臺灣博碩士論文加值系統

PA6纖維具有易染色、高彈性、耐磨、耐高溫等優點。尼龍熱熔膠用於紡織貼合上，具有降低成本、製程短、容易加工、增加商品品質等優點。本研究以乙二胺(Ethylenediamine，EDA)、己二酸二甲酯(Dimethyl adipate，DMA)、己二酸(Adipicacid，AA)、PA6為主要原料，以共聚合的方法合成具有低熔點的尼龍共聚物。
乙二胺是全球生產量僅次於己二胺(Hexamethylenediamine，HMDA)的二元胺類。因此，本實驗中共聚尼龍的合成主要分為三個部分：(1)所使用的二元胺單體BAEA，利用乙二胺與己二酸二甲酯進行胺-酯交換的縮合反應製得；(2)所共聚之尼龍鹽為己二酸與BAEA中和製得；(3)共聚尼龍為PA6與不同共聚比例之BAEA/AA salt進行共聚合。
PA6共聚高分子成功合成後，結構鑑定方面，透過核磁共振光譜儀(1H-NMR)及傅立葉光譜儀(FTIR)進行鑑定；熱性質方面，利用熱示差掃描分析儀(DSC)、動態機械分析儀(DMA)、熱重分析儀(TGA)進行鑑定；而機械強度方面，透過拉伸強度及T型剝離強度的測試，最後進行熔融紡絲及纖維吸濕性的測試。

Polyamide 6 (PA6) fiber has advantage such as high dyeing properties, elasticity, abradability. Nylon hot-melt adhesive(HMA) was used for bondinghas advantage such as low cost, shortprocess, increase the quality oftextile. In this study, we use ethylenediamine (EDA), dimethyl adipate(DMA), adipicacid(AA), and PA6as the material.Synthesis of nylon copolymers with low melting point by copolymerization.
Ethylenediamine is a diamine that the global production is only inferior to hexamethylenediamine (HMDA).Thus, the synthesis of copolymer nylon in this experiment is divided into three parts: (1)Thenovel diamine monomer BAEA used is obtained by condensation reaction of ethylenediamine with dimethyl adipate. (2) The nylon salt is obtained by neutralizing adipic acid with BAEA. (3) Polyamide copolymer was PA6 and BAEA / AA salt with different ratios.
After synthesis of polyamide copolymer, all samples are characterized by Nuclear Magnetic Resonacce (1H-NMR),Fourier Transform Infrared Spectroscopy (FT-IR), Differential Scanning Calorimetry (DSC), Dynamic Mechanical Analysis (DMA), Thermogravimetric Analysis (TGA), tensile test and T-peel. Finally, the melt spinning analysis of spinnability and fiber moisture absorption.

摘要 i
ABSTRACT ii
致謝 iv
目錄 x
表目錄 xiv
圖目錄 xv
第一章 緒論 1
1.1 前言 1
1.2 研究動機 2
第二章 文獻回顧 3
2.1 聚醯胺(尼龍) 3
2.1.1 聚醯胺研發歷史 3
2.1.2 聚醯胺纖維的性能及應用 5
2.1.3 PA6及PA66的性能比較 8
2.2 聚醯胺纖維的技術 10
2.2.1 原料生產 10
2.2.2 聚合技術 12
2.2.3 紡絲技術 14
2.3 聚醯胺的反應機制 15
2.3.1 縮合聚合反應(Polycondensation reaction) 15
2.3.2 固態縮聚反應(Solid-state polycondensation，SSP) 16
2.3.3 氧化降解(Oxidative degradation) 17
2.4 乙二胺(Ethylenediamine，EDA) 19
2.5 聚醯胺的熔點 20
2.6 熱熔膠(Hot-melt adhesive，HMA) 21
2.6.1 聚醯胺熱熔膠的特性 22
2.6.2 聚醯胺熱熔膠的改性方向 22
2.6.3 聚醯胺熱熔膠的應用 23
2.7 熱熔紗(Fusible yarn) 24
第三章 實驗 26
3.1 實驗藥品與材料 26
3.1.1 二元胺單體之實驗藥品 26
3.1.2 尼龍鹽實驗藥品 28
3.1.3 共聚尼龍實驗藥品 29
3.1.4 氘帶溶劑實驗藥品 31
3.2 實驗儀器 32
3.2.1 核磁共振光譜儀 (Nuclear Magnetic Resonance Spectrometer；NMR) 33
3.2.2 傅立葉轉換紅外線光譜儀 (Fourier Transform Infrared Spectrometer；FTIR) 34
3.2.3 熱示差掃描分析儀 (Differential Scanning Calorimetry；DSC) 35
3.2.4 熱重分析儀 (Thermal Gravimetric Analyzer；TGA) 36
3.2.5 動態機械分析儀 (Dynamic Mechanical Analyzer；DMA) 37
3.2.6 熔融紡絲設備(Melt Spinning Equipments) 38
3.2.7 拉伸試驗機(Tensile Testing Machine) 41
3.2.8 恆溫恆濕箱(Environmental Chamber) 42
3.2.9 高壓聚合釜(2L-Autoclave) 43
3.2.10 熔融指數測定機(Melt Flow Indexer) 45
3.4 實驗流程圖 46
3.5 實驗方式 48
3.5.1 二元胺單體合成(BAEA) 48
3.5.2 尼龍鹽製備(BAEA/AA salt) 48
3.5.3 共聚尼龍合成(7.6 mole%) 49
3.6 測試方法及條件 50
3.6.1 核磁共振光譜儀 50
3.6.2 傅立葉轉換紅外線光譜儀 50
3.6.3 熱示差掃描分析儀 50
3.6.4 熱重分析儀 50
3.6.5 動態機械分析儀 50
3.6.6 熔融紡絲 51
3.6.7 拉伸試驗 52
3.6.8 剝離試驗(T-Peel Test) 53
3.6.9 纖維吸濕性測試 54
3.6.10 熔融指數測試 56
3.6.11 相對黏度(Relative viscosity) 56
第四章 結果與討論 57
4.1 二元胺(Diamine)之性質分析 57
4.1.1 1H-NMR結構分析 57
4.1.2 FT-IR官能基分析 58
4.1.3 DSC熱性質分析 59
4.1.4 TGA熱穩定性分析 60
4.2 尼龍鹽(Nylon salt)之性質分析 61
4.2.1 1H-NMR結構分析 61
4.2.2 FT-IR官能基分析 62
4.2.3 DSC熱性質分析 63
4.2.4 TGA熱穩定性分析 64
4.3 聚醯胺(Polyamide)之性質分析 65
4.3.1 1H-NMR結構分析 65
4.3.2 FT-IR官能基分析 69
4.3.3 DSC熱性質分析 71
4.3.4 TGA熱穩定性分析 74
4.3.5 DMA玻璃轉移溫度分析 77
4.3.6 相對黏度(Relative viscosity)分析 80
4.3.7 拉伸試驗分析 81
4.3.8 熔融指數(Melt Index，MI)分析 84
4.3.9 剝離試驗(T-Peel) 85
4.3.10 回潮率 86
第五章 結論 87
參考文獻 89

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