Method for preparing high-purity acetylacetonatodicarbonyl rhodium through using rhodium trichloride
A technology of rhodium acetone dicarbonyl and rhodium trichloride, which is applied in the field of catalysis and can solve problems such as difficult removal of impurities
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Embodiment 1
[0020]1.00 g of rhodium chloride hydrate containing sodium, iron, nickel, and calcium metal impurities (the mass contents of rhodium, sodium, iron, nickel, and calcium are respectively: 35.21%, 0.97%, 0.0143%, 0.0014%, and 0.0256%) and Put 15 ml of N, N-dimethylformamide and 4 ml of acetylacetone in a 50 ml round-bottomed flask, heat to 80°C, keep for 0.5 hour, continue to raise the temperature to 136°C and keep for 1 hour, after the reaction is completed, the reaction solution is naturally Cool to room temperature, add 100 milliliters of deionized water, filter out acetylacetonate rhodium dicarbonyl precipitation after mixing evenly, wash filter cake with deionized water, after the acetylacetonate dicarbonyl rhodium crude product that obtains is dissolved with 40 milliliters of toluene solvent, then with 40 milliliters Wash the toluene phase twice (40×2) with a disodium edetate aqueous solution (mass concentration 0.1%), and then wash the toluene phase once with 40 ml of deion...
Embodiment 2
[0022] 1.00 g of rhodium chloride hydrate containing sodium, iron, nickel, and calcium metal impurities (the mass contents of rhodium, sodium, iron, nickel, and calcium are respectively: 34.87%, 0.69%, 0.0118%, 0.8920%, and 0.0235%) and Put 15 ml of N, N-dimethylformamide and 4 ml of acetylacetone in a 50 ml round-bottomed flask, heat to 80°C, keep for 0.5 hour, continue to raise the temperature to 136°C and keep for 1 hour, after the reaction is completed, the reaction solution is naturally Cool to room temperature, add 100 milliliters of deionized water, filter out the rhodium acetylacetonate precipitate after mixing evenly, wash the filter cake with deionized water, after the crude product of rhodium acetylacetonate dicarbonyl is dissolved with 40 milliliters of toluene solvent, then use 2 milliliters Wash the toluene phase twice (2×2) with an aqueous solution of disodium edetate (mass concentration 2.0%), and then wash the toluene phase once (2×1) with 2 ml of deionized wat...
Embodiment 3
[0024] 1.00 g of rhodium chloride hydrate containing sodium, iron, nickel, and calcium metal impurities (the mass contents of rhodium, sodium, iron, nickel, and calcium are respectively: 34.30%, 0.54%, 0.0124%, 0.0018%, and 0.8630%) and Put 15 ml of N, N-dimethylformamide and 4 ml of acetylacetone in a 50 ml round-bottomed flask, heat to 80°C, keep for 0.5 hour, continue to raise the temperature to 136°C and keep for 1 hour, after the reaction is completed, the reaction solution is naturally Cool to room temperature, add 100 milliliters of deionized water, filter out the rhodium acetylacetonate precipitate after mixing evenly, wash the filter cake with deionized water, after the crude product of rhodium acetylacetonate dicarbonyl is dissolved with 4 milliliters of toluene solvent, then use 8 milliliters Wash the toluene phase twice (8×2) with a disodium edetate aqueous solution (mass concentration 0.6%), and then wash the toluene phase once with 8 ml of deionized water (8×1), t...
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