以冷凍鑄造技術製備魚鱗萃取之氫氧基磷灰石/ 甲基聚醣複合支架用於鉛離子吸附

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研究生：	廖柏翔 Liaw, Bor-Shuang
論文名稱：	以冷凍鑄造技術製備魚鱗萃取之氫氧基磷灰石/ 甲基聚醣複合支架用於鉛離子吸附 Fish Scale-Extracted Hydroxyapatite/Chitosan Composite Scaffolds Fabricated by Freeze Casting for Lead Ion Adsorption
指導教授：	陳柏宇 Chen, Po-Yu
口試委員:	陳盈潔 Chen, Ying-Chieh 李紫原 Lee, Chi-Young
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2019
畢業學年度：	107
語文別：	英文
論文頁數：	124
中文關鍵詞：	魚鱗、氫氧基磷灰石、冷凍鑄造、多孔複合材、離子吸附
外文關鍵詞：	fish scale, hydroxyapatite, freeze casting, porous composite, ion adsorption
相關次數：	點閱：3 下載：0
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氫氧基磷灰石(HA)是一種廣泛存在於自然界的材料，尤其是在生物礦物中，其為生物的硬組織提供了良好的強度以及環境，因此氫氧基磷灰石常被使用為骨骼或是牙齒的支架材料。除了生醫方面的用途，近年來氫氧基磷灰石的離子吸附特性逐漸受到重視。在過去用來作為吸附材料的氫氧基磷灰石多以人工合成，但人工合成的氫氧基磷灰石的成本較高，因此在本篇研究中我們提出使用台灣鯛魚(Oreochromis mossambicus)魚鱗中的氫氧基磷灰石作為原料，來大幅度地減少製造成本以及汙染，魚鱗中萃取的氫氧基磷灰石粉末經過X-ray 繞射儀及粒徑分析儀的評估後，便可用於後續吸附材的製程。此外，我們引進了冷凍鑄造技術，將魚鱗中萃取的氫氧基磷灰石粉與甲基聚醣(CS)相結合，形成一具有方向性的多孔塊材。此種新型多孔塊材可藉由調控冷卻速率形成不同大小的孔洞通道，其微結構也更進一步被掃描式電子顯微鏡(SEM)還有汞壓汞孔徑分佈儀確認，結果顯示此種塊材有著從10奈米到100微米的多階層孔洞。為了瞭解此種多孔複合材的可應用範圍，本實驗中採取了兩種不同的實驗設計，批量吸附(batch processing)以及固定床吸附(fixed-bed processing)，並使用原子吸收光譜(AAS)來確認鉛離子吸附的效率。結果也證實此種新型複合材具有相當卓越的鉛離子吸附能力，藉由在冷凍鑄造過程調控不同的孔徑大小，吸附的表現及可應用範圍也會有著相應的變化。綜言之，本研究從魚鱗中萃取的氫氧基磷灰石所製備之複合多孔塊材在吸附方面有著很好的潛力，可根據是否應用於流體、離子的初始濃度、處理所需的期望時間等因素，適當的改變通道大小，廣泛地被應用於汙水處理領域。

Hydroxyapatite (HA) is a widely known mineral in nature and provides mechanical support for hard tissues, such as bone and teeth. In addition, HA is highlighted as a remarkable green material with high ion removal ability nowadays. However, the source of HA in most studies on wastewater treatment is typically from synthesis, causing the comparatively higher cost and pollution. In this study, we proposed a new approach to obtain HA from Tilapia fish (Oreochromis mossambicus) scales. After cleaning and calcination, fish-scale extracted HA powder was further confirmed by X-ray diffraction (XRD) and particle size analyzer. Thereafter, fish-scale extracted HA powder was combined with chitosan (CS) to form an orderly porous composite by the freeze casting technique, and its microstructure and pore size distribution were further analyzed by SEM and mercury porosimetry. The result demonstrated that the channel size can be modified by controlling proper cooling rate during freeze casting process, and the pore size distribution ranged from 10nm-100μm, corresponding to the interspace of particles and laminar structures. Subsequently, the applicable field of HA/CS composite scaffold was further evaluated by both batch and fixed-bed processes, and the innovative scaffold demonstrated remarkable adsorption capability for lead ion. The adsorption amount was also quantified by the Atomic Absorption Spectrometer (AAS). By tuning the cooling rates during freeze casting, the adsorption behaviors of HA/CS porous composites were distinctly different and can be potentially applied in various fields.

Chapter 1.    Introduction......................1
1.    Background................................1
2.    Goals.....................................3
Chapter 2.    Literature Review.................4
1.    Wastewater Treatment......................4
1.1.    Carbon materials..........................4
1.2.    Mineral materials.........................5
2.    Hydroxyapatite............................7
2.1.    Structure.................................7
2.2.    Production................................8
2.3.    Adsorption Characteristic.................9
2.4.    Hydroxyapatite/Chitosan Composites.......10
3.    Adsorption Analysis......................12
3.1.    Isotherm.................................12
3.2.    Rate Equation............................14
3.3.    Complicate Sorption......................15
4.    Porous Ceramic Materials.................18
4.1.    Replica/Sacrificial templating...........18
4.2.    Blowing..................................19
4.3.    Aerogels.................................20
4.4.    Freeze Casting...........................21
5.    Freeze Casting...........................22
5.1.    Fundamental Principles...................22
5.2.    Preparation and Structure Control........25
5.3.    Developments and Applications............27
Chapter 3.    Experimental Methods.............41
1.    Material Preparation.....................41
1.1.    Hydroxyapatite (HA) Powder Preparation...41
1.2.    Chitosan (CS) Solution Preparation.......42
1.3.    HA/CS Slurry Preparation.................42
2.    Synthesis of Scaffold....................43
2.1.    Freeze Casting...........................43
2.2.    Crosslinking Process.....................44
3.    Characterizations........................46
3.1.    Structural Characterization..............46
3.2.    Pore Size Distribution...................47
3.3.    Compressive Mechanical Testing...........47
3.4.    Evaluation of Environmental Influence....47
4.    Adsorption Experimental Design...........50
4.1.    Batch Processing.........................50
4.2.    Flame Atomic Adsorption Spectroscopy.....50
4.3.    Rate Equation............................52
4.4.    Isotherm.................................52
4.5.    Fixed Bed Process........................52
Chapter 4.    Results and Discussion...........59
1.    Material Analysis........................59
1.1.    Powder Analysis..........................59
1.2.    Chitosan.................................60
2.    Synthesis of Scaffolds...................61
2.1.    Cooling Source of Freeze Casting.........61
2.2.    Crosslinking Process.....................61
3.    Characterizations........................65
3.1.    Porosity.................................65
3.2.    Cooling Rate and Pore Size Distribution..66
3.3.    Compressive Mechanical Behavior..........67
3.4.    Evaluation of Environmental Influence....68
4.    Adsorption Experiment....................70
4.1.    Batch Processing.........................70
4.2.    Rate Equation............................74
4.3.    Precipitation Analysis...................75
4.4.    Isotherm.................................77
4.5.    Fixed Bed Processing.....................79
Chapter 5.    Conclusions......................114
References.......................................118

                                

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