Name: pretreatment of lignocellulosic biomass with low-cost ionic liquids
Uploaded: 2016-08-10T13:00:00.000+00:00
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Description: Watch this Scientific Journal Video about Pretreatment of Lignocellulosic Biomass with Low-cost Ionic Liquids at JoVE.com

作者承认格兰瑟姆研究所气候变化与环境，气候KIC和自然科学研究理事会（EP / K038648 / 1和EP / K014676 / 1）资金和皮埃尔·布维尔为松预处理提供实验数据。

注意:在这个过程中所用的质子离子液体在我们的实验室中合成，但也有一些可能被或成为商购。所得的离子液体是酸性和腐蚀性和可能皮肤/眼刺激物（取决于所用的胺），因此必须小心穿着适当的PPE（实验室外套，安全规范，防护手套）处理。 1.准备<ol><li> 准备和存储的木质纤维素生物质 <ol><li>获得例如百克5公斤之前足够数量的实验的木质纤维素生物质。 注意:每个实验至少需要3克生物量（每个一式三份1克）。 </li><li>将水分含量降低收获后不久和在空气中干燥的形式的生物量存储在实验室。通过对表或长凳扩频生物量和离开它持续2周，或直至它出现干空气干燥生物量。移动和t内翻生物质他的时间来加速这一进程。一年收获之内进行分离实验。 注:直接收获后，木质生物质可以包含最多50重量％的水分，而空气干燥的生物量，这是比较稳定的，含有5-12重量％的水分。 </li><li>研磨筛和生物量为选择粒径范围。存放在塑料袋或其他合适的容器，直到使用干燥的生物质。 注意:对于这个协议处理的小样本，建议降低颗粒大小，例如180-850微米。 </li></ol></li><li> （根据NREL协议）确定生物质的水分含量20 <ol><li>以确定生物质的水分含量，preweigh在分析天平上的一块铝箔（大小约5厘米×5厘米），并记录所述箔（M 箔 ）的重量。称取约100毫克的空气干燥的生物量的在铝箔和记录确切的空气DRI编重量（M ADW）。 </li><li>折叠铝箔在105℃，使一个数据包和放置在风机辅助炉中过夜（至少4小时）。 </li><li>取分组并立即将其放置在干燥器中5分钟，然后立即称重该分组并记录烘箱干燥重量加箔（M ODW +箔 ）的确切重量。根据等式1计算出的生物量MC 的BM的水分含量（以％表示）: <img alt="式（1）" src="/files/ftp_upload/54246/54246eq1.jpg" />式。 1 其中m ODW +贴膜是烘箱干燥的包（烘箱干燥的生物量加箔）的重量中，M 箔在箔的重量而m ADW是生物质的风干重量。所有的重量应该是在g或以mg。 </li></ol></li><li> 离子液体的合成 <ol><li>在通风橱或倒相式音箱，重达1摩尔的胺（三乙胺）与磁力搅拌棒的1升圆底烧瓶中。放置在冰浴中的烧瓶中在磁力搅拌器板。立即加入250毫升加料漏斗，以尽量减少胺的蒸发。 注:确保正确的酸:碱比例的高重要性对实现预处理实验的重复性。 </li><li>使用已知浓度的溶液（在本实施例5摩尔/ L）和一个容量瓶（200ml）中测量出1摩尔硫酸。转移硫酸入加料漏斗和冲洗的任何酸附着于容量瓶的壁与去离子水的加料漏斗。 </li><li>添加硫酸滴加到胺同时剧烈搅拌。确保溶液不升温，因为这将导致胺和酸与碱不准确的比率的沸腾。冲洗使用去离子水，以确保该酸定量转移加料漏斗的内部。 注意:离子液体溶液的大批量可通过增加的胺和硫酸的量以及相应地将烧瓶体积进行。 </li><li>用旋转蒸发器蒸发掉大部分水。水含量应低于为预处理所需的水含量低。 注意:这是没有必要完全干燥的离子液体。它可能是有益的留下一些水在离子液体，如一些干燥的离子液体，其中包括硫酸三乙基氢，在室温下是固体。冷冻干燥机，也可用于降低水含量。 </li></ol></li><li> 在确认和调节的IL溶液中的水含量 注:水的含量是重要的实验变量。有三个来源，在预处理混合物中的水可来自。所有的人都需要被考虑到:（1）包含在合成或购买的离子液体溶液（2）的水的水包含在叔他风干生物质和（3）用移液管以达到最终所需的水含量添加任何水。 <ol><li>确定由根据由滴定仪制造商发出的指令体积Karl Fischer滴定合成或购买的离子液体溶液中的水含量。添加IL几滴成使用预先称重注射器滴定仪。输入加入滴定液的重量，等到滴定仪显示的读数。记录中的水含量。 </li><li>决定的水含量为所述生物质进行预处理。在该实验中，使用20重量％。减少使用旋转蒸发器中的水含量所需的水含量低于5％（重量）并如1.4.1所述确认通过Karl Fischer滴定新水含量。 注意:良好的结果与20重量％的水得到;然而，这可能不总是预处理最佳。较高的水含量可以减少溶剂费用或以较低的粘度进行选择。 </li></ol></li> &lt;LI&gt; 计算实验。 <ol><li>决定离子液体溶液米溶胶，最后和生物质对溶剂的比率的BM /溶胶最终的量。这里，使用10个克含有20％（重量）水和生物质的溶剂的比例为1:10克/ g离子液体溶液。 注:本协议所使用的管最多可容纳18克，IL解决方案，如果与溶剂比生物质为1:10（重量/重量）。高生物质的溶剂比率（高达1:2或甚至1:1）是从经济观点来看有利，但可能在小规模妥协预处理功效。 </li><li>确定用于根据下面的等式2每个样品必需的（无水的）离子液体的量: <img alt="公式（2）" src="/files/ftp_upload/54246/54246eq2.jpg" />式。 2 其中m IL是必需的，以克离子液体中，M 溶胶的量，最后是在克离子液体溶液的所需量和wc 最终&lt;/子&gt;是在离子液体中的溶液所需的水含量（％）。 </li><li>接下来，计算合成或购买离子液体溶液的量根据下面的等式3被添加到每个压力管中: <img alt="公式3" src="/files/ftp_upload/54246/54246eq3.jpg" />式。 3 其中m 溶胶的溶液被添加到每个压力管（克）的量中，M IL是必需的离子液体的量（克）和wc 溶胶是在离子液体溶液中的水含量（％）如通过卡尔·费歇尔滴定法测定。 </li><li>确定使用下面的等式4被添加到离子液体溶液的生物量（烘箱干燥重量为基准）的量。在该实验中，使用1个3g的压力管烘箱干燥芒草生物质。 <img alt="公式4" src="/files/ftp_upload/54246/54246eq4.jpg" />式。 4 其中，ODW是生物质被添加量编入每个压力管（克）中，m 溶胶，最后是离子液体溶液（克）和所需量的BM /溶胶最终是生物质的离子型液体溶液中的所期望的比例。 </li><li>确定需要通过使用下面的等式5被加入到管风干生物质的重量: <img alt="公式5" src="/files/ftp_upload/54246/54246eq5.jpg" />式。五 哪里ADW是要加入的生物量的风干重量入管（克），ODW是烘箱干燥重量为实验（在1.5.4中克测定）所需的生物量和MC BM是值1.2.3确定。 </li><li>计算需要多少水用移液管根据以下等式6来实现所需的最终水含量被加入: <img alt="公式6" src="/files/ftp_upload/54246/54246eq6.jpg" />式。 6 其中m 水的量要添加水，厕所最后是在预处理混合物（这里20重量％）所需的水含量中，M sol.final是溶剂（这里10克）的量，MC BM是空气干燥的生物质中的水分含量中，M BM是要添加风干的生物质的量，厕所溶胶是合成或购买的离子液体溶液的水含量，并且m 溶胶是离子液体溶液的量。 </li></ol></li></ol> 2.预处理注意:该过程可以在任何时候通过使样品在室温下（几天）或在冰箱（更长的时间）被中断。 <ol><li>预称重3支15mL的压力管聚四氟乙烯帽和硅胶O形圈。目视检查压力管，以确保他们没有裂纹或缺陷。 注意:较大压力管接头多种离子液体和生物量如果需要，可以使用，虽然预处理结果不会在不同的小瓶的尺寸处理的样品之间直接比较。我们建议使用前密封帽，为更好的密封。 </li><li>用10毫升吸管，添加所需的离子液体溶液的量进入压力管站在秤上。使用软木环，以保持管站了起来。记录的离子液体溶液的重量增加。在所需量的水添加到用吸管在1.5.6测定该溶液中，假设水的密度为1微克/毫升。 </li><li>放置在天平上的一块铝箔（尺寸长3cm×宽8cm）上的，去皮的平衡和称重出生物量添加所需空气干燥木质纤维素的量。去皮并生物质添加到管。放置空箔背面天平上，并记录的差别。 注意:可替换地，可以使用抗静电称量船。 </li><li>与硅胶O型圈聚四氟乙烯盖合上盖子。检查是否有良好的密封，无需过度紧缩。记录p的重量含生物量和离子液体ressure管。通过使用涡旋振荡器，直到所有的生物量是在与离子液体接触混合管的内容物。 注:并非所有的O型圈材料承受在高温下离子液体接触。我们发现，硅胶效果很好。 </li><li>放置压力管在已预加热到所需温度的风机辅助炉中。例如，离开管8小时，在120℃或在150℃下1小时。 注:时间和温度是重要的实验变量。其它时间 - 温度组合都可以使用。 </li><li>用隔热手套取出从烤箱小瓶并放置在通风橱，让他们冷却至室温。检查瓶的重量，散热，以保证在烹饪过程中没有逃脱后用水。 </li></ol> 3.洗浆<ol><li>传送每个管的内容到使用40毫升绝对的50m​​l离心管中Ë乙醇。使用涡旋振荡器1分钟以混合均匀，并离开所述管在室温下至少1小时摇动该管。 注意:分离还可以使用过滤进行，但是，较少精度可能为建议的样本大小被观察到。 </li><li>使用涡旋振荡器另外30秒摇动该管，然后离心管在2000×g下50分钟。单独的液体通过小心滗析固体。收集液体在一个干净的250ml园有搅拌棒底烧瓶中。 </li><li>加40毫升的新鲜乙醇进50毫升管，并重复步骤3.2三次。 <ol><li>通过将轮除去从离子液体中的乙醇有底的加热块上的烧瓶中。他们每个连接到一个真空泵用冷阱。填充干冰阱和设定的加热至40℃。打开搅拌和泵。 注意:此实验使用自制平行蒸发器根据并行合成建立设置。平行蒸发器也可以是珀切斯编做好准备。备选地，可以使用旋转式蒸发器。 </li></ol></li></ol> 4.纸浆索氏提取<ol><li>湿洗浆转移到纤维素套管，用铅笔标记每个顶针。 </li><li>填150毫升无水乙醇到干净的250ml园底有搅拌棒的烧瓶中。将含有样品的顶针到取40ml索氏提取器中，加入冷凝器和安装连接到再循环冷却器并行提取工作站上的一切。 注意:如果乙醇被用于纸浆转移，只有差至150ml添加到圆底烧瓶中。 </li><li>当所有样品加载，开始搅拌，将温度设定为135℃，并开启再循环装置（温度设定18℃）。提取纸浆样本共20个小时。 </li><li>关闭加热，使回流到打住。然后切换两个搅拌和冷却关闭。就拿顶针了索氏提取器中的使用镊子和让在通风橱中顶针过夜湿纸浆干燥。 </li><li>从索氏提取添加液体从生物质洗涤液，并继续从与平行蒸发器，或在40℃的旋转蒸发器将生物质洗涤蒸发乙醇。 </li><li>从顶针风干纸浆转移到一块配衡铝箔的分析天平上，记录所提取的纸浆的风干重量，并将其转移到经标记的塑料袋中。尽量在不刮顶针材料过墙恢复一切。 </li><li>立即确定纸浆中的水分含量来计算烘箱干燥收率（如前面在步骤1.4示出）。 </li></ol> 5.木质素分离<ol><li>当所有的乙醇蒸发，通过离子液体从圆底烧瓶转移到用30毫升水的50ml离心管沉淀木质素。混合悬挂和离开至少1小时。离心机在2000 xg离心20分钟，并通过倾析从固体溶液中分离出来。 注意:在这个协议中，3当量的水被用作反溶剂。少反溶剂可以使用，如果需要的话。洗涤液可收集，除去水并回收重复使用的离子液体。 </li><li>加入30ml蒸馏水加入到离心管内的木质素沉淀。重复混合，温育1小时，并离心。重复此步骤，共3木质素洗涤。 </li><li>干燥使用真空烘箱并在45℃的刺穿盖子过夜离心管内的木质素。为了确定木质素收率将一块铝箔的天平上，皮重的重量，从烘箱中添加木质素，并立即记录重量。转移木质素到小瓶贮存。 </li></ol>

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Microbiol. Biotechnol. 82 (5), 815-827 (2009).</li><li>Brandt, A., Gr&#228;svik, J., Hallett, J. P., Welton, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Deconstruction+of+lignocellulosic+biomass+with+ionic+liquids.">Deconstruction of lignocellulosic biomass with ionic liquids.</a> Green Chem. 15, 550 (2012).</li><li>Chen, L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Inexpensive+ionic+liquids:[HSO+4]&#8722;-based+solvent+production+at+bulk+scale).">Inexpensive ionic liquids:[HSO 4]&#8722;-based solvent production at bulk scale).</a> Green Chem. 16 (6), 3098-3106 (2014).</li><li>Brandt, A., Chen, L., van Dongen, B. E., Welton, T., Hallett, J. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Structural+changes+in+lignins+isolated+using+an+acidic+ionic+liquid+water+mixture.">Structural changes in lignins isolated using an acidic ionic liquid water mixture.</a> Green Chem. 17, 5019-5034 (2015).</li><li>Sluiter, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=NREL/TP-510-42621.">NREL/TP-510-42621.</a> Determination of Total Solids in Biomass and Total Dissolved Solids in Liquid Process Samples. , (2008).</li><li>Sluiter, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=NREL/+TP+-+510+-+42618Determination+of+Structural+Carbohydrates+and+Lignin+in+Biomass.">NREL/ TP - 510 - 42618Determination of Structural Carbohydrates and Lignin in Biomass.</a> Determination of Structural Carbohydrates and Lignin in Biomass. , (2011).</li><li>Resch, M. G., Baker, S. R., Decker, <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=NREL/TP-5100-63351.">NREL/TP-5100-63351.</a> Low Solids Enzymatic Saccharificatin of Lignocellulosic Biomass. , (2015).</li><li>Brandt, A., Ray, M. J., To, T. Q., Leak, D. J., Murphy, R. J., Welton, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ionic+liquid+pretreatment+of+lignocellulosic+biomass+with+ionic+liquid-water+mixtures.">Ionic liquid pretreatment of lignocellulosic biomass with ionic liquid-water mixtures.</a> Green Chem. 13 (9), 2489-2499 (2011).</li><li>Aver, K., Scortegagna, A., Fontana, R., Camassola, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Saccharification+of+ionic-liquid-pretreated+sugar+cane+bagasse+using+Penicillium+echinulatum+enzymes.">Saccharification of ionic-liquid-pretreated sugar cane bagasse using Penicillium echinulatum enzymes.</a> J Taiwan Inst Chem Eng. 45 (5), 2060-2067 (2014).</li><li>George, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Design+of+low-cost+ionic+liquids+for+lignocellulosic+biomass+pretreatment.">Design of low-cost ionic liquids for lignocellulosic biomass pretreatment.</a> Green Chem. 17 (3), 1728 (2015).</li><li>Verd&#237;a, P., Brandt, A., Hallett, J. P., Ray, M. J., Welton, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fractionation+of+lignocellulosic+biomass+with+the+ionic+liquid+1-butylimidazolium+hydrogen+sulfate.">Fractionation of lignocellulosic biomass with the ionic liquid 1-butylimidazolium hydrogen sulfate.</a> Green Chem. 16 (3), 1617-1627 (2014).</li><li>Brandt, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ionic+liquid+pretreatment+of+lignocellulosic+biomass+with+ionic+liquid-water+mixtures.">Ionic liquid pretreatment of lignocellulosic biomass with ionic liquid-water mixtures.</a> Green Chem. 13 (9), 2489-2499 (2011).</li></ol>

作者什么都没有透露。

对于这里提出的木质纤维素生物质的分馏技术产生一个富含纤维素的纸浆和木质素。大多数的半纤维素的溶解到离子液体和水解，但不恢复。如果半纤维素糖是需要的话，前Ionosolv脱木素半纤维素预萃取步骤可能是必要的。它迄今不可能完全关闭质量平衡为生物量，因为它不可能识别和量化在离子液体中液中发现的所有降解产物，特别是那些从木质素而产生。关于回收和质量平衡的详细研究正在?...

会议人类的能源需求是可持续的，我们的文明所面临的最大挑战之一。能源消耗预计在未来50年内翻番，投入更大的压力对化石燃料资源1通过广泛的化石燃料的使用大气中温室气体（GHG）的建设问题尤其严重，因为二氧化碳从燃烧产生化石燃料的负责人为温室效应50％。2因此，可再生能源和碳中和技术的大规模应用是满足子孙后代的增加能量和物质需要是必不可少的。1，3 植物生物量是最通用的可再生资源，因为它可以被用来生产热，电以及基于碳的化学物质，材料和燃料。在其他生物质类型的木质纤维素生物质的主要优势是高收益的PE其丰富，潜力土地，往往高得多的二氧化碳排放量储蓄R一侧，其中包括在土壤中碳的高保持4,5利用生物质的其它优点还包括当地的可用性，低资本要求将生物质转化为能量，而水土流失防治。8 木质纤维素原料的主要生产国是林业产业和农业部门以及市政废物管理。6木质纤维素生产有潜力扩大，用脑子来限制森林砍伐和避免了更换粮食作物和潜在污染物的释放。7可再生的生物质成为液体运输燃料和化学品的一个可行的普遍来源，它的处理必须成为与化石燃料转化技术在经济上有竞争力。9,10实现这方面的一个关键是要提高产率和生物量衍生的中间体的质量，同时降低成本。&lt;/ P&gt; 木素纤维素含有糖，可通过催化和微生物的转化被转化为燃料和化学品的比例很高。11这些糖是存在于木质纤维素中聚合形式如纤维素和半纤维素。它们可以被水解成葡萄糖和其它糖单体，然后用于生产生物乙醇和其它生物衍生的化学品和溶剂。12 为了访问纤维素糖，生物质的预处理是通过物理，化学，或结合的方法必要的。4预处理可以说是在木质纤维素生物质的物价稳定措施中最昂贵的步骤。因此，研究改进预处理工艺势在必行。 各种预处理技术是可用的。特别感兴趣的是那些分开纤维素（fractionative预处理）的木质素。木质素，在第三主要组分木素纤维素，水解剂以纤维素和半纤维素的访问限制，并降低每吨原料的糖产率。11，如果它是在合适的质量分离的分离木质素可以用作额外的生物精炼中间体13之一fractionative过程是硫酸盐方法，该方法为纸/纤维素生产中最常用的预处理。在硫酸盐法制浆，木片在高压下放入氢氧化钠和硫化钠和加热的混合物中在约170℃的高温下进行。14的碱性反应通过经由亲核打破聚合物下降到短的片段除去半纤维素和木质素和碱催化，并且通过经由酚羟基/醇基团的去质子化的木质素片段溶解。另一种常见的脱木素工艺是有机溶剂法的过程，也片段并溶解木质素和半纤维素。而不是使用碱性aqueo我们的解决方案，如乙醇和乙酸的有机溶剂中在高温下从5-30巴160-200℃，和压力之间的范围内使用。有机溶剂预处理拥有卡夫一些优势制浆，因为它产生较少的空气和水的污染。15这两个过程都具备一定的经济挑战，如果用于生产化学品和燃料，而不是纤维素。16 Ionosolv预处理采用离子液体，这是盐的具有低于100℃熔点和，作为其强大库仑相互作用，非常低的蒸汽压的结果。17这消除在预处理过程的空气污染，并能处理在大气压或接近大气压。 而在费力，多步合成中创建最离子液体，质子离子液体可以在从大宗化学品的一步骤的过程，这使得它们更便宜来合成据估计，一些离子液体可以在批量规模生产要每公斤1.24 $价格这与普通的有机溶剂如丙酮和甲苯18中，在相对 ​​较低的温度和压力下操作的过程中回收和再利用这些定制离子液体的能力使得这个更无害的替代和经济上有吸引力的候选对于生物精炼。 该详细视频协议演示了Ionosolv过程的木质纤维素生物质和富含纤维素的纸浆的最终酶糖化，以及高纯度的无异味的木质素的回收的脱木素实验室规模的版本。19

<table><tbody><tr><td colspan="4">&lt;strong&gt;IL synthesis&lt;/strong&gt;</td></tr><tr><td>Round bottom flask, with standard ground joint 24/29 NS, 1,000 ml</td><td>Lenz</td><td>3 0024 70</td><td>VWR product code 271-1309</td></tr><tr><td>250 ml Addition Funnel, Graduated, 29/26 Joint Size, 0-4&amp;nbsp;mm PTFE Valve</td><td>GPE</td><td>CG-1714-16</td><td></td></tr><tr><td>Dish-shaped dewar flask, SCH 31 CAL&amp;nbsp;</td><td>KGW-Isotherm</td><td>1197</td><td></td></tr><tr><td>Volumetric flask, 200 ml</td><td>VWR</td><td>612-3745&amp;nbsp;</td><td></td></tr><tr><td>Cork rings, pasteur pipettes and teet, wash bottle with deionised water, large magentic stir bar</td><td></td><td></td><td></td></tr><tr><td colspan="4">&lt;strong&gt;Biomass size reduction&lt;/strong&gt;</td></tr><tr><td>Heavy Duty Cutting Mill SM2000&amp;nbsp;</td><td>Retsch&amp;nbsp;</td><td>Discontinued</td><td>Replaced with Cutting Mill SM 200 (20.728.0001)&amp;nbsp;</td></tr><tr><td>Bottom sieves (10 mesh square holes, for particle size &amp;lt;2 mm)</td><td>Retsch&amp;nbsp;</td><td>03.647.0318</td><td>Part of cutting mill</td></tr><tr><td>Analytical Sieve Shaker AS 200</td><td>Retsch&amp;nbsp;</td><td>30.018.0001</td><td>Part of sieving machine</td></tr><tr><td>Test Sieve 200 mm &amp;Oslash; x 50 mm height ISO 3310/1 (180 &amp;micro;m)</td><td>Retsch&amp;nbsp;</td><td>60.131.000180</td><td>Part of sieving machine</td></tr><tr><td>Test Sieve 200 mm &amp;Oslash; x 50 mm height ISO 3310/1 (850 &amp;micro;m)</td><td>Retsch&amp;nbsp;</td><td>60.131.000850</td><td>Part of sieving machine</td></tr><tr><td>Collecting pan, stainless steel, 200&amp;nbsp;mm &amp;Oslash;, height 50 mm</td><td>Retsch&amp;nbsp;</td><td>69.720.0050</td><td>Part of sieving machine</td></tr><tr><td colspan="4">&lt;strong&gt;Rotary evaporator&lt;/strong&gt;</td></tr><tr><td>Rotary evaporator (Rotavapor R-210)</td><td>Buchi&amp;nbsp;</td><td>Discontinued</td><td>Replaced with Rotavapor R-300</td></tr><tr><td>Water bath (Heating bath B-491)</td><td>Buchi&amp;nbsp;</td><td>48201</td><td>Part of rotary evaporator</td></tr><tr><td>Recirculator&amp;nbsp;</td><td>Julabo</td><td>F25</td><td>Part of rotary evaporator</td></tr><tr><td>Vacuum pump (MPC 101 Z)</td><td>Ilmvac GmbH</td><td>412522</td><td>Part of rotary evaporator</td></tr><tr><td>Vacuum controller (Vacuum Control Box VCB 521)</td><td>Ilmvac GmbH</td><td>600053</td><td>Part of rotary evaporator</td></tr><tr><td colspan="4">&lt;strong&gt;Parallel evaporator&lt;/strong&gt;</td></tr><tr><td>StarFish Base Plate 135&amp;nbsp;mm (for Radleys &amp;amp; IKA)</td><td>Radleys</td><td>RR95010</td><td>Part of parallel evaporator</td></tr><tr><td>Monoblock for 5 x 250&amp;nbsp;ml Flasks</td><td>Radleys</td><td>RR95130&amp;nbsp;</td><td>Part of parallel evaporator</td></tr><tr><td>Telescopic 5-way Clamp with Velcro</td><td>Radleys</td><td>RR95400</td><td>Part of parallel evaporator</td></tr><tr><td>Gas/Vacuum Manifold with connectors</td><td>Radleys</td><td>RR95510&amp;nbsp;</td><td>Part of parallel evaporator</td></tr><tr><td>650&amp;nbsp;mm Rod</td><td>Radleys</td><td>RR95665&amp;nbsp;</td><td>Part of parallel evaporator</td></tr><tr><td>Quick Release Male, R/A Barbed 6.4&amp;nbsp;mm + Shut-off (3.2&amp;nbsp;mm ID)</td><td>Radleys</td><td>RR95520</td><td>Part of parallel evaporator</td></tr><tr><td>Stirrer/hot plate</td><td>Radleys</td><td>RR98072</td><td>Part of soxhlet extractor</td></tr><tr><td>Temperature controller</td><td>Radleys</td><td>RR98073</td><td>Part of soxhlet extractor</td></tr><tr><td>Elliptical Stirring Bar 15&amp;nbsp;mm Rare Earth</td><td>Radleys</td><td>RR98097&amp;nbsp;</td><td>Part of parallel evaporator</td></tr><tr><td>Vacuum cold trap, plastic coated, PTFE stopcock</td><td>Chemglass</td><td>CG-4519-01</td><td>Part of parallel evaporator</td></tr><tr><td>Vacuum pump (MPC 101 Z)</td><td>Ilmvac GmbH</td><td>412522</td><td>Part of parallel evaporator</td></tr><tr><td>Tygon tubing E-3603, 6.40&amp;nbsp;mm (internal) 12.80&amp;nbsp;mm (external)</td><td>Saint-Gobain/VWR</td><td>228-1292&amp;nbsp;</td><td>Part of parallel evaporator</td></tr><tr><td colspan="4">&lt;strong&gt;Parallel Soxhlet extractor&lt;/strong&gt;</td></tr><tr><td>StarFish Base Plate 135&amp;nbsp;mm (for Radleys &amp;amp; IKA)</td><td>Radleys</td><td>RR95010&amp;nbsp;</td><td>Part of soxhlet extractor</td></tr><tr><td>Monoblock for 5 x 250&amp;nbsp;ml Flasks</td><td>Radleys</td><td>RR95130&amp;nbsp;</td><td>Part of soxhlet extractor</td></tr><tr><td>Telescopic 5-way Clamp with Velcro</td><td>Radleys</td><td>RR95400&amp;nbsp;</td><td>Part of soxhlet extractor</td></tr><tr><td>Telescopic 5-way Clamp with Silicone Strap and Long Handle</td><td>Radleys</td><td>RR95410&amp;nbsp;</td><td>Part of soxhlet extractor</td></tr><tr><td>Water Manifold with connectors</td><td>Radleys</td><td>RR95500&amp;nbsp;</td><td>Part of soxhlet extractor</td></tr><tr><td>650&amp;nbsp;mm Rod</td><td>Radleys</td><td>RR95665&amp;nbsp;</td><td>Part of soxhlet extractor</td></tr><tr><td>Quick Release Male, R/A Barbed 6.4&amp;nbsp;mm + Shut-off (3.2&amp;nbsp;mm ID)</td><td>Radleys</td><td>RR95520&amp;nbsp;</td><td>Part of soxhlet extractor</td></tr><tr><td>Coil condensers with standard ground joints 29/32 NS</td><td>Lenz</td><td>5.2503.04&amp;nbsp;</td><td>Part of soxhlet extractor</td></tr><tr><td>Extractor Soxhlet 40&amp;nbsp;ml borosilicate glass 29/32 socket 24/29 cone</td><td>Quickfit</td><td>EX5/43&amp;nbsp;</td><td>Part of soxhlet extractor</td></tr><tr><td>Stirrer/hot plate</td><td>Radleys</td><td>RR98072</td><td>Part of soxhlet extractor</td></tr><tr><td>Temperature controller</td><td>Radleys</td><td>RR98073</td><td>Part of soxhlet extractor</td></tr><tr><td>Recirculator</td><td>Grant</td><td>LTC1</td><td>Part of soxhlet extractor</td></tr><tr><td>Cellulose extraction thimble</td><td>Whatman</td><td>2280-228</td><td></td></tr><tr><td>Tweezers</td><td>Excelta</td><td>20A-S-SE</td><td></td></tr><tr><td colspan="4">&lt;strong&gt;Vacuum drying oven&lt;/strong&gt;</td></tr><tr><td>Vacuum drying oven</td><td>Binder</td><td>VD 23</td><td>Part of vacuum oven</td></tr><tr><td>Dewar vessel 2&amp;nbsp;L 100&amp;nbsp;x&amp;nbsp;290&amp;nbsp;mm with handle</td><td>KGW-Isotherm</td><td>10613</td><td>Part of vacuum oven</td></tr><tr><td>Vacuum Trap</td><td>GPE</td><td>CG-4532-01&amp;nbsp;</td><td>Part of vacuum oven</td></tr><tr><td colspan="4">&lt;strong&gt;Other equipment&lt;/strong&gt;</td></tr><tr><td>Analytical balance</td><td>A&amp;amp;D</td><td>GH-252</td><td>accuracy to &amp;plusmn; 0.1 mg</td></tr><tr><td>Volumetric Karl Fischer titrator</td><td>Mettler Toledo</td><td>V20</td><td></td></tr><tr><td>10 ml disposable pipette</td><td>Corning Inc</td><td>Costar 4101 10 mL Stripette</td><td></td></tr><tr><td>Eppendorf Research plus pipette, variable volume, volume 100-1,000&amp;nbsp;&amp;mu;l</td><td>Eppendorf</td><td>3120000062</td><td></td></tr><tr><td>Desiccator</td><td>Jencons</td><td>JENC250-028BOM</td><td></td></tr><tr><td>Ace pressure tube bushing type, Front seal, volume 15&amp;nbsp;ml</td><td>Ace Glass</td><td>8648-04&amp;nbsp;</td><td></td></tr><tr><td>Ace O-rings, silicone, 2.6&amp;nbsp;mm, I.D. 9.2&amp;nbsp;mm&amp;nbsp;</td><td>Ace Glass</td><td>7855216</td><td>O-ring for pressure tube</td></tr><tr><td>Vortex shaker</td><td>VWR International</td><td>444-1378 (UK)</td><td></td></tr><tr><td>Fan-assisted convection oven</td><td>ThermoScientific</td><td>HeraTherm OMH60</td><td></td></tr><tr><td>Oven glove (Crusader Flex)</td><td>Ansel Edmont</td><td>42-325</td><td></td></tr><tr><td>250 ml Round bottom flask single neck ground joint 24/29 (Pyrex)</td><td>Quickfit&amp;nbsp;</td><td>FR250/3S</td><td></td></tr><tr><td>Rotaflo stopcock adapter with cone 24/29</td><td>Rotaflo England</td><td>MF11/2/SC</td><td></td></tr><tr><td>50 ml Falcon tube</td><td>Heraeus/Kendro</td><td>HERA 76002844</td><td></td></tr><tr><td>Centrifuge (Mega Star 3.0)</td><td>VWR&amp;nbsp;</td><td>521-1751</td><td></td></tr><tr><td colspan="4">&lt;strong&gt;Reagents&lt;/strong&gt;</td></tr><tr><td>Ethanol absolute</td><td>VWR</td><td>20820.464</td><td></td></tr><tr><td>Triethylamine</td><td>Sigma-Aldrich</td><td>T0886</td><td></td></tr><tr><td>Sulfuric acid 5 mol/L (10&amp;nbsp;N) AVS TITRINORM volumetric solution Safe-break bottle 2.5&amp;nbsp;L</td><td>VWR</td><td>191665V</td><td></td></tr><tr><td>Purified water (15 M&amp;Omega; ressitance)</td><td>Elga</td><td>CENTRA R200</td><td></td></tr><tr><td colspan="4">&lt;strong&gt;Lignocellulosic biomass&lt;/strong&gt;</td></tr><tr><td>Miscanthus X gigantheus</td><td></td><td></td><td></td></tr><tr><td>Pinus sylvestris</td><td></td><td></td><td></td></tr></tbody></table>

pretreatment of lignocellulosic biomass with low-cost ionic liquids

A number of ionic liquids (ILs) with economically attractive production costs have recently received growing interest as media for the delignification of a variety of lignocellulosic feedstocks. Here we demonstrate the use of these low-cost protic ILs in the deconstruction of lignocellulosic biomass (Ionosolv pretreatment), yielding cellulose and a purified lignin. In the most generic process, the protic ionic liquid is synthesized by accurate combination of aqueous acid and amine base. The water content is adjusted subsequently. For the delignification, the biomass is placed into a vessel with IL solution at elevated temperatures to dissolve the lignin and hemicellulose, leaving a cellulose-rich pulp ready for saccharification (hydrolysis to fermentable sugars). The lignin is later precipitated from the IL by the addition of water and recovered as a solid. The removal of the added water regenerates the ionic liquid, which can be reused multiple times. This protocol is useful to investigate the significant potential of protic ILs for use in commercial biomass pretreatment/lignin fractionation for producing biofuels or renewable chemicals and materials.

除去木质素和木质素沉淀，确切的量回收纸浆和葡萄糖产量取决于所使用的生物质的类型，在该处理在运行温度和治疗的持续时间。短的预处理时间和低的温度下会导致不完全的预处理，而在较高温度下的纤维素变得在离子液体中不稳定，导致水解和降解。选定的离子液体也起着在分馏过程的结果的重要的作用。 图1</st...

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Pretreatment of Lignocellulosic Biomass with Low-cost Ionic Liquids

The pretreatment of lignocellulosic biomass with protic low-cost ionic liquids is shown, resulting in a delignified cellulose-rich pulp and a purified lignin. The pulp gives rise to high glucose yields after enzymatic saccharification.

木质纤维素生物质预处理低成本离子液体

A number of ionic liquids (ILs) with economically attractive production costs have recently received growing interest as media for the delignification of ...

pretreatment-of-lignocellulosic-biomass-with-low-cost-ionic-liquids

Universidad de Cartagena UDEC

Research

JoVE Journal

Environment

17.9K 次观看.  Imperial College London. The pretreatment of lignocellulosic biomass with protic low-cost ionic liquids is shown, resulting in a delignified cellulose-rich pulp and a purified lignin. The pulp gives rise to high glucose yields after enzymatic saccharification.

视频: Pretreatment of Lignocellulosic Biomass with Low-cost Ionic Liquids

Methods for Facilitating Microbial Growth on Pulp Mill Waste Streams and Characterization of the Biodegradation Potential of Cultured Microbes

The kraft process is applied to wood chips for separation of lignin from the polysaccharides within lignocellulose for pulp that will produce a high quality paper. Black liquor is a pulping waste generated by the kraft process that has potential for downstream bioconversion. However, the recalcitrant nature of the lignocellulose resources, its chemical derivatives that constitute the majority of available organic carbon within black liquor, and its basic pH present challenges to microbial biodegradation of this waste material. Methods for the collection and modification of black liquor for microbial growth are aimed at utilization of this pulp waste to convert the lignin, organic acids, and polysaccharide degradation byproducts into valuable chemicals. The lignocellulose extraction techniques presented provide a reproducible method for preparation of lignocellulose growth substrates for understanding metabolic capacities of cultured microorganisms. Use of gas chromatography-mass spectrometry enables the identification and quantification of the fermentation products resulting from the growth of microorganisms on pulping waste. These methods when used together can facilitate the determination of the metabolic activity of microorganisms with potential to produce fermentation products that would provide greater value to the pulping system and reduce effluent waste, thereby increasing potential paper milling profits and offering additional uses for black liquor.

Industrial wastes can be collected and modified to analyze microbial growth. Lignocellulose extraction techniques provide components to analyze specific biodegradation ability. Gas chromatography-mass spectrometry identifies fermentation products of microorganisms grown on pulping waste. These methods determine the metabolic capacity of microorganisms to degrade pulping waste.

方法对纸浆厂污水流和培养微生物的生物降解能力的表征促进微生物生长

The kraft process is applied to wood chips for separation of lignin from the polysaccharides within lignocellulose for pulp that will produce a high ...

科研

环境科学

High-throughput Screening of Recalcitrance Variations in Lignocellulosic Biomass: Total Lignin, Lignin Monomers, and Enzymatic Sugar Release

The conversion of lignocellulosic biomass to fuels, chemicals, and other commodities has been explored as one possible pathway toward reductions in the use of non-renewable energy sources. In order to identify which plants, out of a diverse pool, have the desired chemical traits for downstream applications, attributes, such as cellulose and lignin content, or monomeric sugar release following an enzymatic saccharification, must be compared. The experimental and data analysis protocols of the standard methods of analysis can be time-consuming, thereby limiting the number of samples that can be measured. High-throughput (HTP) methods alleviate the shortcomings of the standard methods, and permit the rapid screening of available samples to isolate those possessing the desired traits. This study illustrates the HTP sugar release and pyrolysis-molecular beam mass spectrometry pipelines employed at the National Renewable Energy Lab. These pipelines have enabled the efficient assessment of thousands of plants while decreasing experimental time and costs through reductions in labor and consumables.

Plant cell wall structure and chemistry traits are evaluated to identify ideal feedstocks for biofuels and bio-materials. Standard methods have limitations when applied to large data sets. These high-throughput pretreatment, enzyme saccharification, and pyrolysis-molecular beam mass spectrometry methods compare large numbers of biomass samples with decreased experimental time and cost.

总木质素，木质素单体，和酶促糖推出:顽拗变奏曲在木质纤维素生物质的高通量筛选

The conversion of lignocellulosic biomass to fuels, chemicals, and other commodities has been explored as one possible pathway toward reductions in the ...

Experimental Protocol for Biodiesel Production with Isolation of Alkenones as Coproducts from Commercial Isochrysis Algal Biomass

The need to replace petroleum fuels with alternatives from renewable and more environmentally sustainable sources is of growing importance. Biomass-derived biofuels have gained considerable attention in this regard, however first generation biofuels from edible crops like corn ethanol or soybean biodiesel have generally fallen out of favor. There is thus great interest in the development of methods for the production of liquid fuels from domestic and superior non-edible sources. Here we describe a detailed procedure for the production of a purified biodiesel from the marine microalgae Isochrysis. Additionally, a unique suite of lipids known as polyunsaturated long-chain alkenones are isolated in parallel as potentially valuable coproducts to offset the cost of biodiesel production. Multi-kilogram quantities of Isochrysis are purchased from two commercial sources, one as a wet paste (80% water) that is first dried prior to processing, and the other a dry milled powder (95% dry). Lipids are extracted with hexanes in a Soxhlet apparatus to produce an algal oil (&#34;hexane algal oil&#34;) containing both traditional fats (i.e., triglycerides, 46-60% w/w) and alkenones (16-25% w/w). Saponification of the triglycerides in the algal oil allows for separation of the resulting free fatty acids (FFAs) from alkenone-containing neutral lipids. FFAs are then converted to biodiesel (i.e., fatty acid methyl esters, FAMEs) by acid-catalyzed esterification while alkenones are isolated and purified from the neutral lipids by crystallization. We demonstrate that biodiesel from both commercial Isochrysis biomasses have similar but not identical FAME profiles, characterized by elevated polyunsaturated fatty acid contents (approximately 40% w/w). Yields of biodiesel were consistently higher when starting from the Isochrysis wet paste (12% w/w vs. 7% w/w), which can be traced to lower amounts of hexane algal oil obtained from the powdered Isochrysis product.

Experimental Protocol for Biodiesel Production with Isolation of Alkenones as Coproducts from Commercial Isochrysis Algal Biomass

Detailed methods are presented for the production of biodiesel along with the co-isolation of alkenones as valuable coproducts from commercial Isochrysis microalgae.

实验协议生产生物柴油与饱和酮的分离从商业余积<em&gt;等鞭金藻</em&gt;藻类生物量

The need to replace petroleum fuels with alternatives from renewable and more environmentally sustainable sources is of growing importance. ...

Measuring the Flight Ability of the Ambrosia Beetle, Platypus Quercivorus (Murayama), Using a Low-Cost, Small, and Easily Constructed Flight Mill

The ambrosia beetle, Platypus quercivorus (Murayama), is the vector of a fungal pathogen that causes mass mortality of Fagaceae trees (Japanese oak wilt). Therefore, knowing the dispersal capacity may help inform trapping/tree removal efforts to prevent this disease more effectively. In this study, we measured the flight velocity and duration and estimated the flight distance of the beetle using a newly developed flight mill. The flight mill is low cost, small, and constructed using commonly available items. Both the flight mill arm and its vertical axis comprise a thin needle. A beetle specimen is glued to one tip of the arm using instant glue. The other tip is thick due to being covered with plastic, thus it facilitates the detection of rotations of the arm. The revolution of the arm is detected by a photo sensor mounted on an infrared LED, and is indicated by a change in the output voltage when the arm passed above the LED. The photo sensor is connected to a personal computer and the output voltage data are stored at a sampling rate of 1 kHz. By conducting experiments using this flight mill, we found that P. quercivorus can fly at least 27 km. Because our flight mill comprises cheap and small ordinary items, many flight mills can be prepared and used simultaneously in a small laboratory space. This enables experimenters to obtain a sufficient amount of data within a short period.

Measuring the Flight Ability of the Ambrosia Beetle, Platypus Quercivorus Murayama, Using a Low-Cost, Small, and Easily Constructed Flight Mill

We developed a low cost and small flight mill, constructed with commonly available items and easily used in experimentation. Using this apparatus, we measured the flight ability of an ambrosia beetle, Platypus quercivorus.

利用低成本、小型、易于建造的Quercivorus测量豚草甲虫、鸭嘴兽的飞行能力 (村山富市)

The ambrosia beetle, Platypus quercivorus (Murayama), is the vector of a fungal pathogen that causes mass mortality of Fagaceae trees (Japanese oak wilt). ...

A Novel Method for the Pentosan Analysis Present in Jute Biomass and Its Conversion into Sugar Monomers Using Acidic Ionic Liquid

Recently, ionic liquids (ILs) are used for biomass valorization into valuable chemicals because of their remarkable properties such as thermal stability, lower vapor pressure, non-flammability, higher heat capacity, and tunable solubility and acidity. Here, we demonstrate a method for the synthesis of C5 sugars (xylose and arabinose) from the pentosan present in jute biomass in a one-pot process by utilizing a catalytic amount of Br&#248;nsted acidic 1-methyl-3-(3-sulfopropyl)-imidazolium hydrogen sulfate IL. The acidic IL is synthesized in the lab and characterized using NMR spectroscopic techniques for understanding its purity. The various properties of BAIL are measured such as acid strength, thermal and hydrothermal stability, which showed that the catalyst is stable at a higher temperature (250 &#176;C) and possesses very high acid strength (Ho 1.57). The acidic IL converts over 90% of pentosan into sugars and furfural. Hence, the presenting method in this study can also be employed for the evaluation of pentosan concentration in other kinds of lignocellulosic biomass.

We present a protocol for the synthesis of C5 sugars (xylose and arabinose) from a renewable non-edible lignocellulosic biomass (i.e., jute) with the presence of Br&#248;nsted acidic ionic liquids (BAILs) as the catalyst in water. The BAILs catalyst exhibited better catalytic performance than conventional mineral acid catalysts (H2SO4 and HCl).

利用酸性离子液体戊聚糖分析黄麻生物量及其转化为糖单体的新方法

Recently, ionic liquids (ILs) are used for biomass valorization into valuable chemicals because of their remarkable properties such as thermal stability, ...

Extraction of Lignin with High &#946;-O-4 Content by Mild Ethanol Extraction and Its Effect on the Depolymerization Yield

Lignin valorization strategies are a key factor for achieving more economically competitive biorefineries based on lignocellulosic biomass. Most of the emerging elegant procedures to obtain specific aromatic products rely on the lignin substrate having a high content of the readily cleavable &#946;-O-4 linkage as present in the native lignin structure. This provides a miss-match with typical technical lignins that are highly degraded and therefore are low in &#946;-O-4 linkages. Therefore, the extraction yields, and the quality of the obtained lignin are of utmost importance to access new lignin valorization pathways. In this manuscript, a simple protocol is presented to obtain lignins with high &#946;-O-4 content by relatively mild ethanol extraction that can be applied to different lignocellulose sources. Furthermore, analysis procedures to determine the quality of the lignins are presented together with a depolymerization protocol that yields specific phenolic 2-arylmethyl-1,3-dioxolanes, which can be used to evaluate the obtained lignins. The presented results demonstrate the link between lignin quality and potential for the lignins to be depolymerized into specific monomeric aromatic chemicals. Overall, the extraction and depolymerization demonstrates a trade-off between the lignin extraction yield and the retention of the native aryl-ether structure and thus the potential of the lignin to be used as the substrate for the production of chemicals for higher-value applications.

Here, we present a protocol to perform ethanol extraction of lignin from several biomass sources. The effect of the extraction conditions on the lignin yield and &#946;-O-4 content are presented. Selective depolymerization is performed on the obtained lignins to obtain high aromatic monomer products.

轻度乙醇萃取高β-o-4 的木质素及其对解聚产率的影响

Lignin valorization strategies are a key factor for achieving more economically competitive biorefineries based on lignocellulosic biomass. Most of the ...

化学

Fractionation of Lignocellulosic Biomass using the OrganoCat Process

The shift from a petroleum-based to a more sustainable and bio-based economy requires the development of new refinery concepts to maintain the supply of raw materials and energy. For these novel and sustainable biorefinery concepts, it is important to use catalysts and solvents that are aligned with the principles of Green Chemistry. Therefore, the implementation of biogenic alternatives can be a promising solution. The lignocellulose pretreatment and fractionation process presented herein-OrganoCat-is an integrated fractionation of lignocellulose into its main components using biogenic acids such as 2,5-furandicarboxylic acid as catalyst. Hemicelluloses and other non-cellulosic polysaccharides are selectively depolymerized by the diluted acid and dissolved, while the crystalline cellulose remains in the solid pulp. In the presence of a second organic phase consisting of biogenic 2-methyltetrahydrofuran, disentangled lignin is extracted in situ. The process allows for the efficient fractionation of the three main components-lignin, cellulose, and non-cellulosic sugars. This helps to focus on the quality of the lignin, the improvement of enzymatic hydrolysis of the cellulose-enriched pulp, and the mild non-cellulosic sugar extraction with low degradation.

OrganoCat is a method for the pretreatment and fractionation of lignocellulose under mild conditions into lignin, fermentable sugars, and cellulose pulp. In a biogenic, biphasic solvent system of water and 2-methyltetrahydrofuran with 2,5-furancarboxylic acid as catalyst, the OrganoCat products are separated in situ for straightforward product recovery.

使用有机催化工艺分馏木质纤维素生物质

The shift from a petroleum-based to a more sustainable and bio-based economy requires the development of new refinery concepts to maintain the supply of ...

Ultrafast Lignin Extraction from Unusual Mediterranean Lignocellulosic Residues

Pretreatment is still the most expensive step in lignocellulosic biorefinery processes. It must be made cost-effective by minimizing chemical requirements as well as power and heat consumption and by using environment-friendly solvents. Deep eutectic solvents (DESs) are key, green, and low-cost solvents in sustainable biorefineries. They are transparent mixtures characterized by low freezing points resulting from at least one hydrogen bond donor and one hydrogen bond acceptor. Although DESs are promising solvents, it is necessary to combine them with an economic heating technology, such as microwave irradiation, for competitive profitability. Microwave irradiation is a promising strategy to shorten the heating time and boost fractionation because it can rapidly attain the appropriate temperature. The aim of this study was to develop a one-step, rapid method for biomass fractionation and lignin extraction using a low-cost and biodegradable solvent. 
In this study, a microwave-assisted DES pretreatment was conducted for 60 s at 800 W, using three kinds of DESs. The DES mixtures were facilely prepared from choline chloride (ChCl) and three hydrogen-bond donors (HBDs): a monocarboxylic acid (lactic acid), a dicarboxylic acid (oxalic acid), and urea. This pretreatment was used for biomass fractionation and lignin recovery from marine residues (Posidonia leaves and aegagropile), agri-food byproducts (almond shells and olive pomace), forest residues (pinecones), and perennial lignocellulosic grasses (Stipa tenacissima). Further analyses were conducted to determine the yield, purity, and molecular weight distribution of the recovered lignin. In addition, the effect of DESs on the chemical functional groups in the extracted lignin was determined by Fourier-transform infrared (FTIR) spectroscopy. The results indicate that the ChCl-oxalic acid mixture affords the highest lignin purity and the lowest yield. The present study demonstrates that the DES-microwave process is an ultrafast, efficient, and cost-competitive technology for lignocellulosic biomass fractionation.

Deep eutectic solvent-based, microwave-assisted pretreatment is a green, fast, and efficient process for lignocellulosic fractionation and high-purity lignin recovery.

超高速利格宁从不寻常的地中海木质细胞残留物中提取

Pretreatment is still the most expensive step in lignocellulosic biorefinery processes. It must be made cost-effective by minimizing chemical requirements ...

High-throughput Saccharification Assay for Lignocellulosic Materials

Polysaccharides that make up plant lignocellulosic biomass can be broken down to produce a range of sugars that subsequently can be 
used in establishing a biorefinery. These raw materials would constitute a new industrial platform, which is both sustainable and carbon neutral, to replace 
the current dependency on fossil fuel. The recalcitrance to deconstruction observed in lignocellulosic materials is produced by several intrinsic properties 
of plant cell walls. Crystalline cellulose is embedded in matrix polysaccharides such as xylans and arabinoxylans, and the whole structure is encased by the 
phenolic polymer lignin, that is also difficult to digest 1. In order to improve the digestibility of plant materials we need to discover the main bottlenecks 
for the saccharification of cell walls and also screen mutant and breeding populations to evaluate the variability in saccharification 2. These tasks require 
a high throughput approach and here we present an analytical platform that can perform saccharification analysis in a 96-well plate format. This platform has 
been developed to allow the screening of lignocellulose digestibility of large populations from varied plant species. We have scaled down the reaction volumes 
for gentle pretreatment, partial enzymatic hydrolysis and sugar determination, to allow large numbers to be assessed rapidly in an automated system.
This automated platform works with milligram amounts of biomass, performing ball milling under controlled conditions to reduce the plant 
materials to a standardised particle size in a reproducible manner. Once the samples are ground, the automated formatting robot dispenses specified and recorded 
amounts of material into the corresponding wells of 96 deep well plate (Figure 1). Normally, we dispense the same material into 4 wells to have 4 replicates for 
analysis. Once the plates are filled with the plant material in the desired layout, they are manually moved to a liquid handling station (Figure 2). In this 
station the samples are subjected to a mild pretreatment with either dilute acid or alkaline and incubated at temperatures of up to 90&deg;C. The pretreatment solution 
is subsequently removed and the samples are rinsed with buffer to return them to a suitable pH for hydrolysis. The samples are then incubated with an enzyme
mixture for a variable length of time at 50&deg;C. An aliquot is taken from the hydrolyzate and the reducing sugars are automatically determined by the MBTH 
colorimetric method.

A simple, rapid method for determining the saccharification potential of large numbers of plant biomass samples is described. The automated platform for this analysis involves the preparation of the plant biomass for analysis in 96 well plates and the subsequent performance of pretreatment, hydrolysis and quantification of the sugars released.

木质纤维素材料的高通量检测糖化

Polysaccharides that make up plant lignocellulosic biomass can be broken down to produce a range of sugars that subsequently can be 
used in establishing ...

生物学

Biofuels: Producing Ethanol from Cellulosic Material

Source: Laboratories of Margaret Workman and Kimberly Frye - Depaul University
In this experiment, cellulosic material (such as corn stalks, leaves, grasses, etc.) will be used as a feedstock for the production of ethanol.&#160;The cellulosic material is first pretreated (ground and heated), digested with enzymes, and then fermented with yeast.&#160;Ethanol production is monitored using an ethanol probe.&#160;The experiment can be extended to optimize ethanol production by varying the feedstock used, pretreatment conditions, enzyme variation, yeast variation, etc.&#160;An alternative method of monitoring the reaction is to measure the carbon dioxide produced (using a gas sensor) instead of the ethanol.&#160;As a low-tech alternative, glucose meters (found in any drug store) can be used to monitor the glucose during the process, if an ethanol probe or carbon dioxide gas sensor is not available.
With an increased emphasis on &#8216;inquiry-based learning&#8221;, scientific probes are becoming more popular.&#160;Handheld devices like the Vernier Lab Quest used in conjunction with a variety of probes (such as those for conductivity, dissolved oxygen, voltage, and more) allow for less focus on collecting data and/or making graphs and more on analyzing the data and making predictions.&#160;Another advantage is that these are small and lightweight and can be taken into the field for measurements.

生物燃料: 生产乙醇从纤维素材料

Source: Laboratories of Margaret Workman and Kimberly Frye - Depaul University
In this experiment, cellulosic material (such as corn stalks, leaves, ...