Alkylated nanoparticles as well as preparation method and application thereof

Abstract

The invention discloses alkylated nanoparticles as well as a preparation method and application thereof, and belongs to the technical field of lubricating materials. The preparation method of the alkylated nanoparticles comprises the following steps: mixing nanoparticles with an organic solvent, and then carrying out ultrasonic treatment to obtain a first mixed solution; mixing the multi-carbon amine and the first mixed solution, heating, stirring and dispersing, and then performing ultrasonic dispersion to obtain a second mixed solution; the second mixed solution is subjected to a reaction through a microwave-assisted ball milling method, and the alkylated nanoparticle material is obtained. In addition, the invention also provides the alkylated nanoparticles which are prepared by the preparation method. In addition, the invention also provides the alkylated nanoparticles prepared by the preparation method or application of the alkylated nanoparticles as a lubricating oil additive. According to the preparation method provided by the invention, the reaction is accelerated, the reaction time is shortened, and the alkylated nanoparticles with excellent lubricating performance can be prepared only by ball milling for 60 minutes.

Description

Technical Field

[0001] The invention relates to the technical field of lubricating materials, and in particular to an alkylated nanoparticle and a preparation method and application thereof. Background Art

[0002] With the continuous development of modern mechanical equipment and the continuous upgrading of precision equipment, friction and wear, as a common problem in daily life, will consume a lot of energy, reduce the service life of mechanical parts, and cause mechanical transmission failure, resulting in increasing attention to the problem of friction and wear. As we all know, adding lubricants is the most effective way to reduce friction and wear. However, traditional lubricants usually contain elements such as sulfur, phosphorus, and chlorine. They are not only easy to decompose, but also cause serious environmental pollution when used in large quantities. Under ordinary working conditions, the friction reduction effect of traditional lubricant additives is general and cannot meet the lubrication of mechanical equipment under high speed, heavy load, high temperature and high pressure working conditions. Therefore, lubricant additives are crucial to improving lubricant performance. Nanomaterials are often used as lubricant additives due to their advantages such as high specific surface area, in-plane strength, weak layer-layer interaction and surface chemical stability. Therefore, nanocomposite lubricant additives with excellent tribological properties have become a new hot spot in the field of lubricants.

[0003] The nanoparticles currently used have broad application prospects, but there are still many scientific and engineering problems that need to be solved. Because of their strong polarity, they are easy to agglomerate, resulting in poor lubrication performance, and they cannot be dispersed for a long time and cannot be stored for a long time. Therefore, more studies use chemical modification methods to synthesize alkylated nanoparticles to achieve the characteristics of not easy to agglomerate and good dispersion. However, the current chemical modification process requires more than 12 hours of reaction time to produce effective products. There are problems such as long reaction time, complex reaction conditions, low yield, etc., which are not conducive to industrialization. In order to solve the above problems, it is urgent to design a convenient and green chemical modification method to synthesize alkylated nanoparticles to configure lubricants with excellent performance. Summary of the invention

[0004] The purpose of the present invention is to overcome the above technical deficiencies, provide an alkylated nanoparticle and a preparation method and application thereof, and solve the technical problem that it takes a long time to prepare the alkylated nanoparticle in the prior art.

[0005] In order to achieve the above technical purpose, the technical solution of the present invention provides a method for preparing alkylated nanoparticles, comprising the following steps:

[0006] S1, mixing the nanoparticles with an organic solvent, and then ultrasonically treating the mixture to obtain a first mixed solution;

[0007] S2, mixing the polyamine and the first mixed solution, heating and stirring to disperse, and then ultrasonically dispersing to obtain a second mixed solution;

[0008] S3. The second mixed solution is reacted by microwave-assisted ball milling to obtain the alkylated nanoparticles.

[0009] In any embodiment, in step S1, the nanoparticles are one or more of graphene oxide, graphene, carbon nanotubes and hexagonal boron nitride; and / or, in step S3, the microwave power in the microwave-assisted ball milling method is 1000-1150W, the ball milling speed is 200rpm-250rpm, and the ball-to-material mass ratio is 2:(1-3).

[0010] In any embodiment, in step S2, the polyamine is one or more of tetradecylamine, pentadecylamine, hexadecylamine, heptadecanylamine and octadecylamine; and / or, in step S1, the organic solvent is a mixture of anhydrous ethanol and N-methylpyrrolidone; the mass ratio of the anhydrous ethanol to the N-methylpyrrolidone is 1:(4-4.5); the mass ratio of the nanoparticles to the organic solvent is 1:(250-280).

[0011] In any embodiment, in step S1, the ultrasonic treatment time is 10-20 min; and / or, in step S2, the mass ratio of the polyamine to the nanoparticles is (1-3):1, and the temperature of the heating, stirring and dispersing is 90-95°C, and the time is 10-20 min.

[0012] In any embodiment, before step S3, the method further includes adding an additive to the second mixed liquid; the additive includes a first sub-additive and / or a second sub-additive; and the mass ratio of the polyamine to the additive is 5:(1-5).

[0013] In any embodiment, the first additive is one or more of dicyclohexylcarbodiimide, diisopropylcarbodiimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide; and / or, the second additive is one or more of 1-hydroxy-7-azobenzotriazole, 1-hydroxybenzotriazole and 1-hydroxy-1H-1,2,3-triazole-4-carboxylic acid ethyl ester.

[0014] In addition, the present invention also provides an alkylated nanoparticle, which is prepared by the above-mentioned preparation method.

[0015] In addition, the present invention also proposes the use of the alkylated nanoparticles prepared by the above preparation method or the above alkylated nanoparticles as lubricating oil additives.

[0016] In any embodiment, the alkylated nanoparticles are added to the base oil, which is then heated and ultrasonically treated at 55-65° C. to obtain the lubricating oil, wherein the alkylated nanoparticles account for 0.01%-2% of the mass of the base oil.

[0017] In any embodiment, before the heating ultrasound, a dispersant is added to the base oil, and the dispersant is one or more of polyisobutylene bissuccinimide, triethylhexyl phosphoric acid, vinyl bisstearamide, stearic acid monoglyceride, polyethylene glycol and monoalkenyl succinimide; the dispersant is 1%-5% of the mass of the base oil.

[0018] Compared with the prior art, the beneficial effects of the present invention include: the preparation method of the alkylated nanoparticles proposed in the present invention comprises mixing the nanoparticles with an organic solvent, and then ultrasonically treating the nanoparticles to obtain a first mixed solution; mixing the polyamines with the first mixed solution and performing heating, stirring and dispersion, and then ultrasonically dispersing the mixture to obtain a second mixed solution; and subjecting the second mixed solution to a reaction by microwave-assisted ball milling to obtain the alkylated nanoparticle material. The ball milling method and microwave technology are combined to accelerate the reaction and shorten the reaction time. The alkylated nanoparticles with excellent lubrication performance can be obtained by ball milling for only 60 minutes, and the alkylated nanoparticles can be used in lubrication of lubricating oils. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is a SEM image of the alkylated nanoparticles-alkylated graphene oxide prepared in Example 1 of the present invention.

[0020] Figure 2 TEM comparison images of the alkylated nanoparticles (a) prepared in Example 1 and the graphene oxide before modification (b).

[0021] Figure 3 XRD comparison diagram of the alkylated nanoparticles (a) prepared in Example 1 and the graphene oxide before modification (b).

[0022] Figure 4 This is a comparison chart of the friction coefficients of castor oil, graphene oxide (GO), and the alkylated nanoparticles prepared in Example 1 as lubricating oil additives.

[0023] Figure 5 The following are actual photographs of graphene oxide (GO) before modification and modified graphene oxide (RGO) of Example 1 after being allowed to stand in castor oil as the base oil for a period of time, wherein a is a actual photograph of the graphene oxide additive before modification and the modified graphene oxide additive after being allowed to stand in castor oil for 1 day, b is a actual photograph of the graphene oxide additive before modification and the modified graphene oxide additive after being allowed to stand for 60 days, and c is a actual photograph of the graphene oxide additive before modification and the modified graphene oxide additive after being allowed to stand for 150 days. DETAILED DESCRIPTION

[0024] The "range" disclosed in the present application is defined in the form of a lower limit and an upper limit, and a given range is defined by selecting a lower limit and an upper limit, and the selected lower limit and upper limit define the boundaries of the particular range. The range defined in this way can be inclusive or exclusive of the end values, and can be arbitrarily combined, that is, any lower limit can be combined with any upper limit to form a range. For example, if a range of 60 to 120 and 80 to 110 is listed for a particular parameter, it is understood that a range of 60 to 110 and 80 to 120 is also expected. In addition, if the minimum range values ​​1 and 2 are listed, and if the maximum range values ​​3, 4 and 5 are listed, the following ranges can all be expected: 1 to 3, 1 to 4, 1 to 5, 2 to 3, 2 to 4 and 2 to 5. In the present application, unless otherwise specified, the numerical range "a to b" represents an abbreviation of any real number combination between a and b, where a and b are both real numbers. For example, the numerical range "0-5" means that all real numbers between "0-5" are listed in this document, and "0-5" is just an abbreviation of these numerical combinations. In addition, when a parameter is expressed as an integer ≥ 2, it is equivalent to disclosing that the parameter is, for example, an integer of 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0025] If there is no special explanation, the "include" and "comprising" mentioned in this application are open-ended or closed-ended. For example, the "include" and "comprising" may mean that other components not listed may also be included or only the listed components may be included or only the listed components may be included.

[0026] If not specifically stated, in this application, the term "or" is inclusive. For example, the phrase "A or B" means "A, B, or both A and B". More specifically, any of the following conditions satisfies the condition "A or B": A is true (or exists) and B is false (or does not exist); A is false (or does not exist) and B is true (or exists); or both A and B are true (or exist).

[0027] This specific embodiment provides a method for preparing alkylated nanoparticles, comprising the following steps:

[0028] S1. Mixing nanoparticles with an organic solvent, and then ultrasonically treating for 10-20 min to obtain a first mixed solution; the nanoparticles are one or more of graphene oxide, graphene, carbon nanotubes and hexagonal boron nitride; the organic solvent is a mixture of anhydrous ethanol and N-methylpyrrolidone; the mass ratio of the anhydrous ethanol to the N-methylpyrrolidone is 1:(4-4.5); the mass ratio of the nanoparticles to the organic solvent is 1:(250-280);

[0029] S2, mixing the polyamine and the first mixed solution and performing heating, stirring and dispersing, and then ultrasonically dispersing to obtain a second mixed solution; the polyamine is one or more of tetradecylamine, pentadecylamine, hexadecylamine, heptadecanylamine and octadecylamine; the mass ratio of the polyamine to the nanoparticles is (1-3):1, and the temperature of the heating, stirring and dispersing is 90-95°C and the time is 10-20min;

[0030] S3. The second mixed liquid is reacted by microwave-assisted ball milling to obtain the alkylated nanoparticle material; in the microwave-assisted ball milling method, the microwave power is 1000-1150W, the ball milling speed is 200rpm-250rpm, and the ball-to-material mass ratio is 2:(1-3).

[0031] In some embodiments, before step S3, the method further includes adding an additive to the second mixed liquid; the additive includes a first sub-additive and / or a second sub-additive; the mass ratio of the polyamine to the additive is 5:(1-5); the first additive is one or more of dicyclohexylcarbodiimide (DCC), diisopropylcarbodiimide (DIC) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (EDCI); and / or the second additive is one or more of 1-hydroxy-7-azobenzotriazole (HOAT), 1-hydroxybenzotriazole (HOBT) and 1-hydroxy-1H-1,2,3-triazole-4-carboxylic acid ethyl ester (HOCT).

[0032] This specific embodiment also provides an alkylated nanoparticle, which is prepared by the above preparation method.

[0033] This specific embodiment also proposes the use of the alkylated nanoparticles obtained by the above preparation method or the above alkylated nanoparticles as a lubricant additive, wherein the alkylated nanoparticles are added to a base oil, and then heated and ultrasonically treated at 55-65° C. to obtain a lubricant, wherein the alkylated nanoparticles account for 0.005%-2% of the mass of the base oil.

[0034] In some embodiments, the method further includes adding a dispersant to the base oil before the heating ultrasound, wherein the dispersant is one or more of polyisobutylene bissuccinimide, triethylhexyl phosphoric acid, vinyl bisstearamide, stearic acid monoglyceride, polyethylene glycol and monoalkenyl succinimide; and the dispersant is 1%-5% of the mass of the base oil.

[0035] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0036] In the present invention, reference is made to “some embodiments”, “this embodiment”, examples, etc., which describe a subset of all possible embodiments, but it can be understood that “some embodiments” may be the same subset or different subsets of all possible embodiments and may be combined with each other without conflict.

[0037] If similar descriptions of "first / second" appear in the application documents, the following instructions are added. In the following description, the terms "first\second\third" involved are merely used to distinguish similar objects and do not represent a specific ordering of the objects. It can be understood that "first\second\third" can be interchanged in a specific order or sequence where permitted, so that the embodiments described herein can be implemented in an order other than that illustrated or described herein.

[0038] In this embodiment, the term "and / or" is merely a description of the association relationship between associated objects, indicating that three relationships may exist. For example, object A and / or object B may represent three situations: object A exists alone, object A and object B exist at the same time, and object B exists alone.

[0039] Hereinafter, the embodiments of the present application will be described. The embodiments described below are exemplary and are only used to explain the present application, and should not be construed as limiting the present application. If no specific techniques or conditions are indicated in the embodiments, the techniques or conditions described in the literature in this area or the product specifications are used. If the manufacturer is not indicated in the reagents or instruments used, they are all conventional products that can be obtained commercially.

[0040] Example 1

[0041] This embodiment provides an alkylated nanoparticle, which is prepared by the following steps:

[0042] S1, dispersing 1 g of graphene oxide nanoparticles in a mixed solution of 50 g of anhydrous ethanol and 200 g of N-methylpyrrolidone, and ultrasonically treating for 10 minutes to obtain a graphene oxide dispersion;

[0043] S2, adding 1g of octadecylamine and the above-mentioned graphene oxide dispersion, heating and stirring at 90°C for 10 minutes to dissolve the solution and disperse it evenly, then ultrasonically dispersing it for 10 minutes, adding 0.2g EDCI and 0.5g HOAT again, stirring and dispersing them for 10 minutes, and then reacting for 60 minutes under the combined action of microwave power 1000W and ball mill speed 200rpm, wherein the ball-to-material ratio is 1:1, and the mixture is centrifuged to obtain a precipitate; the black precipitate obtained by the reaction is centrifuged and collected, and then the product is centrifuged and washed with hot ethanol to eliminate excess octadecylamine, and finally the product is placed in a vacuum drying oven, dried at 50°C for 24h, and then ground and sieved to obtain alkylated graphene oxide nanoparticles.

[0044] The SEM image of the alkylated graphene oxide nanoparticles prepared in this example is as follows: Figure 1 As shown, it exhibits disordered display with more wrinkles and wrinkles, showing many folded shapes and uneven fluffy features. The wrinkled and wrinkled surface is related to the introduced oxygen-containing group defects, indicating that the alkylated graphene oxide nanoparticles are successfully modified.

[0045] TEM images of alkylated graphene oxide nanoparticles are shown in Figure 2 (a), compared with Figure 2 (a) The number of layers and thickness of graphene oxide nanoparticles, indicating that the alkylated graphene oxide particles have fewer layers. The alkylated graphene oxide nanoparticle layer is divided into two parts, resulting in fewer layers in one piece and an increase in the distance between the crystal planes, making it thinner and reducing the agglomeration of graphene oxide.

[0046] The XRD pattern of alkylated graphene oxide nanoparticles is shown in Figure 3 As shown, GO exhibits a characteristic diffraction peak at 2θ = 10.5°, and ODA-GO exhibits a sharp diffraction peak at 2θ = 4.9°. It can be seen that the interlayer spacing of ODA-GO is much larger than that of GO because there are huge octadecyl chains on the basal plane of GO, which shows that the modification of graphene oxide with octadecylamine is successful.

[0047] Example 2

[0048] This embodiment provides an alkylated nanoparticle, which is prepared by the following steps:

[0049] S1, dispersing 1 g of graphene oxide nanoparticles in a mixed solution of 50 g of anhydrous ethanol and 225 g of N-methylpyrrolidone, and ultrasonically treating for 15 minutes to obtain a graphene oxide dispersion;

[0050] S2, adding 1g of tetradecylamine and the dispersion liquid, heating and stirring at 90°C for 15 minutes to dissolve the solution and disperse it evenly, then ultrasonically dispersing it for 10 minutes, adding 0.1g EDCI and 0.5g HOCT again, stirring and dispersing them for 10 minutes, then ultrasonically dispersing them for 10 minutes, and then reacting them for 60 minutes under the combined action of a microwave power of 1000W and a ball milling speed of 200rpm, wherein the ball-to-material ratio is 2:3, and the mixture is centrifuged to obtain a precipitate; the black precipitate obtained by the reaction is centrifuged and collected, and then the product is centrifuged and washed with hot ethanol to eliminate excess octadecylamine, and finally the product is placed in a vacuum drying oven, dried at 50°C for 24h, and then ground and sieved to obtain alkylated graphene oxide nanoparticles.

[0051] Example 3

[0052] This embodiment provides an alkylated nanoparticle, which is prepared by the following steps:

[0053] S1, dispersing 1 g of graphene oxide nanoparticles in a mixed solution of 50 g of anhydrous ethanol and 215 g of N-methylpyrrolidone, and ultrasonically treating for 20 minutes to obtain a graphene oxide dispersion;

[0054] S2, adding 1g of pentadecylamine and graphene oxide dispersion, heating and stirring at 95°C for 10 minutes to dissolve the solution and disperse it evenly, then ultrasonically dispersing it for 10 minutes, adding 0.2g EDCI and 0.4g HOBT again, stirring and dispersing them for 10 minutes, then ultrasonically dispersing them for 10 minutes, and then reacting them for 40 minutes under the combined action of microwave power 1100W and ball mill speed 250rpm, wherein the ball-to-material ratio is 1:3, and centrifuging the mixture to obtain a precipitate; collecting the black precipitate obtained by the reaction by centrifugation, and then centrifugally washing the product with hot ethanol to eliminate excess octadecylamine, and finally placing the product in a vacuum drying oven, drying it at 50°C for 24h, and then grinding and sieving to obtain alkylated graphene oxide nanoparticles.

[0055] Example 4

[0056] This embodiment provides an alkylated nanoparticle, which is prepared by the following steps:

[0057] S1, dispersing 1 g of graphene oxide nanoparticles in a mixed solution of 50 g of anhydrous ethanol and 220 g of N-methylpyrrolidone, and ultrasonically treating for 10 minutes to obtain a graphene oxide dispersion;

[0058] S2, adding 1g of hexadecylamine and graphene oxide dispersion, heating and stirring at 90°C for 20 minutes to dissolve the solution and disperse it evenly, then ultrasonically dispersing it for 10 minutes, adding 0.2g of EDCI and 0.4g of HOAT again, stirring and dispersing it for 10 minutes, then ultrasonically dispersing it for 10 minutes, and then reacting it for 40 minutes under the combined action of microwave power 1150W and ball mill speed 220rpm, wherein the ball-to-material ratio is 1:2, and the mixture is centrifuged to obtain a precipitate; the black precipitate obtained by the reaction is collected by centrifugation, and then the product is centrifuged and washed with hot ethanol to eliminate excess octadecylamine, and finally the product is placed in a vacuum drying oven, dried at 50°C for 24h, and then ground and sieved to obtain alkylated graphene oxide nanoparticles.

[0059] Comparative Example 1

[0060] The difference between this comparative example and Example 1 is that only the hydrothermal stirring method is used instead of the microwave-assisted ball milling method in the preparation of the alkylated nanoparticles, and the other steps and raw materials are the same as those in Example 1; specifically, this comparative example proposes an alkylated nanoparticle, which is prepared by the following steps:

[0061] S1, dispersing 1 g of graphene oxide nanoparticles in a mixed solution of 50 g of anhydrous ethanol and 200 g of N-methylpyrrolidone, and ultrasonically treating for 10 minutes to obtain a graphene oxide dispersion;

[0062] S2, adding 1g of octadecylamine and the above graphene oxide dispersion, heating and stirring at 90°C for 10 minutes to dissolve the solution and disperse it evenly, then ultrasonically dispersing it for 10 minutes, adding 0.2g EDCI and 0.5g HOAT again, stirring and dispersing it for 10 minutes, and then continuing to stir and react for 60 minutes, centrifuging the mixture to obtain a precipitate; collecting the black precipitate obtained by the reaction by centrifugation, then centrifuging the product with hot ethanol to eliminate excess octadecylamine, and finally placing the product in a vacuum drying oven, drying it at 50°C for 24h, and then grinding and sieving to obtain alkylated graphene oxide nanoparticles.

[0063] Comparative Example 2

[0064] The difference between this comparative example and Example 1 is that EDCI and HOAT are not added in the preparation of alkylated nanoparticles, and the other steps and raw materials are the same as those in Example 1.

[0065] Application Example 1

[0066] This application example proposes the application of the alkylated graphene oxide nanoparticles prepared in Example 1 as a lubricant additive, comprising: adding 0.02 g of the alkylated graphene oxide nanoparticles prepared in Example 1 to 39.98 g of castor oil, magnetically stirring for 20 minutes, and then heating and ultrasonicating at 60° C. for 30 minutes, with an ultrasonic power of 700 W, to obtain a lubricant with excellent performance.

[0067] The dispersion stability of alkylated graphene oxide nanoparticles and graphene oxide before modification in base oil (castor oil) was tested. Figure 5 As shown, the Figure 5 In the figure, a is a photo of the real object after standing for 1 day, b is a photo of the real object after standing for 60 days, and c is a photo of the real object after standing for 150 days. The base oil in bottle 1 on the left has 0.05% of graphene oxide added by mass, and the base oil in bottle 2 on the right has 0.05% of alkylated graphene oxide added by mass. Figure 5 It can be seen that the alkylated graphene oxide additive still has good stability when added to castor oil and left to stand for 150 days, and the dispersion stability is relatively excellent.

[0068] Comparative Example 3

[0069] This application example proposes: adding 0.02g of graphene oxide nanoparticles to 39.98g of castor oil and subjecting to magnetic stirring for 20 minutes, and then heating and ultrasonicating at 60°C for 30 minutes with an ultrasonic power of 700W to obtain a lubricating oil with excellent performance.

[0070] Comparative Example 4

[0071] This comparative example proposes a pure base oil lubricant, which is prepared by the following steps: 40g of castor oil is subjected to magnetic stirring for 20 minutes, and then heated and ultrasonicated at 60°C for 30 minutes, with the ultrasonic power used being 700W.

[0072] Comparative Example 5

[0073] 0.02 g of the alkylated graphene oxide nanoparticles prepared in Comparative Example 1 was added to 39.98 g of castor oil and magnetically stirred for 20 minutes, followed by heating and ultrasonication at 60° C. for 30 minutes with an ultrasonic power of 700 W to prepare lubricating oil.

[0074] Comparative Example 6

[0075] 0.02 g of the alkylated graphene oxide nanoparticles prepared in Comparative Example 2 was added to 39.98 g of castor oil and magnetically stirred for 20 minutes, followed by heating and ultrasonication at 60° C. for 30 minutes with an ultrasonic power of 700 W to prepare lubricating oil.

[0076] Tribological tests were performed on the base oil of Example 1 with alkylated graphene oxide added, the base oil of Comparative Example 3 with graphene oxide added, the pure base oil of Comparative Example 4, Comparative Example 5 and Comparative Example 6, respectively. The test results are shown in Figure 4 and Table 1 below.

[0077] Table 1 Wear spot diameter and friction coefficient of alkylated graphene oxide, graphene oxide, base oil (castor oil), comparative example 5 and comparative example 6

[0078]

[0079] Combination Figure 4 As shown in Table 1, the friction coefficient of the pure base oil is 0.066, and the friction coefficient after adding graphene oxide to the base oil is 0.056, which is 15.15% lower than the friction coefficient of the pure base oil; the friction coefficient after adding alkylated graphene oxide to the base oil is 0.050, which is 24.24% lower than the friction coefficient of the pure base oil, indicating that the alkylated graphene oxide has excellent tribological properties as a lubricating additive; in addition, the friction coefficients and wear spot diameters of Comparative Examples 5 and 6 are relatively higher than those of Example 1, which indicates that under two different working conditions, microwave-assisted ball milling technology and the addition of two additives are necessary, and better lubricating oil additives can be prepared.

[0080] The present invention adopts a rapid and green method to synthesize alkylated nanoparticles, shortening the ordinary preparation time by more than 10 times, reducing the amount of raw materials used, greatly reducing the friction coefficient, and thus simply and efficiently preparing lubricating additives, saving a large amount of additive costs, and improving economic and durable benefits.

[0081] The specific implementation of the present invention described above does not constitute a limitation on the protection scope of the present invention. Any other corresponding changes and modifications made based on the technical concept of the present invention should be included in the protection scope of the claims of the present invention.

Claims

1. A method for preparing alkylated nanoparticles, characterized in that: The following steps are involved: S1, mixing the nanoparticles with an organic solvent, and then ultrasonically treating the mixture to obtain a first mixed solution; S2, mixing the polyamine and the first mixed solution, heating and stirring to disperse, and then ultrasonically dispersing to obtain a second mixed solution; S3. The second mixed solution is reacted by microwave-assisted ball milling to obtain the alkylated nanoparticles.

2. The method for preparing alkylated nanoparticles according to claim 1, characterized in that: In step S1, the nanoparticles are one or more of graphene oxide, graphene, carbon nanotubes and hexagonal boron nitride; and / or, in step S3, the microwave power in the microwave-assisted ball milling method is 1000-1150W, the ball milling speed is 200rpm-250rpm, and the ball-to-material mass ratio is 2:(1-3).

3. The method for preparing alkylated nanoparticles according to claim 1, characterized in that: In step S2, the polyamine is one or more of tetradecylamine, pentadecylamine, hexadecylamine, heptadecanylamine and octadecylamine; and / or, in step S1, the organic solvent is a mixture of anhydrous ethanol and N-methylpyrrolidone; the mass ratio of the anhydrous ethanol to the N-methylpyrrolidone is 1:(4-4.5); the mass ratio of the nanoparticles to the organic solvent is 1:(250-280).

4. The method for preparing alkylated nanoparticles according to claim 1, characterized in that: In step S1, the ultrasonic treatment time is 10-20 min; and / or, in step S2, the mass ratio of the polyamine to the nanoparticles is (1-3):1, and the temperature of the heating, stirring and dispersing is 90-95°C and the time is 10-20 min.

5. The method for preparing alkylated nanoparticles according to claim 1, characterized in that: Before step S3, the method further includes adding an additive to the second mixed liquid; the additive includes a first sub-additive and / or a second sub-additive; and the mass ratio of the polyamine to the additive is 5:(1-5).

6. The method for preparing alkylated nanoparticles according to claim 5, characterized in that: The first additive is one or more of dicyclohexylcarbodiimide, diisopropylcarbodiimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide; and / or the second additive is one or more of 1-hydroxy-7-azobenzotriazole, 1-hydroxybenzotriazole and 1-hydroxy-1H-1,2,3-triazole-4-carboxylic acid ethyl ester.

7. An alkylated nanoparticle, characterized in that: The invention is prepared by the preparation method according to any one of claims 1 to 6.

8. Use of the alkylated nanoparticles prepared by the preparation method according to any one of claims 1 to 6 or the alkylated nanoparticles according to claim 7 as lubricating oil additives.

9. The use according to claim 8, characterized in that: The alkylated nanoparticles are added to the base oil, and then heated and ultrasonically treated at 55-65° C. to obtain the lubricating oil, wherein the alkylated nanoparticles account for 0.01%-2% of the mass of the base oil.

10. The use according to claim 9, characterized in that: The method also includes adding a dispersant to the base oil before the heating ultrasound, wherein the dispersant is one or more of polyisobutylene bissuccinimide, triethylhexyl phosphoric acid, vinyl bisstearamide, stearic acid monoglyceride, polyethylene glycol and monoalkenyl succinimide; and the dispersant accounts for 1%-5% of the mass of the base oil.

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