Preparation method of high-temperature-resistant extreme-pressure lubricating oil

Abstract

The invention discloses a preparation method of high-temperature-resistant extreme-pressure lubricating oil, and relates to the technical field of lubricating materials. According to the invention, 1, 1, 3, 3-tetrachloro-1, 3-diphenyl disiloxane and methyl trifluoropropyl cyclotrisiloxane are used as raw materials to prepare the fluorosilicone oil, and the fluorosilicone oil contains a plurality of benzene rings and chlorine atoms, so that the high temperature resistance and stability of the fluorosilicone oil can be improved, meanwhile, a more stable lubricating film can be formed on a friction surface, and the extreme pressure resistance of the fluorosilicone oil is improved; then bentonite and a tungsten diselenide precursor solution are mixed, tungsten diselenide is directly prepared on the surface of bentonite through an ultrasonic pyrolysis method, tungsten diselenide is better combined with active sites on the surface of bentonite through ultrasonic waves, the loading amount of tungsten diselenide is increased, aggregation and loss of the tungsten diselenide additive in the using process are reduced, and the stability of the tungsten diselenide additive is improved. The service life of the tungsten diselenide additive is prolonged, and the high temperature resistance and the extreme pressure resistance of the system are further improved. The lubricating oil prepared by the invention has the effects of high temperature resistance and extreme pressure resistance.

Description

Technical Field

[0001] The present invention relates to the technical field of lubricating materials, in particular to a method for preparing high-temperature resistant extreme-pressure lubricating oil. Background Art

[0002] Lubricants generally consist of two parts: base oil and additives. Base oil is the primary component of lubricants and determines their fundamental properties. Additives, on the other hand, compensate for and improve base oil performance deficiencies, imparting new properties and becoming a crucial component of lubricants. Lubricant base oils are primarily categorized into three main types: mineral base oils, synthetic base oils, and bio-based base oils.

[0003] With the advancement of science and technology, new materials and new processes are constantly emerging, which puts higher requirements on the performance of lubricating oils. Under high temperature, high pressure and heavy load working environments, ordinary lubricating oils may quickly fail, resulting in increased equipment wear and even failure. Especially in key industries such as steel, chemical industry, and electric power, the continuous and stable operation of equipment is crucial to production. Under high temperature and extreme pressure conditions, the adhesion ability of lubricating oils in the existing technology is greatly reduced, and oil dripping is very likely to occur. A large amount of oily coke is also produced, which requires regular cleaning of the coke. Moreover, under high temperature and extreme pressure conditions, lubricating oils evaporate excessively, producing toxic smoke and pungent odorous gases, high oil consumption, and environmental pollution. The existing technology often uses all raw materials to be put into the lubricating oil production equipment at the same time, and the lubricating oil is prepared by stirring, heating, and fully mixing the materials, and then homogenizing and screening. However, there is still the problem of poor high temperature and extreme pressure resistance. Summary of the Invention

[0004] The purpose of the present invention is to provide a high-temperature resistant extreme pressure lubricating oil and a preparation method thereof, so as to solve the problems existing in the prior art.

[0005] In order to solve the above technical problems, the present invention provides the following technical solution: a high-temperature resistant extreme-pressure lubricant, which is prepared by using 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane, methyltrifluoropropylcyclotrisiloxane and a catalyst as raw materials to prepare fluorosilicone oil, and then adding bentonite to modify tungsten diselenide.

[0006] Furthermore, the catalyst is a strongly acidic cation exchange resin or tetramethylammonium hydroxide.

[0007] Furthermore, the strongly acidic cation exchange resin is sulfonated coal or sulfonated styrene cation exchange resin.

[0008] Furthermore, the bentonite-modified tungsten diselenide is prepared by mixing bentonite and a tungsten diselenide precursor solution, and directly preparing tungsten diselenide on the surface of the bentonite by ultrasonic pyrolysis.

[0009] Furthermore, a method for preparing a high temperature resistant extreme pressure lubricant comprises the following preparation steps: (1) Methyl trifluoropropyl cyclotrisiloxane and 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane were mixed at a molar ratio of 1:1.0~1.5, stirred at 200~300 r / min for 20~30 min, added with a catalyst having a molar ratio of 0.11~0.16 times that of methyl trifluoropropyl cyclotrisiloxane, stirred at 100~150 r / min for 20~30 min, heated to 115~120°C, reacted for 7~8h, filtered to obtain the filtrate, and decompressed to 1~2 mmHg and distilled at 70~80°C to obtain fluorosilicone oil; (2) Dissolve selenium dioxide and sodium tungstate in deionized water to ensure that the concentrations of tungsten ions and selenite ions are both 0.2~0.4mol / dm 3 , add hydrazine hydrate (8 to 9 times the mass of sodium tungstate) and bentonite (1.1 to 1.5 times the mass of sodium tungstate), and stir at 300 to 400 r / min for 30 to 40 minutes to obtain a tungsten diselenide precursor; (3) Place the tungsten diselenide precursor solution in an ultrasonic sprayer and transport it to the reactor via nitrogen gas. React for 2 to 3 hours to obtain bentonite-modified tungsten diselenide. (4) The bentonite-modified tungsten diselenide is placed in a ball mill and ground. After grinding, it is added to fluorosilicone oil to obtain a high-temperature resistant extreme pressure lubricant.

[0010] Furthermore, in step (3), the bentonite is prepared by calcining at 450-470° C. for 1-1.5 hours.

[0011] Furthermore, the frequency of the ultrasonic sprayer in step (3) is 1.7-2.0 MHz.

[0012] Furthermore, the flow rate of nitrogen in step (3) is 1.5~2.0dm 3 / min.

[0013] Furthermore, in step (3), the reactor temperature is 600-700°C.

[0014] Furthermore, the particle size of the bentonite-modified tungsten diselenide after grinding in step (4) is 30-40 nm.

[0015] Compared with the prior art, the present invention has the following beneficial effects: The invention uses 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane and methyltrifluoropropylcyclotrisiloxane as raw materials to prepare fluorosilicone oil, and then adds bentonite-modified tungsten diselenide additive to prepare lubricating oil, so as to achieve the effects of high temperature resistance and extreme pressure resistance.

[0016] First, fluorosilicone oil is prepared using 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane and methyltrifluoropropylcyclotrisiloxane as raw materials. Fluorosilicone oil contains multiple benzene rings and chlorine atoms, which can enable fluorosilicone oil to maintain stable performance at higher temperatures and greatly improve the antioxidant ability of fluorosilicone oil, improve the high temperature resistance and stability of fluorosilicone oil, and at the same time help to form a more stable lubricating film on the friction surface, reduce the friction coefficient, thereby reducing wear between friction pairs and improving the extreme pressure resistance of fluorosilicone oil.

[0017] Secondly, the bentonite and tungsten diselenide precursor solution are mixed, and tungsten diselenide is directly prepared on the bentonite surface by ultrasonic pyrolysis. Ultrasonic waves can modify the structure of bentonite, making the structure of bentonite looser and the specific surface area larger, so that more active sites are exposed. Ultrasonic waves can also make the tungsten diselenide precursor solution more evenly distributed on the bentonite surface, so that tungsten diselenide can better combine with the active sites on the bentonite surface, thereby increasing the loading capacity of tungsten diselenide. Ultrasonic waves can also form a stronger interaction force between tungsten diselenide and bentonite, reduce the aggregation and loss of tungsten diselenide additives during use, extend the service life of tungsten diselenide additives, and further improve the system's high temperature resistance and extreme pressure resistance. DETAILED DESCRIPTION

[0018] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0019] In order to more clearly illustrate the method provided by the present invention, the following examples are used to describe in detail the various index testing methods of the high temperature resistant extreme pressure lubricating oil prepared in the following examples. Thermal stability: The same mass of the high-temperature resistant extreme pressure lubricating oils prepared in the examples and comparative examples were tested for their thermal stability at 400°C according to SH / T0680-1999 "Determination of Thermal Stability of Heat Transfer Fluids".

[0020] Oxidation stability: The same mass of high-temperature resistant extreme pressure lubricating oils prepared in the examples and comparative examples were tested for oxidation stability according to SH / T0193-2008 “Determination of oxidation stability of lubricating oils - Rotating oxygen bomb method”.

[0021] Extreme pressure resistance: The high-temperature resistant extreme pressure lubricating oils prepared in the examples and comparative examples of the same mass were tested for their extreme pressure and anti-wear properties using the SRV4 friction and wear tester method in accordance with SH / T0882-2014 "Determination of Extreme Pressure Properties of Lubricating Oils - SRV Testing Machine Method".

[0022] Example 1 A method for preparing high-temperature resistant extreme pressure lubricating oil comprises the following steps: (1) Methyl trifluoropropyl cyclotrisiloxane and 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane were mixed at a molar ratio of 1:1.0, stirred at 200 r / min for 20 min, sulfonated styrene cation exchange resin with a molar ratio of 0.11 times that of methyl trifluoropropyl cyclotrisiloxane was added, stirred at 100 r / min for 20 min, heated to 115°C, reacted for 7 h, filtered to obtain the filtrate, and decompressed to 1 mmHg and distilled at 70°C to obtain fluorosilicone oil; (2) Activated bentonite was prepared by calcining bentonite at 450℃ for 1h. Selenium dioxide and sodium tungstate were dissolved in deionized water to ensure that the concentration of tungsten ion and selenite ion were both 0.2 mol / dm 3 , add hydrazine hydrate (8 times the mass of sodium tungstate) and activated bentonite (1.1 times the mass of sodium tungstate), and stir at 300 r / min for 30 min to obtain tungsten diselenide precursor; (3) Place the tungsten diselenide precursor solution in an ultrasonic sprayer with a frequency of 1.7 MHz and a flow rate of 1.5 dm 3 / min nitrogen was delivered to the reactor, and the temperature was raised to 600℃ and reacted for 2h to obtain bentonite-modified tungsten diselenide; (4) The bentonite-modified tungsten diselenide is placed in a ball mill and ground until the particle size of the bentonite-modified tungsten diselenide is 30 nm. Then, the bentonite-modified tungsten diselenide is added to fluorosilicone oil to obtain a high-temperature resistant extreme pressure lubricant.

[0023] Example 2 A method for preparing high-temperature resistant extreme pressure lubricating oil comprises the following steps: (1) Methyl trifluoropropyl cyclotrisiloxane and 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane were mixed at a molar ratio of 1:1.3, stirred at 250 r / min for 25 min, sulfonated styrene cation exchange resin with a molar ratio of 0.13 times that of methyl trifluoropropyl cyclotrisiloxane was added, stirred at 130 r / min for 25 min, heated to 118°C, reacted for 7 h, filtered to obtain the filtrate, and decompressed to 2 mmHg and distilled at 75°C to obtain fluorosilicone oil; (2) Activated bentonite was prepared by calcining bentonite at 460°C for 1 hour, and selenium dioxide and sodium tungstate were dissolved in deionized water to ensure that the concentrations of tungsten ions and selenite ions were both 0.3 mol / dm 3 , add hydrazine hydrate 8 times the mass of sodium tungstate and activated bentonite 1.3 times the mass of sodium tungstate, and stir at 350r / min for 35min to obtain tungsten diselenide precursor; (3) Place the tungsten diselenide precursor solution in an ultrasonic sprayer with a frequency of 1.8 MHz and a flow rate of 1.8 dm3 / min nitrogen was delivered to the reactor, and the temperature was raised to 650℃ and reacted for 3h to obtain bentonite-modified tungsten diselenide; (4) The bentonite-modified tungsten diselenide is placed in a ball mill and ground until the particle size of the bentonite-modified tungsten diselenide is 35 nm. The fluorosilicone oil is then added to obtain a high-temperature resistant extreme pressure lubricant.

[0024] Example 3 A method for preparing high-temperature resistant extreme pressure lubricating oil comprises the following steps: (1) Methyl trifluoropropyl cyclotrisiloxane and 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane were mixed at a molar ratio of 1:1.5, stirred at 300 r / min for 20-30 min, sulfonated styrene cation exchange resin with a molar ratio of 0.16 times that of methyl trifluoropropyl cyclotrisiloxane was added, stirred at 150 r / min for 30 min, heated to 120°C, reacted for 8 h, filtered to obtain the filtrate, and decompressed to 2 mmHg and distilled at 80°C to obtain fluorosilicone oil; (2) Activated bentonite was prepared by calcining bentonite at 470℃ for 1.5h. Selenium dioxide and sodium tungstate were dissolved in deionized water to ensure that the concentration of tungsten ion and selenite ion were both 0.4 mol / dm 3 , add hydrazine hydrate (9 times the mass of sodium tungstate) and activated bentonite (1.5 times the mass of sodium tungstate), and stir at 400 r / min for 40 min to obtain tungsten diselenide precursor; (3) Place the tungsten diselenide precursor solution in an ultrasonic sprayer with a frequency of 2.0 MHz and a flow rate of 2.0 dm 3 / min nitrogen was delivered to the reactor, and the temperature was raised to 700℃ and reacted for 3h to obtain bentonite-modified tungsten diselenide; (4) The bentonite-modified tungsten diselenide is placed in a ball mill and ground until the particle size of the bentonite-modified tungsten diselenide is 40 nm. Then, the bentonite-modified tungsten diselenide is added to fluorosilicone oil to obtain a high-temperature resistant extreme pressure lubricant.

[0025] Comparative Example 1 The difference between Comparative Example 1 and Example 2 is that step (1) is different. Step (1) is changed to: methyltrifluoropropylcyclotrisiloxane and octamethylcyclotetrasiloxane are mixed in a molar ratio of 1:1.3, stirred at 250 r / min for 25 min, sulfonated styrene-based cation exchange resin with a molar ratio of 0.13 times that of methyltrifluoropropylcyclotrisiloxane is added, stirred at 130 r / min for 25 min, heated to 118°C, reacted for 7 h, filtered to obtain a filtrate, and decompressed to 2 mmHg and distilled at 75°C to obtain fluorosilicone oil; the remaining steps are the same as those in Example 2.

[0026] Comparative Example 2 The difference between Comparative Example 2 and Example 2 lies in the difference in step (2). Step (2) is changed to: dissolve selenium dioxide and sodium tungstate in deionized water to ensure that the concentrations of tungsten ions and selenite ions are both 0.3 mol / dm3, add hydrazine hydrate 8 times the mass of sodium tungstate, and stir at 350 r / min for 35 min to obtain a tungsten diselenide precursor; step (3) is changed to: (3) place the tungsten diselenide precursor solution in an ultrasonic sprayer with a frequency of 1.8 MHz, transport it to a reactor through nitrogen at a flow rate of 1.8 dm3 / min, heat it to 650°C and react for 3 h to obtain tungsten diselenide; the remaining steps are the same as in Example 2.

[0027] Comparative Example 3 The difference between Comparative Example 3 and Example 2 is that there is no step (3), and step (2) is changed to: calcining bentonite at 460°C for 1 hour to obtain activated bentonite; step (4) is changed to: grinding the bentonite in a ball mill until the particle size of the bentonite is 35 nm, and then adding fluorosilicone oil to obtain high-temperature resistant extreme pressure lubricating oil; the remaining steps are the same as those in Example 2.

[0028] Comparative Example 4 The difference between Comparative Example 4 and Example 2 is that there is no step (3). Step (3) is changed to: heating the tungsten diselenide precursor to 200°C, reacting for 48 hours, naturally cooling to room temperature, centrifuging and washing 5 times, washing with 25wt% NaOH solution, filtering and collecting the filtrate, and washing with deionized water until neutral to obtain bentonite-modified tungsten diselenide; the remaining steps are the same as in Example 2.

[0029] Effect Examples Table 1 below shows the performance analysis results of the high temperature resistant extreme pressure lubricating oils of Examples 1 to 3 of the present invention and Comparative Examples 1 to 4.

[0030] Table 1 From the comparison of the experimental data of Example 2 with that of Comparative Example 1, it can be found that the present invention prepares fluorosilicone oil by using 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane and methyltrifluoropropylcyclotrisiloxane as raw materials, which contains multiple benzene rings and chlorine atoms, so that the fluorosilicone oil can maintain stable performance at higher temperatures and greatly improve the antioxidant ability of the fluorosilicone oil, improve the high temperature resistance and stability of the fluorosilicone oil, and at the same time help to form a more stable lubricating film on the friction surface, reduce the friction coefficient, thereby reducing the wear between the friction pairs and improving the extreme pressure resistance of the fluorosilicone oil; from the comparison of the experimental data of Example 2 with that of Comparative Example 2, it can be found that the present invention improves the dispersibility of the tungsten diselenide additive in the lubricating oil by adding bentonite, reduces the aggregation and loss of tungsten diselenide during use, prolongs the service life of the tungsten diselenide additive, and improves the high temperature resistance and extreme pressure resistance of the system by adding bentonite Tungsten improves the high temperature resistance and extreme pressure resistance of the system, can form a protective film on the metal surface to prevent direct contact and wear of the metal surface, has a certain antioxidant effect, and can slow down the oxidation process of lubricating oil at high temperature; from the comparison of the experimental data of Example 2 and Comparative Example 4, it can be found that the present invention uses ultrasonic pyrolysis to directly prepare tungsten diselenide on the surface of bentonite. Ultrasonic waves can modify the structure of bentonite, making the structure of bentonite looser and the specific surface area larger, so that more active sites will be exposed. Ultrasonic waves will also make the tungsten diselenide precursor solution more evenly distributed on the surface of bentonite, so that tungsten diselenide can better combine with the active sites on the surface of bentonite, thereby increasing the loading amount of tungsten diselenide. Ultrasonic waves can also form a stronger interaction force between tungsten diselenide and bentonite, reduce the aggregation and loss of tungsten diselenide additives during use, extend the service life of tungsten diselenide additives, and further improve the high temperature resistance and extreme pressure resistance of the system.

[0031] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims, not the foregoing description, and all variations within the meaning and range of equivalents of the claims are intended to be encompassed therein. Any reference in a claim should not be construed as limiting the claim to which it relates.

Claims

1. A method for preparing a high temperature resistant extreme pressure lubricating oil, characterized in that: The method comprises the following preparation steps: (1) Methyl trifluoropropyl cyclotrisiloxane and 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane were mixed at a molar ratio of 1:1.3, stirred at 250 r / min for 25 min, sulfonated styrene cation exchange resin with a molar ratio of 0.13 times that of methyl trifluoropropyl cyclotrisiloxane was added, stirred at 130 r / min for 25 min, heated to 118°C, reacted for 7 h, filtered to obtain the filtrate, and decompressed to 2 mmHg and distilled at 75°C to obtain fluorosilicone oil; (2) Activated bentonite was prepared by calcining bentonite at 460°C for 1 hour, and selenium dioxide and sodium tungstate were dissolved in deionized water to ensure that the concentrations of tungsten ions and selenite ions were both 0.3 mol / dm 3 , add hydrazine hydrate 8 times the mass of sodium tungstate and activated bentonite 1.3 times the mass of sodium tungstate, and stir at 350r / min for 35min to obtain tungsten diselenide precursor; (3) Place the tungsten diselenide precursor solution in an ultrasonic sprayer with a frequency of 1.8 MHz and a flow rate of 1.8 dm 3 / min nitrogen was delivered to the reactor, and the temperature was raised to 650℃ and reacted for 3h to obtain bentonite-modified tungsten diselenide; (4) The bentonite-modified tungsten diselenide is placed in a ball mill and ground until the particle size of the bentonite-modified tungsten diselenide is 35 nm. The fluorosilicone oil is then added to obtain a high-temperature resistant extreme pressure lubricant.

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