蔗渣及其纤维素在离子液体中的溶解、改性及分离的研究
摘要
随着石油危机和石油化工原料价格的持续上涨,以及人类对环境和健康等问题的日益重视,可再生资源的开发越来越引起了人们的重视。蔗渣是一种典型的农林废弃物,是由甘蔗经制糖压榨后产生的纤维性残渣。通常蔗渣中含有40-50%的纤维素、20-25%的半纤维素和18-24%的木质素。蔗渣及其纤维素具有很多优点,如可再生、易生物降解、对环境友好等特点。然而由于蔗渣等木质纤维难溶于水和常见的有机溶剂,对其开发应用有一定的限制。离子液体具有良好的溶解性能,可以有效的溶解纤维素,这为纤维素的开发和应用提供了一个崭新的平台。本论文以蔗渣及其纤维素为原料,以离子液体为溶剂,针对蔗渣在新型溶剂中转化利用的一系列关键问题,研究了蔗渣及其纤维素在离子液体中的溶解和改性以及蔗渣主要组分在离子液体中的分离。此外,还对离子液体中由蔗渣直接制备机械性能强的纤维进行了探讨。通过研究,得到的主要结论如下:
1.探讨了蔗渣纤维素在离子液体1-丁基-3-甲基咪唑氯盐([C4mim]Cl)中溶解前后物化性能的变化。经研究发现,由于纤维素的聚合度高,在普通加热条件下蔗渣纤维素在离子液体中溶解需要较长的时间(100℃,10h)。在溶解的过程中,蔗渣纤维素没有发生衍生化反应,但是纤维素的结晶区被破坏。再生后,纤维素的聚合度由1278降低到916,初始热解温度由240℃降低到215℃。
2.提出一种快速溶解蔗渣全组分的方法。在普通加热情况下,蔗渣全组分在离子液体[C4mim]Cl中完全溶解需要24h。当溶解温度超过木质素的玻璃转化温度时,蔗渣完全溶解时间可以缩短至2.5h。红外光谱(FT-IR)和固体核磁共振(CP/MAS13C-NMR)分析表明,离子液体[C4mim]Cl只起到溶解作用,蔗渣在离子液体中没有发生衍生化反应。此外还发现,蔗渣在溶解过程中纤维素晶型由纤维素I型转变为纤维素II型,且蔗渣经离子液体溶解再生后乙酰基含量降低。热分析结果表明再生后蔗渣的热稳定性能略有提高,初始热解温度由205℃提高到217℃。
3.以蔗渣纤维素为原料,以4-二甲氨基吡啶(DMAP)为催化剂,在离子液体[C4mim]Cl中制备了一系列高取代度的丁二酰化纤维素和邻苯二甲酰化纤维素。研究发现,当DMAP用量为5%、反应温度为100℃、反应时间为60min时,丁二酰化纤维素取代度最高,为2.34。当DMAP用量为5%、反应温度为80℃、反应时间为60min,邻苯二甲酰化纤维素取代度最高,为1.31。研究还发现,纤维素C2、C3和C6位上的游离羟基均发生了化学反应,其中C6位羟基的反应活性最强。热分析结果表明纤维素衍生物的热稳定性能略有降低。
4.提出了一种在离子液体[C4mim]Cl中制备乙酰化蔗渣的方法。以纯化的N-甲基咪唑和正氯丁烷为原料合成了离子液体[C4mim]Cl,并以合成的离子液体为反应介质,系统地研究了乙酸酐用量、反应温度和反应时间对蔗渣乙酰化产率的影响。结果发现蔗渣均相乙酰化产率随着乙酸酐用量的增加而提高;当反应时间从30min延长到60min时,蔗渣的乙酰化产率也相应的提高;在80-100℃,温度对蔗渣的乙酰化反应影响不大;但是当温度高于110℃时,产物的产率急剧下降。热分析结果表明改性后的蔗渣热稳定性能良好(198℃),吸湿性下降,从蔗渣的5%降低到2%。
5.对蔗渣在离子液体1-乙基-3-甲基咪唑醋酸盐([C2mim]OAc)中的均相溶解及组分分离进行了研究。研究发现,不同的加热方法包括高温快速溶解、低温长时间溶解和微波溶解均可使蔗渣溶解在离子液体[C2mim]OAc中,并可以通过水/丙酮实现纤维物质和木质素的分离。随着溶解温度和溶解时间的延长,回收木质素的产率提高,纤维物质的产率下降,但是纤维物质中木质素的含量也下降。与低温长时间溶解相比,高温快速溶解可以显著提高木质素的去除率,得到低木质素含量的蔗渣纤维物质。微波溶解分离后纤维物质的得率低、木质素含量高,直接导致碳水化合物产率低。此外,可以用液体核磁对蔗渣和纤维物质进行表征。同时发现在离子液体[C2mim]OAc中,蔗渣经高温快速溶解和微波溶解分离后的纤维物质发生了微量的乙酰化反应。
6.对在离子液体中分离蔗渣纤维素和半纤维素进行了研究。以离子液体和氢氧化钠为试剂,可以将离子液体中溶解的蔗渣组分纤维素和半纤维素进行分离。采用离子色谱、FT-IR和核磁共振表征了蔗渣纤维素和半纤维素的结构。结果表明,离子液体[C2mim]OAc和[C4mim]Cl分离的蔗渣纤维素中葡萄糖的含量分别为76.61%和63.05%,还含少量的木糖等半纤维素组成成分;基本不含有木质素。用离子液体[C2mim]OAc和[C4mim]Cl分离的蔗渣半纤维素主要成分为木糖(74.99%和72.79%)、阿拉伯糖(13.54%和13.34%)、葡萄糖(8.82%和11.28%),还含有少量的半乳糖和葡萄糖醛酸;两种半纤维素的结构主要为L-阿拉伯糖-(4-O-甲基-D-葡萄糖醛酸)-D-木聚糖。TGA分析表明,分离得到的纤维素热稳定性略有降低,半纤维素热稳定性与碱溶性半纤维素相当。
7.探讨了以蔗渣、橡木粉和松木粉为原料,直接在离子液体[C2mim]OAc中制备生物质纤维的新方法。研究发现,在离子液体[C2mim]OAc中采用低温长时间溶解制备的纺丝液,只有蔗渣可以得到连续均匀的纤维;而在离子液体[C2mim]OAc中采用高温快速溶解制备的纺丝液,蔗渣、橡木粉和松木粉均可得到纤维。纤维机械性能研究表明,高温快速法制备的蔗渣纤维机械强度要好于低温长时间制备的蔗渣纤维。在三种原料中,蔗渣纤维的机械强度性能最好,应力为125MPa;橡木纤维次之,为102MPa,机械强度也较高;而松木纤维的强度较差,仅为49MPa。此外,两种升温方法制备的蔗渣纤维的结晶形态均发生了变化,由纤维素I型变为纤维素II型结构。
With the impact of fossil fuels depletion and environmental concerns, the developmentof renewable resources has attracted more and more attention. Bagasse is a typicalagricultural and forestry waste, which derives from sugar cane and is the fibrous residue aftercrushing to remove sugar from sugar cane stalks. Generally, bagasse is composed of 40-50%cellulose, 20-25% hemicelluloses and 18-24% lignin. Bagasse and bagasse cellulose havemany advantageous properties, such as sustainable, renewable, biodegradable andenvironmentally friendly. However, bagasse or bagasse cellulose is insoluble in water orcommon organic solvent. This limits the application and exploitation of the biomass. Ionicliquids have been providing a new platform for utilization of cellulose due to their excellentdissolution capacity for cellulose. In this study, the dissolution and modification of bagasseand bagasse cellulose were investigated, and the isolation of cellulose and hemicellulosesfrom bagasse was also explored using ionic liquids as solvents. Moreover, the preparation ofbagasse fibers was discussed in ionic liquid without removal of hemicelluloses and lignin.The primary results are described as follows:
1. The physicochemical properties of native bagasse cellulose and the regenerated oneafter dissolution in ionic liquid 1-butyl-3-methylimidazolium chloride ([C4mim]Cl) werecomparatively studied. The results indicated that it took a long time (over 10 h at 100 oC) tocompletely dissolve cellulose in ionic liquid due to the high degree of polymerization (DP) ofbagasse cellulose. Ionic liquid was the direct solvent of cellulose, and there were noderivatization of cellulose occurred with ionic liquid. However, the crystallinity of cellulosewas destroyed. The DP of the regenerated cellulose decreased from 1278 to 916, and thedecomposition temperature of the regenerated cellulose decreased from 240 oC to 215 oC ascompared to the native bagasse cellulose.
2. Rapid dissolution of bagasse in ionic liquid was proposed at higher temperature. Atthe dissolution temperature above the glass transition temperature of lignin, bagasse could becompletely dissolved in ionic liquid within 2.5 h. However, it took over 24 h to be completelydissolved in the same ionic liquid at lower temperature (100 oC). The results of fourier transform infrared (FT-IR) and solid-state cross-polarization magic angle spinning carbon-13unclear magnetic resonance (CP/MAS 13C-NMR) spectroscopies indicated that [C4mim]Clwas a direct solvent for bagasse. However, the crystallite alignment of cellulose in theregenerated bagasse was converted from cellulose I to cellulose II, and the content of acetylgroup in regenerated bagasse decreased. The regenerated bagasse was more thermally stablethan original bagasse and the decomposition temperature of the regenerated bagasse increasedfrom 205 oC to 217 oC.
3. Succinylation and phthalylation of bagasse cellulose were investigated in ionic liquid[C4mim]Cl using 4-dimethylaminopyridine (DMAP) as a catalyst to produce cellulosederivatives with high degree of substitution (DS). The effects of the dose of catalyst (DMAP),reaction time and reaction temperature on DS of the cellulose derivatives were investigated.The results indicated that the highest DS of succinylated cellulose, 2.34, was obtained at 100oC for 60 min with 5% DMAP, and that of phthalylated cellulose, 1.31, was reached at 80 oCfor 60 min with 5% DMAP. The acylation of three hydroxyl groups at the C6, C2 and C3 incellulose does occur, primarily at C6. The cellulose derivatives showed a lowerdecomposition temperature.
4. Homogeneous acetylation of bagasse was accomplished in ionic liquid [C4mim]Cl.[C4mim]Cl was successfully synthesized using N-methylimidazole and chlorobutane asstarting materials. Using the synthesized [C4mim]Cl as solvent, the effects of the parametersincluding the concentration of the acetic anhydride, reaction time and reaction temperature onweight percent gain (WPG) value of acetylated bagasse were studied. The results indicatedthat the WPG value increased with the increase of DMAP. 60 min was the preferred reactiontime due to the highest WPG of the product. Reaction temperature has few effect on the WPGvalue of the product in the range of 80-100 oC. However, the WPG value significantlydecreased above 110 oC due to the degradation of cellulose and hemicelluloses. All thehydroxyl groups in cellulose, hemicelluloses and lignin could be reacted with aceticanhydride. The TGA analysis indicated that acetylated bagasse was stable up to 198 oC andthe hygroscopicity of the product decreased from 5% to 2%.
5. The dissolution of bagasse and isolation of bagasse components were carried out inionic liquid 1-ethyl-3-methylimidazolium acetate ([C2mim]OAc). It was found that bagasse could be completely dissolved in ionic liquid using different heating methods, includinghigher temperature/shorter time, lower temperature/longer time and microwave irradiation.After the dissolution, the cellulosic materials and lignin could be isolated from bagasse byreconstitution in water/acetone. Increasing dissolution temperature and dissolution time led toan increase in the recovered lignin yield, however, the lower cellulosic material yield withlower lignin content was also obtained. Compared to dissolution at lower temperature/longertime, dissolution of bagasse in [C2mim]OAc at higher temperature/shorter time resulted inhigher delignification and lower lignin content in cellulosic material. The lower yield ofcellulosic material with higher lignin content was obtained by microwave assisted dissolution,which directly resulted in lower yield of carbohydrates. More importantly, the cellulosicmaterials and bagasse could be characterized by liquid 13C-NMR using the ionic liquid assolvent. Moreover, the side reaction (acetylation) occurred using the microwave irradiationmethod or higher temperature/shorter time method.
6. A new method for the isolation of cellulose and hemicelluloses from bagasse usingionic liquid/NaOH was proposed. Ion chromatography, FT-IR, TGA and NMR were used tocharacterize the physicochemical properties of the isolated cellulose and hemicelluloses. Theresults indicated that cellulose samples isolated from [C2mim]OAc/NaOH or[C4mim]Cl/NaOH system mainly contained glucose (76.61% and 63.05%, respectively) witha small amount of xylose, which represents hemicelluloses. The isolated cellulose samplescontained very few lignin. The major monosaccharide in hemicelluloses samples isolatedfrom [C2mim]OAc/NaOH or [C4mim]Cl/NaOH system were xylose (74.99% and 72.79%,respectively), arabinose (13.54% and 13.34%, respectively) and glucose (8.82% and 11.28%,respectively). Galactose and glucuronic acid were observed as minor constituents. Thethermal stability of the hemicelluloses samples was similar to the alkaline hemicelluloses.NMR results implied that the isolated hemicelluloses samples can be structurally defined asL-arabino-(4-O-methyl-D-glucurono)-D-xylan.
7. A new method to prepare biomass fibers directly from bagasse, oak or pine withoutthe removal of hemicelluloses and lignin was presented using ionic liquid as a solvent. Thebagasse fibers could be prepared using either the lower temperature/longer time or higher temperature/shorter time method, while oak and pine fibers can only be prepared using thehigher temperature/shorter time method. The bagasse fibers made with the highertemperature/shorter time method have higher tensile strength compared to those made withlower temperature/longer time method. Fibers with higher tensile strength were obtainedfrom biomass with higher cellulose content, and the fibers made from bagasse (125 MPa) andoak (102 MPa) exhibited higher tensile strength than those from pine (49 MPa). The XRDresults indicated that the crystalline structure of bagasse fiber was transformed from celluloseI in native bagasse to cellulose II.
1.探讨了蔗渣纤维素在离子液体1-丁基-3-甲基咪唑氯盐([C4mim]Cl)中溶解前后物化性能的变化。经研究发现,由于纤维素的聚合度高,在普通加热条件下蔗渣纤维素在离子液体中溶解需要较长的时间(100℃,10h)。在溶解的过程中,蔗渣纤维素没有发生衍生化反应,但是纤维素的结晶区被破坏。再生后,纤维素的聚合度由1278降低到916,初始热解温度由240℃降低到215℃。
2.提出一种快速溶解蔗渣全组分的方法。在普通加热情况下,蔗渣全组分在离子液体[C4mim]Cl中完全溶解需要24h。当溶解温度超过木质素的玻璃转化温度时,蔗渣完全溶解时间可以缩短至2.5h。红外光谱(FT-IR)和固体核磁共振(CP/MAS13C-NMR)分析表明,离子液体[C4mim]Cl只起到溶解作用,蔗渣在离子液体中没有发生衍生化反应。此外还发现,蔗渣在溶解过程中纤维素晶型由纤维素I型转变为纤维素II型,且蔗渣经离子液体溶解再生后乙酰基含量降低。热分析结果表明再生后蔗渣的热稳定性能略有提高,初始热解温度由205℃提高到217℃。
3.以蔗渣纤维素为原料,以4-二甲氨基吡啶(DMAP)为催化剂,在离子液体[C4mim]Cl中制备了一系列高取代度的丁二酰化纤维素和邻苯二甲酰化纤维素。研究发现,当DMAP用量为5%、反应温度为100℃、反应时间为60min时,丁二酰化纤维素取代度最高,为2.34。当DMAP用量为5%、反应温度为80℃、反应时间为60min,邻苯二甲酰化纤维素取代度最高,为1.31。研究还发现,纤维素C2、C3和C6位上的游离羟基均发生了化学反应,其中C6位羟基的反应活性最强。热分析结果表明纤维素衍生物的热稳定性能略有降低。
4.提出了一种在离子液体[C4mim]Cl中制备乙酰化蔗渣的方法。以纯化的N-甲基咪唑和正氯丁烷为原料合成了离子液体[C4mim]Cl,并以合成的离子液体为反应介质,系统地研究了乙酸酐用量、反应温度和反应时间对蔗渣乙酰化产率的影响。结果发现蔗渣均相乙酰化产率随着乙酸酐用量的增加而提高;当反应时间从30min延长到60min时,蔗渣的乙酰化产率也相应的提高;在80-100℃,温度对蔗渣的乙酰化反应影响不大;但是当温度高于110℃时,产物的产率急剧下降。热分析结果表明改性后的蔗渣热稳定性能良好(198℃),吸湿性下降,从蔗渣的5%降低到2%。
5.对蔗渣在离子液体1-乙基-3-甲基咪唑醋酸盐([C2mim]OAc)中的均相溶解及组分分离进行了研究。研究发现,不同的加热方法包括高温快速溶解、低温长时间溶解和微波溶解均可使蔗渣溶解在离子液体[C2mim]OAc中,并可以通过水/丙酮实现纤维物质和木质素的分离。随着溶解温度和溶解时间的延长,回收木质素的产率提高,纤维物质的产率下降,但是纤维物质中木质素的含量也下降。与低温长时间溶解相比,高温快速溶解可以显著提高木质素的去除率,得到低木质素含量的蔗渣纤维物质。微波溶解分离后纤维物质的得率低、木质素含量高,直接导致碳水化合物产率低。此外,可以用液体核磁对蔗渣和纤维物质进行表征。同时发现在离子液体[C2mim]OAc中,蔗渣经高温快速溶解和微波溶解分离后的纤维物质发生了微量的乙酰化反应。
6.对在离子液体中分离蔗渣纤维素和半纤维素进行了研究。以离子液体和氢氧化钠为试剂,可以将离子液体中溶解的蔗渣组分纤维素和半纤维素进行分离。采用离子色谱、FT-IR和核磁共振表征了蔗渣纤维素和半纤维素的结构。结果表明,离子液体[C2mim]OAc和[C4mim]Cl分离的蔗渣纤维素中葡萄糖的含量分别为76.61%和63.05%,还含少量的木糖等半纤维素组成成分;基本不含有木质素。用离子液体[C2mim]OAc和[C4mim]Cl分离的蔗渣半纤维素主要成分为木糖(74.99%和72.79%)、阿拉伯糖(13.54%和13.34%)、葡萄糖(8.82%和11.28%),还含有少量的半乳糖和葡萄糖醛酸;两种半纤维素的结构主要为L-阿拉伯糖-(4-O-甲基-D-葡萄糖醛酸)-D-木聚糖。TGA分析表明,分离得到的纤维素热稳定性略有降低,半纤维素热稳定性与碱溶性半纤维素相当。
7.探讨了以蔗渣、橡木粉和松木粉为原料,直接在离子液体[C2mim]OAc中制备生物质纤维的新方法。研究发现,在离子液体[C2mim]OAc中采用低温长时间溶解制备的纺丝液,只有蔗渣可以得到连续均匀的纤维;而在离子液体[C2mim]OAc中采用高温快速溶解制备的纺丝液,蔗渣、橡木粉和松木粉均可得到纤维。纤维机械性能研究表明,高温快速法制备的蔗渣纤维机械强度要好于低温长时间制备的蔗渣纤维。在三种原料中,蔗渣纤维的机械强度性能最好,应力为125MPa;橡木纤维次之,为102MPa,机械强度也较高;而松木纤维的强度较差,仅为49MPa。此外,两种升温方法制备的蔗渣纤维的结晶形态均发生了变化,由纤维素I型变为纤维素II型结构。
With the impact of fossil fuels depletion and environmental concerns, the developmentof renewable resources has attracted more and more attention. Bagasse is a typicalagricultural and forestry waste, which derives from sugar cane and is the fibrous residue aftercrushing to remove sugar from sugar cane stalks. Generally, bagasse is composed of 40-50%cellulose, 20-25% hemicelluloses and 18-24% lignin. Bagasse and bagasse cellulose havemany advantageous properties, such as sustainable, renewable, biodegradable andenvironmentally friendly. However, bagasse or bagasse cellulose is insoluble in water orcommon organic solvent. This limits the application and exploitation of the biomass. Ionicliquids have been providing a new platform for utilization of cellulose due to their excellentdissolution capacity for cellulose. In this study, the dissolution and modification of bagasseand bagasse cellulose were investigated, and the isolation of cellulose and hemicellulosesfrom bagasse was also explored using ionic liquids as solvents. Moreover, the preparation ofbagasse fibers was discussed in ionic liquid without removal of hemicelluloses and lignin.The primary results are described as follows:
1. The physicochemical properties of native bagasse cellulose and the regenerated oneafter dissolution in ionic liquid 1-butyl-3-methylimidazolium chloride ([C4mim]Cl) werecomparatively studied. The results indicated that it took a long time (over 10 h at 100 oC) tocompletely dissolve cellulose in ionic liquid due to the high degree of polymerization (DP) ofbagasse cellulose. Ionic liquid was the direct solvent of cellulose, and there were noderivatization of cellulose occurred with ionic liquid. However, the crystallinity of cellulosewas destroyed. The DP of the regenerated cellulose decreased from 1278 to 916, and thedecomposition temperature of the regenerated cellulose decreased from 240 oC to 215 oC ascompared to the native bagasse cellulose.
2. Rapid dissolution of bagasse in ionic liquid was proposed at higher temperature. Atthe dissolution temperature above the glass transition temperature of lignin, bagasse could becompletely dissolved in ionic liquid within 2.5 h. However, it took over 24 h to be completelydissolved in the same ionic liquid at lower temperature (100 oC). The results of fourier transform infrared (FT-IR) and solid-state cross-polarization magic angle spinning carbon-13unclear magnetic resonance (CP/MAS 13C-NMR) spectroscopies indicated that [C4mim]Clwas a direct solvent for bagasse. However, the crystallite alignment of cellulose in theregenerated bagasse was converted from cellulose I to cellulose II, and the content of acetylgroup in regenerated bagasse decreased. The regenerated bagasse was more thermally stablethan original bagasse and the decomposition temperature of the regenerated bagasse increasedfrom 205 oC to 217 oC.
3. Succinylation and phthalylation of bagasse cellulose were investigated in ionic liquid[C4mim]Cl using 4-dimethylaminopyridine (DMAP) as a catalyst to produce cellulosederivatives with high degree of substitution (DS). The effects of the dose of catalyst (DMAP),reaction time and reaction temperature on DS of the cellulose derivatives were investigated.The results indicated that the highest DS of succinylated cellulose, 2.34, was obtained at 100oC for 60 min with 5% DMAP, and that of phthalylated cellulose, 1.31, was reached at 80 oCfor 60 min with 5% DMAP. The acylation of three hydroxyl groups at the C6, C2 and C3 incellulose does occur, primarily at C6. The cellulose derivatives showed a lowerdecomposition temperature.
4. Homogeneous acetylation of bagasse was accomplished in ionic liquid [C4mim]Cl.[C4mim]Cl was successfully synthesized using N-methylimidazole and chlorobutane asstarting materials. Using the synthesized [C4mim]Cl as solvent, the effects of the parametersincluding the concentration of the acetic anhydride, reaction time and reaction temperature onweight percent gain (WPG) value of acetylated bagasse were studied. The results indicatedthat the WPG value increased with the increase of DMAP. 60 min was the preferred reactiontime due to the highest WPG of the product. Reaction temperature has few effect on the WPGvalue of the product in the range of 80-100 oC. However, the WPG value significantlydecreased above 110 oC due to the degradation of cellulose and hemicelluloses. All thehydroxyl groups in cellulose, hemicelluloses and lignin could be reacted with aceticanhydride. The TGA analysis indicated that acetylated bagasse was stable up to 198 oC andthe hygroscopicity of the product decreased from 5% to 2%.
5. The dissolution of bagasse and isolation of bagasse components were carried out inionic liquid 1-ethyl-3-methylimidazolium acetate ([C2mim]OAc). It was found that bagasse could be completely dissolved in ionic liquid using different heating methods, includinghigher temperature/shorter time, lower temperature/longer time and microwave irradiation.After the dissolution, the cellulosic materials and lignin could be isolated from bagasse byreconstitution in water/acetone. Increasing dissolution temperature and dissolution time led toan increase in the recovered lignin yield, however, the lower cellulosic material yield withlower lignin content was also obtained. Compared to dissolution at lower temperature/longertime, dissolution of bagasse in [C2mim]OAc at higher temperature/shorter time resulted inhigher delignification and lower lignin content in cellulosic material. The lower yield ofcellulosic material with higher lignin content was obtained by microwave assisted dissolution,which directly resulted in lower yield of carbohydrates. More importantly, the cellulosicmaterials and bagasse could be characterized by liquid 13C-NMR using the ionic liquid assolvent. Moreover, the side reaction (acetylation) occurred using the microwave irradiationmethod or higher temperature/shorter time method.
6. A new method for the isolation of cellulose and hemicelluloses from bagasse usingionic liquid/NaOH was proposed. Ion chromatography, FT-IR, TGA and NMR were used tocharacterize the physicochemical properties of the isolated cellulose and hemicelluloses. Theresults indicated that cellulose samples isolated from [C2mim]OAc/NaOH or[C4mim]Cl/NaOH system mainly contained glucose (76.61% and 63.05%, respectively) witha small amount of xylose, which represents hemicelluloses. The isolated cellulose samplescontained very few lignin. The major monosaccharide in hemicelluloses samples isolatedfrom [C2mim]OAc/NaOH or [C4mim]Cl/NaOH system were xylose (74.99% and 72.79%,respectively), arabinose (13.54% and 13.34%, respectively) and glucose (8.82% and 11.28%,respectively). Galactose and glucuronic acid were observed as minor constituents. Thethermal stability of the hemicelluloses samples was similar to the alkaline hemicelluloses.NMR results implied that the isolated hemicelluloses samples can be structurally defined asL-arabino-(4-O-methyl-D-glucurono)-D-xylan.
7. A new method to prepare biomass fibers directly from bagasse, oak or pine withoutthe removal of hemicelluloses and lignin was presented using ionic liquid as a solvent. Thebagasse fibers could be prepared using either the lower temperature/longer time or higher temperature/shorter time method, while oak and pine fibers can only be prepared using thehigher temperature/shorter time method. The bagasse fibers made with the highertemperature/shorter time method have higher tensile strength compared to those made withlower temperature/longer time method. Fibers with higher tensile strength were obtainedfrom biomass with higher cellulose content, and the fibers made from bagasse (125 MPa) andoak (102 MPa) exhibited higher tensile strength than those from pine (49 MPa). The XRDresults indicated that the crystalline structure of bagasse fiber was transformed from celluloseI in native bagasse to cellulose II.
引文
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