反应详情

50 g (0.15 mol) of untreated lanthanum oxide (Fluka) were converted to the nitrates by adding 68.39 ml of concentrated nitric acid and 1.5 1 of demineralized water. During this, the solution was stirred and gently heated in order to speed up the dissolution process. After cooling the solution to room temperature, 84.27 g (0.67 mol, 1.5 equiv.) of oxalic acid, dissolved in 500 ml of demineralized water, were added with stirring and lanthanum oxalate was precipitated out. Decantation and filtration through a Buchner funnel were then carried out. The resulting white solid was dried overnight in a drying cabinet at 110° C. 78.43 g (0.145 mol, 94.3% of theory) of lanthanum oxalate were obtained. 2 g of the lanthanum oxalate were then calcined in air in a tubular furnace at 650° C. for 18 hours. After cooling to 50° C. in the stream of nitrogen, the prepared, white lanthanum oxide was transferred to a Schlenk tube filled with argon. A further 6 g of lanthanum oxalate were calcined to lanthanum oxide for 18 hours in the muffle furnace at 700° C., cooled in the desiccator and likewise stored in a Schlenk tube under argon.

1. temperaturegently heated in order
2. additionwere added
3. stirringwith stirring
4. customlanthanum oxalate was precipitated out
5. filtrationDecantation and filtration through a Buchner funnel
6. customThe resulting white solid was dried overnight in a drying cabinet at 110° C