HRID1951960

反应详情

EQUATION

反应方程式

HRID 1951960 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture is cooled
  2. customto remove the residues of hydrochloric acid
  3. stirringof stirring for 30 minutes
  4. customa step of separating
  5. waitby settling out, also for 30 minutes
  6. customexcept for the final separating
  7. waitwhich lasts 12 h
  8. distillationThe water/MCH azeotrope is subsequently distilled with a Dean Stark apparatus