反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3.03 g of neodymium oxide containing 72.4% by weight of neodymium, 17.39 g of di(2-ethylhexyl)phosphoric acid (DEHPA), 80 g of methylcyclohexane (MCH) and 0.9 ml of hydrochloric acid at 1 mol/l are introduced into a reactor made inert beforehand with argon. This amount of hydrochloric acid corresponds to 0.06 molar equivalent of HCl relative to the neodymium. The mixture is stirred and brought to 80° C. for 3 h. The mixture is cooled. Three washes with 20 g of water are successively carried out in order to remove the residues of hydrochloric acid. Each wash comprises a step of stirring for 30 minutes and then a step of separating by settling out, also for 30 minutes, except for the final separating by settling out, which lasts 12 h. The water/MCH azeotrope is subsequently distilled with a Dean Stark apparatus. A clear solution of neodymium di(2-ethylhexyl)phosphate in MCH is thus obtained.
WORKUP
后处理
- temperatureThe mixture is cooled
- customto remove the residues of hydrochloric acid
- stirringof stirring for 30 minutes
- customa step of separating
- waitby settling out, also for 30 minutes
- customexcept for the final separating
- waitwhich lasts 12 h
- distillationThe water/MCH azeotrope is subsequently distilled with a Dean Stark apparatus