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Experimental Evaluation of Fluid Shear Stress Impact on Secondary Nucleation in a Solution Crystallization of Paracetamol
Crystal Growth & Design ( IF 3.2 ) Pub Date : 2018-09-26 00:00:00 , DOI: 10.1021/acs.cgd.8b01074 Mustafa Yousuf 1 , Patrick J. Frawley 1
Crystal Growth & Design ( IF 3.2 ) Pub Date : 2018-09-26 00:00:00 , DOI: 10.1021/acs.cgd.8b01074 Mustafa Yousuf 1 , Patrick J. Frawley 1
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Cooling crystallization experiments were performed at 300 and 370 rpm over a range of saturation temperatures for the measurements of the metastable zone width (MSZW) using a large seed of paracetamol crystal in propan-2-ol solution. Particle imaging velocimetry (PIV) was used to quantify the fluid shear stress at each agitation rate employed, which was found to be 0.07 and 0.11 N/m2 respectively. A decrease in MSZW and growth only zone (GNZ) was observed with increasing shear stress, and the secondary nucleation threshold (SNT) was determined with a relative supersaturation ratio (Sr) of 1.17 at 0.07 N/m2 and 1.08 at 0.11 N/m2. Focused beam reflectance measurement (FBRM) displayed an increase in particle counts as nucleation progressed, with total counts increased by 25% at a higher fluid shear as more nuclei were being sheared off from the seed surface. Crystal nuclei breeding is proposed as a mechanism of secondary nucleation, where the surface of a seed crystal served as a nucleation site for the pre-existing clusters in the solution as was evident under scanning electron microscopy (SEM). Secondary nucleation and its link with fluid shear stress, a novel approach established in the present work, will offer a more precise model in process development and scale-up.
中文翻译：
扑热息痛溶液结晶中流体剪切应力对二次成核影响的实验评估
冷却结晶实验是在300到370 rpm的饱和温度范围内进行的，用于在丙-2-醇溶液中使用对乙酰氨基酚晶体的大晶种来测量亚稳区宽度（MSZW）。颗粒成像测速仪（PIV）用于量化所采用的每种搅拌速率下的流体剪切应力，发现其分别为0.07和0.11 N / m 2。随着剪切应力的增加，观察到MSZW和仅生长区（GNZ）的减少，并且确定了次级成核阈值（SNT），相对过饱和比（S r）在0.07 N / m 2时为1.17，在0.11 N时为1.08。 /米2。聚焦光束反射率测量（FBRM）显示，随着成核的进行，颗粒数增加了，在更高的流体剪切力下，随着从种子表面切下更多的核，总颗粒数增加了25％。晶体核育种被认为是二次成核的一种机制，其中晶种表面充当溶液中预先存在的簇的成核位点，这在扫描电子显微镜（SEM）下是显而易见的。二次成核及其与流体剪切应力的联系是本工作中建立的一种新方法，它将为工艺开发和规模扩大提供更精确的模型。
更新日期：2018-09-26
中文翻译：
扑热息痛溶液结晶中流体剪切应力对二次成核影响的实验评估
冷却结晶实验是在300到370 rpm的饱和温度范围内进行的，用于在丙-2-醇溶液中使用对乙酰氨基酚晶体的大晶种来测量亚稳区宽度（MSZW）。颗粒成像测速仪（PIV）用于量化所采用的每种搅拌速率下的流体剪切应力，发现其分别为0.07和0.11 N / m 2。随着剪切应力的增加，观察到MSZW和仅生长区（GNZ）的减少，并且确定了次级成核阈值（SNT），相对过饱和比（S r）在0.07 N / m 2时为1.17，在0.11 N时为1.08。 /米2。聚焦光束反射率测量（FBRM）显示，随着成核的进行，颗粒数增加了，在更高的流体剪切力下，随着从种子表面切下更多的核，总颗粒数增加了25％。晶体核育种被认为是二次成核的一种机制，其中晶种表面充当溶液中预先存在的簇的成核位点，这在扫描电子显微镜（SEM）下是显而易见的。二次成核及其与流体剪切应力的联系是本工作中建立的一种新方法，它将为工艺开发和规模扩大提供更精确的模型。
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