Lubricating grease composition as well as preparation method and application thereof

Abstract

The invention relates to the technical field of lubricating grease, in particular to a lubricating grease composition as well as a preparation method and application thereof. The lubricating grease composition comprises base oil, a thickening agent and an additive, the base oil is composed of alkyl naphthalene synthetic oil and ester synthetic oil; the additive comprises an anti-wear reagent at extreme pressure; the anti-wear reagent at extreme pressure comprises at least two of nano lanthanum fluoride, nano cerium oxide, calcium silicate, triphenyl phosphate, graphite and molybdenum disulfide. The wind power lubricating grease provided by the invention not only has good high and low temperature performance and excellent oxidation resistance, but also has better lubricity and adhesivity, effectively reduces friction and wear of equipment, can meet the operation requirements of wind power equipment under severe conditions such as extreme temperature, humidity and salt mist, and has a wide application prospect. And the phenomena of equipment failure and shutdown caused by poor lubrication are avoided, and the service life of the wind power bearing is greatly prolonged.

Description

Technical Field

[0001] The present invention relates to the technical field of lubricating grease, and in particular to a lubricating grease composition and a preparation method and application thereof. Background Art

[0002] Energy is an important support for the contemporary economy and an important foundation for industrial development. With the rapid development of my country's industry, conventional energy such as coal and oil has been over-consumed, and energy shortages and environmental pollution have become increasingly prominent. The development of clean and renewable energy has become a core part of the national energy strategy. Wind power generation is an important industry for achieving transformation and upgrading in the energy field, a key area for the development of renewable energy, and a preferred measure to promote energy structure adjustment. As one of the most mature, large-scale development conditions and commercial development prospects in the field of renewable energy, wind power generation is widely distributed around the world and has huge reserves. At the same time, with the continuous maturity of wind power-related technologies and the continuous upgrading of equipment, the global wind power industry has developed rapidly. As an important part of maintaining the healthy operation of wind turbines, the performance of grease directly affects the operating efficiency and life of wind power equipment.

[0003] Wind power equipment is usually installed outdoors in harsh working environments, such as extreme temperatures, high humidity, strong winds and sandstorms, etc. These harsh conditions place extremely high demands on the performance of grease, requiring the grease to have excellent high and low temperature, corrosion resistance, extreme pressure and wear resistance and other properties. In addition, the maintenance cycle of wind power equipment is long and the operating environment is harsh, which places higher requirements on the service life and maintenance frequency of grease. However, the wind power grease products currently on the market often cannot fully meet these requirements, causing the equipment to easily malfunction during operation, affecting the stable operation of the wind farm. Therefore, improving the extreme pressure and wear resistance and lubrication life of grease can reduce the amount of grease used, thereby reducing pollution to the environment, extending the grease change cycle and reducing the comprehensive application cost, which is of great practical significance and economic value to the entire society.

[0004] Chinese patent application CN109536249 effectively improves the performance of gear grease by adding hydroisomerized cycloalkane base oil and Fischer-Tropsch synthetic base oil, and ensures that the gear grease still has good thermal oxidation stability under harsh environments and working conditions such as low temperature (-30℃~-40℃) and high temperature (200℃), but the grease is only suitable for yaw system gears. Chinese patent application CN113174286A adopts a fully synthetic base oil formula and active bentonite as a thickener to improve the high and low temperature performance of the grease, but the anti-wear performance needs to be further improved. Summary of the invention

[0005] In order to solve the above technical problems, the present invention provides a grease composition and a preparation method and application thereof, which can increase the service life of the grease and meet the lubrication requirements of wind power equipment in harsh environments.

[0006] Based on this, the present invention has the following technical solutions: In a first aspect, the present invention provides a grease composition comprising: a base oil, a thickener and an additive; the base oil is composed of an alkyl naphthalene synthetic oil and an ester synthetic oil; the additive comprises an extreme pressure anti-wear agent; the extreme pressure anti-wear agent comprises at least two of nano lanthanum fluoride, nano cerium oxide, calcium silicate, triphenyl phosphate, graphite and molybdenum disulfide.

[0007] The present invention finds that the addition of the above-mentioned extrusion anti-wear agent can improve the wear-reducing and anti-wear properties of the grease to a certain extent, which not only reduces the use of traditional anti-wear agents containing environmentally unfriendly elements such as sulfur and phosphorus, improves environmental protection performance, but also extends the service life of wind power equipment, and has a good market prospect.

[0008] Preferably, the extreme pressure anti-wear agent comprises a mixture of nano-lanthanum fluoride, nano-cerium oxide and calcium silicate.

[0009] Preferably, the extreme pressure anti-wear agent comprises a mixture of nano-lanthanum fluoride, nano-cerium oxide and calcium silicate in a mass ratio of 0.5-1.5:0.5-1.5:0.5-1.

[0010] Preferably, the amount of the extreme pressure anti-wear agent in the lubricating oil composition is 1 to 3 wt %.

[0011] Preferably, the mass ratio of the alkyl naphthalene synthetic oil to the ester synthetic oil is 1-3:1-3.

[0012] Preferably, the alkyl naphthalene synthetic oil includes one or more of AN8, AN23 and AN30; the ester synthetic oil includes one or more of pentaerythritol ester, trimethylolpropane trioleate, dioctyl adipate and dioctyl phthalate; more preferably, the alkyl naphthalene synthetic oil is AN23, and the ester synthetic oil is trimethylolpropane trioleate.

[0013] In the present invention, the base oil using the above-mentioned mixing method can better improve the high and low temperature performance of the grease.

[0014] Preferably, the thickener is a complex calcium soap thickener obtained by reacting fatty acids, small molecule acids and calcium hydroxide; wherein the fatty acids include one or more of palmitic acid, myristic acid and lauric acid, and the small molecule acids include one or more of boric acid, phosphoric acid and acetic acid.

[0015] More preferably, the fatty acid is lauric acid, and the small molecule acid is boric acid.

[0016] More preferably, the mass ratio of the fatty acid to the small molecule acid is 3 to 6:1.

[0017] Preferably, the additive comprises an antioxidant, and the antioxidant comprises one or more of octylbutyldiphenylamine, diisooctyldiphenylamine, 2-naphthol and dodecylselenium; more preferably dodecylselenium.

[0018] Preferably, the rust inhibitor includes one or more of dodecenylsuccinic acid, sodium petroleum sulfonate and zinc naphthenate; more preferably, it is dodecenylsuccinic acid.

[0019] Preferably, the grease composition comprises the following components in parts by weight: Base oil 72-90 parts; Thickener 7-15 parts; 1 to 3 parts of extreme pressure anti-wear agent; 0.5-2 parts of antioxidant; 0.5 to 1.5 parts of anti-rust and anti-corrosion agent.

[0020] In the present invention, the grease adopts a scientifically designed base oil, is matched with a special extreme pressure anti-wear agent and an antioxidant with excellent performance, forms a good protective film on the bearing surface, reduces the wear between the bearings, increases the service life of the grease, and meets the lubrication requirements of wind power equipment in harsh environments.

[0021] In a second aspect, the present invention provides a method for preparing the grease composition, comprising the following steps: 50-70wt% of the base oil is mixed with fatty acids and small molecule acids, and the temperature is raised to 85-90°C to obtain a fatty acid solution; after the temperature is raised to 95-100°C, 30-50wt% of calcium hydroxide solution is added for saponification reaction; the temperature is raised to 130-140°C and kept warm; after drainage, the temperature is continued to be raised to the highest refining temperature of 210-220°C and kept warm; the remaining base oil is added and cooled, and after the temperature is lowered to below 80°C, additives are added for homogenization treatment, and then degassing is performed to obtain a grease composition.

[0022] As a preferred embodiment of the present invention, the method for preparing the grease composition comprises the following steps: First, weigh 50% to 70% of alkyl naphthalene synthetic oil and ester synthetic oil into a reactor, add fatty acids and small molecular acids, heat to 85 to 90°C to obtain fatty acid solution, and add 30% to 50% calcium hydroxide solution for saponification reaction. The reaction time is 50 to 60 minutes, and the temperature is controlled at 95 to 100°C to start dripping the remaining calcium hydroxide solution; heat to 130 to 140°C and keep the temperature constant for 60 to 90 minutes; after drainage, continue to heat to the highest refining temperature of 210 to 220°C and keep the temperature constant for 3 to 5 minutes. Add the remaining base oil and cool it down. When the temperature drops to below 80°C, add extreme pressure anti-wear agent, antioxidant, rust and corrosion inhibitor, stir for 30 to 40 minutes, and then pass the material through a three-roller mill for homogenization and degas to obtain a finished grease composition.

[0023] In a third aspect, the present invention provides application of the grease composition in wind power equipment.

[0024] The present invention provides a grease composition and a preparation method and application thereof. By optimizing the composition of base oil and additives, the components are coordinated with each other, which significantly improves the extreme pressure, anti-wear, anti-oxidation, anti-corrosion and anti-rust performance of the grease, so that it can meet the use requirements of wind power bearings, especially meet the use performance requirements under severe environments and working conditions such as sand and dust, rain and snow, and seawater salt spray erosion. In particular, the addition of nano-lanthanum fluoride and nano-cerium oxide improves the wear-reducing and anti-wear performance of the grease to a certain extent, reduces the use of traditional anti-wear agents containing environmentally unfriendly elements such as sulfur and phosphorus, improves environmental protection performance, and prolongs the service life of wind power equipment, which has a good market prospect. DETAILED DESCRIPTION

[0025] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be described clearly and completely below. Obviously, the described embodiments are 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 creative work are within the scope of protection of the present invention.

[0026] Unless otherwise specified, the various raw materials used in the examples and comparative examples are commercially available conventional raw materials, and the technical means used are conventional means well known to those skilled in the art.

[0027] Example 1

[0028] This embodiment provides a grease composition, and the preparation method thereof comprises the following steps: First, weigh 30 parts of AN23 and 18 parts of trimethylolpropane trioleate in a reactor, add 8 parts of lauric acid and 2 parts of boric acid, heat to 85°C to obtain a fatty acid solution, and add 2 parts of calcium hydroxide solution for saponification. The reaction time is 50 minutes, and the temperature is controlled at 95-100°C to start dripping the remaining 3 parts of calcium hydroxide solution; heat to 135°C and keep the temperature constant for 60 minutes; after drainage, continue to heat to the highest refining temperature of 220°C and keep the temperature constant for 5 minutes. Add the remaining 23.5 parts of AN23 and 10 parts of trimethylolpropane trioleate and cool down. When the temperature drops to 80°C, add 1 part of nano lanthanum fluoride, 0.5 parts of nano cerium oxide, 1 part of calcium silicate, 0.5 parts of dodecyl selenium, and 0.5 parts of dodecenyl succinic acid. After stirring for 30 minutes, the material is homogenized by a three-roller machine and degassed to obtain a finished grease.

[0029] Example 2

[0030] This embodiment provides a grease composition, and the preparation method thereof comprises the following steps: First, weigh 35 parts of AN23 and 18 parts of trimethylolpropane trioleate in a reactor, add 7 parts of lauric acid and 2 parts of boric acid, heat to 85°C to obtain a fatty acid solution, and add 2 parts of calcium hydroxide solution for saponification. The reaction time is 60 minutes, and the temperature is controlled at 95-100°C to start dripping the remaining 3 parts of calcium hydroxide solution; heat to 130°C and keep the temperature constant for 60 minutes; after drainage, continue to heat to the highest refining temperature of 210°C and keep the temperature constant for 5 minutes. Add the remaining 15 parts of AN23 and 13 parts of trimethylolpropane trioleate and cool down. When the temperature drops to 80°C, add 1.5 parts of nano lanthanum fluoride, 0.5 parts of nano cerium oxide, 1 part of calcium silicate, 1 part of dodecyl selenium, and 1 part of dodecenyl succinic acid. After stirring for 30 minutes, the material is homogenized by a three-roller machine and degassed to obtain a finished grease.

[0031] Example 3

[0032] This embodiment provides a grease composition, and the preparation method thereof comprises the following steps: First, weigh 28 parts of AN23 and 25 parts of trimethylolpropane trioleate in a reactor, add 6 parts of lauric acid and 1 part of boric acid, heat to 85°C to obtain a fatty acid solution, and add 2 parts of calcium hydroxide solution for saponification. The reaction time is 60 minutes, and the temperature is controlled at 95-100°C to start dripping the remaining 4 parts of calcium hydroxide solution; heat to 130°C and keep the temperature constant for 60 minutes; after drainage, continue to heat to the highest refining temperature of 210°C and keep the temperature constant for 5 minutes. Add the remaining 10 parts of AN23 and 20 parts of trimethylolpropane trioleate and cool down. When the temperature drops to 80°C, add 1 part of nano lanthanum fluoride, 1.5 parts of nano cerium oxide, 0.5 parts of calcium silicate, 0.5 parts of dodecyl selenium, and 0.5 parts of dodecenyl succinic acid. After stirring for 30 minutes, the material is homogenized by a three-roller machine and degassed to obtain a finished grease.

[0033] Example 4

[0034] This embodiment provides a grease composition, and the preparation method thereof comprises the following steps: First, weigh 15 parts of AN23 and 35 parts of trimethylolpropane trioleate in a reactor, add 8 parts of lauric acid and 2 parts of boric acid, heat to 85°C to obtain a fatty acid solution, and add 2 parts of calcium hydroxide solution for saponification. The reaction time is 55 minutes, and the temperature is controlled at 95-100°C to start dripping the remaining 3 parts of calcium hydroxide solution; heat to 140°C and keep the temperature constant for 60 minutes; after drainage, continue to heat to the highest refining temperature of 210°C and keep the temperature constant for 5 minutes. Add the remaining 15 parts of AN23 and 16 parts of trimethylolpropane trioleate and cool down. When the temperature drops to 80°C, add 0.5 parts of nano lanthanum fluoride, 1 part of nano cerium oxide, 0.5 parts of calcium silicate, 1 part of dodecyl selenium, and 1 part of dodecenyl succinic acid. After stirring for 30 minutes, the material is homogenized by a three-roller machine and degassed to obtain a finished grease.

[0035] Example 5

[0036] This embodiment provides a grease composition, and the preparation method thereof comprises the following steps: First, weigh 20 parts of AN23 and 32 parts of trimethylolpropane trioleate in a reactor, add 5 parts of lauric acid and 2 parts of boric acid, heat to 85°C to obtain a fatty acid solution, and add 1.5 parts of calcium hydroxide solution for saponification. The reaction time is 55 minutes, and the temperature is controlled at 95-100°C to start dripping the remaining 2.5 parts of calcium hydroxide solution; heat to 140°C and keep the temperature constant for 60 minutes; after drainage, continue to heat to the highest refining temperature of 210°C and keep the temperature constant for 5 minutes. Add the remaining 10.5 parts of AN23 and 23 parts of trimethylolpropane trioleate and cool down. When the temperature drops to 80°C, add 0.5 parts of nano lanthanum fluoride, 0.5 parts of nano cerium oxide, 0.5 parts of calcium silicate, 1.5 parts of dodecyl selenium, and 0.5 parts of dodecenyl succinic acid. After stirring for 30 minutes, the material is homogenized by a three-roller machine and degassed to obtain a finished grease.

[0037] Comparative Example 1

[0038] This comparative example provides a grease composition, and the preparation method thereof comprises the following steps: First, weigh 55 parts of AN23 into a reactor, add 8 parts of lauric acid and 2 parts of boric acid, heat to 85°C to obtain a fatty acid solution, and add 2 parts of calcium hydroxide solution for saponification. The reaction time is 55 minutes, and the temperature is controlled at 95-100°C to start dripping the remaining 4 parts of calcium hydroxide solution; heat to 130°C and keep the temperature constant for 60 minutes; after drainage, continue to heat to the highest refining temperature of 220°C and keep the temperature constant for 5 minutes. Add the remaining 25 parts of AN23 and cool down. When the temperature drops to 80°C, add 1 part of nano lanthanum fluoride, 0.5 parts of nano cerium oxide, 0.5 parts of calcium silicate, 1 part of dodecyl selenium, and 1 part of dodecenyl succinic acid. After stirring for 30 minutes, the material is homogenized by a three-roller machine and degassed to obtain a finished grease.

[0039] Comparative Example 2

[0040] First weigh 45 parts of trimethylolpropane trioleate into a reactor, add 7 parts of lauric acid and 2 parts of boric acid, heat to 85°C to obtain a fatty acid solution, and add 3 parts of calcium hydroxide solution for saponification. The reaction time is 55 minutes, the temperature is controlled at 95-100°C, and the remaining 4 parts of calcium hydroxide solution are added dropwise; the temperature is raised to 140°C and kept constant for 60 minutes; after drainage, the temperature is continued to rise to the highest refining temperature of 210°C and kept constant for 5 minutes. Add the remaining 34 parts of trimethylolpropane trioleate and cool it down. When the temperature drops to 80°C, add 2 parts of nano cerium oxide, 0.5 parts of calcium silicate, 1.5 parts of dodecyl selenium, and 1 part of dodecenyl succinic acid. After stirring for 30 minutes, the material is homogenized by a three-roller machine and degassed to obtain a finished grease.

[0041] Test example

[0042] The performance of the greases prepared in the above examples and comparative examples was tested, and the test results are shown in Table 1.

[0043] Table 1

[0044] It can be seen from the data in Table 1 that the greases prepared in the embodiments of the present invention all exhibit excellent extreme pressure anti-wear properties, good anti-oxidation properties and low-temperature starting properties, etc., and fully meet the requirements and working conditions of wind power greases. At the same time, the addition of nano-lanthanum fluoride and nano-cerium oxide improves the anti-friction and anti-wear properties of the grease to a certain extent, reduces the use of traditional anti-wear agents containing environmentally unfriendly elements such as sulfur and phosphorus, improves environmental protection performance, and extends the service life of wind power equipment, which has a good market prospect.

[0045] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A grease composition, characterized in that: include: Base oil, thickener and additives; the base oil is composed of alkyl naphthalene synthetic oil and ester synthetic oil; the additives include extreme pressure anti-wear agents; the extreme pressure anti-wear agents include at least two of nano lanthanum fluoride, nano cerium oxide, calcium silicate, triphenyl phosphate, graphite and molybdenum disulfide.

2. The grease composition according to claim 1, characterized in that The extreme pressure anti-wear agent comprises a mixture of nano-lanthanum fluoride, nano-cerium oxide and calcium silicate; preferably, the extreme pressure anti-wear agent comprises a mixture of nano-lanthanum fluoride, nano-cerium oxide and calcium silicate in a mass ratio of 0.5-1.5:0.5-1.5:0.5-1.

3. The grease composition according to claim 2, characterized in that The amount of the extreme pressure anti-wear agent in the grease composition is 1 to 3 wt %.

4. The grease composition according to any one of claims 1 to 3, characterized in that The mass ratio of the alkyl naphthalene synthetic oil to the ester synthetic oil is 1-3:1-3.

5. The grease composition according to any one of claims 1 to 3, characterized in that The thickener is a complex calcium soap thickener, which is obtained by reacting fatty acids, small molecule acids and calcium hydroxide; wherein the fatty acids include one or more of palmitic acid, myristic acid and lauric acid, and the small molecule acids include one or more of boric acid, phosphoric acid and acetic acid; preferably, the mass ratio of the fatty acids to the small molecule acids is 3 to 6:

1.

6. The grease composition according to any one of claims 1 to 3, characterized in that: The additive includes an antioxidant, and the antioxidant includes one or more of octylbutyldiphenylamine, diisooctyldiphenylamine, 2-naphthol and dodecylselenium; more preferably dodecylselenium.

7. The grease composition according to claim 6, characterized in that The additive includes a rust inhibitor, and the rust inhibitor includes one or more of dodecenylsuccinic acid, sodium petroleum sulfonate and zinc naphthenate; more preferably, the rust inhibitor is dodecenylsuccinic acid.

8. The grease composition according to claim 7, characterized in that The invention comprises the following components in parts by weight: Base oil 72-90 parts; Thickener 7-15 parts; 1 to 3 parts of extreme pressure anti-wear agent; 0.5-2 parts of antioxidant; 0.5 to 1.5 parts of anti-rust and anti-corrosion agent.

9. The method for preparing the grease composition according to any one of claims 1 to 8, characterized in that: The steps include: 50-70wt% of the base oil is mixed with fatty acids and small molecule acids, and the temperature is raised to 85-90°C to obtain a fatty acid solution; after the temperature is raised to 95-100°C, 30-50wt% of calcium hydroxide solution is added for saponification reaction; the temperature is raised to 130-140°C and kept warm; after drainage, the temperature is continued to be raised to the highest refining temperature of 210-220°C and kept warm; the remaining base oil is added and cooled, and after the temperature is lowered to below 80°C, additives are added for homogenization treatment, and then degassing is performed to obtain a grease composition.

10. Use of the grease composition according to any one of claims 1 to 8 or the grease composition prepared by the preparation method according to claim 9 in wind power equipment.

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