摘要
研究了以二氯二氨合钯为原料,用盐酸溶液加热溶解使其转化成氯钯酸铵,以氯酸钠作为氧化剂氧化除去铵,氢氧化钠沉淀钯得到纯氢氧化钯,再用浓盐酸溶解之并浓缩结晶得到纯氯化钯的制备工艺。研究结果表明:当每公斤Pd(NH3)2Cl2的氯酸钠用量为2.48kg,HCl(36%)用量为2.75L,钯的浓度为20g/L,氧化时间60min,氧化温度100℃,沉钯pH=10,沉降时钯的浓度为10g/L,洗涤3次,其氢氧化钯的纯度>99.9%(钯的含量75.64%)。制备的氯化钯中钯含量>59.5%,其中铁含量<0.002%,硝酸根含量<0.02%,氯化钯中的杂质总量<0.05%。直收率>99.9%。另外采用此工艺不产生NO等的污染。
A technique of preparing PdCl2 was from Pd(NH3)2Cl2 by oxidation method was studied. The Pd(NH3)2Cl2 was used as raw material, and was it dissolved in HCl solution. The solution was heated and transformed into(NH4)2PdCl2. Ammonium was removed by oxidation.(NH4)2PdCl2 was transformed into Pd(OH)2 by depositing using NaOH. Pd(OH)2 was filtrated and washed,and then dissolved in HCl solution and was concentrated and crystallized. The research results showed that when dosage of sodium chlorate was 2.48kg, HCl(36%) was 2.75L per kilogram Pd(NH3)2Cl2, concentration of Pd was 20g/L,time of oxidization was 60 minutes, temperature of oxidization was 100℃, pH in depositing Pd was 10, concentration of Pd in depositing Pd was 10g/L, Pd(OH)2 was washed 3 times. The purity of Pd(OH)2 produced by using the technique was over 99.9%,Pd in PdCl2 was over 59.5%, Fe was below 0.002%, NO3- was below 0.02%, total impurity in PdCl2 was below 0.05%. Direct recovery was over 99.9% .
出处
《贵金属》
CAS
CSCD
2005年第3期1-7,共7页
Precious Metals
