Ternary two-dimensional material FePS3 lubricating oil additive and method for preparing additive and lubricating oil

Abstract

The invention belongs to the technical field of lubricants, and particularly relates to a ternary two-dimensional material FePS3 lubricating oil additive and a method for preparing the additive and lubricating oil. The ternary two-dimensional crystal material ferrophosphorus trisulfide with the chemical formula of FePS3 is prepared, then simple grinding, ultrasonic treatment, filtering and drying are performed to prepare powder, the powder is added into common lubricating base oil, the friction coefficient and the abrasion volume can be obviously reduced, and compared with other structured two-dimensional materials, the technology is relatively simple, cost is reduced, and the application range is wide. The lubricating oil prepared by the method can be produced in a large scale with high purity, has good antifriction and anti-wear properties, has strong dispersibility in base oil, and can reduce the friction coefficient of the lubricating base oil by 40% and the wear by more than 30% by adding a very small amount of the lubricating oil.

Description

Technical Field

[0001] The present invention belongs to the technical field of lubricants, and particularly relates to a ternary two-dimensional material FePS3 lubricating oil additive and methods for preparing the additive and lubricating oil. Background Art

[0002] Friction is a common phenomenon in daily life and industrial production. Approximately one-third of the world's primary energy is consumed in the process of friction in different forms. Wear caused by friction is one of the main reasons for mechanical equipment failures. As an effective means to solve friction, wear, and lubrication problems, lubricating oil plays an important role in various industries, especially in the automotive and transportation fields. It is regarded as a "key resource" to ensure the normal operation of various transportation vehicles and equipment, extend the service life of components, and improve energy efficiency.

[0003] The role of lubricating oil in the automotive industry is crucial. By reducing friction and protecting key components, lubricating oil helps improve engine performance, extend its service life, and maintain efficient operation while reducing wear. To enhance the lubrication effect of lubricating oil and make up for its deficiencies, lubricating oil additives are usually added to lubricating oil. These additives can significantly improve the comprehensive performance of base oil, and a small amount of addition can produce a large improvement.

[0004] Lubricating oil additives can be divided into three categories: organic, inorganic, and organic-inorganic composite. These three types of additives can all improve the friction reduction and anti-wear performance of lubricating oil, but their effects and applicable scenarios are different. Organic lubricating oil additives usually have higher costs and poor stability, and it is difficult to meet the requirements of long-term use or complex working conditions; inorganic lubricating oil additives have poor solubility, and their friction reduction and anti-wear effects are not as obvious as those of organic additives. Therefore, exploring new lubricating oil additives has become an important way to improve the performance of lubricating oil.

[0005] In recent years, due to their unique structures and excellent physical and chemical properties, two-dimensional materials have shown excellent friction reduction and anti-wear potential in the fields of lubricating materials and lubricating oil additives, and have shown significant advantages in extending the mechanical life, becoming star materials in the research of solid lubricants and lubricating oil additives. Two-dimensional materials can maintain long-term stability in lubricating oil. Experiments and practical applications show that a small amount of two-dimensional material additives can reduce the friction coefficient by more than 30%, and at the same time significantly improve the wear resistance, thereby greatly improving the overall performance and service life of the equipment. For example, when Yanbao Guo et al. used polyalphaolefin 2 (PAO2) as the base oil and added multi-layer graphene as an additive, the tribological properties of the lubricating oil were tested by a four-ball friction tester. The results showed that after adding 0.05 wt% of graphene, PAO2 exhibited the best friction reduction and anti-wear performance, with the friction coefficient reduced by 78% and the wear scar diameter significantly reduced.

[0006] However, the current application of two-dimensional materials in lubricant additives still faces some problems. For example, graphene is prone to agglomeration in lubricating oils; molybdenum disulfide (MoS2) is prone to moisture absorption and failure, which limits their wide application as lubricant additives. In addition, the preparation process of some structured two-dimensional materials is relatively complex, and there is an urgent need to develop new two-dimensional materials to further promote the development of lubricant additive technology. Summary of the Invention

[0007] The present invention discloses a ternary two-dimensional material FePS3 lubricant additive and methods for preparing the additive and lubricating oil. By preparing a ternary two-dimensional crystal material - iron phosphosulfide, with the chemical formula FePS3, and then through simple grinding, ultrasonic treatment, filtration, and drying to form a powder, adding it to common lubricating base oils can significantly reduce the friction coefficient and wear volume. Compared with other structured two-dimensional materials, not only is the process relatively simple, the cost is reduced, high-purity and large-batch production can be carried out, but also it has good friction-reducing and anti-wear properties, has strong dispersibility in base oils, and adding a very small amount can reduce the friction coefficient of the lubricating base oil by 40% and the wear by more than 30%.

[0008] To achieve the above object, the technical solution of the present invention is:

[0009] Ternary two-dimensional material FePS3 lubricant additive, wherein the additive is a nanosheet of iron phosphosulfide, with the chemical formula FePS3.

[0010] Preparation method of ternary two-dimensional material FePS3 lubricant additive, wherein the nanosheet of iron phosphosulfide is prepared from a single crystal of iron phosphosulfide, and the size of the single crystal of iron phosphosulfide is 5×5×0.3 mm to 12×5×0.3 mm, obtained by chemical vapor transport method.

[0011] Preferably, the nanosheet of iron phosphosulfide is obtained by liquid-phase ultrasonic exfoliation method, including the following steps:

[0012] (1) Prepare a single crystal of iron phosphosulfide by chemical vapor transport method, and then grind it with a mortar to obtain iron phosphosulfide powder;

[0013] (2) After mixing the iron phosphosulfide powder with a polar organic solvent, use a probe ultrasonic crusher for ultrasonic exfoliation treatment, then use a high-speed stirrer for high-speed stirring, and then place the obtained mixed solution in a centrifuge to filter and separate the sediment, and perform drying treatment to obtain iron phosphosulfide nanosheets.

[0014] Preferably, in the step (1), grinding is performed with a mortar for 2 - 30 min.

[0015] Preferably, in the step (1), the average particle size of the iron phosphide trisulfide powder is 5 - 30 μm, and the average thickness is 500 - 2000 nm.

[0016] Preferably, in the step (2), the polar organic solvent is one or a mixture of several of anhydrous ethanol, acetone, NMP, and DMF.

[0017] Preferably, in the step (2), in the ultrasonic exfoliation treatment: the ultrasonic power is 200 - 600 W, and the time is 10 - 200 min; when high-speed stirring, the rotation speed of the stirrer is 100 - 2000 r / min; when centrifuging: the rotation speed is 100 - 5000 r / min, and the centrifugation time is 10 - 60 min; the drying temperature range is 40 - 100 °C.

[0018] Preferably, in the step (2), the average particle size of the prepared iron phosphide trisulfide nanosheets is 20 - 100 nm, and the average thickness is 1 - 5 nm.

[0019] A preparation method of a lubricating oil containing a ternary two-dimensional material FePS3 lubricating oil additive includes the following steps: Select 10 - 500 mg of iron phosphide trisulfide nanosheets, add them to 9.5 - 9.99 g of base oil to obtain a new lubricating oil with a mass fraction of 0.1% - 5%, and perform sufficient ultrasonic mixing using a probe ultrasonic, with an ultrasonic power of 200 - 1200 W and a mixing time of 10 - 60 min.

[0020] Preferably, in the preparation method of the lubricating oil, the base oil is one or a mixture of several of polyethylene glycols with different molecular weights, polyalphaolefins, or hexadecane.

[0021] The beneficial effects of the ternary two-dimensional material FePS3 lubricating oil additive and the methods for preparing the additive and the lubricating oil of the present invention are as follows:

[0022] The lubricating oil additive material used in the present invention is a ternary two-dimensional material with a low interlayer shear force, and interlayer sliding is relatively easy; the two-dimensional nanoparticles can fill the pits on the surface of the friction pair to form a smoother surface, thereby reducing wear. Therefore, adding the nanosheets to the lubricating base oil can improve the friction reduction and anti-wear performance of the lubricating base oil. In addition, the lubricating oil additive prepared in the present invention has a simple preparation method and can be added to the lubricating base oil after simple treatment, significantly reducing the friction coefficient and wear volume of the lubricating base oil. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is an AFM diagram of the iron phosphide trisulfide nanosheets provided by the present invention;

[0024] Figure 2Height curve of iron phosphide trisulfide nanosheets provided by the present invention;

[0025] Figure 3 Curve graph showing the change of friction coefficient of the lubricating base oil and the new lubricating oil provided in Example 11 over time;

[0026] Figure 4 Wear scar diagram of the lubricating base oil provided in Example 11;

[0027] Figure 5 Wear scar diagram of the new lubricating oil provided in Example 11;

[0028] Figure 6 Curve graph showing the change of friction coefficient of the lubricating base oil and the new lubricating oil provided in Example 12 over time;

[0029] Figure 7 Curve graph showing the change of friction coefficient of the lubricating base oil and the new lubricating oil provided in Example 13 over time. Detailed implementation manners

[0030] The following description is only for the preferred embodiments of the present invention and is not intended to limit the protection scope of the present invention. Any modifications, equivalent replacements, and improvements made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

[0031] The following embodiments can be understood as separately expressing a part of the local structure or method of the present invention, or can also be understood as the embodiments combined with each other to explain the connotation of the structure or method in a larger scope of the present invention.

[0032] Example 1

[0033] Ternary two-dimensional material FePS3 lubricating oil additive, and the additive is a nanosheet of iron phosphide trisulfide with the chemical formula FePS3.

[0034] Example 2

[0035] Preparation method of ternary two-dimensional material FePS3 lubricating oil additive, and the nanosheet of iron phosphide trisulfide is prepared from a single crystal of iron phosphide trisulfide. The size of the single crystal of iron phosphide trisulfide is 5×5×0.3 mm and is obtained by chemical vapor transport method.

[0036] Example 3

[0037] Preparation method of ternary two-dimensional material FePS3 lubricating oil additive, and the nanosheet of iron phosphide trisulfide is prepared from a single crystal of iron phosphide trisulfide. The size of the single crystal of iron phosphide trisulfide is 12×5×0.3 mm and is obtained by chemical vapor transport method.

[0038] Example 4

[0039] The nanosheets of iron trisulfide phosphide are prepared by a liquid-phase ultrasonic exfoliation method, including the following steps:

[0040] (1) Prepare single crystals of iron trisulfide phosphide by chemical vapor transport method, and then grind them using a mortar to obtain iron trisulfide phosphide powder;

[0041] (2) After mixing the iron trisulfide phosphide powder and the polar organic solvent anhydrous ethanol, use a probe ultrasonic crusher for ultrasonic exfoliation treatment, then use a high-speed stirrer for high-speed stirring, and then place the obtained mixed solution in a centrifuge to filter and separate the sediment, and perform drying treatment to obtain iron trisulfide phosphide nanosheets.

[0042] Example 5

[0043] In the step (1) described above, grind for 2 min using a mortar.

[0044] In the step (1) described above, the average particle size of the iron trisulfide phosphide powder is 5 μm, and the average thickness is 500 nm.

[0045] In the step (2) described above, the polar organic solvent is acetone.

[0046] In the step (2) described above, during the ultrasonic exfoliation treatment: the ultrasonic power is 200 W and the time is 10 min; during high-speed stirring, the stirrer speed is 100 r / min; during centrifugation: the speed is 100 r / min and the centrifugation time is 10 min; the drying temperature is 40 °C.

[0047] In the step (2) described above, the average particle size of the prepared iron trisulfide phosphide nanosheets is 20 nm, and the average thickness is 1 nm.

[0048] Example 6

[0049] In the step (1) described above, grind for 30 min using a mortar.

[0050] In the step (1) described above, the average particle size of the iron trisulfide phosphide powder is 30 μm, and the average thickness is 2000 nm.

[0051] In the step (2) described above, the polar organic solvent is NMP.

[0052] In the step (2) described above, during the ultrasonic exfoliation treatment: the ultrasonic power is 600 W and the time is 200 min; during high-speed stirring, the stirrer speed is 2000 r / min; during centrifugation: the speed is 5000 r / min and the centrifugation time is 60 min; the drying temperature is 100 °C.

[0053] In the step (2), the average particle size of the prepared iron phosphide trisulfide nanosheets is 100 nm, and the average thickness is 5 nm.

[0054] Example 7

[0055] In the step (2), the polar organic solvent is DMF.

[0056] Example 8

[0057] A preparation method of a lubricating oil containing a ternary two-dimensional material FePS3 lubricating oil additive includes the following steps: Select 10 mg of iron phosphide trisulfide nanosheets and add them to 9.99 g of a base oil polyethylene glycol to obtain a new lubricating oil with a mass fraction of iron phosphide trisulfide of 0.1%, and perform sufficient ultrasonic mixing using a probe ultrasonic wave with an ultrasonic power of 200 W and a mixing time of 10 min.

[0058] Example 9

[0059] A preparation method of a lubricating oil containing a ternary two-dimensional material FePS3 lubricating oil additive includes the following steps: Select 500 mg of iron phosphide trisulfide nanosheets and add them to 9.5 g of a base oil polyalphaolefin to obtain a new lubricating oil with a mass fraction of iron phosphide trisulfide of 5%, and perform sufficient ultrasonic mixing using a probe ultrasonic wave with an ultrasonic power of 1200 W and a mixing time of 60 min.

[0060] Example 10

[0061] In the preparation method of the lubricating oil, the base oil is hexadecane.

[0062] Example 11

[0063] Add 50 mg of FePS3 powder as an additive to 9.95 g of n-hexadecane lubricant (lubricating base oil) to obtain a lubricating oil containing 0.5% by mass of FePS3, and ultrasonically treat the lubricating oil for 30 min with an ultrasonic power of 600 W to make it fully mixed in the n-hexadecane lubricating base oil to obtain a new lubricating oil.

[0064] Perform tribological performance tests on the prepared new lubricating oil and the lubricating base oil n-hexadecane. The test equipment is a friction and wear tester (TRB, Anton Paar), using a reciprocating mode. The upper friction pair uses a GCr15 steel ball with a diameter of 6 mm, and the lower friction pair is GCr15. Before the experiment, the friction pairs are successively ultrasonically treated in acetone and ethanol for 10 minutes, then rinsed with deionized water, and finally dried in an oven. The test load is 5 N, the frequency is 2 Hz, and the amplitude is 2 mm. The change in the friction coefficient of the lubricating base oil used in this example between GCr15 over time is as Figure 3As shown by the curve on the upper middle side, the average friction coefficient is about 0.181. The variation of the friction coefficient of the new lubricating oil used in this embodiment between GCr15 with time is as Figure 3 shown by the curve on the lower middle side, and the average friction coefficient is about 0.11. The friction coefficient is reduced by 39.2%. The wear scar picture of the lubricating base oil used in this embodiment during friction between GCr15 is as Figure 4 shown, and the wear scar width is about 213.5 μm; the wear scar picture of the new lubricating oil used in this embodiment during friction between GCr15 is as Figure 5 shown, the wear scar width is about 141.27 μm, and the wear scar width is reduced by 33.8%.

[0065] Example 12

[0066] 100 mg of FePS3 powder was added as an additive to 9.9 g of polyalphaolefin (PAO20) lubricant to obtain a lubricating oil containing 1% by mass of FePS3. The lubricating oil was ultrasonically treated for 30 min with an ultrasonic power of 600 W to make it fully mixed in the PAO20 lubricating base oil, thus obtaining a new lubricating oil.

[0067] The tribological properties of the prepared new lubricating oil and the lubricating base oil PAO20 were tested. The test equipment was a tribometer (TRB, Anton Paar), using a reciprocating mode. The upper friction pair used a GCr15 steel ball with a diameter of 6 mm, and the lower friction pair was GCr15. Before the experiment, the friction pairs were ultrasonically treated in acetone and ethanol for 10 minutes successively, then rinsed with deionized water, and finally dried in an oven. The test load was 5 N, the frequency was 2 Hz, and the amplitude was 2 mm. The variation of the friction coefficient of the lubricating base oil used in this embodiment between GCr15 with time is as Figure 6 shown by the black line (the upper curve), and the average friction coefficient is about 0.105. The variation of the friction coefficient of the new lubricating oil used in this embodiment between GCr15 with time is as Figure 6 shown by the lower curve, and the average friction coefficient is about 0.098. The friction coefficient is reduced by 7%.

[0068] Example 13

[0069] 50 mg of FePS3 powder was added as an additive to 9.95 g of polyalphaolefin (PAO40) lubricant to obtain a lubricating oil containing 0.5% by mass of FePS3. The lubricating oil was ultrasonically treated for 30 min with an ultrasonic power of 600 W to make it fully mixed in the PAO40 lubricating base oil, thus obtaining a new lubricating oil.

[0070] The tribological properties of the prepared new lubricating oil and the lubricating base oil PAO40 were tested. The testing equipment was a tribometer (TRB, Anton Paar), using a reciprocating mode. The upper friction pair was a GCr15 steel ball with a diameter of 6 mm, and the lower friction pair was GCr15. Before the experiment, the friction pairs were ultrasonically treated in acetone and ethanol for 10 minutes successively, then rinsed with deionized water, and finally dried in an oven. The test load was 5 N, the frequency was 2 Hz, and the amplitude was 2 mm. The change of the friction coefficient of the lubricating base oil used in this example between GCr15 with time is as shown by the black line (the upper curve) in Figure 7 and the average friction coefficient is about 0.121. The change of the friction coefficient of the new lubricating oil used in this example between GCr15 with time is as shown by the lower curve in Figure 7 and the average friction coefficient is about 0.101. The friction coefficient is reduced by 16.5%.

Claims

1. Ternary two-dimensional material FePS3 lubricant additive, characterized by: The additive is a nanosheet of iron phosphorus trisulfide, and the chemical formula is FePS3.

2. The method for preparing the ternary two-dimensional material FePS3 lubricating oil additive according to claim 1, characterized in that: The phosphorus iron trisulfide nanosheet is prepared from a single crystal of phosphorus iron trisulfide, the single crystal of phosphorus iron trisulfide has a size of 5×5×0.3mm to 12×5×0.3mm, and is prepared by a chemical vapor transport method.

3. The method for preparing the ternary two-dimensional material FePS3 lubricating oil additive as claimed in claim 2, characterized in that: The nanosheets of phosphorus iron trisulfide are prepared by liquid phase ultrasonic exfoliation method, which comprises the following steps: (1) preparing ferrous phosphorus trisulfide single crystals by chemical vapor transport method, and then grinding the single crystals by mortar to obtain ferrous phosphorus trisulfide powders; (2) After the phosphorus iron trisulfide powder and the polar organic solvent are mixed, an ultrasonic peeling treatment is performed using a probe ultrasonic crusher, and then a high-speed stirrer is used for high-speed stirring. The resulting mixed solution is then placed in a centrifuge, the sediment is filtered and separated, and then dried to obtain phosphorus iron trisulfide nanosheets.

4. The method for preparing the ternary two-dimensional material FePS3 lubricating oil additive as claimed in claim 3, characterized in that: In the step (1), grinding is performed in a mortar for 2-30 minutes; the average particle size of the ferrous phosphorus trisulfide powder is 5-30 μm, and the average thickness is 500-2000 nm.

5. The method for preparing the ternary two-dimensional material FePS3 lubricating oil additive as claimed in claim 4, characterized in that: In the step (2), the polar organic solvent is one or a mixture of anhydrous ethanol, acetone, NMP, and DMF; during the ultrasonic stripping treatment: the ultrasonic power is 200-600W, and the time is 10-200min; during high-speed stirring, the stirrer speed is 100-2000r / min; during centrifugation: the speed is 100-5000r / min, and the centrifugation time is 10-60min; the drying temperature range is 40-100°C.

6. The method for preparing the ternary two-dimensional material FePS3 lubricating oil additive as claimed in claim 5, characterized in that: In the step (2), the average particle size of the prepared iron phosphide trisulfide nanosheets is 20 to 100 nm, and the average thickness is 1 to 5 nm.

7. A method for preparing a lubricating oil containing a ternary two-dimensional material FePS3 lubricating oil additive, characterized by: The phosphorus iron trisulfide nanosheets prepared by the method according to claim 6 include the following steps: selecting 10-500 mg of phosphorus iron trisulfide nanosheets, adding them to 9.5-9.99 g of base oil to obtain a new lubricating oil with a mass fraction of 0.1%-5%, and using probe ultrasound for sufficient ultrasonic mixing, the ultrasonic power is 200-1200 W, and the mixing time is 10-60 min.

8. A method for preparing a lubricating oil containing a ternary two-dimensional material FePS3 lubricating oil additive as claimed in claim 7, characterized in that: In the method for preparing the lubricating oil, the base oil is a mixture of one or more of polyethylene glycols or polyalphaolefins or hexadecane with different molecular weights.

Images