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研究生:郭廸揚
研究生(外文):Dih-Yang Kuo
論文名稱:自稻殼原料生產纖維素與木質素之研究
論文名稱(外文):Production of Cellulose and Lignin from Rice Husks
指導教授:孫幸宜
口試委員:李思禹顧野松
口試日期:2017-06-20
學位類別:碩士
校院名稱:國立中興大學
系所名稱:化學工程學系所
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:2017
畢業學年度:105
語文別:中文
論文頁數:82
中文關鍵詞:稻殼纖維素木質素漂白處理
外文關鍵詞:Rice huskCelluloseLigninBleaching
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稻米佔臺灣主要糧食作物總量的75%之多,每年約會產生30萬公噸的稻殼。其中稻殼中含有的纖維素與木質素被廣泛應用於複合材料與環氧樹脂技術中,因此本研究利用農業廢棄物稻殼生產纖維素與木質素,來達到環保、無成本及廢棄物再利用的效果。本研究也為相關研究中少數同時探討並聯生產纖維素與木質素兩種物質之研究,從中找出快速的處理程序以及高純度的產物。將稻殼經過鹼(NaOH)處理以及亞氯酸鈉漂白處理,於121℃下以6MNaOH反應120分鐘,料液比為1g稻殼比30mL NaOH,並且漂白3次,得到純度91%的纖維素,其回收率為60.7% ;再將鹼處理後製造之鹼處理上清液(稻殼黑液)以乙醇沉澱法(使用50% H2SO4調整pH至5.5)分離半纖維素與其他雜質,最後加4% H2SO4至pH=2,使木質素沉澱,最終得到純度93.6%木質素,回收率為57.8% 。再以FTIR、SEM、TGA、XRD與ESCA探討研究生產之纖維素、木質素與文獻、商業產品的差別,結果顯示其性質、結構都與文獻及商業產品一致,除了XRD的結果顯示纖維素為型態Ⅰ及型態Ⅱ之組合。本研究最終提出了一種使用台灣主要的農業廢棄物得到高純度的纖維素與木質素之方法,純化的木質纖維素可以進一步反應,改質成具有功能性的天然高分子,可以得到廣大的應用。
Lignocelluloses (cellulose, hemicellulose, and lignin) are abundant in plants, and they are important materials widely used in diverse industries. Recovery and purification of lignocellulosic materials from non-food plant wastes are attracting more and more attention due to the benefits of cost efficiency and environmental sustainability. Since rice is the main grain cereal in Taiwan, a large quantity of rice husks (RH) is generated every year. Accordingly, this study focused on the purification of cellulose and lignin from these free lignocellulosic biomass. Via two parallel processes, high-purity cellulose and lignin could be produced concurrently from the same raw material. Based on 1 g RH, the optimum conditions for the production of 91.7 wt% cellulose are the alkali treatment using 30 mL of 6 M NaOH at 121°C for 120 min, followed by sequential NaClO2 bleaching in three times. In the parallel process, lignin was isolated from the supernatant obtained after NaOH treatment via ethanol precipitation (adjusting pH to 5.5 by 50% H2SO4 and mixing in a 3-fold volume of 95% ethanol, to remove the precipitate of hemicellulose) and acid precipitation (adjusting the pH of the above supernatant to 2 by 4% H2SO4, to get the precipitate of lignin). The purity of lignin was 92.7 wt% for RH raw material. The purified lignocellulosic products were then characterized by SEM, FTIR, TGA,XRD, and ESCA. Their properties and structures are consistent with commercial products, except that cellulose is a combination of type І and type ?, indicated from the XRD results. In summary, this study presents a promising approach to produce high-purity cellulose and lignin from the popular agricultural wastes in Taiwan, RH. The purified lignocelluloses could be further reacted and modified into functional materials for versatile applications.
目錄
誌謝 け
中文摘要 げ
英文摘要 こ
目錄 ざ
表目錄 し
圖目錄 じ
第一章 緒論 …1
1.1前言 1
1.2研究動機 1
1.3研究目的 2
第二章 文獻回顧 5
2.1木質纖維素簡介 5
2.2纖維素簡介 5
2.3半纖維素簡介 5
2.4木質素簡介 10
2.5木質纖維素之前處理 10
2.5.1物理性前處理 14
2.5.2化學性前處理 14
2.6提取纖維素之方法 14
2.7提取木質素之方法 17
2.8提高酸沉澱木質素純度方法 19
第三章 材料與方法 20
3.1研究架構 20
3.2實驗材料與儀器 20
3.2.1材料 20
3.2.2實驗儀器與設備 20
3.3分析方法 22
3.3.1稻殼成分分析 22
3.3.2葡萄糖、木糖、阿拉伯糖、半乳糖、甘露糖之定性及定量分析 .26
3.3.3鹼處理製備纖維素方法 32
3.3.4亞氯酸鈉處理(漂白處理). 32
3.3.5乙醇沉澱方法 32
3.3.6酸沉澱方法 32
3.4性質分析 33
3.4.1場發射掃描式電子顯微鏡 33
3.4.2傅立葉轉換紅外線光譜儀 33
3.4.3熱重量分析儀 34
3.4.4高解析X光繞射儀 34
3.4.5化學分析電子能譜儀 34
第四章 結果與討論 35
4.1稻殼與商業纖維素、木質素之組成成分 35
4.2鹼處理稻殼之效果 35
4.2.1鹼處理之濃度影響 35
4.2.2鹼處理之反應時間影響 35
4.3亞氯酸鈉漂白處理稻殼之結果 42
4.3.1漂白次數對纖維素純度之影響 42
4.4乙醇沉澱半纖維素結果 42
4.5酸沉澱木質素結果 48
4.5.1木質素酸沉澱結果 48
4.6纖維素與木質素回收率結果 48
4.7纖維素產物之特性分析 51
4.7.1纖維素之FTIR分析結果 51
4.7.2纖維素之TGA分析結果 51
4.7.3纖維素之SEM分析結果 55
4.7.4纖維素之XRD分析結果 57
4.7.5纖維素之ESCA分析結果 57
4.8木質素產物之特性分析 61
4.8.1木質素之FTIR分析結果 61
4.8.2木質素之TGA分析結果 61
4.8.3木質素之SEM分析結果 65
4.8.4木質素之之XRD分析結果 65
4.8.5木質素之ESCA分析結果 65
4.8.6木質素之GPC分析結果 65
4.9生產成本 72
第五章 結論與建議 74
5.1結論 74
5.2建議 74
參考文獻 76
附錄 78
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