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针对头孢拉定反应结晶工艺,设计了双股进料结晶体系,将结晶环境控制在介稳区,有效避免自发成核,操作简单,容易控制。采用单因素法研究了结晶液初始浓度,料液流加速率,搅拌速率,结晶pH范围,晶种添加量以及养晶时间对结晶产品收率,晶习及粒度分布的影响,确定了优化的工艺参数:结晶液初始浓度(溶质质量/溶剂质量)0.43 g/g,料液流加速率2 mL/min,pH 2.5~2.7,晶种添加量按公式计算,养晶时间60 min,搅拌速率为140 r/min可以得到均匀的棒状晶体,搅拌速率为70 r/min可以得到均匀的簇状聚结体,晶习完整,粒度分布均匀,收率可以达到92%。
According to the cephradine reaction crystallization process, a double-strand feed crystallization system is designed to control the crystallization environment in the metastable zone and avoid spontaneous nucleation effectively. The operation is simple and easy to control. The influence of the initial concentration of crystallization liquid, the rate of feed liquid flow, the stirring rate, the pH range of crystal, the amount of seed crystal and the time of crystal-keeping on the yield, crystallization and particle size distribution of crystalline product were studied by single factor method. Process parameters: the initial concentration of the crystallization solution (solute mass / solvent mass) 0.43 g / g, feed liquid flow rate 2 mL / min, pH 2.5 ~ 2.7, the amount of seed crystals added according to the formula, holding time 60 min, A uniform rod-like crystal was obtained at 140 r / min. The uniform cluster-like aggregates were obtained at a stirring rate of 70 r / min. The crystal habit was complete and the particle size distribution was uniform. The yield could reach 92%.