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研究生:張朕杰
研究生(外文):chang chen chieh
論文名稱:纖維素觸媒酯化之探討
論文名稱(外文):study on the catalytic esterification of cellulose
指導教授:吳文海
指導教授(外文):Wu Wen Hai
學位類別:碩士
校院名稱:南台科技大學
系所名稱:化學工程與材枓工程系
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2010
畢業學年度:98
語文別:中文
論文頁數:63
中文關鍵詞:醋酸纖維素取代度
外文關鍵詞:cellulose acetatedegree of substitution
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本次研究係以棉花(cotton)為原料經由酯化反應,合成醋酸纖維素,再進行反應時間、反應溫度、觸媒量、混合觸媒對醋酸化程度(degree of acetylation)、取代度(degree of substitution,DS)和分子量(molecular weight)的探討。先以傅立葉轉換式紅外光譜儀(FT-IR)和核磁共振光譜儀(NMR)進行醋酸纖維素的結構鑑定,再以化學滴定法與膠體滲透層析儀(GPC)進行取代度和分子量之變化探討。
從實驗結果可知,當反應溫度改變時,若反應器瓶口為密閉,則醋酸化程度及取代度會隨反應溫度上升而增加,分子量則會減少;若反應器瓶口為開放,則醋酸化程度、取代度及分子量皆會隨反應溫度上升而下降。當反應時間改變時,若反應器瓶口為密閉,則醋酸化程度及取代度會隨反應時間增加而增加,分子量會減少;若反應器瓶口為開放,醋酸化程度、取代度及分子量皆會隨反應時間增加而下降。
當觸媒量增加,醋酸化程度、取代度會隨著觸媒量的增加而增加,分子量則會漸少。反應時加入氯仿,可以發現產品的分子量及取代度值會比沒加氯仿來的高,品質比較好且雜質較少。棉花經過不同的前處理方式,產品的色澤也會有所不同,以色澤來看,產品顏色的白晰度為:前處理方式C>前處理方式B>前處理方式A。

分子量分佈控制效果會隨著選擇的溶劑不同而有不同的效果,在本次實驗中,分子量分佈控制效果由高到低的排列為:80%冰醋酸>25%冰醋酸>丙酮。紙漿前處理發現,經過強鹼前處理後,前處理方式C的色澤會白許多,而與棉花前處理相比,會因紙漿中所含木質素較多,經過前處理後仍未完全清除,故在外觀上會比棉花前處理方式C來的黃許多。
In this study, the cotton as the raw material compound was synthesized by the esterification to cellulose acetate, and we investigated the reaction time, reaction temperature, catalyst volume, catalyst type on the degree of acetylation, degree of substitution, and molecular weight. The result was analyzed by fourier transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance spectroscopy (NMR) for structural identification of cellulose acetate and the chemical titration method and gel penetration chromatography (GPC) for studying the degree of substitution and molecular weight.
The experimental results have found that the degree of acetylation, degree of substitution and molecular weight were various on the different reaction temperature, reaction time, catalyst volume, and reaction conditions. When changing the reaction temperature, reaction time and the closed-type reactor, the degree of acetylation and degree of substitution were increasing when the reaction time or temperature increased, and molecular weight was decreasing when the reaction temperature increased; however, if the reaction temperature, reaction time and open-type reactor, the degree of acetylation and degree of substitution were decreasing when the reaction time or temperature increased. When changing the catalyst volume, the degree of acetylation and degree of substitution were increasing when catalyst volume increased, and the degree of substitution was slightly increasing when the reaction time increased.

The product have the better quality and less impurities when added the chloroform during the reaction, but the molecular weight and the degree of substitution were lower without chloroform. The cotton have various preprocessing, and the color also have different. Comparing the white color degrees of products were: preprocessing C > preprocessing B > preprocessing A.
Controlling the efficiency of molecular weight contribution was changed with different solvent. In this study, comparing the control of the efficiency of molecular weight contribution were: 80 % glacial acetic acid > 25 % glacial acetic acid > acetone. For the pulp preprocessing, the preprocessing C was more whiteness after the alkali treatment. Compare with preprocessing of the cotton, the pulp contain more lignin, and it was hardly purge after the pre-treatment, so the appearance was more yellowish to the preprocessing C.
摘 要…..…………………....……………...…………………I
英 文 摘 要…...……………………………………………………II
目 次……………………………..…………………………IV
表 目 錄………………………………………………..………VI
圖 目 錄………………………………………….……………VII
第一章 緒 論…………………………………………………………1
1.1 前言......................................................................................1
1.2 纖維之發展與種類...…..........……........….………………3
1.3 棉花....................................................................................13
1.4 纖維素................................................................................18
1.5 醋酸纖維素........................................................................28
第二章 實 驗......................................................................................34
2.1 實驗設備............................................................................34
2.2 實驗藥品............................................................................35
2.3 實驗架構............................................................................36
2.4 分析方法............................................................................37
第三章 結果與討論................................................................................38
3.1 產物結構鑑定....................................................................38
3.2 反應溫度影響之探討........................................................41
3.3 反應時間影響之探討........................................................44
3.4 觸媒量影響之探討............................................................49
3.5 氯仿影響之探討…………................................................51
3.6 前處理影響之探討............................................................53
3.7 分子量分佈控制之探討....................................................55
3.8 紙漿為原料之探討............................................................57
第四章 結 論......................................................................................59
參考文獻..................................................................................................61
附件一…………………………………………………………….…….63
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