氢还原重量法测定硝酸铑产品中铑含量

根据冶金工艺中铑的精炼原理,建立了氢还原重量法测定硝酸铑产品中铑含量的方法。研究并优化了测定条件,考察了杂质元素对铑分析结果的影响。结果表明:在0.3～0.9 mol/L硝酸介质中,硝酸铑与氯化铵形成一种(NH₄)₃ RhCl₆红色络合物晶体,该晶体经过在约100 ℃烘干水分、350 ℃分解铵盐、750 ℃氢还原为海绵铑和105 ℃干燥后可以采用重量法测定其中的铑。用该方法测定硝酸铑产品中质量分数为6.55%、7.36%、8.05% 、9.99%和20.05%铑的极差(R)为±0.01%,标准偏差(SD)为0.004 1%,相对标准偏差(RSD,n=22)在0.02%～0.06%范围。本法测定结果较YS/T 594-2006标准配套分析方法的准确度和精密度高。     

硫酸亚铁电位滴定法测定金、钯合金中金的不确定度评定

通过硫酸亚铁电位滴定法测定AuBe1、AuNi9、AuAgCu35-5、PdAgCuAuPtZn30-14-10-10-1合金中Au的实践,分析了测定不同Au含量过程中的不确定度来源,建立了数学模型,计算了各标准不确定度分量、合成标准不确定度和扩展不确定度。结果表明：测定合金样品中9.99%、60.16%、90.85%、98.93%的Au含量,扩展不确定度分别为0.02%、0.14%、0.22%、0.24%。     

Reviews of Metallurgical Technology to Recovery Platinum Group Metals from Secondary Resource in China

China is extremely poor in mineral resources of Platinum Group Metals (PGMs), productive output of PGMs from mineral resource is 2.5 tons per year. At the same time, China is the biggest PGMs consumption country in the world, the mineral resource of PGMs is critical shortage, it shows the importance of recycling the secondary resource of PGMs. Sino-Platinum Metals Resource (Yimen) Co., Ltd. is the leader in recycling of PGMs from secondary resource, and has made outstanding contributions to China PGMs secondary resources recycling. This article elucidates the current situation of secondary resources recovery and development of metallurgical technology for PGMs.     

钌的氯配合物及其分离提纯理论基础

介绍了钌的溶解、分离、精炼提纯过程中常用的化学反应,总结了四氧化钌、钌的氯配合物及水合阳离子等独特的性质,以及这些特性在分离提纯中的应用。     

EDTA差减滴定法测定钼精矿和钼焙砂中钼含量

用盐酸羟胺还原钼(Ⅵ)至钼(Ⅴ),EDTA络合钼(Ⅴ)及共存离子,锌盐滴定过量EDTA求得合量。于等量试液中不加盐酸羟胺,EDTA络合共存离子,滴定至近终点用酒石酸钾钠掩蔽钼(Ⅵ),锌盐滴定过量EDTA求得分量。二者之差即为钼量。2%～5%钨(Ⅵ)、铬(Ⅵ)或钒(Ⅴ)等共存离子不干扰测定。测定10.00～15.00 mg钼,相对误差-0.20%～+0.20%,测定37%～57%的钼含量,相对标准偏差0.10%～0.15%,样品加标准回收率99.60%～100.80%。方法结果准确度与钼酸铅重量法的一致,但本法选择性好、分析快速。     

氯铂酸铵酸洗除杂精炼铂

提出通过酸洗氯铂酸铵除杂精炼铂的方法。研究了酸种类、酸浓度、固液比、温度对酸洗除杂效率的影响,优选条件下90%以上的Na、Al、Fe、Si被去除,铂溶解率低于0.3%,酸洗氯铂酸铵制备的海绵铂除Sn外其余杂质含量达到SM-Pt 99.95标准。对酸洗过程Sn的行为研究结果表明,酸洗或煅烧氯铂酸铵都可以去除以(NH₄)₂SnCl₆形式存在的Sn,实现相同的除Sn效果,但不能去除以SnO₂形式存在的Sn。     

Study on the Recovery of Rhodium from Spent Organic Rhodium Catalysts of Acetic Acid Industry Using Pyrometallurgical Process

A new process recycling rhodium from organic waste containing rhodium in acetic acid industry is developed. Use the special affinity of base metal sulfides (FeS, Ni2S3 , CuS, etc.) on platinum group metals, adopting high nickel matte trapping-aluminothermic activation method to recovery rhodium from incinerator residue of organic rhodium waste. The method is shorter process, lower equipment requirement, and the higher activity of rhodium black. In pyrometallurgy enrichment process,the recovery rate of rhodium reached 94.65%, the full flow of rhodium recovery rate was 92.04%.     

化学沉淀法制备高纯钌粉试验研究

研究了以RuCl_3溶液为原料、采用氯化铵沉淀—煅烧—(高能球磨)—氢还原法制备高纯钌粉。试验结果表明:煅烧后直接氢还原得到的钌粉呈多孔不规则形状,粉末颗粒尺寸5~8μm;经过高能球磨再还原得到的钌粉呈团聚的海绵状,颗粒尺寸约1μm;钌粉纯度均为99.95%以上。     

溶剂萃取法从含微量贵金属废液中回收铂钯

采用溶剂萃取技术从含微量贵金属的废液中回收铂和钯。结果表明：在有机相为3%LIX84-I+97%Solvesso150、0.1 mol/L HCl、相比为1∶3的条件下,可以从废液中高效选择萃取钯,钯萃取率达99.9%以上;在有机相为8%TOA+92%磺化煤油、0.1 mol/L HCl、相比为1∶5的条件下,钯萃余液中铂的萃取率达99.95%以上,实现贵金属的有效回收。相较于沉淀法和置换法,溶剂萃取法操作更简单、金属回收率更高,且可一步实现贵金属的回收与分离,处理后的废水可直接并入常规污水处理流程,达到环保要求。     

Toward high stability single crystal material by structural regulation with high and low temperature mixing sinter

Single-crystal cathode materials are a potential research focus for high-nickel ternary cathode materials owing to their high compaction density and good electrochemical stability. However, in the traditional sintering process, lithium is lost because of the long-time and higher-temperature sintering, which reduces the migration energy barrier of Ni²⁺ and increases the degree of mixing of Li⁺ and Ni²⁺. Herein, for the first time, a method for short-time high-temperature sintering combined with low-temperature heat preservation is proposed to prepare LiNi_0.6Co_0.6Mn_0.2O₂ (NCM622) single crystal materials in a mixed molten salt system of LiOH and Li₂CO₃. In analyses of morphology, structure and electrochemical properties, the prepared NCM622 exhibits excellent cycling stability owing to an ordered layered structure and low cation mixing degree. The single-crystal material shows an excellent capacity retention of 93.19% (150.49–140.24mAh·g^?1) after 100 cycles at 1 C in the voltage range of 2.8–4.3 V. The single crystal particles exhibit reliable stability after long cycling without microcracks in the cycled particles. Furthermore, the preparation cost could be significantly reduced with a closed loop of the flux salt. The short-time high-temperature combined with the low-temperature holding sintering method may provide an effective strategy for the synthesis of other single-crystal materials with excellent electrochemical properties.