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

Abstract

The application discloses a preparation method of high-temperature-resistant extreme-pressure lubricating oil and relates to the technical field of lubricating materials. The fluorosilicone oil is prepared by using 1,1,3,3-tetrachloro-1,3-diphenyl disiloxane and methyl trifluoropropyl cyclotrisiloxane as raw materials, contains multiple benzene rings and chlorine atoms, can improve the high-temperature resistance and stability of the fluorosilicone oil, can help to form a more stable lubricating film on a friction surface, and can improve the extreme-pressure resistance of the fluorosilicone oil. Then, bentonite and a tungsten diselenide precursor solution are mixed, and the tungsten diselenide is directly prepared on the surface of the bentonite by using an ultrasonic pyrolysis method. The ultrasonic wave makes the tungsten diselenide better combine with active sites on the surface of the bentonite, improves the loading capacity of the tungsten diselenide, reduces the aggregation and loss of the tungsten diselenide additive during use, prolongs the service life of the tungsten diselenide additive, and further improves the high-temperature resistance and extreme-pressure resistance of the system. The prepared lubricating oil has the effects of high-temperature resistance and extreme-pressure resistance.

Description

Technical Field

[0001] This invention relates to the field of lubrication materials technology, specifically to a method for preparing a high-temperature and extreme-pressure lubricating oil. Background Technology

[0002] Lubricating oils generally consist of two parts: base oil and additives. Base oil is the main component of lubricating oil, determining its basic properties, while additives compensate for and improve the shortcomings of the base oil, imparting certain new properties, and are an important component of lubricating oils. Lubricating oil base oils are mainly divided into three categories: mineral base oils, synthetic base oils, and bio-based base oils.

[0003] With the advancement of technology, new materials and processes are constantly emerging, placing higher demands on the performance of lubricating oils. Under high-temperature, high-pressure, and heavy-load operating environments, ordinary lubricating oils may rapidly fail, leading to accelerated equipment wear and even malfunctions. This is particularly true in critical industries such as steel, chemicals, and power, where continuous and stable equipment operation is crucial for production. Current lubricating oils, under high-temperature and extreme-pressure conditions, exhibit significantly reduced adhesion, easily resulting in oil dripping and the production of large amounts of oily coke, requiring regular cleaning. Furthermore, under these conditions, excessive volatilization of the lubricating oil produces toxic fumes and irritating gases, leading to high oil consumption and environmental pollution. Current technologies often involve simultaneously feeding all raw materials into lubricating oil production equipment, using stirring, heating, homogenization, and sieving to prepare the lubricating oil. However, this method still suffers from poor high-temperature and extreme-pressure resistance. Summary of the Invention

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

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution: a high-temperature and extreme-pressure lubricating oil, wherein the high-temperature and extreme-pressure lubricating oil 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-modified tungsten diselenide.

[0006] Furthermore, the catalyst is either a strong acid cation exchange resin or tetramethylammonium hydroxide.

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

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

[0009] Furthermore, a method for preparing a high-temperature and extreme-pressure resistant lubricating oil includes the following preparation steps:

[0010] (1) Methyltrifluoropropylcyclotrisiloxane and 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane are mixed at a molar ratio of 1:1.0~1.5 and stirred at 200~300 r / min for 20~30 min. A catalyst with a molar ratio of 0.11~0.16 times that of methyltrifluoropropylcyclotrisiloxane is added and stirred at 100~150 r / min for 20~30 min. The temperature is raised to 115~120℃ and the reaction is carried out for 7~8 h. The filtrate is filtered and distilled under reduced pressure to 1~2 mmHg at 70~80℃ to obtain fluorosilicone oil.

[0011] (2) Dissolve selenium dioxide and sodium tungstate in deionized water to ensure that the concentrations of tungsten ions and selenite ions are both 0.2~0.4 mol / dm³. 3 Add hydrazine hydrate at 8-9 times the mass of sodium tungstate and bentonite at 1.1-1.5 times the mass of sodium tungstate, and stir at 300-400 r / min for 30-40 min to obtain tungsten diselenide precursor;

[0012] (3) Place the tungsten diselenide precursor solution in an ultrasonic sprayer and transport it to the reactor through nitrogen gas. React for 2-3 hours to obtain bentonite-modified tungsten diselenide.

[0013] (4) Bentonite-modified tungsten diselenide is ground in a ball mill and then added to fluorosilicone oil to obtain high-temperature extreme pressure lubricating oil.

[0014] Furthermore, in step (3), the bentonite is prepared by calcining at 450~470℃ for 1~1.5h.

[0015] Furthermore, the frequency of the ultrasonic sprayer in step (3) is 1.7~2.0MHz.

[0016] Furthermore, in step (3), the flow rate of nitrogen is 1.5~2.0 dm. 3 / min.

[0017] Furthermore, in step (3), the reactor temperature is 600~700℃.

[0018] Furthermore, in step (4), the particle size of the bentonite-modified tungsten diselenide after grinding is 30~40nm.

[0019] Compared with the prior art, the beneficial effects achieved by the present invention are:

[0020] This 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 additives to obtain lubricating oil, so as to achieve the effects of high temperature resistance and extreme pressure resistance.

[0021] First, fluorosilicone oil is prepared using 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane and methyltrifluoropropylcyclotrisiloxane as raw materials. Containing multiple benzene rings and chlorine atoms, this process allows the fluorosilicone oil to maintain stable performance at higher temperatures and significantly improves its oxidation resistance, high-temperature resistance, and stability. Simultaneously, it helps form a more stable lubricating film on the friction surface, reducing the friction coefficient and thus decreasing wear between friction pairs, thereby improving the extreme pressure resistance of the fluorosilicone oil.

[0022] Secondly, bentonite and tungsten diselenide precursor solutions are mixed, and tungsten diselenide is prepared directly on the surface of bentonite using ultrasonic pyrolysis. Ultrasonic waves can modify the structure of bentonite, making it more porous and with a larger specific surface area, thus exposing more active sites. Ultrasonic waves also make the tungsten diselenide precursor solution more evenly distributed on the bentonite surface, allowing tungsten diselenide to better bind with the active sites on the bentonite surface, increasing the tungsten diselenide loading. Ultrasonic waves can also create stronger interaction forces between tungsten diselenide and bentonite, reducing the aggregation and loss of tungsten diselenide additives during use, extending the service life of tungsten diselenide additives, and further improving the high-temperature resistance and extreme pressure resistance of the system. Detailed Implementation

[0023] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0024] To more clearly illustrate the method provided by the present invention, the following embodiments are provided in detail. The test methods for various indicators of the high-temperature extreme pressure lubricating oil prepared in the following embodiments are as follows:

[0025] Thermal stability: The high-temperature extreme pressure lubricating oils prepared by the same mass of the examples and comparative examples were tested at 400℃ according to SH / T0680-1999 "Determination of thermal stability of heat transfer fluids".

[0026] Oxidation stability: The high-temperature extreme pressure lubricating oils prepared by the same mass of the examples and comparative examples were tested for oxidation stability in accordance with SH / T0193-2008 "Determination of Oxidation Stability of Lubricating Oils - Rotating Oxygen Bomb Method".

[0027] Extreme pressure resistance: The extreme pressure and anti-wear characteristics of the lubricating oils prepared by the same mass of the examples and comparative examples were tested by SRV4 friction and wear performance according to SH / T0882-2014 "Determination of extreme pressure performance of lubricating oils - SRV test machine method".

[0028] Example 1

[0029] A method for preparing a high-temperature and extreme-pressure resistant lubricating oil includes the following preparation steps:

[0030] (1) Methyltrifluoropropylcyclotrisiloxane and 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane were mixed at a molar ratio of 1:1.0 and stirred at 200 r / min for 20 min. Sulfonated styrene-based cation exchange resin with a molar ratio of 0.11 times that of methyltrifluoropropylcyclotrisiloxane was added and stirred at 100 r / min for 20 min. The mixture was heated to 115 °C and reacted for 7 h. The filtrate was filtered and distilled at 70 °C under reduced pressure to 1 mmHg to obtain fluorosilicone oil.

[0031] (2) Activated bentonite was prepared by calcining bentonite at 450℃ for 1 hour. Selenium dioxide and sodium tungstate were dissolved in deionized water to ensure that the concentrations of tungsten ions and selenite ions were both 0.2 mol / dm³. 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;

[0032] (3) The tungsten diselenide precursor solution was placed in an ultrasonic sprayer with a frequency of 1.7 MHz and passed through a flow rate of 1.5 dm. 3 Nitrogen gas at a rate of 1 / min is fed into the reactor, and the temperature is raised to 600℃ and reacted for 2 hours to obtain bentonite-modified tungsten diselenide.

[0033] (4) Place the bentonite-modified tungsten diselenide in a ball mill and grind it until the particle size of the bentonite-modified tungsten diselenide is 30 nm. Then add it to fluorosilicone oil to obtain high-temperature extreme pressure lubricating oil.

[0034] Example 2

[0035] A method for preparing a high-temperature and extreme-pressure resistant lubricating oil includes the following preparation steps:

[0036] (1) Methyltrifluoropropylcyclotrisiloxane and 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane were mixed at a molar ratio of 1:1.3 and 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 was added and stirred at 130 r / min for 25 min. The mixture was heated to 118 °C and reacted for 7 h. The filtrate was filtered and distilled at 75 °C under reduced pressure to 2 mmHg to obtain fluorosilicone oil.

[0037] (2) Activated bentonite was prepared by calcining bentonite at 460℃ for 1 hour. 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 / dm³. 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 350 r / min for 35 min to obtain tungsten diselenide precursor;

[0038] (3) The tungsten diselenide precursor solution was placed in an ultrasonic sprayer with a frequency of 1.8 MHz and passed through a flow rate of 1.8 dm. 3 Nitrogen gas at a rate of 1 / min is fed into the reactor, and the temperature is raised to 650℃ and reacted for 3 hours to obtain bentonite-modified tungsten diselenide.

[0039] (4) Place the bentonite-modified tungsten diselenide in a ball mill and grind it until the particle size of the bentonite-modified tungsten diselenide is 35 nm. Then add it to fluorosilicone oil to obtain high-temperature extreme pressure lubricating oil.

[0040] Example 3

[0041] A method for preparing a high-temperature and extreme-pressure resistant lubricating oil includes the following preparation steps:

[0042] (1) Methyltrifluoropropylcyclotrisiloxane and 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane are mixed at a molar ratio of 1:1.5 and stirred at 300 r / min for 20-30 min. Sulfonated styrene-based cation exchange resin with a molar ratio of 0.16 times that of methyltrifluoropropylcyclotrisiloxane is added and stirred at 150 r / min for 30 min. The mixture is heated to 120 °C and reacted for 8 h. The filtrate is filtered and distilled at 80 °C under reduced pressure to 2 mmHg to obtain fluorosilicone oil.

[0043] (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 concentrations of tungsten ions and selenite ions were both 0.4mol / dm³. 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;

[0044] (3) The tungsten diselenide precursor solution was placed in an ultrasonic sprayer with a frequency of 2.0 MHz and passed through a flow rate of 2.0 dm³. 3 Nitrogen gas at a rate of 1 / min is delivered to the reactor, and the temperature is raised to 700℃ and reacted for 3 hours to obtain bentonite-modified tungsten diselenide.

[0045] (4) Place the bentonite-modified tungsten diselenide in a ball mill and grind it until the particle size of the bentonite-modified tungsten diselenide is 40 nm. Then add it to fluorosilicone oil to obtain high-temperature extreme pressure lubricating oil.

[0046] Comparative Example 1

[0047] 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 filtrate, and distilled at 75°C under reduced pressure to 2 mmHg to obtain fluorosilicone oil; the remaining steps are the same as in Example 2.

[0048] Comparative Example 2

[0049] The difference between Comparative Example 2 and Example 2 lies in step (2). Step (2) is changed to: dissolving 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, adding hydrazine hydrate at 8 times the mass of sodium tungstate, and stirring at 350 r / min for 35 min to obtain tungsten diselenide precursor; step (3) is changed to: (3) placing the tungsten diselenide precursor solution in an ultrasonic sprayer with a frequency of 1.8 MHz, and conveying it to the reactor through nitrogen gas at a flow rate of 1.8 dm3 / min, heating it to 650℃ and reacting for 3 h to obtain tungsten diselenide; the remaining steps are the same as in Example 2.

[0050] Comparative Example 3

[0051] The difference between Comparative Example 3 and Example 2 is that step (3) is omitted, and step (2) is changed to: calcining bentonite at 460°C for 1 hour to obtain activated bentonite; step (4) is changed to: placing bentonite in a ball mill for grinding until the particle size of bentonite is 35nm and then adding it to fluorosilicone oil to obtain high temperature and extreme pressure lubricating oil; the remaining steps are the same as in Example 2.

[0052] Comparative Example 4

[0053] The difference between Comparative Example 4 and Example 2 is that step (3) is omitted. 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 taking the filtrate, washing with deionized water until neutral to obtain bentonite-modified tungsten diselenide; the remaining steps are the same as in Example 2.

[0054] Example of effect

[0055] Table 1 below shows the performance analysis results of the high-temperature extreme pressure lubricating oils of Examples 1 to 3 and Comparative Examples 1 to 4 of the present invention.

[0056] Table 1

[0057]

[0058] A comparison of the experimental data from Example 2 and Comparative Example 1 reveals that the present invention, by using 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane and methyltrifluoropropylcyclotrisiloxane as raw materials to prepare fluorosilicone oil, contains multiple benzene rings and chlorine atoms. This allows the fluorosilicone oil to maintain stable performance at higher temperatures and greatly improves its oxidation resistance, high-temperature resistance, and stability. Simultaneously, it helps form a more stable lubricating film on the friction surface, reducing the friction coefficient and thus reducing wear between friction pairs, thereby improving the extreme pressure resistance of the fluorosilicone oil. A comparison of the experimental data from Example 2 and Comparative Example 2 reveals that the present invention, by adding bentonite, improves the dispersibility of tungsten diselenide additives in lubricating oil, reduces the aggregation and loss of tungsten diselenide during use, extends the service life of tungsten diselenide additives, and improves the high-temperature resistance and extreme pressure resistance of the system. A comparison of the experimental data from Example 2 and Comparative Example 3 reveals that the present invention, by adding bentonite... Tungsten enhances the system's high-temperature resistance and extreme pressure resistance. It can form a protective film on the metal surface, preventing direct contact and wear, and has a certain antioxidant effect, slowing down the oxidation process of lubricating oil at high temperatures. A comparison of experimental data from Example 2 and Comparative Example 4 reveals that this invention utilizes ultrasonic pyrolysis to directly prepare tungsten diselenide on the surface of bentonite. Ultrasonic waves can modify the structure of bentonite, making it more porous and increasing its specific surface area, thus exposing more active sites. Ultrasonic waves also make the tungsten diselenide precursor solution more evenly distributed on the bentonite surface, allowing tungsten diselenide to better bind with the active sites on the bentonite surface, increasing the tungsten diselenide loading. Furthermore, ultrasonic waves can create stronger interaction forces between tungsten diselenide and bentonite, reducing the aggregation and loss of tungsten diselenide additives during use, extending the service life of the additives, and further improving the system's high-temperature resistance and extreme pressure resistance.

[0059] 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 implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No markings in the claims should be construed as limiting the scope of the claims.

Claims

1. A method for preparing a high-temperature and extreme-pressure resistant lubricating oil, characterized in that, The preparation steps include the following: (1) Methyltrifluoropropylcyclotrisiloxane and 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane were mixed at a molar ratio of 1:1.3 and 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 was added and stirred at 130 r / min for 25 min. The mixture was heated to 118 °C and reacted for 7 h. The filtrate was filtered and distilled at 75 °C under reduced pressure to 2 mmHg to obtain fluorosilicone oil. (2) Activated bentonite was prepared by calcining bentonite at 460℃ for 1 hour. 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 / dm³. 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 350 r / min for 35 min to obtain tungsten diselenide precursor; (3) The tungsten diselenide precursor solution was placed in an ultrasonic sprayer with a frequency of 1.8 MHz and passed through a flow rate of 1.8 dm. 3 Nitrogen gas at a rate of 1 / min is fed into the reactor, and the temperature is raised to 650℃ and reacted for 3 hours to obtain bentonite-modified tungsten diselenide. (4) Place the bentonite-modified tungsten diselenide in a ball mill and grind it until the particle size of the bentonite-modified tungsten diselenide is 35 nm. Then add it to fluorosilicone oil to obtain high-temperature extreme pressure lubricating oil.

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