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研究生： 杜威達
Wei-Da Tu
論文名稱： 濕式粉末聚合於高速高剪力環境下之成長行為研究
An investigation into the high shear wet granulation behaviours and the regime map development
指導教授： 蕭述三
Shu-San Hsiau
口試委員:
學位類別： 博士
Doctor
系所名稱： 工學院 - 機械工程學系
Department of Mechanical Engineering
畢業學年度： 97
語文別： 英文
論文頁數： 129
中文關鍵詞： 粉末 、聚合 、剪力 、粒徑 、混合 、成長 、攪拌
外文關鍵詞： regime map, particle size, liquid-to-solid ratio, L/S, impeller speed, growth behaviour, high shear mixer, granulation, agglomeration
相關次數： 點閱：15  下載：0 
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    • 「濕式顆粒聚合作用」常見於自然界中。其原理也經常被工業界使用來處理粉顆粒材料，例如製藥、粉末冶金、食品、農業、化工原料等等。其基本的過程是利用液體使顆粒彼此沾黏，藉以聚合成形，並利用各種操作條件與材料特性，來達到特定材料性質的技術。
    高速、高剪力聚合機器 (high shear granulator)是工業界常見之儀器，因為高剪力的作用可以處理各種黏度範圍之添加液體。因此本文以該儀器為研究對象，並搭配常見之化工原料進行研究。分析方式則採用力學分析與質料交換的觀點來判定各個操作條件下的統御機制，與成長模式的定義。在假設粉末不溶解在添加液體中的前提下，本研究發現粉末材料的尺寸對於聚合現象有很大的影響，包括成長率、初始粒徑以及最終粒徑。液體添加量的影響則表現在液體分佈的速率與顆粒沾黏能力上。此外，顆粒聚合成功的關鍵在於彼此順利沾黏並且發生塑性變形。其中塑性變形的程度除了液體添加量以外還受到攪拌速率的影響，兩者呈現非線性關係。在成長模式方面，本研究所發展之預測方式可以釐清目前理論的混淆之處。根據該預測模式發現：同樣的固體與液體材料可以透過適當的操作設計，展現出所有的成長模式。此外，亦發現粒徑集中化的關鍵在於液體分佈集中化，恰與其他儀器相同 [1]。這些發現的應用皆對目前業界有高度應用的價值。最後本論文也提供了數項值得延伸的研究主題與建議。

    This thesis investigated the interactions between materials properties and operating conditions in high shear wet granulation. It was found that particles sizes between 1.5 to 85 μm had a significant effect on the granule size growth rate, final average size of granules and the distribution of granule size. The liquid-to-solid (L/S) ratio had a significant effect on the growth rate as well. It was possibly because more binder addition could result in better deformability, which is essential for colliding granules to be adhered onto each other permanently. The effect of L/S on agglomeration depended on the magnitude of impeller speed, and the relationship of each other is not linear.
    This thesis also proposed a more clarified definition to allocate the accurate boundaries between steady growth, induction behaviour and the rapid growth on the growth regime map. This can enable a better prediction of granulation behaviours. A growth regime map for this thesis was drawn. This map showed that a single system of solid and binder can exhibit five growth behaviours. A pre-requisite of monomodal GSD (granule size distribution) was found the same with that in a rotating drum [1]. Several suggested experiments regarding its microscopic description and other possible investigation plans were proposed in Chapter 5.

    摘要 i Abstract ii Acknowledgment iii Content iv List of figures vi List of tables viii Nomenclature ix Chapter 1 Introduction 1 1.1 Definition of granulation 1 1.2 Classification of size enlargement processes 1 1.2.1 Growth/tumble agglomeration 2 1.2.2 Coating/Layering 3 1.2.3 Agglomeration using pressure 3 1.2.4 Thermal effects 4 1.2.5 Drop formation 4 1.3 Applications and objectives 4 1.4 Economic scale 6 Chapter 2 Theories and mechanisms 8 2.1 Granulation processes (wet granulation) 8 2.1.1 Wetting and nucleation 8 2.1.2 Consolidation and growth 13 2.1.3 Attrition and breakage 17 2.2 Growth regime map 23 2.2.1 Evolution 23 2.2.2 Limitations of the regime map 29 2.3 Effects of operating conditions 32 2.3.1 Effects of impeller speed and effects of a chopper 32 2.3.2 Effects of particle size and the distribution 34 2.3.3 Effects of the nature of the liquid binder 35 2.4 Equipments for wet granulation 37 2.5 Population balance model 39 2.6 Motives 42 Chapter 3 The effect of powder size on induction behaviour and binder distribution 44 3.1 Preface 44 3.2 Experiment 46 3.2.1 Materials 46 3.2.2 Equipments 47 3.2.3 Experimental processes 50 3.3 Results and discussions 51 3.3.1 Mean diameter of the granules: L/S = 20% 51 3.3.2 Mean diameter of the granules: L/S = 17% 54 3.3.3 Mean diameter of the granules: comparisons 56 3.3.4 GSD measurements: L/S = 20% 59 3.3.5 GSD measurements: L/S = 17% 63 3.3.6 Binder distribution: 20% 67 3.3.7 Binder distribution: 17% 71 3.3.8 Binder distribution: comparisons 74 3.4 Conclusions 77 Chapter 4 Exploring the regime map for high-shear mixer granulation 78 4.1 Preface 78 4.2 Experiment 82 4.2.1 Materials 82 4.2.2 Experimental setups and processes 84 4.3 Results and discussions 87 4.3.1 Effects of the L/S ratio and impeller speed 87 4.3.2 GSD and the change of specific granules sizes 91 4.3.2.1 Nucleation only 91 4.3.2.2 Steady growth 93 4.3.2.3 Induction behavior 97 4.3.2.4 Rapid growth 100 4.3.2.5 Unconstrained growth 102 4.3.2.6 Reproducibility tests 104 4.3.3 Regime map for the system 107 4.4 Conclusions 109 Chapter 5 Future works & suggestions 110 5.1 Scope of the chapter 110 5.2 The key to achieve uniform GSD 110 5.3 The most favorite growth behaviour 112 5.4 Formulation design 114 5.5 Temperature distribution within the mixing field 115 Chapter 6 Conclusions 119 Reference list 121

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