头孢他啶双股进料结晶工艺的研究

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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184 μm，径距为1.290，收率可以达到80%。

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	王竟
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	杨梦德
	刘宝树

关键词：头孢他啶反应结晶双股进料收率晶习粒度分布

Abstract： 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 184 μm and diameter distance of 1.290, and the yield can reach 80%.

Keywords： ceftazidime reactive crystallization dual feed yield crystal habits crystal size distribution

Received 2022-10-25;

Fund:河北省自然科学基金（B2020208095）。

Corresponding Authors: 刘宝树,教授,E-mail:lbs99@163.com;杨梦德,工程师,E-mail:yangmd2005@163.com。 Email: lbs99@163.com;yangmd2005@163.com

About author: 王竟(1998-),男,硕士研究生,现从事药物结晶研究。

引用本文:

王竟, 孙华, 杨梦德, 刘宝树.头孢他啶双股进料结晶工艺的研究[J]. 化学工业与工程, 2023,40(1): 90-95

WANG Jing, SUN Hua, YANG Mengde, LIU Baoshu.The dual feed crystallization process of ceftazidime[J]. Chemcial Industry and Engineering, 2023,40(1): 90-95

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