采用外冷凝装置代替醋酸钯制备工艺中的回流装置,实现了冰醋酸的回收和结晶母液体积的控制.确定了溶解10 g海绵钯需要250 mL冰醋酸和5 mL硝酸的最佳溶剂用量,同时得出醋酸钯母液钯质量浓度为65 g/L时醋酸钯的产率最高.经2次结晶,醋酸钯的总产率为98.46%.改进后工艺稳定,产率提高,成本节约,钯的总回收率达99.95%以上,红外光谱结果表明产物为三聚体醋酸钯.
The outer condenser was used as a substitute for circulator reflux in the process of palladium(Ⅱ) diacetate preparation, in order to recover glacial acetic acid and to adjust the volume of crystalline palladium(Ⅱ) diacetate mother solution. It was found by the research that the optimal amounts of 250 mL glacial acetic acid and 5 mL nitric acid are required for dissolution of per 10 g palladium sponge. When the concentration of the mother solution is palladium 65 g/L, the crystal yield maximum of palladium(Ⅱ) diacetate could be reached. The yield of crystalline trimeric palladium(Ⅱ) diacetate is 98.46% via two step crystallize. The modified method possesses the advantages of stable process, yield improving and cost saving, the total recovery of palladium is up to 99.95%. It was proved by infrared spectrum (IR) that the product is trimeric palladium(Ⅱ) diacetate.
参考文献
| [1] | Eugene A Hausman;Cranford N J;James R Grasso et al.Palladium diacetate and method for its preparation[P].US,3318891,1967. |
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