诺氟沙星生产中溴的循环使用研究

Recycle of Bromine in Production of Norfloxacin

通过气相色谱仪和气相色谱-质谱联用仪确定了某制药厂用回收的溴化钠生产的溴乙烷中所含杂质的具体成分及其含量。并分析讨论了溴乙烷中各杂质来源。通过测定溴化钠、碳酸钠在不同温度、不同浓度的乙醇溶液中的溶解度,确定了回收溴化钠的最佳工艺条件。实验结果证明:用60%的乙醇溶液分两次在50℃时溶解溴渣,NaBr的回收率达到98.0%,二次溶解则能达到99.0%。用该法回收的溴化钠用于制备溴乙烷,当NaBr∶H2O∶C2H5OH∶H2SO4=1∶5.00∶1.30∶2.13时,纯度高达98.0%,回收率为79.6%,满足工业化生产的要求。

The content and ingredient as well as origins of impurity in bromoethane made from dregs of bromine at a pharmaceutical manufacturer was analysed through GC and GC-MS. The best technical condition of reclaiming sodium bromide was determined by measuring solubility of sodium bromide and sodium carbonate in ethanol of various temperature and concentration. Experiment results showed that dregs of bromine was dissolved by 60% ethanol at 50℃ twice, with first recovery rate of sodium bromide up to 98.0% and that of second 99.0%. The reclaimed sodium bromide was used to prepare bromoethane, with purity up to 98.0% and efficiency of reclaiming 79.6% when the proportion of sodium bromide, water, ethanol and vitriol was 1:5.00:1.30:2.13, which can satisfy the industrialized production.