Open gear oil as well as preparation method and application thereof

Abstract

The invention provides open gear oil as well as a preparation method and application thereof, and belongs to the technical field of industrial open gear lubrication. Layered long-chain alkyl antimony mercaptide is adopted as a solid lubricant, belongs to an organic-inorganic hybrid material, has good compatibility with lubricating oil, is compounded with a dispersing agent, realizes good dispersion stability, has good compounding synergy with gear oil antioxidants, tackifiers, extreme pressure anti-wear agents and antirust agents, and can be used for lubricating oil. Therefore, the solid lubricant component in the open gear oil provided by the invention has the characteristics of comprehensive element composition and crystal structure of the solid lubricant, shows excellent extreme pressure, bearing, anti-wear, anti-friction and lubricating properties, is suitable for various harsh working conditions, and effectively saves energy and reduces consumption.

Description

Technical Field

[0001] The invention relates to the technical field of industrial open gear lubrication, and in particular to an open gear oil and a preparation method and application thereof. Background Art

[0002] As one of the key components of power transmission, open gears play an important role in large-scale equipment in industries such as cement production, metal smelting, ore mining, and fertilizer manufacturing. In actual applications, gear damage caused by insufficient lubrication or lubrication failure accounts for about 18.2% of the total number of failures, which highlights the key role of lubricants in the normal operation of open gears. At present, there is a lack of lubricating products for open gears on the market, resulting in a limited variety of lubricants recommended by equipment manufacturers, which in turn makes low-grade oils or alternative oils widely used in equipment operation. Therefore, it is necessary to develop new high-performance open gear oils.

[0003] Open gear oil is mainly used in extra-large rotating equipment with low speed and heavy load. The unit area load of the transmission gear tooth surface is high, which is easy to generate noise and vibration. Therefore, the gear oil must have a strong load-bearing capacity. Solid lubricants have the advantages of wide operating temperature range, strong load-bearing capacity, and good anti-stick and slip properties. They are one of the important additives to improve the load-bearing capacity of gear oil. High-quality solid lubricants can also provide protection for metal surfaces in oil products, enhance the transmission efficiency of gears, and save energy. According to research, high-quality extreme pressure open gear oil products generally add solid lubricants such as graphite and molybdenum disulfide to improve performance. This type of material has a typical layered crystal structure and can exert good anti-wear properties, but traditional pure inorganic solid lubricants have problems such as insufficient dispersibility in lubricating oils. Summary of the invention

[0004] The object of the present invention is to provide an open gear oil and a preparation method and application thereof, wherein the open gear oil has excellent extreme pressure, load-bearing, anti-wear and friction-reducing properties.

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

[0006] The present invention provides an open gear oil, comprising the following raw materials in parts by weight:

[0007]

[0008]

[0009] The solid lubricant is a long-chain alkyl mercaptan antimony with a layered structure.

[0010] Preferably, the method for preparing the layered long-chain alkyl antimony thiolate comprises the following steps:

[0011] The antimony source, the sulfur source and the organic solvent are mixed to carry out a hybridization reaction to obtain a long-chain alkylthiol antimony with a layered structure;

[0012] The antimony source includes antimony trichloride, antimony acetate or antimony trioxide;

[0013] The sulfur source includes n-dodecyl mercaptan, 1-tetradecyl mercaptan or 1-hexadecyl mercaptan.

[0014] Preferably, the molar ratio of the antimony element in the antimony source to the sulfur element in the sulfur source is 1:(3-8); the temperature of the hybridization reaction is 25-100° C., and the time is 1-10 h.

[0015] Preferably, the base oil is one or more of silicone oil, alkylbenzene oil, mineral hydrocarbon oil, synthetic hydrocarbon oil, polyether oil, and synthetic ester oil.

[0016] Preferably, the dispersant is one or more of bis-alkenyl succinimide, polyisobutylene monosuccinimide and boron phosphated polyisobutylene bis-succinimide.

[0017] Preferably, the antioxidant is one or more of alkylated N-phenyl-α-naphthylamine, butyl octyl diphenylamine, 2,6-di-tert-butyl-p-cresol and zinc diamyl dithiocarbamate; the tackifier is one or more of ethylene propylene copolymer, methacrylate and styrene isoprene.

[0018] Preferably, the extreme pressure anti-wear agent is one or more of sulfided olefins, di-n-butyl phosphite, alkyl thiophosphates and sulfided triglycerides; the rust inhibitor is one or more of dodecenylsuccinic acid, zinc cyclohexanecarboxylate and alkyl sulfonate rust inhibitors.

[0019] The present invention provides a method for preparing the open gear oil described in the above technical solution, comprising the following steps:

[0020] According to the mass ratio, the base oil is heated to 35-90° C., a dispersant and a tackifier are added, and a first stirring and mixing is performed to obtain a first mixed material;

[0021] The first mixed material is mixed with an extreme pressure anti-wear agent and a solid lubricant, and a second stirring and mixing is performed to obtain a second mixed material;

[0022] The second mixed material is mixed with an antioxidant and a rust inhibitor, and after a third stirring and mixing process, degassing is performed to obtain an open gear oil.

[0023] Preferably, the first stirring and mixing has a rotation speed of 300-1000 r / min and a time of 30-90 min; the second stirring and mixing has a rotation speed of 200-800 r / min and a time of 1-5 h; the third stirring and mixing has a rotation speed of 200-800 r / min and a time of 1-3 h.

[0024] The present invention provides the use of the open gear oil described in the above technical solution or the open gear oil prepared by the preparation method described in the above technical solution in a low-speed and heavy-load extra-large rotating equipment.

[0025] The present invention provides an open gear oil, which adopts organic-inorganic hybrid material layered long-chain alkyl mercaptan Sb (SC n H 2n+1 )3 (where n=12, 14 or 16) as a solid lubricant, has a layered structure and a polarity close to that of the base oil, contains classic lubricating extreme pressure elements, has good compatibility with lubricating oil, and is easy to disperse. The sulfur and antimony elements in this material are both classic lubricating elements, among which sulfur is a classic lubricating extreme pressure element. Under high temperature and load conditions, sulfur reacts with metal to form a boundary lubricating film with low shear strength, thereby providing extreme pressure performance; antimony is a classic lubricating and anti-wear element. At the same time, this type of material has a layered crystal structure, and its single layer is a sandwich structure, with an inorganic two-dimensional Sb / S center layer between two organic layers in which two upright alkyl chains are covalently bonded to sulfur atoms. The solid lubricant component in the open gear oil provided by the present invention has the above-mentioned comprehensive elemental composition and crystal structure characteristics, exhibits excellent extreme pressure, load-bearing, anti-wear, and friction-reducing lubrication properties, is suitable for a variety of harsh working conditions, and effectively saves energy and reduces consumption.

[0026] The solid lubricant preparation method adopted by the present invention is simple and easy to implement, can effectively reduce the cost of industrial application, and is easy to realize industrialization.

[0027] The present invention adopts layered long-chain alkyl mercaptan antimony as a solid lubricant for the first time. As an organic-inorganic hybrid material, it has good compatibility with lubricating oil and is compounded with a dispersant to achieve good dispersion stability. In addition, the solid lubricant layered long-chain alkyl mercaptan antimony has good compound synergy with classic antioxidants, tackifiers, extreme pressure antiwear agents, and rust inhibitors for gear oil. The open gear oil provided by the present invention has high extreme pressure performance, effectively prolongs the service life of the open gear oil, and reduces maintenance costs and the frequency of failures. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 The XRD diagram of the layered long-chain alkyl mercaptan antimony product obtained in Examples 1 to 3. DETAILED DESCRIPTION

[0029] In the present invention, unless otherwise specified, the required raw materials or reagents are commercially available products well known to those skilled in the art.

[0030] The present invention provides an open gear oil, comprising the following raw materials in parts by weight:

[0031]

[0032] The solid lubricant is a long-chain alkyl mercaptan antimony with a layered structure.

[0033] Calculated by weight, the raw materials for preparing the open gear oil provided by the present invention include 85 to 95 parts of base oil, preferably 88 to 92 parts.

[0034] In the present invention, the base oil is preferably one or more of silicone oil, alkylbenzene oil, mineral hydrocarbon oil, synthetic hydrocarbon oil, polyether oil, and synthetic ester oil. When the base oil is two or more of the above, the present invention has no special restrictions on the ratio of different types of base oils, and any ratio is acceptable.

[0035] In the present invention, the silicone oil is preferably dimethyl silicone oil or ethyl silicone oil; the alkylbenzene oil is preferably V-9050; the mineral hydrocarbon oil is preferably 150BS or 120BS; the synthetic hydrocarbon oil is preferably PAO100 or PAO300; the polyether oil is preferably polyethylene glycol 200; and the synthetic ester oil is preferably trimethylolpropane oleate.

[0036] Based on the mass fraction of the base oil, the raw materials for preparing the open gear oil provided by the present invention include 0.5 to 1.5 parts of a dispersant, preferably 0.6 to 1.2 parts, and more preferably 0.9 to 1.0 parts; the dispersant is one or more of diene succinimide, polyisobutylene monosuccinimide and boron phosphated polyisobutylene bissuccinimide; when the dispersant is two or more of the above, the present invention has no special limitation on the ratio of different types of dispersants, and any ratio is acceptable.

[0037] Based on the mass fraction of the base oil, the raw material for preparing the open gear oil provided by the present invention includes 0.1 to 1.5 parts of antioxidant, preferably 0.3 to 1.3 parts, more preferably 0.6 to 1.2 parts, and further preferably 0.8 to 1.0 parts. In the present invention, the antioxidant is one or more of alkylated N-phenyl-α-naphthylamine, butyl octyl diphenylamine, 2,6-di-tert-butyl-p-cresol and zinc diamyl dithiocarbamate; when the antioxidant is two or more of the above, the present invention has no special limitation on the ratio of different types of antioxidants, and any ratio is acceptable.

[0038] Based on the mass fraction of the base oil, the raw materials for preparing the open gear oil provided by the present invention include 1.8 to 4.0 parts of a tackifier, preferably 2.0 to 3.5 parts, and more preferably 2.3 to 3.0 parts. The tackifier is one or more of ethylene propylene copolymer, methacrylate and styrene isoprene. When the tackifier is two or more of the above, the present invention has no special limitation on the ratio of different types of tackifiers, and any ratio is acceptable.

[0039] Based on the mass fraction of the base oil, the raw materials for preparing the open gear oil provided by the present invention include 2.0 to 5.0 parts of solid lubricant, preferably 2.2 to 4.5 parts, more preferably 2.5 to 3.5 parts, and further preferably 3.0 parts.

[0040] In the present invention, the solid lubricant is a long-chain alkyl antimony mercaptan with a layered structure, and the preparation method of the long-chain alkyl antimony mercaptan with a layered structure preferably comprises the following steps:

[0041] An antimony source, a sulfur source and an organic solvent are mixed to carry out a hybridization reaction to obtain a long-chain alkyl mercaptan antimony with a layered structure; the antimony source includes antimony trichloride, antimony acetate or antimony trioxide; the sulfur source includes n-dodecyl mercaptan, 1-tetradecyl mercaptan or 1-hexadecyl mercaptan.

[0042] The layered long-chain alkyl mercaptan Sb(SC n H 2n+1 )3 (wherein n = 12, 14 or 16) is preferably prepared according to the prior art [Yu N, Zhu Y, Wang T, et al. Long-Chain Molecular Crystals Antimony (III) Alkanethiolates Sb (SC n H 2n+1 )3(n≥12):Synthesis,Crystal and ElectronicStructures,and Supramolecular Self-Assembly via Secondary Interactions[J].Inorganic chemistry,2024,63,17651-17661].

[0043] In the present invention, the molar ratio of the antimony element in the antimony source to the sulfur element in the sulfur source is preferably 1:(3-8), more preferably 1:(3-4); the temperature of the hybridization reaction is preferably 25-100°C, more preferably 40-80°C, further preferably 60°C, and the time is preferably 1-10h, more preferably 3-8h, further preferably 4-5h.

[0044] In the present invention, the organic solvent is preferably DMF (N,N-dimethylformamide) or anhydrous ethanol. The present invention has no special limitation on the amount of the organic solvent, which can be adjusted according to actual needs to ensure the completion of the reaction.

[0045] The present invention preferably dissolves the antimony source in an organic solvent, drops a sulfur source into the obtained mixed solution, stirs for reaction, washes with DMF or anhydrous ethanol, filters and then dries at room temperature to obtain a long-chain alkyl mercaptan antimony with a layered structure.

[0046] Based on the mass fraction of the base oil, the raw materials for preparing the open gear oil provided by the present invention include 0 to 2.0 parts of extreme pressure anti-wear agent, preferably 0.5 to 1.5 parts, and more preferably 1.0 parts. The extreme pressure anti-wear agent is one or more of sulfided olefins, di-n-butyl phosphite, alkyl thiophosphates, and sulfided triglycerides; the sulfided olefins are preferably sulfided isobutylene, and the alkyl thiophosphates are preferably zinc dialkyl dithiophosphates.

[0047] When the extreme pressure and anti-wear agents are two or more of the above, the present invention has no special limitation on the ratio of different types of extreme pressure and anti-wear agents, and any ratio is acceptable.

[0048] Based on the mass fraction of the base oil, the raw materials for preparing the open gear oil provided by the present invention include 0.6 to 1.0 parts of a rust inhibitor, preferably 0.7 to 0.9 parts; the rust inhibitor is one or more of dodecenylsuccinic acid, zinc cyclohexane and alkyl sulfonate rust inhibitors; the alkyl sulfonate rust inhibitor is preferably calcium dinonylnaphthalenesulfonate.

[0049] When the rust inhibitor is two or more of the above, the present invention has no special limitation on the ratio of different types of rust inhibitors, and any ratio is acceptable.

[0050] The present invention provides a method for preparing the open gear oil described in the above technical solution, comprising the following steps:

[0051] According to the mass ratio, the base oil is heated to 35-90° C., a dispersant and a tackifier are added, and a first stirring and mixing is performed to obtain a first mixed material;

[0052] The first mixed material is mixed with an extreme pressure anti-wear agent and a solid lubricant, and a second stirring and mixing is performed to obtain a second mixed material;

[0053] The second mixed material is mixed with an antioxidant and a rust inhibitor, and after a third stirring and mixing process, degassing is performed to obtain an open gear oil.

[0054] In the present invention, the base oil is more preferably heated to 45 to 80°C, and further preferably to 50 to 60°C.

[0055] In the present invention, the rotation speed of the first stirring and mixing is preferably 300-1000 r / min, more preferably 400-500 r / min, and the time is preferably 30-90 min; the rotation speed of the second stirring and mixing is preferably 200-800 r / min, more preferably 400-600 r / min, and the time is preferably 1-5 h, more preferably 2-4 h; the rotation speed of the third stirring and mixing is preferably 200-800 r / min, more preferably 400-600 r / min, and the time is preferably 1-3 h, more preferably 2-3 h.

[0056] The present invention preferably puts the base oil into a reactor according to the mass ratio, stirs and heats to 35-90°C; puts the dispersant and the viscosity enhancer into the reactor according to the proportion, and performs the first stirring and mixing; puts the extreme pressure anti-wear agent and the solid lubricant into the reactor according to the proportion, and performs the second stirring and mixing; adds the antioxidant and the rust inhibitor into the reactor in sequence according to the proportion, and performs the third stirring and mixing, and degassing to obtain the open gear oil with high extreme pressure performance.

[0057] The layered long-chain alkyl mercaptan antimony in the present invention can produce a compounding effect with functional additives due to its elemental and structural characteristics:

[0058] (1) Synergy with antioxidants: Layered long-chain alkyl mercaptan antimony itself has excellent antioxidant properties. The thiol group in its molecule can produce adsorption with the metal surface, build a protective layer on the metal surface, effectively isolate oxygen and oxidizing substances from contact with the metal surface, and thus inhibit the oxidation process. Traditional antioxidants (such as phenolic or amine antioxidants) mainly prevent oxidation reactions by capturing free radicals and decomposing peroxides. The present invention combines layered long-chain alkyl mercaptan antimony with traditional antioxidants to exert antioxidant effects on multiple levels, thereby significantly improving the antioxidant capacity of gear oil;

[0059] (2) Synergy with thickeners: Thickeners are oil-soluble chain polymers with molecular weights ranging from tens of thousands to millions. Thickeners dissolve in lubricating oil. As the temperature of the lubricating oil increases, the filaments stretch, the effective volume increases, and the resistance to the flow of the lubricating oil increases, resulting in a relatively significant increase in the viscosity of the lubricating oil. The layered long-chain alkyl mercaptan antimony in the present invention has a relatively long alkyl chain, which can play a role in stretching the filaments within a certain range. The combination of the two can exert a better synergistic effect.

[0060] (3) Synergy with extreme pressure anti-wear agents: Extreme pressure agents generally contain specific lubricating elements. Under extreme environments such as high temperature and high pressure, extreme pressure anti-wear additives react chemically with the metal surface to form a protective layer with low shear strength, effectively reducing friction and wear. Layered long-chain alkyl antimony mercaptides also contain the classic lubricating extreme pressure element sulfur, which can form a protective layer on the metal surface. The present invention uses layered long-chain alkyl antimony mercaptides and extreme pressure anti-wear agents in combination. The protective layers formed can complement each other and work together to improve the integrity and firmness of the protective layer, thereby enhancing the wear resistance of the gear oil under extreme pressure conditions;

[0061] (4) Synergy with rust inhibitors: The function of rust inhibitors is to form a strong adsorption film on the metal surface to inhibit the contact of oxygen and water, especially water, with the metal surface, so that the metal will not rust. Rust inhibitors are composed of strong polar groups and appropriate lipophilic groups. Layered long-chain alkyl mercaptan antimony has a certain polarity and can also form an adsorption film on the metal surface, which overlaps and cooperates with the protective film of the rust inhibitor, further enhancing the protective effect on the metal surface and improving the rust prevention performance of the gear oil.

[0062] The present invention provides the use of the open gear oil described in the above technical solution or the open gear oil prepared by the preparation method described in the above technical solution in a low-speed, heavy-loaded extra-large rotating device. The present invention has no special limitation on the method of application, and the application can be carried out according to methods well known in the art.

[0063] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0064] Example 1

[0065] 1.0 g (0.0033 mol) of antimony acetate and 50 mL of DMF were added to a 100 mL beaker. 2.59 g (0.01 mol) of 1-hexadecanethiol was added dropwise to the resulting mixture. A white flocculent precipitate was immediately formed. The precipitate was stirred at 25 °C for 1 h, washed with anhydrous ethanol, filtered, and dried at room temperature to obtain layered hexadecanethiol antimony Sb (SC 16 H 33 )3.

[0066] 95g 150BS (Shenzhen Zhongruntong Chemical Co., Ltd.) was put into a reactor, stirred and heated to 90°C; 0.5g polyisobutylene monosuccinimide (T151, Jinzhou Kangtai Lubricant Additive Co., Ltd.) and 1.8g ethylene propylene copolymer (T613, Duorun Petrochemical Co., Ltd.) were put into the reactor in proportion and stirred at 1000r / min for 90min; 1.0g zinc dialkyl dithiophosphate (T202, Wuxi Nanfang Petroleum Additive Co., Ltd.) and 2.0g of the layered hexadecyl mercaptan prepared above were sequentially put into the reactor in proportion and stirred at 800r / min for 5h; 0.1g butyl octyl diphenylamine (T534, Beijing Xingpu Fine Chemical Technology Development Co., Ltd.), 0.6g neutral dinonyl naphthalene sulfonate calcium (Vanlube RI-CSN, Vanderbilt Company) were added into the reactor in sequence and stirred at a speed of 800 r / min for 3 h; degassing was performed before discharging to obtain an open gear oil containing layered hexadecyl antimony mercaptan.

[0067] Example 2

[0068] 4.02 g (0.0138 mol) of antimony trioxide and 80 mL of anhydrous ethanol were added to a 100 mL beaker, and 12.64 g (0.0548 mol) of 1-tetradecyl mercaptan was added dropwise to the resulting mixture. A white flocculent precipitate was immediately formed. The mixture was reacted at 100 ° C and stirred for 10 h. After washing with DMF, filtering and drying at room temperature, layered tetradecyl mercaptan antimony Sb (SC 14 H 29 )3.

[0069] 88g PAO300 (Shenzhen Huameite Lubrication Technology Co., Ltd.) was put into the reactor, stirred and heated to 80°C; 1.0g of diene succinimide (T154, Shanghai Hairun Additive Co., Ltd.) and 3.5g of styrene isoprene (T661, Binzhou Kunhou Chemical Co., Ltd.) were put into the reactor in proportion and stirred at 800r / min for 1h; 1.5g of sulfided isobutylene (T321, Binzhou Kunhou Chemical Co., Ltd.) and 4.5g of layered tetradecyl antimony mercaptan were put into the reactor in proportion and stirred at 600r / min for 4h; 1.0g of butyl octyl diphenylamine (T534, Beijing Xingpu Fine Chemical Technology Development Co., Ltd.) and 0.6g of dodecenyl succinic acid (T746, Wuxi Nanfang Petroleum Additive Co., Ltd.) were added into the reactor in proportion and stirred at 600r / min for 3h; degassing was performed before discharging to obtain an open gear oil containing layered tetradecyl antimony mercaptan.

[0070] Example 3

[0071] 1.0 g (0.0033 mol) of antimony acetate and 50 mL of DMF were added to a 100 mL beaker, and 2.59 g (0.0128 mol) of n-dodecyl mercaptan was added dropwise to the resulting mixture. A white flocculent precipitate was immediately formed. The mixture was reacted at 40 ° C and stirred for 5 h. After washing with anhydrous ethanol, the mixture was filtered and dried at room temperature to obtain layered dodecyl mercaptan antimony Sb (SC 12 H 25 )3.

[0072] 85g 120BS (Shenzhen Zhongruntong Chemical Co., Ltd.) was put into the reactor, stirred and heated to 35°C; 1.5g boron phosphated polyisobutylene bissuccinimide (KT 1356PB, Jinzhou Kangtai Lubricant Additive Co., Ltd.) and 4.0g ethylene propylene copolymer (T613, Duorun Petrochemical Co., Ltd.) were put into the reactor in proportion and stirred at 300r / min for 30min; 2.0g di-n-butyl phosphite (T304, Shandong Ruixing Flame Retardant Technology Co., Ltd.) and 5.0g layered dodecyl mercaptan antimony were put into the reactor in proportion and stirred at 200r / min for 1h; 1.5g 2,6-di-tert-butyl-p-cresol (RC7110, Rhein Chemie De Cairun Co., Ltd.) and 1.0 g of zinc cyclohexane (RC4530, Rhein Chemie Co., Ltd.) were added into the reaction kettle in sequence and stirred at 200 r / min for 1 h. The open gear oil containing layered antimony dodecyl mercaptan was obtained by degassing before discharging.

[0073] Example 4

[0074] 4.02 g (0.0138 mol) of antimony trioxide and 80 mL of DMF were added to a 100 mL beaker. 12.64 g (0.0548 mol) of 1-tetradecyl mercaptan was added dropwise to the resulting mixture. A white flocculent precipitate was immediately formed. The mixture was reacted at 100 ° C and stirred for 10 h. After washing with anhydrous ethanol, filtering and drying at room temperature, layered tetradecyl mercaptan antimony Sb (SC 14 H 29 )3.

[0075] 95g of polyethylene glycol 200 (Haian Petrochemical Plant, Jiangsu Province) was put into a reactor, stirred and heated to 45°C; 0.6g of polyisobutylene monosuccinimide (T151, Jinzhou Kangtai Lubricant Additive Co., Ltd.) and 1.8g of ethylene propylene copolymer (T613, Duorun Petrochemical Co., Ltd.) were put into the reactor in proportion and stirred at 500r / min for 30min; 1.0g of zinc dialkyl dithiophosphate (T202, Wuxi Nanfang Petroleum Additive Co., Ltd.) and 2.2g of layered tetradecyl antimony mercaptan were put into the reactor in proportion and stirred at 400r / min for 2h; 0.8g of zinc diamyl dithiocarbamate (VanlubeAZ, Vanderbilt Company) and 0.7g of neutral calcium dinonylnaphthalenesulfonate (Vanlube RI-CSN, Vanderbilt Company) were added into the reactor in sequence and stirred at 400 r / min for 2 h. The open gear oil containing layered tetradecyl antimony mercaptan was obtained by degassing before discharging.

[0076] Example 5

[0077] 1.0 g (0.0033 mol) of antimony acetate and 50 mL of anhydrous ethanol were added to a 100 mL beaker, and 2.59 g (0.01 mol) of 1-hexadecanethiol was added dropwise to the resulting mixture. A white flocculent precipitate was immediately formed. The mixture was reacted at 60 ° C and stirred magnetically for 3 h. After washing with DMF, filtering and drying at room temperature, layered hexadecylthiocarbamide antimony Sb (SC 16 H 33 )3.

[0078] 85g of dimethyl silicone oil (Shandong Longhui Chemical Co., Ltd.) was put into the reactor, stirred and heated to 40°C; 1.5g of diene succinimide (T154, Shanghai Hairun Additive Co., Ltd.) and 4.0g of styrene isoprene (T661, Binzhou Kunhou Chemical Co., Ltd.) were put into the reactor in proportion and stirred at 400r / min for 1h; 1.5g of di-n-butyl phosphite (T304, Shandong Ruixing Flame Retardant Technology Co., Ltd.) and 4.5g of layered hexadecyl mercaptan antimony were put into the reactor in proportion and stirred at 400r / min for 2h; 0.5g of 2,6-di-tert-butyl-p-cresol (RC7110, Rhein Chemie De Cairun Co., Ltd.) and 1.0 g of zinc cyclohexaneate (RC4530, Rhein Chemie Co., Ltd.) were added to the reactor in sequence and stirred at 400 r / min for 1 h. Degassing was performed before discharging to obtain an open gear oil containing layered hexadecyl mercaptan antimony.

[0079] Example 6

[0080] In a 100 mL beaker, 1.85 g (0.0081 mol) of antimony trichloride and 50 mL of anhydrous ethanol were added, and 6.08 g (0.03 mol) of n-dodecyl mercaptan was added dropwise to the resulting mixture. A white flocculent precipitate was immediately formed. The mixture was reacted at 80 ° C and stirred magnetically for 8 h. After washing with DMF, filtering and drying at room temperature, layered dodecyl mercaptan antimony Sb (SC 12 H 25 )3.

[0081] 88g of ethyl silicone oil (Hubei Chenghai Chemical Co., Ltd.) was added to the reactor, stirred and heated to 50°C; 1.0g of boron phosphated polyisobutylene bissuccinimide (KT 1356PB, Jinzhou Kangtai Lubricant Additive Co., Ltd.), 3.5g methacrylate (KFD9100, Shenyang Great Wall Lubricant Manufacturing Co., Ltd.) were put into the reactor and stirred at 600r / min for 30min; 1.5g sulfurized triglyceride (RC2410, Rhein Chemie Company) and 4.0g layered antimony dodecyl mercaptan were added to the reactor in proportion, and stirred at 400r / min for 4h; 1.0g butyl octyl diphenylamine (T534, Beijing Xingpu Fine Chemical Technology Development Co., Ltd.) and 0.7g dodecenyl succinic acid (T746, Wuxi Nanfang Petroleum Additive Co., Ltd.) were added to the reactor in proportion, and stirred at 500r / min for 3h; degassing was performed before discharging to obtain open gear oil containing layered antimony dodecyl mercaptan.

[0082] Example 7

[0083] 1.0 g (0.0033 mol) of antimony acetate and 50 mL of DMF were added to a 100 mL beaker. 2.59 g (0.01 mol) of 1-hexadecanethiol was added dropwise to the resulting mixture. A white flocculent precipitate was immediately formed. The precipitate was stirred at 25 °C for 4 h, washed with anhydrous ethanol, filtered, and dried at room temperature to obtain layered hexadecanethiol antimony Sb (SC 16 H 33 )3.

[0084] 92g PAO100 (Shenzhen Huameite Lubrication Technology Co., Ltd.) was put into the reactor, stirred and heated to 50°C; 0.9g polyisobutylene monosuccinimide (T151, Jinzhou Kangtai Lubricant Additive Co., Ltd.) and 2.3g ethylene propylene copolymer (T613, Duorun Petrochemical Co., Ltd.) were put into the reactor in proportion and stirred at 600r / min for 1h; 1.5g sulfided isobutylene (T321, Binzhou Kunhou Chemical Co., Ltd.) and 3.5g layered hexadecyl mercaptan antimony were put into the reactor in proportion and stirred at 500r / min for 3h; 1.3g alkylated N-phenyl-α-naphthylamine (Vanlube 1202, Vanderbilt Company), 0.9g neutral dinonylnaphthalenesulfonate calcium (Vanlube RI-CSN, Vanderbilt Company) were added into the reactor in sequence and stirred at a speed of 600 r / min for 2 h. The open gear oil containing layered hexadecyl antimony mercaptan was obtained by degassing before discharging.

[0085] Example 8

[0086] 4.02 g (0.0138 mol) of antimony trioxide and 80 mL of DMF were added to a 100 mL beaker. 12.64 g (0.0548 mol) of 1-tetradecyl mercaptan was added dropwise to the resulting mixture. A white flocculent precipitate was immediately formed. The mixture was reacted at 80 ° C and stirred magnetically for 10 h. The mixture was washed with anhydrous ethanol, filtered, and dried at room temperature to obtain layered tetradecyl mercaptan antimony Sb (SC 14 H 29 )3.

[0087] 95g V-9050 (Shanghai Daopu Chemical Co., Ltd.) was added to the reactor, stirred and heated to 60°C; 0.8g diene succinimide (T154, Shanghai Hairun Additive Co., Ltd.) and 1.8g styrene isoprene (T661, Binzhou Kunhou Chemical Co., Ltd.) were added to the reactor in proportion and stirred at 400r / min for 1h; 1.0g zinc dialkyl dithiophosphate (T202, Wuxi Nanfang Petroleum Additive Co., Ltd.) and 3.0g layered tetradecyl mercaptan antimony were added to the reactor in proportion and stirred at 400r / min for 2h; 0.8g zinc diamyl dithiocarbamate (Vanlube AZ, Vanderbilt Company) and 0.8g dodecenylsuccinic acid (T746, Wuxi Nanfang Petroleum Additives Co., Ltd.) were added into the reactor in sequence and stirred at 500r / min for 1h. The open gear oil containing layered tetradecyl antimony mercaptan was obtained by degassing before discharging.

[0088] Example 9

[0089] 1.85 g (0.0081 mol) of antimony trichloride and 100 mL of anhydrous ethanol were added to a 100 mL beaker, and 6.08 g (0.03 mol) of n-dodecyl mercaptan was added dropwise to the resulting mixture. A white flocculent precipitate was immediately formed. The mixture was reacted at 60 ° C and stirred for 5 h. After washing with DMF, filtering and drying at room temperature, layered dodecyl mercaptan antimony Sb (SC 12 H 25 )3.

[0090] 85g of trimethylolpropane oleate (Shandong Xinfa Ruijie New Material Technology Co., Ltd.) was put into a reactor, stirred and heated to 45°C; 1.2g of boron phosphated polyisobutylene bissuccinimide (KT 1356PB, Jinzhou Kangtai Lubricant Additive Co., Ltd.) and 4.0g of methyl methacrylate (KFD9100, Shenyang Great Wall Lubricant Manufacturing Co., Ltd.) were put into the reactor in proportion and stirred at 500r / min for 30min; 1.5g of di-n-butyl phosphite (T304, Shandong Ruixing Flame Retardant Technology Co., Ltd.) and 5.0g of layered dodecyl mercaptan were put into the reactor in proportion and stirred at 400r / min for 4h; 0.3g of 2,6-di-tert-butyl-p-cresol (RC7110, Rhein Chemie De Cairun Co., Ltd.) and 1.0 g of zinc cyclohexane (RC4530, Rhein Chemie Co., Ltd.) were added into the reaction kettle in sequence and stirred at 400 r / min for 3 h. The open gear oil containing layered antimony dodecyl mercaptan was obtained by degassing before discharging.

[0091] Example 10

[0092] 1.85 g (0.0081 mol) of antimony trichloride and 100 mL of DMF were added to a 100 mL beaker, and 6.08 g (0.03 mol) of n-dodecyl mercaptan was added dropwise to the resulting mixture. A white flocculent precipitate was immediately formed. The mixture was reacted at 40 ° C and stirred for 8 h. After washing with anhydrous ethanol, filtering and drying at room temperature, layered dodecyl mercaptan antimony Sb (SC 12 H 25 )3.

[0093] 92g 150BS (Shenzhen Zhongruntong Chemical Co., Ltd.) was put into a reactor, stirred and heated to 90°C; 0.9g boron phosphated polyisobutylene bissuccinimide (KT 1356PB, Jinzhou Kangtai Lubricant Additive Co., Ltd.) and 2.3g methacrylate (KFD9100, Shenyang Great Wall Lubricant Manufacturing Co., Ltd.) were put into the reactor in proportion and stirred at 1000r / min for 90min; 1.5g sulfurized triglyceride (RC2410, Rhein Chemie) and 2.5g layered dodecyl mercaptan antimony were put into the reactor in proportion and stirred at 800r / min for 5h; 0.6g alkylated N-phenyl-α-naphthylamine (Vanlube1202, Vanderbilt), 0.9g neutral dinonylnaphthalenesulfonate calcium (Vanlube RI-CSN, Vanderbilt Company) were added into the reactor in sequence and stirred at a speed of 800 r / min for 3 h; degassing was performed before discharging to obtain an open gear oil containing layered dodecyl antimony mercaptan.

[0094] Comparative Example 1

[0095] The solid lubricant was molybdenum disulfide (Henan Bangrun Chemical Products Co., Ltd.).

[0096] 92g 150BS (Shenzhen Zhongruntong Chemical Co., Ltd.) was added to the reactor, stirred and heated to 90°C; 0.9g boron phosphated polyisobutylene bissuccinimide (KT 1356PB, Jinzhou Kangtai Lubricant Additive Co., Ltd.) and 2.3g methacrylate (KFD9100, Shenyang Great Wall Lubricant Manufacturing Co., Ltd.) were added to the reactor in proportion and stirred at 1000r / min for 90min; 1.5g sulfurized triglyceride (RC2410, Rhein Chemie) and 2.5g molybdenum disulfide were added to the reactor in proportion and stirred at 800r / min for 5h; 0.6g alkylated N-phenyl-α-naphthylamine (Vanlube1202, Vanderbilt), 0.9g neutral calcium dinonylnaphthalenesulfonate (Vanlube RI-CSN, Vanderbilt Company) were added into the reactor in sequence and stirred at a speed of 800 r / min for 3 h; degassing was performed before discharging to obtain an open gear oil containing molybdenum disulfide.

[0097] Characterization and performance testing

[0098] 1) Figure 1 is the XRD pattern of the long-chain alkyl mercaptan antimony product prepared in Examples 1 to 3; Figure 1 It can be seen that the layered long-chain alkylthiolate antimony Sb(SC n H 2n+1 )3 (n=12, 14 and 16) samples.

[0099] 2) The samples prepared in the above examples were subjected to tribological (including physical, chemical and lubrication) performance tests:

[0100] Measure the lubricating oil copper sheet corrosion according to GB / T5096 standard;

[0101] Determine kinematic viscosity according to GB / T265 standard and its method;

[0102] According to GB / T3142 and SH / T0204-92 standards, the maximum no-seizure load P is determined by the four-ball method. B , sintering load P D and wear spot diameter WSD;

[0103] The friction reduction performance was measured using SRV according to ASTM D5707 and expressed as the coefficient of friction (μ).

[0104] The test results are shown in Table 1.

[0105] Table 1 Performance data of open gear oil in Examples 1 to 10 and Comparative Example 1

[0106]

[0107]

[0108] From the data comparison in Table 1, it can be seen that the open gear oil containing lamellar long-chain alkyl mercaptan of the present invention has excellent physical and chemical properties, and the extreme pressure (sintering load P D value), carrying capacity (P B value), anti-wear (WSD) and friction reduction performance (μ) are all very good.

[0109] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. An open gear oil, characterized in that: The preparation comprises the following raw materials in parts by weight: The solid lubricant is a long-chain alkyl mercaptan antimony with a layered structure.

2. The open gear oil according to claim 1, characterized in that: The method for preparing the layered long-chain alkyl antimony thiol comprises the following steps: The antimony source, the sulfur source and the organic solvent are mixed to carry out a hybridization reaction to obtain a long-chain alkylthiol antimony with a layered structure; The antimony source includes antimony trichloride, antimony acetate or antimony trioxide; The sulfur source includes n-dodecyl mercaptan, 1-tetradecyl mercaptan or 1-hexadecyl mercaptan.

3. The open gear oil according to claim 2, characterized in that: The molar ratio of the antimony element in the antimony source to the sulfur element in the sulfur source is 1:(3-8); the temperature of the hybridization reaction is 25-100° C., and the time is 1-10 hours.

4. The open gear oil according to claim 1, characterized in that: The base oil is one or more of silicone oil, alkylbenzene oil, mineral hydrocarbon oil, synthetic hydrocarbon oil, polyether oil, and synthetic ester oil.

5. The open gear oil according to claim 1, characterized in that: The dispersant is one or more of bis-alkenyl succinimide, polyisobutylene monosuccinimide and boron phosphated polyisobutylene bis-succinimide.

6. The open gear oil according to claim 1, characterized in that: The antioxidant is one or more of alkylated N-phenyl-α-naphthylamine, butyl octyl diphenylamine, 2,6-di-tert-butyl-p-cresol and zinc diamyl dithiocarbamate; the tackifier is one or more of ethylene propylene copolymer, methacrylate and styrene isoprene.

7. The open gear oil according to claim 1, characterized in that: The extreme pressure anti-wear agent is one or more of sulfided olefins, di-n-butyl phosphite, alkyl thiophosphates and sulfided triglycerides; the rust inhibitor is one or more of dodecenylsuccinic acid, zinc cyclohexanecarboxylate and alkyl sulfonate rust inhibitors.

8. The method for preparing the open gear oil according to any one of claims 1 to 7, characterized in that: The following steps are involved: According to the mass ratio, the base oil is heated to 35-90° C., a dispersant and a tackifier are added, and a first stirring and mixing is performed to obtain a first mixed material; The first mixed material is mixed with an extreme pressure anti-wear agent and a solid lubricant, and a second stirring and mixing is performed to obtain a second mixed material; The second mixed material is mixed with an antioxidant and a rust inhibitor, and after a third stirring and mixing process, degassing is performed to obtain an open gear oil.

9. The preparation method according to claim 8, characterized in that: The first stirring and mixing has a rotation speed of 300 to 1000 r / min and a time of 30 to 90 min; the second stirring and mixing has a rotation speed of 200 to 800 r / min and a time of 1 to 5 h; the third stirring and mixing has a rotation speed of 200 to 800 r / min and a time of 1 to 3 h.

10. Use of the open gear oil according to any one of claims 1 to 7 or the open gear oil prepared by the preparation method according to any one of claims 8 to 9 in ultra-large rotating equipment with low speed and heavy load.

Images