氯钌酸铵一步法制备钌粉研究

Research on One-Step Preparation Ruthenium Powder with Diammonium Hexachlororuthenate (Ⅳ)

利用热重质谱法(TG-MS)探究氯钌酸铵(NP)一步法制备钌(Ru)粉的分解机理,并采用单因素法研究煅烧时间、煅烧温度和物料量对NP分解率的影响,最后使用正交法优化工艺参数.结果表明,NP的热分解分两步进行,NP在300~363℃之间受热转化为含Ru中间产物并释放NH_(3)和HC_(1)气体;在363~420℃之间,NH3将Ru(Ⅳ)还原为单质Ru并产生N_(2)和HC_(l)气体.煅烧温度对NP的分解率影响最大.NP一步法制备Ru粉的最佳工艺参数为:煅烧温度为500℃,煅烧时间为80min,物料量为40g,分解率高达99.6%,NP基本分解完全.

Thermogravimetric mass spectrometry is used to analyse the decomposition mechanism of diammonium hexachlororuthenate(Ⅳ)(NP)one-step preparation of ruthenium(Ru)powder,and the effects of calcination time,calcination temperature and material amount on the decomposition rate of NP is studied by the single-factor method.Finally,the process parameters are optimized by the orthogonal method.The results show that the thermal decomposition reaction of NP proceeds in two steps.Between 300℃ and 363℃,NP is thermally converted into Ru containing intermediates with releasing NH_(3) and HCl gases;NH_(3) reduced Ru(Ⅳ)to elemental Ru and produced N_(2) and HCl gases from 363℃to 420℃.Calcination temperature has the greatest effect on the decomposition rate of NP.The optimal process parameters for preparing Ru powder by NP one-step method are as follows:calcination temperature 500℃,calcination time 80 min,and material amount 40 g,the decomposition rate is as high as 99.6%and the decomposition of NP is completed.