ICP-AES法测定废催化剂不溶渣中的铂、钯和铑

采用碱熔-碲共沉淀分离富集,用电感-耦合等离子体发射光谱法(ICP-AES)测定精细化工废催化剂不溶渣中的铂、钯、铑含量。系统考察了碱熔解和碲共沉淀富集分离的条件,研究了碲富集物中的主要元素和比例,确定了ICP-AES法测定铂、钯、铑的条件。结果表明,碱熔-共沉淀能够充分分离富集样品中的铂、钯、铑;测定催化剂不溶渣中653~3652 g/t铂、447~3804 g/t钯、539~6433g/t铑时,相对标准偏差(RSD)、样品加标回收率分别为铂0.84%~1.78%、97.0%~99.4%,钯1.05%~1.82%、97.0%~100.6%,铑1.00%~2.12%、98.2%~100.4%。方法分析快速、易于掌握,已用于生产分析中。     

从废NiPt靶材中回收铂、镍的研究

针对废NiPt靶材，提出采用选择性溶解-中和沉淀工艺回收镍，铂富集物王水溶解-氧化水解除杂-氯化铵沉淀-煅烧工艺回收铂。结果表明，在硫酸浓度40%、溶解温度85℃、溶解时间4 h、液固比4的条件下，镍溶解率大于99.4%，镍回收率大于99%。铂富集物通过王水溶解、氧化水解除杂、氯化铵沉淀、煅烧后，获得纯度大于99.99%的海绵铂，铂回收率大于99.5%。     

密闭消解-ICP-AES法测定硅铁合金中的铂、钯、铑量

研究了硅铁合金富集物样品溶解条件及铁、硅对铂、钯、铑测定的干扰情况。在聚四氟乙烯消化罐中,用盐酸-双氧水(15+3)将样品于150℃恒温密闭消解8 h以上,用ICP-AES测定铂、钯、铑含量。结果表明,在选定的溶解和测定条件下,铂、钯、铑测定相对标准偏差<2%,加标回收率为97%～102%。与碱熔-碲共沉淀-ICP-AES法进行对比,结果一致性好。可满足硅铁合金富集物中铂、钯、铑的测定要求。     

硝酸工厂铂合金催化网的铂耗

铂耗和氨耗是硝酸生产的主要技术指标。在流动氧气氛模拟条件下,以及800~950℃的硝酸生产实际氨氧化环境中,Pt-Rh二元和Pt-Pd-Rh三元合金及其催化网的失重和铂耗均遵循相同的模式,即ΔW/S=Kt2/3与ΨΣ=K't2/3。工厂实际测定数据表明,在常压氨氧化法生产硝酸过程中,Pt-12Pd-3.5Rh合金催化网的铂耗为0.044 g Pt/t(HNO3),比Pt-4Pd-3.5Rh合金催化网的铂耗(0.061g Pt/t(HNO3))低28%;在中压氨氧化法生产硝酸过程中,Pt-12Pd-3.5Rh合金催化网的铂耗为0.121g Pt/t(HNO3),比Pt-5Rh和Pt-10Rh合金催化网的铂耗(0.15~0.153 g Pt/t(HNO3))低21%,而其氨耗比后者降低3%~7%。研究结果证明,在Pt-Rh合金中添加钯或在Pt-Pd-Rh合金中增加钯含量明显降低催化合金的铂耗。     

铂钯铑分离提纯方法览要

1.引言铂钯铑合金材料有着极广泛的应用。这些材料在使用过程中,由于受到高温或其他恶劣环境的影响而被腐蚀和污染,从而失却原有卓越的物化特性和催化特性。从废料中回收铂钯铑及其合金,在贵金属生产中占据重大的比例。不过,某些材料可以用简单的方法再生,某些材料则必须经历十分复杂的分离提纯工艺之后才能重新使用。本文根据不同的分离提纯方法,综述其工艺原理及应用状况,希望有益于同行。     

ICP-AES测定等离子熔炼合金中的铂、钯和铑

建立了一种以碱熔-碲共沉淀分离、电感耦合等离子体发射光谱(ICP-AES)测定等离子熔炼合金样品中铂、钯和铑含量的方法。研究了样品处理和测定条件。结果表明,样品与过氧化钠混匀,在730℃马弗炉中保温25 min后,熔融物可用稀盐酸完全浸出;在盐酸介质中,加入碲溶液和二氯化锡溶液微沸30 min,所得铂、钯和铑共沉淀充分;在选定条件下,对铂、钯和铑含量为0.5~7.0、2.0~40.2和0.2~7.0 g/kg的样品,测定相对标准偏差(RSD)分别为0.44%~1.52%、0.58%~1.06%和0.61%~1.98%,加标回收率分别为99.4%~101%、99.1%~100.5%和98.3%~101%。     

从铂钯精矿中回收铂、钯和金

采用焙烧-预浸出-氯化浸出-萃取-精制工艺处理铜冶炼阳极泥产出铂钯精矿回收铂、钯、金。结果表明,氯化液采用亚硫酸钠控制电位还原,金回收率99%;金还原后液采用二异戊基硫醚萃取钯,氨水反萃,钯回收率90%;萃钯余液采用三烷基胺萃取铂,氢氧化钠反萃,铂回收率90%。铂、钯符合国标99.99%产品要求,粗金粉品位97.09%。     

硝酸工厂回收铂的原理和方法

综述硝酸生产过程中铂合金催化网的损耗以及回收铂的原理与方法，讨论了高钯合金捕集网回收铂的原理、效率和效益等问题。     

湿-火联合法从汽车尾气失效催化剂中提取铂族金属新工艺研究

针对活性组分溶解法从汽车尾气失效催化剂中提取铂、钯、铑,其浸出残渣存在贵金属含量高、回收率低的问题进行研究,提出了湿-火联合法从汽车尾气失效催化剂中提取铂、钯、铑的新技术方案,采用该工艺可使铂、钯、铑的回收率较活性组分溶解法分别提高了23.53%、2.80%和18.81%。     

合金成分对铂合金耐热性的影响

众所周知,在热循环次数一定的情况下,铂合金的耐热性取决于它的成分。因此,在研制新型多组元铂合金时,必须确定它在经常性热循环作用下的工作性能。本文研究了铑含量(5～20%)和钯含量(5～25%)对二元铂合金和三元铂合金     

氨氧化用铂合金催化网技术进展

随着我国化工、材料行业的不断发展,使得对氨氧化用铂合金贵金属催化网技术的要求也越来越高。介绍了铂合金催化网应用状况、铂合金技术发展状况、各种技术的优缺点及铂合金催化网未来发展方向。     

两种钯合金网在硝酸催化网中捕集铂的比较

钯合金可在氨氧化反应中捕集铂,对某硝酸厂使用PdNi合金网和双功效铂催化剂(DEC)功能网捕集铂的效果进行了对比,并对捕集机理进行了分析。结果表明,DEC功能网比PdNi合金网的铂耗低26%,保持机组稳定运行、做好氨空气净化、及时更换催化剂等措施有利于降低铂耗。     

铂合金催化网焊接参数分析

在铂合金催化网的制造中，一般采用下料拼焊的方法满足幅宽与网径的要求。催化网在应用中，要经受高温、氧化、压力、冲击、摩擦磨损的作用，本文据此对催化网的焊接过程参数进行一般分析。     

稀土强化Pt-Pd-Rh合金针织催化网在硝酸生产常压炉中的应用研究

在H厂生产硝酸的2套机组4台氨氧化常压炉中用Pt-Rh或Pt-Pd-Rh针织催化网作实验,并将稀土强化Pt-Pd-Rh针织催化网与该2种催化网进行了应用比较.用化学分析、光谱定量、光电子能谱、扫描电镜等方法分析了样品的组成及状态.结果表明,优化配套的稀土强化Pt-Pd-Rh针织催化网转化效率高、吨酸铂耗低、使用寿命长,合金中Pt高温氧化轻微,Rh的表面氧化及富集减弱,催化效果明显.提出了氨氧化常压炉用铂合金针织催化网的配套措施.     

硝酸工业用铂合金催化网的发展

铂合金催化网是氨氧化法制备硝酸不可缺少的催化剂。生产中要求铂网氨转化率高、铂耗低、耐腐蚀性强、高温强度高、抗粘结和抗毒性强。围绕如何提高催化网的使用性能,评述了铂合金催化网材料制造从一元金属到多元合金的发展,以及织网方法从编织到针织的发展。     

从失效Pt-V/C催化剂中回收铂的新工艺

由于化学性质相似,铂钒分离提纯比较困难。对失效Pt-V/C催化剂中铂的回收进行了研究,重点考察了盐酸浓度、温度和氯化铵的用量3种工艺参数对铂钒分离的影响,得出优化的工艺条件:在室温下,盐酸浓度为3.0 mol/L,氯化铵与铂的质量比为4~5,可以实现铂的有效沉淀分离。经精炼可以获得纯度为99.95%的海绵铂,铂的回收率大于99.5%。     

从废氧化铝载体催化剂中回收铂的研究现状

废氧化铝载体铂催化剂具有极高的价值，从废催化剂中回收铂意义重大。综述了从废氧化铝载体铂催化剂中回收铂的技术现状，并对主要回收工艺存在的优缺点进行了评述。湿法工艺存在难以处理复杂物料和综合利用废液等问题，火法工艺存在对设备要求高和造渣方法局限等问题，尚未大规模工业应用。未来废催化剂数量庞大且成分愈发复杂，开发更加高效清洁的回收工艺是未来的主要发展趋势。     

Electrocatalytic oxidation of glucose on gold–platinum nanocomposite electrodes and platinum-modified gold electrodes

Electrochemical oxidation of glucose on gold–platinum nanocomposite electrodes and platinum-modified gold electrodes was investigated with cyclic voltammetry. Gold–platinum nanoparticles were prepared by reducing aqueous solutions containing chlorauric acid and chloroplatinic acid, and the electrodes were obtained by depositing the gold–platinum nanoparticles from the colloidal solutions onto substrates. The gold–platinum nanocomposite electrodes display high electrocatalytic activity for the glucose oxidation in alkaline solution, showing 0.30–0.35 V negative shift in peak potential as compared with bare gold electrodes, and maintain stable catalytic activity in the reaction. The results of experiments indicate that both gold and platinum act as the dehydrogenation site and gold also functions to regenerate platinum from poisoned platinum. Surface modification of gold electrodes by platinum deposition also increases electrocatalytic activity of the electrodes for the glucose oxidation, showing about 0.10 V negative shift in peak potential, but a gradual decline in reactivity is observed.     

PtCoCr catalysts for fuel cell cathodes: Electrochemical activity, Pt content, substrate nature, structure and corrosion properties

Creation of multicomponent catalytic systems is the main way to decrease the content of or completely replace Pt in fuel cell cathodes. Compared to the conventional catalytic systems, production of PtCoCr catalysts on different substrates (XC-72 carbon nanotubes, TiO₂) differs in high-temperature conditions and the use of nitrogen-containing transient-metal precursors. According to electrochemical and structural studies, during synthesis and subsequent treatment, alloy nanoparticles with a core-shell structure enriched in platinum are formed on a carbon material doped with nitrogen. The ligand effect of the alloy core results in an increase in the electron density of the platinum d-level, acceleration of oxygen reduction, and deceleration of water molecule discharge and platinum corrosion. A architecture of membrane electrode assembly involving PtCoCr-based active layers of varying composition is developed for fuel cells operating at a temperature of 65°C in hydrogen-air and hydrogen-oxygen environments. In both cases, the use of PtCoCr instead of monoplatinum catalysts enabled us to halve the platinum consumption at the same discharge current density and specific power. The results of life testing and potential cycling of membrane electrode assemblies under severe conditions showed that the resistance of PtCoCr systems is not inferior to platinum.     

Gold, an alternative to platinum group metals in automobile catalytic converters

Catalytic convertors based on the use of platinum, palladium and rhodium play a major role in the cleaning of automobile emissions. Gold, when dispersed as nano-sized particles, has demonstrated significant activity in the conversion of toxic components, including carbon monoxide, unburnt hydrocarbons and nitrogen oxides, in engine emissions and some advantages over the platinum group metals. Some research outcomes on the application of nano-sized gold for the conversion of these components are reviewed. Several key issues in relation to its performance and applicability in catalytic convertors such as low-temperature activity and thermal stability and the possibilities of substituting platinum group metals for automobile emission control with gold are discussed.