研究生: |
蔡芳昌 Fang-chang Tsai |
---|---|
論文名稱: |
活性塑膠包裝材料的製備與研究 Preparation and Investigation of Active plastic Package Materials |
指導教授: |
葉正濤
Jen-taut Yeh |
口試委員: |
張豐志
Feng-chih Chang 陳幹男 Kan-nan Chen 黃繼遠 Chi-yuan Huang 芮祥鵬 Syang-peng Rwei 許應舉 Ying-gev Hsu 黃國賢 Kuo-shien Huang 賴顯松 Sang-song Lai |
學位類別: |
博士 Doctor |
系所名稱: |
工程學院 - 材料科學與工程系 Department of Materials Science and Engineering |
論文出版年: | 2007 |
畢業學年度: | 95 |
語文別: | 中文 |
論文頁數: | 218 |
中文關鍵詞: | 改質聚醯胺 、乙烯乙烯醇共聚物 、奈米尼龍掺混物 、抗壞血酸 、鐵粉 、改性鐵粉 、氧氣滲透速率 、脫氧性質 |
外文關鍵詞: | modified polyamide, ethylene vinyl alcohol copolymer, nylon 6 clay, ascorbic acid, iron, modified iron, oxygen permeation rates, oxygen depletion properties |
相關次數: | 點閱:288 下載:2 |
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本論文主要是針對聚丙烯(polypropylene, PP),聚丙烯/改質聚醯胺(modified polyamide, MPA)/乙烯乙烯醇共聚物(ethylene vinyl alcohol copolymer, EVOH)(PP/MPAEVOH)摻混物製備與對汽油阻隔性質進行研究; 亦選取奈米尼龍掺混物(nylon 6 clay, NYC)搭配MPA掺混製備改質聚醯胺奈米尼龍掺混物(MPANYC)塑膠並對其氧氣滲透阻隔性能進行研究。 另一方面,為了改善現今包裝材料產品保存包裝內容的時效,採用抗壞血酸(ascorbic acid, Vc)、鐵粉(iron, Fe)與改性鐵粉(modified iron, MFe)鐵粉分別作為主要的脫氧劑成分摻混加入具較高透氧與透水率的乙烯-醋酸乙烯酯共聚合物(Ethylene vinyl acetate,EVA)塑膠中製備成活性塑膠包裝材料並研究其脫氧性能。
結果發現純PP瓶阻隔汽油滲透之效果非常差,但在PP內摻混10wt%的較適化MPA、MPAEVOH配方進行吹瓶後, PP/MPA吹瓶樣品之汽油阻隔滲透速率已分別較原PP 與PP/EVOH PP吹瓶樣品慢了10.1及1.2倍。 其中 PP/MPAEVOH系列吹瓶樣品對汽油之滲透阻隔性質隨MPAEVOH內EVOH達一最適化添加量時其阻隔效果達最佳化,且在其吹瓶樣品內可發現明顯被拉長的MPAEVOH積層結構。比如, PP/MPA5EVOH1吹瓶樣品之汽油滲透速率僅2.5×10-2g/day已明顯較PP/MPA吹瓶樣品之滲透速率(2.8×10-1g/day)為慢,其汽油滲透阻隔改善倍率已是原PP與PP/MPA瓶之108與11倍。 為了解上述這些有趣的汽油滲透阻隔性質,PP, PP/EVOH, PP/MPA 與PP/MPAEVOH 樣品的流變、熱學、X光繞射(WAXD)與FT-IR性質也在本文中進行詳細研究與討論。
另一方面值得注意的當摻混NYC入MPA後,MPANYC吹膜樣品的氧氣滲透速率明顯比MPA與NYC好。 事實上,MPANYC吹膜樣品的氧氣滲透速率隨著其內NYC 含量達20 wt%之最適化值時, MPA4NYC1 吹膜樣品的氧氣阻隔改善倍率已達105倍。 此種阻隔氧氣滲透之性質已與文獻中所報導之PVDC 吹膜樣品的阻隔氧氣滲透性能相近。 類似於上述NYC含量對氧氣滲透性質之影響,NYC含量對MPANYC吹膜樣品之自由體積性質(如Rf, Vf與Fv 等數值)的影響亦有相似的趨勢。 比如,MPANYC 樣品隨其內NYC含量達20%時Rf, Vf, I3與Fv 數值均分別達到一最小數值。 寬角X光繞射性質建議MPA分子和NYC樹脂中的PA分子在任何比例下是相容的, 因原先對應於MPA內PA的晶形結晶熔融吸熱峰及X光繞射峰幾乎消失不見。 進一步的TEM型態分析發現,當NYC含量達到20wt%時,在MPA4NYC1 及 MPA8NYC1 超薄切片樣品上發現了明顯延長、重疊長度接近700nm的clay矽酸鹽片層結構。 但當NYC含量低於20%,這些在MPANYC 超薄切片樣品上發現的clay矽酸鹽片層長度明顯隨其內NYC含量下降而下降。 上述MPANYC樣品阻隔性質改善的原因推測乃歸因於其明顯減少了自由體積性質(如Rf, Vf與Fv 數值)或被拉長的連續clay矽酸鹽片層結構。
最後,本文研究了脫氧塑膠的製備及其各種性能。三種脫氧塑膠分別以抗壞血酸(Vc)、鐵粉(Fe)、改性鐵粉(MFe)和抗壞血酸的混合物作為脫氧劑,選用具有高透氧性和高透水汽率的高分子材料EVA為基材。分別研究脫氧劑配方、用量對所製備脫氧塑膠脫氧與抗張性能的影響。 結果發現EFe 和EMFe系列樣品的抗張強度和斷裂伸長率比含相同重量脫氧劑成分的EVc系列樣品為高。另一方面,EVcMFe系列樣品的抗張強度和斷裂伸長率隨複合脫氧劑中Vc 含量的減少而明顯增大。進一步的脫氧性能測試結果清楚地表明,以經氯化鈉改性後的鐵粉作脫氧劑製備的脫氧膜的脫氧性能大大優於分別以相同重量的未經氯化鈉改性的鐵粉和Vc作脫氧劑製備的脫氧膜。將Vc和MFe混合物作為複合脫氧劑混入EVA中,當抗壞血酸與改性鐵粉的重量比為3/7至5/5之間時,EVcMFe 樣品的脫氧性能表現出特殊的增效效果。為了進一步研究這種增效效果產生的原因,用SEM和EDX對EVcMFe系列樣品中以各種比例抗壞血酸和改性鐵粉為脫氧劑的樣品作了結構分析。對EVcMFe系列樣品表面結構分析表明:當Vc與MFe的重量比在3/7至5/5之間時,改性鐵粉表面輕輕裹著一層抗壞血酸又沒有被抗壞血酸粉體過分包裹;而當Vc與MFe的重量比大於5/5時,在EVcMFe樣品中MFe幾乎被抗壞血酸粉體包裹。 此外還對EVc,、EFe、 EMFe 和 EVcMFe 系列樣品之所以產生上述有趣脫氧性質的機理進行了探討。另外,減小鐵粉粒徑,增加環境的濕度和溫度都有助於提高脫氧膜的脫氧速率。經貯存實驗顯示,脫氧膜確實可以減緩模擬食品中的油脂氧化。
Investigation of the gasoline permeation resistance of the as-blow-molded polypropylene, polypropylene / ethylene vinyl alcohol (PP/EVOH), polypropylene / modified polyamide (PP/MPA) and polypropylene / blends of modified polyamide and ethylene vinyl alcohol (PP/MPAEVOH) bottles. Investigation of the oxygen barrier and blending properties of the modified polyamide (MPA) and nylon 6 clay (NYC) blends (MPANYC) were also carried out in this study. Last but not least, the tensile and oxygen depletion properties of EVA resins blended with varying compositions of iron (Fe), modified iron (MFe) and/or ascorbic acid (Vc) oxygen scavengers were systematically investigated. The permeation resistance of gasoline improved dramatically after blending MPAEVOH barrier resins in PP matrices during blow molding processes. Surprisingly, by using proper compositions of MPAEVOH resins, the gasoline permeation rate of PP/MPA5EVOH1 bottles is only 0.025 g/day at 40°C, which is about 108 and 11 times slower than those of the PP and PP/MPA bottles, respectively. The oxygen permeation rate of the NYC film specimen is slightly lower than that of the MPA film specimen. After blending NYC in MPA, the oxygen barrier properties of the MPANYC film specimens are significantly better than those of the MPA and NYC film specimens. The oxygen permeation rates of MPANYC film specimens reduce significantly and reach the minimum as their NYC contents increase to 20 wt%. In fact, at 20 wt% optimum amount of NYC, the oxygen barrier improvement of MPA4NYC1 film specimen reach 105 time value, which is significantly better than those of other MPANYC film specimens and is at the same order of magnitude of barrier improvement as those of PVDC film specimens reported in the literature. Similar NYC content dependence was found on the plots of Rf, Vf,I3 and Fv values vs. the NYC contents of MPANYC specimens. The minimum Rf, Vf,I3 and Fv values of MPANYC specimens were always found as their NYC contents reach about 20 wt%. The X-ray diffraction properties suggest that MPA molecules are miscible with the nylon 6 molecules present in the NYC resin at any proportion, since the characteristic diffraction peaks of form PA crystals originally associated with the MPA resin almost disappear after blending varying amounts of NYC in MPA resins. Further morphological investigations found that demarcated structures of elongated and overlapped clay layers were found on the microtomed surfaces of MPANYC specimens as their NYC contents reach 20.0 wt. %, at which the lengths of the elongated and overlapped clay layers can reach about 700 nm. However, at NYC contents lower than 20.0 wt%, the lengths of these “elongated and overlapped” clay layers reduce significantly as the NYC contents continue to reduce. Presumably, the improved barrier properties of the MPANYC film specimens are mainly attributed to the reduced free volume properties (i.e. Rf, Vf and Fv values) and the elongated and continuous laminas of nanometer clays.
The tensile and oxygen depletion properties of EVA resins blended with varying compositions of iron, modified iron and ascorbic acid oxygen scavengers were systematically investigated. As expected, f and f values of EVc and EMFe series samples decrease significantly as their MFe and Vc contents increase, respectively. In contrast, EFe and EMFe series samples always exhibit significantly higher f and f values than EVc series samples filled with the same oxygen scavenger contents. Moreover, the f and f values of the EVcMFe series samples increase significantly as the Vc loadings present in the oxygen scavenger compounds decrease. Presumably, this is due to the fact that the volumes of the Fe and MFe powders are much smaller than those of the ascorbic acid powders with the same weight loadings, since the degree of “stress concentration” and “early breakage of EVA molecules” at the boundaries is expected to reduce as the volume loadings of the oxygen scavengers reduce. The oxygen depletion experiments clearly suggest that the oxygen depletion rates of modified iron powders filled EMFe series samples are much faster than those of EVc and EFe series samples filled with the same weight loadings of ascorbic acid and pure iron powders, respectively, wherein the EVc series samples exhibit slightly slower oxygen depletion rates than those of the corresponding EFe series samples. After blending Vc together with MFe oxygen scavenger compounds in the EVA resins, a “synergistic” effect on the oxygen depletion properties of the EVcMFe samples was observed when the weight ratios of Vc to MFe oxygen scavengers are between 3/7 to 5/5. In fact, the O2r values present in the airtight flask of EVc5MFe5 specimen at varying time are even lower than those of the EMFe10 specimen. However, at weight ratios of Vc to MFe higher than 5/5, the O2r values present in the airtight flask of EVc7MFe3 and EVc9MFe1 specimens at varying time are significantly higher than their theoretical O2r values estimated using “simple mixing rule”. Further SEM and EDX analysis of the compositions on the surfaces of EVcMFe series samples indicate that the ascorbic acid powders were found surrounding but not over-wrapping on the surfaces of the MFe powders as the weight ratios of Vc to MFe present in the EVcMFe specimens are between 3/7 and 5/5. On the other hand, the MFe powders found in the EVcMFe specimens were nearly wrapped by the ascorbic acid powders as the weight ratios of Vc to MFe are more than 5/5. Possible mechanisms account for these interesting oxygen depletion properties of EVc, EFe, EMFe and EVcMFe series samples are proposed.
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