Chelated lithium molybdenum ion lubricating oil additive and its preparation method and application

Abstract

The present invention discloses a chelated lithium molybdenum ion lubricating oil additive and its preparation method and application. The preparation method includes the following steps: add kaolin and hexadecyltrimethoxysilane to deionized water, react with magnetic stirring and ultrasonic treatment, and then stir; after the reaction, filter, wash and dry the reaction product to obtain alkylated kaolin; then add alkylated kaolin and aminopropyltrimethoxysilane to deionized water, react with magnetic stirring and ultrasonic treatment, and then stir; after the reaction, centrifuge, wash and dry the reaction product to obtain aminated / alkylated kaolin; then add aminated / alkylated kaolin to chelated lithium molybdenum ion solution, react with stirring; after the reaction, filter, wash and dry the reaction product to obtain chelated lithium molybdenum ion lubricating oil additive. The prepared additive has good dispersibility in base oil and has excellent friction reducing and anti-friction ability.

Description

[Technical field]

[0001] The present invention relates to the technical field of lubricating oils, in particular to a chelated lithium molybdenum ion lubricating oil additive and its preparation method and application. [Background technology]

[0002] Lubricants are liquid or semi-solid lubricants that are applied to mechanical parts in industries such as aviation, machining, metallurgy, automobiles, transportation, and coal to reduce friction and protect machines and processed products. They mainly play the roles of lubrication, cooling assistance, rust prevention, cleaning, sealing, and buffering. Generally, lubricants consist of two parts: base oil and additives. Base oil is the main component of lubricants and determines the basic properties of lubricants. Additives give lubricants new performance by compensating for or improving the performance deficiencies of base oil. In other words, they are important components of lubricants, and their type, quality, and addition ratio have a direct impact on the usage performance of lubricants.

[0003] Nano additives are mainly used in lubrication as friction reducers, antiwear agents, extreme pressure additives, conformability agents, etc., and have acquired completely new physical and chemical properties due to their special effects (e.g., surface and interface effects, small size effects, size effects, etc.). Nano additives have superior performance that is incomparable to conventional additives or lubricants, and therefore have the potential to replace conventional additives.

[0004] With people's emphasis on environmental protection and the continuous development of nanomaterial technology, the development of clean, non-polluting / low-polluting micro-nano lubricant additives has become one of the fastest-growing research topics. Two-dimensional layered materials have a layered structure. That is, the atoms in each atomic layer are connected by strong covalent bonds, and adjacent atomic layers are connected by weak van der Waals forces, so the layers tend to slide against each other. Therefore, all materials widely used for solid lubrication have a layered structure. Among two-dimensional layered materials, silicate minerals do not pollute the environment and are inexpensive. In addition, research has revealed that silicate minerals such as kaolin, montmorillonite, and serpentine have a certain friction-reducing and anti-friction effect as lubricant additives.

[0005] Patent Document 1 discloses a high-performance water-soluble lubricating oil for racks. The lubricating oil contains, by weight, 80 to 100 parts of base oil, 3 to 5 parts of hydroxyethyl cellulose, 6 to 8 parts of sodium polyacrylate, 8 to 12 parts of ethylene glycol, 1 to 2 parts of modified graphite powder, 3 to 9 parts of a polymer blend of nano kaolin and nano aluminum oxide, 0.3 to 0.5 parts of polyvinyl alcohol emulsion, 5 to 15 parts of a stabilizer, 2 to 10 parts of a surfactant, 0.2 to 1 part of an antifoaming agent, and 30 to 70 parts of deionized water. By combining various additives, it is possible to improve various performances of the lubricating oil and to enhance the stability and lubricating effect of the lubricating oil. In addition, this makes it possible to effectively prevent the occurrence of damage such as wear and scratches on the rack tooth surface and extend the service life of the rack.

[0006] However, kaolin has poor dispersion stability in liquid lubricating media and is prone to aggregation and precipitation due to its own characteristics such as solid particle nature, high chemical activity, and ease of adsorption, etc. Therefore, not only is it unable to effectively exert its friction reduction, friction prevention, and self-repairing functions, but it may also cause abrasive wear due to aggregation.

[0007] Ionic liquids have good properties such as non-volatility, non-flammability, thermal stability, low melting point and good electrical conductivity, making them ideal lubricating materials. In 2001, Ye et al. were the first in the world to discover that ionic liquids are multifunctional lubricants with excellent performance. They conducted detailed and systematic research on ionic liquid lubricating materials, attracting great attention from researchers at home and abroad. To date, ionic liquids have already been widely used as base oils, additives, lubricating films and conductive lubricating greases. However, research has revealed that while ordinary ionic liquids can be dissolved in polyethylene glycols with high polarity, their solubility in hydrocarbon lubricating oils with low polarity is very low (<<1%). [Prior art documents] [Patent documents]

[0008] [Patent Document 1] China Patent Application Publication No. 107446682A Summary of the Invention [Problem to be solved by the invention]

[0009] In order to overcome the drawbacks of the prior art, the present invention aims to provide a chelated lithium molybdenum ion lubricating oil additive, which has good dispersibility in base oil and excellent friction reducing and anti-friction effects, and its preparation method and application. [Means for solving the problem]

[0010] To achieve the above objectives, the present invention adopts the following technical solutions.

[0011] The method for preparing the chelated lithium molybdenum ion lubricant additive includes the following steps:

[0012] (1) Kaolin and hexadecyltrimethoxysilane are added to deionized water, and the mixture is reacted by stirring with a magnetic stirrer and ultrasonic treatment, and then the reaction product is filtered, washed, and dried to obtain alkylated kaolin.

[0013] (2) The alkylated kaolin and aminopropyltrimethoxysilane are added to deionized water, and the mixture is reacted by stirring after magnetic stirring and ultrasonic treatment. After the reaction is completed, the reaction product is centrifuged, washed, and dried to obtain aminated / alkylated kaolin.

[0014] (3) The aminated / alkylated kaolin is added to the lithium molybdenum ion chelate solution and reacted with stirring. After the reaction is completed, the reaction product is filtered, washed and dried to obtain the lithium molybdenum ion chelate lubricating oil additive.

[0015] Preferably, in the step (1), the mass / volume ratio of kaolin, hexadecyltrimethoxysilane, and deionized water is 1 g:0.05-0.5 g:100 mL.

[0016] Preferably, in step (1), magnetic stirring is performed for 10 to 20 minutes, ultrasonic treatment is performed for 30 to 60 minutes, and the reaction is performed under reaction conditions of 40 to 60° C. for 2 to 6 hours.

[0017] Preferably, in step (2), the mass / volume ratio of alkylated kaolin, aminopropyltrimethoxysilane, and deionized water is 1 g:0.05-0.2 g:100 mL.

[0018] Preferably, in step (2), the magnetic stirring time is 15 to 30 minutes, the ultrasonic treatment is 10 to 20 minutes, and the reaction is carried out under reaction conditions of 50 to 80° C. for 4 to 10 hours.

[0019] Preferably, in step (3), the chemical formula of the chelated lithium molybdenum ion is Li2C10H16N2O8Mo, and the concentration of the chelated lithium molybdenum ion solution is 0.1-1 wt%.

[0020] Preferably, in step (3), the method for preparing the chelated lithium molybdenum ion solution is as follows: EDTA is weighed and dissolved in dilute ammonia water to form an EDTA solution with a concentration of 1 mol / L. Next, lithium acetate and molybdenum nitrate are weighed and added to the EDTA solution in a molar ratio of EDTA:Li:Mo=1:1-2:0.5-1, and the mixture is stirred at 80°C to react for 2 hours to obtain a chelated lithium molybdenum ion solution.

[0021] Preferably, in step (3), the reaction is carried out under stirring at a reaction condition of 70 to 90° C. for 6 to 10 hours. In addition, the mass / volume ratio of aminated / alkylated kaolin to the chelated lithium molybdenum ion solution is 1 g:30 to 50 mL.

[0022] The present invention further claims protection for lubricating oil additives prepared using said process.

[0023] The present invention further claims the application of said additive in lubricating oil, the concentration of said additive in the lubricating oil being 0.01-0.13 wt%.

[0024] Preferably, the lubricant includes Kunlun Scorpio F5000 lubricant, SF15W-40 type lubricant and Great Wall SJ10W-40 lubricant, or mineral base oil, synthetic base oil. Effect of the Invention

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] 1) In the present invention, the layered structure of kaolin is advantageous in reducing momentum transport between fluid layers, and the fluid layers are separated, so that the fluid resistance is reduced and the oil viscosity is reduced. In addition, the dispersibility of kaolin in oil is improved by sequentially modifying kaolin with hexadecyltrimethoxysilane and aminopropyltrimethoxysilane, so that more lubricating oil molecules can be delivered to the friction surface. In addition, a mechanical deposition film is formed in the depression of the friction surface to fill and repair the friction surface, improving the lubrication efficiency.

[0027] 2) In the lubricating oil additive of the present invention, the chelated lithium molybdenum ion is bonded to the surface of aminated / alkylated kaolin, thereby improving the compatibility of the chelated lithium molybdenum ion with the oil phase. During the friction process, the chelated lithium molybdenum ion can undergo complex tribochemical reactions with the elements on the surface of the friction pair, and a boundary lubricating film is formed on the surface of the friction pair. This provides the additive with good friction reduction and anti-friction capabilities. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0028] In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be described in more detail in the following in combination with examples. Of course, the specific examples described herein are only for illustrating the present invention, and are not intended to limit the present invention.

[0029] Unless otherwise specified, all of the chemical reagents and materials in the present invention are commercially available or synthesized from commercially available raw materials.

[0030] Kaolin with a particle size of 0.5 to 2 μm was purchased from Fuhua Nano Materials Co., Ltd.

[0031] Chelated lithium molybdenum ion solution was provided by Yatian Group.

[0032] The present invention will now be further described with reference to specific examples.

[0033] Example 1

[0034] The preparation method of the chelated lithium molybdenum ion lubricant additive included the following steps:

[0035] (1) 1g of kaolin and 0.5g of hexadecyltrimethoxysilane were added to 100mL of deionized water, magnetically stirred for 20min, and ultrasonically treated for 60min. Then, the mixture was stirred at 60℃ for 6h and reacted. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain alkylated kaolin.

[0036] (2) 1 g of alkylated kaolin and 0.2 g of aminopropyltrimethoxysilane were added to 100 mL of deionized water, magnetically stirred for 30 min, and ultrasonically treated for 20 min. The mixture was then stirred at 80°C for 10 h and reacted. After the reaction was completed, the reaction product was centrifuged, washed, and dried to obtain aminated / alkylated kaolin.

[0037] (3) 1 g of aminated / alkylated kaolin was added to 50 mL of 1 wt% chelated lithium molybdenum ion solution, and the mixture was stirred at 90° C. for 10 hours to react. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain a chelated lithium molybdenum ion lubricant additive.

[0038] The prepared additive was added to SF15W-40 type lubricating oil at a concentration of 0.13 wt%.

[0039] Example 2

[0040] The preparation method of the chelated lithium molybdenum ion lubricant additive included the following steps:

[0041] (1) 1g of kaolin and 0.05g of hexadecyltrimethoxysilane were added to 100mL of deionized water, magnetically stirred for 10min, and ultrasonically treated for 30min. The mixture was then stirred at 40℃ for 2h and reacted. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain alkylated kaolin.

[0042] (2) 1g of alkylated kaolin and 0.05g of aminopropyltrimethoxysilane were added to 100mL of deionized water, magnetically stirred for 15min, and ultrasonically treated for 10min. The mixture was then stirred at 50℃ for 4h and reacted. After the reaction was completed, the reaction product was centrifuged, washed, and dried to obtain aminated / alkylated kaolin.

[0043] (3) 1 g of aminated / alkylated kaolin was added to 30 mL of 0.1 wt% chelated lithium molybdenum ion solution, and the mixture was stirred at 70°C for 6 hours to react. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain a chelated lithium molybdenum ion lubricant additive.

[0044] The prepared additive was added to SF15W-40 type lubricating oil at a concentration of 0.01 wt%.

[0045] Example 3

[0046] The preparation method of the chelated lithium molybdenum ion lubricant additive included the following steps:

[0047] (1) 1g of kaolin and 0.2g of hexadecyltrimethoxysilane were added to 100mL of deionized water, magnetically stirred for 15min, and ultrasonically treated for 40min. The mixture was then stirred at 50℃ for 3h and reacted. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain alkylated kaolin.

[0048] (2) 1g of alkylated kaolin and 0.1g of aminopropyltrimethoxysilane were added to 100mL of deionized water, magnetically stirred for 20min, and ultrasonically treated for 15min. The mixture was then stirred at 60℃ for 6h, and after the reaction was completed, the reaction product was centrifuged, washed, and dried to obtain aminated / alkylated kaolin.

[0049] (3) 1 g of aminated / alkylated kaolin was added to 40 mL of 0.6 wt% chelated lithium molybdenum ion solution, and the mixture was stirred at 80°C for 8 hours to react. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain a chelated lithium molybdenum ion lubricant additive.

[0050] The prepared additive was added to SF15W-40 type lubricating oil at a concentration of 0.05 wt%.

[0051] Example 4

[0052] The preparation method of the chelated lithium molybdenum ion lubricant additive included the following steps:

[0053] (1) 1g of kaolin and 0.3g of hexadecyltrimethoxysilane were added to 100mL of deionized water, magnetically stirred for 18min, and ultrasonically treated for 50min. The mixture was then stirred at 55℃ for 5h and reacted. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain alkylated kaolin.

[0054] (2) 1g of alkylated kaolin and 0.15g of aminopropyltrimethoxysilane were added to 100mL of deionized water, magnetically stirred for 25min, and ultrasonically treated for 15min. The mixture was then stirred at 70℃ for 8h, and after the reaction was completed, the reaction product was centrifuged, washed, and dried to obtain aminated / alkylated kaolin.

[0055] (3) 1 g of aminated / alkylated kaolin was added to 45 mL of 0.8 wt% chelated lithium molybdenum ion solution, and the mixture was stirred at 80° C. for 9 hours to react. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain a chelated lithium molybdenum ion lubricant additive.

[0056] The prepared additive was added to SF15W-40 type lubricating oil at a concentration of 0.1 wt%.

[0057] Comparative Example 1

[0058] The method for preparing the lubricating oil additive included the following steps:

[0059] (1) 1 g of kaolin and 0.2 g of aminopropyltrimethoxysilane were added to 100 mL of deionized water, magnetically stirred for 30 min, and ultrasonically treated for 20 min. The mixture was then stirred at 80°C for 10 h and reacted. After the reaction was completed, the reaction product was centrifuged, washed, and dried to obtain aminated kaolin.

[0060] (2) 1 g of aminated kaolin was added to 50 mL of 1 wt% chelated lithium molybdenum ion solution, and the mixture was stirred at 90°C for 10 hours to react. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain the additive.

[0061] The prepared additive was added to SF15W-40 type lubricating oil at a concentration of 0.13 wt%.

[0062] Comparative Example 2

[0063] The method for preparing the lubricating oil additive included the following steps:

[0064] (1) 1g of kaolin and 0.5g of hexadecyltrimethoxysilane were added to 100mL of deionized water, magnetically stirred for 20min, and ultrasonically treated for 60min. Then, the mixture was stirred at 60℃ for 6h and reacted. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain alkylated kaolin.

[0065] (2) 1 g of alkylated kaolin was added to 50 mL of 1 wt% chelated lithium molybdenum ion solution, and the mixture was stirred at 90°C for 10 hours to react. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain the additive.

[0066] The prepared additive was added to SF15W-40 type lubricating oil at a concentration of 0.13 wt%.

[0067] Comparative Example 3

[0068] The method for preparing the lubricating oil additive included the following steps:

[0069] (1) 1g of kaolin and 0.5g of hexadecyltrimethoxysilane were added to 100mL of deionized water, magnetically stirred for 20min, and ultrasonically treated for 60min. Then, the mixture was stirred at 60℃ for 6h and reacted. After the reaction was completed, the reaction product was filtered, washed, and dried to obtain alkylated kaolin.

[0070] (2) 1 g of alkylated kaolin and 0.2 g of aminopropyltrimethoxysilane were added to 100 mL of deionized water, magnetically stirred for 30 min, and ultrasonically treated for 20 min. The mixture was then stirred at 80°C for 10 h and reacted. After the reaction was completed, the reaction product was centrifuged, washed, and dried to obtain aminated / alkylated kaolin.

[0071] The prepared aminated / alkylated kaolin was added to SF15W-40 type lubricating oil at a concentration of 0.13 wt%.

[0072] The lubricating oils prepared in Examples 1 to 4 and Comparative Examples 1 to 3 were examined for their friction prevention and friction reduction performance using an SGW-10A four-ball friction and wear tester. High-quality chromium alloy bearing steel GCr15 was used for the steel balls used in the experiment. The Rockwell hardness HRC was 64 to 66, and the diameter was 12.7 mm. During the experiment, the load was 147 N, the rotation speed was 1200 r / min, and the time was 60 min. After the experiment, the steel balls were cleaned and the size of the friction mark diameter on the steel balls after the friction experiment was observed using an optical microscope. In addition, the mass loss of the steel balls before and after the experiment was measured using a 0.1 mg electronic balance. The measurement results are shown in Table 1.

[0073] [Table 1]

[0074] The above description is merely a preferred specific embodiment of the present invention, and the scope of protection of the present invention is not limited thereto. Within the technical scope disclosed in the present invention, any equivalent replacement or modification made by a person skilled in the art based on the technical solutions and inventive ideas of the present invention shall be covered by the scope of protection of the present invention.

Claims

1. 1. A method for preparing a chelated lithium molybdenum ion lubricating oil additive comprising the steps of: (1) adding kaolin and hexadecyltrimethoxysilane to deionized water, and reacting by stirring after magnetic stirring and ultrasonic treatment; after the reaction is completed, filtering, washing and drying the reaction product to obtain alkylated kaolin; (2) adding alkylated kaolin and aminopropyltrimethoxysilane to deionized water, and reacting by stirring after magnetic stirring and ultrasonic treatment; after the reaction is completed, the reaction product is centrifuged, washed and dried to obtain aminated / alkylated kaolin; (3) adding aminated / alkylated kaolin to a chelated lithium molybdenum ion solution, stirring to react, and filtering, washing and drying the reaction product after the reaction is completed to obtain a chelated lithium molybdenum ion lubricating oil additive.

2. 2. The method according to claim 1, wherein in step (1), the mass / volume ratio of kaolin, hexadecyltrimethoxysilane, and deionized water is 1 g:0.05-0.5 g:100 mL.

3. The preparation method according to claim 1, characterized in that in step (1), the magnetic stirring is performed for 10-20 min, the ultrasonic treatment is performed for 30-60 min, and the reaction condition is 40-60°C for 2-6 h.

4. The preparation method according to claim 1, characterized in that in step (2), the mass volume ratio of alkylated kaolin, aminopropyltrimethoxysilane and deionized water is 1 g:0.05-0.2 g:100 mL.

5. The preparation method according to claim 1, characterized in that in step (2), the magnetic stirring time is 15-30 min, the ultrasonic treatment is 10-20 min, and the reaction condition is 50-80°C, and the reaction is carried out for 4-10 h.

6. 2. The method according to claim 1, wherein in step (3), the chemical formula of the lithium molybdenum ion chelate is Li2C10H16N2O8Mo, and the concentration of the lithium molybdenum ion chelate solution is 0.1-1 wt%.

7. The preparation method according to claim 1, characterized in that in step (3), the reaction conditions are 70-90°C, and the reaction is carried out under stirring for 6-10 h, and the mass volume ratio of aminated / alkylated kaolin to chelated lithium molybdenum ion solution is 1 g:30-50 mL.

8. A lubricating oil additive prepared using the method of any one of claims 1 to 7.

9. 9. The application of the additive according to claim 8 in a lubricating oil, The application is characterized in that the concentration of said additive in the lubricating oil is 0.01 to 0.13 wt %.

10. 9. The application of the additive according to claim 8 in a lubricating oil, The lubricant is selected from the group consisting of Kunlun Tianzhong F5000 lubricant, SF15W-40 type lubricant and Great Wall SJ10W-40 lubricant, mineral base oil, and synthetic base oil.

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