覆盆子酮油析结晶过程研究  

Investigation on the oiling out crystallization of raspberry ketone

作　　者：韦健 朱亮 沙作良 王彦飞 杨立斌 WEI Jian;ZHU Liang;SHA Zuoliang;WANG Yanfei;YANG Libin(College of Chemical Engineering and Materials Science of Tianjin University of Science and Technology,Tianjin 300450,China)

机构地区：[1]天津科技大学化工与材料学院,天津300450

出　　处：《化学工业与工程》2022年第1期66-74,共9页Chemical Industry and Engineering

基　　金：天津企业特派员基金项目(JCTPJC56300)。

摘　　要：实验结果显示覆盆子酮在正丙醇-水的混合溶剂中进行冷却结晶时会发生油析现象,而油析现象的发生会对最终结晶产品的质量造成一定的影响。为了抑制覆盆子酮结晶过程的油析现象,对这一现象进行了系统研究。首先应用FBRM对覆盆子酮在正丙醇-水混合溶剂中的油析热力学数据进行了实验测定,确定了油析曲线、澄清曲线、溶解度曲线与超溶解度曲线,测定了油析介稳区,并绘制了油析结晶介稳相图。结合覆盆子酮油析结晶介稳相图,系统考察了影响覆盆子酮油析行为的关键因素,以及有效的油析行为抑制方法。实验研究表明,溶液的初始浓度、降温速率和搅拌速率是覆盆子酮结晶过程油析现象形成的主要影响因素。同时考察了晶种添加量、晶种添加时机以及养晶时间等结晶工艺参数对覆盆子酮油析行为的影响,建立并优化了覆盆子酮结晶过程油析抑制工艺。Experimental results indicated that the oiling out phenomenon generally occurred during the cooling crystallization of raspberry ketone in the mixed solvent of n-propanol-water, and the occurrence of oiling out phenomenon will affect the quality of the final crystal product. In order to suppress the occurrence of oiling out phenomenon in the cooling crystallization process of raspberry ketone, a systematic investigation on this phenomenon had been carried out. Firstly, FBRM was used to determine the thermodynamic data of raspberry ketone in n-propanol-water mixed solvent. The oiling out curve, clarification curve, solubility curve and supersolubility curve were experimentally determined, and the oiling out metastable zone was established. Subsequently, the metastable phase diagram of oiling out crystallization was measured. Combined with the metastable phase diagram of oiling out crystallization of raspberry ketone, the key factors that have the influence on the oiling out behavior of raspberry ketone and the effective methods to inhibit the oiling out behavior were investigated. Experimental results have shown that the initial concentration of the solution, cooling rate and stirring rate are the crucial factors for the generation of oiling out during the cooling crystallization process of raspberry ketone. In addition, the effects of seed addition strategies on the inhibition of oiling out behavior of raspberry ketone were investigated, and the optimized crystallization process of raspberry ketone that can avoid the oiling out was established.

关 键 词：覆盆子酮结晶 油析热力学 油析抑制 冷却结晶 相平衡 

分 类 号：TS343.3[轻工技术与工程]