摘要 |
PURPOSE:To deposit the titled ammonium salt, by thermally decomposing 1,1'- peroxydicyclohexylamine at a high temperature, quenching the resultant product, acidifying the quenched product, extracting the acidified product with water, separating the obtained extract into an aqueous layer and oily layer, adding aqueous ammonia to the oily layer, extracting and removing impurities. CONSTITUTION:1,1-Peroxydicyclohexylamine 1 is thermally decomposed in a thermal decomposition column 3, quenched with cooling water 23 and adjusted to pH <=4 in a pH adjusting vessel 9. The acidified product is then led to a water extraction column 4 and separated into an aqueous layer 12 containing epsilon-caprolactam and an oily layer 15 containing 11-cyanoundecanoic acid. The aqueous layer 12 is partially used as the cooling water 23. The oily layer 15 is mixed with a solution containing ammonia and water and led to an organic solvent extraction column 5 to convert the 11-cyanoundecanoic acid and isomers thereof into ammonium salts, which are then migrated into an aqueous layer 17. Cyclohexanone and other impurities are removed with an extracting organic solvent 13 and the aqueous layer 17 is successively led to crystallization vessels 6 and 8 to afford the aimed high-purity ammonium 11-cyanoundacanoate.
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