反应详情

To a crosslinked copolymer of chloromethylstyrene-divinylbenzene (weight ratio of chloromethylstyrene to divinylbenzene: 80/20) was added ethyl iminodiacetate in an amount two times the molar amount of chloromethyl groups of the crosslinked copolymer of chloromethylstyrene-divinylbenzene, and reaction was allowed to proceed at 120° C. for 24 hours. The obtained solid product was filtered off using a glass filter and washed with acetone. Thus, there was obtained a granular iminodiacetic acid type chelating resin having a particle diameter of 74 to 147μ [100 to 200 mesh (Tyler)] (hereinafter referred to as "Adsorbent A"). The degree of coversion was 70%. The obtained chelating resin was packed in a glass-made column equipped with a stopcock for an outlet at the bottom thereof and a jacket and having an inside diameter of 10 mm and a length of 1000 mm. Then the temperature of the whole column was maintained at 50° C., and to the column at its top was supplied an aqueous ammonia having a pH value of 9.0, with the outlet opened by switching the stopcock. The supply of the aqueous ammonia was continued until the pH value of the solution flowing out of the outlet of the column reached 9.0. Thus, the chelating resin was equilibrated with the solution. Then 150 ml of an aqueous solution containing 15 mM each of lanthanum (III) chloride and neodymium (III) chloride and adjusted, by an aqueous hydrogen chloride solution, to have a pH value of 4.0 was supplied to the top of the column at a rate of 3.5 ml/min. Subsequently, a 0.1M aqueous hydrogen chloride solution was fed to the top of the column at a rate of 3.5 ml/min. It took 2 hours for the rear portion of the adsorption band to flow out of the column. During the supply of the 0.1M aqueous hydrogen chloride solution, the rear boundary of the adsorption band which was visible due to the purple neodymium ions present in the rear portion of the band was kept clear. The eluate from the bottom of the column was collected in 5-ml fractions. The concentration of the rare earth elements in each fraction was determined using X-ray fluorescent spectrometer VXQ-150 (an apparatus manufactured and sold by Shimadzu Corporation, Japan).

1. filtrationThe obtained solid product was filtered off
2. filtrationfilter
3. washwashed with acetone