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研究生：	盧昱丞 Lu, Yu-Cheng
論文名稱：	以化學改質法進行寶特瓶回收料高值化之研究 Study on High-value Utilization of Recycled PET Bottles by Chemical Modification
指導教授：	陳志勇 Chen, Chuh-Yung
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2021
畢業學年度：	109
語文別：	中文
論文頁數：	166
中文關鍵詞：	熔融聚合法、環狀結構二元醇、化學混摻、高分子混摻、聚對苯二甲酸乙二酯、發泡材
外文關鍵詞：	polycondensation, cycloaliphatic diols, chemical blend, polymer blend, polyethylene terephthalate, foam material
相關次數：	點閱：125 下載：0
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本研究以化學混摻的方式將聚對苯二甲酸乙二酯(Polyethylene terephthalate，PET)與不同種多元醇(Polyol)進行酯交換反應，提升回收PET的性質及其應用於高值化產品。在PET中添加具有環狀結構的1,4-環己二甲醇(1,4-CHDM)或奇數碳鏈的二元醇(如1,3-丙二醇(1,3-PD)、1,5-戊二醇(1,5-PDO))進行酯交換反應，可降低PET的結晶性，改善其加工性，其中以1,4-CHDM效果較為顯著。另外以六氫鄰苯二甲酸酐(HHPA)或甲基六氫鄰苯二甲酸酐(4MHHPA)與乙二醇(EG)或1,4-丁二醇(1,4-BG)進行開環反應，並將製備的polyol與PET進行熔融聚合反應，可得無結晶性的改質PET(mPET)。mPET與乙烯/醋酸乙烯酯共聚物(EVA)以雙螺桿進行高分子物理混摻，其混摻體的熔體強度皆提升，在混摻體斷裂面會產生均勻球狀相分離。進一步地以175 ℃進行mPET/EVA混摻體的化學發泡，可成功製備出泡孔大小均一，且直徑介於150-200 μm的發泡體。其中以EVA/PET-(HHPA-EG)混摻發泡體具有最好的延伸率、撕裂強度及永久壓縮歪。
另一方面，以長碳鏈的二元醇(如聚乙二醇(PEG)、聚四氫呋喃(PTMEG))與PET進行化學改質混摻，經拉力測試結果顯示mPET聚合物延展性隨著長碳鏈分子量的增加和添加比例的提高而增加；應力強度則隨著延伸率的增加而下降。碳酸二甲酯(DMC)與PEG製備的PDP多元醇加入PET進行化學混摻時，透過拉力及熱重分析儀(TGA)結果顯示，PET-PDP聚合物相對於PET-PEG聚合物有較佳的應力強度及裂解溫度。進一步地將PET-20 mol% PDP聚合物與PET進行物理熔融混摻，其混摻體具有較佳的應力強度及延展性，尤其以PET/PET-PDP=2/3效果最好。混摻體經DSC分析其顯示PET的結晶峰有顯著地增加，適用於纖維材料及射出成型之應用。

Polyethylene terephthalate(PET) and different kinds of polyol were transesterified chemical blending to improve the properties of recycled PET and its application to high-value products. Add 1,4-Cyclohexanedimethanol (1,4-CHDM) or odd-numbered carbon chain diols (such as 1,3-Propanediol (1,3-PD), 1,5-Pentanediol (1,5-PDO)) undergoes the transesterification reaction, which can reduce the crystallinity of PET and improve its processability. Among 1,4-CHDM is more effective. In addition, Hexahydrophthalic anhydride (HHPA) or Methylhexahydrophthalic anhydride (4MHHPA) and ethylene glycol (EG) or 1,4-butanediol (1,4-BG) are used for ring opening reaction and melt polymerization of the prepared polyol with PET to obtain modified PET (mPET) without crystallinity. mPET blend with ethylene/vinyl acetate copolymer (EVA) by twin screw, the melt strength of the polymer blend is improved, and uniform spherical phase separation occurs on the fracture surface of the polymer blend. Further chemical foaming of the mPET/EVA blend at 175℃ can successfully prepare foams with uniform cell sizes and diameters between 150-200 μm. Among them, EVA/PET-(HHPA-EG) blended foam has the best elongation, tear strength and permanent compression distortion.
On the other hand, long-carbon chain glycols (such as Polyethylene glycol (PEG), P olytetrahydrofuran (PTMEG)) are chemically modified and blended with PET. The tensile test results show that the elongation of mPET polymer increases in the molecular weight of the carbon chain and the addition ratio; the stress intensity decreases with the increase in elongation. When the PDP polyol prepared from dimethyl carbonate (DMC) and PEG is added to PET for chemical blending, the results of tensile test and thermogravimetric analyzer (TGA) show that PET-PDP copolymer’s stress intensity and cracking temperature is better than PET-PEG copolymer. Furthermore, PET-20 mol% PDP copolymer and PET are physically melt blended, and the polymer blend has better stress strength and elongation, especially when PET/PET-PDP=2/3 polymer blend has the best effect. DSC analysis of the polymer blend shows that the crystallization peak has increased significantly, which is suitable for fiber materials and injection molding applications

摘  要	I
Abstract	III
致謝	XXI
總 目 錄	XXIII
圖 目 錄	XXVII
表 目 錄	XXXIII
第一章 緒論	1
第二章 文獻回顧	5
2-1 聚對苯二甲酸乙二酯(PET)	5
2-2 回收寶特瓶	7
2-2-1 物理PET回收	8
2-2-2 化學PET回收	8
2-3 高分子混摻(Polymer Blending)	15
2-3-1 PET/PBT共混合物	15
2-3-2 PET/PTT共混合物	16
2-4 化學混摻	19
2-4-1 PBT型及PTT型多嵌段共聚物	20
2-4-2多嵌段共聚物可加工性	20
2-4-3多嵌段共聚物的透明性	22
2-5 觸媒	24
2-5-1 縮聚反應催化劑	24
2-5-2 水滑石觸媒(LDH)	26
2-5-3 水滑石插層改質製備方法	27
2-5-4 水滑石觸媒催化縮聚機制	28
2-6 發泡聚合物	32
2-6-1 EVA發泡材	32
2-6-2 EVA發泡材的機械強度	32
2-7 研究動機與目的	34
第三章 實驗內容	35
3-1 實驗藥品	35
3-2 實驗儀器	37
3-3 實驗步驟	39
3-3-1高壓反應器操作步驟(PET化學改質)	39
3-3-2高壓反應器操作步驟(合成 Polyol)	41
3-3-3PET化學改質	42
3-3-4自備多元醇寡聚物	46
3-3-5以自備多元醇寡聚物改質PET	49
3-3-7 PET與mPET(PET-PDP聚合物)之混摻	52
3-3-8 LDH-S之製備	52
3-3-9	EVA/mPET 化學發泡	53
3-4 儀器分析方法	54
第四章 結果與討論	60
4-1 LDH-S的鑑定	61
4-1-1 LDH-S之XRD鑑定	61
4-1-2 LDH-S的FTIR鑑定	62
4-1-3 LDH-S組成鑑定	63
4-2 短碳鏈多元醇改質聚對苯二甲酸乙二酯	65
4-2-1 環狀脂肪族二元醇改質聚對苯二甲酸乙二酯(PET-1,4-CHDM)	65
4-2-1-1 不同比例的PET-1,4-CHDM聚合物之結構鑑定	65
4-2-1-2 不同比例的PET-1,4-CHDM聚合物之熱性質分析	67
4-2-1-3 不同比例的PET-1,4-CHDM聚合物之機械性質分析	70
4-2-1-4 PET-1,4-CHDM聚合物的結晶型態分析	71
4-2-2 轉酯化觸媒的影響	75
4-2-2-1 以LDH-S為觸媒的PET-1,4-CHDM聚合物之結構鑑定	75
4-2-2-2 以LDH-S為觸媒的PET-20mol% 1,4-CHDM聚合物之熱性質分析	77
4-2-2-3 以LDH-S為觸媒的PET-20mol% 1,4-CHDM聚合物機械性質分析	79
4-2-3 奇數碳鏈二元醇改質聚對苯二甲酸乙二酯(PET-diol)	81
4-2-3-1 不同碳數PET-diol之結構鑑定	81
4-2-3-2 不同碳數PET-diol聚合物之熱性質分析	84
4-2-3-3 不同碳數PET-diol聚合物之機械性質分析	86
4-2-3-4 PET-1,3-PD及PET-1,5-PDO聚合物的結晶型態分析	88
4-2-4 環狀脂肪族多元醇(HHPA-diol & 4MHHPA-diol)寡聚物	91
4-2-4-1 HHPA-diol及4MHHPA-diol Polyol之結構鑑定	91
4-2-4-2 以HHPA-diol及4MHHPA-diol改質PET及其結構鑑定	94
4-2-4-3 以HHPA-diol及4MHHPA-diol改質PET之聚合物熱性質分析	95
4-2-4-4 以HHPA-diol及4MHHPA-diol改質PET之聚合物機械性質分析	98
4-2-4-5 以HHPA-diol及4MHHPA-diol改質PET的結晶型態分析	99
4-3  PET發泡行為之研究	105
4-3-1 EVA/mPET混摻體之可發泡性	105
4-3-2 EVA/mPET混摻體發泡體之泡孔結構及機械性質	112
4-4 長碳鏈脂肪族多元醇改質聚對苯二甲酸乙二酯	120
4-4-1 聚乙二醇改質聚對苯二甲酸乙二酯(PET-PEG)	120
4-4-1-1 不同比例及分子量的PET-PEG聚合物之結構鑑定	120
4-4-1-2 不同比例及PEG分子量的PET-PEG聚合物之熱性質分析	122
4-4-1-3 不同比例及PEG分子量的PET-PEG聚合物之機械性質分析	125
4-4-2 以LDH-S觸媒製備的PET-PEG聚合物	129
4-4-2-1 以LDH-S觸媒製備的PET-PEG聚合物之結構鑑定	129
4-4-2-2 以LDH-S觸媒製備的PET-PEG聚合物熱性質分析	131
4-4-2-3 以LDH-S觸媒製備的PET-PEG聚合物之機械性質分析	133
4-4-3 聚四氫呋喃改質聚對苯二甲酸乙二酯(PET-PTMEG)	135
4-4-3-1 PET-PTMEG聚合物之結構鑑定與本質黏度測量	135
4-4-3-2 不同比例PET-PTMEG聚合物之熱性質分析	137
4-4-3-3 不同比例PET-PTMEG聚合物之機械性質分析	139
4-4-4 長碳鏈二元醇( PDP)的製備	143
4-4-4-1 PDP polyol之結構鑑定	143
4-4-4-2 以PDP改質PET及其結構鑑定	144
4-4-4-3  不同比例的PET-PDP聚合物之熱性質分析	145
4-4-4-4 不同比例的PET-PDP聚合物之機械性質分析	148
4-5 PET/PET-PDP混摻體	151
4-5-1 不同比例的PET/PET-PDP混摻體之物性分析	151
4-5-2 不同比例的PET/PET-PDP混摻體之熱性質分析	153
第五章 總結	156
第六章 參考文獻	158
                                    

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