节点文献
离子液体处理稻杆制备还原糖及其回收的研究
Preparation of Reducing Sugar Using Rice Straw Pretreated by Ionic Liquid and the Recycle of the Ionic Liquid
【作者】 李莹莹;
【导师】 巩桂芬;
【作者基本信息】 哈尔滨理工大学 , 材料学, 2013, 硕士
【摘要】 当今人类社会面临着资源短缺和环境问题的双重挑战,生物质能源因其原料资源潜力大、成本低等优点备受关注。生物质产业的主要功能是替代化石能源、保护环境、促进农村经济发展。中国水稻产量长居世界第一,有着丰富的储备资源。从经济价值、环境保护、新能源等角度出发,本文采用离子液体对稻杆进行预处理,利用处理后的纤维素与纤维素酶的作用制备还原糖,并对离子液体进行回收,再用回收后的离子液体处理稻杆,考察回收后离子液体的性能。本实验合成离子液体1-烯丙基-3-甲基咪唑氯盐([AMIM]Cl),通过FT-IR和1HNMR谱图的分析确定合成物质为目标产物[AMIM]Cl。用[AMIM]Cl溶解稻杆纤维素,通过对固液比、温度、溶解时间等因素的影响进行研究,探讨了离子液体溶解稻杆纤维素的机理,得出最佳溶解参数:固液比1:9,温度110℃,时间2h。采用减压蒸馏回收废液中的离子液体[AMIM]Cl,回收率可达90%。通过FT-IR和1HNMR鉴定回收离子液体结构仍为[AMIM]Cl;使用1-5次的离子液体[AMIM]Cl处理纤维素的还原糖转化率由82.08%降低到44.44%(未处理的稻杆还原糖转化率为31.94%),离子液体回收率由90%下降到25.32%;通过SEM观察再生纤维素的微观形貌发现,随离子液体使用次数增加,对纤维素的破坏程度会降低。回收离子液体过程中分离出的残渣,是导致回收率下降的关键因素。采用SEM、FT-IR、X射线光电子能谱(XPS)对残渣进行分析:通过对外观形貌分析确定了残渣中稻杆的存在;FT-IR测定出[AMIM]Cl的存在;对XPS测定出的С1s、O1s、N1s、Cl2p能谱分析,验证残渣是稻杆和离子液体[AMIM]Cl的混合物。
【Abstract】 Nowadays, we face with the challenges of the shortage of resources and theissues of environment. Much attention has been paid to biological energy source(BER), owning to its advantages of its great potentiality of raw material and lowcost and so on. The main function of the BER is an alternative to fossil energy,protecting the environment and promoting rural economic development. Chineserice production is the first place in the world, with a wealth of reserve resources.From the perspective as the economic value, environmental protection, and newenergy, we adopt ionic liquid in the pretreatment of straw and utilize processedcellulose and cellulase to prepare the reducing sugar. Then the recycled ionicliquid is utilized in the processing of straw to study the performance of therecycled ionic liquid.In the experiment, we have prepared the [AMM]Cl, and its structure wasdetermined through FT-IR and1HNMR. Rice straw cellulose was dissolved in theionic liquids, then the mechanism of the process was investigated by studying theinfluence factors (the ratio of solid-liquid, temperature, and dissolving time).Then the most appropriate parameters of solution were obtained: the ratio ofsolid-liquid is1:9,110℃and2hours.The recovery of the waste ionic liquid [AMIM]Cl reached90%through themethod of the reduced pressure distillation. The structure of [AMIM]Cl was notchanged after recovery by FT-IR and1HNMR spectrum analysis. The [AMIM]Clwas used5time, the reducing sugar conversion rate reduces from82.08%to44.44%(the reducing sugar conversion rate of the untreated straw is31.94%),and the ionic liquid recovery rate decreases reduces from90%to25.32%.Through the SEM observation of the regenerated cellulose’s microstructure, we found, the damage for cellulose will be weakened with used times of ionicliquids increasing.The residues, what was separated after recycle of [AMIM]Cl, is the keyfactors in the decline of recycle rate. The mixture components are analyzed usingthese methods (SEM, FT-IR and XPS). The mixture contains straw by theanalysis of the morphology; It proved that there is [AMIM]Cl in the residues byFT-IR and C1s, O1s, N1s and Cl2p determined by XPS. The residues is mixtureof straw and [AMIM]Cl.
【Key words】 Ionic liquid; synthesization; straw cellulose; reducing sugar; recycle;