應用田口法於奈米纖維素混摻PU成膜物性之最佳化研究

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题名:	應用田口法於奈米纖維素混摻PU成膜物性之最佳化研究 Design of Optimal Factors for Nano Cellulose Mixed PU for Film-Forming by Taguchi Method
作者:	朱冠宇
贡献者:	化學工程與材料工程學系奈米材料碩士班
关键词:	奈米纖維素水性聚氨酯研磨法田口法主成分分析法 Nano cellulose Waterborne polyurethane Grinding method Taguchi method Principal component analysis
日期:	2021
上传时间:	2023-02-20 09:43:08 (UTC+8)
摘要:	本研究以連續式石臼物理研磨法對水熱及解纖處理後紙漿製備奈米纖維素。利用SEM觀察在研磨6小時後奈米纖維素平均寬度達到72.7nm；以FT-IR確認其分子構造；在沉降測試中研磨時間達5小時後奈米纖維素皆無發生沉降；纖維素經研磨處理後聚合度有顯著的下降，研磨達6小時後纖維已奈米化值為309；TGA測試中原料經前處理後Td50由288℃提升至315℃。利用二聚酸(DOA)、1,4-丁二醇(1,4-BG)製備軟鏈，並與聚己二酸乙二醇丁二醇酯(PEBA)、2,2-二羟甲基丙酸(DMPA)、4,4-二環己基甲烷二異氰酸酯(HMDI)，合成一系列陰離子水性聚氨酯。經FT-IR分析，NCO鍵最終趨近於0，表示合成順利成功，並探討其水溶液性質。合成之水性聚氨酯皆具有降低表面張力之能力、接觸角比純水大、低起泡性、對酸有較好緩衝能力、耐鹼穩定性佳。以合成之水性聚氨酯HEDT003作為基材，製備之奈米纖維素作為補強材，進行混摻製備不同奈米纖維素添加比例之複合薄膜。隨著奈米纖維素添加比例上升，光澤度下降、硬度上升、膨潤係數上升、重量保留率上升、熱性質上升、機械性能上升，當添加比例超過20%時，重量保留率、熱性質、機械性能皆有下降的趨勢。研究中利用田口方法規劃四個控制因子及三項水準之L9(34)直交表，並以拉伸強度、拉伸伸長率、重量保留率作為三個品質特性，探討在單一品質特性中各因子的最佳化參數組合，經由確認實驗證實所有品質特性中S/N比皆落在95%信賴區間內，表示實驗具有再現性及信賴度。研究最後使用主成分分析法，對於田口所選擇之品質特性，進行多品質特性分析，經分析結果得到多品質特性之參數組合為A3B2C2D3，而此組合之最大拉伸強度為18.545(kg/cm2)、最大伸長率為254.267%、重量保留率為99.1%。 In this study, Preparation of nanocellulose from pulp after hydrothermal method by using mortar physical grinding method. SEM observation showed that the average width was 72.7 nm after grinding for 6 hours. The molecular structure was confirmed by FTIR. In the settlement test, there was no settlement after grinding for 5 hours. A significant decrease in the degree of polymerization indicates that the fibers are nanofibers. In TGA test, the thermal properties of raw materials were improved after pretreatment. Synthesized a series of anionic waterborne polyurethanes by dimeric acid, 1,4-butanediol, polyether block amide, 2,2-Bis(hydroxymethyl)propionic acid and 4,4- hexamethylenediisocyanate. FT-IR analysis showed that NCO bond tended to be flat indicating that the synthesis was successful. In the aqueous solution test, waterborne polyurethane had the ability of reducing surface tension, larger contact angle than pure water, low foaming property, better buffering ability to acid and good alkali resistance. PU / CNF films with different proportion of nano cellulose were prepared by mixing the synthesized waterborne polyurethane HEDT003 as the matrix and nano cellulose as the reinforcements. With the increase of the proportion of nano cellulose, the gloss decreased, but the hardness, swelling coefficient, weight retention, thermal properties and mechanical properties increased. When the proportion of nano cellulose was more than 20%, the weight retention, thermal properties and mechanical properties decreased. Taguchi method is used to plan L9 (34) orthogonal table with four control factors and three levels. Using tensile strength, tensile elongation and weight retention as three quality characteristics. The optimal parameter combination of various factors in a single quality characteristic. Through confirmation experiments that the S / N ratio of all quality characteristics falls within the 95% confidence interval indicating that the experiment has reproducibility and reliability. Finally, principal component analysis was used to analyze the multi quality characteristics. The results showed that the parameter combination of multi quality characteristics is A3B2C2D3 . The maximum tensile strength is 18.545 (kg/cm2), the maximum elongation is 254.267%, and the weight retention rate is 99.1%.
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