亚硝酸甲酯羰基化合成草酸二甲酯废旧催化剂Pd/α-Al2O3中Pd的提取
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摘要
采用HCl+H_2O_2混合溶液浸泡废旧催化剂Pd/α-Al_2O_3,滤掉氧化铝球颗粒,加入氨水沉淀滤液中Pd之外的微量杂质并过滤,在滤液中加入丁基钠黄药,形成Pd化合物沉淀,过滤,100℃烘干,350℃焙烧,生成PdO,纯度99. 541%,再用H_2或CO在≥700℃下还原,得到纯Pd。该方法成本低,相对于王水法更环保、高效,Pd回收率> 99. 99%。
Waste catalyst Pd/α-Al_2O_3 was dipped into the mixture solution of HCl and H_2O_2,and then filtered to remove Al_2O_3 particles. NH_4OH was added to the filtrate to precipitate impurity except for Pd and filtered secondly. C_4H_9OOSSNa was added to the filtrate to precipitate Pd and filtered thirdly. The wet filter cake obtained was oven-dried at 100 ℃,and then calcined in air at 350 ℃ to get PdO with purity of 99. 541%. PdO was reduced by H_2 or CO at temperature above 700 ℃. This method with Pd recovery higher than 99. 99% shows lower cost,better for environmental protection and higher efficient comparing with aqua rejia method.
Waste catalyst Pd/α-Al_2O_3 was dipped into the mixture solution of HCl and H_2O_2,and then filtered to remove Al_2O_3 particles. NH_4OH was added to the filtrate to precipitate impurity except for Pd and filtered secondly. C_4H_9OOSSNa was added to the filtrate to precipitate Pd and filtered thirdly. The wet filter cake obtained was oven-dried at 100 ℃,and then calcined in air at 350 ℃ to get PdO with purity of 99. 541%. PdO was reduced by H_2 or CO at temperature above 700 ℃. This method with Pd recovery higher than 99. 99% shows lower cost,better for environmental protection and higher efficient comparing with aqua rejia method.
引文
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[4]梁茂辉,曹沛,战福清.从氧化铝载体的废钯催化剂中回收钯的工艺研究及生产技术新突破[J].中国物质再生,1997,(7):13-16.
[5]刘春奇,杨惠林,李大树.从废把催化剂中回收钯——渗滤浸出法处理低品位废把催化剂[J].有色矿冶,1996,(4):34-37.
[6]李耀星,萨支琳.对从氧化铝为载体的含钯废催化剂中所得粗钯精制工艺的改进[J].中国物资再生,1998,(1):12-13.
[2]李牟,辛爱铀.含钯废催化剂回收概况[J].化工环保,1989,9(5):276-279.
[3]孙锦宜.废钯催化剂的回收技术[J].金陵石油化工,1995,(2):41-43.
[4]梁茂辉,曹沛,战福清.从氧化铝载体的废钯催化剂中回收钯的工艺研究及生产技术新突破[J].中国物质再生,1997,(7):13-16.
[5]刘春奇,杨惠林,李大树.从废把催化剂中回收钯——渗滤浸出法处理低品位废把催化剂[J].有色矿冶,1996,(4):34-37.
[6]李耀星,萨支琳.对从氧化铝为载体的含钯废催化剂中所得粗钯精制工艺的改进[J].中国物资再生,1998,(1):12-13.