تفاعل #2039143

ord-fe5b5a2ec70d47678dea4be2ff829a1a

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىbrought to 80° C. until complete disappearance of the solid, i.e., in this case, 1 h
  2. 2
    درجة الحرارةThe mixture is cooled
  3. 3
    أخرىto remove the inorganic residues
  4. 4
    workup.STIRRINGof stirring for 30 minutes
  5. 5
    أخرىa step of separating
  6. 6
    أخرىexcept for the final separating
  7. 7
    workup.WAITwhich lasts 12 h
  8. 8
    workup.DISTILLATIONThe water/MCH azeotrope is subsequently distilled with a Dean Stark apparatus

الإجراء التجريبي

2.88 g of neodymium oxide containing 72.4% by weight of neodymium, 0.53 g of an aqueous solution of neodymium nitrate containing 24.4% by weight of neodymium, 17.39 g of di(2-ethylhexyl)phosphoric acid (DEHPA), and 80 g of methylcyclohexane (MCH) are introduced into a reactor made inert beforehand with argon. The mixture is stirred and brought to 80° C. until complete disappearance of the solid, i.e., in this case, 1 h. The mixture is cooled. Three washes with 20 g of water are successively carried out in order to remove the inorganic residues. 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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08404821B2uspto-grants-2013_03