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FBRM and PVM investigations of the double feed semi-batch crystallization of 6-aminopenicillanic acid

Min SU, Lin WANG, Hua SUN, Jingkang WANG

《化学科学与工程前沿（英文）》 2009年第3卷第3期页码 282-288 doi: 10.1007/s11705-009-0018-7

摘要： 6-Aminopenicillanic acid (6-APA) is a crucial pharmaceutical intermediate in the chemistry of semi-synthetic antibiotics. The focused beam reflectance measurement (FBRM) technology and particle vision measurement (PVM) technology were employed to the processes of online-monitoring of 6-APA crystallization behavior in a double-feeding semi-batch crystallizer. Experiments were carried out with four kinds of double-feeding policies and the results were compared with the traditional single-feeding. Records and analysis of FBRM indicated that the nucleation of double feeding policy was much higher than single policy, and chord length of 6-APA was almost determined and had little change after the nucleation peak. Ostwald ripening process had no significant effect on further growth of 6-APA crystal. PVM images showed that the crystal habit of 6-APA was continuously changed during the crystallization process. The development of (002) face in the final crystal for the five feeding policies were different.

关键词： 6-aminopenicillanic acid crystallization double-feeding FBRM PVM crystal habit

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Precipitation study of CO

Siming Chen, Yue Wu, Geoffrey W. Stevens, Guoping Hu, Wenshou Sun, Kathryn A. Mumford

《化学科学与工程前沿（英文）》 2020年第14卷第3期页码 415-424 doi: 10.1007/s11705-019-1882-4

摘要： Focused beam reflectance measurement (FBRM) and C nuclear magnetic resonance ( C NMR) analysis were used to study the precipitation process of CO -loaded potassium glycinate (KGLY) solutions at different CO loadings, during the addition of ethanol as an antisolvent at a rate of 10 mL·min . The volume ratio of ethanol added to the KGLY solution (3.0 mol·L , 340 mL) ranged from 0 to 3.0. Three solid-liquid-liquid phases were formed during the precipitation process. The FBRM results showed that the number of particles formed increased with CO loading and ethanol addition for CO -unsaturated KGLY solutions, whilst for CO -saturated KGLY solution it first increased then decreased to a stable value with ethanol addition. C NMR spectroscopic analysis showed that the crystals precipitated from the CO -unsaturated KGLY solutions consisted of glycine only, and the quantity crystallised increased with CO loading and ethanol addition. However, a complex mixture containing glycine, carbamate and potassium bicarbonate was precipitated from CO -saturated KGLY solution with the maximum precipitation percentages of 94.3%, 31.4% and 89.6%, respectively, at the ethanol volume fractions of 1.6, 2.5 and 2.3.

关键词： crystallization precipitation glycinate FBRM ¹³C NMR