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首页> 外文期刊>Crystal growth & design >Experimental Evaluation of Fluid Shear Stress Impact on Secondary Nucleation in a Solution Crystallization of Paracetamol
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Experimental Evaluation of Fluid Shear Stress Impact on Secondary Nucleation in a Solution Crystallization of Paracetamol

机译:对乙酰氨基酚溶液结晶中次生次核的流体剪切应力的实验评价

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摘要

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/m(2) 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 (S-r) of 1.17 at 0.07 N/m(2) and 1.08 at 0.11 N/m(2). 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 preexisting 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.
机译:在300和370rpm在丙酰胺溶液中使用大种子的亚乙酰氨基醇晶体进行测量,在300和370rpm下在300和370rpm下进行冷却结晶实验。颗粒成像速度(PIV)用于在所用搅拌速率下量化流体剪切应力,分别发现为0.07和0.11n / m(2)。通过增加剪切应力观察到MSZW和生长区域(GNZ)的降低,并在0.07n / m(2)和0.11时的相对过饱和比(SR)测定次要成核阈值(SNT)。 n / m(2)。聚焦光束反射测量(FBRM)显示颗粒计数的增加,因为成核进展,在较高的流体剪切中,从种子表面剪切较高的核剪切时,总计数增加25%。提出了晶体核育种作为次生成核的机制,其中晶晶的表面用作溶液中扫描电子显微镜(SEM)下的溶液中预先存在的簇的成核位点。二次成核及其与流体剪切应力的联系,这项在本作工作中建立的新方法,将在工艺开发和扩展方面提供更精确的模型。

著录项

  • 来源
    《Crystal growth & design》 |2018年第11期|共10页
  • 作者单位

    Univ Limerick Bernal Inst Synth &

    Solid State Pharmaceut Ctr SSPC Castletroy Limerick Ireland;

    Univ Limerick Bernal Inst Synth &

    Solid State Pharmaceut Ctr SSPC Castletroy Limerick Ireland;

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  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 晶体学;
  • 关键词

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