Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Common Agitated Tank Common Agitated Tank Common Agitated Tank Common Agitated TankCommon Agitated Tank Common Agitated Tank Common Agitated TankCommon

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林柏岩(Po-Yen Lin) 查詢紙本館藏

畢業系所

化學工程與材料工程學系

論文名稱

(Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Effects of Baffle Configuration and Vessel Size on Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Spherical Agglomerates of Dimethyl Fumarate in a Common Agitated Tank Common Agitated Tank Common Agitated Tank Common Agitated TankCommon Agitated Tank Common Agitated Tank Common Agitated TankCommon)

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摘要(中)

本篇論文的研究主旨在於探討不同平板式檔板與攪拌槽大小對富馬酸二甲酯球晶製程影響。在本篇研究中，我們運用0.5公升、2公升與10公升攪拌槽進行富馬酸二甲酯球晶製程，三種不同規格檔板被運用在相同攪拌槽與相同操作條件進行球晶製備，其分別為美國標準規格檔板、歐洲標準規格檔板與川島規格檔板，為了系統性地挑選球晶製程溶劑組合，我們對富馬酸二甲酯進行初始溶劑篩選，藉由初始溶劑篩選的結果可以建立富馬酸二甲酯的溶劑組合表以進行溶劑挑選。
由球晶顆粒大小分佈直方圖，我們發現在相同操作條件與相同桶槽大小下，球晶大小分佈會因為攪拌槽安裝不同規格檔板產生變化，此外，當以不同大小攪拌槽進行相同操作，球晶的產量會隨著攪拌槽放大而下降。本研究中，傅立葉轉換紅外線光譜儀、常溫示差掃描熱分析儀與X光繞射分析儀被運用來鑑定產物的晶型排列與結晶度，綜合紅外光圖譜、熱分析圖譜與X光繞射圖譜分析結果，產物的晶形排列不會受到球晶製程影響但結晶度具有差異，有關球晶溶離速率、顆粒流動性、機械強度與密度方面，相同大小的球晶會具有相同的溶離速率與流動性，然而，相同大小的球晶機械強度與密度會因為攪拌槽大小與檔板的不同而改變，較大的攪拌槽與較窄的檔板會使得球晶機械強度與密度下降，而藉由拉長攪拌時間則可以提高球晶機械強度與密度。

摘要(英)

The aim of this thesis is to study the effects of baffle configuration and different vessel sizes on the spherical agglomeration process. Spherical agglomeration was operated in the 0.5 L-, 2 L-, 10 L-sized stirred vessels with the standard dimensions and the arrangement of impeller diameter, impeller location and liquid level. The stirred vessel installed with the standard US vertical baffle type or the European baffle type, or the Kawashima baffle type was used to prepare the spherical agglomerates of dimethyl fumarate. Initial solvent screening was used to establish the form space of dimethyl fumarate for selecting the useful solvent combination in spherical agglomeration process. It was found that the particle size distribution of agglomerates prepared in the stirred vessel installed with different baffle types at the same operating conditions could vary significantly, and plenty of powders did not assemble into granules in the large size of vessel under the same operating conditions. The polymorphism of spherical agglomerates did not transform after cohering the powders into the granules, but the crystallinity of the agglomerates was slightly altered. The size-related properties, such as dissolution profile and flowability, of granules from the same size cut remained unchanged. The interior structure-related properties, such as density and mechanical property, of granules from the same size cut upon baffle change and scale up were decayed. However, granules could become denser and stronger by prolonged maturation time.

關鍵字(中)

★ 球晶
★ 製成放大
★ 檔板
★ 富馬酸二甲酯

關鍵字(英)

★ spherical agglomeration
★ scale up
★ baffle type
★ dimethyl fumarate

論文目次

摘要 i
Abstract ii
Acknowledgement iii
List of Figures vii
List of Tables xi
Chapter 1 Excusive Summary 1
1.1 Introduction 2
1.2 Introduction of Dimethyl Fumarate 7
1.3 Conceptual Framework 9
1.4 References 10
Chapter 2 Brief review 16
2.1 Spherical Crystallization Techniques 16
2.1.1 Spherical Agglomeration Method (SA) 17
2.1.2 Quasi-Emulsion Solvent Diffusion Method (QESD) 19
2.1.3 Ammonia Diffusion System (ADS) 21
2.1.4 Neutralization Method (NT) 22
2.1.5 Crystal-Co-Agglomeration Technique (CCA) 23
2.2 Effect of Operating Parameters 25
2.2.1 Bridging Liquid Type and Amount of Bridging Liquid 25
2.2.2 Agitator Speed 26
2.2.3 Maturation Time 26
2.2.4 Initial Particle Size and Solid Loading 27
2.2.5 Feeding Rate 27
2.2.6 Temperature 27
2.3 References 28
Chapter 3 Preparation and Characterization of Spherical Agglomerates in Dimethyl Fumarate 33
3.1 Introduction 33
3.1.1 The Effect of Inner Arrangement in a Stirred Vessel 33
3.2 Materials 37
3.2.1 Chemical 37
3.2.2 Solvents 37
3.3 Experimental Procedures 39
3.3.1 Initial Solvent Screening 39
3.3.2 Ball Milling 39
3.3.3 Spherical Agglomeration 40
3.3.4 Analytical Measurements 44
3.3.5 Instrumentation 51
3.4 Results and Discussion 54
3.4.1 Solvent Combination 54
3.4.2 Range of Operating Conditions 57
3.4.3 Effect of Operating Parameters 60
3.4.4 Characterizations of Agglomerates 61
3.4.5 Effect of Baffle Width 63
3.4.6 Effect of Vessel Size 70
3.4.7 Dissolution Behavior 81
3.5 Conclusions 85
3.6 References 86
Chapter 4 Future works 91

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Chapter 3
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指導教授

李度(Tu Lee)

審核日期

2015-7-29

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