CN115651743B - Lubricating composition capable of forming graphene in situ, and preparation method and application thereof - Google Patents
Lubricating composition capable of forming graphene in situ, and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a lubricating composition capable of forming graphene in situ, and a preparation method and application thereof, and belongs to the technical field of lubricating materials. The lubricating composition provided by the invention comprises metal particles and an active organic compound, and can realize in-situ formation of graphene in a friction process. In the friction process, the active organic compound generates a tribochemical reaction under the action of normal force and shearing stress to generate a carbon-containing compound, the carbon-containing compound can serve as a solid lubricant of a friction interface, and the metal particles can further catalyze the carbon-containing compound to generate graphitization conversion to form graphene with excellent lubricating performance, so that better lubricating performance is provided for a lubricating system. The lubricating composition provided by the invention combines the tribochemical reaction of the organic compound with metal catalysis, so that graphene is formed in situ in the friction process to reduce friction and abrasion.
Description
Technical Field
The invention relates to the technical field of lubricating materials, in particular to a lubricating composition capable of forming graphene in situ, and a preparation method and application thereof.
Background
Friction between mechanical parts can create significant energy losses, resulting in immeasurable economic losses. The corresponding wear accelerates the ageing of the mechanical parts and shortens the service life of the machine. Lubricating oils have a variety of functions including lubrication, cooling, rust protection, cleaning, sealing, and buffering, and are widely used in the mechanical field to reduce friction and wear. However, as the severity of practical application conditions increases, the lubricating ability of lubricating oils needs to be further improved. Accordingly, various materials including carbon and its derivatives, metals, metal oxides, sulfides, rare earth compounds, nitrogen-containing heterocyclic compounds, borates, ionic liquids, and the like have been used as lubricating oil additives to improve the lubricating properties thereof. Among them, carbon materials are receiving a great deal of attention for their environmental friendliness, excellent mechanical properties, thermal stability, chemical stability, and unique self-lubricating properties. However, typical carbon lubricating materials, such as graphene, fullerene, carbon quantum dot or carbon nanotube, require a complicated synthesis process and a large amount of energy input, which not only causes environmental pollution but also increases production costs.
Disclosure of Invention
The invention aims to provide a lubricating composition capable of forming graphene in situ, a preparation method and application thereof, wherein the lubricating composition can realize graphene in situ formation in a friction process and improve lubricating performance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a lubricating composition capable of forming graphene in situ, which comprises metal particles, an active organic compound and base lubricating oil; the reactive organic compound contains a polyvalent carbocycle and a carboxyl group.
Preferably, the mass of the metal particles is 0.1 to 2% of the mass of the base lubricating oil.
Preferably, the mass of the active organic compound is 0.5 to 4% of the mass of the base lubricating oil.
Preferably, the metal particles include any one of zinc particles, copper particles, nickel particles, iron particles, and cobalt particles.
Preferably, the active organic compound includes any one of cyclopropanecarboxylic acid, cyclopropane-1, 1-dicarboxylic acid, cyclobutane-1, 1-dicarboxylic acid, and ring Ding Jiasuan.
Preferably, the base lubricating oil comprises any one of polyalphaolefins, dioctyl sebacate, 500N and perfluoropolyethers.
The invention provides a preparation method of the lubricating composition, which comprises the following steps:
and mixing the metal particles, the active organic compound and the base lubricating oil under the ultrasonic condition to obtain the lubricating composition capable of forming graphene in situ.
Preferably, the temperature of the mixing is 25-50 ℃ and the time is 0.5-3 h.
The invention provides an application of the lubricating composition prepared by the technical scheme or the preparation method of the technical scheme in the lubricating field.
The invention provides a lubricating composition capable of forming graphene in situ, which comprises metal particles, an active organic compound and base lubricating oil; the reactive organic compound contains a polyvalent carbocycle and a carboxyl group. The lubricating composition provided by the invention comprises metal particles and an active organic compound, and can realize in-situ formation of graphene in a friction process. The active organic compound contains a multi-carbon ring in a structure, and the ring stress enables the active organic compound to have metastable property and easily generate chemical reaction; furthermore, the active organic compound contains carboxyl in the structure, so that the interaction with the friction interface can be enhanced. The metal particles have the ability to catalyze graphitization of carbon-containing compounds, and this catalytic ability is further enhanced in the presence of frictional heat and triboelectricity during the friction process. In the friction process, the active organic compound generates a tribochemical reaction under the action of normal force and shearing stress to generate a carbon-containing compound, the carbon-containing compound can serve as a solid lubricant of a friction interface, and the metal particles can further catalyze the carbon-containing compound to generate graphitization conversion to form graphene with excellent lubricating performance, so that better lubricating performance is provided for a lubricating system. The lubricating composition provided by the invention combines the tribochemical reaction of the organic compound with metal catalysis, so that graphene is formed in situ in the friction process to reduce friction and abrasion.
The lubricating composition disclosed by the invention is simple in preparation method, excellent in tribological property and good in practical industrial application prospect.
Drawings
FIG. 1 is a plot of the coefficient of friction of PAO-4 base oil and the lubricating composition of example 1;
FIG. 2 shows the wear scar morphology of the lower test disc after friction testing of the PAO-4 base oil (a) and the lubricating composition (b) of example 1 and after friction testing of the PAO-4 base oil (c) and the lubricating composition (d) of example 1;
fig. 3 is a wear debris morphology after friction testing of the lubricating composition of example 1: (a) transmitting an electron microscope image; (b) a local high resolution transmission electron microscope image;
fig. 4 shows the appearance of the abrasive dust (a) after the friction test of the lubricating composition of example 2 and the appearance of the abrasive dust (b) after the friction test of the lubricating composition of example 3.
Detailed Description
The invention provides a lubricating composition capable of forming graphene in situ, which comprises metal particles, an active organic compound and base lubricating oil; the reactive organic compound contains a polyvalent carbocycle and a carboxyl group.
In the present invention, the desired materials are commercially available products well known to those skilled in the art unless specified otherwise.
The lubricating composition capable of forming graphene in situ provided by the invention comprises metal particles; the metal particles preferably include any one of zinc particles, copper particles, nickel particles, iron particles, and cobalt particles. The metal particles of the present invention are preferably elemental metal particles, and the particle diameter is preferably 1 to 3. Mu.m. In the present invention, the mass of the metal particles is preferably 0.1 to 2% of the mass of the base lubricating oil, more preferably 1.5%. According to the invention, the metal particles are utilized to play a catalytic role, so that graphitization conversion of the active organic compound is promoted, and graphene is formed.
The lubricating composition capable of forming graphene in situ provided by the invention comprises an active organic compound; the reactive organic compound contains a polyvalent carbocycle and a carboxyl group. In the present invention, the active organic compound preferably includes any one of cyclopropanecarboxylic acid, cyclopropane-1, 1-dicarboxylic acid, cyclobutane-1, 1-dicarboxylic acid, and ring Ding Jiasuan. In the present invention, the mass of the active organic compound is preferably 0.5 to 4% of the mass of the base lubricating oil, more preferably 2%. The present invention utilizes active organic compounds as a carbon source for graphene formation.
The lubricating composition capable of forming graphene in situ provided by the invention comprises base lubricating oil; the base lubricating oil preferably comprises any one of polyalphaolefins, dioctyl sebacate, 500N and perfluoropolyethers; the polyalphaolefin is preferably PAO-4. The base lubricating oil of the present invention serves as the base lubricating oil for the lubricating composition.
The invention provides a preparation method of the lubricating composition, which comprises the following steps:
and mixing the metal particles, the active organic compound and the base lubricating oil under the ultrasonic condition to obtain the lubricating composition capable of forming graphene in situ.
The present invention preferably incorporates the metal particles and the reactive organic compound together into the base lubricating oil.
In the present invention, the temperature of the mixing is preferably 25 to 50 ℃, and the time is preferably 0.5 to 3 hours, more preferably 1 hour; the parameters of the ultrasound are not particularly limited in the present invention, and ultrasound conditions may be provided according to procedures well known in the art.
The invention provides an application of the lubricating composition prepared by the technical scheme or the preparation method of the technical scheme in the lubricating field. The method of application of the present invention is not particularly limited, and may be applied according to methods well known in the art.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the following examples, the metal particles used were elemental metal particles having a particle diameter of 1 to 3. Mu.m.
Example 1
Copper metal particles and cyclopropanecarboxylic acid are added into PAO-4 base oil together according to the mass fraction of 1.5wt% and 2wt%, and ultrasonic treatment is carried out for 1h at the temperature of 25 ℃ to obtain the cyclopropanecarboxylic acid/copper lubricating composition.
Example 2
Cobalt metal particles and ring Ding Jiasuan were added together to PAO-4 base oil at mass fractions of 1.5wt% and 2wt%, respectively, and sonicated at 25℃for 1h to give a ring Ding Jiasuan/cobalt lubricating composition.
Example 3
Nickel metal particles and cyclopropane-1, 1-dicarboxylic acid are added into dioctyl sebacate base oil together according to the mass fraction of 2wt% and 2wt%, and ultrasonic treatment is carried out for 1h at the temperature of 25 ℃ to obtain the cyclopropane-1, 1-dicarboxylic acid/nickel lubricating composition.
Performance testing
1) And performing friction test by adopting a ball disc reciprocating mode of the SRV fretting friction wear testing machine. The lower test disc (24.0 mm in diameter and 7.9mm in height) and the upper test ball (10 mm in diameter) are made of GCr15 bearing steel, the hardness is 650-700HV, and the surface roughness is less than 20nm. To reduce contamination, the steel disc and steel ball were ultrasonically cleaned with petroleum ether prior to the friction test. The volume of lubricant used for each friction test was 0.025mL. The friction test was carried out for 30min at a frequency of 25Hz, an amplitude of 1mm, a load of 50N and a test temperature of 25 ℃.
FIG. 1 is a graph showing the real-time change in friction coefficient of PAO-4 base oil and the lubricating composition of example 1 (cyclopropanecarboxylic acid/copper lubricating system). The friction coefficient of PAO-4 gradually increased to 0.25 five minutes after the start of the test and fluctuated drastically throughout the test. However, for the cyclopropanecarboxylic acid/copper lubricating composition, the coefficient of friction remained stable at around 0.13 throughout the 30min test, and the coefficient of friction curve became smoother.
FIG. 2 is a plot of the plaque diameter after a friction test of PAO-4 base oil (a) and lubricating composition (b) provided in example 1; (c) PAO-4 base oil and (d) wear scar morphology of the lower test disc after friction testing of the lubricating composition provided in example 1. As can be seen from the diameter of the abrasive spots and the shape of the abrasive marks in FIG. 2, the diameter of the abrasive spots formed after the PAO-4 friction test is up to 0.502mm, and the shape of the abrasive marks of the lower test disc shows that the sliding surface is seriously damaged, and furrows and serious plastic deformation exist at the abrasive marks; the abrasion mark of the lower test disc was very smooth with only slight furrows, with the abrasion mark diameter of the abrasion test of the cyclopropanecarboxylic acid/copper lubricating composition reduced to 0.328 mm. The above results indicate that the cyclopropanecarboxylic acid/copper lubricating composition has excellent antiwear and antifriction capabilities compared to PAO-4.
2) The abrasion dust generated by the cyclopropanecarboxylic acid/copper lubricating composition provided in example 1 was observed with a transmission electron microscope, and the results are shown in fig. 3, (a) transmission electron microscope images; (b) a local high resolution transmission electron microscope image. As can be seen from FIG. 3 a, the abrasive dust consists of spherical particles of different sizes, as shown in FIG. 3 b, the localized high resolution transmission electron microscopy image of the abrasive dust further shows that the spherical particles are actually Fe 3 O 4 Particles (lattice spacing of 0.21nm corresponds to Fe 3 O 4 (400) crystal plane); meanwhile, lattice fringes with the interval of 0.34nm can be observed, and the existence of graphene is directly proved.
As can be seen from fig. 1 to 3, during the friction test, cyclopropanecarboxylic acid undergoes a tribochemical reaction under the action of normal force and shear stress to produce hydrocarbons. The hydrocarbon is graphitized under the catalysis of copper, and finally the graphene with excellent lubricating performance is formed. Wear of metal surfaces while producing Fe 3 O 4 Particles, interfaceShearing to form a spherical structure, wherein the graphene is also coated on Fe in the dynamic process of friction 3 O 4 Around the particles. This unique wear dust composition and structure imparts excellent tribological properties to the cyclopropanecarboxylic acid/copper lubricating composition.
3) The ring Ding Jiasuan/cobalt lubricating composition provided in example 2 was friction tested using the ball-disc reciprocation mode of the SRV fretting wear tester. The lower test disc (24.0 mm in diameter and 7.9mm in height) and the upper test ball (10 mm in diameter) are made of GCr15 bearing steel, the hardness is 600-650HV, and the surface roughness is less than 25nm. In order to reduce pollution, the steel disc and the steel ball are ultrasonically cleaned with petroleum ether before friction test. The volume of lubricant used for each friction test was 0.025mL. The friction test was carried out for 30min at a frequency of 25Hz, an amplitude of 1mm, a load of 50N and a test temperature of 25 ℃.
The results show that the maximum coefficient of friction for PAO-4 can reach 0.25, but for the ring Ding Jiasuan/cobalt lubricating composition, the coefficient of friction has stabilized around 0.125 throughout the 30 minute test. The plaque diameter of the ring Ding Jiasuan/cobalt lubricating composition was also reduced from 0.502mm to 0.350mm compared to PAO-4. The above results demonstrate that the ring Ding Jiasuan/cobalt lubricating composition has excellent antiwear and antifriction capabilities compared to PAO-4.
In fig. 4 a is the appearance of the swarf after friction testing of the lubricating composition of example 2, and as shown in fig. 4 a, graphene formation was also observed in the swarf produced by the ring Ding Jiasuan/cobalt lubricating composition.
4) The cyclopropane-1, 1-dicarboxylic acid/nickel lubricating composition provided in example 3 was subjected to a tribological test using the ball-disc reciprocation mode of an SRV fretting wear tester. The lower test disc (24.0 mm in diameter and 7.9mm in height) and the upper test ball (10 mm in diameter) are made of GCr15 bearing steel, the hardness is 650-700HV, and the surface roughness is less than 20nm. In order to reduce pollution, the steel disc and the steel ball are ultrasonically cleaned with petroleum ether before friction test. The volume of lubricant used for each friction test was 0.025mL. The friction test was carried out for 30min at a frequency of 25Hz, an amplitude of 1mm, a load of 50N and a test temperature of 25 ℃.
The results showed that the friction coefficient of dioctyl sebacate increased rapidly to about 0.17 after the start of the test. However, for the cyclopropane-1, 1-dicarboxylic acid/nickel lubricating composition, the coefficient of friction was stable at around 0.12 throughout the 30min test. The diameter of the abrasive spots formed after the dioctyl sebacate friction test is 0.375mm, and the diameter of the abrasive spots formed by the cyclopropane-1, 1-dicarboxylic acid/nickel lubricating composition friction test is reduced to 0.225mm. The above results indicate that the cyclopropane-1, 1-dicarboxylic acid/nickel lubricating composition has excellent anti-wear and anti-friction capabilities compared to dioctyl sebacate.
Fig. 4 b shows the appearance of the swarf after friction testing of the lubricating composition of example 3, and as shown in fig. 4 b, graphene formation was also observed in swarf produced from the cyclopropane-1, 1-dicarboxylic acid/nickel lubricating composition.
From the above examples, the lubricating composition provided by the present invention can realize in-situ formation of graphene during friction to reduce friction and wear.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (5)
1. A lubricating composition capable of forming graphene in situ, comprising metal particles, an active organic compound, and a base lubricating oil; the active organic compound contains a polybasic carbocycle and a carboxyl group;
the metal particles are metal simple substance particles with the particle size of 1-3 mu m;
the mass of the active organic compound is 2wt% of the mass of the base lubricating oil;
the active organic compound comprises any one of cyclopropanecarboxylic acid, cyclopropane-1, 1-dicarboxylic acid, cyclobutane-1, 1-dicarboxylic acid and ring Ding Jiasuan;
the metal particles include any one of zinc particles, copper particles, nickel particles, iron particles, and cobalt particles.
2. The lubricating composition of claim 1, wherein the mass of the metal particles is 0.1 to 2wt% of the mass of the base lubricating oil.
3. The method of preparing a lubricating composition of any of claims 1-2, comprising the steps of:
and mixing the metal particles, the active organic compound and the base lubricating oil under the ultrasonic condition to obtain the lubricating composition capable of forming graphene in situ in the friction process.
4. The method according to claim 3, wherein the mixing temperature is 25-50 ℃ and the mixing time is 0.5-3 hours.
5. Use of a lubricating composition according to any one of claims 1 to 2 or a lubricating composition prepared by a method according to any one of claims 3 to 4 in the lubrication field.
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