties. Therefore, MOFs must undergo activation to unlock their potential functions. Activating MOFs through heat treatment removes residual material from the pores while exposing the metal centers and functional groups (such as carboxyl and hydroxyl groups) on their surfaces. The activated MOFs exhibit significantly enhanced chemical adsorption capacity and a higher surface area, and their porous structure provides an ideal vehicle for designing lubrication functions. The role of activated MOFs in lubrication systems is primarily reflected in two aspects. First, the exposed metal centers can chemically adsorb with lubricant components or the metal surface, forming a stable lubricating film, thereby reducing wear at the frictional contact interface. Second, the open pore structure endows the MOF with a high material storage capacity, enabling the loading of functional additives within the pores, providing ideal reaction space and bonding interfaces for subsequent chemical modification. Furthermore, the thermal stability of the MOF is further enhanced during the activation process, enabling it to maintain structural integrity and functional stability under harsh conditions such as high temperature and extreme pressure. After activation, the MOF is surface functionalized with 1,2-ethanedithiol. 1,2-Ethanedithiol is a small molecule containing dithiol groups. The -SH groups in its molecular structure can chemically bond with the metal centers on the MOF surface, forming a surface-modified MOF material. This modification process significantly enhances the anti-wear properties of the MOF. The thiol groups have excellent interfacial lubrication properties. Under friction conditions, they can form a chemical adsorption film on the metal surface, reducing direct contact between the metals and thereby reducing the friction coefficient and wear rate. Furthermore, thiol groups can decompose at high temperatures to form metal sulfides, which further optimize the material's anti-wear properties with their excellent solid lubrication properties. Through surface modification, the lubrication function of MOFs is significantly enhanced, while their surface chemical properties are also more diverse, providing a more stable and active binding interface for subsequent composites with ionic liquids.
[0018] In the present invention, a polyionic liquid (PIL) was synthesized through a free radical polymerization reaction of 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, bismaleimide, and ammonium persulfate. In this process, ammonium persulfate acts as a free radical initiator, decomposing to produce free radicals that trigger the polymerization of bismaleimide, forming a cross-linked polymer network. Simultaneously, the ionic liquid is embedded into the polymer backbone through electrostatic interactions. This structural design endows the polyionic liquid with excellent lubricity and thermal stability. The low shear viscosity and polarity of the ionic liquid enable it to form a dense lubricating film on the friction surface, significantly reducing the coefficient of friction. Furthermore, the ionic liquid's high-temperature resistance and antioxidant properties ensure the stability of the lubrication system under extreme conditions. After the polyionic liquid is synthesized, it is compounded with a functionalized MOF to form a MOF@PIL composite powder. The core of this compounding process lies in the effective filling and bonding of the polyionic liquid to the surface and pores of the MOF. The PIL molecules are loaded onto the MOF surface and pores through interactions such as electrostatic adsorption, hydrogen bonding, and chemical bonding. This loading not only enhances the lubricity of the MOF but also further optimizes the interfacial chemistry of the composite material through the fluidity and polarity of the polyionic liquid. The high surface area and pore structure of the MOF provide an ideal physical support for the dispersion of the polyionic liquid, while the lubricating properties of the polyionic liquid complement the deficiencies of the MOF in tribological performance. This combination of properties achieves a synergistic enhancement of lubricity. In the final optimization stage of the composite, zinc ions were added to further enhance its lubricity. As a functional additive, zinc ions coordinate with the imidazolium cations in the polyionic liquid and the active sites on the MOF surface, forming stable zinc complexes. Under frictional conditions, these complexes react with the metal surface to form a zinc phosphide or zinc oxide lubricating film. This lubricating film, with its high hardness and chemical stability, significantly enhances the anti-wear properties of the composite material. Furthermore, the zinc phosphide film exhibits excellent wear resistance under high pressure, effectively dissipating frictional stress and reducing localized damage to the metal surface.
[0019] The functional optimization of the MOF@PIL composite powder is not only reflected in the microscopic level of material design, but also demonstrates significant synergistic effects in its actual performance under friction conditions. During the friction process, PIL, through its fluidity and lubricating properties, forms a dense lubricating film on the metal surface, reducing the shear stress and friction coefficient at the friction interface. Simultaneously, MOF, due to its surface active sites and pore structure, can capture oxygen free radicals generated at the friction interface, inhibiting oxidation reactions that damage the lubricating film. Furthermore, the high mechanical strength and chemical stability of MOF ensure the structural integrity of the lubricating film under high pressure, while the dynamic lubrication properties of the polyionic liquid further enhance the film's self-healing ability. This multi-layered synergistic effect enables the MOF@PIL composite to exhibit excellent performance in extreme pressure and wear environments. Combined with microencapsulation technology, the MOF@PIL composite powder synergizes with other lubricating additives, further enhancing the lubricant's overall performance. The microencapsulation delays the release of active components, ensuring the lubricant's stability over extended use. As the functional core component, MOF@PIL provides continuous lubrication protection at the friction interface. Through the mutual cooperation of polyoxometalates, phosphates and MOF@PIL, the lubricant forms a multilayer protective film on the friction surface.
[0020] The present invention enhances the overall performance of the lubricant through the interaction between various materials and functional components. First, the synergistic effect of polyoxometalates (POMs) on the metal surface. POMs are highly active chemically, exhibiting excellent thermal stability and chemical reactivity, particularly under extreme friction conditions. During the friction process, POMs adhere to the metal surface through chemical adsorption and undergo interfacial reactions with metal atoms, forming a dense metal oxide film. This film is highly hard and can effectively withstand friction loads while reducing direct contact between metals, thereby reducing wear. However, the function of POMs does not work in isolation; their synergistic effect with other components greatly enhances the stability and efficiency of the process. The introduction of ammonium cerium nitrate provides important chemical support for the lubricating properties of POMs. Cerium ions, through their unique redox properties, interact with POMs at the friction interface. Cerium ions can capture oxygen free radicals generated during friction, thereby inhibiting oxidation reactions that damage the lubricating film. This not only protects the structural integrity of the POMs but also further enhances the chemical stability of the lubricating film. Furthermore, cerium ions react with the metal surface at the friction interface to form a cerium oxide film. This film, superimposed on the oxide film formed by the polyoxometallic clusters, creates a multi-layered lubricating protective structure. The layered nature of the cerium oxide film further disperses frictional stress, enhancing the shear resistance and high-temperature resistance of the lubricating film. The polyoxometallic clusters also form a significant synergistic effect with phosphates. Phosphates react with metal surfaces under friction to form an in-situ phosphate film, and the polyoxometallic clusters, through their highly reactive oxygen cluster structure, provide favorable conditions for the growth of this phosphate film. Specifically, the polyoxometallic clusters capture highly reactive oxygen radicals and metal ions at the friction interface, ensuring a more uniform phosphate reaction. Furthermore, the chemical stability of the phosphate film, combined with the hardness of the polyoxometallic cluster film, effectively resists lubricating film breakdown in high-pressure and high-temperature environments. This composite protective film exhibits excellent shear resistance and self-healing capabilities. When the lubricating film is damaged, phosphate ions rapidly adsorb to the metal surface, filling the damaged area and maintaining the integrity of the lubricating film.
[0021] The combination of MOF and PIL in the present invention is another key link in optimizing the function of the lubrication system. MOF, with its high specific surface area, porous structure and active sites, provides an ideal platform for the loading of PIL. After the MOF is activated, its surface metal centers and ligand functional groups are exposed, showing higher chemical adsorption capacity and material storage capacity. During the composite process, PIL is loaded on the surface and in the pores of MOF through electrostatic interaction, hydrogen bonding and chemical bonding, forming a stable composite structure. This composite design significantly improves the stability and dynamic lubrication performance of the lubricating film. During the friction process, PIL plays its core lubrication role. The ionic liquid component in PIL can form a dense lubricating film on the friction surface, reducing the shear stress at the friction interface. MOF, on the other hand, assumes the functions of material storage and interface protection. Its pores can capture the oxygen free radicals generated during the friction process, inhibiting the damage of the lubricating film to the oxidation reaction. At the same time, MOF provides additional mechanical support for the lubricating film through its high strength and chemical stability. The fluidity and dynamic lubrication properties of PILs, which continuously coat the friction surface under the influence of frictional heat, combined with the chemical adsorption capacity of MOFs ensure the integrity of the lubricating film under high-pressure conditions. This synergistic effect achieves multi-level optimization of the lubricating film's functionality, not only reducing the coefficient of friction but also extending the lubricant's service life.
[0022] Thiol-modified MOFs further enhance their lubricity. The MOF surface is chemically modified with 1,2-ethanedithiol to impart dithiol groups. This modification enhances the interfacial lubrication properties of the MOF. Under frictional conditions, the thiol groups chemically adsorb to the metal surface, forming a stable interfacial film. This adsorption film effectively reduces direct metal-metal contact and reduces wear. Furthermore, at high temperatures, the thiol groups may decompose to form a metal sulfide film, which further enhances the anti-wear properties of the lubricating film through its excellent solid lubrication properties. The thiol groups also form a significant interfacial synergistic effect with the PIL. The imidazolium cations in the PIL electrostatically bind to the polar portion of the thiol groups, strengthening the interfacial bond between the MOF and PIL. Under the influence of frictional heat, the thiol groups may also undergo an interfacial reaction with the ionic liquid components, forming an additional lubricating film. This interfacial reaction exhibits strong shear resistance under extreme pressure conditions, enabling the lubricating film to withstand higher friction loads. The introduction of zinc ions in the experimental scheme further optimizes the performance of the lubricating film. Zinc ions can coordinate with functional groups in PILs and MOFs to form stable zinc complexes. These complexes chemically react with the metal surface under friction conditions to form zinc phosphide or zinc oxide films. These films, with their high hardness and high-temperature resistance, significantly enhance the anti-wear capabilities of the lubricating film. Furthermore, the zinc phosphide film exhibits excellent wear resistance under high-pressure conditions, effectively dissipating frictional stress while reducing localized damage to the metal surface. Zinc ions also form complex synergistic interactions with polyoxometalates and phosphates, further enhancing the stability and chemical protection of the lubricating film.
[0023] As a preferred technical solution of the present invention, in step A1, the mass volume ratio of the ammonium molybdate to the first portion of deionized water is 17 g:60 mL;
[0024] In some optional embodiments, the mass volume ratio of the sodium tungstate to the second portion of deionized water is 13 g:40 mL;
[0025] In some optional embodiments, the mass volume ratio of the ammonium cerium nitrate to the third portion of deionized water is 1 g:4 mL;
[0026] In some optional embodiments, the mass ratio of ammonium molybdate, sodium tungstate, ammonium cerium nitrate and citric acid is 17:13:10:4.
[0027] As a preferred technical solution of the present invention, in step A2, the mass ratio of phosphoric acid, boric acid and boron nitride is 50:5:1;
[0028] In some optional embodiments, the mass ratio of the boric acid to deionized water is 1:30;
[0029] In some optional embodiments, the mass ratio of boron nitride to anhydrous ethanol is 1:15.
[0030] As a preferred technical solution of the present invention, in step S1, the mass ratio of the multi-metal complex solution, the phosphate precursor, butylated hydroxytoluene and isopropanol is 300:150:1:50;
[0031] In some optional embodiments, the first temperature is 40-50°C, for example, it can be 40°C, 41°C, 42°C, 43°C, 44°C, 45°C, 46°C, 47°C, 48°C, 49°C or 50°C, but is not limited to the listed values, and other unlisted values within the temperature range are also applicable.
[0032] The stirring time at the first temperature is 30-40 min, for example, it can be 30 min, 31 min, 32 min, 33 min, 34 min, 35 min, 36 min, 37 min, 38 min, 39 min or 40 min, but is not limited to the listed times, and other unlisted times within the time range are also applicable.
[0033] In some optional embodiments, the mass volume ratio of the urea, formaldehyde solution, deionized water and benzaldehyde oxime is 30 g:45 mL:100 mL:1 g.
[0034] In some optional embodiments, the mass ratio of the urea-formaldehyde resin precursor, melamine formaldehyde resin and deionized water is 4:1:6;
[0035] In some optional embodiments, the mass ratio of the inner core phase solution, the outer shell phase solution and the emulsifier is 100:100:1;
[0036] In some optional embodiments, the emulsifier is Tween-20;
[0037] In some optional embodiments, the second temperature is 60-70°C, for example, it can be 60°C, 61°C, 62°C, 63°C, 64°C, 65°C, 66°C, 67°C, 68°C, 69°C or 70°C, but is not limited to the listed values, and other unlisted values within the temperature range are also applicable.
[0038] The stirring time at the second temperature is 1-2 hours, for example, 1 hour, 1.1 hours, 1.2 hours, 1.3 hours, 1.4 hours, 1.5 hours, 1.6 hours, 1.7 hours, 1.8 hours, 1.9 hours or 2 hours, but is not limited to the listed times, and other times not listed within the time range are also applicable.
[0039] As a preferred technical solution of the present invention, in step S2, the MOF is ZIF-8;
[0040] In some optional embodiments, the third temperature is 200-250°C, for example, it can be 200°C, 205°C, 210°C, 215°C, 220°C, 225°C, 230°C, 235°C, 240°C, 245°C or 250°C, but is not limited to the listed values, and other unlisted values within the temperature range are also applicable.
[0041] In some optional embodiments, the third temperature holding time is 5-6h, for example, it can be 5.0h, 5.1h, 5.2h, 5.3h, 5.4h, 5.5h, 5.6h, 5.7h, 5.8h, 5.9h or 6.0h, but is not limited to the listed times, and other unlisted times within the time range are also applicable.
[0042] In some optional embodiments, the mass ratio of the activated MOF to 1,2-ethanedithiol is 20:3;
[0043] In some optional embodiments, the mass volume ratio of the activated MOF to the first portion of DMF is 20 g:10 mL;
[0044] In some optional embodiments, the room temperature standing time is 6-8h, for example, it can be 6h, 6.2h, 6.4h, 6.6h, 6.8h, 7h, 7.2h, 7.4h, 7.6h, 7.8h or 8h, but is not limited to the listed times, and other unlisted times within the time range are also applicable.
[0045] In some optional embodiments, the mass ratio of the 1-ethyl-3-methylimidazoline bis(trifluoromethylsulfonyl)imide, bismaleimide, ammonium persulfate and the anti-wear component MOF is 12:4:1:40;
[0046] In some optional embodiments, the mass volume ratio of the 1-ethyl-3-methylimidazoline bis(trifluoromethylsulfonyl)imide to the second portion of DMF is 1 g:5 mL;
[0047] The stirring time at the second temperature is 2-3 hours, for example, 2 hours, 2.1 hours, 2.2 hours, 2.3 hours, 2.4 hours, 2.5 hours, 2.6 hours, 2.7 hours, 2.8 hours, 2.9 hours or 3 hours, but is not limited to the listed times, and other times not listed within the time range are also applicable.
[0048] In some optional embodiments, the mass volume ratio of the bismaleimide to the zinc ion solution is 2 g:1 mL;
[0049] The stirring time is 1-2 hours, for example, 1 hour, 1.1 hours, 1.2 hours, 1.3 hours, 1.4 hours, 1.5 hours, 1.6 hours, 1.7 hours, 1.8 hours, 1.9 hours or 2 hours, but is not limited to the listed times, and other times not listed within the time range are also applicable.
[0050] In some optional embodiments, the mass ratio of the microcapsules to the MOF@PIL composite powder is 2:1.
[0051] In a second aspect, the present invention provides an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material prepared by the preparation method described in the first aspect.
[0052] Compared with the prior art, the present invention has the following beneficial effects: (1) Through microencapsulation technology, the multi-metal complex and the phosphate precursor are encapsulated in a resin shell to form a stable core-shell structure. The microcapsule shell is composed of urea-formaldehyde resin and melamine-formaldehyde resin, has good chemical inertness and mechanical strength, and can be stably dispersed in lubricating oil for a long time. Under friction contact or high temperature and high pressure conditions, it can gradually release the active components in the core, generate a chemical reaction film on the metal surface, reduce the friction coefficient, and enhance the wear resistance; (2) The MOF composite material significantly improves the chemical reaction activity and thermal stability of the anti-wear component through the sulfurization modification of 1,2-ethanedithiol and the introduction of ionic liquid. The sulfurization modification process introduces active sulfur groups, which can react with metal at high temperature. Surface reaction generates a dense metal sulfide protective film, thereby reducing direct contact between metals. In addition, the addition of ionic liquid gives MOF materials excellent lubrication properties and thermal stability, which can maintain the integrity of the lubricating oil film under high temperature conditions and further reduce the friction coefficient; (3) By combining multifunctional microcapsules and MOF composites, multi-level synergistic effects are achieved to enhance the comprehensive performance of lubricants. Microcapsules provide controllable release of anti-wear components, while MOF composites have high specific surface area and multifunctional active sites, which can further improve the anti-wear efficiency. During the friction process, the multi-metal complexes and phosphates released by the microcapsules work together with the active components of the MOF composite to form a multi-layer protective film on the metal surface, thereby providing anti-wear and anti-oxidation properties. BRIEF DESCRIPTION OF THE DRAWINGS
[0053] Figure 1 TEM image of the microcapsules provided in Example 1 of the present invention;
[0054] Figure 2 This is the SEM image of the MOF@PIL composite powder provided in Example 1 of the present invention. DETAILED DESCRIPTION
[0055] The technical solutions of the present invention are described in detail below in conjunction with specific embodiments and the accompanying drawings. The embodiments described herein are specific embodiments of the present invention and are used to illustrate the concept of the present invention; these descriptions are explanatory and exemplary and should not be understood as limiting the embodiments of the present invention and the scope of protection of the present invention. In addition to the embodiments described herein, those skilled in the art can also adopt other obvious technical solutions based on the contents disclosed in the claims of this application and its specification, including technical solutions that adopt any obvious replacements and modifications made to the embodiments described herein.
[0056] The chemical reagents used in the examples and comparative examples of the present invention are all commercially available products and have not been subjected to any further purification treatment.
[0057] Example 1
[0058] This embodiment provides an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material and a preparation method thereof, wherein the preparation method specifically comprises the following steps:
[0059] A1. Disperse 17 g of ammonium molybdate in 60 mL of deionized water, 13 g of sodium tungstate in 40 mL of deionized water, and 10 g of ammonium cerium nitrate in 40 mL of deionized water. Add the ammonium molybdate solution to the sodium tungstate solution, then add the ammonium cerium nitrate solution, and then add 4 g of citric acid. Adjust the pH to 6 to obtain a multi-metal complex solution.
[0060] A2: Disperse 50 g of phosphoric acid and 5 g of boric acid in 150 mL of deionized water, adjust the temperature to 60°C, and stir to obtain a phosphate solution. Disperse 1 g of boron nitride in 15 g of anhydrous ethanol and add the solution to the phosphate solution. Adjust the pH to 7 to obtain a phosphate precursor.
[0061] S1, 300g of multi-metal complex solution, 150g of phosphate precursor, 1g of butylated hydroxytoluene and 50g of isopropanol were mixed, the temperature was adjusted to 44°C and stirred for 31min to obtain a core phase solution, 60g of urea and 90mL of 37wt.% formaldehyde solution were dispersed in 200mL of deionized water, the pH was adjusted to 7, the mixture was heated to 70°C, 2g of benzaldehyde oxime was added and stirred to obtain a urea-formaldehyde resin precursor, 200g of urea-formaldehyde resin precursor and 50g of melamine formaldehyde resin were dispersed in 300g of deionized water, 1% by mass ammonium chloride solution was added to adjust the pH to 4.5 to obtain a shell phase solution, and the core phase solution and shell phase solution were mixed with an emulsifier, the temperature was adjusted to 68°C and stirred for 1.6h, centrifuged, washed, and vacuum dried to obtain microcapsules;
[0062] S2, MOF was placed at 210 ° C for 5.5 hours to obtain activated MOF, 200g of activated MOF and 30g of 1,2-ethanedithiol were dispersed in 100mL of DMF, and the mixture was allowed to stand at room temperature and then centrifuged and dried to obtain the anti-wear component MOF, 60g of 1-ethyl-3-methylimidazoline bis(trifluoromethylsulfonyl)imide, 20g of bismaleimide and 5g of ammonium persulfate were dispersed in 300mL of DMF, mixed evenly, and then 200g of anti-wear component MOF was added. The temperature was adjusted to 62 ° C under a nitrogen atmosphere and stirred for 2.1 hours. Then 10mL of 20wt.% zinc ion solution was added and stirred for 1.2 hours. After the reaction, the mixture was centrifuged, washed and dried to obtain MOF@PIL composite powder. 50g of microcapsules were mixed with 25g of MOF@PIL composite powder to obtain an industrial lubricant extreme pressure anti-wear agent containing self-healing materials.
[0063] Figure 1 This is the TEM image of the microcapsules prepared in this example. It can be clearly seen that the microcapsules have a uniform spherical structure, a smooth surface, and no obvious collapse; Figure 2 This is the SEM image of the MOF@PIL composite powder prepared in this example.
[0064] Example 2
[0065] This embodiment provides an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material and a preparation method thereof, wherein the preparation method specifically comprises the following steps:
[0066] A1. Disperse 17 g of ammonium molybdate in 60 mL of deionized water, 13 g of sodium tungstate in 40 mL of deionized water, and 10 g of ammonium cerium nitrate in 40 mL of deionized water. Add the ammonium molybdate solution to the sodium tungstate solution, then add the ammonium cerium nitrate solution, and then add 4 g of citric acid. Adjust the pH to 6 to obtain a multi-metal complex solution.
[0067] A2: Disperse 50 g of phosphoric acid and 5 g of boric acid in 150 mL of deionized water, adjust the temperature to 60°C, and stir to obtain a phosphate solution. Disperse 1 g of boron nitride in 15 g of anhydrous ethanol and add the solution to the phosphate solution. Adjust the pH to 7 to obtain a phosphate precursor.
[0068] S1, 300g of multi-metal complex solution, 150g of phosphate precursor, 1g of butylated hydroxytoluene and 50g of isopropanol were mixed, the temperature was adjusted to 49°C and stirred for 38min to obtain a core phase solution, 60g of urea and 90mL of 37wt.% formaldehyde solution were dispersed in 200mL of deionized water, the pH was adjusted to 7, the mixture was heated to 70°C, 2g of benzaldehyde oxime was added and stirred to obtain a urea-formaldehyde resin precursor, 200g of urea-formaldehyde resin precursor and 50g of melamine formaldehyde resin were dispersed in 300g of deionized water, 1% by mass ammonium chloride solution was added to adjust the pH to 4.5 to obtain a shell phase solution, and the core phase solution and shell phase solution were mixed with an emulsifier, the temperature was adjusted to 61°C and stirred for 1.1h, centrifuged and washed, and vacuum dried to obtain microcapsules;
[0069] S2, MOF was placed at 240 ° C for 5.1 hours to obtain activated MOF, 200g of activated MOF and 30g of 1,2-ethanedithiol were dispersed in 100mL of DMF, and the mixture was allowed to stand at room temperature and then centrifuged and dried to obtain the anti-wear component MOF, 60g of 1-ethyl-3-methylimidazoline bis(trifluoromethylsulfonyl)imide, 20g of bismaleimide and 5g of ammonium persulfate were dispersed in 300mL of DMF, mixed evenly, and then 200g of anti-wear component MOF was added. The temperature was adjusted to 67 ° C under a nitrogen atmosphere and stirred for 2.8 hours. Then 10mL of 20wt.% zinc ion solution was added and stirred for 1.9 hours. After the reaction, the mixture was centrifuged, washed and dried to obtain MOF@PIL composite powder. 50g of microcapsules were mixed with 25g of MOF@PIL composite powder to obtain an industrial lubricant extreme pressure anti-wear agent containing self-healing materials.
[0070] Example 3
[0071] This embodiment provides an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material and a preparation method thereof, wherein the preparation method specifically comprises the following steps:
[0072] A1. Disperse 17 g of ammonium molybdate in 60 mL of deionized water, 13 g of sodium tungstate in 40 mL of deionized water, and 10 g of ammonium cerium nitrate in 40 mL of deionized water. Add the ammonium molybdate solution to the sodium tungstate solution, then add the ammonium cerium nitrate solution, and then add 4 g of citric acid. Adjust the pH to 6 to obtain a multi-metal complex solution.
[0073] A2: Disperse 50 g of phosphoric acid and 5 g of boric acid in 150 mL of deionized water, adjust the temperature to 60°C, and stir to obtain a phosphate solution. Disperse 1 g of boron nitride in 15 g of anhydrous ethanol and add the solution to the phosphate solution. Adjust the pH to 7 to obtain a phosphate precursor.
[0074] S1, 300g of multi-metal complex solution, 150g of phosphate precursor, 1g of butylated hydroxytoluene and 50g of isopropanol were mixed, the temperature was adjusted to 41°C and stirred for 34min to obtain a core phase solution, 60g of urea and 90mL of 37wt.% formaldehyde solution were dispersed in 200mL of deionized water, the pH was adjusted to 7, the mixture was heated to 70°C, 2g of benzaldehyde oxime was added and stirred to obtain a urea-formaldehyde resin precursor, 200g of urea-formaldehyde resin precursor and 50g of melamine formaldehyde resin were dispersed in 300g of deionized water, 1% by mass ammonium chloride solution was added to adjust the pH to 4.5 to obtain a shell phase solution, and the core phase solution and shell phase solution were mixed with an emulsifier, the temperature was adjusted to 64°C and stirred for 1.4h, centrifuged, washed, and vacuum dried to obtain microcapsules;
[0075] S2, MOF is placed at 250°C for 5.8 hours to obtain activated MOF, 200g of activated MOF and 30g of 1,2-ethanedithiol are dispersed in 100mL of DMF, and the mixture is allowed to stand at room temperature and then centrifuged and dried to obtain the anti-wear component MOF, 60g of 1-ethyl-3-methylimidazoline bis(trifluoromethylsulfonyl)imide, 20g of bismaleimide and 5g of ammonium persulfate are dispersed in 300mL of DMF, mixed evenly, and then 200g of anti-wear component MOF is added. The temperature is adjusted to 61°C under a nitrogen atmosphere and stirred for 2.4 hours, and then 10mL of 20wt.% zinc ion solution is added and stirred for 1.4 hours. After the reaction is completed, the mixture is centrifuged, washed and dried to obtain MOF@PIL composite powder, and 50g of microcapsules are mixed with 25g of MOF@PIL composite powder to obtain an industrial lubricant extreme pressure anti-wear agent containing self-healing materials.
[0076] Example 4
[0077] This embodiment provides an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material and a preparation method thereof, wherein the preparation method specifically comprises the following steps:
[0078] A1. Disperse 17 g of ammonium molybdate in 60 mL of deionized water, 13 g of sodium tungstate in 40 mL of deionized water, and 10 g of ammonium cerium nitrate in 40 mL of deionized water. Add the ammonium molybdate solution to the sodium tungstate solution, then add the ammonium cerium nitrate solution, and then add 4 g of citric acid. Adjust the pH to 6 to obtain a multi-metal complex solution.
[0079] A2: Disperse 50 g of phosphoric acid and 5 g of boric acid in 150 mL of deionized water, adjust the temperature to 60°C, and stir to obtain a phosphate solution. Disperse 1 g of boron nitride in 15 g of anhydrous ethanol and add the solution to the phosphate solution. Adjust the pH to 7 to obtain a phosphate precursor.
[0080] S1, 300g of multi-metal complex solution, 150g of phosphate precursor, 1g of butylated hydroxytoluene and 50g of isopropanol were mixed, the temperature was adjusted to 43°C and stirred for 36min to obtain a core phase solution, 60g of urea and 90mL of 37wt.% formaldehyde solution were dispersed in 200mL of deionized water, the pH was adjusted to 7, the mixture was heated to 70°C, 2g of benzaldehyde oxime was added and stirred to obtain a urea-formaldehyde resin precursor, 200g of urea-formaldehyde resin precursor and 50g of melamine formaldehyde resin were dispersed in 300g of deionized water, 1% by mass ammonium chloride solution was added to adjust the pH to 4.5 to obtain a shell phase solution, and the core phase solution and shell phase solution were mixed with an emulsifier, the temperature was adjusted to 66°C and stirred for 1.9h, centrifuged and washed, and vacuum dried to obtain microcapsules;
[0081] S2, MOF was placed at 220 ° C for 5.3 hours to obtain activated MOF, 200g of activated MOF and 30g of 1,2-ethanedithiol were dispersed in 100mL of DMF, and the mixture was allowed to stand at room temperature and then centrifuged and dried to obtain the anti-wear component MOF, 60g of 1-ethyl-3-methylimidazoline bis(trifluoromethylsulfonyl)imide, 20g of bismaleimide and 5g of ammonium persulfate were dispersed in 300mL of DMF, mixed evenly, and then 200g of anti-wear component MOF was added. The temperature was adjusted to 69 ° C under a nitrogen atmosphere and stirred for 2.7h, and then 10mL of 20wt.% zinc ion solution was added and stirred for 1.6h. After the reaction, the mixture was centrifuged, washed and dried to obtain MOF@PIL composite powder. 50g of microcapsules were mixed with 25g of MOF@PIL composite powder to obtain an industrial lubricant extreme pressure anti-wear agent containing self-healing materials.
[0082] Comparative Example 1
[0083] This comparative example provides an industrial lubricant extreme pressure anti-wear agent containing self-repairing materials and a preparation method thereof. The difference between it and Example 1 is that the mass of 1,2-ethanedithiol in S2 is 60g, which is 30g more than that in Example 1. The other process parameters and operating conditions are exactly the same as those in Example 1.
[0084] Comparative Example 2
[0085] This comparative example provides an industrial lubricant extreme pressure anti-wear agent containing self-repairing materials and a preparation method thereof. The difference between it and Example 1 is that the mass of 1,2-ethanedithiol in S2 is 5g, which is 25g less than that in Example 1. The other process parameters and operating conditions are exactly the same as those in Example 1.
[0086] Comparative Example 3
[0087] This comparative example provides an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material and a preparation method thereof. The difference between it and Example 1 is that the mass of 1-ethyl-3-methylimidazoline bis(trifluoromethylsulfonyl)imide in S2 is 120 g, which is 60 g more than that in Example 1. The other process parameters and operating conditions are exactly the same as those in Example 1.
[0088] Comparative Example 4
[0089] This comparative example provides an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material and a preparation method thereof. The difference between it and Example 1 is that the mass of 1-ethyl-3-methylimidazoline bis(trifluoromethylsulfonyl)imide in S2 is 10 g, which is 50 g less than that in Example 1. The other process parameters and operating conditions are exactly the same as those in Example 1.
[0090] The lubricating oil components are: 80 parts base oil, 5 parts extreme pressure anti-wear agent, 0.5 parts dimethyl silicone oil, 1 part anti-emulsifier D114, 2 parts sodium sulfonate, 3 parts succinimide, 1 part alkyl phenol calcium sulfide. B ) and sintering load (P D )The test method is GB / T 3142-2019, and the test results are shown in Table 1.
[0091] Table 1 Test results of an industrial lubricant extreme pressure antiwear agent containing self-repairing material in Examples 1-4 and Comparative Examples 1-4
[0092] Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 <![CDATA[P B (N)]]> 1320 1340 1360 1370 980 1050 1000 950 <![CDATA[P D (N)]]> 3650 3500 3700 3550 2200 2350 2750 2150
[0093] As shown in Table 1, compared to Example 1, the maximum no-seize load and sintering load of Comparative Example 1 are both reduced; the maximum no-seize load and sintering load of Comparative Example 2 are also reduced. 1,2-Ethanedithiol chemically adsorbs to the metal active sites on the MOF surface through the thiol group, forming a stable thiol-modified layer. The thiol group has strong metallophilic properties and can chemically adsorb to the metal surface at the friction contact interface, forming a chemisorbed film. In Comparative Example 1, the excessive amount of 1,2-Ethanedithiol on the MOF surface may shield its metal active sites, weakening the MOF's ability to capture oxygen free radicals or synergize with other additives. Furthermore, an excessively thick adsorption layer may exhibit uneven distribution at the friction interface, making the lubricating film susceptible to localized rupture or delamination under high pressure, reducing its effectiveness. In Comparative Example 2, the insufficient amount of 1,2-Ethanedithiol on the MOF surface leads to an incomplete thiol-modified layer, reducing the coverage of the chemisorbed film at the friction interface. This prevents the lubricant from effectively reducing direct contact between the metal surfaces, resulting in a decrease in the maximum no-seize load and sintering load.
[0094] As shown in Table 1, compared to Example 1, both the maximum no-seizure load and the sintering load decreased in Comparative Example 3; and both the maximum no-seizure load and the sintering load decreased in Comparative Example 4. The imidazolium cation and the bis(trifluoromethylsulfonyl)imide anion in 1-ethyl-3-methylimidazolinium bis(trifluoromethylsulfonyl)imide interact through electrostatic interactions and hydrogen bonding, forming a dense lubricating film on the friction surface. This lubricating film exhibits low shear viscosity and high thermal stability. In Comparative Example 3, the excessive amount of 1-ethyl-3-methylimidazolinium bis(trifluoromethylsulfonyl)imide reduces the adhesion of the lubricating film, making it difficult to stably adhere to the metal surface under high pressure and susceptible to shear damage. In Comparative Example 4, the insufficient amount of 1-ethyl-3-methylimidazolinium bis(trifluoromethylsulfonyl)imide results in uneven distribution of the lubricating film at the friction interface, increasing the direct contact area between the metal surfaces and reducing the maximum no-seizure load and the sintering load.
[0095] The above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention fall within the protection scope and disclosure scope of the present invention.
Claims
1. A method for preparing an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material, characterized in that: The preparation method comprises: S1, mixing a multi-metal complex solution, a phosphate precursor, butylated hydroxytoluene and isopropyl alcohol to obtain a core phase solution, dispersing a urea-formaldehyde resin precursor and a melamine-formaldehyde resin in deionized water, adjusting the pH to 4.5 to obtain a shell phase solution, and then mixing the core phase solution and the shell phase solution with an emulsifier to obtain microcapsules; S2, keeping MOF warm to obtain activated MOF, dispersing the activated MOF and 1,2-ethanedithiol in the first portion of DMF to obtain the anti-wear component MOF, dispersing 1-ethyl-3-methylimidazoline bis(trifluoromethylsulfonyl)imide, bismaleimide and ammonium persulfate in the second portion of DMF, then adding the anti-wear component MOF and zinc ion solution to obtain MOF@PIL composite powder, mixing the microcapsules with the MOF@PIL composite powder to obtain an industrial lubricant extreme pressure anti-wear agent containing self-healing materials.
2. The method for preparing an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material according to claim 1, characterized in that: The preparation method of the multi-metal complex solution comprises: A1. Disperse ammonium molybdate in the first portion of deionized water, disperse sodium tungstate in the second portion of deionized water, and disperse ammonium cerium nitrate in the third portion of deionized water. Add the ammonium molybdate solution to the sodium tungstate solution, then add the ammonium cerium nitrate solution, and add citric acid to adjust the pH to 6 to obtain a multi-metal complex solution.
3. The method for preparing an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material according to claim 1, characterized in that: The preparation method of the phosphate precursor comprises: A2, disperse phosphoric acid and boric acid in deionized water, adjust the temperature to 60°C and stir to obtain a phosphate solution, then disperse boron nitride in anhydrous ethanol and add the solution to the phosphate solution, adjust the pH to 7, and obtain a phosphate precursor.
4. The method for preparing an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material according to claim 1, characterized in that: The preparation method of the urea-formaldehyde resin precursor comprises: Urea and formaldehyde solution are dispersed in deionized water, the pH is adjusted to 7, the solution is heated to 70° C., and benzaldehyde oxime is added to obtain a urea-formaldehyde resin precursor.
5. The method for preparing an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material according to claim 1, characterized in that: In S1, The mass ratio of the multi-metal complex solution, phosphate precursor, butylated hydroxytoluene and isopropanol is 300:150:1:50; The mass ratio of the urea-formaldehyde resin precursor to the melamine-formaldehyde resin is 4:
1.
6. The method for preparing an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material according to claim 1, characterized in that: In S2, The mass ratio of the activated MOF to 1,2-ethanedithiol is 20:3; The mass ratio of the 1-ethyl-3-methylimidazoline bis(trifluoromethylsulfonyl)imide, bismaleimide, ammonium persulfate and the anti-wear component MOF is 12:4:1:40; The mass ratio of the microcapsules to the MOF@PIL composite powder is 2:
1.
7. The method for preparing an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material according to claim 2, characterized in that: In A1, The mass ratio of the ammonium molybdate, sodium tungstate, ammonium cerium nitrate and citric acid is 17:13:10:
4.
8. The method for preparing an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material according to claim 3, characterized in that: In A2, The mass ratio of the phosphoric acid, boric acid and boron nitride is 50:5:
1.
9. The method for preparing an industrial lubricant extreme pressure anti-wear agent containing a self-repairing material according to claim 4, characterized in that: The mass volume ratio of the urea, formaldehyde solution and benzaldehyde oxime is 30g:45mL:1g.
10. An industrial lubricant extreme pressure antiwear agent containing a self-repairing material obtained by the preparation method according to any one of claims 1 to 9.
Citation Information
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