Hydrochloric Acid → HCID 178443865, compound

HRID 1951960Notes

Reaction equation

HRID 1951960 reaction equation
[O-2].[Nd+3:2].[O-2].[O-2].[Nd+3].[Nd].[CH2:7]([CH:9]([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:10][O:11][P:12](=[O:23])([OH:22])[O:13][CH2:14][CH:15]([CH2:20][CH3:21])[CH2:16][CH2:17][CH2:18][CH3:19])[CH3:8].CC1CCCCC1.Cl>O>[CH2:7]([CH:9]([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:10][O:11][P:12]([O-:23])([O:13][CH2:14][CH:15]([CH2:20][CH3:21])[CH2:16][CH2:17][CH2:18][CH3:19])=[O:22])[CH3:8].[Nd+:2]

Participants

7

Reactant 5

HCID 313Hydrochloric Acid3×HCID 7962MethylcyclohexaneHCID 9275Bis(2-ethylhexyl) phosphateHCID 23934Neodymium2×HCID 159373Neodymium sesquioxide

Product 1

HCID 178443865HCID 178443865, compoundYield 100%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

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

  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

Sources & evidence

ORD record
ord-22cb2c0c68154ae7a00a1260b0094ac1
Source dataset
uspto-grants-2013_03
Patent number
US08404821B2

Reaction notes

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