Preparation method of trivalent rhodium acetate tripolymer
A technology of rhodium acetate trimer and glacial acetic acid, which is applied in the field of preparation of trivalent rhodium acetate trimer, can solve problems such as easy dehydration, poor solubility, and long synthesis time, so as to accelerate precipitation reaction, increase reaction rate, shorten The effect of the production cycle
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[0043] A preparation method of trivalent rhodium acetate trimer, comprising the following steps:
[0044] (1) After mixing the rhodium powder and potassium chloride, feed chlorine gas at a flow rate of 0.1 to 5 L / min, and react at 500 to 800° C. for 1 to 5 hours;
[0045] (2) Dissolve the product obtained in step (1) in water, filter, add 10-40wt% potassium hydroxide solution to the filtrate so that the pH value is between 7-10, react for 0.5-2h, filter and wash , obtain rhodium hydroxide;
[0046] (3) add water, 60~65wt% nitric acid and glacial acetic acid in rhodium hydroxide, the mass ratio of described rhodium hydroxide, water, nitric acid and glacial acetic acid is 1:2~30:0.5~3:1~5, React at 30-90° C. for 0.5-3 hours, evaporate the solution to dryness, use glacial acetic acid to remove the nitrate, and then use water to remove the acid to obtain trivalent rhodium acetate trimer.
[0047] Optionally, in step (2), before adding potassium hydroxide, add positively modified...
Embodiment 1
[0053] A preparation method of trivalent rhodium acetate trimer, comprising the following steps:
[0054] (1) Mix 30g of rhodium powder and 100g of potassium chloride evenly, put it into a quartz boat, transfer it to a medium-temperature tube furnace at 600°C, feed chlorine gas at a flow rate of 1L / min, and react for 3h.
[0055] (2) Dissolve the product obtained in step (1) in 0.5L water, filter, add 15wt% potassium hydroxide solution to the filtrate to adjust the pH to 8.0, react for 1h, filter, and wash with 2L deionized water several times to obtain Pure rhodium hydroxide. After detection, the yield of preparing rhodium hydroxide by potassium chlororhodate is 96.0%.
[0056] (3) Get rhodium hydroxide (0.100mol) containing 10.29g of rhodium, add 100g of deionized water to it, then add 29.08g of 65% analytically pure nitric acid and 28.00g of glacial acetic acid at the same time, stir and reflux at 60°C for 1h, filter , placed in an evaporating dish and evaporated to dryne...
Embodiment 2
[0058] A preparation method of trivalent rhodium acetate trimer, comprising the following steps:
[0059] (1) Mix 100g of rhodium powder and 200g of potassium chloride evenly, put it into a quartz boat, transfer it to a medium-temperature tube furnace at 650°C, feed chlorine gas at a flow rate of 4L / min, and react for 2h.
[0060] (2) Dissolve the product obtained in step (1) in 1L of water, filter, add 25wt% potassium hydroxide solution to the filtrate to adjust the pH to 9.0, react for 1.5h, filter, and wash with 6L of deionized water several times to obtain Pure rhodium hydroxide. After detection, the yield of preparing rhodium hydroxide by potassium chlororhodate is 96.1%.
[0061] (3) get the rhodium hydroxide (0.488mol) that rhodium content is 50.23g, add 400g deionized water wherein, add 65% analytical pure nitric acid 150.00g and glacial acetic acid 300.00g simultaneously again, 80 ℃ stir and reflux 1.5h, Filter, place in an evaporating dish and evaporate to dryness;...
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