阅读说明：本技术 纳米二硫化钼/黑磷纳米片复合润滑油添加剂的制备方法 (Preparation method of nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive ) 是由 王伟 董少文 侯婷丽 高原 王庆娟 王快社 于 2020-04-30 设计创作，主要内容包括：本发明公开了一种纳米二硫化钼/黑磷纳米片复合润滑油添加剂的制备方法,采用液相剥离法制备黑磷纳米片,将黑磷粉体均匀分散到N-甲基吡咯烷酮溶剂中,超声,取上清液离心,重复几次离心,将离心出来的黑磷纳米片洗涤,干燥；将黑磷纳米片分散到具有钼酸铵和硫化钠的反应液中,超声均匀后通过溶剂热法可得到纳米二硫化钼/黑磷纳米片复合润滑油添加剂。该复合润滑油添加剂的制备原料易得、方法简便,能有效的提高在摩擦过程中减摩润滑性能,能够应用于机械运转,机械设备油润滑等领域。(The invention discloses a preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive, which comprises the steps of preparing a black phosphorus nanosheet by adopting a liquid phase stripping method, uniformly dispersing black phosphorus powder into an N-methyl pyrrolidone solvent, carrying out ultrasonic treatment, centrifuging supernatant, repeating the centrifugation for several times, washing the centrifuged black phosphorus nanosheet, and drying; dispersing the black phosphorus nanosheets into a reaction solution containing ammonium molybdate and sodium sulfide, and obtaining the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive through a solvothermal method after ultrasonic homogenization. The composite lubricating oil additive has the advantages of easily obtained preparation raw materials and simple and convenient method, can effectively improve the antifriction lubricating property in the friction process, and can be applied to the fields of mechanical operation, oil lubrication of mechanical equipment and the like.)

1. A preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite material is characterized by comprising the following steps: the preparation method comprises the following steps:

(1) preparation of black phosphorus nanosheet

Putting the black phosphorus powder into an N-methyl pyrrolidone solvent, performing ultrasonic treatment in a cold water bath for multiple times, centrifuging, and drying in a vacuum environment to obtain black phosphorus nanosheets;

(2) preparation of precursor solution

Dispersing ammonium molybdate and sodium sulfide in water to obtain a reaction solution, adding the black phosphorus nanosheet into the reaction solution, and performing ultrasonic treatment to obtain a precursor solution;

(3) preparation of composite materials

And adding a reducing agent into the precursor solution, carrying out solvothermal reaction, centrifuging after the reaction is finished, taking the precipitate, and drying to obtain the nano molybdenum disulfide/black phosphorus nanosheet composite material.

2. The preparation method of the nano molybdenum disulfide/black phosphorus nanosheet composite material as claimed in claim 1, wherein in step (1), 5-10 parts of black phosphorus powder are placed in 20000-plus 30000 parts of N-methylpyrrolidone solvent, ultrasonic treatment is carried out in a cold water bath for 8-10h, centrifugation is carried out for 20-30min at the rotating speed of 3000-plus 5000rpm after ultrasonic treatment, the supernatant is taken to be centrifuged for 20-30min at the rotating speed of 7000-plus 9000rpm, finally the supernatant is taken to be centrifuged for 20-30min at the rotating speed of 10000-plus 12000rpm, precipitates are taken, and drying is carried out at 40-60 ℃ in a vacuum environment to obtain the black phosphorus nanosheets.

3. The preparation method of the nano molybdenum disulfide/black phosphorus nanosheet composite material as claimed in claim 1, wherein in step (2), 5-8 parts of ammonium molybdate and 5-8 parts of sodium sulfide are dispersed in 1000-2000 parts of deionized water to obtain a reaction solution, 3-5 parts of black phosphorus nanosheet is added into the reaction solution, and a precursor solution is obtained after ultrasonic treatment for 0.5-1 h.

4. The method for preparing the nano molybdenum disulfide/black phosphorus nanosheet composite material as claimed in claim 1, wherein in step (3), the precursor solution is poured into a reaction kettle, 300 parts of hydrazine hydrate solution is added into the reaction kettle in an amount of 100-.

5. A preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive is characterized by comprising the following steps: the preparation method comprises the following steps:

(1) preparation of nano molybdenum disulfide/black phosphorus nanosheet composite according to the method of claim 1

(2) Preparation of composite lubricating oil additive

And dispersing the nano molybdenum disulfide/black phosphorus nanosheet composite material into base oil to obtain the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive.

6. The nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive prepared according to the preparation method of claim 5, which is characterized in that: the nano molybdenum disulfide structure is a layered structure with the size of 200-400nm and the number of layers of 1-3; the size of the black phosphorus nano-sheet structure is 300-500nm, and the number of layers is 3-5.

Technical Field

The invention relates to a preparation method of a nano composite lubricating oil additive, in particular to a preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive.

Background

With the continuous progress of industrial technology, the working environment of various mechanical equipment and parts thereof becomes more complex and severe, and the traditional mineral-based lubricating oil is far from sufficient. In order to reduce friction and wear, various friction-reducing lubricant additives are widely used in extreme pressure additives for lubricating oils. The formation of an effective lubricating film through tribochemical reactions during the rubbing process is the key to the ability of the friction pair surface to resist gluing. Due to the importance of lubrication and the limited availability of existing lubrication methods, the development of lubricant additives with good performance is critical to achieving high reliability and long service life of mechanical equipment.

Molybdenum disulfide as an important transition group metal sulfide has the characteristic of a hexagonal system layered structure, and is bonded in a molecular layer through a strong chemical bond and bonded between layers through weak van der waals force, so that interlayer slippage can occur under low shear stress, and the molybdenum disulfide is widely used in the field of lubrication. Therefore, the molybdenum disulfide lubricating additive plays an important role in reducing friction and remarkably improving the anti-loading performance and performance.

In recent years, Black Phosphorus (BP), a novel two-dimensional material, has received much attention from researchers at home and abroad due to its special two-dimensional structure and thermodynamic stability. At present, the application of the nano molybdenum disulfide/black phosphorus nanosheet composite material in the field of lubricating additives does not exist.

Disclosure of Invention

The invention provides a preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive, which overcomes the defects of the existing traditional lubricating oil additive.

The technical scheme of the invention is as follows:

the invention provides a preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite material, which is prepared according to the following method, and comprises the following specific steps:

(1) preparation of black phosphorus nanosheet

Placing 5-10 parts of black phosphorus powder in 20000-plus 30000 parts of N-methylpyrrolidone solvent, carrying out ultrasonic treatment in a cold water bath for 8-10h, centrifuging at the rotating speed of 3000-plus 5000rpm for 20-30min after ultrasonic treatment, taking the supernatant, centrifuging at the rotating speed of 7000-plus 9000rpm for 20-30min, finally taking the supernatant, centrifuging at the rotating speed of 10000-plus 12000rpm for 20-30min, taking the precipitate, and drying at 40-60 ℃ in a vacuum environment to obtain black phosphorus nanosheets;

(2) preparation of precursor solution

Dispersing 5-8 parts of ammonium molybdate and 5-8 parts of sodium sulfide in 1000-2000 parts of deionized water to obtain a reaction solution, adding 3-5 parts of black phosphorus nanosheet into the reaction solution, and performing ultrasonic treatment for 0.5-1h to obtain a precursor solution.

(3) Preparation of composite materials

Pouring the precursor solution into a reaction kettle, adding 300 parts of 100-plus-one hydrazine hydrate solution into the reaction kettle, carrying out solvothermal reaction for 18-20h at the reaction temperature of 180-plus-one 210 ℃, after the reaction is finished and the sample is naturally cooled, centrifuging for 5-10min at the rotation speed of 10000-plus-one 12000rpm, taking the precipitate, drying at the temperature of 40-60 ℃ in a vacuum environment to obtain the nano molybdenum disulfide-black phosphorus alkene composite material,

the invention also provides a preparation method of the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive, which is prepared according to the following method, and the preparation method comprises the following specific steps:

(1) preparation of black phosphorus nanosheet

Placing 5-10 parts of black phosphorus powder in 20000-plus 30000 parts of N-methylpyrrolidone solvent, performing ultrasonic treatment in a cold water bath for 8-10h, centrifuging at the rotating speed of 3000-plus 5000rpm for 20-30min after ultrasonic treatment, taking the supernatant, centrifuging at the rotating speed of 7000-plus 9000rpm for 20-30min, finally taking the supernatant, centrifuging at the rotating speed of 10000-plus 12000rpm for 20-30min, taking the precipitate, and drying at 40-60 ℃ in a vacuum environment to obtain black phosphorus nanosheets;

(2) preparation of precursor solution

Dispersing 5-8 parts of ammonium molybdate and 5-8 parts of sodium sulfide in 1000-2000 parts of deionized water to obtain a reaction solution, adding 3-5 parts of black phosphorus nanosheet into the reaction solution, and performing ultrasonic treatment for 0.5-1h to obtain a precursor solution.

(3) Preparation of nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive

Pouring the precursor solution into a reaction kettle, adding 300 parts of 100-plus-material hydrazine hydrate solution into the reaction kettle, carrying out solvothermal reaction for 18-20h at the reaction temperature of 180-plus-material 210 ℃, after the reaction is finished and the sample is naturally cooled, centrifuging for 5-10min at the rotation speed of 10000-plus-material 12000rpm, taking the precipitate, drying at the temperature of 40-60 ℃ in a vacuum environment to obtain the nano molybdenum disulfide-black phosphorus alkene composite material, and dispersing the nano molybdenum disulfide-black phosphorus alkene composite material into base oil to obtain the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive.

Finally, the invention also discloses a composite lubricant additive prepared according to the method, wherein the nano molybdenum disulfide structure is a layered structure with the size of 200-400nm and the number of layers of 1-3; the size of the black phosphorus nanosheet structure is 30-500nm, and the number of layers is 3-5.

Compared with the prior art, the invention has the advantages that:

by adopting a solvothermal method, due to Van der Waals force between the molybdenum disulfide and the black phosphorus and full contact of reactants, the generated molybdenum disulfide is easier to load on the black phosphorus nanosheet, and the molybdenum disulfide and the black phosphorus can play a role in synergistic lubrication on a friction interface more efficiently, so that the antifriction lubrication performance under a high-load environment is ensured.

The black phosphorus is prepared by adopting a liquid phase stripping method, so that the black phosphorus is stripped in an N-methyl pyrrolidone solvent, the black phosphorus nanosheet is prevented from being oxidized, and the performance of the black phosphorus nanosheet is not influenced.

Drawings

FIG. 1(a) is a transmission electron microscope image of nano molybdenum disulfide prepared by the method of the present invention;

FIG. 1(b) is a transmission electron microscope image of nano molybdenum disulfide prepared by the method of the present invention;

FIG. 2(a) is a transmission electron microscope image of a black phosphorus nanosheet prepared by the method of the present invention;

FIG. 2(b) is a transmission electron microscope image of a black phosphorus nanosheet prepared by the method of the present invention;

fig. 3 is a friction coefficient diagram of the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive prepared in example 1 under different loads.

Detailed Description

The inventor of the application finds that the combination of the nano molybdenum disulfide and the black phosphorus nanosheet is not ideal enough in the process of research, and finally researches a hydrothermal method through multi-aspect research, which is different from the traditional hydrothermal method, so that the nano molybdenum disulfide and the black phosphorus nanosheet are combined in a hydrothermal reaction kettle under high pressure and high temperature, the intermolecular force can be overcome, and the performances of the nano molybdenum disulfide and the black phosphorus nanosheet are not influenced.

The present invention will be described in further detail with reference to the accompanying drawings and examples.