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研究从头孢曲松生产母液中回收2-巯基苯并噻唑(以下简称M),提出了蒸发结晶-加碱联合处理回收M的新工艺。采用失重法首次研究了M在不同溶剂体系中的溶解度,采用HPLC法测定母液蒸发浓缩结晶和加碱处理回收得到的M的质量分数。结果表明,M在丙酮中溶解度为15 g(常温),在乙醇中溶解度为2.5 g(常温),水的存在会使M在溶媒中的溶解度大幅降低,1.3 g[m(乙醇)∶m(水)=0.4∶0.6,75℃];母液蒸发浓缩至85%时,M的收率可达98.6%,蒸发结晶和加碱处理回收得到的M的质量分数分别为98.2%和98.7%。该工艺不需要大量水的加入,降低了溶剂回收系统的能耗,酸碱用量少,无二次污染,不堵塞管道,已成功用于工业化生产。
In this paper, 2-mercaptobenzothiazole (hereinafter referred to as M) was recovered from the mother liquor of ceftriaxone production, and a new process for the recovery of M by evaporation and crystallization combined with alkali was proposed. The solubility of M in different solvent systems was studied by weight loss method for the first time. The mass fraction of M recovered by evaporation and concentration of mother liquor and alkali treatment was determined by HPLC. The results showed that the solubility of M in acetone was 15 g (normal temperature) and the solubility in ethanol was 2.5 g (normal temperature). The presence of water greatly reduced the solubility of M in the medium. The solubility of 1.3 g [m Water) = 0.4: 0.6, 75 ° C]. When the mother liquor was concentrated by evaporation to 85%, the yield of M reached 98.6%. The mass fraction of M recovered by evaporation crystallization and alkali treatment were 98.2% and 98.7%, respectively. The process does not require the addition of a large amount of water, which reduces the energy consumption of the solvent recovery system, requires less acid and alkali, has no secondary pollution and does not block the pipeline and has been successfully used in industrialized production.