Lubricating oil complex-phase additive and preparation method thereof
A technology of additives and lubricating oils, which is applied in the direction of additives, lubricating compositions, petroleum industry, etc., can solve the problems of limited improvement of lubricating oil anti-friction and anti-wear properties, and achieve the effects of increasing the allowable limit, avoiding agglomeration, and reducing accumulation
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Embodiment 1
[0045] The preparation method of nano-diamond surface grafted amino group is:
[0046] (1) Mix nano-diamonds with mixed acid, soak for 12 hours; then ultrasonicate for 15 hours, filter, wash with running water, and dry, repeat twice to obtain carboxylated nano-diamonds, wherein the mixed acid is concentrated sulfuric acid and concentrated nitric acid according to the ratio of 1:1 volume ratio mixing;
[0047] (2) Mix carboxylated nano-diamonds and thionyl chloride at a ratio of 1g: 10ml, heat in an oil bath at 50°C for 12h, stir and reflux for 14h, centrifuge the thionyl chloride, wash it with an organic solvent, and dry it in vacuum , to obtain the nano-diamond of acid chloride;
[0048] (3) Mix the chlorinated nano-diamond and diethylenetriamine according to the mass ratio of 1:9, then add it into N,N'-dimethylformamide, and stir and react at 80°C for 24h under the protection of nitrogen , and then distilled off N,N'-dimethylformamide under reduced pressure, washed with an...
Embodiment 2
[0050] The preparation method of nano-diamond surface grafted amino group is:
[0051] (1) Mix nano-diamond with mixed acid, soak for 20h; then ultrasonic for 30h, filter, wash with running water, and dry, repeat twice to obtain carboxylated nano-diamond, wherein mixed acid is concentrated sulfuric acid and concentrated nitric acid according to the ratio of 1:1 volume ratio mixing;
[0052] (2) Mix the carboxylated nano-diamond and thionyl chloride according to the ratio of 1g: 15ml, heat in an oil bath at 60°C for 16h, stir and reflux for 24h, centrifuge the thionyl chloride, wash it with an organic solvent, and dry it in vacuum , to obtain the nano-diamond of acid chloride;
[0053] (3) Mix the acid-chlorinated nano-diamond and diethylenetriamine at a mass ratio of 1:11, then add it to N,N'-dimethylformamide, and stir and react at 90°C for 36h under the protection of nitrogen , and then distilled off N,N'-dimethylformamide under reduced pressure, washed with an organic sol...
Embodiment 3
[0055] The preparation method of nano-diamond surface grafted amino group is:
[0056] (1) Mix nano-diamond with mixed acid, soak for 28h; then ultrasonic for 46h, filter, wash with running water, and dry, repeat 3 times to obtain carboxylated nano-diamond, wherein mixed acid is concentrated sulfuric acid and concentrated nitric acid according to the ratio of 1:1 volume ratio mixing;
[0057] (2) Mix carboxylated nano-diamonds and thionyl chloride at a ratio of 1g:20ml, heat in an oil bath at 70°C for 24 hours, stir and reflux for 48 hours, centrifuge the thionyl chloride, wash it with an organic solvent, and dry it in vacuum , to obtain the nano-diamond of acid chloride;
[0058] (3) Mix the acid-chlorinated nano-diamond and diethylenetriamine at a mass ratio of 1:15, then add it to N,N'-dimethylformamide, and stir and react at 98°C for 48h under the protection of nitrogen , and then distilled off N,N'-dimethylformamide under reduced pressure, washed with an organic solvent...
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