Extreme pressure anti-wear perfluoropolyether lubricating grease and preparation method thereof
By combining perfluoropolyether, thickener and additives, extreme pressure anti-wear perfluoropolyether grease is prepared, which solves the problems of poor extreme pressure anti-wear performance and pollution in the preparation process in the existing technology, and realizes long-term lubrication protection and industrial production in extreme environments.
Patent Information
- Application Number
- CN202511344535.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-19
- Publication Date
- 2025-12-05
AI Technical Summary
Existing perfluoropolyether greases have poor extreme pressure anti-wear performance under extremely harsh environments, and their preparation process uses highly toxic substances, making large-scale promotion difficult.
Extreme pressure anti-wear perfluoropolyether grease is prepared by using a combination of perfluoropolyether, thickener polytetrafluoroethylene and various additives through a specific process, including stirring, heating, water cooling and grinding, to form a uniform and stable colloidal structure and enhance extreme pressure anti-wear performance.
The prepared grease provides long-lasting lubrication protection under high temperature and high load conditions, extends equipment service life, reduces maintenance costs, and is suitable for large-scale industrial production.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of lubricating grease, in particular to an extreme pressure and anti-wear perfluoropolyether grease and a preparation method thereof. BACKGROUND
[0002] As a kind of semi-solid lubricant, lubricating grease is widely used in bearing, gear, guide rail, sealing element and other key friction pairs of various mechanical equipment. Its core function is to form a stable lubricating film on the friction surface, reduce friction and wear, prevent corrosion and dust sealing, thereby prolonging the service life of equipment, and ensuring operation reliability and efficiency. With the development of modern industrial technology, more and more equipment needs to operate in extreme harsh environments, such as ultra-low temperature (e.g. below ~60℃), ultra-high temperature (e.g. above 200℃), strong oxidation environment, chemical corrosive medium and high vacuum or special atmosphere. Perfluoropolyether oil has excellent thermal oxidation stability, long-term stable operation in a wide temperature range (~60-260℃), excellent chemical inertness, low volatility and non-flammability due to its unique molecular structure (mainly C-F bond, no C-H bond). The existing preparation method of perfluoropolyether grease is to modify extreme pressure and anti-wear additives under the action of fluorine gas and add them to the grease, thereby obtaining perfluoropolyether grease with excellent extreme pressure and anti-wear performance. The perfluoropolyether acyl fluoride and fluorine gas used in this existing method are both highly toxic substances and can cause environmental pollution, making it difficult to be widely promoted in actual production. Moreover, the existing perfluoropolyether grease has poor extreme pressure and anti-wear performance, which cannot meet the use requirements of extreme pressure and anti-wear performance under harsh working conditions, and there is an urgent need to develop a perfluoropolyether grease with simple process and excellent extreme pressure and anti-wear performance. SUMMARY
[0003] In view of the shortcomings of the prior art, the present application provides an extreme pressure and anti-wear perfluoropolyether grease and a preparation method thereof. The perfluoropolyether grease has excellent extreme pressure and anti-wear performance, and the components and preparation process are simple, which is suitable for large-scale industrial promotion.
[0004] To achieve the above-mentioned purpose, the present application provides an extreme pressure and anti-wear perfluoropolyether grease, which comprises the following components by mass percentage: perfluoropolyether 60-75%, thickening agent 25-40%, and additive 0.01-3%; the chemical formula of the perfluoropolyether is CF3CF2CF2O(CF(CF3)CF2O) n CF2-CF3; the thickening agent is polytetrafluoroethylene; and the additive comprises a combination of one or more of alkyl phosphite, zinc alkyl dithiophosphate, zinc sulfophosphor octyl butyl salt, liquid dithiophosphate derivative, sodium nitrite, barium petroleum sulfonate, benzene propyl triazole, benzene propyl thiazole and disodium sebacate.
[0005] As a further setting of the present application, the molecular weight of the perfluoropolyether is set to 3000-9000 g / mol.
[0006] As a further setting of the present application, the molecular weight of the perfluoropolyether is set to 4000-6000 g / mol.
[0007] As a further setting of the present application, the polytetrafluoroethylene particle size is 1-10 μm.
[0008] As a further setting of the present application, the polytetrafluoroethylene particle size is 2-4 μm.
[0009] The beneficial effects of such a setting are: such a setting, through precise component design, achieves comprehensive optimization of performance. The core base oil perfluoropolyether adopts a specific chemical formula structure, and the stability of its molecular chain provides excellent high-temperature oxidation resistance and chemical inertness for the grease. When the molecular weight is controlled in the range of 3000-9000 g / mol, especially in the range of 4000-6000 g / mol, both good low-temperature fluidity and viscosity stability at high temperatures can be ensured, avoiding lubrication failure. The thickening agent is polytetrafluoroethylene with a particle size of 1-10 μm, and the optimal particle size of 2-4 μm can form a uniform and stable colloidal structure with perfluoropolyether, significantly improving the mechanical stability and shear resistance of the grease, and reducing the loss of thickening agent during use. The additives work synergistically: sulfur and phosphorus additives such as alkyl phosphite and zinc alkyl dithiophosphate can form a dense protective film on the friction surface, significantly enhancing the extreme pressure and wear resistance; sodium nitrite and barium petroleum sulfonate can effectively inhibit metal corrosion; benzene propyl triazole and benzene propyl thiazole play a metal passivation role to avoid metal surface corrosion; and disodium sebacate improves the water resistance of the grease. The multi-component synergy significantly extends the service life of the grease, making it suitable for equipment lubrication under severe working conditions.
[0010] As the present application also discloses a preparation method of the extreme pressure and wear-resistant perfluoropolyether grease, comprising the following steps: adding polytetrafluoroethylene to perfluoropolyether, stirring and mixing at a temperature of 70-100℃ for 1-2h; then heating to 110-130℃, stirring and mixing for 1-2h; then heating to 170-190℃, stirring and mixing for 0.5-1h; water cooling to 70-90℃, adding additives, stirring and mixing for 15-45min; finally, the mixture is ground for 1-2h.
[0011] The beneficial effects of such arrangement are: after the first step of adding polytetrafluoroethylene into perfluoropolyether, stirring at 70-100℃ for 1-2h can realize the preliminary dispersion of the thickening agent, avoiding agglomeration; continuing to stir at 110-130℃ can promote the compatibility of polytetrafluoroethylene and base oil, laying the foundation for the formation of colloidal structure; stirring at 170-190℃ for 0.5-1h can further strengthen the stability of the system and improve the high-temperature resistance of the grease. Adding additives after water cooling to 70-90℃ can not only ensure the full dissolution and dispersion of the additives, but also prevent the decomposition of the additives caused by high temperature; 1-2h of grinding treatment can refine the particles and homogenize the system, ensuring the uniformity of product performance. The whole process does not require complex equipment, the steps are coherent and easy to control, and meets the efficient and low-cost demand of industrial large-scale production. The final product, with excellent extreme pressure and wear resistance, oxidation stability and high-temperature stability, can provide long-term lubrication protection for bearings in complex environments such as high temperature and high load, reducing equipment maintenance costs. DETAILED DESCRIPTION
[0012] The first embodiment of the extreme pressure and wear-resistant perfluoropolyether grease and its preparation method provided by the application is as follows: 130g of polytetrafluoroethylene powder (purchased from Fuzhou Taipuda New Material Co., Ltd., with an average particle size of 3-5μm) is added into 300g of perfluoropolyether oil (purchased from Haishifu Chemical Co., Ltd., with a molecular formula of CF3CF2CF2O(CF(CF3)CF2O) n CF2-CF3, and an average molecular weight of 4800), and stirring and mixing are carried out at 90℃ for 1h. Then, stirring and mixing are carried out at 120℃ for 1h. Then, stirring and mixing are carried out at 180℃ for 40min. The grease is cooled to 80℃ in water, 0.5g of preservative benzene propyl triazole (purchased from Aladdin Chemical Co., Ltd.) and 2.2g of disodium sebacate (purchased from Aladdin Chemical Co., Ltd.) are added, and stirring is carried out for 15min. Then, 2.2g of anti-wear additive alkyl phosphite (purchased from Lubrizol Additives (Zhuhai) Co., Ltd.) and 2.2g of zinc dialkyldithiophosphate (purchased from Lubrizol Additives (Zhuhai) Co., Ltd.) are added, and stirring is carried out for 15min. Finally, the perfluoropolyether grease is collected after being ground on a three-roll grinding machine for 1h.
[0013] The second embodiment of the extreme pressure and wear-resistant perfluoropolyether grease and its preparation method provided by the application is as follows: 120g of polytetrafluoroethylene powder (purchased from Fuzhou Taipuda New Material Co., Ltd., with an average particle size of 5-8μm) is added into 320g of perfluoropolyether oil (purchased from Haishifu Chemical Co., Ltd., with a molecular formula of CF3CF2CF2O(CF(CF3)CF2O) nCF2-CF3, average molecular weight 3600) was stirred at 80℃ for 1.5h. The temperature was raised to 110℃ and stirred for 1.5h. Then the temperature was raised to 170℃ and stirred for 50min. The grease was cooled to 80℃ in water, and preservative benzene propyl thiazole (purchased from Aradin Chemical Trading Co., Ltd.) 2g and sodium nitrite (purchased from Aradin Chemical Trading Co., Ltd.) 2g were added and stirred for 15min. Then anti-wear additive alkyl phosphite (purchased from Lubrizol Additives (Zhuhai) Co., Ltd.) 1.5g and sulfur phosphorus butyloctyl zinc salt (purchased from Lubrizol Additives (Zhuhai) Co., Ltd.) 1.5g were added and stirred for 15min. Finally, the grease was ground on a three-roll mill for 1.5h, and the perfluoropolyether grease was collected.
[0014] The present application provides a third embodiment of an extreme pressure anti-wear perfluoropolyether grease and a preparation method thereof. 140g of polytetrafluoroethylene powder (purchased from Fuzhou Taipuda New Material Co., Ltd., average particle size 1-3μm) was added to 300g of perfluoropolyether oil (purchased from Haishifu Chemical Co., Ltd., molecular formula CF3CF2CF2O(CF(CF3)CF2O) n CF2-CF3, average molecular weight 7000) was stirred at 100℃ for 2h. The temperature was raised to 130℃ and stirred for 2h. Then the temperature was raised to 190℃ and stirred for 1h. The grease was cooled to 90℃ in water, and preservative benzene propyl thiazole (purchased from Aradin Chemical Trading Co., Ltd.) 0.5g and sodium nitrite (purchased from Aradin Chemical Trading Co., Ltd.) 2.2g were added and stirred for 15min. Then anti-wear additive liquid dithiophosphate derivative (purchased from Lubrizol Additives (Zhuhai) Co., Ltd.) 4g was added and stirred for 15min. Finally, the grease was ground on a three-roll mill for 2h, and the perfluoropolyether grease was collected.
[0015] The present application provides a fourth embodiment of an extreme pressure anti-wear perfluoropolyether grease and a preparation method thereof. 130g of polytetrafluoroethylene powder (purchased from Fuzhou Taipuda New Material Co., Ltd., average particle size 5-8μm) was added to 300g of perfluoropolyether oil (purchased from Haishifu Chemical Co., Ltd., molecular formula CF3CF2CF2O(CF(CF3)CF2O) nThe grease was cooled in water to 90℃, and 2.2 g of preservative benzenepropanethiazole (purchased from Aradin Chemical Trade Co., Ltd.) and 2.2 g of disodium sebacate (purchased from Aradin Chemical Trade Co., Ltd.) were added, and stirred for 15 min; then 4 g of anti-wear additive liquid dithiophosphate derivative (purchased from BASF Co., Ltd.) was added, and stirred for 15 min. Finally, the grease was ground on a three-roll mill for 2 h, and the perfluoropolyether grease was collected.
[0016] A comparative example was provided based on the above four embodiments. 130 g of polytetrafluoroethylene micro powder (purchased from Fuzhou Taipuda New Material Co., Ltd., average particle size 3-5 μm) was added to 300 g of perfluoropolyether oil (purchased from Haishifu Chemical Co., Ltd., molecular formula CF3CF2CF2O(CF(CF3)CF2O) n The grease was cooled in water to 90℃, and 2.2 g of preservative benzenepropanethiazole (purchased from Aradin Chemical Trade Co., Ltd.) and 2.2 g of disodium sebacate (purchased from Aradin Chemical Trade Co., Ltd.) were added, and stirred for 15 min; then 4 g of anti-wear additive liquid dithiophosphate derivative (purchased from BASF Co., Ltd.) was added, and stirred for 15 min. Finally, the grease was ground on a three-roll mill for 2 h, and the perfluoropolyether grease was collected.
[0017] The perfluoropolyether greases prepared in the examples and comparative examples were tested for performance, and the test results are shown in Table 1:
[0018]
[0019] Table 1
[0020] According to Examples 1-4 and Comparative Example 1 and Table 1, in the present application, the extreme pressure and wear resistance of the grease is significantly improved by the reasonable collocation of additives, but the cone penetration, working temperature, oil separation and evaporation degree of the obtained grease product are hardly affected. This shows that, in the present application, the reasonable collocation of additives is added when preparing the grease product, which can improve the extreme pressure and wear resistance of the grease product without reducing the original performance of the grease product. It can provide long-term lubrication protection for bearings in complex working environments.
[0021] The above examples are only one of the preferred specific examples of the present application, and the usual changes and substitutions made by those skilled in the art within the scope of the technical solutions of the present application are all included in the protection scope of the present application.
Claims
1. An extreme pressure anti-wear perfluoropolyether grease characterized in that: Comprises the following components in mass percentage: perfluoropolyether 60-75%, thickening agent 25-40%, additive 0.01-3%; the chemical formula of the perfluoropolyether is CF3CF2CF2O(CF(CF3)CF2O) n CF2-CF3; the thickening agent is polytetrafluoroethylene; the additive comprises a combination of one or more of alkyl phosphite, zinc alkyl dithiophosphate, zinc sulfophenobutyl octyl, liquid dithiophosphate derivative, sodium nitrite, barium petroleum sulfonate, benzene propyl triazole, benzene propyl thiazole, and disodium sebacate.
2. The extreme pressure anti-wear perfluoropolyether grease according to claim 1, characterized in that: The molecular weight of the perfluoropolyether is set to 3000-9000 g / mol.
3. The extreme pressure anti-wear perfluoropolyether grease according to claim 2, characterized in that: The molecular weight of the perfluoropolyether is set to 4000-6000 g / mol.
4. The extreme pressure anti-wear perfluoropolyether grease according to claim 1, characterized in that: The polytetrafluoroethylene particle size is 1-10 μm.
5. The extreme pressure anti-wear perfluoropolyether grease according to claim 4, characterized in that: The polytetrafluoroethylene particle size is 2-4 μm.
6. A process for the preparation of the extreme pressure anti-wear perfluoropolyether grease according to claims 1 to 5, characterized by: The polytetrafluoroethylene is added to the perfluoropolyether, and the mixture is stirred at a temperature of 70-100°C for 1-2 h; then the temperature is raised to 110-130°C, and the mixture is stirred for 1-2 h; then the temperature is raised to 170-190°C, and the mixture is stirred for 0.5-1 h; the temperature is lowered to 70-90°C by water cooling, the additive is added, and the mixture is stirred for 15-45 min; finally, the mixture is subjected to grinding treatment, and the grinding time is set to 1-2 h.