臺灣博碩士論文加值系統

本研究以聚丙烯（PP）作為高分子基材，聚六亞甲基鹽酸胍（PHGH）作為抗菌高分子填料，聚丙烯接枝馬來酸酐（PP-g-MA）作為相容劑改善PP與PHGH之相容性；過氧化二異丙苯（DCP）作為架橋劑將PP與PHGH鍵結並增加物理性質。PP與PHGH由熔融混煉法製備抗菌複合材料，並以熱壓成型機將抗菌複合材料壓製成薄膜，抗菌複合材料進行抗菌測試、拉伸測試、示差掃描量熱法（DSC）、X射線衍射測試（XRD）、傅立葉紅外線轉換光譜儀（FT-IR）、釋放評估、變色評估(CIELAB)、偏光顯微鏡觀察。
　　本實驗結果發現PP/PHGH複合材料具有優良的抗菌性能，當PHGH添加量為10 wt%時，對大腸桿菌和金黃色葡萄球菌之抑菌率達到100 %，藉由釋放性評估能發現，因PHGH高度親水性使其快速釋放，達到高效滅菌之性能。物理性質方面，FTIR顯示PHGH包覆於PP基材並為物理混合；XRD確認添加PHGH會降低PP之結晶度但無影響晶型；偏光顯微鏡圖像示出PHGH會充當PP的成核劑，降低球晶尺寸；DSC明確表示PHGH對PP的熔融溫度以及結晶溫度之影響，其熔融溫度並無太大差異，也進一步證實晶型沒有改變，而結晶溫度有些許的提升，能判斷出PHGH幫助PP成核，有利於加工；而隨著PHGH添加量提高，PP拉伸性能有所下降，但提高複合材料的剛性；變色評估數據分析，PHGH會因為熱加工導致顏色有所改變，呈現微黃色，含量越高顏色越趨明顯。PP/PHGH複合薄膜綜合以上結果，PHGH於10 wt%得到最佳實驗參數。
　　本研究為了增加PHGH抗菌時效，以PP/PHGH複合材料分別添加PP-g-MA與DCP將PHGH穩固於PP基材。實驗結果顯示，添加PP-g-MA能將PHGH加固於PP基材中，定量抗菌測試顯示出較差的抗菌效果，當PP-g-MA含量越多時，抗菌效果隨之降低，其因通過共價鍵結使PHGH少量游離出PP/PHGH/PP-g-MA複合材料，達到長效抗菌效果，可以從抗菌定性測試中明顯觀測到，當PP-g-MA添加至10 wt%時得到良好的抑菌效果，而15、20 wt%抑菌效果明顯下降。其物理性質與PP/PHGH無太大差異，但於變色評估中可以看出，當PP-g-MA含量增加顏色差異有降低趨勢，其因PHGH包覆於PP基材，使其於熱加工時降低PHGH與熱能接觸，減少熱加工促使PHGH變色之情況。由上述可以確定，PP-g-MA添加至10 wt%為最佳實驗參數。添加DCP結果顯示，定性定量抗菌測試於0.1 wt%至0.3 wt%都顯現出優秀的抗菌效果，其以自由基方式將PHGH交聯於PP主鏈上，使PP-g-PHGH複合材料表面也含有PHGH並充分與細菌接觸，達到優異的抗菌結果。於物理性能有所提升，當添加0.1 DCP時，拉伸性能大幅度改善且接近於PP原始拉伸強度，0.2 wt%和0.3 wt%與PP/PHGH相比並沒有太大差異，而結晶溫度略微降低，使加工溫度更為廣泛，隨著DCP含量提升降低PHGH顏色之改變，改善色彩應用侷限。DCP含量於0.1 wt%便得到最佳抗菌性，但於0.2 wt%才使得抗菌性延長，為最佳長效抗菌薄膜。
關鍵字：聚丙烯（PP）、聚六亞甲基鹽酸胍（PHGH）、抗菌劑

In this study, polypropylene (PP) is used as polymeric substrate, whilst polyhexamethylene guanidine hydrochloride (PHGH) is used an antimicrobial polymer filler. Then, polypropylene grafted maleic anhydride (PP-g-MA) is used a compatilizer in order to improve the compatibility between PP and PHGH. Moreover, dicumyl peroxide (DCP) is used as a crosslinking agent, increasing the bonding between PP and PHGH and improving the physical properties. As a result, PP and PHGH are processed with melt compounding and the hot pressing in order to form composite films. The physical properties of antimicrobial polymer composite films are evaluated using qualitative and quantitative antibacterial assays, tensile test, differential scanning calorimetry (DSC), X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FT-IR), release assessment, CIELAB, and polarized light microscopy. The test results indicate that PP/PHGH composites have good antibacterial properties. When 10 wt% of PHGH is added, the composites have a 100 % antibacterial efficacy against Staphylococcus aureus (S. aureus) and Escherichia coli (E. coli). The release assessment results show that the composites can efficiently release drug to attain a high antibacterial efficacy due to the fact that PHGH is highly hydrophilic. Based on the results of physical properties, FTIR shows that PHGH is enwrapped in PP substrate in a physical mixing manner. XRD analysis shows that the addition of PHGH has a negative influence on the crystallinity but no influence on crystal form. The polarized light microscopy shows that PHGH serves as the nucleating agent, which contributes to decrease the spherocrystal size. DSC result indicates the influence of the addition of PHGH on the melting temperature and crystallization temperature of PP. The addition of PHGH does not affect the melting temperature or the crystal forms of PP. However, there is a marginal influence of the addition of PHGH on the crystallization temperature, which contributes to the crystal nucleation and the formation of PP. Moreover, increasing the amount of PHGH has a negative influence on the tensile properties, but a positive influence on the rigidity of the composites. According to CIELAB, thermal processing causes the shade of PHGH gradually to change and become yellowish. The more the PHGH, the darker the shade.
PP-g-MA or DCP is added to PP to secure the presence of PHGH in the composites so as to improve the antibacterial efficacy of PHGH. The test results show that using PP-g-MA can secure PHGH in the PP substrates, and quantitative antimicrobial assay confirms lower antibacterial activities. The antibacterial effect is inversely proportional to the amount of PP-g-MA. The covalent bond makes a small amount of PHGH dissociate from PP/PHGH/PP-g-MA composites, attaining a long term antibacterial effect but having similar physical properties to those of PP/PHGH composites. CIELAB results show that when PP-g-MA is increased, PHGH is enwrapped in PP substrate, thereby decreasing the change in shades caused by the decreased thermal processing with the thermal energy.
Using DCP to secure PHGH in the PP substrate contributes to a good antibacterial effect in both the qualitative and quantitative antibacterial tests. The free radicals of DCP crosslink PHGH to the main molecular chains of PP, allowing the surface of PP-g-PHGH composite abundant with PHGH to completely contact the bacteria, thereby yields extraordinary antibacterial effect. Moreover, using 0.1 DCP helps to improve the physical performances: the tensile properties are significantly improved and close to the original tensile strength of PP. In addition, the crystallization temperature is slightly decreased, which provides a greater range of thermal processing and improves the changes in colors of PHGH. Therefore, there is a greater range in color for applications.

目錄
摘要 I
ABSTRACT III
目錄 VI
第一章 前言 1
1.1 研究背景與意義 1
1.1.1 抗菌高分子材料種類 1
1.1.2 聚丙烯（PP） 2
1.1.3 聚六亞甲基鹽酸胍（PHGH） 3
1.1.4 高分子材料之改質 6
1.2 文獻回顧 9
1.3 相關專利 15
1.4 研究動機 28
1.5 研究目的 30
第二章 原理 32
2.1　混煉加工原理 32
2.2 熱壓成型加工原理 33
2.3 抗菌原理與測試 36
2.3.1　物理滅菌法 36
2.3.2　化學消毒法 42
2.3.3　抗菌測試 46
第三章 材料與方法 53
3.1　實驗材料 53
3.2　實驗流程及說明 55
3.2.1　PHGH高分子材料製備 55
3.2.2　PP/PHGH高分子抗菌複合材料實驗流程 57
3.2.3　PP/PHGH/PP-g-MA高分子抗菌複合材料實驗流程 59
3.2.4　PP-g-PHGH高分子抗菌複合材料實驗流程 61
3.3　實驗測試方法 63
3.4　實驗器材與設備 68
第四章 結果與討論 69
4.1 PHGH高分子材料性質分析 69
4.1.1 PHGH高分子材料核磁共振分析(1H-NMR) 69
4.1.2 PHGH高分子材料熱重分析（TGA） 71
4.1.3 PHGH高分子材料分子量分析 71
4.1.4 PHGH高分子材料抗菌分析 74
4.2 PP/PHGH高分子抗菌複合材料性質分析 77
4.2.1 PP/PHGH高分子抗菌複合材料FTIR分析 77
4.2.2 PP/PHGH高分子抗菌複合材料XRD分析 77
4.2.3 PP/PHGH高分子抗菌複合材料抗菌分析 80
4.2.4 PP/PHGH高分子抗菌複合材料拉伸性能分析 92
4.2.5 PP/PHGH高分子抗菌複合材料DSC分析 94
4.2.6 PP/PHGH高分子抗菌複合材料結晶型態之觀察 96
4.2.7 PP/PHGH高分子抗菌複合材料變色分析 96
4.2.8 PP/PHGH高分子抗菌複合材料釋放性分析 99
4.3 PP /PHGH/PP-g-MA高分子抗菌複合材料性質分析 101
4.3.1 PP /PHGH/PP-g-MA高分子抗菌複合材料FTIR分析 102
4.3.2 PP /PHGH/PP-g-MA高分子抗菌複合材料XRD分析 102
4.3.3 PP /PHGH/PP-g-MA高分子抗菌複合材料抗菌分析 104
4.3.4 PP /PHGH/PP-g-MA高分子抗菌複合材料拉伸性能分析 111
4.3.5 PP /PHGH/PP-g-MA高分子抗菌複合材料DSC分析 113
4.3.6 PP /PHGH/PP-g-MA高分子抗菌複合材料結晶型態之觀察 115
4.3.7 PP /PHGH/PP-g-MA高分子抗菌複合材料變色分析 115
4.3.8 PP /PHGH/PP-g-MA高分子抗菌複合材料釋放性分析 118
4.4 PP-g-PHGH高分子抗菌複合材料性質分析 120
4.4.1 PP-g-PHGH高分子抗菌複合材料FTIR分析 121
4.4.2 PP-g-PHGH高分子抗菌複合材料XRD分析 121
4.4.3 PP-g-PHGH高分子抗菌複合材料抗菌分析 123
4.4.4 PP-g-PHGH高分子抗菌複合材料拉伸性能分析 129
4.4.5 PP-g-PHGH高分子抗菌複合材料DSC分析 131
4.4.6 PP-g-PHGH高分子抗菌複合材料結晶型態之觀察 133
4.4.7 PP-g-PHGH高分子抗菌複合材料變色分析 133
4.4.8 PP-g-PHGH高分子抗菌複合材料釋放性分析 136
第五章 結論 138
第六章 建議 141
參考文獻 143

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