Methylcyclohexane → HCID 178443865, compound

Participants

Reaction Steps

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 0.054 g acetic acid at 99.8% are introduced into a reactor made inert beforehand with argon. This amount of acetic acid corresponds to 0.06 molar equivalent of CH3COOH 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, 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 is for an overnight period. 16 g, 24.2 g and then 17.1 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 2.3%, a residual free acidity expressed as percentage by weight of DEHPA of 2.65%, and a water content of 77 ppm. In this case, the molar ratios are the following: DEHPA/Nd=0.51 and water/Nd=0.026. The attack yield is 100%.

Provenance & Evidence