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Solvent extraction separation and recovery of palladium and platinum from chloride leach liquors of spent automobile catalyst

机译:汽车废催化剂氯化物浸出液中溶剂萃取分离和回收钯和铂

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摘要

Spent catalysts from automobile industry contain environmentally critical and economically valuable metals such as Pt, Pd, Fe, Ni, Mn, and Cr. In this paper, we report the solvent extraction separation and recovery of palladium (Pd) and platinum (Pt) from hydrochloric acid leach liquors of spent automobile catalyst employing precipitation and solvent extraction methods. Composition of synthetic leach liquor (IX) used for the present study contains (mg/L): Pd-150, Pt-550, Mn-500, Ni-1000, Fe-1500, Cr-100 and 3 M HCl. Variation of tri-n-butyl phosphate (TBP) in the range from 0.0018 to 0.183 M in kerosene indicated selective and quantitative extraction of Pd even at the lowest extractant concentration. McCabe-Thiele plot for Pd extraction with 0.0054 M TBP predicted complete separation of metal in two stages at an aqueous to organic (A/O) phase ratio of 3.75. Counter-current batch extraction simulation (CCES) of Pd at an A/O of 3.75 resulted in a raffinate containing 0.13 mg/L of Pd, corresponding to Pd extraction efficiency of 99.9%. Stripping of Pd from loaded organic (LO) phase at O/A ratio of 5 with 0.5 M thiourea and 0.1 M HCl indicated 1.1 mg/L of Pd in spent organic (SO), with a stripping efficiency of 99.8%. The strip solution (SS) contains 2.8 g/L of Pd, with overall enrichment factor of 18.8 times. From the Pd-raffinate, complete removal of iron (Fe), 72% Cr and 5% Ni and 9.2% Mn was achieved at an aqueous pH of 3.2; whereas the loss of Pt was ~9.1 %. The observed loss of Pt was due to adsorption of metal on the hydrated iron oxide generated in situ. Variation of Aliquat 336 in the range from 0.002 to 0.22 M on the extraction of Pt from Pd-Fe free raffinate showed selective extraction of Pt and reached to 99.7% at 0.011M concentration. McCabe-Thiele plot for Pt extraction with 0.011 M Aliquat 336 predicted >99% extraction of Pt in two stages at A/O phase ratio of 3 and two stages of stripping with 0.5 M each of thiourea and HCl at an O/A phase ratio 4. Extraction and stripping simulation tests confirmed Pt extraction and stripping efficiency of 99.83 and 99.9%, respectively with an enrichment factor of 12 times. Finally, complete flow sheet of the process for the separation and recovery of Pd and Pt as chlorides was demonstrated.
机译:来自汽车工业的废催化剂包含对环境至关重要且具有经济价值的金属,例如Pt,Pd,Fe,Ni,Mn和Cr。本文报道了采用沉淀法和溶剂萃取法从废旧汽车催化剂的盐酸浸提液中萃取分离和回收钯(Pd)和铂(Pt)的方法。用于本研究的合成浸出液(IX)的成分包含(mg / L):Pd-150,Pt-550,Mn-500,Ni-1000,Fe-1500,Cr-100和3 M HCl。煤油中磷酸三正丁酯(TBP)的变化范围为0.0018至0.183 M,这表明即使在最低萃取剂浓度下,Pd的选择性和定量萃取也是如此。用0.0054 M TBP萃取Pd的McCabe-Thiele图预测,在水与有机(A / O)相比为3.75的情况下,金属可以分两个阶段完全分离。在A / O为3.75的条件下对Pd进行逆流分批萃取模拟(CCES),得到的萃余液含有0.13 mg / L的Pd,对应的Pd萃取效率为99.9%。用0.5 M的硫脲和0.1 M HCl以5的O / A比从负载的有机(LO)相中萃取Pd表明,废有机(SO)中的Pd含量为1.1 mg / L,萃取效率为99.8%。试纸溶液(SS)含2.8 g / L的Pd,总富集系数为18.8倍。在3.2的水溶液pH值下,可以从钯-残液中完全去除铁(Fe),72%的铬和5%的镍以及9.2%的锰。 Pt的损失约为9.1%。观察到的Pt损失是由于金属吸附在原位生成的水合氧化铁上。从不含Pd-Fe的残液中提取Pt时,Aliquat 336的变化范围为0.002至0.22 M,这表明Pt有选择地提取,在0.011M的浓度下达到了99.7%。用0.011 M Aliquat 336萃取Pt的McCabe-Thiele图预测在A / O相比为3的两个阶段中萃取Pt的> 99%,以及在O / A相比中分别用硫脲和HCl分别萃取0.5 M的两个阶段4.萃取和剥离模拟试验证实铂的萃取和剥离效率分别为99.83和99.9%,富集系数为12倍。最后,展示了用于分离和回收氯化物的钯和铂的完整工艺流程图。

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