A fiber lubricating oil for motors and its preparation method
By adding modified cotton fibers and zinc sulfide to PAO synthetic oil, a three-dimensional network structure and protective film are formed, which solves the problems of high cost and insufficient heat resistance of high-end lubricating oils and achieves efficient and stable fiber lubrication effect.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-11
- Publication Date
- 2026-03-17
AI Technical Summary
Existing high-end lubricating oil P2AO 180NP is costly and its supply chain is easily constrained. Furthermore, metal additives in traditional lubricating oils can easily cause fiber corrosion, and ordinary PAO base oils have limited heat resistance and friction reduction effects, making it difficult to meet the high-efficiency and precision upgrade requirements of the motor industry.
Using PAO synthetic oil as the base, thickeners and antioxidants are added, and benzoquinone-aminosilane cotton fibers and composite additives are added at room temperature and pressure. The cotton fibers are modified to improve their hydrophobicity and heat resistance, forming a three-dimensional network structure to encapsulate the base oil. Zinc sulfide is added to improve friction reduction.
It improves the high-temperature resistance and continuous lubrication ability of lubricating oil, reduces evaporation loss, enhances the dispersibility and stability of fiber lubricating oil, extends service life, and replaces the performance of P2AO 180NP.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of fiber lubricant technology, specifically to a motor fiber lubricant and its preparation method. Background Technology
[0002] In the field of industrial motor lubrication, high-end synthetic lubricants such as P2AO 180NP occupy an important position due to their excellent high and low temperature stability, anti-wear properties, and long-lasting performance. However, they also suffer from high costs and supply chain constraints. As the motor industry upgrades towards higher efficiency and precision, the requirements for low volatility and compatibility with fiber materials in lubricants are becoming increasingly stringent. Metal additives in traditional lubricants can easily cause fiber corrosion, and ordinary PAO base oils have limited heat resistance and friction-reducing effects, making them difficult to replace P2AO 180NP.
[0003] In conclusion, the preparation of a fiber lubricant for motors is of great significance. Summary of the Invention
[0004] The purpose of this invention is to provide a motor fiber lubricant and its preparation method to solve the problems raised in the prior art.
[0005] To achieve the above objectives, the present invention provides the following technical solution:
[0006] A method for preparing a fiber lubricating oil for electric motors includes the following steps:
[0007] Step 1: Mix amino POSS and amino-modified zinc sulfide in a certain proportion to obtain a composite additive;
[0008] Step 2: Mix PAO, tackifier, and antioxidant evenly, heat to 105~110℃, add benzoquinone-aminosilane cotton fiber and stir at 0.03~0.05MPa for 40~50 minutes. Under normal temperature and pressure, add barium petroleum sulfonate and composite additives, and stir for 15~20 hours to obtain motor fiber lubricating oil.
[0009] In a more optimized form, the raw materials of the motor fiber lubricant include the following components: by mass parts, 80-85 parts PAO, 1-3 parts tackifier, 0.8-1.5 parts antioxidant, 10-15 parts benzoquinone-aminosilane cotton fiber, 1-1.2 parts barium petroleum sulfonate, and 2-3 parts composite additives.
[0010] In the scheme, the PAO comprises PAO10 and PAO4 in a mass ratio of 3:1; the average particle size of the benzoquinone-aminosilane cotton fiber is 5~10μm.
[0011] In the scheme, the preparation method of oxidized cotton fiber is as follows: (1) Cotton fiber is placed in 18wt% sodium hydroxide solution for 2 hours, washed and dried to obtain activated cotton fiber; (2) Activated cotton fiber is added to 6g / mL sodium periodate solution, stirred at 50℃ for 3 hours in the dark, and then placed in 0.8g / mL glycerol solution for 1.5 hours, washed and dried to obtain oxidized cotton fiber.
[0012] In a more optimized manner, the mass ratio of aminoPOSS to amino-modified zinc sulfide is 1:(2~3).
[0013] The preparation method of aminoPOSS in the scheme is as follows: 20 mL of methyltrichlorosilane is added to 200 mL of acetone, stirred at 60 °C for 40 minutes, deionized water is slowly added dropwise, refluxed for 22 hours, cooled to room temperature, filtered, washed with acetone, pyridine is added and stirred overnight to remove insoluble matter, washed and filtered with an equal volume of concentrated hydrochloric acid and ice water mixture, washed with deionized water until neutral, dried, and 6 g of it is mixed with 100 mL of triethylamine and 200 mL of tetrahydrofuran, heated to 65 °C, and KH550-tetrahydrofuran is added (6 mL of KH550 is added to 100 mL of tetrahydrofuran to obtain KH550-tetrahydrofuran), refluxed for 22 hours, cooled to room temperature, filtered, washed and filtered with an equal volume of concentrated hydrochloric acid and ice water mixture, washed with deionized water until neutral, to obtain aminoPOSS.
[0014] A more optimized method for preparing the benzoquinone-aminosilane cotton fiber is as follows: (1) 1,3-bis(3-aminopropyl)tetramethyldisiloxane is added to DMF and mixed evenly. Oxidized cotton fiber is added and stirred continuously. The temperature is raised to 50~60℃ and stirred for 2~2.5 hours. The mixture is washed and dried to obtain aminosilane-cotton fiber. (2) Gallic acid, EDC·HCl and NHS are added to methanol and stirred for 1~2 hours under ice-water bath conditions. Aminosilane-cotton fiber is added and stirred for 30~40 minutes. The mixture is then transferred to room temperature and stirred for 15~20 hours. The mixture is washed and dried. The mixture is added to Tris solution and stirred evenly for 8~12 hours. The mixture is washed and dried to obtain benzoquinone-aminosilane cotton fiber.
[0015] An optimized method is to use a mass ratio of 1,3-bis(3-aminopropyl)tetramethyldisiloxane to oxidized cotton fibers of (3~5):1.
[0016] In a more optimized form, the raw material for the benzoquinone-aminosilane cotton fiber includes the following components: by mass parts, 2-3 parts gallic acid, 2.5-3 parts EDC·HCl, 1.6-2 parts NHS, and 8-10 parts aminosilane-cotton fiber; the pH of the Tris solution is 7.8-8.2.
[0017] A more optimized method involves adding zinc sulfide to ethanol-toluene under nitrogen protection and mixing them evenly. Acrylamide, 1,4-butanediol diacrylate, dodecyl methacrylate, and AIBN are then added. The mixture is stirred at 65-70°C for 7-8 hours, washed, and dried to obtain amino-modified zinc sulfide.
[0018] In a more optimized form, the raw material for the amino-modified zinc sulfide comprises the following components: by mass parts, 3-5 parts zinc sulfide, 0.3-0.5 parts acrylamide, 0.7-1 part 1,4-butanediol diacrylate, 1-1.2 parts dodecyl methacrylate, 0.2-0.25 parts AIBN, and 30-50 parts ethanol-toluene; wherein the mass ratio of ethanol to toluene in the ethanol-toluene mixture is 1:(1-3).
[0019] The method for preparing zinc sulfide is as follows: 100 mL of sodium sulfide solution (concentration of 1 M) is added dropwise to 100 mL of zinc chloride solution (concentration of 1 M), stirred at 70 °C for 1.5 hours, and after a white precipitate appears, it is filtered, dried, and placed in hydrochloric acid solution (concentration of 0.1 M) overnight. The pH of the precipitate is washed to 5, dried, and zinc sulfide is obtained.
[0020] Compared with the prior art, the beneficial effects of the present invention are:
[0021] This application uses PAO synthetic oil as the base, adds tackifiers and antioxidants to make a base oil, then adds benzoquinone-aminosilane cotton fiber under certain conditions and stirs it. Under normal temperature and pressure, barium petroleum sulfonate and composite additives are added to prepare motor fiber lubricating oil.
[0022] In this solution, PAO provides a high-temperature resistance foundation for fiber lubricating oil; the addition of antioxidants can inhibit the oxidative degradation of PAO under high-temperature and oxidative environments, further improving its service life.
[0023] During motor operation, high temperatures cause the base oil to evaporate, reducing the lubricating oil's sustained lubricity. To address this issue, cotton fibers are introduced into the lubricating oil. The three-dimensional network structure of cotton fibers can encapsulate PAO within the fibers, forming an oil-storing structure. However, cotton fibers have poor high-temperature resistance and are hydrophilic, thus affecting the performance of the lubricating oil. To solve this problem, this method involves oxidizing cotton fibers to introduce aldehyde groups, which then react with the amino group at one end of 1,3-bis(3-aminopropyl)tetramethyldisiloxane to improve the hydrophobicity of the cotton fibers, resulting in aminosilane-cotton fibers. The remaining amino group reacts with the carboxyl group on gallic acid, and then is placed in a Tris solution to form a benzoquinone structure, resulting in benzoquinone-aminosilane cotton fibers. The benzoquinone group has strong polarity and a conjugated system, which can form a protective film at the friction interface through physical adsorption or chemical action, reducing wear. It can also enhance the heat resistance of the fibers and reduce oxidative degradation at high temperatures.
[0024] In this process, cotton fibers are modified with 1,3-bis(3-aminopropyl)tetramethyldisiloxane (siloxane chain) and gallic acid (benzene ring structure), which introduces more heat-resistant silicon-oxygen bonds (-Si-O-Si-, high bond energy, and better temperature resistance than C-C bonds) and aromatic ring structures on the surface, thus improving the thermal stability of the cotton fibers themselves. In addition, 1,3-bis(3-aminopropyl)tetramethyldisiloxane has hydrophobicity, which can improve the dispersibility of cotton fibers in PAO. The three-dimensional network formed by cotton fibers can reduce the evaporation loss of base oil at high temperatures and enhance the high-temperature continuous lubrication capability. Furthermore, the addition of POSS, which, together with 1,3-bis(3-aminopropyl)tetramethyldisiloxane, imparts strong hydrophobicity to the system, reducing water ingress. At high temperatures, water can exacerbate oil film emulsification and additive hydrolysis, while hydrophobicity can reduce this risk and maintain oil film stability and friction reduction at high temperatures.
[0025] To further improve the lubricity of fiber lubricating oil, zinc sulfide was added. However, the poor dispersibility of zinc sulfide in PAO affected the performance of the fiber lubricating oil. Therefore, free radical polymerization was initiated by AIBN (azobisisobutyronitrile). 1,4-Butanediol diacrylate contains two carbon-carbon double bonds, and the polymer network continuously expands during the free radical polymerization process. The introduction of dodecyl methacrylate can improve the dispersibility of zinc sulfide in PAO, thereby improving the friction reduction and high temperature resistance of the fiber lubricating oil.
[0026] Furthermore, the benzoquinone groups on the benzoquinone-aminosilane cotton fiber can form covalent bonds with the amino groups on amino POSS and amino-modified zinc sulfide, enhancing the stability of the molecular structure and reducing decomposition at high temperatures. At the same time, the conjugated system (the reaction product of benzoquinone and amino groups) and the cage-like structure of POSS can inhibit free radical-induced oxidation reactions, extend the service life of the lubricating oil, and the composite system after the reaction is more hydrophobic. Moreover, the chemical bonding avoids the separation of different polar components, improves the dispersion uniformity in PAO, and reduces the lubrication effect affected by poor dispersion. Detailed Implementation
[0027] In the following detailed embodiments, each part refers to a mass fraction. The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0028] In this embodiment, it should be noted that there are no special restrictions on the manufacturers of the raw materials involved in this invention; exemplarily, they include:
[0029] The CAS number for 1,3-bis(3-aminopropyl)tetramethyldisiloxane is 2469-55-8; the CAS number for EDC·HCl (1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride) is 25952-53-8; the CAS number for NHS (N-hydroxysuccinimide) is 6066-82-6; the CAS number for gallic acid is 149-91-7; and the CAS number for Tris (tris(hydroxymethyl)aminomethane) is 77-86- 1; Acrylamide CAS number is 79-06-1; 1,4-Butanediol diacrylate CAS number is 1070-70-8; Dodecyl methacrylate CAS number is 142-90-5; AIBN (azobisisobutyronitrile) CAS number is 78-67-1; Tackifier is polyisobutylene, catalog number A00293; Antioxidant is Antioxidant 1010; Barium petroleum sulfonate CAS number is 70984-10-0, catalog number W00527.
[0030] Example 1: A method for preparing a motor fiber lubricant, comprising the following steps:
[0031] The preparation method of benzoquinone-aminosilane cotton fiber is as follows: (1) 1,3-bis(3-aminopropyl)tetramethyldisiloxane and oxidized cotton fiber are weighed at a mass ratio of 4:1; 1,3-bis(3-aminopropyl)tetramethyldisiloxane is added to DMF and mixed evenly, oxidized cotton fiber is added, stirring is continued, the temperature is raised to 55℃, stirring is carried out for 2 hours, washed and dried to obtain aminosilane-cotton fiber; (2) 2 parts gallic acid, 2.5 parts EDC·HCl and 1.8 parts NHS are added to methanol, stirred for 2 hours under ice water bath conditions, 10 parts aminosilane-cotton fiber are added, stirring is continued for 40 minutes, stirred at room temperature for 18 hours, washed and dried, added to Tris solution (pH 8.0), stirred evenly for 10 hours, washed and dried to obtain benzoquinone-aminosilane cotton fiber (average particle size is 7μm);
[0032] The preparation method of amino-modified zinc sulfide is as follows: Under nitrogen protection, 4 parts of zinc sulfide are added to 40 parts of ethanol-toluene (the mass ratio of ethanol to toluene is 1:2) and mixed evenly. Then, 0.3 parts of acrylamide, 0.7 parts of 1,4-butanediol diacrylate, 1 part of dodecyl methacrylate, and 0.22 parts of AIBN are added. The mixture is stirred at 70°C for 7 hours, washed, and dried to obtain amino-modified zinc sulfide.
[0033] Step 1: Mix amino POSS and amino-modified zinc sulfide at a mass ratio of 1:3 to obtain a composite additive;
[0034] Step 2: Mix 80 parts of PAO (including PAO10 and PAO4 in a mass ratio of 3:1), 2 parts of tackifier, and 1.2 parts of antioxidant evenly, heat to 105℃, add 10 parts of benzoquinone-aminosilane cotton fiber and stir at 0.03MPa for 40 minutes. At room temperature and pressure, add 1.2 parts of barium petroleum sulfonate and 2 parts of composite additive, and stir for 18 hours to obtain motor fiber lubricating oil.
[0035] Example 2, a method for preparing a motor fiber lubricant, includes the following steps:
[0036] The preparation method of benzoquinone-aminosilane cotton fiber is as follows: (1) 1,3-bis(3-aminopropyl)tetramethyldisiloxane and oxidized cotton fiber are weighed at a mass ratio of 4:1; 1,3-bis(3-aminopropyl)tetramethyldisiloxane is added to DMF and mixed evenly, oxidized cotton fiber is added, stirring is continued, the temperature is raised to 55℃, stirring is carried out for 2 hours, washed and dried to obtain aminosilane-cotton fiber; (2) 2 parts gallic acid, 2.5 parts EDC·HCl and 1.8 parts NHS are added to methanol and stirred for 2 hours under ice water bath conditions, 10 parts aminosilane-cotton fiber are added, stirring is continued for 40 minutes, and then stirred at room temperature for 18 hours. After washing and drying, it is added to Tris solution (pH 8.0), stirred evenly for 10 hours, washed and dried to obtain benzoquinone-aminosilane cotton fiber (average particle size is 7μm);
[0037] The preparation method of amino-modified zinc sulfide is as follows: Under nitrogen protection, 4 parts of zinc sulfide are added to 40 parts of ethanol-toluene (the mass ratio of ethanol to toluene is 1:2) and mixed evenly. Then, 0.3 parts of acrylamide, 0.7 parts of 1,4-butanediol diacrylate, 1 part of dodecyl methacrylate, and 0.22 parts of AIBN are added. The mixture is stirred at 70°C for 7 hours, washed, and dried to obtain amino-modified zinc sulfide.
[0038] Step 1: Mix amino POSS and amino-modified zinc sulfide at a mass ratio of 1:3 to obtain a composite additive;
[0039] Step 2: Mix 85 parts PAO (including PAO10 and PAO4 in a mass ratio of 3:1), 2 parts tackifier, and 1.2 parts antioxidant evenly, heat to 105℃, add 13 parts benzoquinone-aminosilane cotton fiber and stir at 0.03MPa for 40 minutes. At room temperature and pressure, add 1.2 parts barium petroleum sulfonate and 2 parts composite additive, and stir for 18 hours to obtain motor fiber lubricating oil.
[0040] Example 3: A method for preparing a motor fiber lubricant, comprising the following steps:
[0041] The preparation method of benzoquinone-aminosilane cotton fiber is as follows: (1) 1,3-bis(3-aminopropyl)tetramethyldisiloxane and oxidized cotton fiber are weighed at a mass ratio of 4:1; 1,3-bis(3-aminopropyl)tetramethyldisiloxane is added to DMF and mixed evenly, oxidized cotton fiber is added, stirring is continued, the temperature is raised to 55℃, stirring is carried out for 2 hours, washed and dried to obtain aminosilane-cotton fiber; (2) 2 parts gallic acid, 2.5 parts EDC·HCl and 1.8 parts NHS are added to methanol and stirred for 2 hours under ice water bath conditions, 10 parts aminosilane-cotton fiber are added, stirring is continued for 40 minutes, and stirred at room temperature for 18 hours, washed and dried, added to Tris solution (pH 8.0), stirred evenly for 10 hours, washed and dried to obtain benzoquinone-aminosilane cotton fiber;
[0042] The preparation method of amino-modified zinc sulfide is as follows: Under nitrogen protection, 4 parts of zinc sulfide are added to 40 parts of ethanol-toluene (the mass ratio of ethanol to toluene is 1:2) and mixed evenly. Then, 0.3 parts of acrylamide, 0.7 parts of 1,4-butanediol diacrylate, 1 part of dodecyl methacrylate, and 0.22 parts of AIBN are added. The mixture is stirred at 70°C for 7 hours, washed, and dried to obtain amino-modified zinc sulfide.
[0043] Step 1: Mix amino POSS and amino-modified zinc sulfide at a mass ratio of 1:3 to obtain a composite additive;
[0044] Step 2: Mix 80 parts of PAO (including PAO10 and PAO4 in a mass ratio of 3:1), 2 parts of tackifier, and 1.2 parts of antioxidant evenly, heat to 105°C, add 15 parts of benzoquinone-aminosilane cotton fiber and stir at 0.03 MPa for 40 minutes. At room temperature and pressure, add 1.2 parts of barium petroleum sulfonate and 3 parts of composite additive, and stir for 18 hours to obtain motor fiber lubricating oil.
[0045] Comparative Example 1 is based on Example 2, but without the introduction of a benzoquinone group; the remaining operating steps remain unchanged;
[0046] The preparation method of gallic acid-aminosilane cotton fiber is as follows: (1) 1,3-bis(3-aminopropyl)tetramethyldisiloxane and oxidized cotton fiber are weighed at a mass ratio of 4:1; 1,3-bis(3-aminopropyl)tetramethyldisiloxane is added to DMF and mixed evenly, oxidized cotton fiber is added, stirring is continued, the temperature is raised to 55℃, stirring is carried out for 2 hours, washed and dried to obtain aminosilane-cotton fiber; (2) 2 parts gallic acid, 2.5 parts EDC·HCl and 1.8 parts NHS are added to methanol and stirred for 2 hours under ice water bath conditions, 10 parts aminosilane-cotton fiber are added, stirring is continued for 40 minutes, and then stirred at room temperature for 18 hours, washed and dried to obtain gallic acid-aminosilane cotton fiber;
[0047] The preparation method of amino-modified zinc sulfide is as follows: Under nitrogen protection, 4 parts of zinc sulfide are added to 40 parts of ethanol-toluene (the mass ratio of ethanol to toluene is 1:2) and mixed evenly. Then, 0.3 parts of acrylamide, 0.7 parts of 1,4-butanediol diacrylate, 1 part of dodecyl methacrylate, and 0.22 parts of AIBN are added. The mixture is stirred at 70°C for 7 hours, washed, and dried to obtain amino-modified zinc sulfide.
[0048] Step 1: Mix amino POSS and amino-modified zinc sulfide at a mass ratio of 1:3 to obtain a composite additive;
[0049] Step 2: Mix 85 parts PAO (including PAO10 and PAO4 in a mass ratio of 3:1), 2 parts tackifier, and 1.2 parts antioxidant evenly, heat to 105℃, add 13 parts gallic acid-aminosilane cotton fiber and stir at 0.03MPa for 40 minutes. At room temperature and pressure, add 1.2 parts barium petroleum sulfonate and 2 parts composite additive, and stir for 18 hours to obtain motor fiber lubricating oil.
[0050] Comparative Example 2 is based on Example 2, except that no dodecyl methacrylate was added to the amino-modified zinc sulfide; the other operating steps remained unchanged.
[0051] The preparation method of benzoquinone-aminosilane cotton fiber is as follows: (1) 1,3-bis(3-aminopropyl)tetramethyldisiloxane and oxidized cotton fiber are weighed at a mass ratio of 4:1; 1,3-bis(3-aminopropyl)tetramethyldisiloxane is added to DMF and mixed evenly, oxidized cotton fiber is added, stirring is continued, the temperature is raised to 55℃, stirring is carried out for 2 hours, washed and dried to obtain aminosilane-cotton fiber; (2) 2 parts gallic acid, 2.5 parts EDC·HCl and 1.8 parts NHS are added to methanol and stirred for 2 hours under ice water bath conditions, 10 parts aminosilane-cotton fiber are added, stirring is continued for 40 minutes, and stirred at room temperature for 18 hours, washed and dried, added to Tris solution (pH 8.0), stirred evenly for 10 hours, washed and dried to obtain benzoquinone-aminosilane cotton fiber;
[0052] The preparation method of amino-modified zinc sulfide is as follows: under nitrogen protection, 4 parts of zinc sulfide are added to 40 parts of ethanol-toluene (the mass ratio of ethanol to toluene is 1:2) and mixed evenly. Then, 0.3 parts of acrylamide, 0.7 parts of 1,4-butanediol diacrylate and 0.22 parts of AIBN are added. The mixture is stirred at 70°C for 7 hours, washed and dried to obtain amino-modified zinc sulfide.
[0053] Step 1: Mix amino POSS and amino-modified zinc sulfide at a mass ratio of 1:3 to obtain a composite additive;
[0054] Step 2: Mix 85 parts PAO (including PAO10 and PAO4 in a mass ratio of 3:1), 2 parts tackifier, and 1.2 parts antioxidant evenly, heat to 105℃, add 13 parts benzoquinone-aminosilane cotton fiber and stir at 0.03MPa for 40 minutes. At room temperature and pressure, add 1.2 parts barium petroleum sulfonate and 2 parts composite additive, and stir for 18 hours to obtain motor fiber lubricating oil.
[0055] Comparative Example 3 was based on Example 2, but without the addition of amino POSS; the remaining operating steps remained unchanged.
[0056] The preparation method of benzoquinone-aminosilane cotton fiber is as follows: (1) 1,3-bis(3-aminopropyl)tetramethyldisiloxane and oxidized cotton fiber are weighed at a mass ratio of 4:1; 1,3-bis(3-aminopropyl)tetramethyldisiloxane is added to DMF and mixed evenly, oxidized cotton fiber is added, stirring is continued, the temperature is raised to 55℃, stirring is carried out for 2 hours, washed and dried to obtain aminosilane-cotton fiber; (2) 2 parts gallic acid, 2.5 parts EDC·HCl and 1.8 parts NHS are added to methanol and stirred for 2 hours under ice water bath conditions, 10 parts aminosilane-cotton fiber are added, stirring is continued for 40 minutes, and stirred at room temperature for 18 hours, washed and dried, added to Tris solution (pH 8.0), stirred evenly for 10 hours, washed and dried to obtain benzoquinone-aminosilane cotton fiber;
[0057] The preparation method of amino-modified zinc sulfide is as follows: Under nitrogen protection, 4 parts of zinc sulfide are added to 40 parts of ethanol-toluene (the mass ratio of ethanol to toluene is 1:2) and mixed evenly. Then, 0.3 parts of acrylamide, 0.7 parts of 1,4-butanediol diacrylate, 1 part of dodecyl methacrylate, and 0.22 parts of AIBN are added. The mixture is stirred at 70°C for 7 hours, washed, and dried to obtain amino-modified zinc sulfide.
[0058] 85 parts of PAO (including PAO10 and PAO4 in a mass ratio of 3:1), 2 parts of tackifier, and 1.2 parts of antioxidant were mixed evenly and heated to 105°C. 13 parts of benzoquinone-aminosilane cotton fiber were added and stirred at 0.03 MPa for 40 minutes. At room temperature and pressure, 1.2 parts of barium petroleum sulfonate and 2 parts of amino-modified zinc sulfide were added and stirred for 18 hours to obtain motor fiber lubricating oil.
[0059] Test experiment: (1) According to the "Standard Test Method for Evaporation Loss of Greases and Oils" (ASTM D972), the evaporation loss (wt%) of Examples 1-3, Comparative Examples 1-3, and P2AO 180NP was tested. The temperature was set at 100℃ and the time was 22 hours.
[0060] (2) The flash points of Examples 1-3, Comparative Examples 1-3, and P2AO 180NP were tested according to ASTM D92, "Method for determination of flash point and ignition point using Cleveland open cup".
[0061] Table 1
[0062]
[0063] Conclusions: Comparative Example 1, based on Example 3, did not introduce benzoquinone groups; gallic acid was not oxidized to benzoquinone, leading to a decrease in performance; because benzoquinone groups have strong polarity and a conjugated system, they form a protective film at the friction interface, reducing wear; and can enhance the heat resistance of fibers, reducing oxidative degradation at high temperatures; Comparative Example 2, based on Example 3, did not add dodecyl methacrylate to the amino-modified zinc sulfide; the absence of dodecyl methacrylate in amino-modified zinc sulfide reduced hydrophobicity and weakened the encapsulation of the base oil, resulting in a decrease in the performance of Comparative Example 2; Comparative Example 3, based on Example 3, did not add POSS; without amino POSS, the spatial barrier effect of the cage structure is missing, the hydrophobicity and interfacial stability of the composite additive decrease, the base oil volatility is most significant, evaporation loss increases, and the flash point decreases.
[0064] In the existing technology, the evaporation loss of P2AO 180NP is ≤1wt%, and the flash point is ≥230℃. The fiber lubricating oil prepared by this method is expected to replace P2AO 180NP.
[0065] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention.
Claims
1. A process for the preparation of an electrical machine fibre lubricating oil characterised in that: The method comprises the following steps: Step 1: mixing amino POSS and amino modified zinc sulfide according to a certain proportion to obtain a composite additive; Step 2: uniformly mixing PAO, tackifier and antioxidant, heating to 105-110 DEG C, adding benzoquinone-amino silane cotton fiber, stirring at 0.03-0.05 MPa for 40-50 minutes, adding petroleum barium sulfonate and the composite additive under normal temperature and pressure, and stirring for 15-20 hours to obtain motor fiber lubricating oil; The preparation method of the benzoquinone-amino silane cotton fiber is as follows: (1) uniformly mixing 1,3-bis(3-aminopropyl)tetramethyldisiloxane into DMF, adding oxidized cotton fiber, continuously stirring, heating to 50-60 DEG C, and stirring for 2-2.5 hours, and then washing and drying to obtain amino silane-cotton fiber; (2) adding gallic acid, EDC·HCl and NHS into methanol, stirring for 1-2 hours under ice water bath, adding the amino silane-cotton fiber, continuously stirring for 30-40 minutes, stirring for 15-20 hours after being transferred to room temperature, and then washing and drying, adding into Tris solution, uniformly stirring for 8-12 hours, and then washing and drying to obtain the benzoquinone-amino silane cotton fiber; The preparation method of the oxidized cotton fiber is as follows: (1) treating cotton fiber in 18wt% sodium hydroxide solution for 2 hours, and then washing and drying to obtain activated cotton fiber; (2) adding the activated cotton fiber into 6g / mL sodium periodate solution, stirring for 3 hours under 50 DEG C in dark, treating in 0.8g / mL glycerol solution for 1.5 hours, and then washing and drying to obtain the oxidized cotton fiber; The preparation method of the amino modified zinc sulfide is as follows: uniformly mixing zinc sulfide into ethanol-toluene under nitrogen protection, adding acrylamide, 1,4-butanediol diacrylate, dodecyl methacrylate and AIBN, stirring for 7-8 hours under 65-70 DEG C, and then washing and drying to obtain the amino modified zinc sulfide; The preparation method of the amino POSS is as follows: adding 20mL methyltrichlorosilane into 200mL acetone, stirring for 40 minutes under 60 DEG C, slowly dropping deionized water, refluxing for 22 hours, cooling to room temperature, filtering, washing with acetone, adding pyridine and stirring overnight, removing insoluble substances, adding equal volume of mixed solution of concentrated hydrochloric acid and ice water to wash and filter, washing with deionized water until neutral, drying, uniformly mixing 6g of the product with 100mL triethylamine and 200mL tetrahydrofuran, heating to 65 DEG C, adding KH550-tetrahydrofuran (6mL KH550 is added into 100mL tetrahydrofuran to obtain KH550-tetrahydrofuran), refluxing for 22 hours, cooling to room temperature, filtering, washing with equal volume of mixed solution of concentrated hydrochloric acid and ice water, and washing with deionized water until neutral to obtain the amino POSS.
2. A process for the preparation of an electrical machine fibre lubricating oil as claimed in claim 1, characterized in that: The raw material of the motor fiber lubricating oil comprises the following components: 80-85 parts of PAO, 1-3 parts of tackifier, 0.8-1.5 parts of antioxidant, 10-15 parts of benzoquinone-amino silane cotton fiber, 1-1.2 parts of barium petroleum sulfonate, and 2-3 parts of composite additive.
3. A process for the preparation of a motor fibre lubricating oil as claimed in claim 1, wherein: The mass ratio of the amino POSS and the amino-modified zinc sulfide is 1:(2-3).
4. A process for the preparation of a motor fibre lubricating oil as claimed in claim 1, wherein: The mass ratio of the 1,3-bis(3-aminopropyl)tetramethyldisiloxane and the oxidized cotton fiber is (3-5):
1.
5. A process for the preparation of a motor fibre lubricating oil as claimed in claim 1, wherein: The raw material of the benzoquinone-amino silane cotton fiber comprises the following components: 2-3 parts of gallic acid, 2.5-3 parts of EDC·HCl, 1.6-2 parts of NHS, 8-10 parts of amino silane-cotton fiber; the pH of the Tris solution is 7.8-8.
2.
6. A process for the preparation of a motor fibre lubricating oil as claimed in claim 1, wherein: The raw material of the amino-modified zinc sulfide comprises the following components: 3-5 parts of zinc sulfide, 0.3-0.5 parts of acrylamide, 0.7-1 part of 1,4-butanediol diacrylate, 1-1.2 parts of dodecyl methacrylate, 0.2-0.25 parts of AIBN, and 30-50 parts of ethanol-toluene; the mass ratio of ethanol and toluene in the ethanol-toluene is 1:(1-3).
7. The motor fiber lubricating oil is prepared by the preparation method of the motor fiber lubricating oil according to any one of claims 1-6.
Citation Information
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