Non-aqueous solution homogeneous phase reduction preparation of nano metallic ruthenium
A nano metal, non-aqueous solution technology, applied in the field of homogeneous reduction preparation of nano metal ruthenium in non-aqueous solution
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[0017] Preparation steps of the present invention:
[0018] (1) According to the concentration range, the basic coordination compound used to absorb ruthenium ions is dissolved in an inert solvent to become carrier solution I, and the neutral coordination compound or neutral coordination compound used to absorb monovalent copper ions The compound is mainly dissolved in an inert solvent into a coordination compound in which an acidic coordination compound is added to become a carrier solution II;
[0019] (2) dissolving the compound containing ruthenium ions in carrier solution I to prepare reaction solution I, and preparing a source solution containing ruthenium ions, dissolving monovalent copper ions in carrier solution II to prepare reaction solution II;
[0020] (1) The reaction solution I obtained in the step (2) is mixed with the step reaction solution II to generate a reaction, the volume ratio of the two reaction solutions is 4:1~1:4, stirring and mixing, and observing ...
Embodiment 1
[0024] First, trioctylamine is dissolved in kerosene, and it is prepared into 1 liter of carrier solution, and the volume concentration of the coordination compound is 20%; Ruthenium nitrate is dissolved in it, and it is prepared into a saturated reaction solution containing ruthenium ions; then copper nitrite is dissolved in In the kerosene containing 20% tributyl phosphate and 10% di(2-ethylhexyl) phosphoric acid, prepare 0.3 liters of saturated reaction solution containing monovalent copper ions; The reaction solution was mixed with a volume ratio of 3:1, and stirred electrically for 120 minutes. After the reaction was completed, after standing for 6 hours, it can be seen that the solution gradually changed from brown to dark green, and turned grayish black due to the generation of precipitates; The solution is filtered through filter paper, washed with acetone, and dried to obtain nano-metal ruthenium products with an average size of about 9 nm.
Embodiment 2
[0026] First, trilaurylamine is dissolved in paraffin oil to prepare 1 liter of carrier solution, and the volume concentration of the coordination compound is 15%; ruthenium nitrate is dissolved in it to prepare a saturated reaction solution containing ruthenium ions; then copper nitrite is dissolved In paraffin oil containing 10% of di(2-ethylhexyl) phosphate (2-ethylhexyl) ester and 20% of n-butyl dibutyl phosphate, prepare 0.2 liter of saturated reaction solution containing monovalent copper ions; Mix the reaction solution containing ruthenium and the reaction solution containing monovalent copper ions at a volume ratio of 2:1, and stir it electrically for 60 minutes. After the reaction is completed, after standing for 8 hours, it can be seen that it gradually changes from brown to dark green, and due to precipitation The product turns gray and black; the solution containing the generated precipitate is filtered through filter paper, washed with acetone, and dried to obtain ...
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