A kind of lithium composite grease and preparation method thereof
A lithium-composite and lubricating grease technology, applied in the field of lubricating grease, can solve the problems of enhanced non-radiative attenuation process and reduced fluorescence quantum yield
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Embodiment 1
[0041] 200 mL of polyphosphoric acid (PPA), 0.2 mol of o-aminothiophenol and 0.2 mol of p-bromosalicylic acid were added to a 500 mL three-necked flask, and the reaction was stirred at 160° C. for 6 h under nitrogen protection. After the reactant is cooled, it is diluted with a large amount of ice water, adjusted to neutrality with 10% sodium hydroxide solution and saturated sodium carbonate solution, a large amount of solid is precipitated, and the crude product is obtained by filtration. Dissolve the crude product with 1,4-dioxane, filter to remove insoluble impurities, add an appropriate amount of water to the filtrate, collect the precipitated solid, and dry it in a vacuum oven at 60°C to obtain 2-(2'-hydroxyl- 4-Bromophenyl)benzothiazole in 54% yield. The NMR results are: 1 H NMR (400MHz, DMSO-d6), δ (TMS, ppm): 11.71 (s, 1H), 8.02 (d, 1H), 7.88 (d, 1H), 7.62 (d, 1H), 7.45 (m, 1H) ),7.33(m,1H),6.24(d,1H),6.15(d,1H,),5.95(s,2H).MS(ESI-TOF):304.95([M+H] + ).
[0042] Th...
Embodiment 2
[0045] Into a 100 mL Schlenk reaction flask, add 10 mmol of 2-(2'-hydroxy-4-bromophenyl) benzothiazole, 30 mmol of 4-(dicyanovinyl) phenylacetylene, 1 mmol of cuprous iodide, and 1 mmol of triphenylphosphine. Under nitrogen protection, 0.2 mmol of tetrakistriphenylphosphine palladium and 50 mL of tetrahydrofuran / triethylamine (2 / 1, v / v) were added, and the reaction was carried out at room temperature for 48 hours. After the reaction, filter and spin dry the filtrate, use dichloromethane / methanol (20 / 1, v / v) mixed solvent as eluent to separate and purify the product by column chromatography to obtain 2-(2'- Hydroxy-4'-dicyanovinylbenzynyl)benzothiazole, yellow solid product in 57% yield. The NMR results are: 1 H NMR (400MHz, CDCl 3 ), δ(TMS, ppm): 11.71(s, 1H), 8.02(d, 1H), 7.98(d, 1H), 7.78(s, 1H), 7.62(d, 2H), 7.58(d, 1H) ,7.45(m,1H),7.35(d,2H),7.33(m,1H),6.24(d,1H),6.15(d,1H,).MS(MALDI-TOF):m / z calcd:403.1 [M] + , found: 403.1.
[0046] The reaction formula of embodime...
Embodiment 3
[0049] 50 grams of 500SN base oil, 10 grams of 12-hydroxystearic acid, and 3.3 grams of sebacic acid were mixed and heated to 85°C in a reaction kettle, and 0.5 grams of 2-(2'-hydroxy-4'-dicyanovinyl Benzynyl) benzothiazole was dissolved in 10 grams of toluene and added to the reactor. 2.8 grams of lithium hydroxide monohydrate and 18 grams of distilled water were mixed and heated to 95 ° C. After all the lithium hydroxide was dissolved, it was added dropwise to the reactor. Carry out saponification reaction for 20min, stir and heat up to 110-150°C for dehydration and detoluene removal, then continue to heat up to 210°C for high-temperature refining for 10min, add 36.5 grams of 500SN base oil, cool to 110°C, add 0.5g of diphenylamine, petroleum sulphur Barium acid 0.5g, cooled to room temperature and ground into grease.
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