A lubricating oil thickening factor and a semi-solid lubricant usable in a vacuum environment and a preparation method thereof

Abstract

The present invention provides a lubricating oil thickening factor and a semi-solid lubricant that can be used in a vacuum environment, as well as a preparation method thereof, relating to the technical field of lubricating materials. The lubricating oil thickening factor provided by the present invention has raw materials including an active component, an organic small molecule compound, a nitrate, a polyacid salt, and water; the active component includes n-octylamine and / or oleylamine, the organic small molecule compound includes cyclohexane and / or octadecane, the nitrate includes yttrium nitrate and / or cerium nitrate, and the polyacid salt includes phosphomolybdic acid and / or silicotungstic acid. Adding the lubricating oil thickening factor provided by the present invention to a base lubricating oil can obtain a semi-solid lubricant with low cost and extremely low volatility in a vacuum by a simple method. It has a good lubricating effect under a vacuum (0 to 5×10-3 Pa), has ultra-low friction, and greatly reduces the damage to the friction pair; in addition, the semi-solid form can prevent problems such as the creep and leakage of the lubricating oil.

Description

Technical Field

[0001] The invention relates to the technical field of lubricating materials, and in particular to a lubricating oil thickening factor and a semi-solid lubricant that can be used in a vacuum environment and a preparation method thereof. Background Art

[0002] With the rapid development of aerospace technology, more and more mechanical parts need to operate in a vacuum environment. Compared with traditional lubrication methods, lubrication under vacuum is one of the modern advanced lubrication technologies. Lubrication under vacuum has many advantages, such as good lubrication effect at medium and high temperatures and high speeds, low lubricant dosage, and long equipment service life. However, vacuum conditions also bring some constraints. Due to the extremely low pressure in a vacuum environment, the volatile components in the lubricating material can be easily evaporated, resulting in a gradual decrease in lubrication performance during long-term use. Secondly, if the lubricating material releases gas molecules in a vacuum environment, these gas molecules will contaminate the surface of the device, causing it to lose its finish and affect the performance and life of the device. It is precisely because of these stringent requirements that challenges are brought to solving vacuum lubrication technology problems.

[0003] At present, the commonly used lubricants are liquid lubricants and solid lubricants. Liquid lubricants such as perfluoropolyether (PFPE) have very low vapor pressure and good high temperature resistance; solid lubricants such as molybdenum disulfide (MOS 2 ) Due to its special layered structure, it has high load-bearing capacity and low friction coefficient, and is a commonly used solid lubricant. However, in a vacuum environment, since there is no gas or other impurities to affect the physical and chemical properties of the substance itself, the requirements for materials are usually relatively high. Therefore, vacuum lubrication materials are difficult to select, especially for harsh vacuum conditions. At present, there are few lubricating materials that can meet the lubrication needs of mechanical equipment in a vacuum environment. Summary of the invention

[0004] In view of this, the object of the present invention is to provide a lubricating oil thickening factor and a semi-solid lubricant that can be used in a vacuum environment and a preparation method thereof. The lubricating oil thickening factor provided by the present invention is added to a base lubricating oil, and the obtained semi-solid lubricant is subjected to vacuum (0 to 5×10 -3 Pa) has a good lubrication effect.

[0005] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0006] The invention provides a lubricating oil thickening factor, the preparation raw materials of which include active components, organic small molecule compounds, nitrates, polyacid salts and water; the active components include n-octylamine and / or oleylamine, the organic small molecule compounds include cyclohexane and / or octadecane, the nitrates include yttrium nitrate and / or cerium nitrate, and the polyacid salts include phosphomolybdic acid and / or silicotungstic acid.

[0007] Preferably, the dosage ratio of the active component, the organic small molecule compound, the nitrate, the polyacid salt and water is (1-10) mL: (10-60) mL: (0.1-2) g: (0.1-10) g: (40-80) mL.

[0008] The present invention provides a method for preparing the lubricating oil thickening factor described in the above technical solution, comprising the following steps:

[0009] The active component, the organic small molecule compound, the nitrate, the polyacid and water are mixed to carry out a hydrothermal reaction to obtain the lubricating oil thickening factor.

[0010] Preferably, the temperature of the hydrothermal reaction is 100-210° C., and the time is 4-18 hours.

[0011] Preferably, after the hydrothermal reaction, the obtained oil phase is further washed, and the washing reagent used is at least one of ethanol, n-octane, cyclohexane, chloroform and petroleum ether.

[0012] The present invention provides a semi-solid lubricant that can be used in a vacuum environment, comprising a base lubricating oil and a thickening factor, wherein the thickening factor is the lubricating oil thickening factor described in the above technical solution or the lubricating oil thickening factor prepared by the preparation method described in the above technical solution.

[0013] Preferably, the base lubricant oil comprises one or more of poly-α-olefin, polyalkylated cyclopentane, polysiloxane, silicone oil, silicone hydrocarbon and perfluoropolyether.

[0014] Preferably, the mass ratio of the thickening factor to the base lubricating oil is 1:0.1 to 1:50.

[0015] Preferably, the pressure of the vacuum environment is 0 to 5×10 -3 Pa.

[0016] The present invention provides a method for preparing a semi-solid lubricant that can be used in a vacuum environment as described in the above technical solution, comprising the following steps:

[0017] The thickening factor and the base lubricating oil are stirred and mixed, and then allowed to stand to obtain the semi-solid lubricant that can be used in a vacuum environment.

[0018] The present invention provides a lubricating oil thickening factor, the preparation raw materials include active components, organic small molecule compounds, nitrates, polyacid salts and water; the active components include n-octylamine and / or oleylamine, the organic small molecule compounds include cyclohexane and / or octadecane, the nitrates include yttrium nitrate and / or cerium nitrate, and the polyacid salts include phosphomolybdic acid and / or silicotungstic acid. In the present invention, the lubricating oil thickening factor is combined together by multi-level interaction forces such as van der Waals force, electrostatic interaction and coordination between the active components, organic small molecule compounds, nitrates, polyacid salts and the like.

[0019] The present invention provides a method for preparing the lubricating oil thickening factor described in the above technical solution. The present invention adopts a hydrothermal synthesis method to prepare the lubricating oil thickening factor. The method is green, environmentally friendly, pollution-free, simple to operate, and inexpensive.

[0020] The present invention provides a semi-solid lubricant that can be used in a vacuum environment, comprising a base lubricating oil and a thickening factor, wherein the thickening factor is the lubricating oil thickening factor described in the above technical solution or the lubricating oil thickening factor prepared by the preparation method described in the above technical solution. In the present invention, the thickening factor is combined together by multi-level interaction forces such as van der Waals force, electrostatic interaction, coordination effect, etc. between the components, and then combined with the lubricating oil through strong interaction to form an inseparable whole, so it has good stability in a vacuum environment. At the same time, the thickening factor has low volatility in a vacuum and can exist stably in a vacuum. The present invention provides a semi-solid lubricant with extremely low volatility in a vacuum, which can exist stably in a vacuum environment. In a vacuum (0 to 5×10 -3 Pa), has a good lubrication effect, has ultra-low friction, and greatly reduces the damage to the friction pair; in addition, the semi-solid form can prevent the creep and leakage of lubricating oil, greatly expands the system of vacuum lubrication materials, and promotes the practical application of vacuum lubrication technology. The results of the embodiment show that the semi-solid lubricant provided by the present invention has a good lubrication effect at 2×10 -3 After 30 minutes under Pa vacuum, the mass loss is only 1.23%, and the friction coefficient is stable around 0.08-0.10, so it has good application prospects in the aerospace field.

[0021] The present invention provides a method for preparing the semi-solid lubricant that can be used in a vacuum environment as described in the above technical solution. The present invention only requires stirring and mixing the base lubricating oil and the thickening factor and letting them stand to prepare the semi-solid lubricant. The preparation method is simple, easy to operate, and is conducive to large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a physical picture of the semi-solid lubricant prepared in Example 1;

[0023] Figure 2 This is a curve diagram showing the change of the friction coefficient of the semi-solid lubricant prepared in Example 2 over time;

[0024] Figure 3 This is a curve chart showing the change of the friction coefficient of the semi-solid lubricant prepared in Example 3 over time. DETAILED DESCRIPTION

[0025] The invention provides a lubricating oil thickening factor, the preparation raw materials of which include active components, organic small molecule compounds, nitrates, polyacid salts and water; the active components include n-octylamine and / or oleylamine, the organic small molecule compounds include cyclohexane and / or octadecane, the nitrates include yttrium nitrate and / or cerium nitrate, and the polyacid salts include phosphomolybdic acid and / or silicotungstic acid.

[0026] The raw materials for preparing the lubricating oil thickening factor provided by the present invention preferably include oleylamine, octadecane, cerium nitrate, silicotungstic acid and water, or include oleylamine, cyclohexane, cerium nitrate, phosphomolybdic acid and water, or include n-octylamine, octadecane, yttrium nitrate, silicotungstic acid and water.

[0027] In the present invention, the dosage ratio of the active component, organic small molecule compound, nitrate, polyacid salt and water is preferably (1-10) mL: (10-60) mL: (0.1-2) g: (0.1-10) g: (40-80) mL, more preferably (2-8) mL: (10-40) mL: (0.1-1) g: (0.5-5) g: (50-70) mL, and further preferably (3-5) mL: (12-25) mL: (0.5-0.8) g: (0.5-1.2) g: 60 mL.

[0028] The present invention provides a method for preparing the lubricating oil thickening factor described in the above technical solution, comprising the following steps:

[0029] The active component, the organic small molecule compound, the nitrate, the polyacid and water are mixed to carry out a hydrothermal reaction to obtain the lubricating oil thickening factor.

[0030] The present invention has no special requirements for the mixing method. The components can be evenly mixed using a mixing method well known to those skilled in the art, and an emulsion is formed after the mixing. In the present invention, the temperature of the hydrothermal reaction is preferably 100-210°C, specifically 100°C, 110°C, 120°C, 130°C, 140°C, 150°C, 160°C, 170°C, 180°C, 190°C, 200°C, 210°C, and the time of the hydrothermal reaction is preferably 4-18h, specifically 4h, 6h, 8h, 10h, 12h, 14h, 16h, 18h.

[0031] During the hydrothermal reaction, the thickening factors are combined together through multi-level interaction forces such as van der Waals force, electrostatic interaction, coordination effect, etc. between the components, among which nitrates and polyacid salts undergo a replacement reaction (cations of nitrates react with anions of polyacids) to form a main body, and active components and organic small molecule compounds act as ligands and are combined with the main body through coordination and van der Waals force.

[0032] After the hydrothermal reaction is completed, a mixed system of oil phase and water phase is formed. In the present invention, the water phase is preferably discarded, and the obtained oil phase is washed and centrifuged to obtain the lubricating oil thickening factor; the reagent used in the washing is preferably at least one of ethanol, n-octane, cyclohexane, chloroform and petroleum ether, and the number of washings is preferably 3 times. The present invention removes excess active components and organic small molecule compounds through the washing.

[0033] The present invention adopts a hydrothermal synthesis method to prepare the lubricating oil thickening factor. The method is green, environmentally friendly, pollution-free, simple to operate, cheap and low in cost.

[0034] The present invention provides a semi-solid lubricant that can be used in a vacuum environment, comprising a base lubricating oil and a thickening factor, wherein the thickening factor is the lubricating oil thickening factor described in the above technical solution or the lubricating oil thickening factor prepared by the preparation method described in the above technical solution.

[0035] In the present invention, the base lubricant preferably includes one or more of polyalphaolefin, polyalkylated cyclopentane, polysiloxane, silicone oil, silicone hydrocarbon and perfluoropolyether, and the polyalphaolefin preferably includes one or more of polyalphaolefin-10, polyalphaolefin-20, polyalphaolefin-30 and polyalphaolefin-40. In the present invention, the mass ratio of the thickening factor to the base lubricant is preferably 1:0.1 to 1:50, more preferably 1:1 to 1:25, and further preferably 1:10 to 1:20. In the present invention, the semi-solid lubricant is light yellow.

[0036] In the present invention, the pressure of the vacuum environment is preferably 0 to 5×10 -3 Pa, more preferably 1×10 -4 ~2×10 -3 Pa. The semi-solid lubricant provided by the present invention can exist stably in a vacuum environment, has extremely low volatility, has a good lubrication effect in a vacuum environment, and can reduce damage to the friction pair; at the same time, the semi-solid form can effectively solve the problems of lubricating oil creep and leakage, thereby reducing the wear on mechanical parts and extending the service life of the machine.

[0037] The present invention provides a method for preparing a semi-solid lubricant that can be used in a vacuum environment as described in the above technical solution, comprising the following steps:

[0038] The thickening factor and the base lubricating oil are stirred and mixed, and then allowed to stand to obtain the semi-solid lubricant that can be used in a vacuum environment.

[0039] In the present invention, the thickening factor is preferably added to the base lubricating oil for stirring and mixing. In the present invention, the stirring speed of the stirring and mixing is preferably 20 to 300 r / min, the stirring time is preferably 1 to 20 min, and the standing time is preferably 0.5 to 2 h.

[0040] The semi-solid lubricant can be prepared by simply mixing the base lubricating oil and the thickening factor and letting them stand. The preparation method is simple, easy to operate and conducive to large-scale production.

[0041] In order to further illustrate the present invention, the lubricating oil thickening factor and the semi-solid lubricant usable in a vacuum environment and the preparation method provided by the present invention are described in detail below in conjunction with examples, but they should not be construed as limiting the scope of protection of the present invention.

[0042] Example 1

[0043] 5 mL of oleylamine, 15 mL of octadecane, 0.8 g of cerium nitrate, 0.5 g of silicotungstic acid and 60 mL of water were mixed, subjected to hydrothermal reaction at 180° C. for 12 h, and the oil phase product was washed with ethanol and chloroform and centrifuged to obtain a thickening factor.

[0044] 0.5 g of the thickening factor was added as an additive to 7.5 g of silicone oil (base lubricant), wherein the mass ratio of the thickening factor to the base lubricant was 1:15, and then the mixture was fully stirred and allowed to stand to obtain a semi-solid lubricant.

[0045] Figure 1 This is a physical picture of the semi-solid lubricant prepared in Example 1.

[0046] Example 2

[0047] 5 mL of oleylamine, 25 mL of cyclohexane, 0.1 g of cerium nitrate, 1 g of phosphomolybdic acid and 40 mL of water were mixed, subjected to a hydrothermal reaction at 160° C. for 10 h, and then the oil phase product was washed and centrifuged with a mixed solution of ethanol and n-octane (the volume ratio of ethanol to n-octane was 1:5) to obtain a thickening factor.

[0048] 1 g of the above thickening factor was added as an additive to 10 g of perfluoropolyether (base lubricant), wherein the mass ratio of the thickening factor to the base lubricant was 1:10, and then the mixture was fully stirred and allowed to stand to obtain a semi-solid lubricant.

[0049] Example 3

[0050] 3 mL of n-octylamine, 12 mL of octadecane, 0.5 g of yttrium nitrate, 1.2 g of silicotungstic acid and 60 mL of water were mixed, subjected to a hydrothermal reaction at 200° C. for 8 h, and then the oil phase product was washed with petroleum ether and cyclohexane and centrifuged to obtain a thickening factor.

[0051] 0.5 g of the thickening factor was added as an additive to 10 g of poly-α-olefin-20 (base lubricant), wherein the mass ratio of the thickening factor to the base lubricant was 1:20, and then the mixture was fully stirred and allowed to stand to obtain a semi-solid lubricant.

[0052] The semi-solid lubricants prepared in Examples 1 to 3 were subjected to vacuum tribological performance tests using a vacuum friction and wear tester (VFBT-4000) with four-ball friction, and the friction pair was a steel ball (GCr15) with a diameter of 12.7 mm. Before the experiment, the steel ball was ultrasonically treated in petroleum ether and acetone for 15 minutes. The friction test was carried out at 2×10 -3 Pa vacuum environment for 30 minutes, the test load is 200N, the speed is 1200±10r / min. The test results are as follows:

[0053] The semi-solid lubricant prepared in Example 1 is stable at around 0.08.

[0054] Figure 2 The friction coefficient of the semi-solid lubricant prepared in Example 2 changes with time. Figure 2 It can be seen that the friction coefficient of the semi-solid lubricant of Example 2 is around 0.07 and then stabilizes at around 0.10.

[0055] Figure 3 The friction coefficient of the semi-solid lubricant prepared in Example 3 changes with time. Figure 3 It can be seen that the friction coefficient of the semi-solid lubricant of Example 3 is around 0.07 and then stabilizes at around 0.10.

[0056] The semisolid lubricant prepared in Example 3 was placed in a 2×10 -3 The mass loss was only 1.23% under vacuum at Pa for 30 min.

[0057] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be regarded as the protection scope of the present invention.

Claims

1. A lubricating oil thickening factor, characterized in that: The preparation raw materials include active components, organic small molecule compounds, nitrates, polyacid salts and water; the active components include n-octylamine and / or oleylamine, the organic small molecule compounds include cyclohexane and / or octadecane, the nitrates include yttrium nitrate and / or cerium nitrate, and the polyacid salts include phosphomolybdic acid and / or silicotungstic acid; the dosage ratio of the active components, organic small molecule compounds, nitrates, polyacid salts and water is (1-10) mL: (10-60) mL: (0.1-2) g: (0.1-10) g: (40-80) mL; The method for preparing the lubricating oil thickening factor comprises the following steps: The active component, organic small molecule compound, nitrate, polyacid and water are mixed for hydrothermal reaction to obtain the lubricating oil thickening factor; the temperature of the hydrothermal reaction is 100-210° C. and the time is 4-18 hours.

2. The method for preparing the lubricating oil thickening factor according to claim 1, characterized in that: The following steps are involved: The active component, organic small molecule compound, nitrate, polyacid and water are mixed for hydrothermal reaction to obtain the lubricating oil thickening factor; the temperature of the hydrothermal reaction is 100-210° C. and the time is 4-18 hours.

3. The preparation method according to claim 2, characterized in that: After the hydrothermal reaction, the obtained oil phase is washed, and the washing reagent is at least one of ethanol, n-octane, cyclohexane, chloroform and petroleum ether.

4. A semi-solid lubricant that can be used in a vacuum environment, characterized in that: The invention comprises a base lubricating oil and a thickening factor, wherein the thickening factor is the lubricating oil thickening factor according to claim 1 or the lubricating oil thickening factor prepared by the preparation method according to any one of claims 2 to 3; the pressure of the vacuum environment is 0 to 5×10 -3 Pa.

5. The semi-solid lubricant according to claim 4, characterized in that The base lubricating oil comprises one or more of poly-α-olefin, polyalkylated cyclopentane, polysiloxane, silicone oil, silicone hydrocarbon and perfluoropolyether.

6. The semi-solid lubricant according to claim 4 or 5, characterized in that: The mass ratio of the thickening factor to the base lubricating oil is 1:0.1 to 1:

50.

7. The method for preparing a semi-solid lubricant that can be used in a vacuum environment according to any one of claims 4 to 6, characterized in that: The following steps are involved: The thickening factor and the base lubricating oil are stirred and mixed, and then allowed to stand to obtain the semi-solid lubricant that can be used in a vacuum environment.

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