系統識別號 | U0002-1108202115530800 |
---|---|
DOI | 10.6846/TKU.2021.00244 |
論文名稱(中文) | 生物可分解聚(3-羥基丁酯-co-4-羥基丁酯)/醋酸丁酸纖維素摻合物之物理、機械與形狀記憶性質 |
論文名稱(英文) | Physical,mechanical and shape memory properties of biodegradable poly(3-hydroxybutyrate-co-4-hydroxybutyrate)/cellulose acetate butyrate blends |
第三語言論文名稱 | |
校院名稱 | 淡江大學 |
系所名稱(中文) | 化學工程與材料工程學系碩士班 |
系所名稱(英文) | Department of Chemical and Materials Engineering |
外國學位學校名稱 | |
外國學位學院名稱 | |
外國學位研究所名稱 | |
學年度 | 109 |
學期 | 2 |
出版年 | 110 |
研究生(中文) | 蔡泓鈺 |
研究生(英文) | Hong-Yu Tsai |
學號 | 608400098 |
學位類別 | 碩士 |
語言別 | 繁體中文 |
第二語言別 | |
口試日期 | 2021-07-20 |
論文頁數 | 108頁 |
口試委員 |
指導教授
-
董崇民(tmdon@mail.tku.edu.tw)
委員 - 邱文英(ycchiu@ntu.edu.tw) 委員 - 賴森茂(smlai@niu.edu.tw) |
關鍵字(中) |
聚羥基丁酯 纖維素 形狀記憶 相容性 |
關鍵字(英) |
poly(3-hydroxybutyrate-co-4-hydroxybutyrate) cellulose acetate butyrate shape memory polymer compatibility |
第三語言關鍵字 | |
學科別分類 | |
中文摘要 |
醋酸丁酸纖維素(cellulose acetate butyrate,CAB)具有高透明度、優良抗濕、耐紫外光、耐寒、柔韌、透明、電絕緣等優秀的性能且無毒性,且可溶於多種溶劑,但加工範圍窄,造成加工上有困難,而聚(3-羥基丁酯-co-4-羥基丁酯) (poly(3-hydroxybutyrate-co-4-hydroxybutyrate),P34HB)具有生物可分解性、生物來源、生物相容性,且機械性質好,但熱穩定性差的特性,為了保留其多項優秀的性能,同時又可以使CAB加工溫度降低,因此本研究利用熔融混摻將CAB與P34HB進行混合,目的是使混摻物同時具有CAB及P34HB的優點,並且克服他們的缺點,針對CAB/P34HB摻合物,測量不同組成摻合物之熱性質、物理性質、機械性質以及形狀記憶性質。而結合DSC及DMA測試可以確定CAB與P34HB並不如文獻中所說的完全相容,在P34HB含量少於20 % 時,CAB與P34HB才會完全相容,且在機械性質測試中發現抗張強度、楊氏模數及降伏強度在P34HB含量大於20 wt % 時也會有較大的改變,而利用DMA測得摻合物之形狀記憶性質則是隨著P34HB含量的增加會使摻合物的形狀恢復溫度降低,摻合物的形狀回復率隨著P34HB含量的增加而降低,在P34HB含量為20 wt %有最低之形狀回復率(Rr),繼續增加P34HB含量時,形狀回復率反而上升。 |
英文摘要 |
Cellulose acetate butyrate (CAB) has excellent properties such as high transparency, excellent moisture resistance, UV resistance, cold resistance, flexibility, transparency, electrical insulation, etc. It is non-toxic and soluble in a variety of solvents, but has a processing range Narrow, causing difficulties in processing, while poly(3-hydroxybutyrate-co-4-hydroxybutyrate) (P34HB) has biodegradability, biological origin, Biocompatibility, good mechanical properties, but poor thermal stability. In order to retain many of its excellent properties and reduce the processing temperature of CAB, this study uses melt blending to mix CAB and P34HB. The purpose is Make the blends have the advantages of CAB and P34HB at the same time, and overcome their shortcomings, for CAB/P34HB blends, measure the thermal properties, physical properties, mechanical properties and shape memory properties of the blends of different compositions. Combined with DSC and DMA tests, it can be determined that CAB and P34HB are not completely compatible as stated in the literature. When the content of P34HB is less than 20%, CAB and P34HB are completely compatible, and the tensile strength is found in the mechanical property test.,Young’s modulus and yield strength will also change greatly when the content of P34HB is greater than 20 wt%, and the shape memory properties of the blend measured by DMA will increase the content of P34HB. When the shape recovery temperature decreases, the shape recovery rate of the blend decreases with the increase of the P34HB content. When the P34HB content is 20 wt %, the shape recovery rate (Rr) is the lowest. When the P34HB content continues to be increased, the shape recovery rate increases instead. |
第三語言摘要 | |
論文目次 |
摘要 I 目錄 I 圖目錄 IV 表目錄 IX 第一章緒論 1 1.1 前言 1 1.2 研究目的與動機 1 第二章文獻回顧 3 2.1生物降解高分子 3 2.1.1生物降解高分子的種類 4 2.2聚羥基烷酯類 (Poly(hydroxyalkanoates);PHAs) 6 2.2.1 PHAs的發展史 6 2.2.2 PHAs的種類 6 2.2.3 PHAs的應用 6 2.3纖維素類(Cellulose) 7 2.3.1 Cellulose發展史 7 2.3.2 Cellulose種類 7 2.3.3 Cellulose應用 7 2.4 高分子摻合物 8 2.4.1 製備摻合物的方式 9 2.4.2 摻合物相容性 10 2.5 聚羥基烷酯摻合物的研究 12 2.6 纖維素摻合物的研究 13 2.7 纖維素與聚羥基烷酯摻合 14 2.8 高分子分解機制 15 2.8.1 生物降解 16 2.9 形狀記憶高分子 (Shape Memory Polymer, SMP) 17 2.9.1 形狀記憶高分子發展 20 2.10 形狀記憶高分子的應用 21 2.10.1 航太工程 21 2.10.2 生物醫學 22 第三章實驗方法與步驟 23 3.1 實驗藥品 23 3.2 實驗儀器 24 3.3 實驗步驟 27 3.3.1 利用溶劑法製備CAB/P34HB摻合物 27 3.3.2 利用熔融混練法製備CAB/P34HB摻合物 27 3.4 性質測試與結構分析 29 3.4.1 CAB/P34HB 摻合物化學結構分析(FTIR–ATR) 29 3.4.2 結晶構造分析(XRD) 29 3.4.3 薄膜結構觀察(SEM) 29 3.4.4 CAB/P34HB摻合物熱性質與相容性測試(DSC分析) 29 3.4.5 熱重損失測試(TGA) 29 3.4.6 拉伸機械性質測試(Tensile mechanical properties) 29 3.4.7 動態機械測試(DMA) 30 3.4.8 透明度及抗UV測試(UV-Vis Spectrophotometer) 30 3.4.9 形狀記憶測試(Shape memory test ) 31 3.4.10 CAB/P34HB表面結構觀察(AFM) 31 3.4.11 疏水性測試(Contact Angle) 31 3.4.12 酵素分解測試(脂肪酶) 31 第四章結果與討論 32 4.1 溶劑摻混s-CAB/P34HB摻合物 32 4.1.1 溶劑摻混s-CAB/P34HB相容性 32 4.1.2 結晶構造分析(XRD) 36 4.2 熔融摻混m-CAB/P34HB 摻合物 37 4.2.1 m-CAB/P34HB 摻合物化學結構分析(ATR) 37 4.2.2 m-CAB/P34HB 結晶構造分析(XRD) 39 4.2.3 m-CAB/P34HB 薄膜結構觀察(SEM) 40 4.2.4 CAB/P34HB 摻合物的相容性 60 4.2.5 m-CAB/P34HB 摻合物之熱重損失測試(TGA) 63 4.2.6 摻合物拉伸性質測試(Tensile mechanical properties) 66 4.2.7 m-CAB/P34HB 摻合物動態機械測試(DMA) 71 4.2.8 m-CAB/P34HB透明度及抗UV測試(UV-Vis Spectrophotometer) 77 4.2.9 m-CAB/P34HB形狀記憶測試 78 4.2.10 CAB/P34HB 表面結構觀察(AFM) 89 4.2.11 疏水性測試(Contact Angle) 93 第五章結論 97 參考文獻 98 附錄 103 A. P34HB 組成分析(NMR) 103 B. m-C6P4低溫範圍動態機械測試(DMA) 105 C. C8P2及C6P4 97 ℃ 形狀記憶(DMA) 108 圖目錄 圖2-1有氧條件下高分子生物降解的機制3 3 圖2-2可生物降解和不可生物降解的塑料5 4 圖2-3 PHA的合成6 5 圖2-4 纖維素的不同來源19 8 圖2-5 DSC熱分析圖(a)可混溶的摻合物(b)接近相分離的可混溶的摻合物(c)接近完全不混溶的部分可混溶的摻合物和(d)不可混溶摻合物29。 11 圖2-6高分子降解種類41 15 圖2-7雙向形狀記憶高分子的(A)機械力與(B)能量表示圖47 18 圖2-8形狀記憶高分子在航太工程的應用46 21 圖2-9形狀記憶高分子於生物醫學上之應用46 22 圖3-1 ASTM D 638 Type Ⅴ 標準試片圖 30 圖4-1 利用溶劑混練法製備不同比例s-CAB/P34HB摻合物第一次升溫圖,升溫速率10 ℃/min 33 圖4-2 利用溶劑混練法製備不同比例s-CAB/P34HB摻合物第二次升溫圖升溫速率10 ℃/min 33 圖4-3 利用溶劑混練法製備不同比例CAB/P34HB摻合物的XRD圖 36 圖4-4熱壓製備CAB及P34HB的 FTIR圖(CAB先經過混練) 38 圖4-5 熔融混練法製備不同比例m-CAB/P34HB 摻合物的FTIR圖 38 圖4-6 利用熔融混練法熱壓製備不同比例CAB/P34HB的XRD圖 39 圖4-7 m-CAB表面SEM圖 41 圖4-8 m-CAB淬斷面SEM圖 41 圖4-9 m-C9P1摻合物表面SEM圖 42 圖4-10 m-C9P1摻合物淬斷面SEM圖 42 圖4-11 m-C8P2摻合物表面SEM圖 43 圖4-12 m-C8P2摻合物淬斷面SEM圖 43 圖4-13 m-C7P3摻合物表面SEM圖 44 圖4-14 m-C7P3摻合物淬斷面SEM圖 44 圖4-15 C-C6P4摻合物表面SEM圖 45 圖4-16 m--C6P4摻合物淬斷面SEM圖 45 圖4-17 c-P34HB表面SEM圖 46 圖4-18 c-P34HB淬斷面SEM圖 46 圖4-19 m-CAB拉伸斷裂平面SEM圖 47 圖4-20 m-CAB拉伸斷裂面SEM圖 47 圖4-21 m-C9P1摻合物拉伸斷裂平面SEM圖 48 圖4-22 m-C9P1摻合物拉伸斷裂面SEM圖 48 圖4-23 m-C8P2摻合物拉伸斷裂平面SEM圖 49 圖4-24 m-C8P2摻合物拉伸斷裂面SEM圖 49 圖4-25 m-C7P3摻合物拉伸斷裂平面SEM圖 50 圖4-26 m-C7P3摻合物拉伸斷裂面SEM圖 50 圖4-27 m-C6P4摻合物拉伸斷裂平面SEM圖 51 圖4-28 m-C6P4摻合物拉伸斷裂面SEM圖 51 圖4-29 c-P34HB拉伸斷裂平面SEM圖 52 圖4-30 c-P34HB拉伸斷裂面SEM圖 52 圖4-31 m-CAB經Lipase分解95天後的SEM圖 53 圖4-32 m-C9P1經Lipase分解95天後的SEM圖 54 圖4-33 m-C8P3經Lipase分解95天後的SEM圖 55 圖4-34 m-C7P3經Lipase分解95天後的SEM圖 56 圖4-35 m-C6P4經Lipase分解95天後的SEM圖 57 圖4-36 c-P34HB經Lipase分解95天後的SEM圖 58 圖4-37 不同比例摻合物DSC第一次升溫圖 61 圖4-38 不同比例摻合物DSC第二次升溫圖 61 圖4-39 不同比例m-CAB/P34HB熱重損失圖。 64 圖4-40 不同比例m-CAB/P34HB摻合物熱重損失一次微分圖。 64 圖4-41 不同比例m-CAB/P34HB摻合物拉伸應力應變圖。 67 圖4-42 不同比例m-CAB/P34HB摻合物之斷裂伸長率。 67 圖4-43 不同比例m-CAB/P34HB摻合物之破壞強度。 68 圖4-44 不同比例m-CAB/P34HB摻合物之降伏強度。 68 圖4-45 不同比例m-CAB/P34HB摻合物之楊氏模數。 69 圖4-46 CAB/P34HB摻合物經拉力測試後之斷裂樣品(由右至左為1 = CAB、2 = C9P1、3 = C8P2、4 = C7P3、5 = C6P4、6 = C5P5、7 = P34HB)。 70 圖4-47 不同比例m-CAB/P34HB摻合物儲存模量(E’)圖。 72 圖4-48 不同比例m-CAB/P34HB摻合物損失模量圖(E”)。 72 圖4-49不同比例m-CAB/P34HB摻合物的損耗正切圖(Tanδ)。 73 圖4-50 不同比例m-CAB/P34HB摻合物在30 ℃ 下的儲存模量(E’)圖。 73 圖4-51 不同比例m-CAB/P34HB摻合物在30 ℃ 下的損失模量(E”)圖。 74 圖4-52 不同比例m-CAB/P34HB摻合物在30 ℃ 下的損耗正切(Tanδ)圖。 74 圖4-53 由DMA求得之Tg擬合Gordon-Taylor equation (為實際值)。 75 圖4-54 由DMA求得之Tg擬合Fox equation (為實際值)。 76 圖4-55 由DSC求得之Tg擬合Fox equation (為實際值)。 76 圖4-56 CAB、P34HB及不同比例m-CAB/P34HB摻合物在不同波長的穿透率,薄膜厚度約為0.4 mm 77 圖4- 57 m-CAB形狀記憶測試之應力、應變與溫度關係圖 82 圖4- 58 m-CAB形狀記憶測試之應力、應變、溫度對時間做圖 82 圖4- 59 m-C9P1形狀記憶測試之應力、應變與溫度關係圖 83 圖4- 60 m-C9P1形狀記憶測試之應力、應變、溫度對時間做圖 83 圖4-61 m-C8P2形狀記憶測試之應力、應變與溫度關係圖 84 圖4-62 m-C8P2形狀記憶測試之應力、應變、溫度對時間做圖 84 圖4- 63 m-C7P3形狀記憶測試之應力、應變與溫度關係圖 85 圖4- 64 m-C7P3形狀記憶測試之應力、應變、溫度對時間做圖 85 圖4-65 m-C6P4形狀記憶測試之應力、應變與溫度關係圖 86 圖4-66 m-C6P4形狀記憶測試之應力、應變、溫度對時間做圖 86 圖4-67 m-C5P5形狀記憶測試之應力、應變與溫度關係圖 87 圖4-68 m-C5P5形狀記憶測試之應力、應變、溫度對時間做圖 87 圖4-69 不同比例m-CAB/P34HB摻合物形狀固定率(Rf) 88 圖4-70 不同比例m-CAB/P34HB摻合物形狀回復率(Rr) 88 圖4-71 C-CAB表面AFM圖 90 圖4-72 C-C9P1表面AFM圖 90 圖4-73 C-C8P2表面AFM圖 91 圖4-74 C-C7P3表面AFM圖 91 圖4-75 C-C6P4表面AFM圖 92 圖4-76 C-P34HB表面AFM圖 92 圖4-77 m-CAB接觸角圖 93 圖4-78 m-C9P1接觸角圖 93 圖4-79 m-C8P2接觸角圖 94 圖4-80 m-C7P3接觸角圖 94 圖4-81 m-C6P4接觸角圖 95 圖4-82 m-P34HB接觸角圖 95 圖4-83 不同比例m-CAB/P34HB摻合物接觸角度圖 96 圖A-1 P34HB NMR圖 103 圖A-2 CAB NMR圖 104 圖B-1 C6P4摻合物低溫範圍儲存模量(E’)圖,頻率 = 1 Hz , 105 圖B-2 C6P4摻合物低溫範圍損失模量(E”)圖,頻率 = 1 Hz , 106 圖B-3 C6P4摻合物低溫範圍損耗正切圖(Tanδ),頻率 = 1 Hz , 107 圖C-1 C8P2形狀記憶 108 圖C-2 C6P4形狀記憶 108 表目錄 表3-1 溶劑混練製備各比例代號表 27 表3-2 熔融混練製備各比例代號表 28 表4-1 溶劑混練法治被不同比例CAB/P34HB摻合物第一次升溫圖 34 表4-2 溶劑混練法治被不同比例CAB/P34HB摻合物第二次升溫圖 35 表4-3 不同比例CAB/P34HB經酵素分解後重量(mg) 59 表4-4 不同比例CAB/P34HB經酵素分解後厚度(mm) 59 表4-5 不同組成m-CAB/P34HB摻合物的熱轉移溫度 62 表4-6 m-CAB/P34HB摻合物的熱降解溫度及殘渣量表 65 表4-7 不同比例CAB/P34HB摻合物之拉伸機械性質 69 表4-8 不同比例CAB/P34HB動態機械性 71 表4-9 利用DMA進行形狀記憶測試條件 79 表4-10 不同比例CAB/P34HB 摻合物形狀固定率(Rf)及形狀回復率(Rr) 80 表4-11 不同步驟應變圖 81 表4-12 不同比例CAB/P34HB透光度、接觸角、表面粗糙度 96 |
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