泰乐菌素结晶工艺研究

摘要

结晶过程是影响晶体质量的关键步骤.本实验采用溶析结晶工艺对泰乐菌素结晶过程进行研究,以收率、粒度和粒度分布为目标,考察了水和丙酮质量比、晶种加入量(质量分数)、结晶温度、初始浓度、搅拌转速、陈化时间和流加速率等操作因素对结晶过程的影响.结果表明:所有参数在考察的条件范围内都明显地影响产品的收率;除了温度和搅拌转速外,其他参数都对产品粒度有较明显的影响;对产品粒度分布影响较大的是品种加入量,温度和搅拌强度.通过分析各种因素影响得到泰乐菌素较佳结晶工艺条件:水和丙酮质量比4∶1,晶种加入量0.5％,结晶温度40℃,初始质量分数1.08 g/g,搅拌转速250 r/min,陈化时间12 h,流加速率先0.3 mL/min,后0.89 mL/min.%The crystallization process is a key step to affect the quality of crystals.The process conditions for dilution crystallization of tylosin were studied,while the effect of the mass ratio of water to acetone,content of crystal seeds (mass fraction),temperature,initial mass fraction,agitation speed,aging time and in-flux rate of diluents on the yield,particle size (MS) and size distribution (CV) of tylosin were explored experimentally in detail.The results show that the yield of tylosin is affected significantly by all kinds of operating parameters,MS of tylosin is influenced by the operating parameters except temperature and agitation speed,the parameters of content of crystal seeds,temperature and agitation speed impact on CV of tylosin.The optimum operation conditions was obtained:the mass ratio of water to acetone 4∶ 1,content of crystal seeds 0.5 ％,temperature 40 ℃,initial mass fraction 1.08 g/g,agitation speed 250 r/min,aging time 12 h and in-flux rate of diluents from 0.3 mL/min to 0.89 mL/min.