Preparation method of high-purity iridium trichloride
A technology of pure iridium trichloride and ammonium chloride, which is applied in chemical instruments and methods, inorganic chemistry, ruthenium/rhodium/palladium/osmium/iridium/platinum halides, etc., can solve the difficulty of iridium trichloride purification and production Low efficiency, cumbersome process and other problems, to achieve the effect of high yield, high production efficiency and simple process
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Embodiment 1
[0029] Step 1, alkali fusion. Mix the iridium powder with sodium peroxide, sodium hydroxide, and sodium carbonate evenly and put it into an iron crucible. The mass ratio of iridium powder: sodium peroxide: sodium hydroxide: sodium carbonate is 1:1:3:1, and melt at high temperature , The melting temperature is 610°C, the melting time is 3h, and the cooled molten salt is taken out.
[0030] Step 2, slowly dissolve the molten salt with dilute hydrochloric acid, and adjust the pH<1, then add aqua regia to boil, filter off the insoluble residue, add ammonium chloride to the filtrate, keep the concentration of ammonium chloride at about 17%, boil, and filter to obtain Ammonium chloroiridate as a black solid.
[0031] Step 3, pre-purification. Add hydrazine hydrochloride to the black solid ammonium chloroiridate, the dosage of hydrazine hydrochloride is hydrazine hydrochloride: iridium powder = 1:2.13, heat and stir to dissolve the solid slowly, and filter again to obtain ammonium ...
Embodiment 2
[0037] Step 1, alkali fusion. Mix iridium powder with sodium peroxide, sodium hydroxide, and sodium carbonate evenly and put them into a melting crucible. The mass ratio of iridium powder: sodium peroxide: sodium hydroxide: sodium carbonate is 1:0.8:5:1.5, and melt at high temperature , The melting temperature is 550°C, the melting time is 2h, and the cooled molten salt is taken out.
[0038] Step 2, slowly dissolve the molten salt with dilute hydrochloric acid, and adjust the pH to be acidic, then add aqua regia to boil, filter off the insoluble residue, add ammonium chloride to the filtrate, keep the concentration of ammonium chloride at about 10%, boil, and filter to obtain Ammonium chloroiridate as a black solid.
[0039] Step 3, add hydrazine hydrochloride to the black solid ammonium chloroiridate, the dosage of hydrazine hydrochloride is hydrazine hydrochloride: iridium powder = 1:2.13, heat and stir to dissolve the solid slowly, and filter again to obtain ammonium chlo...
Embodiment 3
[0045] Step 1, alkali fusion. Mix iridium powder with sodium peroxide, sodium hydroxide, and sodium carbonate evenly and put them into an iron crucible. The mass ratio of iridium powder: sodium peroxide: sodium hydroxide: sodium carbonate is 1:1:4:1, and melt at high temperature , The melting temperature is 500°C, the melting time is 4h, and the cooled molten salt is taken out.
[0046] Step 2, slowly dissolve the molten salt with dilute hydrochloric acid, and adjust the pH to be acidic, then add aqua regia to boil, filter off the insoluble residue, add ammonium chloride to the filtrate, the concentration of ammonium chloride is 20% of the total concentration of the solution, boil, Ammonium chloroiridate was obtained by filtration as a black solid.
[0047] Step 3, add hydrazine hydrochloride to the black solid ammonium chloroiridate, the dosage of hydrazine hydrochloride is hydrazine hydrochloride: iridium powder = 1:2.13, heat and stir to dissolve the solid slowly, and filt...
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