Neodymium(III) chloride

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of cobalt chloride having a gravity of 1.20 g/cm3 containing ammonium chloride was mixed while stirring with a solution of neodymium chloride and heated to 50° C. A stoichiometric equivalent quantity of sodium carbonate solution of 60° C. having a gravity of 1.05 g/cm3 was added to the mixed solution while stirring. The precipitates of cobalt carbonate and neodymium carbonate were obtained after reaction, filtrated in a vacuum filtrator to remove the mother liquid, washed by distilled water of 90° C. for 6 times, dried at 200° C., crushed and sieved by a 20 mesh sieve, reduced at 600° C. in hydrogen for 3 h, then crushed again and sieved by a 100 mesh sieve. The prepared cobalt powder contained 2.8% (wt.) neodymium. was mixed was added to the mixed solution The precipitates of cobalt carbonate

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of cobalt chloride having a gravity of 1.20 g/cm3 containing ammonium chloride was mixed while stirring with a solution of neodymium chloride and heated to 50° C. A stoichiometric equivalent quantity of sodium carbonate solution of 60° C. having a gravity of 1.05 g/cm3 was added to the mixed solution while stirring. The precipitates of cobalt carbonate and neodymium carbonate were obtained after reaction, filtrated in a vacuum filtrator to remove the mother liquid, washed by distilled water of 90° C. for 6 times, dried at 200° C., crushed and sieved by a 20 mesh sieve, reduced at 600° C. in hydrogen for 3 h, then crushed again and sieved by a 100 mesh sieve. The prepared cobalt powder contained 2.8% (wt.) neodymium. was mixed was added to the mixed solution The precipitates of cobalt carbonate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Adding 6 m3 of neodymium chloride solution (1.5 mol/L) into a reactor containing 27.5 m3 of the above magnesium bicarbonate solution to react for 3 hour at 35° C., and controlling the pH value of mother liquor at 8.0, neodymium ions are precipitated, and then neodymium carbonate is obtained after filtration, washing and drying. At last, neodymium oxide is obtained from calcination of neodymium carbonate at 650° C. for 2 hours. to react for 3 hour at 35° C. are precipitated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Adding 6 m3 of neodymium chloride solution (1.5 mol/L) into a reactor containing 27.5 m3 of the above magnesium bicarbonate solution to react for 3 hour at 35° C., and controlling the pH value of mother liquor at 8.0, neodymium ions are precipitated, and then neodymium carbonate is obtained after filtration, washing and drying. At last, neodymium oxide is obtained from calcination of neodymium carbonate at 650° C. for 2 hours. to react for 3 hour at 35° C. are precipitated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2.88 g of neodymium oxide containing 72.4% by weight of neodymium, 0.58 g of an aqueous solution of neodymium chloride containing 22.2% 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. for 5 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. The mixture is cooled to remove the inorganic residues of stirring for 30 minutes a step of separating by settling out, also for 30 minutes except for the final separating which lasts 12 h The water/MCH azeotrope is subsequently distilled with a Dean Stark apparatus

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Preparation of amine ligands was generally accomplished without exclusion of air and moisture, unless otherwise stated. All manipulations involving metal complexes were carried out under an inert atmosphere of oxygen-free UHP grade argon using standard Schlenk techniques, or under oxygen-free helium in a Vacuum Atmospheres glovebox. Chemicals were obtained from the following suppliers and used as received: Lancaster Synthesis—hexafluorobenzene, 3,5-bis(trifluoromethyl)aniline, pentafluoroaniline, 2,6-difluoroaniline, dichlorodiphenylsilane, dichlorodimethylsilane, paraformaldehyde, potassium hydroxide, 1-hexene, potassium carbonate; Aldrich—1.6 M n-butyllithium in hexane, triphenylsilane, chloroform; Strem—zirconium tetrachloride, neodymium trichloride, Fisher Scientific—methanol, ethanol, Albermarle—methylaluminoxane (30% solution in toluene); Fluka—lithium amide, 1,2-phenylene diamine, 1,8-diaminonaphthalene, 2,6-dimethylaniline, Acros—sodium sulfate, JT Baker—potassium hydroxide, NaH was obtained as a 60% dispersion in mineral oil, washed with hexane, filtered, and vacuum dried. Neodymium tris(bis(trimethylsilyl)amide) was prepared by reaction of anhydrous neodymium trichloride with three equivalents of potassium bis(trimethylsilyl)amide in refluxing THF for 24 hours, followed by low-temperature crystallization from hexane. Solvents (hexane, diethyl ether, tetrahydrofuran, toluene) were degassed and distilled from sodium benzophenone ketyl under argon. Dimethyl sulfoxide was distilled from calcium hydride under argon. Bis(triiethylsilyl)ether was distilled from potassium under argon. Benzene-d6, THF-d8, and toluene-d8 were degassed, dried over Na—K alloy, and then trap-to-trap distilled before use. washed with hexane filtered vacuum dried followed by low-temperature crystallization from hexane Solvents (hexane, diethyl ether, tetrahydrofuran, toluene) were degassed distilled from sodium benzophenone ketyl under argon Dimethyl sulfoxide was distilled from calcium hydride under argon Bis(triiethylsilyl)ether was distilled from potassium under argon Benzene-d6, THF-d8, and toluene-d8 were degassed dried over Na—K alloy trap-to-trap distilled before use

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of cobalt chloride having a gravity of 1.20 g/cm3 containing ammonium chloride was mixed while stirring with a solution of neodymium chloride and heated to 50° C. A stoichiometric equivalent quantity of sodium carbonate solution of 60° C. having a gravity of 1.05 g/cm3 was added to the mixed solution while stirring. The precipitates of cobalt carbonate and neodymium carbonate were obtained after reaction, filtrated in a vacuum filtrator to remove the mother liquid, washed by distilled water of 90° C. for 6 times, dried at 200° C., crushed and sieved by a 20 mesh sieve, reduced at 600° C. in hydrogen for 3 h, then crushed again and sieved by a 100 mesh sieve. The prepared cobalt powder contained 2.8% (wt.) neodymium. was mixed was added to the mixed solution The precipitates of cobalt carbonate