High-temperature-resistant extreme-pressure lubricating oil and preparation method thereof

Abstract

The invention discloses high-temperature-resistant extreme-pressure lubricating oil and a preparation method thereof, 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 invention relates to the technical field of lubricating materials, in particular to a high temperature resistant extreme pressure lubricating oil and a preparation method thereof. Background Art

[0002] Lubricating oil generally consists of two parts: base oil and additives. Base oil is the main component of lubricating oil and determines the basic properties of lubricating oil. Additives can make up for and improve the deficiencies in the performance of base oil and give it some new properties. They are an important part of lubricating oil. Lubricating oil base oil is mainly divided into three categories: mineral base oil, synthetic base oil and bio-base oil.

[0003] With the advancement of science and technology, new materials and new processes continue to emerge, and higher requirements are placed on the performance of lubricants. Under high temperature, high pressure and heavy load working environments, ordinary lubricants may quickly fail, resulting in increased equipment wear and even failure. Especially in key industries such as steel, chemical, and electric power, the continuous and stable operation of equipment is essential for production. Under high temperature and extreme pressure conditions, the adhesion ability of lubricants in the prior art is greatly reduced, and oil dripping is very likely to occur, and a large amount of oily coke is produced, which requires regular cleaning of the coke. Moreover, under high temperature and extreme pressure conditions, lubricants evaporate excessively, producing toxic smoke and pungent odor gases, large oil consumption, and environmental pollution. In the prior art, all raw materials are often put into the lubricant production equipment at the same time, and the lubricant is prepared by stirring, heating, and fully mixing the materials, and then homogenizing and sieving, but there is still a 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 solutions: a high temperature resistant extreme pressure lubricating oil, wherein the high temperature resistant 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 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 bentonite by ultrasonic pyrolysis.

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

[0010] (1) Methyl trifluoropropyl cyclotrisiloxane and 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane are mixed at a molar ratio of 1:1.0-1.5, stirred at 200-300 r / min for 20-30 min, a catalyst with a molar ratio of 0.11-0.16 times of methyl trifluoropropyl cyclotrisiloxane is added, stirred at 100-150 r / min for 20-30 min, heated to 115-120° C., reacted for 7-8 h, filtered to obtain a filtrate, and decompressed to 1-2 mmHg and distilled at 70-80° C. 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 / dm 3 , add hydrazine hydrate with a mass of 8 to 9 times that of sodium tungstate and bentonite with a mass of 1.1 to 1.5 times that of sodium tungstate, and stir at 300 to 400 r / min for 30 to 40 minutes to obtain a tungsten diselenide precursor;

[0012] (3) placing a tungsten diselenide precursor solution in an ultrasonic sprayer, transporting it to a reactor via nitrogen, and reacting for 2 to 3 hours to obtain bentonite-modified tungsten diselenide;

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

[0014] Furthermore, in step (3), the bentonite is prepared by calcining at 450-470° C. for 1-1.5 hours.

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

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

[0017] Furthermore, in step (3), the reactor temperature is 600-700°C.

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

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

[0020] 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.

[0021] 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 help 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 fluorosilicone oil.

[0022] Secondly, the bentonite and tungsten diselenide precursor solution are mixed, and tungsten diselenide is directly prepared on the surface of bentonite by ultrasonic pyrolysis. Ultrasonic waves can modify the structure of bentonite, making the structure of bentonite looser and larger in specific surface area, so that more active sites are exposed. Ultrasonic waves can 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 system's high temperature resistance and extreme pressure resistance. DETAILED DESCRIPTION

[0023] 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 described embodiments 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 work are within the scope of protection of the present invention.

[0024] 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 are as follows:

[0025] Thermal stability: The same mass of high temperature resistant extreme pressure lubricating oils prepared in the embodiment and the comparative example were tested for thermal stability at 400°C according to SH / T0680-1999 “Method for Determination of Thermal Stability of Heat Transfer Fluids”.

[0026] 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".

[0027] Extreme pressure resistance: The high temperature resistant extreme pressure lubricating oils prepared in the embodiment and the comparative example of the same mass were tested for their extreme pressure and anti-wear properties using SRV4 friction and wear performance in accordance with SH / T0882-2014 "Determination of Extreme Pressure Performance of Lubricating Oils - SRV Testing Machine Method".

[0028] Example 1

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

[0030] (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 a filtrate, and reduced pressure to 1 mmHg and distilled at 70° C. to obtain fluorosilicone oil;

[0031] (2) Bentonite was calcined at 450°C for 1 h to obtain activated bentonite, and selenium dioxide and sodium tungstate were dissolved in deionized water to ensure that the concentrations of tungsten ions and selenite ions were both 0.2 mol / dm 3 , add hydrazine hydrate with a mass of 8 times that of sodium tungstate and activated bentonite with a mass of 1.1 times that of sodium tungstate, and stir at 300r / min for 30min to obtain a tungsten diselenide precursor;

[0032] (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;

[0033] (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, and then added to fluorosilicone oil to obtain a high temperature resistant extreme pressure lubricating oil.

[0034] Example 2

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

[0036] (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 a filtrate, and reduced pressure to 2 mmHg and distilled at 75° C. to obtain fluorosilicone oil;

[0037] (2) Activated bentonite was prepared by calcining bentonite at 460°C for 1 h, 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;

[0038] (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℃ for reaction for 3h to obtain bentonite-modified tungsten diselenide;

[0039] (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, and then added to fluorosilicone oil to obtain a high temperature resistant extreme pressure lubricating oil.

[0040] Example 3

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

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

[0043] (2) Activated bentonite was prepared by calcining bentonite at 470°C for 1.5 h, and selenium dioxide and sodium tungstate were dissolved in deionized water to ensure that the concentrations of tungsten ions and selenite ions were both 0.4 mol / dm 3 , add hydrazine hydrate with a mass of 9 times that of sodium tungstate and activated bentonite with a mass of 1.5 times that of sodium tungstate, and stir at 400r / min for 40min to obtain a tungsten diselenide precursor;

[0044] (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℃ for 3h to obtain bentonite-modified tungsten diselenide;

[0045] (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, and then added to fluorosilicone oil to obtain a high temperature resistant 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 the filtrate, and decompressed to 2 mmHg and distilled at 75° C. to obtain fluorosilicone oil; the remaining steps are the same as 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: 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 with a mass of 8 times that 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, react for 3 h to obtain tungsten diselenide; the remaining steps are the same as those in Example 2.

[0050] Comparative Example 3

[0051] 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 1h to obtain activated bentonite; step (4) is changed to: grinding the bentonite in a ball mill until the particle size of the bentonite is 35nm and then adding fluorosilicone oil to obtain high temperature resistant extreme pressure lubricating oil; the remaining steps are the same as Example 2.

[0052] Comparative Example 4

[0053] The difference between Comparative Example 4 and Example 2 is that there is no step (3), and 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 the filtrate, and washing with deionized water until neutral to obtain bentonite-modified tungsten diselenide; the remaining steps are the same as Example 2.

[0054] Effect example

[0055] 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.

[0056]

[0057] From the comparison of the experimental data of Example 2 with that of Comparative Example 1, it can be found that the present invention uses 1,1,3,3-tetrachloro-1,3-diphenyldisiloxane and methyltrifluoropropylcyclotrisiloxane as raw materials to prepare fluorosilicone oil, 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 factor, 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; from the comparison of the experimental data of Example 2 with that of Comparative Example 3, 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. 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, and the ultrasonic wave can modify the structure of bentonite, making the structure of bentonite looser and larger in specific surface area, so that more active sites are exposed to the outside, and the ultrasonic wave can 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, and increase 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.

[0058] It will be apparent to those skilled in the art that the 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 the spirit or essential features of the invention. 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, and it is intended that all variations within the meaning and scope of the equivalent elements of the claims be included in the invention. Any marking in a claim should not be considered as limiting the claim to which it relates.

Claims

1. A high temperature resistant extreme pressure lubricating oil, characterized in that: The high temperature resistant 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 to modify tungsten diselenide.

2. A high temperature resistant extreme pressure lubricating oil according to claim 1, characterized in that: The catalyst is a strongly acidic cation exchange resin or tetramethylammonium hydroxide.

3. A high temperature resistant extreme pressure lubricating oil according to claim 2, characterized in that: The strongly acidic cation exchange resin is sulfonated coal or sulfonated styrene cation exchange resin.

4. The high temperature resistant extreme pressure lubricating oil according to claim 1, characterized in that: 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 bentonite by ultrasonic pyrolysis.

5. 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 are mixed at a molar ratio of 1:1.0-1.5, stirred at 200-300 r / min for 20-30 min, a catalyst with a molar ratio of 0.11-0.16 times of methyl trifluoropropyl cyclotrisiloxane is added, stirred at 100-150 r / min for 20-30 min, heated to 115-120° C., reacted for 7-8 h, filtered to obtain a 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 0.2-0.4 mol / dm 3 , add hydrazine hydrate with a mass of 8 to 9 times that of sodium tungstate and bentonite with a mass of 1.1 to 1.5 times that of sodium tungstate, and stir at 300 to 400 r / min for 30 to 40 minutes to obtain a tungsten diselenide precursor; (3) placing a tungsten diselenide precursor solution in an ultrasonic sprayer, transporting it to a reactor via nitrogen, and reacting for 2 to 3 hours to obtain bentonite-modified tungsten diselenide; (4) The bentonite-modified tungsten diselenide is ground in a ball mill, and then added to fluorosilicone oil to obtain a high temperature resistant extreme pressure lubricating oil.

6. The method for preparing a high temperature resistant extreme pressure lubricating oil according to claim 5, characterized in that: In the step (3), the bentonite is prepared by calcining at 450-470° C. for 1-1.5 hours.

7. The method for preparing a high temperature resistant extreme pressure lubricating oil according to claim 5, characterized in that: The frequency of the ultrasonic sprayer in step (3) is 1.7 to 2.0 MHz.

8. The method for preparing a high temperature resistant extreme pressure lubricating oil according to claim 5, characterized in that: The flow rate of nitrogen in step (3) is 1.5-2.0 dm 3 / min.

9. The method for preparing a high temperature resistant extreme pressure lubricating oil according to claim 5, characterized in that: In the step (3), the reactor temperature is 600-700°C.

10. The method for preparing a high temperature resistant extreme pressure lubricating oil according to claim 5, characterized in that: The particle size of the bentonite-modified tungsten diselenide after grinding in the step (4) is 30-40 nm.

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