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废催化剂中贵金属钌的回收
Recovery of Ruthenium from Waste Catalysts
【摘要】 采用碱熔—氧化蒸馏的方法从废催化剂中回收Ru。工艺路线为:Ru→可溶性钌酸盐→RuO4→RuC l3盐酸溶液→β-RuC l3.xH2O晶体。KNO3/KOH作碱熔剂,程序升温至6 5 0℃,并恒温3 h,然后沸水浸渍;NaC lO+H2SO4作氧化剂,以盐酸—乙醇溶液(1∶1)作吸收液,75℃左右减压蒸馏,系统压力0.06~0.08 MPa,吸收并还原RuO4气体,得到RuC l3盐酸溶液。β-RuC l3.xH2O晶体可由RuC l3盐酸溶液常压/减压蒸馏至干涸得到。无负载催化剂钌回收率可达到93%,负载钌催化剂回收率可达到90%。采用分层碱熔法比混合碱熔法钌回收率可高出10个百分点,HC l+MnO2作氧化剂得到的回收率比NaC lO+H2SO4高出6个百分点。
【Abstract】 A method of alkali fusion-oxidated distillaion is used in reclaiming ruthenium from the waste catalysts.The process is briefly described as follows: decomposition of ruthenium→sodium ruthenium→RuO4→the hydrochloric acid of ruthenium chloride→the crystal of β-RuCl3·xH2O.The mixture of KNO3/KOH is used as alkali-fusion agent,the reactants are calcinated in a temperature programming from room-temperature to 650 ℃ and kept for 3 h,the melts were leached by boiled water;the mixture of NaClO+H2SO4 is used as oxidant,then the ruthenium tetroxide could be obtained.The mixture of hydrochloric acid and ethanol is used as absorption solution in this oxidation distillation system which is carried out at 75 ℃ in a range of 0.06~0.08 MPa,ruthenium chloride could be obtained by reducing ruthenium tetroxide.The crystal of β-RuCl3·xH2O could be obtained by vacuum distillation or air distillation.The recovery of the supported and unsupported catalysts could be achieved 90% and 93%,respectively.The recovery of layered alkali fusion is much higher 10% than that of mixed alkali fusion,and the primary recovery of oxidation HCl+MnO2 can be much higher 6% than that of NaClO+H2SO4.
- 【文献出处】 河南化工 ,Henan Chemical Industry , 编辑部邮箱 ,2007年04期
- 【分类号】X78
- 【被引频次】11
- 【下载频次】845