Method for recovering rhodium to produce rhodium chloride hydrate from oxo synthesis reaction waste rhodium catalyst
A hydrated rhodium chloride, rhodium catalyst technology, applied in chemical instruments and methods, inorganic chemistry, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, etc., can solve the problem of low efficiency and complex post-processing of the all-liquid-phase digestion method , rhodium loss and other problems, to avoid rhodium loss, simple operation, high rhodium yield effect
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Embodiment 1
[0027] Take 500g of rhodium-containing waste catalyst (rhodium content 1750ppm) and put it into a 1L two-necked flask, add 80g of dimethylformamide, place it in an oil bath with magnetic stirring, connect one port to the condensing device and the tail gas treatment device, and the other port to nitrogen , start stirring and mixing, slowly introduce nitrogen, and raise the temperature step by step: first, control the temperature of the oil bath to 90°C, and evaporate the light components; When no liquid drops flowed out again, the temperature of the oil bath was controlled to 180° C., and the temperature was kept constant for 1.5 hours to obtain 116.5 g of raffinate.
[0028] Add 120mL ethanol to the residual liquid to dilute, filter with a sand core funnel, wash the filter residue three times with 60mL ethanol, blow dry, add 37% hydrochloric acid 10mL, 30% hydrogen peroxide 5mL to dissolve the filter residue successively, and collect the rhodium chloride solution , after dilut...
Embodiment 2
[0034] The raw material, raw material quantity, device and steps are the same as in Example 1, except that 60g of dimethylformamide is added; the temperature is raised step by step: firstly, the temperature of the oil bath is controlled to 90°C, and the light components are evaporated; Control the temperature of the oil bath to 155°C; when there is no droplet flowing out of the evaporation and condensation device again, control the temperature of the oil bath to 185°C and keep the temperature constant for 2.0 hours. 102.8 g of raffinate was obtained.
[0035] Analysis and testing results show that the total amount of impurity elements in rhodium trichloride is 0.046%, which meets the first-grade product quality index of YS / T593-2006, and the calculated rhodium yield is 99.5%.
Embodiment 3
[0037] Get 50g of rhodium-containing waste catalyst distillation rhodium slag (rhodium content 4.7%) and add in 500mL two-necked flask, add 120g of dimethylformamide, place in an oil bath with magnetic stirring, connect a condensing device and a tail gas treatment device at one port, Connect the other port with nitrogen, turn on stirring and mixing, slowly introduce nitrogen, and increase the temperature step by step: first control the temperature of the oil bath to 90°C, and evaporate the light components; when there is no liquid drop out of the evaporation and condensation device, control the temperature of the oil bath to 158°C ; When no liquid drops flow out from the evaporating and condensing device again, control the temperature of the oil bath to 185° C. and keep the temperature constant for 2 hours. 43.5 g of raffinate was obtained.
[0038]Add 50 mL of ethanol to the residual liquid to dilute, filter with a sand core funnel, wash the filter residue three times with 90...
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