A lithium-based lubricating grease composition with excellent wear resistance and a preparing method thereof
A technology of grease composition and lithium-based grease, which is applied in the field of grease, can solve the problems of poor water resistance, poor anti-wear performance, poor oxidation resistance, etc., achieve good high temperature resistance, improve wear reduction ability and The effect of antioxidant capacity
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[0046] Among the present invention, the preparation method of the compound of structure shown in formula (I) preferably comprises:
[0047] (a) react aniline, sulfur chloride and 4-chloroaniline to generate intermediate M shown in formula (II),
[0048]
[0049] (b) carrying out nucleophilic substitution reaction between the intermediate M obtained in step (a) and dimercapto-1,3,4-thiadiazole under alkaline conditions to generate the multi-effect additive shown in formula (I),
[0050]
[0051] In step (a) of the present invention, the specific mode of reacting aniline, sulfur chloride and 4-chloroaniline preferably includes:
[0052] (i) fully reacting aniline and sulfur chloride at -20-0°C in the first solvent under an inert atmosphere;
[0053] (ii) Add 4-chloroaniline into the reaction system of step (i), and react at 15-30° C. for 1-3 h.
[0054] In the present invention, the inert atmosphere can be a conventional inert atmosphere in the field, for example, it can...
Embodiment
[0092] The following examples will further illustrate the present invention, but do not limit the present invention thereby.
[0093] In the following examples and comparative examples:
[0094] The method for monitoring the complete reaction: thin-layer chromatography (TLC) fluorescence color method.
[0095] Total yield = molar amount of final product / molar amount of aniline × 100%
[0096] The physical and chemical analysis method of the product: the element content was determined by inductively coupled plasma ion emission spectrometry.
[0097] Structural characterization method: NMR method ( 1 H spectrum, 13 C carbon spectrum), high-resolution mass spectrometry.
preparation example
[0099] Fill a 500ml flask with an electromagnetic stirrer (stirring speed is 300rpm) with nitrogen protection, add 150ml of dichloromethane, then add 0.2mol of sulfur chloride, fully cool in an ice-water bath, add 0.2mol of aniline . Remove the ice-water bath after monitoring until the reaction is complete, and place it at room temperature of 25°C. After the reaction system gradually rises to 25°C, add 4-chloroaniline in 3 times for reaction. The amount added each time is the same, and 4-chloroaniline is added in total 0.15mol. After the reaction was continued for 2 hours, 30ml of saturated brine was added to quench the reaction, and then the reaction system was transferred to a separatory funnel, washed with 50ml of distilled water and 50ml of saturated brine, and dried by adding 10g of anhydrous lithium sulfate at 25°C for 20min. The filtered filtrate was evaporated to remove the solvent at 40° C. and 0.05 MPa to obtain intermediate M1.
[0100] Fill a 500ml flask with an ...
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