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METHOD FOR PREPARING CHROMIUM(III) PYRIDINE-2-CARBOXYLATE USING 2-OP RECTIFICATION RESIDUES

机译:用2-OP整流残基制备吡啶-2-羧酸铬(III)的方法

摘要

A method for preparing chromium(III) pyridine-2-carboxylate using 2-OP rectification residues, including: subjecting the 2-OP rectification residues to in-situ catalytic pyrolysis and vacuum distillation, room-temperature crystallization and separation, recrystallization and dehydration, alkali-catalyzed hydrolysis, acidification and complexation, and separation, washing and drying to prepare a chromium(III) pyridine-2-carboxylate product, of which a yield is greater than 50% of the weight of the 2-OP rectification residues. The acidification and complexation includes: cooling the aqueous solution containing sodium pyridine-2-carboxylate obtained from the alkali-catalyzed hydrolysis to a temperature below 50° C.; adjusting the aqueous solution to pH 3.0-8.5 with 5-50 wt % dilute H2SO4 or 3-30 wt % dilute HCl followed by batchwise addition of CrCl3, Cr(NO3)3 or Cr2(SO4)3 for complexation at 20-70° C. to obtain a slurry containing chromium(III) pyridine-2-carboxylate, which is separated, washed and dried to obtain a chromium(III) pyridine-2-carboxylate product with a purity of 98.5% or more.
机译:一种利用2-OP精馏残基制备吡啶-2-羧酸铬(III)的方法,包括:对2-OP精馏残基进行原位催化热解和真空蒸馏,室温结晶分离,重结晶脱水,碱催化水解,酸化和络合以及分离,洗涤和干燥,以制备吡啶-2-羧酸铬(III)产物,其收率大于2-OP精馏残渣重量的50%。所述酸化和络合包括:将由碱催化水解获得的含有吡啶-2-羧酸钠的水溶液冷却至低于50℃的温度;用5-50 wt%的稀H 2 SO 4 或3-30 wt%的稀HCl将水溶液调节至pH 3.0-8.5,然后分批添加CrCl 3 ,Cr(NO 3 3 或Cr 2 (SO 4 3 在20-70°C下络合以获得包含吡啶-2-羧酸铬(III)的浆料,将其分离,洗涤并干燥以获得吡啶-2-羧酸铬(III)产物纯度达到98.5%或更高。

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