Synthetic ester wind power gear oil base oil and preparation method thereof

Abstract

The invention relates to the technical field of wind power gear oil, in particular to synthetic ester wind power gear oil base oil and a preparation method thereof, and the synthetic ester wind power gear oil base oil is prepared according to the following steps: mixing neopentyl polyol, dicarboxylic acid, monobasic fatty alcohol and monobasic carboxylic acid according to a specific proportion and sequence, adopting inert gas as a water-carrying agent and shielding gas, and reacting at the temperature of 60-80 DEG C for 1-2 hours to obtain the synthetic ester wind power gear oil base oil. And carrying out esterification reaction under the action of a tin-based esterification catalyst, and carrying out liquid-solid separation on the esterification product and the catalyst while the esterification product is hot. The synthetic ester wind power gear oil base oil disclosed by the invention has excellent viscosity-temperature performance, low-temperature performance and biodegradability, belongs to environment-friendly lubricating oil base oil, and can meet the lubrication protection requirements under harsh working conditions; the problems that existing special gear oil for wind power generation is insufficient in comprehensive performance, short in service life, prone to causing environmental pollution and the like can be effectively solved.

Description

Technical Field

[0001] The invention relates to the technical field of wind power gear oil, and relates to a synthetic ester wind power gear oil base oil and a preparation method thereof. Background Art

[0002] Since large-scale wind power bases are usually built in remote areas with rich wind energy resources such as mountains, deserts, Gobi, and beaches, wind turbines are easily affected by the different climate conditions in various regions when they are in outdoor service for a long time. The variable speed gearbox, as the core transmission system of power transmission, needs to withstand the changes in ambient temperature and wind speed load during actual operation, which directly determines the working efficiency and service life of wind turbines. Relevant surveys show that about half of the unit's shutdown failures come from the failure of the gearbox. Inconvenient transportation leads to high difficulty and risk factors in disassembly, maintenance, and oil change operations. Frequent oil changes will also increase labor costs. Therefore, choosing the right gear oil to lubricate and maintain the variable speed gearbox is of great significance to ensure the safe and stable operation of wind turbines, extend the service life of equipment, reduce operation and maintenance costs, and improve the economic benefits of enterprises.

[0003] Wind power gear oil generally needs to have excellent viscosity-temperature performance and low-temperature fluidity, provide effective lubrication protection for gears in a wide operating temperature range, be able to adapt to the cold start environment, have strong thermal oxidation stability, inhibit the formation of sludge and foam, and have a long oil change cycle. The grades of gear oil are mainly divided according to viscosity. Kinematic viscosity is an important indicator for measuring the strength and fluidity of oil film. Appropriate lubricant viscosity is conducive to the protection of the gear system. In view of the low-speed and heavy-load working characteristics of the speed change gearbox, gear oil with a viscosity grade of ISO VG320 is currently generally selected. High-viscosity lubricants are conducive to the formation of thicker dynamic pressure oil films, which can withstand larger loads and reduce tooth surface wear.

[0004] In wind power gear oil, the base oil component accounts for more than 95wt%, so the quality of the base oil largely determines the performance of the gear oil. At present, wind power gear oil mainly includes mineral-based lubricants and synthetic hydrocarbon lubricants. Traditional mineral-based lubricants are limited by performance. Although they are cheap, they have a short service life and cannot meet the use requirements under harsh working conditions. Synthetic hydrocarbon lubricants have poor compatibility with sealing materials and will inevitably leak and discharge into the natural environment during equipment operation and oil changes. The difficulty in degradation of mineral oil and synthetic hydrocarbons will cause nearby water bodies and soil to be polluted. Ester synthetic oils have excellent anti-wear and lubricating properties and are biodegradable. They are generally used as blending components in the field of lubricants, but their application as base oils for wind power gear oils is not common. Most synthetic ester base oils can only reach low viscosity levels, and research and reports on high-viscosity and high-performance synthetic esters are relatively scarce.

[0005] A Chinese patent document with publication number CN102766504B discloses an industrial gear lubricant composition that resists micropitting, wherein the base oil comprises at least one deeply refined mineral oil, which is then formulated with a variety of additives. Although the gear oil described in the application has good anti-wear, anti-micropitting and antioxidant properties, it does not reflect whether its low-temperature performance can meet the harsh working environment requirements of wind turbines. Moreover, it contains mineral oil components that are difficult to biodegrade, and still cannot avoid the risk of polluting the ecological environment.

[0006] A Chinese patent document with announcement number CN102041148B discloses a synthetic gear oil for wind power generation. The gear oil is mainly based on dibasic acid pentaerythritol complex ester as a base oil, and is prepared by blending one or more dibasic acid pentaerythritol C5 to C18 complex esters with industrial gear oil composite additives and an appropriate amount of anti-foaming agent in a required proportion. The gear oil has a long service life, improved compatibility with sealing materials, and is biodegradable and will not cause pollution to the environment. However, the design of its ester molecular structure is not entirely reasonable, and its viscosity-temperature performance and hydrolysis stability are poor, and there are certain limitations.

[0007] It can be seen that the wind power gear oil involved in the above patent documents still has technical problems to be solved, such as poor overall performance, short service life and difficulty in biodegradation. Summary of the invention

[0008] The present invention provides a synthetic ester wind power gear oil base oil and a preparation method thereof, which overcomes the above-mentioned deficiencies of the prior art and can effectively solve the problem of poor comprehensive performance of the existing wind power gear oil.

[0009] One of the technical solutions of the present invention is achieved by the following measures: A method for preparing a synthetic ester wind power gear oil base oil is carried out according to the following method: S1, mixing a required amount of dicarboxylic acid and monohydric fatty alcohol, introducing an inert gas as a water-carrying agent and a protective gas, and causing an esterification reaction under the action of an esterification catalyst to obtain a mixed dicarboxylic acid monoester; S2, adding a required amount of neopentyl polyol and monocarboxylic acid to the mixed dicarboxylic acid monoester and mixing, introducing an inert gas as a water-carrying agent and a protective gas, and continuing the esterification reaction under the action of an esterification catalyst to obtain an esterification product containing a composite polyol ester; S3, separating and refining the esterification product containing the complex polyol ester to obtain a synthetic ester wind power gear oil base oil.

[0010] The following is a further optimization and / or improvement of one of the above-mentioned technical solutions: In the above step S1, the dicarboxylic acid is one or more dicarboxylic acids with a carbon chain length of C4 to C10, and the monohydric fatty alcohol is one or more normal straight-chain or isomeric branched monohydric fatty alcohols with a carbon chain length of C4 to C12.

[0011] In the above step S1, the dicarboxylic acid is one or more of glutaric acid, adipic acid and azelaic acid, and the monohydric fatty alcohol is one or more of 2-ethylhexanol, 6-methylheptanol and 2-octanol.

[0012] In the above step S2, the neopentyl polyol is one or more of neopentyl glycol, trimethylolpropane, and pentaerythritol, and the monocarboxylic acid is one or more of normal straight-chain or isomeric branched monocarboxylic acids with a carbon chain length of C5 to C18.

[0013] In the above step S2, the neopentyl polyol is pentaerythritol, and the monocarboxylic acid is one or more of n-octanoic acid, n-nonanoic acid and 2-ethylhexanoic acid.

[0014] In the above step S1, the molar ratio of the dicarboxylic acid to the monohydric fatty alcohol is (1.0 to 1.2):1.

[0015] In the above step S1, the molar ratio of the dicarboxylic acid to the monohydric fatty alcohol is 1:1.

[0016] In the above step S2, the molar ratio of neopentyl polyol, monocarboxylic acid and mixed dicarboxylic acid monoester is 1:(1.5 to 2.5):(1.5 to 2.0).

[0017] In the above step S2, the molar ratio of neopentyl polyol, monocarboxylic acid and mixed dicarboxylic acid monoester is 1:(2.25 to 2.45):(1.55 to 1.75).

[0018] In the above steps S1 and S2, the inert gas is one of nitrogen, argon and carbon dioxide; in step S1, based on the total mass of the added reaction materials (dicarboxylic acid and monohydric fatty alcohol), the purge flow rate of the inert gas introduced into each gram of the reaction materials is 1.0 mL / min to 3.0 mL / min; in step S2, based on the total mass of the added reaction materials (mixed dicarboxylic acid monoester, neopentyl polyol and monocarboxylic acid), the purge flow rate of the inert gas introduced into each gram of the reaction materials is 1.0 mL / min to 3.0 mL / min.

[0019] In the above steps S1 and S2, the inert gas is nitrogen; in step S1, based on the total mass of the added reaction materials (dicarboxylic acid and monohydric fatty alcohol), the purge flow rate of the inert gas introduced into each gram of the reaction materials is 2.0 mL / min; in step S2, based on the total mass of the added reaction materials (mixed dicarboxylic acid monoester, neopentyl polyol and monocarboxylic acid), the purge flow rate of the inert gas introduced into each gram of the reaction materials is 2.0 mL / min.

[0020] In the above steps S1 and S2, the esterification catalyst is a tin-based esterification catalyst, and is one of stannous oxide, tin dioxide, stannous chloride, tin tetrachloride, stannous sulfate, stannous octoate and stannous oxalate; in step S1, the amount of the esterification catalyst added is 1.0wt% to 2.0wt% of the total mass of the reaction materials (dicarboxylic acid and monohydric fatty alcohol) added in step S1; in step S2, the amount of the esterification catalyst added is 1.0wt% to 2.0wt% of the total mass of the reaction materials (mixed dicarboxylic acid monoester, neopentyl polyol and monocarboxylic acid) added in step S2.

[0021] In the above steps S1 and S2, the esterification catalyst is stannous oxide; in step S1, the amount of the esterification catalyst added is 1.2wt% to 1.5wt% of the total mass of the reaction materials (dicarboxylic acid and monohydric fatty alcohol) added in step S1; in step S2, the amount of the esterification catalyst added is 1.2wt% to 1.5wt% of the total mass of the reaction materials (mixed dicarboxylic acid monoester, neopentyl polyol and monocarboxylic acid) added in step S2.

[0022] In the above step S1, the temperature of the esterification reaction is 150°C to 170°C, and the reaction time is 1h to 2h. In the step S2, the temperature of the esterification reaction is 160°C to 180°C, and the reaction time is 6h to 8h.

[0023] In the above step S1, the temperature of the esterification reaction is 155°C to 165°C, and the reaction time is 1.5 hours. In the step S2, the temperature of the esterification reaction is 170°C to 180°C, and the reaction time is 7 hours.

[0024] In the above steps S1 and S2, the esterification reaction is carried out under mechanical stirring at a stirring rate of 500 r / min to 700 r / min.

[0025] In the above steps S1 and S2, the esterification reaction is carried out under mechanical stirring at a stirring rate of 600 r / min to 700 r / min.

[0026] In the above step S3, the separation and purification is one of centrifugation, suction filtration and pressure filtration, and the temperature during separation is 120°C to 160°C.

[0027] In the above step S3, the separation and purification is performed by suction filtration, and the temperature during separation is 140°C to 150°C.

[0028] The second technical solution of the present invention is achieved through the following measures: a synthetic ester wind power gear oil base oil is obtained by a preparation method of a synthetic ester wind power gear oil base oil.

[0029] The synthetic ester wind power gear oil base oil of the present invention has excellent viscosity-temperature performance, low temperature performance and biodegradability, is an environmentally friendly lubricant base oil, can meet the lubrication and protection requirements under harsh working conditions, and can effectively solve the problems of insufficient comprehensive performance, short service life and easy environmental pollution in existing wind power generation special gear oils. DETAILED DESCRIPTION

[0030] The present invention is not limited by the following embodiments, and specific implementation methods can be determined according to the technical scheme of the present invention and actual conditions. Unless otherwise specified, the various chemical reagents and chemicals mentioned in the present invention are all known and commonly used chemical reagents and chemicals in the prior art; the percentages in the present invention are all mass percentages unless otherwise specified.

[0031] The present invention will be further described below in conjunction with embodiments: Example 1: The preparation method of the synthetic ester wind power gear oil base oil is carried out according to the following method: S1, mixing a dicarboxylic acid and a monohydric fatty alcohol in a certain proportion, introducing an inert gas as a water-carrying agent and a protective gas, and causing an esterification reaction under the action of an esterification catalyst to obtain a mixed dicarboxylic acid monoester; S2, mixing neopentyl polyol, monocarboxylic acid and mixed dicarboxylic acid monoester in proportion, introducing inert gas as a water-carrying agent and protective gas, and continuing esterification reaction under the action of an esterification catalyst to obtain an esterification product containing a composite polyol ester; S3, separating and refining the esterification product containing the complex polyol ester to obtain a synthetic ester wind power gear oil base oil.

[0032] Example 2: As an optimization of the above example, in step S1, the dicarboxylic acid is one or more dicarboxylic acids with a carbon chain length of C4 to C10, and the monohydric fatty alcohol is one or more normal straight-chain or isomeric branched monohydric fatty alcohols with a carbon chain length of C4 to C12.

[0033] Example 3: As an optimization of the above example, in step S1, the dicarboxylic acid is one or more of glutaric acid, adipic acid and azelaic acid, and the monohydric fatty alcohol is one or more of 2-ethylhexanol, 6-methylheptanol and octanol.

[0034] Example 4: As an optimization of the above example, in step S2, the neopentyl polyol is one or more of neopentyl glycol, trimethylolpropane, and pentaerythritol, and the monocarboxylic acid is one or more of normal straight-chain or isomeric branched monocarboxylic acids with a carbon chain length of C5 to C18.

[0035] Embodiment 5: As an optimization of the above embodiment, in step S2, the neopentyl polyol is pentaerythritol, and the monocarboxylic acid is one or more of n-octanoic acid, n-nonanoic acid and 2-ethylhexanoic acid.

[0036] Example 6: As an optimization of the above example, in step S1, the molar ratio of the dicarboxylic acid to the monohydric fatty alcohol is (1.0 to 1.2):1.

[0037] Example 7: As an optimization of the above example, in step S1, the molar ratio of the dicarboxylic acid to the monohydric fatty alcohol is 1:1.

[0038] Example 8: As an optimization of the above example, in step S2, the molar ratio of neopentyl polyol, monocarboxylic acid and mixed dicarboxylic acid monoester is 1:(1.5 to 2.5):(1.5 to 2.0).

[0039] Example 9: As an optimization of the above example, in step S2, the molar ratio of neopentyl polyol, monocarboxylic acid and mixed dicarboxylic acid monoester is 1:(2.25 to 2.45):(1.55 to 1.75).

[0040] Example 10: As an optimization of the above example, in steps S1 and S2, the inert gas is one of nitrogen, argon and carbon dioxide; in step S1, based on the total mass of the added reaction materials (dicarboxylic acid and monohydric fatty alcohol), the purge flow rate of the inert gas introduced into each gram of the reaction materials is 1.0 mL / min to 3.0 mL / min; in step S2, based on the total mass of the added reaction materials (mixed dicarboxylic acid monoester, neopentyl polyol and monocarboxylic acid), the purge flow rate of the inert gas introduced into each gram of the reaction materials is 1.0 mL / min to 3.0 mL / min.

[0041] Example 11: As an optimization of the above example, in steps S1 and S2, the inert gas is nitrogen; in step S1, based on the total mass of the added reaction materials (dicarboxylic acid and monohydric fatty alcohol), the purge flow rate of the inert gas introduced into each gram of the reaction materials is 2.0 mL / min; in step S2, based on the total mass of the added reaction materials (mixed dicarboxylic acid monoester, neopentyl polyol and monocarboxylic acid), the purge flow rate of the inert gas introduced into each gram of the reaction materials is 2.0 mL / min.

[0042] Example 12: As an optimization of the above example, in steps S1 and S2, the esterification catalyst is a tin-based esterification catalyst, and is one of stannous oxide, tin dioxide, stannous chloride, tin tetrachloride, stannous sulfate, stannous octoate and stannous oxalate; in step S1, the amount of the esterification catalyst added is 1.0wt% to 2.0wt% of the total mass of the reaction materials (dicarboxylic acid and monohydric fatty alcohol) added in step S1; in step S2, the amount of the esterification catalyst added is 1.0wt% to 2.0wt% of the total mass of the reaction materials (mixed dicarboxylic acid monoester, neopentyl polyol and monocarboxylic acid) added in step S2.

[0043] Example 13: As an optimization of the above example, in steps S1 and S2, the esterification catalyst is stannous oxide; in step S1, the amount of the esterification catalyst added is 1.2wt% to 1.5wt% of the total mass of the reaction materials (dicarboxylic acid and monohydric fatty alcohol) added in step S1; in step S2, the amount of the esterification catalyst added is 1.2wt% to 1.5wt% of the total mass of the reaction materials (mixed dicarboxylic acid monoester, neopentyl polyol and monocarboxylic acid) added in step S2.

[0044] Example 14: As an optimization of the above example, in step S1, the temperature of the esterification reaction is 150°C to 170°C, and the reaction time is 1h to 2h. In step S2, the temperature of the esterification reaction is 160°C to 180°C, and the reaction time is 6h to 8h.

[0045] Example 15: As an optimization of the above example, in step S1, the temperature of the esterification reaction is 155°C to 165°C, and the reaction time is 1.5 hours. In step S2, the temperature of the esterification reaction is 170°C to 180°C, and the reaction time is 7 hours.

[0046] Example 16: As an optimization of the above example, in steps S1 and S2, the esterification reaction is carried out under mechanical stirring at a stirring rate of 500 r / min to 700 r / min.

[0047] Example 17: As an optimization of the above example, in steps S1 and S2, the esterification reaction is carried out under mechanical stirring, and the stirring rate is 600 r / min to 700 r / min.

[0048] Example 18: As an optimization of the above example, in step S3, separation and purification is one of centrifugation, suction filtration and pressure filtration, and the temperature during separation is 120°C to 160°C.

[0049] Example 19: As an optimization of the above example, in step S3, the separation and purification is performed by suction filtration, and the temperature during separation is 140°C to 150°C.

[0050] Compared with the prior art, the present invention has the following beneficial effects: The present invention obtains a synthetic ester wind power gear oil base oil with excellent performance by mixing neopentyl polyol, dicarboxylic acid, monohydric fatty alcohol and monocarboxylic acid in a specific ratio and order, using inert gas as a water-carrying agent and a protective gas, carrying out an esterification reaction under the action of a tin-based esterification catalyst, and then separating the reaction product from the catalyst while hot, and obtaining a synthetic ester wind power gear oil base oil with a kinematic viscosity of 293.77 mm at 40°C. 2 / s to 339.16mm 2 / s, viscosity index not less than 162, pour point not higher than -33℃.

[0051] Compared with the prior art, the synthetic ester wind power gear oil base oil of the present invention has good viscosity-temperature performance, low temperature performance, hydrolysis stability, thermal oxidation stability and biodegradability, and is an environmentally friendly lubricant base oil. Its rich polar ester groups can be adsorbed on the metal surface to form a firm and lasting interface oil film, which can significantly reduce the wear and abrasion of bearings and tooth surfaces, and has good solubility and low ecotoxicity, can improve the miscibility with other composite additives, and can also dissolve the primary oxidation products in oil products and additives, greatly reduce the generation rate of sludge, and can maintain a long service life under harsh working conditions. It can effectively solve the problems of insufficient performance, short service life and easy environmental pollution existing in the current wind power gear oil, and can provide good lubrication protection for the main gearbox of the wind turbine generator set, ensure the normal operation of the gear transmission device of large heavy-duty machinery, and improve the transmission and conversion efficiency of wind energy.

[0052] The preparation method of the synthetic ester wind power gear oil base oil provided by the present invention is a combined preparation process by adopting a heterogeneous esterification catalytic reaction system, inert gas instead of organic solvent as a water-carrying agent and protective gas, and a simple esterification product separation and purification process, which effectively avoids the disadvantages of complex product post-processing procedures, high waste emissions, serious equipment corrosion and environmental pollution, and harm to the health of operators in the traditional esterification production process.

[0053] Example 20: The preparation method of the synthetic ester wind power gear oil base oil is carried out according to the following method: S1, in a reactor equipped with a stirring device, a condensation water separator, a thermometer and a carrier gas conduit, adipic acid, azelaic acid and 2-ethylhexanol in a molar ratio of 0.50:0.50:1 are mixed, nitrogen is used as a water-carrying agent and a protective gas, based on the total mass of the added reaction materials (adipic acid, azelaic acid and 2-ethylhexanol), 1.5wt% of stannous oxide is added to the total mass of the reaction materials, 2.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 160°C for reaction for 1.5h to obtain a mixed dicarboxylic acid monoester; S2, pentaerythritol, n-octanoic acid and mixed dicarboxylic acid monoesters in a molar ratio of 1:2.5:1.5 are mixed, 1.5 wt% of stannous oxide is added to the total mass of the reaction materials (pentaerythritol and n-octanoic acid), 2.0 mL / min of nitrogen is introduced into each gram of the reaction materials for purging and a stirring rate of 600 r / min is maintained, and after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 180° C. and the reaction is carried out for 7.0 h to obtain an esterification product containing a composite polyol ester; S3, cooling the esterification product containing the complex polyol ester to 150° C. and filtering and separating the product to obtain a synthetic ester wind power gear oil base oil.

[0054] Example 21: The preparation method of the synthetic ester wind power gear oil base oil is carried out according to the following method: S1, in a reactor equipped with a stirring device, a condensation water separator, a thermometer and a carrier gas conduit, adipic acid, azelaic acid and 2-ethylhexanol in a molar ratio of 0.8:0.2:1 are mixed, nitrogen is used as a water-carrying agent and a protective gas, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (adipic acid, azelaic acid and 2-ethylhexanol), 2.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 160°C for reaction for 1.5h to obtain a mixed dicarboxylic acid monoester; S2, pentaerythritol, octanoic acid and mixed dicarboxylic acid monoesters in a molar ratio of 1:2.35:1.65 are mixed, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (pentaerythritol and octanoic acid), 2.0mL / min of nitrogen is introduced into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, and after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 180°C and the reaction is carried out for 7.0h to obtain an esterification product containing a composite polyol ester; S3, cooling the esterification product containing the complex polyol ester to 160° C. and filtering and separating the product to obtain a synthetic ester wind power gear oil base oil.

[0055] Example 22: The preparation method of the synthetic ester wind power gear oil base oil is carried out according to the following method: S1, in a reactor equipped with a stirring device, a condensation water separator, a thermometer and a carrier gas conduit, adipic acid, glutaric acid and 2-ethylhexanol in a molar ratio of 0.75:0.25:1 are mixed, nitrogen is used as a water-carrying agent and a protective gas, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (adipic acid, glutaric acid and 2-ethylhexanol), 2.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 160°C for reaction for 1.5h to obtain a mixed dicarboxylic acid monoester; S2, pentaerythritol, n-octanoic acid and mixed dicarboxylic acid monoesters in a molar ratio of 1:2.27:1.73 are mixed, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (pentaerythritol and n-octanoic acid), 2.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, and after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 170°C and react for 6.0h to obtain an esterification product containing a composite polyol ester; S3, cooling the esterification product containing the complex polyol ester to 120° C. and filtering and separating the product to obtain a synthetic ester wind power gear oil base oil.

[0056] Example 23: The preparation method of the synthetic ester wind power gear oil base oil is carried out according to the following method: S1, in a reactor equipped with a stirring device, a condensation water separator, a thermometer and a carrier gas conduit, adipic acid, azelaic acid and 2-ethylhexanol in a molar ratio of 0.75:0.25:1 are mixed, nitrogen is used as a water-carrying agent and a protective gas, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (adipic acid, azelaic acid and 2-ethylhexanol), 2.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 160°C for reaction for 1.5h to obtain a mixed dicarboxylic acid monoester; S2, pentaerythritol, n-nonanoic acid and mixed dicarboxylic acid monoesters in a molar ratio of 1:2.4:1.6 are mixed, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (pentaerythritol and n-nonanoic acid), 2.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 180°C and the reaction is carried out for 7.0h to obtain an esterification product containing a composite polyol ester; S3, cooling the esterification product containing the complex polyol ester to 150° C. and filtering and separating the product to obtain a synthetic ester wind power gear oil base oil.

[0057] Example 24: The preparation method of the synthetic ester wind power gear oil base oil is carried out according to the following method: S1, in a reactor equipped with a stirring device, a condensation water separator, a thermometer and a carrier gas conduit, adipic acid, azelaic acid and octanol in a molar ratio of 0.75:0.25:1 are mixed, nitrogen is used as a water-carrying agent and a protective gas, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (adipic acid, azelaic acid and octanol), 1.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 170°C for reaction for 1.0h to obtain a mixed dicarboxylic acid monoester; S2, pentaerythritol, 2-ethylhexanoic acid and mixed dicarboxylic acid monoesters in a molar ratio of 1:2:2 are mixed, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (pentaerythritol and 2-ethylhexanoic acid), 1.0mL / min of nitrogen is introduced into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 180°C and the reaction is carried out for 8.0h to obtain an esterification product containing a composite polyol ester; S3, cooling the esterification product containing the complex polyol ester to 160° C. and filtering and separating the product to obtain a synthetic ester wind power gear oil base oil.

[0058] Example 25: The preparation method of the synthetic ester wind power gear oil base oil is carried out according to the following method: S1, in a reactor equipped with a stirring device, a condensation water separator, a thermometer and a carrier gas conduit, adipic acid, azelaic acid and 2-ethylhexanol in a molar ratio of 0.75:0.25:1 are mixed, nitrogen is used as a water-carrying agent and a protective gas, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (adipic acid, azelaic acid and 2-ethylhexanol), 3.0mL / min of nitrogen is passed into each gram of the reaction material for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 160°C and the reaction is reacted for 2.0h to obtain a mixed dicarboxylic acid monoester; S2, pentaerythritol, trimethylolpropane, n-octanoic acid and mixed dicarboxylic acid monoesters in a molar ratio of 0.67:0.33:1.835:1.835 are mixed, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (pentaerythritol, trimethylolpropane and n-octanoic acid), 3.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 180°C and the reaction is carried out for 7.0h to obtain an esterification product containing a composite polyol ester; S3, cooling the esterification product containing the complex polyol ester to 150° C. and filtering and separating the product to obtain a synthetic ester wind power gear oil base oil.

[0059] Example 26: The preparation method of the synthetic ester wind power gear oil base oil is carried out according to the following method: S1, in a reactor equipped with a stirring device, a condensation water separator, a thermometer and a carrier gas conduit, adipic acid, azelaic acid and 2-ethylhexanol in a molar ratio of 0.96:0.24:1 are mixed, nitrogen is used as a water-carrying agent and a protective gas, 1.0wt% of stannous oxide is added to the total mass of the reaction materials (adipic acid, azelaic acid and 2-ethylhexanol), 2.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 160°C and the reaction is reacted for 1.5h to obtain a mixed dicarboxylic acid monoester; S2, pentaerythritol, n-octanoic acid and mixed dicarboxylic acid monoesters in a molar ratio of 1:2.46:1.54 are mixed, 1.0 wt% of stannous oxide is added to the total mass of the reaction materials (pentaerythritol and n-octanoic acid), 2.0 mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600 r / min is maintained, and after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 170° C. and the reaction is carried out for 6.0 hours to obtain an esterification product containing a composite polyol ester; S3, cooling the esterification product containing the complex polyol ester to 120° C. and filtering and separating the product to obtain a synthetic ester wind power gear oil base oil.

[0060] Example 27: The preparation method of the synthetic ester wind power gear oil base oil is carried out according to the following method: S1, in a reactor equipped with a stirring device, a condensation water separator, a thermometer and a carrier gas conduit, adipic acid, azelaic acid and 2-ethylhexanol in a molar ratio of 0.88:0.22:1 are mixed, nitrogen is used as a water-carrying agent and a protective gas, 2.0wt% of stannous oxide is added to the total mass of the reaction materials (adipic acid, azelaic acid and 2-ethylhexanol), 2.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 150°C for reaction for 1.0h to obtain a mixed dicarboxylic acid monoester; S2, pentaerythritol, n-octanoic acid and mixed dicarboxylic acid monoesters in a molar ratio of 1:2.46:1.54 are mixed, 2.0wt% of stannous oxide is added to the total mass of the reaction materials (pentaerythritol and n-octanoic acid), 2.0mL / min of nitrogen is introduced into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, and after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 180°C and the reaction is carried out for 7.0h to obtain an esterification product containing a composite polyol ester; S3, cooling the esterification product containing the complex polyol ester to 140° C. and filtering and separating the product to obtain a synthetic ester wind power gear oil base oil.

[0061] Example 28: The preparation method of the synthetic ester wind power gear oil base oil is carried out according to the following method: S1, in a reactor equipped with a stirring device, a condensation water separator, a thermometer and a carrier gas conduit, adipic acid, azelaic acid and 2-ethylhexanol in a molar ratio of 0.8:0.2:1 are mixed, nitrogen is used as a water-carrying agent and a protective gas, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (adipic acid, azelaic acid and 2-ethylhexanol), 2.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 160°C and the reaction is reacted for 2.0h to obtain a mixed dicarboxylic acid monoester; S2, pentaerythritol, neopentyl glycol, n-octanoic acid and mixed dicarboxylic acid monoesters in a molar ratio of 0.75:0.25:1.5:2.0 are mixed, 1.5wt% of stannous oxide is added to the total mass of the reaction materials (pentaerythritol, neopentyl glycol and n-octanoic acid), 2.0mL / min of nitrogen is passed into each gram of the reaction materials for purging and a stirring rate of 600r / min is maintained, after the reaction materials are evenly mixed, the reaction temperature is controlled to rise to 160°C and the reaction is carried out for 8.0h to obtain an esterification product containing a composite polyol ester; S3, cooling the esterification product containing the complex polyol ester to 150° C. and filtering and separating the product to obtain a synthetic ester wind power gear oil base oil.

[0062] Example 29: The properties of the synthetic ester wind power gear oil base oil prepared in Examples 20 to 28 of the present invention, including kinematic viscosity, viscosity index and pour point, were evaluated, and the evaluation results are shown in Table 1. As can be seen from Table 1, the kinematic viscosity of the synthetic ester wind power gear oil base oil obtained by the preparation method of Examples 20 to 28 of the present invention has reached the viscosity grade of ISO VG320 wind power gear oil, and its kinematic viscosity at 40°C is 293.77 mm 2 / s to 339.16mm 2 / s, and the viscosity index is not less than 162, and the pour point is not higher than -33°C, indicating that the synthetic ester wind power gear oil base oil of the present invention has excellent viscosity-temperature performance and low-temperature performance, ensuring high oil film strength and excellent low-temperature fluidity.

[0063] In summary, the synthetic ester wind power gear oil base oil of the present invention has excellent viscosity-temperature performance, low temperature performance and biodegradability, and is an environmentally friendly lubricant base oil that can meet the lubrication and protection requirements under harsh working conditions. It can effectively solve the problems of insufficient comprehensive performance, short service life and easy environmental pollution in existing wind power generation special gear oils.

[0064] The synthetic ester wind power gear oil base oil of the present invention gives full play to the advantage of the ester molecular structure that is easy and flexible to control, overcomes the defects of traditional gear lubricants such as non-biodegradability, poor compatibility with other additives and short service life, can meet the lubrication and maintenance requirements under harsh working conditions, and ensure the safe and stable operation of wind power transmission gearboxes.

[0065] The above technical features constitute the embodiments of the present invention, which have strong adaptability and implementation effect. Non-essential technical features can be added or reduced according to actual needs to meet the requirements of different situations.

Claims

1. A method for preparing a synthetic ester wind power gear oil base oil, characterized in that Proceed as follows: S1, mixing a required amount of dicarboxylic acid and monohydric fatty alcohol, introducing an inert gas as a water-carrying agent and a protective gas, and causing an esterification reaction under the action of an esterification catalyst to obtain a mixed dicarboxylic acid monoester; S2, adding a required amount of neopentyl polyol and monocarboxylic acid to the mixed dicarboxylic acid monoester and mixing, introducing an inert gas as a water-carrying agent and a protective gas, and continuing the esterification reaction under the action of an esterification catalyst to obtain an esterification product containing a composite polyol ester; S3, separating and refining the esterification product containing the complex polyol ester to obtain a synthetic ester wind power gear oil base oil.

2. The method for preparing the synthetic ester wind power gear oil base oil according to claim 1, characterized in that In step S1, the dicarboxylic acid is one or more of the dicarboxylic acids having a carbon chain length of C4 to C10, and the monohydric fatty alcohol is one or more of the normal straight-chain or isomeric branched monohydric fatty alcohols having a carbon chain length of C4 to C12; or / and, in step S2, the neopentyl polyol is one or more of neopentyl glycol, trimethylolpropane, and pentaerythritol; and the monocarboxylic acid is one or more of the normal straight-chain or isomeric branched monocarboxylic acids having a carbon chain length of C5 to C18.

3. The method for preparing the synthetic ester wind power gear oil base oil according to claim 1 or 2, characterized in that In step S1, the dicarboxylic acid is one or more of glutaric acid, adipic acid and nonanedioic acid, and the monohydric fatty alcohol is one or more of 2-ethylhexanol, 6-methylheptanol and sec-octanol; or / and, in step S2, the neopentyl polyol is pentaerythritol, and the monocarboxylic acid is one or more of n-octanoic acid, n-nonanoic acid and 2-ethylhexanoic acid.

4. The method for preparing the synthetic ester wind power gear oil base oil according to any one of claims 1 to 3, characterized in that In step S1, the molar ratio of dicarboxylic acid to monohydric fatty alcohol is 1.0 to 1.2:1; or / and, in step S2, the molar ratio of neopentyl polyol, monocarboxylic acid and mixed dicarboxylic acid monoester is 1:1.5 to 2.5:1.5 to 2.

0.

5. The method for preparing the synthetic ester wind power gear oil base oil according to claim 4, characterized in that In step S1, the molar ratio of dicarboxylic acid to monohydric fatty alcohol is 1:1; or / and, in step S2, the molar ratio of neopentyl polyol, monocarboxylic acid and mixed dicarboxylic acid monoester is 1:2.25 to 2.45:1.55 to 1.

75.

6. The method for preparing the synthetic ester wind power gear oil base oil according to any one of claims 1 to 5, characterized in that In steps S1 and S2, the inert gas is one of nitrogen, argon and carbon dioxide; in step S1, based on the total mass of the reaction material added, the purge flow rate of the inert gas introduced into each gram of the reaction material is 1.0 mL / min to 3.0 mL / min; in step S2, based on the total mass of the reaction material added, the purge flow rate of the inert gas introduced into each gram of the reaction material is 1.0 mL / min to 3.0 mL / min; or / and, in steps S1 and S2, the esterification catalyst is a tin-based esterification catalyst, and is one of stannous oxide, tin dioxide, stannous chloride, tin tetrachloride, stannous sulfate, stannous octoate and stannous oxalate; in step S1, the amount of the esterification catalyst added is 1.0 wt% to 2.0 wt% of the total mass of the reaction material added in step S1; in step S2, the amount of the esterification catalyst added is 1.0 wt% to 2.0 wt% of the total mass of the reaction material added in step S2.

7. The method for preparing the synthetic ester wind power gear oil base oil according to claim 6, characterized in that In steps S1 and S2, the inert gas is nitrogen; in step S1, based on the total mass of the reaction material added, the purge flow rate of the inert gas introduced into each gram of the reaction material is 2.0 mL / min; in step S2, based on the total mass of the reaction material added, the purge flow rate of the inert gas introduced into each gram of the reaction material is 2.0 mL / min; or / and, in steps S1 and S2, the esterification catalyst is stannous oxide; in step S1, the amount of the esterification catalyst added is 1.2 wt% to 1.5 wt% of the total mass of the reaction material added in step S1; in step S2, the amount of the esterification catalyst added is 1.2 wt% to 1.5 wt% of the total mass of the reaction material added in step S2.

8. The method for preparing the synthetic ester wind power gear oil base oil according to any one of claims 1 to 7, characterized in that In step S1, the temperature of the esterification reaction is 150°C to 170°C, and the reaction time is 1h to 2h; in step S2, the temperature of the esterification reaction is 160°C to 180°C, and the reaction time is 6h to 8h; or / and, in steps S1 and S2, the esterification reactions are both carried out under mechanical stirring, and the stirring rate is 500r / min to 700r / min; or / and, in step S3, separation and purification is one of centrifugation, suction filtration and filter pressing, and the temperature during separation is 120°C to 160°C.

9. The method for preparing the synthetic ester wind power gear oil base oil according to claim 8, characterized in that In step S1, the temperature of the esterification reaction is 155°C to 165°C, and the reaction time is 1.5 hours; in step S2, the temperature of the esterification reaction is 170°C to 180°C, and the reaction time is 7 hours; or / and, in steps S1 and S2, the esterification reactions are both carried out under mechanical stirring, and the stirring rate is 600r / min to 700r / min; or / and, in step S3, the separation and purification is suction filtration, and the temperature during separation is 140°C to 150°C. 10 . A synthetic ester wind turbine gear oil base oil obtained by the method for preparing a synthetic ester wind turbine gear oil base oil according to any one of claims 1 to 9.

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