摘要
针对头孢他啶结晶产品聚结、晶习差、粒度分布不均匀等问题,设计了双股进料结晶工艺,并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、温度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)0.33 g·g^(-1),料液流加速率0.14 mL·min^(-1),温度27℃,养晶时间60 min,搅拌速率为250 r·min^(-1)可以得到均匀的片状头孢他啶晶体,晶习完整,中值粒径达到184μm,径距为1.290,收率可以达到80%。
To solve the problems of ceftazidime crystalline product coalescence,crystal habit difference,and uneven particle size distribution,the dual feed crystallization was used to control the crystallization environment within the metastable zone,successfully avoiding the spontaneous nucleation,and the operation was simple and easy to control.The influences of initial concentration,feeding speed,stirring rate,temperature and crystal growing time on the yield,crystal habits and crystal size distribution of products were studied using single factor experimental method.The optimum operation conditions were as follow:at 0.33 g·g^(-1) initial concentration,0.14 mL·min^(-1) feeding speed,27℃,60 min crystal growing time,stirring rate of 250 r·min^(-1),the flake crystal products with whole crystal habits and homogeneous size distribution were obtained,a median particle size of 184μm and diameter distance of 1.290,and the yield can reach 80%.
作者
王竟
孙华
杨梦德
刘宝树
WANG Jing;SUN Hua;YANG Mengde;LIU Baoshu(College of Chemical and Pharmaceutical Engineering,Hebei University of Science and Technology,Shijiazhuang 050018,China;NCPC Hebei Huamin Pharmaceutical Co.,Ltd.,Shijiazhuang 052160,China)
出处
《化学工业与工程》
CAS
CSCD
北大核心
2023年第1期90-95,共6页
Chemical Industry and Engineering
基金
河北省自然科学基金(B2020208095)。
关键词
头孢他啶
反应结晶
双股进料
收率
晶习
粒度分布
ceftazidime
reactive crystallization
dual feed
yield
crystal habits
crystal size distribution
