- 學位論文
以熱接枝法製備馬來酸酐接枝澱粉之研究
The Preparation and Investigation of Maleic Anhydride Grafted Starch by Thermal Grafting Method
摘要
本研究利用熱接枝聚合反應將馬來酸酐接枝於樹薯澱粉上，實驗中以三種不同接枝反應時間(3小時、6小時、9小時)與不同濃度之馬來酸酐 (0wt%、1wt%、2 wt%、3 wt%)對樹薯澱粉進行熱接枝聚合反應。最後將其接枝澱粉(3w/6h-MAST)依照不同含量(4phr、8phr、12phr)添加於甘油中形成新塑化劑後，利用塑譜儀與澱粉混煉製備樣品。 藉由FTIR分析結果得知，於波數1700 cm-1至1720 cm-1之間出現一特徵峰，該特徵峰為C=O。從13C-NMR得知，3w/6h-MAST之圖譜發現兩特徵峰位於131 ppm以及166 ppm，131ppm為C=C鍵結；位於166 ppm則為-COO-。由FTIR以及13C-NMR分析可得到，馬來酸酐接枝於澱粉主鏈上。從XRD分析得知，藉由熱接枝反應，樹薯澱粉之結晶性遭受破壞，導致澱粉之特徵峰(15°、17°、18°、23°)消失，因此接枝澱粉的XRD圖譜中形成一非晶相之曲線。由SEM分析可知，樹薯澱粉的顆粒大小約10至20 μm，經由熱接枝後，由於結晶性受到破壞，澱粉形成平滑表面。從TGA得知，當熱裂解溫度400 ℃時，澱粉的熱重損失為80 %，當馬來酸酐添加3 wt%時，其熱重損失降低到60 %至70 %，這是因為馬來酸酐接枝於澱粉主鏈上，改變了澱粉之熱穩定性。拉伸試驗可知，當接枝澱粉與甘油混合形成一新塑化劑，與澱粉混煉時，當接枝澱粉含量達12phr時，澱粉混煉物之熔融指數從0.14 g/10 min提升至5.54 g/10 min應力值從0.85 MPa 提升至2.4 MPa。土壤掩埋六天後，澱粉混煉物(RST)重量損失約95 %，添加接枝澱粉，澱粉混煉物(MAST/RST)分解時間延長至八至十天，重量損失約95 %。
並列摘要
In this work, Maleic anhydride(MA) was grafted onto tapioca starch(MAST) by thermal grafting polymerization. The different contents of Maleic anhydride (0 wt%、1 wt%、2 wt%、3 wt%) reacted onto tapioca starch with the three kinds of reaction times (3h、6h、9h) by thermal grafting polymerization reaction. Finally, the different contents (4phr、8phr、12phr) of 3w/6h-MAST were mixed with glycerol to become new plasticizer that blended with starch (MAST/RST) in plasti-corder. The analysis by FTIR showed a new peak that at about 1700 cm-1 to 1720 cm-1 in the name of C=O. In the analysis by 13C-NMR, the pattern of 3w/6h-MAST was appeared two peaks at 131ppm and 166ppm. The 131ppm represented C=C and 166ppm represented -COO-. Consequently, the FTIR and 13C-NMR spectrum showed that Maleic anhydride was grafted onto the backbone of starch. In the XRD patterns, the crystalline of raw starch (RST) was decreased by thermal grafting polymerization reaction. The diffraction peaks (15°、17°、18°、23°) of starch was disappeared and turn into broad smoothly carve in the XRD patterns. In the SEM, tapioca starch was displayed as a grain size about diameter 10 to 20 μm. After thermal grafting process, the surface structure became a smoothly state. According to the TGA analysis, the weight loss of starch was about 80 % at about 400 ℃. But as 3 wt% of Maleic anhydride was added, the weight loss of sample was decreased 60 % to 70 %. Maleic anhydride was grafted onto backbone of starch and the thermal behavior of grafted starch was changed. In tensile strength measurement, as the content of new plasticizer was added till 12phr in the starch blend, the MFI for 12phr MAST/RST could be increased from 0.14 g/10 min to 5.54 g/10 min and the tensile strength could be increased from 0.85 MPa to 2.4 MPa. In Soil buried test, the weight loss of RST was over 95 % in soil at sit days. After added MAST into the MAST/RST, the weight loss of MAST/RST were over 95 % in soil about eight to ten days.
參考文獻
延伸閱讀
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