Temperature rise inhibition friction modifier for lubricating oil and preparation method thereof

Through the graft reaction of high-saturated alkyl glycerides with sulfur-containing modifiers and aqueous ammonium molybdate, a lubricating oil additive with excellent high-temperature stability and oxidation resistance was prepared, which solved the problem of poor temperature rise inhibition effect of oil-soluble organic molybdenum additives in the prior art in high-iron gearboxes, and achieved efficient use of lubricating oil.

CN120505133APending Publication Date: 2025-08-19TIANJIN RES INST FOR ADVANCED EQUIP TSINGHUA UNIV +1
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Patent Information

Application Number
CN202510631694.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-16
Publication Date
2025-08-19

AI Technical Summary

Technical Problem

The existing oil-soluble organic molybdenum additives have poor high temperature stability in high-iron gearboxes and cannot effectively suppress temperature rise, resulting in unstable train operation.

Method used

After reacting with a sulfur-containing modifier with a highly saturated alkyl glyceride, it is grafted with an organic amine and ammonium molybdate aqueous solution under specific conditions to prepare a temperature rise-resistance friction-repressing agent for lubricating oil, which optimizes the antioxidant and coordination bond structure of the additive.

Benefits of technology

It improves the high temperature stability and oxidation resistance of lubricating oil, reduces the generation of sludge, and ensures the effective use of lubricating oil in high-iron gearboxes.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a temperature rise inhibition friction modifier for lubricating oil and a preparation method thereof. The preparation method comprises the following steps: S1, raising the temperature of glyceride containing highly saturated alkyl acid, adding a sulfur-containing modifier, raising the temperature, keeping the temperature for reaction, cooling, and adding organic amine for reaction to obtain modified alkanolamide; s2, dissolving the modified alkanolamide obtained in the step S1 into an organic solvent, heating, adding an ammonium molybdate aqueous solution for reaction, and performing post-treatment to obtain the temperature rise inhibition friction modifier for the lubricating oil. The raw materials and process conditions are optimized, high-temperature and high-pressure or vacuum conditions are not needed, the reaction loss is reduced, and the prepared temperature rise inhibition friction modifier has good stability, oil solubility, corrosion resistance and oxidation resistance.
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Description

Technical Field

[0001] The invention belongs to the technical field of lubricating oil additives, and in particular relates to a temperature rise suppressing friction modifier for lubricating oil and a preparation method thereof. Background Art

[0002] As the lubricant for high-speed rail gearboxes, gear oil must not only prevent gear wear but also dissipate heat and reduce temperatures. As high-speed trains continue to increase in speed, the heat generated by gear meshing and oil agitation increases, leading to rising gear oil temperatures. Excessively high oil temperatures can trigger train protection devices, causing trains to slow down, disrupting normal traffic flow, and resulting in significant economic losses and adverse social impacts.

[0003] Currently, R.T. Vanderbilt's MOLYVAN 855 (8.0 wt.% molybdenum content), MOLYVAN 3000 (10 wt.% molybdenum content), and Asahi Kasei Corporation's Sakura-lube 700 (4.4 wt.% molybdenum content) represent the cutting-edge of oil-soluble organic molybdenum additives. Chinese patent CN102453589A reports an oil-soluble organic molybdenum additive with excellent structural stability and friction-reducing properties. The overall preparation process uses five raw materials: castor oil, oleic acid, diethanolamine, hydroxyethylethylenediamine, and ammonium molybdate. The process requires a negative pressure environment and a reaction time of over 13 hours. This process is complex and requires constant pressure control.

[0004] Most commercially available oil-soluble organic molybdenum additives have poor high-temperature stability and are unable to withstand the harsh environment of high-speed rail gearboxes. Therefore, it is imperative to develop a simple, efficient, stable, and low-cost method for preparing oil-soluble organic molybdenum additives. Summary of the Invention

[0005] In view of this, the present invention aims to provide a temperature-rise suppressing friction modifier for lubricating oil and a preparation method thereof, so as to solve at least one technical problem in the background technology.

[0006] To achieve the above object, the technical solution of the present invention is achieved as follows:

[0007] A method for preparing a temperature-rise suppressing friction modifier for lubricating oil comprises the following steps:

[0008] S1: heating a glyceride containing a highly saturated alkyl acid, adding a sulfur-containing modifier and then heating it, maintaining the temperature for reaction, cooling it and then adding an organic amine to react to obtain a modified alkanolamide;

[0009] S2: dissolving the modified alkanolamide obtained in step S1 in an organic solvent, adding an aqueous ammonium molybdate solution at a higher temperature for reaction, and obtaining a temperature rise suppressing friction modifier for lubricating oil after post-treatment.

[0010] Furthermore, the step S1 contains high saturated alkyl acid glyceride including C 12 ~C 18 A natural vegetable oil product containing highly saturated straight-chain alkyl glycerides.

[0011] Furthermore, the highly saturated alkyl glyceride contained in step S1 includes one or more of shea butter, cocoa butter, coconut oil, and palm kernel oil.

[0012] Furthermore, the sulfur-containing modifier in step S1 includes one or more of sulfur powder, hydrogen sulfide, carbon disulfide, potassium sulfide, and sodium sulfide.

[0013] Furthermore, the temperature of the highly saturated alkyl glyceride in step S1 is raised to 100° C. to 180° C.;

[0014] and / or, the temperature raised after adding the sulfur-containing modifier in step S1 is 185° C. to 210° C.;

[0015] And / or, after adding the sulfur-containing modifier in step S1, the temperature is raised and the temperature is maintained to react for 2 hours to 20 hours;

[0016] And / or, in step S1, the temperature of the modified alkanolamide obtained after cooling and then adding the organic amine for reaction is 100° C. to 180° C., and the reaction time is 2 h to 8 h.

[0017] Furthermore, the organic amine in step S1 includes one or both of hydroxyethylethylenediamine and diethylenetriamine;

[0018] The molar ratio of the organic amine to the glyceride containing highly saturated alkyl acid is 0.01-5, preferably 0.1-2; the molar ratio of the ammonium molybdate to the glyceride containing highly saturated alkyl acid is 0.01-5, preferably 0.1-3.

[0019] Furthermore, the organic solvent in step S2 includes petroleum ether or solvent oil;

[0020] And / or, the temperature of the reaction of adding the ammonium molybdate aqueous solution in step S2 is 80° C. to 180° C., preferably, the temperature is 130° C. to 140° C., and the reaction time is 2 h to 8 h, preferably, the reaction time is 4 h to 5 h;

[0021] And / or, the post-treatment in step S2 includes filtering out impurities and removing the organic solvent by distillation under reduced pressure to obtain the temperature rise suppressing friction modifier for lubricating oil.

[0022] The temperature-rise-suppressing friction modifier for lubricating oil is prepared by the method for preparing the temperature-rise-suppressing friction modifier for lubricating oil.

[0023] When the above-mentioned lubricating oil is high-speed rail gear oil or wind power gear oil, it can effectively reduce friction and suppress temperature rise.

[0024] Furthermore, the temperature rise suppression friction modifier for lubricating oil is added in an amount of 0.5 wt.% to 5 wt.% in the lubricating oil, and preferably added in an amount of 0.5 wt.% to 2 wt.%.

[0025] Compared with the prior art, the temperature-rise-suppressing friction modifier for lubricating oil and the preparation method thereof described in the present invention have the following advantages:

[0026] 1. This application uses animal and plant oils with higher saturation to reduce the double bond content in the product molecules and enhance the antioxidant properties of oil-soluble groups.

[0027] 2. This application introduces a modifier to reduce the unsaturation of the additive itself, and introduces sulfur into the additive to enhance its antioxidant properties, so that it can be stable under high temperature and high shear conditions and reduce the generation of sludge.

[0028] 3. When diethanolamine or hydroxyethylethylenediamine is used as the grafting raw material of the present application, esters will inevitably be generated in the product, and the position connected to the molybdenum atom is a hydroxyl group. When diethylenetriamine is used, the formation of ester groups in the molecule is avoided, and the coordinating atoms of the molybdenum core are optimized to be diamine groups, thereby enhancing the high-temperature stability of the additive's coordinating atoms, enhancing its hydrolysis resistance, and reducing its decomposition and precipitation at high temperatures.

[0029] 4. This application improves the saturation of the additive itself and optimizes the metal coordination bond to enhance the antioxidant properties of the additive itself and its effect on the antioxidant properties of the oil, thereby achieving a reduction in the content of high-temperature oxidation sludge. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] The accompanying drawings, which constitute part of the present invention, are provided to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are provided to explain the present invention and do not constitute an undue limitation of the present invention. In the accompanying drawings:

[0031] Figure 1 This is an infrared analysis comparison chart of Example 1 of the present invention and Comparative Example 1. DETAILED DESCRIPTION

[0032] It should be noted that, in the absence of conflict, the embodiments of the present invention and the features in the embodiments may be combined with each other.

[0033] The present invention will be described in detail below with reference to the accompanying drawings and in conjunction with embodiments.

[0034] Example 1

[0035] 47.5 g of coconut oil was added to a 250 mL three-necked flask equipped with a condenser and a thermometer. The flask was heated in an oil bath to approximately 110° C. to 120° C. 2 g of sulfur powder was added to the reaction system, and the temperature was raised to 195° C. and maintained for 8 hours. The temperature was then lowered to 125° C. 15 g of diethylenetriamine was added dropwise to the reaction system and mechanical stirring was continued at the same temperature for 6 hours. After the reaction was completed, the heating was turned off, and the temperature was allowed to cool to room temperature before being collected for later use to obtain modified coconut oil amide.

[0036] Modified coconut oil amide was added to a 250mL three-necked flask, 10mL of petroleum ether was added, heating and stirring were turned on, and the heating temperature was controlled at 100°C to 110°C. Without stopping stirring, 46g of an 18wt.% aqueous solution of ammonium molybdate was added dropwise to the reaction system using a constant pressure titration funnel, and refluxed at 100°C to 110°C for 5h. After the reaction was completed, the reaction liquid was cooled to below 50°C, the reaction product was centrifuged and filtered to remove incompletely reacted ammonium molybdate, and the resulting filtrate was decompressed and distilled to remove the solvent, leaving the remaining liquid as the target product.

[0037] Example 2

[0038] 47.5 g of shea butter was added to a 250 mL three-necked flask equipped with a condenser and a thermometer. The flask was heated in an oil bath to approximately 110°C to 120°C. 2 g of sulfur powder was added to the reaction system, and the temperature was raised to 195°C and maintained for 8 hours. The temperature was then lowered to 125°C. 15 g of diethylenetriamine was added dropwise to the reaction system, and mechanical stirring was continued at this temperature for 6 hours. After the reaction was completed, the heat was turned off, and the temperature was allowed to cool to room temperature before being collected for later use to obtain modified shea butter amide.

[0039] Modified shea butter amide is added to a 250mL three-necked flask, 10mL petroleum ether is added, heating and stirring are turned on, and the heating temperature is controlled at 100°C to 110°C. Without stopping stirring, 46g of an ammonium molybdate aqueous solution of 18wt.% is added dropwise using a constant pressure titration funnel to the reaction system, and refluxed and separated for 5h at 100°C to 110°C. After the reaction completes, the question response liquid is cooled to below 50°C, the reaction product is centrifuged and filtered to remove incompletely reacted ammonium molybdate, and the filtrate obtained is decompressed and distilled to remove the solvent, and the remaining liquid is the target product.

[0040] Example 3

[0041] 47.5 g of cocoa butter was added to a 250 mL three-necked flask equipped with a condenser and thermometer. The flask was heated in an oil bath to approximately 110°C to 120°C. 2 g of sulfur powder was added to the reaction system, and the temperature was raised to 195°C and maintained for 8 hours. The temperature was then lowered to 125°C. 15 g of diethylenetriamine was added dropwise to the reaction system, and mechanical stirring was continued at this temperature for 6 hours. After the reaction was completed, the heat was turned off, and the temperature was allowed to cool to room temperature before being collected for later use to obtain modified cocoa butter amide.

[0042] The modified cocoa fat amide was added to a 250 mL three-necked flask, 10 mL of petroleum ether was added, heating and stirring were started, and the heating temperature was controlled at 100 ° C to 110 ° C. Without stopping stirring, 46 g of an 18 wt.% ammonium molybdate aqueous solution was added dropwise to the reaction system using a constant pressure titration funnel, and refluxed at 100 ° C to 110 ° C for 5 hours. After the reaction was completed, the reaction liquid was cooled to below 50 ° C, the reaction product was centrifuged and filtered to remove the incompletely reacted ammonium molybdate, and the filtrate was distilled under reduced pressure to remove the solvent, and the remaining liquid was the target product.

[0043] Example 4

[0044] 47.5 g of coconut oil was added to a 250 mL three-necked flask equipped with a condenser and a thermometer. The flask was heated to 125° C. in an oil bath. 15 g of diethylenetriamine was added dropwise to the reaction system and mechanical stirring was continued at the same temperature for 6 h. After the reaction was completed, the heat was turned off and the temperature was allowed to cool to room temperature before collection to obtain cocoamide.

[0045] Coconut amide was added to a 250mL three-necked flask, 10mL of petroleum ether was added, heating and stirring were turned on, and the heating temperature was controlled at 100°C to 110°C. Without stopping stirring, 46g of an 18wt.% aqueous solution of ammonium molybdate was added dropwise to the reaction system using a constant pressure titration funnel, and refluxed at 100°C to 110°C for 5h. After the reaction was completed, the reaction liquid was cooled to below 50°C, the reaction product was centrifuged and filtered to remove incompletely reacted ammonium molybdate, and the filtrate was decompressed and distilled to remove the solvent, and the remaining liquid was the target product.

[0046] Example 5

[0047] 47.5 g of coconut oil was added to a 250 mL three-necked flask equipped with a condenser and a thermometer. The flask was heated in an oil bath to approximately 110°C to 120°C. 2 g of sulfur powder was added to the reaction system, and the temperature was raised to 195°C and maintained for 8 hours. The temperature was then lowered to 125°C, and 15 g of diethanolamine was dropwise added to the reaction system. Mechanical stirring was continued at this temperature for 6 hours. After the reaction was completed, the heat was turned off, and the temperature was allowed to cool to room temperature before being collected for later use to obtain modified coconut amide.

[0048] Modified coconut oil amide was added to a 250mL three-necked flask, 10mL of petroleum ether was added, heating and stirring were turned on, and the heating temperature was controlled at 100°C to 110°C. Without stopping stirring, 46g of an 18wt.% aqueous solution of ammonium molybdate was added dropwise to the reaction system using a constant pressure titration funnel, and refluxed at 100°C to 110°C for 5h. After the reaction was completed, the reaction liquid was cooled to below 50°C, the reaction product was centrifuged and filtered to remove incompletely reacted ammonium molybdate, and the resulting filtrate was decompressed and distilled to remove the solvent, leaving the remaining liquid as the target product.

[0049] Example 6

[0050] 47.5 g of coconut oil was added to a 250 mL three-necked flask equipped with a condenser and a thermometer. The flask was heated in an oil bath to approximately 110° C. to 120° C. 2 g of sulfur powder was added to the reaction system, the temperature was raised to 195° C. and maintained for 8 hours, then cooled to 125° C. 15 g of hydroxyethylethylenediamine was added dropwise to the reaction system and mechanical stirring was continued at the same temperature for 6 hours. After the reaction was completed, the heating was turned off, and the temperature was allowed to cool to room temperature before being collected for later use to obtain modified coconut oil amide.

[0051] Modified coconut oil amide was added to a 250mL three-necked flask, 10mL of petroleum ether was added, heating and stirring were turned on, and the heating temperature was controlled at 100°C to 110°C. Without stopping stirring, 46g of an 18wt.% aqueous solution of ammonium molybdate was added dropwise to the reaction system using a constant pressure titration funnel, and refluxed at 100°C to 110°C for 5h. After the reaction was completed, the reaction liquid was cooled to below 50°C, the reaction product was centrifuged and filtered to remove incompletely reacted ammonium molybdate, and the resulting filtrate was decompressed and distilled to remove the solvent, leaving the remaining liquid as the target product.

[0052] Example 7

[0053] 47.5 g of coconut oil was added to a 250 mL three-necked flask equipped with a condenser and a thermometer. The flask was heated to 125°C in an oil bath. 15 g of hydroxyethylethylenediamine was added dropwise to the reaction system and mechanical stirring was continued at this temperature for 6 hours. After the reaction was completed, the heat was turned off and the temperature was allowed to cool to room temperature before collection to obtain cocoamide.

[0054] Coconut amide was added to a 250mL three-necked flask, 10mL of petroleum ether was added, heating and stirring were turned on, and the heating temperature was controlled at 100°C to 110°C. Without stopping stirring, 46g of an 18wt.% aqueous solution of ammonium molybdate was added dropwise to the reaction system using a constant pressure titration funnel, and refluxed at 100°C to 110°C for 5h. After the reaction was completed, the reaction liquid was cooled to below 50°C, the reaction product was centrifuged and filtered to remove incompletely reacted ammonium molybdate, and the filtrate was decompressed and distilled to remove the solvent, and the remaining liquid was the target product.

[0055] Example 8

[0056] 47.5 g of coconut oil was added to a 250 mL three-necked flask equipped with a condenser, thermometer, and waste gas recovery bottle. The flask was heated to approximately 50° C. in an oil bath. Hydrogen sulfide gas was introduced into the reaction system for 20 minutes, then the temperature was raised to 195° C. and maintained for 8 hours. The temperature was then lowered to 125° C. 15 g of diethylenetriamine was added dropwise to the reaction system and mechanical stirring was continued at this temperature for 6 hours. After the reaction was completed, the heat was turned off, and the temperature was allowed to cool to room temperature before being collected for later use to obtain modified coconut amide.

[0057] Modified coconut oil amide was added to a 250mL three-necked flask, 10mL of petroleum ether was added, heating and stirring were turned on, and the heating temperature was controlled at 100°C to 110°C. Without stopping stirring, 46g of an 18wt.% aqueous solution of ammonium molybdate was added dropwise to the reaction system using a constant pressure titration funnel, and refluxed at 100°C to 110°C for 5h. After the reaction was completed, the reaction liquid was cooled to below 50°C, the reaction product was centrifuged and filtered to remove incompletely reacted ammonium molybdate, and the resulting filtrate was decompressed and distilled to remove the solvent, leaving the remaining liquid as the target product.

[0058] Example 9

[0059] 47.5g coconut oil is added into the there-necked flask with condensation and thermometer of 250mL, and there-necked flask is heated to about 50 DEG C in an oil bath, and 2g sodium sulfide is added in the reaction system, 20g 10% sulfuric acid solution, is warming up to 105 DEG C and maintains 5h, is warming up to 195 DEG C and maintains 3h, is cooled to 125 DEG C, 15g diethylenetriamine is dripped into the reaction system and continues mechanical stirring 6h at this temperature. After reaction terminates, heating is turned off, and after its temperature is cooled to room temperature, washing and rotary evaporation are collected for standby use, and modified coconut oil amide is obtained.

[0060] Modified coconut oil amide was added to a 250mL three-necked flask, 10mL of petroleum ether was added, heating and stirring were turned on, and the heating temperature was controlled at 100°C to 110°C. Without stopping stirring, 46g of an 18wt.% aqueous solution of ammonium molybdate was added dropwise to the reaction system using a constant pressure titration funnel, and refluxed at 100°C to 110°C for 5h. After the reaction was completed, the reaction liquid was cooled to below 50°C, the reaction product was centrifuged and filtered to remove incompletely reacted ammonium molybdate, and the resulting filtrate was decompressed and distilled to remove the solvent, leaving the remaining liquid as the target product.

[0061] Example 10

[0062] 47.5 g of coconut oil was added to a 250 mL three-necked flask equipped with a condenser and a thermometer. The flask was heated in an oil bath to approximately 110°C to 120°C. 15 g of hydroxyethylethylenediamine was added dropwise to the reaction system and mechanical stirring was continued at the same temperature for 3 hours. After the reaction was completed, the heat was turned off and the mixture was cooled to room temperature before being collected for later use to obtain cocoamide.

[0063] Coconut amide was added to a 250mL three-necked flask, 10mL of petroleum ether was added, heating and stirring were turned on, and the heating temperature was controlled at 100°C to 110°C. Without stopping stirring, 46g of an 18wt.% aqueous solution of ammonium molybdate was added dropwise to the reaction system using a constant pressure titration funnel, and refluxed at 100°C to 110°C for 5h, 5g of carbon disulfide was added, and the reaction was continued for 10h. After the reaction was completed, the reaction liquid was cooled to below 50°C, the reaction product was centrifuged and filtered to remove incompletely reacted ammonium molybdate, and the filtrate was decompressed and distilled to remove the solvent, and the remaining liquid was the target product.

[0064] Comparative Example 1

[0065] Add 47.5 g of soybean oil to a 250 mL three-necked flask equipped with a condenser and thermometer. Heat the flask in an oil bath to approximately 110°C to 120°C. Add 15 g of hydroxyethylethylenediamine dropwise to the reaction system and continue mechanically stirring at this temperature for 3 hours. After the reaction is complete, turn off the heat, wait until the temperature cools to room temperature, and collect the resulting mixture for later use to obtain soybean oil amide.

[0066] Soybean amide was added to a 250 mL three-necked flask, 10 mL of petroleum ether was added, heating and stirring were started, and the heating temperature was controlled at 100°C to 110°C. Without stopping stirring, 46 g of an 18 wt.% aqueous solution of ammonium molybdate was added dropwise to the reaction system using a constant pressure titration funnel, and the mixture was refluxed and separated at 100°C to 110°C for 5 hours. After the reaction was completed, the reaction liquid was cooled to below 50°C, the reaction product was centrifuged and filtered to remove the incompletely reacted ammonium molybdate, and the filtrate was distilled under reduced pressure to remove the solvent, and the remaining liquid was the target product.

[0067] Comparative Example 2

[0068] MOLYVAN 855 from RT Vanderbilt was used as comparative product 2.

[0069] Comparative Example 3

[0070] RT Vanderbilt's MOLYVAN 3000 was used as comparative product 3.

[0071] Comparative Example 4

[0072] 47.5 g of stearic acid was added to a 250 mL three-necked flask equipped with a condenser and thermometer. The flask was heated in an oil bath to approximately 110°C to 120°C. 15 g of hydroxyethylethylenediamine was added dropwise to the reaction system and mechanical stirring was continued at this temperature for 3 hours. After the reaction was completed, the heat was turned off and the mixture was allowed to cool to room temperature before being collected for later use to obtain soybean oil amide.

[0073] Soybean amide was added to a 250 mL three-necked flask, 10 mL of petroleum ether was added, heating and stirring were started, and the heating temperature was controlled at 100°C to 110°C. Without stopping stirring, 46 g of an 18 wt.% aqueous solution of ammonium molybdate was added dropwise to the reaction system using a constant pressure titration funnel, and the mixture was refluxed and separated at 100°C to 110°C for 5 hours. After the reaction was completed, the reaction liquid was cooled to below 50°C, the reaction product was centrifuged and filtered to remove the incompletely reacted ammonium molybdate, and the filtrate was distilled under reduced pressure to remove the solvent, and the remaining liquid was the target product.

[0074] Comparative Example 5

[0075] Add 47.5 g of soybean oil to a 250 mL three-necked flask equipped with a condenser and thermometer. Heat the flask in an oil bath to approximately 110°C to 120°C. Add 15 g of hydroxyethylethylenediamine dropwise to the reaction system and continue mechanically stirring at this temperature for 3 hours. After the reaction is complete, turn off the heat, wait until the temperature cools to room temperature, and collect the resulting mixture for later use to obtain soybean oil amide.

[0076] Application Example 1

[0077] Lubricating additive appearance, molybdenum content and oil solubility test. Molybdenum content is tested using ASTM D4951-14 method. The additive is dissolved in 120# solvent oil at 1% and stirred at 65℃ for 1 hour. For high temperature solubility, the sample is placed in a 100℃ oven for observation. For low temperature solubility, the sample is placed in a -7℃ refrigerator for observation.

[0078] Table 1 Oil solubility results

[0079]

[0080]

[0081] Application Example 2

[0082] The anti-copper corrosion test was carried out on a JSR2101 copper corrosion tester produced by Hunan Jinshi Petrochemical Instrument Co., Ltd. The experimental conditions were: 121°C, test time 3h, and the results are shown in Table 1.

[0083] Table 2 Results of copper sheet corrosion resistance

[0084] sample Copper corrosion (T2 copper) blank 1b Example 1 1b Example 2 1b Example 3 1b Example 4 1b Example 6 1b Example 7 1b Example 8 1b Example 9 3a Example 10 1b Comparative Example 1 1b Comparative Example 2 1b Comparative Example 3 3a

[0085] Application Example 3

[0086] Tribological properties were tested using the SRV-5 test using a 1% addition of the additive to Shell Helia Ultra 0W-20 oil at 120°C, 2 mm, 50 Hz, 2 h, GCr15 steel disc / ball. Wear spots were observed directly via a microscope.

[0087] Table 3 Friction reduction and anti-wear properties

[0088]

[0089] Application Example 4

[0090] The antioxidant properties were evaluated by adding 0.8% of the additive to the gearbox oil, placing it in a 135°C oven for 72 hours, and observing the corrosion and sludge formation on 45# steel sheets as catalysts. The gearbox oil contained 3.35% of an anti-scuffing agent (T321), 2.46% of extreme pressure and anti-wear agents (QT301, T308, T309, P120), 0.10% of a metal deactivator (T553, T406E), 0.12% of an ashless dispersant (RF1161H), 0.05% of a rust inhibitor (RF1106D), 0.03% of an anti-foaming agent (155), 5% of a viscosity index improver (V6520), 9% of an ester oil (3970), 5% of HVIS150BS, and the balance of PAO (PAO6 and PAO40).

[0091] Table 4 Antioxidant properties

[0092]

[0093]

[0094] The oil-solubility results of this application show that the various high-saturation vegetable oils selected can effectively connect to inorganic molybdenum ligands, among which diethylenetriamine and hydroxyethylethylenediamine can both ensure that the additive has a high molybdenum content, while the molybdenum content of the additive with diethanolamine as a linker is low. This is because the core process of the present invention is that the ester group in the vegetable oil undergoes a substitution reaction with a polyamino compound to generate an amide group, while in Comparative Example 4, the carboxyl group and the amino group condense to generate an amide group, and no reaction occurs when the conditions are not changed. As for hydroxyethylethylenediamine and diethylenetriamine as linkers, they cannot be simply replaced under the existing conditions, and it is necessary to explore and design the test conditions based on the characteristics of the triamino compound. Application Examples 2 and 3 show that although the present invention introduces a modifier to improve its antioxidant properties, it does not affect its copper sheet corrosion performance and tribological properties. The additive prepared in Comparative Example 1 exhibits excellent oil solubility and friction-reducing and anti-wear properties. However, Application Example 4 demonstrates its poor oxidation resistance. This is due to the presence of carbon-carbon double bonds and the potential for ester groups within the molecule, making its molecular structure susceptible to oxidation. Furthermore, the presence of free hydroxyl groups after the coordination bonds break can act as free radical initiators, potentially leading to base oil oxidation and increasing sludge. Therefore, the present invention optimizes both the oily and linking groups and creatively introduces a modifier. This improves oxidation resistance without compromising the additive's inherent corrosion resistance, ensuring the thermal stability of the oil product, demonstrating significant innovation.

[0095] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for preparing a temperature-rise suppressing friction modifier for lubricating oil, characterized in that: The steps include: S1: heating a glyceride containing a highly saturated alkyl acid, adding a sulfur-containing modifier and then heating it, maintaining the temperature for reaction, cooling it and then adding an organic amine to react to obtain a modified alkanolamide; S2: dissolving the modified alkanolamide obtained in step S1 in an organic solvent, adding an aqueous ammonium molybdate solution at a higher temperature for reaction, and obtaining a temperature rise suppressing friction modifier for lubricating oil after post-treatment.

2. The method for preparing a temperature-rise suppressing friction modifier for lubricating oil according to claim 1, characterized in that: Step S1 contains high saturated alkyl acid glyceride including C 12 ~C 18 A natural vegetable oil product containing highly saturated straight-chain alkyl glycerides.

3. The method for preparing a temperature-rise suppressing friction modifier for lubricating oil according to claim 1, characterized in that: The highly saturated alkyl glyceride contained in step S1 includes one or more of shea butter, cocoa butter, coconut oil, and palm kernel oil.

4. The method for preparing a temperature-rise-suppressing friction modifier for lubricating oil according to claim 1, characterized in that: The sulfur-containing modifier in step S1 includes one or more of sulfur powder, hydrogen sulfide, carbon disulfide, potassium sulfide, and sodium sulfide.

5. The method for preparing a temperature-rise suppressing friction modifier for lubricating oil according to claim 1, characterized in that: The temperature of the highly saturated alkyl glyceride in step S1 is raised to 100° C. to 180° C.; and / or, the temperature raised after adding the sulfur-containing modifier in step S1 is 185° C. to 210° C.; And / or, after adding the sulfur-containing modifier in step S1, the temperature is raised and the temperature is maintained to react for 2 hours to 20 hours; And / or, in step S1, the temperature of the modified alkanolamide obtained after cooling and then adding the organic amine for reaction is 100° C. to 180° C., and the reaction time is 2 h to 8 h.

6. The method for preparing a temperature-rise suppressing friction modifier for lubricating oil according to claim 1, characterized in that: The organic amine in step S1 includes one or both of hydroxyethylethylenediamine and diethylenetriamine; The molar ratio of the organic amine to the glyceride containing highly saturated alkyl acid is 0.01-5, preferably 0.1-2; the molar ratio of the ammonium molybdate to the glyceride containing highly saturated alkyl acid is 0.01-5, preferably 0.1-3.

7. The method for preparing a temperature-rise suppressing friction modifier for lubricating oil according to claim 1, characterized in that: The organic solvent in step S2 includes petroleum ether or solvent oil; And / or, the temperature of the reaction of adding the ammonium molybdate aqueous solution in step S2 is 80° C. to 180° C., preferably, the temperature is 130° C. to 140° C., and the reaction time is 2 h to 8 h, preferably, the reaction time is 4 h to 5 h; And / or, the post-treatment in step S2 includes filtering out impurities and removing the organic solvent by distillation under reduced pressure to obtain the temperature rise suppressing friction modifier for lubricating oil.

8. The temperature-rise-suppressing friction modifier for lubricating oil prepared by the method for preparing the temperature-rise-suppressing friction modifier for lubricating oil according to any one of claims 1 to 7.

9. The temperature-rise-suppressing friction modifier for lubricating oil according to claim 8 is used as a friction-reducing additive and a temperature-rise suppressant in lubricating oil, characterized in that: When the lubricating oil is high-speed rail gear oil or wind power gear oil, it can effectively reduce friction and suppress temperature rise.

10. The use according to claim 9, characterized in that: The temperature rise suppression friction modifier for lubricating oil is added in an amount of 0.5 wt.% to 5 wt.% in the lubricating oil, and preferably added in an amount of 0.5 wt.% to 2 wt.%.

Citation Information

Patent Citations

  • Sulfur-phosphor-free oil-soluble organic molybdenum additive

    CN102453589A