Method for preparing high-purity rhodium trichloride from oxo reaction waste rhodium catalyst digestion solution
A rhodium catalyst and oxo synthesis technology, applied in chemical instruments and methods, inorganic chemistry, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, etc., can solve ion exchange burden, cation pre-removal, and affect ion exchange The effect and efficiency of impurity removal, etc., to achieve the effect of reducing the burden of impurity removal and efficient extraction
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Embodiment 1
[0024] Get waste rhodium catalyst digestion solution (rhodium content 0.35%, sulfate radical content 75.20%, phosphate radical content 17.50%, iron content 0.040%, nickel content 0.0025%, calcium content 0.42%) 20 grams, dilute with 40 grams of deionized water to obtain Digestion diluent.
[0025] In addition, weigh 0.2 grams of analytically pure sodium sulfide and make a 12% solution with deionized water (in the form of S 2- gauge), heated to 60°C.
[0026] Control the temperature of the digestion diluent to 80°C, and slowly add the prepared hot sodium sulfide solution while stirring to carry out the precipitation reaction. After the precipitation is completed, filter and wash the precipitate with 6mol / L hydrochloric acid.
[0027] Separately take commercially available 37% analytically pure hydrochloric acid and commercially available 30% analytically pure hydrogen peroxide, and prepare a mixed solution at a volume ratio of 1:1.
[0028] Dissolve the precipitate with the p...
Embodiment 2
[0034] The operation process is the same as in Example 1, and the difference is that the digestion solution is diluted with 6 grams of water, and sodium sulfide is made into a 4% solution (in S 2- meter); the sodium sulfide solution was heated to 90°C, and the temperature of the digestion diluent was controlled to be 120°C;
[0035] Wash the rhodium sulfide precipitate with 12mol / L hydrochloric acid; dissolve the rhodium sulfide precipitate, hydrochloric acid and hydrogen peroxide mixture, and the ratio of hydrochloric acid volume to hydrogen peroxide volume is 3:1.
[0036] The analysis and detection results of the obtained rhodium trichloride showed that the total amount of impurity elements in the rhodium trichloride was 0.026%, which was in line with the first-grade product quality index of YS / T593-2006, and the rhodium yield was calculated to be 99.4%.
Embodiment 3
[0038] The operation process is the same as in Example 1, and the difference is that the digestion solution is diluted with 15 grams of water, and sodium sulfide is made into a 10% solution (in S 2- meter); the sodium sulfide solution was heated to 80°C, and the temperature of the digestion diluent was controlled to be 110°C;
[0039] Wash the rhodium sulfide precipitate with 10mol / L hydrochloric acid; dissolve the rhodium sulfide precipitate, hydrochloric acid and hydrogen peroxide mixture, and the ratio of hydrochloric acid volume to hydrogen peroxide volume is 2:1.
[0040] The analysis and detection results of the obtained rhodium trichloride showed that the total amount of impurity elements in the rhodium trichloride was 0.022%, which was in line with the first-grade product quality index of YS / T593-2006, and the rhodium yield was calculated to be 99.7%.
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