CN113460980A - Fluorinated boron nitride nanosheet, high-performance industrial lubricating grease and preparation method thereof - Google Patents

Fluorinated boron nitride nanosheet, high-performance industrial lubricating grease and preparation method thereof Download PDF

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CN113460980A
CN113460980A CN202110879017.9A CN202110879017A CN113460980A CN 113460980 A CN113460980 A CN 113460980A CN 202110879017 A CN202110879017 A CN 202110879017A CN 113460980 A CN113460980 A CN 113460980A
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lubricating grease
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CN113460980B (en
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樊小强
甘超亮
李�浩
孙奇
李文
朱旻昊
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Southwest Jiaotong University
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    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/06Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
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    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy

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Abstract

The invention discloses a fluorinated boron nitride nanosheet and high-performance industrial lubricating grease and a preparation method thereof. The controllable preparation of the F-BNNSs can be realized by controlling the addition amount of the solid acid and the reaction time, and the F-BNNSs with different fluorine contents can be obtained. The prepared F-BNNSs has good compatibility with a lubricating grease dispersing agent, shows more excellent antifriction and antiwear performance than the traditional h-BNNSs, is used for preparing high-performance industrial lubricating grease, and can maintain excellent lubricating performance in various contact forms, external environments and harsh working conditions.

Description

Fluorinated boron nitride nanosheet, high-performance industrial lubricating grease and preparation method thereof
Technical Field
The invention belongs to the field of preparation and application of lubricating materials, and particularly relates to a fluorinated boron nitride nanosheet, high-performance industrial lubricating grease and a preparation method thereof.
Background
The friction and wear problem of moving parts in mechanical equipment causes a large amount of energy waste and part scrap, and in order to improve the energy utilization rate and prolong the service life of equipment, high-performance industrial lubricating grease needs to be researched urgently. Many domestic and foreign documents and patents prove that the nano material has excellent antifriction and antiwear performance as an industrial lubricating grease additive. The hexagonal boron nitride nanosheet (h-BNNSs) has a unique atomic-level two-dimensional lamellar structure, is connected into a six-membered ring by a B-N bond in the layer, has the strength which is comparable to that of graphene, can be well adsorbed on a friction pair interface to form a protective film, prevents the surface of the friction pair from directly contacting, and further reduces friction and wear. However, unlike graphene, in addition to weak van der waals force between h-BNNSs layers, due to the difference in electronegativity between B atoms and N atoms, non-negligible ion attraction exists between adjacent B atoms and N atoms, thereby increasing the shear strength and frictional force between h-BNNSs layers, limiting the lubricating performance thereof. Simulation analysis based on Density Functional Theory (DFT) showed that: by doping foreign atoms (C, H, P, F and the like), the interlayer friction of the h-BNNSs can be obviously reduced, and the tribological performance of the h-BNNSs is improved. Wherein, the F atom has the strongest electronegativity, and the doped F atom can effectively enhance the repulsive force between h-BNNSs layers, thereby playing the role of reducing the polarity and friction between the layers. Thus, fluorinated boron nitride nanosheets (F-BNNSs) have been considered by many researchers as an emerging high performance lubricant.
However, it is very challenging to realize the application of F-BNNSs in industrial lubricating greases. Currently, F-BNNSs are synthesized experimentally by a few research teams, but use fluorinating agents (ammonium fluoride, fluorine)Boric acid, ammonium fluoroborate, etc.) have strong corrosiveness and toxicity, and have great harm to human bodies and the environment. For example, it has been reported that ammonium fluoride (NH) is added in a ball milling process4F) The aqueous solution can be used as a medium to effectively strip h-BN, and simultaneously, the ammonium fluoride can be used as a fluorine source to prepare F-BNNSs. However, ammonium fluoride (NH)4F) Can be decomposed into ammonia (NH) when heated or in water3) The aqueous solution of the fluorine Hydride (HF) is strongly acidic, can corrode glass and metal, is corrosive to human skin, can cause eye, respiratory tract and skin burn when being contacted with the product, and causes dental fluorosis and fluoroostenosis when being contacted for a long time. If such harmful fluorine-containing agents are to be avoided, the fluorine source must be provided by means of expensive ion sputtering equipment, which greatly increases the preparation cost of F-BNNSs and prevents the wide application thereof as a lubricating material in industry. In addition, the prior preparation technology is difficult to realize the controllable preparation of the F-BNNSs, namely, the fluorine content of the F-BNNSs is effectively regulated and controlled by adjusting process parameters. Due to the limitation of the preparation process, the F-BNNSs prepared by the existing method has generally low fluorine content (less than 6 percent), so the lubricating property improving effect is limited. Therefore, the preparation method selects the green, nontoxic and pollution-free fluorinating agent, develops a convenient, controllable and low-cost preparation technology, and has great significance for realizing the practical application of the F-BNNSs in the industrial lubricating grease.
Disclosure of Invention
In view of the key scientific and technical problems mentioned in the background, a first object of the present invention is to provide a process for the controlled preparation of F-BNNSs. The method adopts a green, nontoxic and pollution-free fluorinating agent as a fluorine source, and the F-BNNSs can be prepared by adopting a simple chemical reaction. The fluorine content of the F-BNNSs can be adjusted by changing the dosage of the fluorinating agent and the reaction time, and the fluorinating agent selected by the method has strong reaction activity so as to break through the limit of the inherent chemical inertness of the h-BNNSs and obtain the F-BNNSs with high fluorine content. The method has the advantages of simple preparation, low cost, environmental protection and industrial batch production; it is a second object of the present invention to provide a high performance F-BNNSs lubricity additive. The additive has higher fluorine content, good compatibility with a dispersant, stable dispersion in industrial lubricating grease, and better tribological performance than the conventional h-BNNSs; it is a third object of the present invention to provide a method of using a high performance F-BNNSs lubricity additive. The using method must aim at all industrial lubricating oil and lubricating grease at the same time, the F-BNNSs as an additive must be uniformly dispersed in the lubricating grease, and the preparation method should be simple, easy to operate, time-saving, and not require complex and expensive equipment; the fourth purpose of the invention is to provide a series of high-performance industrial F-BNNSs nanometer lubricating grease. F-BNNSs additive and dispersant with highest fluorine content and optimal lubricating property are added into various industrial basic grease to prepare a series of F-BNNSs nano lubricating grease with excellent performance. The nano lubricating grease can keep excellent lubricating performance under various contact forms, external environments and harsh working conditions, and compared with basic grease, the friction coefficient of the nano lubricating grease is reduced by more than 20%, and the wear rate is reduced by more than 70%.
In order to solve the problems, the technical scheme of the invention is as follows:
the fluorinated boron nitride nanosheet is obtained by a controllable preparation method of the fluorinated boron nitride nanosheet, and the preparation method comprises the following steps:
a1: dispersing a certain amount of hexagonal boron nitride (h-BN) powder into Isopropanol (IPA), sealing the mixture in a micro reaction kettle, heating the mixture to 180 ℃ for reaction for 12 hours, and using magnetic stirring to assist stripping in the reaction process so as to obtain hexagonal boron nitride nanosheets (h-BNNSs) with atomic thickness;
a2: mixing h-BNNSs with an environment-friendly solid acid in a certain proportion, dispersing the mixture into an organic solvent, heating the mixture in a micro reaction kettle to a certain temperature, and reacting for a period of time to obtain fluorinated boron nitride nanosheets (F-BNNSs);
preferably, the solid environmentally friendly acid in step a2 is perfluorosulfonic acid or any concentration of dispersion thereof.
Preferably, the h-BNNSs are mixed with an environmentally friendly solid acid in any ratio in step a 2.
Preferably, the organic solvent in step a2 is a non-flammable organic reagent capable of uniformly dispersing h-BNNSs and perfluorosulfonic acid and generating high pressure at high temperature, including but not limited to N, N-dimethylformamide solvent (DMF).
Preferably, the certain temperature in the step A2 is not lower than 200 ℃, and the certain time is not less than 3 h.
The invention also provides a high-performance F-BNNSs lubricating additive, which is prepared by the preparation method and has better tribological performance than the conventional h-BNNSs. In particular, F-BNNSs (denoted as F-BNNSs) were prepared when h-BNNSs was added at 60mg, the perfluorosulfonic acid dispersion was added at 2.0ml, and the reaction time was 24 hours2.0-24) The fluorine content is the highest and reaches 14.6 percent, and the lubricating oil has the best lubricating performance. At 120N, 150N as base oil, containing 1 wt% of F-BNNSs2.0-24The friction coefficient of the additive lubricating oil is reduced by 32.3% compared with that of the base oil, and the wear rate is reduced by over 91%.
The invention also provides a preparation method of the high-performance industrial lubricating grease, and a method for uniformly dispersing the F-BNNSs additive and the dispersing agent into the industrial lubricating grease. Wherein the addition amount of the F-BNNSs is between 0.1 and 20 percent, and the addition amount of the dispersing agent is between 0.1 and 30 percent. For F-BNNSs nano lubricating oil, ultrasonic dispersion is adopted, and the power is within the range of 100-600W; for F-BNNSs nanometer lubricating grease, a common lubricating grease additive mixing instrument such as a grinding machine is adopted for repeatedly grinding and mixing to ensure that the additive is uniformly dispersed.
The invention also provides a series of high-performance industrial nano lubricating grease, and F-BNNSs with optimal lubricating performance is selected2.0-24And proper dispersant is added to various industrial basic greases to prepare a series of F-BNNSs nano lubricating greases with excellent performance. The nano lubricating grease can keep excellent lubricating performance under various contact forms, external environments and harsh working conditions, and compared with basic grease, the friction coefficient of the nano lubricating grease can be reduced by more than 20%, and the wear rate can be reduced by more than 70%.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages and positive effects: hair brushThe invention provides a controllable preparation method of fluorinated boron nitride nanosheets (F-BNNSs), which is characterized in that green, nontoxic and pollution-free perfluorosulfonic acid is used as a fluorine source, and the F-BNNSs can be prepared by one-step solvothermal reaction. The method successfully realizes the controllable regulation (4.09-14.6%) of the F-BNNSs fluorine content by changing the consumption of the perfluorosulfonic acid and the reaction time, the perfluorosulfonic acid selected by the method has strong reaction activity, and can break through the limit of the inherent chemical inertness of h-BNNSs to obtain the F-BNNSs (F-BNNSs) with high fluorine content2.0-24Fluorine content 14.6%). The method is simple in preparation, low in cost, green and environment-friendly, and can be used for industrial mass production. The invention also provides a high-performance lubricating additive (F-BNNSs)2.0-24) The additive has high fluorine content, is well compatible with a dispersant, can be stably dispersed in industrial lubricating grease, and has more excellent tribological properties than the conventional h-BNNSs. The invention also provides a series of high-performance industrial nano lubricating grease, which is prepared from the F-BNNSs with optimal lubricating performance2.0-24The additive and the dispersant are added into various industrial basic greases to prepare a series of nano lubricating greases with excellent performance. The nano lubricating grease can keep excellent lubricating performance under various contact forms, external environments and severe working conditions. In particular, 150N as base oil, at 120N, contains 1 wt.% F-BNNSs2.0-24The friction coefficient of the additive lubricating oil is reduced by 32.3% compared with that of the base oil, and the wear rate is reduced by over 91%.
Drawings
FIG. 1 is an X-ray photoelectron spectrum of F-BNNSs, abbreviated as F-BNNSsx-yIn the figure, x represents the amount of perfluorosulfonic acid dispersion (example concentration in the figure is 5%) in milliliters (ml) in the case of a fixed mass of h-BNNSs (example concentration in the figure is 60mg), and y represents the solvothermal reaction time in hours (h). The X-ray photoelectron spectrum result of the F-BNNSs proves that: the F-BNNSs fluorine content can be effectively regulated and controlled by controlling the experimental conditions (the addition amount of the perfluorosulfonic acid dispersion liquid and the reaction time) in the method;
FIG. 2 shows the average friction coefficient and wear rate of 150N base oil, F-BNNSs nano-lubricating oil, base oil, dispersant and lubricant at 60Nh-BNNSs served as a control. Experiments show that the antifriction and antiwear performance of the F-BNNSs is more excellent than that of base oil, a dispersing agent and h-BNNSs, the lubricating performance of the F-BNNSs is more excellent along with the increase of the fluorine content, and particularly, when the fluorine content is the highest, the F-BNNSs2.0-24Exhibits optimal tribological properties;
FIG. 3 is a graph showing that F-BNNSs is 120N, 150N base oil2.0-24Average coefficient of friction and wear rate of (c) with base oil and h-BNNSs as controls. The results show that F-BNNSs are comparable to the comparative base oils2.0-24The friction coefficient is reduced by 32.3%, and the wear rate is reduced by over 91%;
Detailed Description
The fluorinated boron nitride nanosheet and the high-performance industrial lubricating grease and the preparation method thereof provided by the invention are further described in detail with reference to the accompanying drawings and specific examples. Advantages and features of the present invention will become apparent from the following description and from the claims.
It should be noted that although the hexagonal boron nitride nanosheet (h-BNNSs) has a unique atomic-scale two-dimensional lamellar structure and has a strength comparable to that of graphene, besides weak van der waals force between h-BNNSs layers, non-negligible ions of B atoms and N atoms between adjacent layers attract each other, so that the shear strength and friction force between h-BNNSs layers are increased, and the lubricating performance of the h-BNNSs layers is limited. Simulation analysis based on Density Functional Theory (DFT) showed that: by doping foreign atoms (C, H, P, F and the like), the interlayer friction of the h-BNNSs can be obviously reduced, and the tribological performance of the h-BNNSs is improved. Wherein, the F atom has the strongest electronegativity, and the doped F atom can effectively enhance the repulsive force between h-BNNSs layers, thereby playing the role of reducing the polarity and friction between the layers. However, it is very challenging to realize the application of F-BNNSs in industrial lubricating greases. At present, although a few research teams synthesize F-BNNSs through experimental means, all the used fluorinating agents (ammonium fluoride, fluoroboric acid, ammonium fluoroborate and the like) have strong corrosivity and toxicity and have great harm to human bodies and environment. For example, it has been reported that ammonium fluoride (NH) is added in a ball milling process4F) The aqueous solution can be used as a medium to effectively strip h-BN, and simultaneously, the ammonium fluoride can be used as a fluorine source to prepare F-BNNSs.However, ammonium fluoride (NH)4F) Can be decomposed into ammonia (NH) when heated or in water3) The aqueous solution of the fluorine Hydride (HF) is strongly acidic, can corrode glass and metal, is corrosive to human skin, can cause eye, respiratory tract and skin burn when being contacted with the product, and causes dental fluorosis and fluoroostenosis when being contacted for a long time. If such harmful fluorine-containing agents are to be avoided, the fluorine source must be provided by means of expensive ion sputtering equipment, which greatly increases the preparation cost of F-BNNSs and prevents the wide application thereof as a lubricating material in industry. In addition, the prior preparation technology is difficult to realize the controllable preparation of the F-BNNSs, namely, the fluorine content of the F-BNNSs is effectively regulated and controlled by adjusting process parameters. Due to the limitation of the preparation process, the F-BNNSs prepared by the existing method has generally low fluorine content (less than 6 percent), so the lubricating property improving effect is limited.
The inventor finds that the F-BNNSs can be prepared by selecting green, nontoxic and pollution-free perfluorosulfonic acid as a fluorinating agent and carrying out one-step solvothermal reaction, and the controllable preparation of the F-BNNSs can be realized by changing the addition amount and the reaction time of the perfluorosulfonic acid, so that the F-BNNSs with different fluorine contents can be obtained. The prepared F-BNNSs has good compatibility with a lubricating grease dispersant, and shows more excellent antifriction and antiwear performance than the traditional h-BNNSs. In addition, the perfluorinated sulfonic acid fluorinating agent selected by the method has strong reaction activity, and can break through the limit of the inherent chemical inertness of h-BNNSs to obtain F-BNNSs with high fluorine content. In particular, when the h-BNNSs is added in an amount of 60mg, the perfluorosulfonic acid dispersion (5%) is added in an amount of 2.0ml, and the reaction time is 24 h. The obtained additive is named as F-BNNSs2.0-24The fluorine content is the highest and reaches 14.6%, and the lubricating oil has the best lubricating performance. At 120N, 150N as base oil, containing 1 wt% of F-BNNSs2.0-24The friction coefficient of the lubricating oil of the additive is reduced by 32.3 percent compared with that of base oil, the wear rate is reduced by over 91 percent, and the lubricating oil is expected to replace the traditional h-BNNSs to become a new generation of high-performance industrial lubricating grease additive.
In view of the above, the preparation method of the fluorinated boron nitride nanosheet and the high-performance industrial lubricating grease comprises the following steps:
a1: dispersing a certain amount of hexagonal boron nitride (h-BN) powder into Isopropanol (IPA), sealing the mixture in a micro reaction kettle, heating the mixture to 180 ℃ for reaction for 12 hours, and using magnetic stirring to assist stripping in the reaction process so as to obtain hexagonal boron nitride nanosheets (h-BNNSs) with atomic thickness;
a2: mixing h-BNNSs with an environment-friendly solid acid in a certain proportion, dispersing the mixture into an organic solvent, heating the mixture in a micro reaction kettle to a certain temperature, and reacting for a period of time to obtain fluorinated boron nitride nanosheets (F-BNNSs);
in a preferred embodiment of the present invention, the solid acid in step A2 is a perfluorosulfonic acid dispersion with a solid content of 5 wt%.
In a preferred embodiment of the present invention, the h-BNNSs and the solid environment-friendly acid are mixed in the step a2 according to a ratio of: on the premise that the dosage of the fixed h-BNNSs is 60mg, the dosage of the perfluorosulfonic acid dispersion liquid is 0.5-2.0 ml.
In a preferred embodiment of the present invention, the organic solvent in step a2 is N, N-Dimethylformamide (DMF).
In a preferred embodiment of the present invention, the temperature in the step A2 is 200-220 ℃, and the time is 12-24 hours.
The fluorinated boron nitride nanosheet prepared by the invention is used as a high-performance F-BNNSs2.0-24A lubricious additive.
The invention also provides a preparation method of the high-performance industrial lubricating grease, namely a method for uniformly mixing the F-BNNSs additive and the dispersing agent into the industrial lubricating grease. The addition amount of F-BNNSs is 0.5-3%, and the addition amount of the dispersing agent is 1-10%. Wherein, for the F-BNNSs nanometer lubricating oil, ultrasonic dispersion is adopted, and the power is within the range of 100-600W; for F-BNNSs nano grease, a grinding machine is adopted for repeated grinding and mixing to ensure that the additive is uniformly dispersed.
The invention also provides a series of high-performance industrial nano lubricating grease, and F-BNNSs with optimal lubricating performance is selected2.0-24And proper dispersant is added to various industrial basic greases to prepare a series of F-BNNSs nano lubricating greases with excellent performance. The nano lubricating grease can be applied to various contact shapesExcellent lubricating performance is kept under the conditions of formula, external environment and harsh working conditions.
FIG. 1 is an X-ray photoelectron spectrum of F-BNNSs, abbreviated as F-BNNSsx-yIn the figure, x represents the amount of perfluorosulfonic acid dispersion (example concentration in the figure is 5%) in milliliters (ml) in the case of a fixed mass of h-BNNSs (example concentration in the figure is 60mg), and y represents the solvothermal reaction time in hours (h). The X-ray photoelectron spectrum result of the F-BNNSs proves that: the F-BNNSs fluorine content can be effectively regulated and controlled by controlling the experimental conditions (the addition amount of the perfluorosulfonic acid dispersion liquid and the reaction time) in the method;
example 1
Dispersing 60mg of h-BNNSs and 0.5ml of perfluorosulfonic acid (solid content is 5%) into 30ml of DMF, heating to 200 ℃ in a micro reaction kettle, and reacting for 12h to obtain the fluorinated boron nitride nanosheet named as F-BNNSs0.5-12
Example 2
Dispersing 60mg of h-BNNSs and 0.5ml of perfluorosulfonic acid (solid content is 5%) into 30ml of DMF, heating to 200 ℃ in a micro reaction kettle, and reacting for 24h to obtain the fluorinated boron nitride nanosheet named as F-BNNSs0.5-24
Example 3
Dispersing 60mg of h-BNNSs and 1.0ml of perfluorosulfonic acid (solid content is 5%) into 30ml of DMF, heating to 200 ℃ in a micro reaction kettle, and reacting for 12h to obtain the fluorinated boron nitride nanosheet named as F-BNNSs1.0-12
Example 4
Dispersing 60mg of h-BNNSs and 1.0ml of perfluorosulfonic acid (solid content is 5%) into 30ml of DMF, heating to 200 ℃ in a micro reaction kettle, and reacting for 24h to obtain fluorinated boron nitride nanosheets named F-BNNSs1.0-24
Example 5
Dispersing 60mg of h-BNNSs and 2.0ml of perfluorosulfonic acid (solid content is 5%) into 30ml of DMF, heating to 200 ℃ in a micro reaction kettle, and reacting for 12h to obtain the fluorinated boron nitride nanosheet named as F-BNNSs2.0-12
Example 6
Dispersing 60mg of h-BNNSs and 2.0ml of perfluorosulfonic acid (solid content is 5%) into 30ml of DMF, heating to 200 ℃ in a micro reaction kettle, and reacting for 24h to obtain the fluorinated boron nitride nanosheet named as F-BNNSs2.0-24
Description of the drawings: the concentration of the perfluorosulfonic acid dispersion can be any concentration, the reaction temperature is higher than 200 ℃, the reaction time is longer than 3 hours, the parameters mentioned in the above examples are only used as preferable references, and do not represent all the examples.
The F-BNNSs lubricant additive (1 wt%) prepared in examples 1-6 and polyisobutylene succinimide dispersant (1 wt%) were added into industrial lubricating oil (150N), and subjected to ultrasonic dispersion at 300W for 30 minutes to prepare F-BNNSs nano lubricating oil. FIG. 2 shows the average friction coefficient and wear rate of F-BNNSs under 60N, and compared with base oil, dispersant and h-BNNSs, experiments show that the average friction coefficient and wear rate of F-BNNSs are lower than those of base oil, dispersant and h-BNNSs, and the antifriction property of F-BNNSs is more and more excellent with the increase of fluorine content, particularly, the F-BNNSs with the highest fluorine content2.0-24Exhibit optimal tribological properties. The friction test results fully illustrate the advantage of F-BNNSs as a lubricious additive.
F-BNNSs prepared in example 62.0-24Adding a lubricating additive (1 wt%) and a polyisobutylene succinimide dispersant (1 wt%) into industrial lubricating oil (150N), and performing 300W ultrasonic dispersion for 30 minutes to obtain F-BNNSs2.0-24Nanometer lubricating oil. FIG. 3 is F-BNNSs at 120N2.0-24Average coefficient of friction and wear rate of (d) were compared with base oil and h-BNNSs. The results show that F-BNNSs2.0-24Has more excellent tribological properties than base oil and h-BNNSs, and F-BNNSs than base oil2.0-24The friction coefficient is reduced by 32.3%, and the wear rate is reduced by more than 91%. This indicates that the performance advantage of the F-BNNSs additive is more pronounced than that of conventional h-BNNSs at high loads.
In conclusion, the fluorinated boron nitride nanosheet, the high-performance industrial lubricating grease and the preparation method thereof are environment-friendly, simple in process and controllable in fluorine content. The prepared F-BNNSs has good compatibility with a lubricating grease dispersant, and shows more excellent antifriction and antiwear performance than the traditional h-BNNSs. Under certain experimental conditions, F-BNNSs with high fluorine content can be prepared, so that excellent lubricating performance is obtained, and the F-BNNSs is expected to replace the traditional h-BNNSs and become a new generation of high-performance industrial lubricating grease additive.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments. Even if various changes are made to the present invention, it is still within the scope of the present invention if they fall within the scope of the claims of the present invention and their equivalents.

Claims (10)

1. The preparation method of the fluorinated boron nitride nanosheet is characterized by comprising the following steps:
a1: dispersing a certain amount of hexagonal boron nitride h-BN powder into isopropanol IPA, sealing the mixture in a micro reaction kettle, heating the mixture to 180 ℃ for reaction for 12 hours, and carrying out magnetic stirring assisted stripping in the reaction process to obtain hexagonal boron nitride nanosheets h-BNNSs with atomic thickness;
a2: mixing h-BNNSs with environment-friendly solid acid in a certain proportion, dispersing the mixture into an organic solvent, heating the mixture in a micro reaction kettle to a certain temperature, and reacting for a period of time to obtain the fluorinated boron nitride nanosheet F-BNNSs.
2. A method of making fluorinated boron nitride nanoplates as in claim 1, wherein the environmentally friendly solid acid in step a2 is perfluorosulfonic acid or a dispersion thereof at any concentration.
3. A method of producing fluorinated boron nitride nanoplates as in claim 1, wherein the organic solvent in step a2 is N, N-dimethylformamide solvent DMF.
4. A method for preparing fluorinated boron nitride nanosheets according to claim 1, wherein the temperature in step a2 is not lower than 200 ℃ for a period of time not less than 3 hours.
5. Fluorinated boron nitride nanoplates, characterised in that they are obtainable by the preparation process according to any one of claims 1 to 4.
6. Use of fluorinated boron nitride nanoplates according to claim 5 as an industrial lubricating grease additive.
7. The preparation method of the high-performance industrial lubricating grease is characterized by comprising the following steps:
s1: adding a proper amount of the fluorinated boron nitride nanosheet F-BNNSs and a dispersing agent of claim 5 into industrial lubricating grease, and completely dispersing to obtain F-BNNSs nano lubricating grease;
s2: the prepared F-BNNSs nano lubricating grease can be directly applied to various contact forms, external environments and working conditions under the condition of good dispersion, and if layering occurs, the step S1 is repeated to uniformly mix the additive and the industrial lubricating grease again;
adding F-BNNSs and a dispersing agent into the industrial lubricating grease, wherein the adding amount of the F-BNNSs is between 0.1 and 20 percent, and the adding amount of the dispersing agent is between 0.1 and 30 percent.
8. The method for preparing high-performance industrial lubricating grease as claimed in claim 7, wherein the dispersant in the step S1 is polyisobutylene succinimide; the industrial lubricating grease is one or a mixture of more of vegetable oil, mineral oil, synthetic oil, mineral oil lubricating grease and synthetic oil lubricating grease.
9. The method for preparing high performance industrial lubricating grease as claimed in claim 7, wherein the step of S1 is to fully disperse the lubricating grease, wherein, for F-BNNSs nanometer lubricating grease, ultrasonic dispersion is adopted, and the power is within the range of 100-600W; for F-BNNSs nanometer lubricating grease, a lubricating grease additive mixing instrument is adopted for repeatedly grinding and mixing to ensure that the additive is uniformly dispersed.
10. A high-performance industrial lubricating grease characterized by being obtained by the production method as claimed in any one of claims 7 to 9.
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