A kind of preparation method and application of nano cobalt tungstate cesium salt
A cesium tungstate and nano-cobalt technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of easy agglomeration and poor dispersion.
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Embodiment 1
[0034] The preparation of embodiment 1 nano cobalt tungstate cesium salt
[0035] 1) Dissolve 9.907g of sodium tungstate dihydrate (0.003mol) in 20mL of water, then add 1.8mL of glacial acetic acid, white flocs appear in the reaction, and then disappear quickly. Then use pH test paper to test, adjust the pH to about 7, dissolve 1.256g cobalt acetate tetrahydrate in 6mL-7mL water, then add 2 drops of glacial acetic acid, the solution is purple; heat the sodium tungstate solution to near boiling (with tiny bubbles ), under stirring, immediately add cobalt acetate solution, the solution becomes turbid black green, obtain the first mixed solution, make the first mixed solution slightly boil for 15min, then add 14.715g CsCl (0.088mol), during this process the solution The color gradually changed to dark green and finally green, the solution was concentrated and cooled to room temperature;
[0036]2) adding an appropriate amount of hydroxylamine hydrochloride to the concentrated so...
Embodiment 2
[0039] Application of embodiment 2 nano cobalt tungstate cesium salt in the preparation of 4-(4-fluorobenzylamino)-1-methylpiperidine
[0040] Dissolve 10.54g (0.085mol) of N-methylpiperid-4-one (N-methylpiperid-4-one) and 11.30g (0.10mol) of 4-fluorobenzylamine (4-fluorobenzylamine) in 30mL of toluene, add 0.5 g of nano-cobalt cesium tungstate prepared according to Example 1 was used as a catalyst, heated to reflux to separate water, and when no water flowed out of the water separator, about 2-2.8 mL of water was separated. Then it was cooled, and the toluene was distilled off under reduced pressure. After cooling, add 50 mL of absolute ethanol, add 3.5 g of sodium borohydride in batches, stir for 40 min after the addition, and heat to reflux for 4 h after the completion of the reaction. After cooling, 60 ml of 10% hydrochloric acid was slowly added dropwise, and then refluxed for 1 hour. After cooling, the ethanol was evaporated under reduced pressure. Sodium carbonate wa...
Embodiment 3
[0044] Embodiment 3: the preparation of nano cobalt tungstate cesium salt
[0045] 1) Dissolve 4.9635g of sodium tungstate dihydrate (0.015mol) in 10mL of water, then add 1.0mL of glacial acetic acid, white flocs appear in the reaction, and then disappear quickly. Then use pH test paper to test, adjust the pH to about 7, dissolve 0.5014g of cobalt nitrate in 5mL of water, then add 2 drops of glacial acetic acid, the solution is purple; heat the sodium tungstate solution to near boiling (it only needs to have tiny bubbles) , add cobalt acetate solution immediately under stirring, the solution becomes turbid black green, obtain the first mixed solution, make the first mixed solution slightly boil for 15min, add 7.352g CsCl (0.044mol) again, the solution color changes gradually during this process It is dark green, and finally turns green, the solution is concentrated and cooled to room temperature;
[0046] 2) Add 0.7 g of hydroxylamine hydrochloride to the concentrated solutio...
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