Sulfuric Acid → Rhodium(III) sulfate

Participants

Reaction Steps

The technique for preparing this rhodium sulfate complex is described by the flow chart of FIG. 3. Rhodium is refluxed in sulfuric acid as shown to produce a rhodium sulfate concentrate. The rhodium sulfate is then neutralized with a mild base, in this case, ammonium hydroxide, by the two procedures shown in the figure. The first, Process A, is the conventional hydrolysis in which the acid and base are simply combined, with both reagents typically at room temperature. The neutralization reaction is exothermic, and the solution characteristically heats to a temperature substantially above room temperature. In the process of the invention, Process B, the neutralization reaction is controlled by cooling the rhodium sulfate to a temperature below room temperature, e.g., below 20° C., and maintaining the reagent mixture at a temperature below 25° C. during the reaction. This can be achieved by actively cooling the reaction vessel. In practice, it was found that using a jacketed reaction vessel, and flowing cool or cold water, e.g. water at 10° C., through the vessel jacket, the temperature of the reagent mixture can be controlled to a temperature below 25° C. Without active cooling during the reaction, as described above, the reagent mixture heats to a temperature above 25° C.

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