Nitric Acid → HCID 178443865, compound

HRID 1951963Notes

Reaction equation

HRID 1951963 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.[N+]([O-])(O)=O>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 944Nitric Acid3×HCID 7962MethylcyclohexaneHCID 9275Bis(2-ethylhexyl) phosphateHCID 23934Neodymium2×HCID 159373Neodymium sesquioxide

Product 1

HCID 178443865HCID 178443865, compoundYield 95%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

3.03 g of neodymium oxide containing 72.4% by weight of neodymium, 16.15 g of di(2-ethylhexyl)phosphoric acid (DEHPA), 80 g of methylcyclohexane (MCH) and 1.8 ml of nitric acid at 0.5 mol/l are introduced into a reactor made inert beforehand with argon. This amount of nitric acid corresponds to 0.06 molar equivalent of HNO3 relative to the neodymium. The mixture is stirred and brought to 80° C. until the presence of solid can no longer be distinguished visually, i.e., in this case, 3 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. 20 g, 19.5 g and then 19.5 g are thus recovered. The water/MCH azeotrope is subsequently distilled with a Dean Stark apparatus. A solution of neodymium di(2-ethylhexyl)phosphate in MCH, with a clear appearance, is thus obtained. It is characterized by a content of neodymium in solution of 2.05%, a residual free acidity expressed as percentage by weight of DEHPA of 1.59%, and a water content of 209 ppm. In this case, the molar ratios are the following: DEHPA/Nd=0.34 and water/Nd=0.08. The attack yield is 95%.

Workup

  1. custombrought to 80° C. until the presence of solid
  2. customin this case, 3 h
  3. temperatureThe mixture is cooled
  4. customto remove the inorganic residues
  5. stirringof stirring for 30 minutes
  6. customa step of separating
  7. custom20 g, 19.5 g and then 19.5 g are thus recovered
  8. distillationThe water/MCH azeotrope is subsequently distilled with a Dean Stark apparatus

Sources & evidence

ORD record
ord-ba6902fb71954f5db753ac5f0aeae7b7
Source dataset
uspto-grants-2013_03
Patent number
US08404821B2

Reaction notes

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