CN110724573A - Lubricating oil additive, lubricating oil and preparation method thereof - Google Patents

Lubricating oil additive, lubricating oil and preparation method thereof Download PDF

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CN110724573A
CN110724573A CN201911063597.3A CN201911063597A CN110724573A CN 110724573 A CN110724573 A CN 110724573A CN 201911063597 A CN201911063597 A CN 201911063597A CN 110724573 A CN110724573 A CN 110724573A
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lubricating oil
parts
graphene
weight
additive
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刘朝军
郭玉芬
张慧涛
刘兆平
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Ningbo Graphene Innovation Center Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M141/00Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
    • C10M141/12Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic compound containing atoms of elements not provided for in groups C10M141/02 - C10M141/10
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M177/00Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04Elements
    • C10M2201/041Carbon; Graphite; Carbon black
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2227/00Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/09Complexes with metals

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  • Lubricants (AREA)

Abstract

The application provides a lubricating oil additive, lubricating oil and a preparation method thereof, and belongs to the technical field of lubricating oil. The lubricating oil additive is in a gel form, and comprises 1-2 parts by weight of ferrocene organogelling agent, 5-10 parts by weight of graphene powder, 20-40 parts by weight of oleic acid and 10-20 parts by weight of polycarbon amine. The lubricating oil comprises base oil and lubricating oil additives, wherein the lubricating oil additives are dispersed in the base oil, and the lubricating oil additives dispersed in the base oil are colloidal particles. The lubricating oil additive is added into the lubricating oil, so that long-term lubrication protection can be formed on a friction pair, and the protection effect of graphene can be better exerted.

Description

Lubricating oil additive, lubricating oil and preparation method thereof
Technical Field
The application relates to the technical field of lubricating oil, in particular to a lubricating oil additive, lubricating oil and a preparation method thereof.
Background
In recent years, with the continuous upgrading and upgrading of machine equipment and the continuous improvement of running load and speed, the demand of lubricating oil products is gradually increased, and the performance requirements of the lubricating oil products are also improved. The lubricating oil is used for reducing the friction and the wear of machinery, improving the mechanical efficiency, reducing the energy consumption, preventing sintering and prolonging the mechanical life. It is known that frictional wear is one of the main causes of energy loss and equipment failure.
With the intensive research of nano materials, many researchers find that after the nano particles are dispersed in the lubricating oil, the lubricating oil can play a role in resisting wear and can effectively improve the friction performance of the lubricating oil. The addition of graphene to the lubricating oil enables the friction coefficient and the friction patch diameter to be reduced. However, the inventor finds that if a large amount of graphene is added into the lubricating oil, the graphene with high addition amount is easy to be layered and agglomerated to form large graphite particles, and the large particles not only cannot play a role in lubricating and reducing friction, but also increase abrasion and influence the overall performance of the lubricating oil; if a small amount of graphene is added into the lubricating oil, the function of reducing the friction coefficient to a certain extent can be achieved in a short time, but with the prolonging of time, the graphene can be gradually and continuously consumed along with the abrasion, the amount of the graphene playing a lubricating role can be less and less, and finally the protective effect on the friction side of an engine and the like is lost.
Disclosure of Invention
The application aims to provide a lubricating oil additive, a lubricating oil and a preparation method thereof, which can form long-term lubrication protection on a friction pair and better exert the protection effect of graphene.
In a first aspect, an embodiment of the present application provides a lubricating oil additive, which is in a gel form, and includes, by weight, 1 to 2 parts of a ferrocene organogelator, 5 to 10 parts of graphene powder, 20 to 40 parts of oleic acid, and 10 to 20 parts of polycarbon amine.
Pz orbits of carbon atoms in the graphene, which are vertical to the plane of the layer, can form a large pi bond penetrating through all the layers of polyatomic atoms, and can be easily combined with lipophilic groups in oleic acid and polycarbon amines, so that oleic acid and polycarbon amines are attached to the surface of the graphene, and the gel-like graphene additive is formed after the materials are mixed with the ferrocene organic gelling agent. The graphene additive is composed of a plurality of colloidal particles, at normal temperature, graphene is wrapped in the colloidal particles, and at the temperature higher than 50 ℃ or in a disturbance state, the graphene in the colloidal particles is released into base oil of lubricating oil to protect a friction pair; after the graphene is used for a period of time and the machine is stopped, the graphene is adsorbed in the colloidal particles, so that the graphene is prevented from agglomerating; and when the graphene is used for the next time, releasing the graphene again, and repeating the steps. Can form long-term lubrication protection on the friction pair and better play the protection role of the graphene.
In one possible embodiment, the structural formula of the ferrocene organogelator is:
Figure BDA0002257995530000021
Figure BDA0002257995530000022
wherein R is-NHNH-and Chol is cholesterol.
The special ferrocene organogelator has stronger gelatination, graphene is more easily released under the condition of heating or disturbance, and the graphene is more easily adsorbed by colloidal particles under the condition of normal temperature or no disturbance, so that the performance of the graphene is better exerted.
In one possible embodiment, the graphene powder has a sheet diameter of 1 to 10 μm and a thickness of 0.33 to 3 nm. The sheet diameter and the thickness of the graphene are within the range, so that the graphene is not easy to consume when the friction pair is protected; when the friction pair is not protected, the graphene is easily adsorbed by colloidal particles, and the graphene is prevented from being agglomerated.
In one possible embodiment, the polycarboamines include one or more of tetradecylamine, pentadecylamine, hexadecylamine, heptadecylamine, and octadecylamine. Has more lipophilic groups and is easy to be attached to the surface of the graphene.
In a second aspect, embodiments of the present application provide a lubricating oil, which includes a base oil and the above lubricating oil additive, wherein the lubricating oil additive is dispersed in the base oil, and the lubricating oil additive dispersed in the base oil is in a colloidal particle shape.
When the lubricating oil additive is added into base oil, the lubricating oil additive is not directly and completely compatible with the base oil, but is dispersed in the base oil in a colloidal particle shape. At normal temperature, the graphene is wrapped in the colloidal structure, and is released into the base oil of the lubricating oil at the temperature higher than 50 ℃ or in a disturbance state, so that a friction pair is protected; after the graphene is used for a period of time and the machine is stopped, the graphene is adsorbed in the colloidal structure, so that the graphene is prevented from being agglomerated; and when the graphene is used for the next time, releasing the graphene again, and repeating the steps. Can form long-term lubrication protection on the friction pair and better play the protection role of the graphene.
In one possible embodiment, the weight ratio of base oil to lubricating oil additive is (50-100): 1. in order to have a better lubricating effect.
In a third aspect, embodiments of the present application provide a method for preparing a lubricating oil additive, including the following steps: mixing and dispersing 20-40 parts by weight of oleic acid, 10-20 parts by weight of polycarbon amine, 150 parts by weight of liquid hydrocarbon and 5-10 parts by weight of graphene powder to obtain a first mixed material. And removing the liquid hydrocarbon in the first mixed material to obtain a second mixed material. Mixing the second mixed material with 1-2 parts by weight of ferrocene organogelator, and dispersing for 20-60min at the temperature of 110-130 ℃.
In the first mixed material, due to the action of liquid hydrocarbon, the polycarbon amine and oleic acid substances can be uniformly dispersed, so that more polycarbon amine and oleic acid substances are attached to the surface of the graphene. After the liquid hydrocarbon in the first mixed material is removed, the liquid hydrocarbon and the ferrocene organic gelling agent are dispersed for 20-60min at the temperature of 110-130 ℃, and a gelatinous lubricating oil additive can be formed so as to play the role of graphene.
In one possible embodiment, the liquid hydrocarbon comprises one or more of n-hexane, n-heptane, n-octane, and n-nonane. Oleic acid and polycarbon amine substances can be better dispersed and are more uniformly dispersed, so that lipophilic groups of the oleic acid and the polycarbon amine substances are attached to the surface of the graphene.
In one possible embodiment, a method of preparing a first blend comprises: mixing oleic acid, polycarbon amine and liquid hydrocarbon, and dispersing at 50-70 deg.C for 20-60min to obtain first mixture. And mixing and dispersing the graphene powder and the first mixture for 2-6 h.
The preparation method comprises the steps of uniformly dispersing oleic acid and polycarbon amine substances in liquid hydrocarbon, adding graphene, mixing and dispersing, and enabling the surface of the graphene to be capable of being attached with more lipophilic groups, so that the oleic acid and the polycarbon amine substances are combined with the graphene and formed on the surface of the graphene.
In one possible embodiment, the step of heating is carried out under sealing conditions at a temperature of 140 ℃ and 160 ℃ for a period of 6-12 h. Further, the gel-like lubricating oil additive is heated for 6-12 hours under the sealing condition of 140-160 ℃, so that colloidal particles of the lubricating oil additive can be dispersed more uniformly, the release of graphene and the adsorption of graphene are facilitated, and the function of the graphene is better played.
In a fourth aspect, embodiments of the present application provide a lubricating oil additive prepared by the above method. The lubricating oil additive obtained by the method is in a gel state.
In a fifth aspect, embodiments of the present application provide a lubricating oil, including the lubricating oil additive prepared by the above method, wherein the weight ratio of the base oil to the lubricating oil additive is (50-100): 1. the lubricating oil additive is in a gel form, and after the lubricating oil additive is dispersed in the base oil, the lubricating oil additive is not directly and completely compatible with the base oil, but is dispersed in the base oil in a colloidal particle shape.
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In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments are briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive efforts and also belong to the protection scope of the present application.
FIG. 1 is an SEM image of a lubricating oil additive provided in example 1 of the present application after the lubricating oil additive is dispersed in a base oil.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The graphene has high thermal conductivity, high in-plane mechanical strength and low friction coefficient, so that the graphene can be added into lubricating oil. However, the inventors have found through research that if graphene is directly mixed with base oil and then used as lubricating oil, self-stacking phenomenon occurs due to long-time friction of graphene, graphene is agglomerated, the lubricating effect cannot be achieved, and the friction coefficient is increased; if the amount of the graphene is reduced, the graphene is continuously consumed along with abrasion, the amount of the graphene is less and less, and the function of reducing friction is finally not achieved.
Therefore, the application provides a special lubricating oil additive, after adding this lubricating oil additive in lubricating oil, can improve the reunion of graphite alkene and from the stacking phenomenon, can avoid the consumption of graphite alkene again and can not play the effect that reduces friction, make graphite alkene can form permanent lubrication protection to the friction pair, exert the guard action of graphite alkene better.
Wherein the lubricating oil comprises base oil and the lubricating oil additive. The weight ratio of the base oil to the lubricating oil additive is (50-100): 1. for example: the weight ratio of base oil to lubricant additive is 50:1, 60:1, 70:1, 80:1, 90:1, or 100: 1.
alternatively, the base oil may be a national standard three-type base oil, or a PAO (Poly Alpha olefin) base oil, or other base oils that can be used as lubricating oils.
The lubricant additive is gel-like, and after the lubricant additive is dispersed in the base oil, the lubricant additive is in the form of rubber particles. The lubricating oil additive comprises, by weight, 1-2 parts of ferrocene organogelling agent, 5-10 parts of graphene powder, 20-40 parts of oleic acid and 10-20 parts of polycarbon amine.
Because pz orbits of carbon atoms in the graphene powder, which are vertical to the layer plane, can form a large pi bond penetrating through all layers of polyatomic atoms, the surface of the graphene is easy to combine with lipophilic groups in oleic acid and polycarbon amines, so that oleic acid and polycarbon amines are adhered to the surface of the graphene, and the graphene is mixed with the ferrocene organogelator to form the gel-like graphene additive.
The gel-like graphene additive is composed of a plurality of colloidal particles and has a gelling property. The graphene additive is mixed with the base oil to form the lubricating oil, the graphene additive is suspended in the base oil and exists in a colloidal form, and the colloidal lubricating oil additive is filtered and blocked by a machine when the lubricating oil is placed in an engine. At normal temperature, the kinetic energy of the colloidal particles is small, two ends of the colloidal particles are connected with each other to form a net structure, and the graphene, the oleic acid on the surface of the graphene and the polycarbon amine substance are in the pores of meshes of the net structure and are in a gel state. When lubricating oil is used, the temperature of the lubricating oil is increased due to mechanical friction, the lubricating oil is disturbed, the kinetic energy of colloidal particles is increased, the movement speed of the colloidal particles is increased, the connection between the colloidal particles can be eliminated, the reticular structure does not exist, and the colloidal particles are in a free state, so that gel is converted into sol, graphene in the colloidal particles is released, and the graphene passes through a machine filter and enters a friction pair, so that the graphene plays an effective wear-resistant and loss-reducing role in the lubricating oil.
In the using process of the lubricating oil, the colloidal particle lubricating oil additive is slowly dissolved in the base oil, so that the graphene can be slowly released in the base oil, part of the lubricating oil additive is still dispersed in the base oil in a colloidal particle shape and is blocked by a mechanical filter, and the part of the graphene is temporarily stored in the colloidal particle structure and cannot enter a friction pair. Along with the friction, the graphene released into the base oil is agglomerated, the protection effect on the friction pair is gradually lost, and the graphene is adsorbed by colloidal particles after being circulated to the colloidal particles in the filter, so that the graphene is prevented from being accumulated to form abrasive particles, dry friction and abrasive particle abrasion are prevented, and the effects of wear resistance and wear reduction are more easily exerted.
Along with the continuous going on of friction, the solubility of gel also can be along with the rising of temperature and the continuous going on of friction and increase gradually, and the gel that does not form the sol this moment can turn into the sol gradually, and then releases not reunion graphite alkene and gets into in the machine oil, continues to protect the friction pair, can effectively guarantee the effective concentration of graphite alkene in lubricating oil, prolongs the live time of graphite alkene.
The lubricating oil additive for slowly releasing the graphene can effectively ensure the dispersibility of the graphene in the base oil, avoid the phenomena of self-stacking and agglomeration of the graphene in the base oil, and fully play the roles of reducing friction and resisting loss of the graphene in the lubricating oil.
Optionally, the lubricating oil additive comprises, by weight, 1.2-1.8 parts of ferrocene organogelator, 6-8 parts of graphene powder, 25-30 parts of oleic acid and 12-18 parts of polycarbon amine. For example: the weight portion of the ferrocene organogelator is 1 portion, 1.2 portions, 1.5 portions, 1.8 portions or 2 portions; the graphene powder is 5 parts, 6 parts, 7 parts, 8 parts or 10 parts by weight; the oleic acid accounts for 20 parts, 25 parts, 28 parts, 30 parts or 40 parts by weight; the weight portion of the polycarbon amine is 10 portions, 12 portions, 15 portions, 18 portions or 20 portions. Wherein, the structural formula of the ferrocene organogelator can be:
Figure BDA0002257995530000071
Figure BDA0002257995530000072
wherein R is-NHNH-, -Chol is cholesterol. Optionally, the cholesterol is a derivative of cyclopentanoperhydrophenanthrene. The ferrocene organogelator is a product of the national medicine group.
The ferrocene organogelator has stronger gelatination, graphene is more easily released under the condition of heating or disturbance, and the graphene is more easily adsorbed by colloidal particles under the condition of normal temperature or no disturbance, so that the performance of the graphene is better exerted.
In other embodiments, the structural formula of the ferrocene organogelator may also be:
or
Figure BDA0002257995530000074
Optionally, the graphene powder has a sheet diameter of 1-10 μm and a thickness of 0.33-3 nm. For example: the graphene powder has a sheet diameter of 1 μm, 3 μm, 5 μm, 8 μm, or 10 μm and a thickness of 0.33nm, 0.5nm, 1nm, 2nm, or 3 nm.
The polycarboamines include one or more of tetradecylamine, pentadecylamine, hexadecylamine, heptadecylamine, and octadecylamine. For example: the polycarbon amine can be tetradecylamine; the polycarbon amine may be pentadecamine; the polycarboamine may be hexadecylamine; the polycarboamine may be heptadecaamine; the polycarboamine may be octadecylamine; the polycarbon amine can be a mixture of tetradecylamine and pentadecamine; the polycarbon amine can be a mixture of decatetramine and hexadecylamine; the polycarbon amine can be a mixture of tetradecylamine and heptadecylamine; the polycarbon amine can be a mixture of tetradecylamine and octadecylamine; the polycarbon amine can be a mixture of decatetramine, pentadecamine and hexadecylamine; the polycarbon amine can be a mixture of deca-tetramine, pentadecamine and hepta-heptadecamine; the polycarbon amine can be a mixture of deca-tetramine, pentadecamine and octadecylamine; the polycarboamines may be tetradecylamine, pentadecylamine, hexadecylamine, heptadecylamine, octadecylamine, etc.
The preparation method of the lubricating oil additive comprises the following steps:
s10, mixing 20-40 parts by weight of oleic acid, 10-20 parts by weight of polycarbon amine and 150-300 parts by weight of liquid hydrocarbon, and dispersing at 50-70 ℃ for 20-60min to obtain a first mixture. The polycarboamine and oleic acid substances can be uniformly dispersed in the liquid hydrocarbon.
Optionally, 20-40 parts by weight of oleic acid and 10-20 parts by weight of polycarbon amine are added into 150-300 parts by weight of liquid hydrocarbon, and are stirred and dispersed in a water bath (50-70 ℃) for 20-60min, so that the oleic acid and the polycarbon amine are fully dissolved, and a first mixture is obtained.
In some embodiments, the temperature of the water bath may be 50 ℃, 55 ℃, 60 ℃, 65 ℃ or 70 ℃; the water bath dispersion time can be 20min, 30min, 40min, 50min or 60 min.
Wherein the liquid hydrocarbon may be a C5-C16 hydrocarbon compound. Optionally, the liquid hydrocarbon comprises one or more of n-hexane, n-heptane, n-octane, and n-nonane. For example: the liquid hydrocarbon may be n-hexane; the liquid hydrocarbon may be n-heptane; the liquid hydrocarbon may be n-octane; the liquid hydrocarbon may be n-nonane; the liquid hydrocarbon can be a mixture of n-hexane and n-heptane; the liquid hydrocarbon can be a mixture of n-hexane and n-octane; the liquid hydrocarbon can be a mixture of n-hexane and n-nonane; the liquid hydrocarbon can be a mixture of n-hexane, n-heptane and n-octane; the liquid hydrocarbon can be a mixture of n-hexane, n-heptane and n-nonane; the liquid hydrocarbon may be n-hexane, n-heptane, a mixture of n-octane and n-nonane, etc.
And S20, mixing and dispersing 5-10 parts by weight of graphene powder and the first mixture for 2-6h to obtain a first mixed material. The lipophilic groups of oleic acid and polycarbon amine substances can be attached to the surface of the graphene, so that the graphene, the oleic acid and the polycarbon amine molecules are combined.
Optionally, 5-10 parts by weight of graphene powder is added into the first mixture, and after stirring and dispersing for 30min, the first mixture is obtained by ball milling and dispersing for 2-6h in a high-energy ball mill, so that oleic acid and polycarbon amine substances are combined with graphene as much as possible. Wherein, the time of ball milling dispersion can be 2h, 3h, 4h, 5h or 6 h.
In other embodiments, the step S10 and the step S20 may be combined into one step to prepare, for example: mixing and dispersing 20-40 parts of oleic acid, 10-20 parts of polycarbon amine, 150-300 parts of liquid hydrocarbon and 5-10 parts of graphene powder to obtain a first mixed material.
And S30, removing the liquid hydrocarbon in the first mixed material to obtain a second mixed material. And removing the solvent in the first mixed material, and drying the first mixed material in a vacuum oven for 20-30min to obtain a second mixed material.
S40, mixing the second mixture with 1-2 parts by weight of ferrocene organogelator, and dispersing for 20-60min at the temperature of 110-130 ℃ to obtain the gelatinous lubricating oil additive (third mixture).
Optionally, 1-2 parts by weight of ferrocene organogelling agent is added into the second mixed material, and the mixture is sealed, heated, stirred and dispersed for 20-60min in an oil bath (110-.
In some embodiments, the temperature of the oil bath may be 110 ℃, 115 ℃, 120 ℃, 125 ℃, or 130 ℃; the time for heating, stirring and dispersing by oil bath can be 20min, 30min, 40min, 50min or 60 min.
S50, further processing the lubricating oil additive, and heating for 6-12h under the sealing condition of the temperature of 140-160 ℃. Optionally, the third mixture is sealed in a high-pressure reaction kettle with a polytetrafluoroethylene lining, heated for 6-12h at the temperature of 140-160 ℃, and taken out for cooling, so that the lubricating oil additive for slow release of graphene can be obtained.
After the lubricating oil additive obtained by the method is added into base oil, the lubricating oil additive can be used as lubricating oil, so that long-term lubrication protection can be formed on a friction pair, and the protection effect of graphene can be better exerted.
Examples
The component contents of the lubricating oil additives and the methods for their preparation are shown in table 1,
TABLE 1 lubricating oil additive compositions and methods of making the same
Figure BDA0002257995530000091
Figure BDA0002257995530000101
The lubricating oil additives prepared in examples 1 to 7 and comparative examples 1 to 8 were added to the base oil to conduct the examination of frictional properties, respectively. The specific method is that 1 part or 0.5 part of lubricating oil additive is respectively added into 50 parts of base oil, heated for 5min at 60 ℃, and then the friction performance of the target product is tested by a four-ball machine to obtain the following table 2,
TABLE 2 Friction Properties of lubricating oils
Figure BDA0002257995530000102
Figure BDA0002257995530000111
As can be seen from Table 2, it can be seen that the absence of the ferrocene organogelator results in an increase in the friction coefficient and an increase in the wear scar diameter of the lubricating oil as compared to the comparative example 1, and the friction coefficient and the wear scar diameter are comparable to those of the blank (no lubricating oil additive added). Therefore, it can be shown that the addition of ferrocene organogel can improve the lubricating effect of the lubricating oil additive.
As can be seen from comparison of examples 1-4 with comparative example 2, if the amine polypeptide is an amine salt, the friction coefficient of the lubricating oil increases, the wear scar diameter increases, and the dissolution time of the lubricating oil additive increases. Therefore, it can be shown that the amine salts of the polypeptides reduce the lubricating effect of the lubricating oil additive.
As can be seen from comparison of example 1 with comparative example 3, the lubricating effect of the lubricating oil additive obtained without adding oleic acid was poor.
It can be seen from examples 1 and 4 and comparative example 4 that the lubricating oil additive obtained without adding the polycarbon amine-based substance has poor lubricating effect.
As can be seen from comparison of examples 1 to 4 with comparative example 5, if graphene is replaced with graphene oxide, the friction coefficient of the lubricating oil increases and the wear scar diameter increases. Therefore, it can be said that graphene oxide decreases the lubricating effect of the lubricating oil additive.
As can be seen from comparison of example 1 with comparative example 6, if no liquid hydrocarbon is added at the time of preparing the lubricating oil additive, the lubricating effect of the resulting lubricating oil additive is poor.
As can be seen from comparison of example 1, example 2 and comparative example 7, if the graphene and the ferrocene are added in one step and mixed with the oleic acid, the peptide amine and the liquid hydrocarbon, the lubricating effect of the obtained lubricating oil additive is poor.
Comparing example 1 with example 2, it can be seen that the lubricating oil additive obtained by dissolving oleic acid and the peptide amine in liquid hydrocarbon and adding graphene has better lubricating effect.
In comparison between example 1 and example 3, it can be seen that the lubricating oil additive obtained without heat treatment after addition of the ferrocene organogelling agent has a slightly inferior lubricating effect.
Comparing example 1 with example 4, it can be seen that the lubricating oil additive obtained by using octadecylamine or tetradecylamine as the polypeptide amine substance has better lubricating effect.
Examples of the experiments
The lubricant additive obtained in example 1 was dispersed in the base oil at a weight ratio of 1:50, and after the lubricant additive was dispersed in the base oil, the lubricant additive had a gel-coated graphene, so that the color was darker than that of the base oil, and a sample in which the lubricant and the lubricant additive were dispersed was taken out, the lubricant was removed, the lubricant additive was dried, and the lubricant additive was detected by scanning electron microscopy to obtain an SEM image of the dispersed lubricant additive, as shown in fig. 1, and as can be seen from fig. 1, the obtained lubricant additive had a granular structure. If the lubricating oil additive is directly detected by a scanning electron microscope, the lubricating oil additive is of a lamellar structure. It can be concluded that after the lubricant additive is added to the base oil, the gelatinous lubricant additive is dispersed in the base oil in the form of colloidal particles.
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

Claims (10)

1. The lubricating oil additive is characterized by being in a gel state and comprising 1-2 parts by weight of ferrocene organogelling agent, 5-10 parts by weight of graphene powder, 20-40 parts by weight of oleic acid and 10-20 parts by weight of polycarbon amine.
2. The lubricating oil additive of claim 1, wherein the ferrocene organogelator has the formula:
Figure FDA0002257995520000011
wherein R is-NHNH-and Chol is cholesterol.
3. The lubricant additive according to claim 1 or 2, wherein the graphene powder has a flake diameter of 1 to 10 μm and a thickness of 0.33 to 3 nm;
optionally, the polycarboamines include one or more of tetradecylamine, pentadecylamine, hexadecylamine, heptadecylamine, and octadecylamine.
4. A lubricating oil comprising a base oil and the lubricating oil additive of any one of claims 1 to 3, said lubricating oil additive being dispersed in said base oil, and said lubricating oil additive being dispersed in said base oil in the form of colloidal particles;
optionally, the weight ratio of the base oil to the lubricating oil additive is (50-100): 1.
5. a preparation method of a lubricating oil additive is characterized by comprising the following steps:
mixing and dispersing 20-40 parts by weight of oleic acid, 10-20 parts by weight of polycarbon amine, 150 parts by weight of liquid hydrocarbon and 5-10 parts by weight of graphene powder to obtain a first mixed material;
removing the liquid hydrocarbon in the first mixed material to obtain a second mixed material;
mixing the second mixture with 1-2 parts by weight of ferrocene organogelling agent, and dispersing for 20-60min at the temperature of 110-130 ℃.
6. The method of claim 5, wherein the liquid hydrocarbon comprises one or more of n-hexane, n-heptane, n-octane, and n-nonane.
7. A method of preparing according to claim 6, characterized in that said first mix preparation method comprises:
mixing the oleic acid, the polycarbon amine and the liquid hydrocarbon, and dispersing at 50-70 ℃ for 20-60min to obtain a first mixture;
mixing and dispersing the graphene powder and the first mixture for 2-6 h.
8. The method of manufacturing according to claim 5, further comprising: heating for 6-12h under the sealing condition of the temperature of 140-160 ℃.
9. A lubricating oil additive, characterized by being produced by the production method according to any one of claims 5 to 8.
10. A lubricating oil comprising a base oil and the lubricating oil additive of claim 9, in a weight ratio of (50-100): 1.
CN201911063597.3A 2019-11-01 2019-11-01 Lubricating oil additive, lubricating oil and preparation method thereof Pending CN110724573A (en)

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