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研究生:徐廷豪
研究生(外文):Ting-Hao Hsu
論文名稱:以超臨界二氧化碳技術探討不同硬度熱塑性聚氨酯之發泡行為
論文名稱(外文):Foaming Behavior of Thermoplastic Polyurethane with different Hardness by Supercritical CO2
指導教授:葉樹開
指導教授(外文):Shu-Kai Yeh
口試委員:楊銘乾蘇至善
口試委員(外文):Ming-Chien YangChie-Shaan Su
口試日期:2019-7-26
學位類別:碩士
校院名稱:國立臺灣科技大學
系所名稱:材料科學與工程系
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2019
畢業學年度:107
語文別:中文
論文頁數:150
中文關鍵詞:超臨界二氧化碳批次發泡熱塑性聚氨酯硬度添加劑
外文關鍵詞:supercritical carbon dioxidebatch foamingthermoplastic polyurethanehardnessadditives
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 熱塑性聚氨酯(TPU)主要是由硬鏈段及軟鏈段彼此交互連接所組成。由於其廣泛的硬度分布,使TPU發泡材能應用於許多領域,但因TPU複雜的結晶行為和收縮情形,難以控制不同種類TPU達到最佳之發泡效果。目前很少有文獻在ETPU泡珠製備方面,針對不同硬度TPU的發泡行為作詳細探討。
  本研究採用三種不同硬度(85A、90A、95A)的聚醚系TPU,利用超臨界二氧化碳作為發泡劑,以一步法批次發泡製備泡材,對泡孔結構與發泡溫度和壓力的關係進行廣泛的研究。泡孔尺寸在50μm左右,膨脹率達6倍以上,收縮率10%左右。
  首先以85A-TPU的軟化點作為參考溫度,在不同壓力(1100-2000 psi)下含浸,結果發現以Psat = 1100 psi的條件最符合用來製備泡珠(較佳的穩定膨脹比及較低的收縮率),混煉會顯著改變泡孔型態,泡孔密度增加了近百倍。
  因此在Psat = 1100 psi下,探討含浸溫度分別對三種不同硬度TPU泡孔型態之影響。另外透過熱分析及物性分析發現,相分離的趨勢會隨著硬度提高越來越明顯,使硬段的晶體堆疊,有更難以發泡的趨勢,其中尤以95A-PR的發泡效果下降最多。
接著我們嘗試以三種不同功能之添加劑-成核劑(talc),擴鏈劑(ADR),抗縮劑(ABS),各別對發泡效果較佳的85A及90A-TPU之泡材進行分析及改善。結果發現,對硬度較低的85A-TPU,talc對發泡效果的改善較為顯著,原因可能與硬段含量及排列有關。
  本實驗成功分析不同硬度之聚醚系TPU因混煉造成的發泡行為,並篩選出適合用於製備TPU泡珠的硬度種類及發泡條件。
Thermoplastic polyurethane (TPU) is mainly composed of different hard segments and soft segments, such a wide range of hardness, TPU foams are suitable for many applications. At the moment, very few studies have investigated the foaming behavior of different hardness TPU in expanded thermoplastic polyurethane (ETPU) bead foam manufacturing.
  In this study, polyether TPUs (85A, 90A, and 95A) with different hardness were foamed through one-step batch foaming using super critical CO2 as the blowing agent. The cell size, expansion ratio, cell density, and shrinkage ratio versus foaming temperature and foaming pressure were studied intensively.
  First, the softening temperature of 85A-TPU was applied as the reference temperature and the sample was saturated at various pressures from 2000 psi to 1100 psi. When the saturation pressure reduced to 1100 psi, the foam shrinkage phenomena was significantly alleviated and the highest expansion ratio was obtained. After compounding, the cell density was increased by almost two orders of magnitude.
  Therefore, at Psat = 1100 psi, the influence of saturated temperature on the three different hardness of TPU’s cell morphology was investigated. In addition, through thermal analysis and physical property analysis, it was found that the phase separation became more obvious with increasing hardness. The crystallization of hardsegments made foaming more difficult.
In the second part of this study, three different functional additives - nucleating agent (talc), chain extender (ADR) and anti-shrinkage agent (ABS) were added to improve the cell structure of 85A and 90A-TPU. It was found that the improvement of foaming effect of additives was more significant for the low hardness TPU (85A-TPU), which may be related to arrangement of hard segments. In summary, we can choose optimum foaming conditions and hardness to prepare ETPU bead foam.
摘要 I
Abstract III
誌謝 V
目錄 VI
圖目錄 IX
表目錄 XIII
第一章 緒論 1
1.1 前言 1
第二章 文獻回顧 4
2.1 熱塑性聚氨酯 4
2.1.1 TPU的結構與反應機制 5
2.1.2 TPU微相分離 6
2.1.3 TPU的分類 7
2.2 高分子發泡材料 9
2.2.1 發泡劑種類 10
2.2.2 發泡機制 13
2.3 物理發泡製程 25
2.3.1批次發泡 25
2.3.2 泡珠材料 27
2.4 添加劑 31
2.4.1 擴鏈劑-ADR 32
2.4.2 成核劑-滑石粉 33
2.4.3 抗縮劑-ABS 33
第三章 實驗方法 36
3.1實驗藥品 36
3.2實驗儀器 38
3.3實驗步驟 41
3.3.1 實驗流程圖 41
3.3.2 混煉不同硬度之TPU 42
3.3.3 混煉TPU與不同比例添加劑 42
3.3.4 射出啞鈴型試片(拉伸試驗) 42
3.3.5 熱壓成型(流變試驗) 43
3.3.6 一步法批次發泡 43
3.4測量方法 44
3.4.1 熔融指數分析儀(Melt Flow Index) 44
3.4.2 熱示差掃描量熱儀(DSC) 45
3.4.3 調製式動態熱機械分析儀 (TMA) 45
3.4.4 超效能高分子層析系統(APC) 46
3.4.5 機械性質量測-拉伸試驗 47
3.4.6 流變學實驗 48
3.4.7 硬度量測 48
3.4.8 掃描式電子顯微鏡(SEM) 49
3.4.9 泡材密度(foam density)及膨脹倍率(expansion ratio)量測 49
3.4.10 泡孔尺寸(cell size)計算 50
3.4.11 泡孔密度(cell density)計算 50
3.4.12 泡壁厚度(cell wall thickness)計算 50
第四章 結果與討論 52
4.1 不同硬度熱塑性聚氨酯之材料性質分析 52
4.1.1 混煉數據分析與熔融指數(MFI)量測 52
4.1.2 硬度量測 56
4.1.3 分子量量測 56
4.1.4 流變性質-剪切黏度分析 57
4.1.5 拉伸試驗 58
4.1.6 熱塑性聚氨酯之熱分析 59
4.2 不同含浸壓力及溫度對泡材之影響 67
4.2.1不同含浸壓力對泡材之影響 68
4.2.2 不同含浸溫度對泡材之影響 72
4.3 不同硬度熱塑性聚氨酯之發泡行為 78
4.3.1 混煉加工對熱塑性聚氨酯發泡材之影響 78
4.3.2 不同硬度熱塑性聚氨酯泡材膨脹分析 82
4.3.3不同硬度熱塑性聚氨酯之泡孔分析 84
4.4 泡材收縮與回膨探討 88
4.4.1 不同含浸壓力對泡材收縮之影響 89
4.4.2 混煉對泡材收縮之影響 90
4.4.3 硬度對泡材收縮之影響 91
4.5 添加劑對不同硬度熱塑性聚氨酯之影響 93
4.5.1 添加劑/熱塑性聚氨酯之物性分析 94
4.5.2添加劑對熱塑性聚氨酯泡材之影響 95
4.5.3添加劑對不同硬度熱塑性聚氨酯泡材之影響 101
第五章 結論 105
參考文獻 106
附錄A 85A-AR不同含浸壓力的發泡情形(Tsat=150 °C) 118
附錄B 85A-AR不同含浸溫度的發泡情形(Psat = 2000 psi) 120
附錄C 添加劑/85A及90A-TPU剪切黏度分析 122
附錄D 添加劑/90A-TPU之材料分析 124
附錄E 擴鏈劑(1 wt% ADR)/90A-TPU發泡情形 125
附錄F 抗縮劑(5 wt% ABS)/90A-TPU發泡情形 126
附錄G 各硬度TPU材料分析及泡材分析總表 128
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