Calcium-based lubricating grease composition with excellent antifriction property and preparation method therefor
A lubricating grease composition and technology of calcium-based lubricating grease, applied in the field of lubricating grease, can solve the problems of limited hardening improvement, long production time, hardening of composite calcium-based lubricating grease, etc. The effect of good high temperature resistance
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[0047] Among the present invention, the preparation method of the compound of structure shown in formula (I) preferably comprises:
[0048] (a) react aniline, sulfur chloride and 4-chloroaniline to generate intermediate M shown in formula (II),
[0049]
[0050] (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),
[0051]
[0052] In step (a) of the present invention, the specific mode of reacting aniline, sulfur chloride and 4-chloroaniline preferably includes:
[0053] (i) fully reacting aniline and sulfur chloride at -20-0°C in the first solvent under an inert atmosphere;
[0054] (ii) Add 4-chloroaniline into the reaction system of step (i), and react at 15-30° C. for 1-3 h.
[0055] In the present invention, the inert atmosphere can be a conventional inert atmosphere in the field, for example, it can...
Embodiment
[0093] The following examples will further illustrate the present invention, but do not limit the present invention thereby.
[0094] In the following examples and comparative examples:
[0095] The method for monitoring the complete reaction: thin-layer chromatography (TLC) fluorescence color method.
[0096] Total yield = molar amount of final product / molar amount of aniline × 100%
[0097] The physical and chemical analysis method of the product: the element content was determined by inductively coupled plasma ion emission spectrometry.
[0098] Structural characterization method: NMR method ( 1 H spectrum, 13 C carbon spectrum), high-resolution mass spectrometry.
preparation example
[0100] 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 continuing the reaction 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 calcium 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.
[0101] Fill a 500ml flask with an ele...
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