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METHOD OF RECOVERING COPPER-VANADIUM CATALYST FROM MOTHER LIQUORS IN ADIPIC ACID PRODUCTION

机译:从己酸生产中的母液中回收铜钒催化剂的方法

摘要

FIELD: industrial organic synthesis. SUBSTANCE: invention relates to synthesis of adipic acid via oxidation of cyclohexanol and/or cellohexanone with nitric acid in presence of copper-vanadium catalyst. The latter is commonly recovered by concentrating mother liquors using evaporation until residue containing dicarboxylic acids $$$, copper and vanadium salts, non-reacted nitric acid and water is obtained followed by isolating catalyst and returning it into the oxidation step, whereupon dicarboxylic acids $$$ are isolated at lowered temperature. Invention consists in that mother liquor evaporated to 65-75 vt % concentration of dicarboxylic acids $$$ is mixed with mother liquor from dicarboxylic acids $$$ crystallization step observing weight ratio 1 to 1-1.5, respectively. Resulting suspension is crystallized at temperature below -10 C, preferably from -10 to - 15 C, wet crystals of dicarboxylic acids $$$ are separated, and mother liquor obtained is divided into two streams, one of which is used to dilute the deposit and the other is returned into oxidation step. EFFECT: simplified and enhanced catalyst recovery; utilized mixture of dicarboxylic acids $$$ 1 dwg, 1 tbl
机译:领域:工业有机合成。发明领域本发明涉及在铜-钒催化剂存在下通过用硝酸氧化环己醇和/或纤维己酮来合成己二酸。后者通常通过蒸发浓缩母液进行回收,直到获得含有二羧酸$$,铜和钒盐,未反应的硝酸和水的残留物,然后分离催化剂并将其返回到氧化步骤,于是二羧酸在较低的温度下隔离$$。发明在于将蒸发至浓度为65-75vt%的二元羧酸的母液与来自二元羧酸的结晶步骤的母液混合,分别观察重量比为1至1-1.5。将得到的悬浮液在低于-10℃,优选-10至-15℃的温度下结晶,分离出二元羧酸的湿晶体$$,并将获得的母液分成两股物流,其中一股用于稀释沉积物。另一个返回氧化步骤。效果:简化并提高了催化剂的回收率;使用的二元羧酸混合物$$$ 1 dwg,1 tbl

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