这项工作得到了中国农业科学与技术创新研究院 (grant CARS-19)、中国农业科技学院 (ASTIP-IBFC07)、创新基金 (赠款号) 等专项基金的支持。为东华大学研究生 (格兰特号 16D310107), "小萍科技创新团队" (产业化综合研究 & 开发的麻纤维生物脱胶), 中国奖学金委员会。

1. 苎麻的氧化脱胶
<ol><li>
氧化脱胶液的制备
	<ol>
<li>溶解 2 g H2O2, 1 克碱 (混合镁 (OH)2和氢氧化钠), 0.4 克 Na5P3O10, 0.1 克蒽醌和0.2 克 HEDP 在100毫升蒸馏水中做脱胶解决方案。</li>
	</ol>
</li>
	<li>
苎麻的氧化脱胶
	<ol>
<li>在脱胶液中浸泡10克生苎麻, 并在85° c 下冲刷60分钟。</li>
		<li>将温度提高到125° c (压力为0.6 公斤), 再冲刷60分钟。 注: 有关提高温度的说明, 请参阅讨论。</li>
	</ol>
</li>
	<li>
苎麻纤维的还原
	<ol>
<li>在100毫升蒸馏水中溶解0.4 克 NaHSO3 , 以制备还原溶液。然后, 在90° c 的还原液中对脱胶纤维进行60分钟的处理。 注: 在氧化反应中产生的纤维素中的羧基和醛类会导致氢键的还原, 从而损害纤维的性能。通过将羧基和醛基转化为羟基, 可以改善纤维的性能。</li>
	</ol>
</li>
	<li>
后续处理
	<ol>
<li>用去离子水彻底清洗脱胶苎麻纤维。</li>
		<li>将纤维浸泡在90° c 的脱胶油中15分钟, 然后将纤维在烤箱 (125 ° c) 中干燥4小时。</li>
	</ol>
</li>
</ol>2. 脱胶溶液性能的测试
<ol><li>
Mg (OH) 的溶解度测试2
	<ol>
<li>在100毫升蒸馏水中溶解2克毫克 (OH)2 。</li>
		<li>另外, 溶解2克毫克 (OH)2在100毫升溶液与完全可溶性脱胶添加剂, 包括 0.4 g Na5P3O10和 0.2 g HEDP。</li>
		<li>提高在步骤2.2.1 和2.2.2 中描述的溶液的温度到85° c。</li>
		<li>用烧结光盘提取溶毫克 (OH)2 。</li>
		<li>用以下公式计算 Mg (OH)2的溶解度: <img alt="Equation 2" src="/files/ftp_upload/56461/56461eq2.jpg"> 注意: 这里的m (g) 是溶 Mg (OH)2的重量。</li>
	</ol>
</li>
	<li>
Mg (OH)2替代率对脱胶液 pH 值、有向值和残余 H2O2含量的影响 注意:12,19是重要的水化学参数, 它为环境水的氧化或还原能力提供了一个测量工具。具有较强氧化性能的溶液具有较高的物性值。mg (oh)2替代率是指在总碱用量为 10% (织物重量) 下, 由 mg (oh)2取代的氢氧化钠的摩尔比例。<ol>
<li>根据步骤 60%, 分别准备0%、20%、40%、80%、100% 和1.1 的镁 (OH)2替代率的脱胶解决方案。</li>
		<li>将原苎麻浸泡在步骤2.2.1 中描述的脱胶溶液中。</li>
		<li>根据步骤1.2 开始脱胶过程。</li>
		<li>用蒸馏水冲洗混合的可处理电极, 并在空气中烘干。然后在脱胶解决方案中浸泡混合的可检测的电极仪表, 每10分钟读取一次可解的值. 将 ph 电极计浸在脱胶溶液中, 每10分钟读出 ph 值。</li>
		<li>根据中国标准 GB 22216-20087的高锰酸钾4滴定法, 测试脱胶解决方案的 H2O2内容, 每10分钟进行一次。</li>
	</ol>
</li>
</ol>3. 苎麻纤维性能测试
<ol><li>
脱胶产量
	<ol>
<li>用以下公式计算脱胶率: <img alt="Equation 3" src="/files/ftp_upload/56461/56461eq3.jpg"> 注: 在这里, w (g) 是纤维在脱胶后的干重;W (g) 是苎麻在脱胶前的干重。</li>
	</ol>
</li>
	<li>
纤维的残余牙龈 注: 根据中国标准 5889-86, 对纤维的残余牙龈进行了测试。<ol>
<li>测量称量瓶中纤维 (约5克) 的干重, 并将其浸泡在装有150毫升氢氧化钠溶液 (20 克/升) 的烧瓶中 (回流冷凝管)。</li>
		<li>将温度提高到100° c, 并保持在这个温度为1小时。</li>
		<li>刷新碱液溶液。</li>
		<li>将温度提高到100° c, 并保持2小时。</li>
		<li>在样品筛中清洗纤维。</li>
		<li>测量称量瓶中纤维的干重。</li>
		<li>使用以下等式计算纤维的残余牙龈: <img alt="Equation 4" src="/files/ftp_upload/56461/56461eq4.jpg"> 注: 这里 m (g) 是纤维的干重;M (g) 是碱精练后苎麻的干重。</li>
	</ol>
</li>
	<li>
PD 试验 注: 根据国标 GB 5888-8615测试苎麻纤维的 PD 值。<ol>
<li>脱脂在 2:1 (v/五) 苯和乙醇混合物中浸入苎麻纤维。</li>
		<li>在室温下在空气中蒸发溶剂。</li>
		<li>使用剪刀将样品切成短片 (每样1-2 毫米, 约20-23 毫克)。</li>
		<li>在称量容器中, 将样品保持在控制湿度 (20 ±2° c, 相对湿度 = 65 ± 2%) 中, 直到它达到平衡含水量, 然后才能除去测试目的所需的材料。</li>
		<li>将一根铜线 (直径0.5 毫米) 浸在浓硝酸中, 其次为98% 无水乙二胺。然后, 用蒸馏水彻底冲洗铜颗粒。</li>
		<li>将纤维样品和铜颗粒放在塑料瓶中 (顶部)。</li>
		<li>在塑料瓶中加入10毫升蒸馏水和10毫升1摩尔/L cupriethylenediamine 溶液, 搅拌使用磁性搅拌棒, 准备 0.2 g/100 毫升 (约) 苎麻纤维 cupriethylenediamine 溶液。</li>
		<li>将6.5 毫升苎麻纤维 cupriethylenediamine 溶液转化为乌粘度计测定其内在粘度。用下列公式计算相对粘度: <img alt="Equation 5" src="/files/ftp_upload/56461/56461eq5.jpg"> 注: 这里ηr是相对粘度, t (s) 是苎麻纤维 cupriethylenediamine 溶液流经乌粘度计的平均时间, 而 t0 (s) 是0.5 摩尔/L cupriethylenediamine 溶液流经的平均时间乌粘度计。</li>
		<li>用以下公式计算苎麻纤维的 PD 值: <img alt="Equation 6" src="/files/ftp_upload/56461/56461eq6.jpg"> 注: 这里 [η] 是本征粘度, [η] ×C 值可从中国标准 GB 5888-86 的表中获得, C 是苎麻纤维 cupriethylenediamine 溶液的浓度。</li>
	</ol>
</li>
	<li>
纤维的线性密度
	<ol>
<li>使用以下等式计算纤维的线性密度: <img alt="Equation 7" src="/files/ftp_upload/56461/56461eq7.jpg"> 注: 这里 Lc是切割长度 (40 mm), n是纤维的数量, g (g) 是纤维的重量。纤维的线性密度是指在苎麻 (12%) 正式重拾的情况下, 1000 米长纤维的重量。</li>
	</ol>
</li>
	<li>
机械性能测试
	<ol>
<li>平衡在标准大气条件下的纤维样品 (T = 20 ±2° c, RH = 65% ± 2%) 为 24 h。</li>
		<li>在20° c、RH 65% 和 0.3 cN/dtex 的预张力下, 使用纤维强度仪测试纤维断裂的韧性、断裂伸长率和工作。将夹紧距离设置为 20 mm, 底部夹具的下降速度为 20 mm/分钟7,15。</li>
	</ol>
</li>
	<li>
脱胶废水的 COD 值
	<ol>
<li>根据国标/T 15456-2008 工业循环冷却水对脱胶废水 cod 的测定 cod-高锰酸钾法的检测方法 "7,15。</li>
	</ol>
</li>
	<li>
XRD 测试
	<ol>
<li>利用 x-射线衍射获得纤维的结晶度。记录 XRD 模式 2θ = 5-60 °的衍射仪配有石墨单色仪和 Cu Kα辐射在λ = 0.154 nm (40 伏, 200 毫安)。</li>
	</ol>
</li>
	<li>
FTIR 分析
	<ol>
<li>利用光谱仪获得了光纤的 FTIR 模式。将扫描时间设置为 30, 范围在 4,000-400 cm-1, 分辨率为8厘米-1。用红外光谱分析法测定处理纤维中的化学官能团。</li>
	</ol>
</li>
</ol>

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作者没有什么可透露的。

Mg (OH)2的设置取代率和反应温度是该协议的重点。Mg (OH)2取代率可以影响脱胶溶液的 pH 值和氧化能力。最好的 Mg (OH)2替代率苎麻脱胶是 20%, 因为纤维素不能得到足够的保护下的替代率低于 20%, 和过量的剩余牙龈 (低 DP 值和结晶度) 将保留在纤维低于 20% (图 4A) 的替代率。
反应温度会影响过氧化氢的反应途径。苎麻氧化脱胶过程中?...

苎麻, 俗称 "中国草", 是一种多年生草本植物, 其纤维可作为纺织工业的优良材料1,2。它是中国原产的主要经济作物之一;中国苎麻产量占世界总产量的90% 以上1,2。苎麻纤维是最强和最长的植物纤维之一, 光泽与几乎柔滑的外观3,4。苎麻纤维长的长度使其适合于单纤维纺丝, 在麻纤维中很少见到。苎麻纤维织物具有冷却、抗菌、导热性能优异、透气性好等优点,等3,4
纤维素是苎麻纤维的主要成分, 苎麻中的其他成分如果胶、木质素、水溶性物质等, 被定义为牙龈5,6。苎麻纤维可通过溶于含有化学试剂的溶液中的牙龈来提取, 该过程定义为脱胶5,6。主要有两种苎麻纤维提取方法: 化学脱胶和生物脱胶。传统化学脱胶工艺中脱胶废水的能耗、时间消耗和 COD 值都比较高, 在高压下用浓碱液精练法提取纤维素纤维6至 8 h7,8.另外, 生物脱胶是苎麻纤维提取的一种环保选择。然而, 苛刻的反应条件和先进的设备抑制其进一步的工业应用9,10。因此, 用碱过氧化氢进行氧化脱胶, 提出了一种有价值的、可供选择的应用重点, 因为它需要较短的脱胶时间和较低的脱胶温度11,12。然而, 由于过氧化物的强氧化能力, 在脱胶过程中可能会发生大量的纤维素降解, 这会对纤维性能造成很大的损害13,14。这是苎麻碱氧化脱胶的最大缺点。
在以前的研究中, 苎麻纤维被提取的碱过氧化氢系统只支持氢氧化钠15。然而, 由于氢氧化钠的强碱性, 过氧化氢的氧化反应速度难以控制, 从而对处理后的纤维7造成很大的损害。为了改善苎麻纤维的性能, 本研究采用氢氧化钠和氢氧化镁组成的控释碱源, 为碱性过氧化氢系统的 pH 值提供了一个碱条件和缓冲剂16,17。
这项技术背后的基本原理可以描述如下。氢氧化镁在蒸馏水中略有溶解性, 它可以用 OH-的消耗逐渐溶入脱胶溶液, 并使脱胶液的 pH 值和氧化能力保持在适当的范围内18。氢氧化镁的取代率 (SR) 被定义为氢氧化镁在总碱用量为10% 时所取代的氢氧化钠的摩尔比例, 并可通过以下公式计算替代率。此外, Mg2 +可以防止过度氧化导致的纤维素降解,19,20。
<img alt="Equation 1" src="/files/ftp_upload/56461/56461eq1.jpg">
在这里, M2 (g) 是重量的 Mg (OH)2, M1 (g) 是氢氧化钠的重量, 40 是氢氧化钠的分子量, 58 是分子量的 mg (oh)2, 2 是在 mg (oh)2中的 "职业" 的数量, 而 SR 是替代率。
本协议的技术可以推广到碱式过氧化氢系统中的植物材料的提取、漂白和改性。然而, 必须指出的是, 碱性过氧化氢系统的 pH 值和反应温度的选择是这项技术的关键21。碱性过氧化氢系统的 pH 值可以通过改变置换率17来调整。碱过氧化氢体系的 pH 值和氧化能力随取代率的增加而降低。当反应温度设定在85° c 时, 自由基反应在系统中起主要作用, 系统的强氧化性适合于溶解物料;当反应温度设定在125° c 时, 自由基反应被抑制, 系统中存在大量的呼出, 使系统适合漂白19。

<table><tbody><tr><td>Hydrogen peroxide, 30%</td><td>Fisher Scientific</td><td>H325-100</td><td>Chemical for degumming</td></tr><tr><td>Magnesium hydroxide, 99%</td><td>Fisher Scientific</td><td>AA1236722</td><td>Chemical for degumming</td></tr><tr><td>Sodium hydroxide</td><td>Fisher Scientific</td><td>S318-1</td><td>Chemical for degumming</td></tr><tr><td>Sodium bisulfite</td><td>Fisher Scientific</td><td>S654-500</td><td>Chemical for degumming</td></tr><tr><td>Sodium tripolyphosphate</td><td>Fisher Scientific</td><td>AC218675000</td><td>Chemical for degumming</td></tr><tr><td>Anthraquinone, &gt;98%</td><td>Fisher Scientific</td><td>AC104930500</td><td>Chemical for degumming</td></tr><tr><td>1-Hydroxy Ethylidene-1,1-Diphosphonic Acid</td><td>Fisher Scientific</td><td>50-901-10243</td><td>Chemical for degumming</td></tr><tr><td>Degumming oil</td><td>Minglong auxiliaries limited liability company, Yiyang, Hunan,China</td><td>&amp;mdash;&amp;mdash;</td><td>Chemical for degumming</td></tr><tr><td>Ethyl alcohol</td><td>Fisher Scientific</td><td>A962-4</td><td>Chemical for testing</td></tr><tr><td>Benzene</td><td>Fisher Scientific</td><td>AA43817AE</td><td>Chemical for testing</td></tr><tr><td>Copper wire,0.5mm (0.02in) dia</td><td>Fisher Scientific</td><td>AA10783H4</td><td>Chemical for testing</td></tr><tr><td>Cupriethylenediamine solution 1mol/L</td><td>Fisher Scientific</td><td>24991</td><td>Chemical for testing, caution toxic</td></tr><tr><td>Nitric acid (65% ~68% )</td><td>Fisher Scientific</td><td>A200-612GAL</td><td>Chemical for testing, caution</td></tr><tr><td>Ethylenediamine</td><td>Fisher Scientific</td><td>AC118420100</td><td>Chemical for testing</td></tr><tr><td>Potassium permanganate</td><td>Fisher Scientific</td><td>P279-500</td><td>Chemical for testing</td></tr><tr><td>Sulphuric acid</td><td>Fisher Scientific</td><td>A300C-212</td><td>Chemical for testing</td></tr><tr><td>Silver sulfate</td><td>Fisher Scientific</td><td>S190-25</td><td>Chemical for testing</td></tr><tr><td>Raw ramie</td><td>Guangyuan limited liability company, Changde, Hunan,China</td><td>&amp;mdash;&amp;mdash;</td><td>Raw materials</td></tr><tr><td>Electric-heated&amp;nbsp;thermostatic&amp;nbsp;water&amp;nbsp;bath</td><td>Senxin Experiment equipment limited liability company,Shanghai,China</td><td>DK-S28</td><td>Equipments for degumming</td></tr><tr><td>High temperature lbaorator dyeing machine</td><td>Shanghai Longda chemcials Crop.</td><td>RY-1261</td><td>Equipments for degumming</td></tr><tr><td>Thermometer</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>100 &amp;deg;C</td><td>Equipments for degumming</td></tr><tr><td>Vacuum suction machine</td><td>Yukang KNET ,Shanghai,China</td><td>SHB-IIIA</td><td>Equipments for testing Mg(OH)2 solublity</td></tr><tr><td>Suction flask</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>1000mL</td><td>Equipments for testing Mg(OH)2 solublity</td></tr><tr><td>Sand-core funnels</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>35mL</td><td>Equipments for testing Mg(OH)2 solublity</td></tr><tr><td>Oxidation reduction potential meter</td><td>Dapu instrument, Shanghai, China</td><td>MODEL 421</td><td>Equipments for testing ORP value</td></tr><tr><td>pH meter</td><td>Hanna instruments,Beijing,China</td><td>HI 98129</td><td>Equipments for testing pH value</td></tr><tr><td>Acid burette</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>50mL</td><td>Equipments for testing H2O2 content</td></tr><tr><td>Flask</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>250 mL/500 mL</td><td>Equipments for testing H&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;2&lt;/sub&gt; content;&amp;nbsp; residual gums content</td></tr><tr><td>Electric furnace</td><td>Jiangyi Experiment instruments limited liability company,Shanghai,China</td><td>800-2000W</td><td>Equipments for testing residual gums content</td></tr><tr><td>Reflux condensing tube</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>250mL</td><td>Equipments for testing residual gums content; COD value</td></tr><tr><td>Fiber cutter (40mm)</td><td>Changzhou No.2 Textile Machine Co.,Ltd</td><td>Y171A</td><td>Equipments for testing fiber density</td></tr><tr><td>Ostwald viscometer</td><td>Taizhou, jiaojiang, glass instruments company</td><td>0.6mm</td><td>Equipments for testing fiber PD value</td></tr><tr><td>Spherical fat extractor</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>250mL</td><td>Equipments for testing fiber PD value</td></tr><tr><td>Soxhlet extractor</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>250mL</td><td>Equipments for testing fiber PD value</td></tr><tr><td>Torsion&amp;nbsp;balance</td><td>Liangping instrucments Co.,Ltd,Shanghai, China</td><td>JN-B</td><td>Equipments for testing fiber density</td></tr><tr><td>Fiber strength instrument</td><td>Xinxian instruments, shanghai,China</td><td>XQ-2</td><td>Equipments for testing fiber tensile property</td></tr><tr><td>Tension clamp</td><td>Depu textile technology Co.,Ltd, Changzhou, jiangsu, China</td><td>0.3cN/dtex</td><td>Equipments for testing fiber tensile property</td></tr><tr><td>COD&amp;nbsp;thermostatic&amp;nbsp;heater</td><td>Qiangdao Xuyu environment protection technology Lit company</td><td>DL-801A</td><td>Equipments for testing COD value</td></tr><tr><td>FTIR</td><td>Thermo Fisher, America</td><td>Nicolet</td><td>FTIR analysis</td></tr><tr><td>XRD</td><td>Rigaku, Japan</td><td>D/max-2550 PC</td><td>XRD analysis</td></tr><tr><td>Electronic balance</td><td>Shanghai jingtian Electronic instrument Co.,Ltd</td><td>FA2004A</td><td>Generral equipments</td></tr><tr><td>Drying oven</td><td>Tonglixinda&amp;nbsp; instruments, Tianjin,China</td><td>101-2AS</td><td>Generral equipments</td></tr><tr><td>Weighing bottle</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>50x30</td><td>Generral equipments</td></tr><tr><td>Beaker</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>500mL</td><td>Generral equipments</td></tr><tr><td>Sample sieve</td><td>Xiaojin hardware instruments Co.,Ltd, Shangyu, Zhejiang</td><td>120 mesh</td><td>Generral equipments</td></tr><tr><td>Glass rod</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>&amp;mdash;&amp;mdash;</td><td>Generral equipments</td></tr><tr><td>Cylinder</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>250mL, 50mL</td><td>Generral equipments</td></tr><tr><td>Pipette</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>5mL, 10mL</td><td>Generral equipments</td></tr><tr><td>Rubber&amp;nbsp;suction&amp;nbsp;bulb</td><td>Sichuan Shubo (group)Co.,Ltd</td><td>&amp;mdash;&amp;mdash;</td><td>Generral equipments</td></tr><tr><td>Orign</td><td>OriginLab</td><td>8.0</td><td>Software for figure drawing</td></tr></tbody></table>

extraction of ramie fiber in alkali hydrogen peroxide system supported by controlled-release alkali source

本协议演示了一种在受控释碱源支持的碱过氧化氢系统中, 在苎麻纤维上精练的方法。苎麻提取纤维是一种重要的纺织材料。在以前的研究中, 苎麻纤维被提取的碱过氧化氢系统只支持氢氧化钠。然而, 由于氢氧化钠的强碱性, 过氧化氢的氧化反应速度难以控制, 从而对处理后的纤维造成很大的损害。在本协议中, 一种由氢氧化钠和氢氧化镁组成的控释碱源, 用于提供碱性条件和缓冲碱氢 peroxidesystem 的 pH 值。氢氧化镁的取代率可以调节过氧化氢体系的 pH 值, 对纤维性能有很大的影响。ph 值和氧化还原电位值, 代表了碱过氧化氢系统的氧化能力, 分别采用 ph 计和检测仪进行监测。采用高锰酸钾4滴定法测定了萃取过程中碱过氧化氢体系中的剩余过氧化氢含量, 以及纤维萃取后废水的化学需氧量 (COD) 值。用精密电子天平测量纤维的收率, 用化学分析法测定纤维的残余牙龈。用乌粘度计测定了纤维的聚合度 (PD 值)。用纤维强度仪测定纤维的拉伸性能, 包括韧性、伸长率和断裂。利用傅里叶变换红外光谱和 X 射线衍射对纤维的官能团和晶体性质进行了表征。该方案证明, 控释碱源能改善碱性过氧化氢体系中提取的纤维的性能。

研究了在蒸馏水和脱胶溶液中 Mg (OH)2的溶解度 (图 1)。测试了镁 (OH)2取代率对脱胶溶液 pH 值和可解性值 (图 2) 的影响。用不同 Mg (OH)2替代率计算了纤维脱胶的脱胶率和残余牙龈 (图 3)。用 DP 值、结晶度、纤维拉伸性能 (图 4) 和废水 COD 值 (图 5<...

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Extraction of Ramie Fiber in Alkali Hydrogen Peroxide System Supported by Controlled-release Alkali Source

缓释碱源负载碱性过氧化氢体系中苎麻纤维的提取

本文介绍了一种在受控释碱源支持的碱性过氧化氢体系中提取苎麻纤维的方案。

This protocol demonstrates a method for ramie fiber extraction by scouring raw ramie in an alkali hydrogen peroxide system supported by a ...

extraction-ramie-fiber-alkali-hydrogen-peroxide-system-supported

Research

JoVE Journal

Chemistry

11.3K 次观看.  Donghua University. 本文介绍了一种在受控释碱源支持的碱性过氧化氢体系中提取苎麻纤维的方案。

视频: Extraction of Ramie Fiber in Alkali Hydrogen Peroxide System Supported by Controlled-release Alkali Source

Extraction of Structural Extracellular Polymeric Substances from Aerobic Granular Sludge

To evaluate and develop methodologies for the extraction of gel-forming extracellular polymeric substances (EPS), EPS from aerobic granular sludge (AGS) was extracted using six different methods (centrifugation, sonication, ethylenediaminetetraacetic acid (EDTA), formamide with sodium hydroxide (NaOH), formaldehyde with NaOH and sodium carbonate (Na2CO3) with heat and constant mixing). AGS was collected from a pilot wastewater treatment reactor. The ionic gel-forming property of the extracted EPS of the six different extraction methods was tested with calcium ions (Ca2+). From the six extraction methods used, only the Na2CO3 extraction could solubilize the hydrogel matrix of AGS. The alginate-like extracellular polymers (ALE) recovered with this method formed ionic gel beads with Ca2+. The Ca2+-ALE beads were stable in EDTA, formamide with NaOH and formaldehyde with NaOH, indicating that ALE are one part of the structural polymers in EPS. It is recommended to use an extraction method that combines physical and chemical treatment to solubilize AGS and extract structural EPS.

The protocol provides a methodology to solubilize aerobic granular sludge in order to extract alginate-like extracellular polymers (ALE).

从好氧颗粒污泥结构胞外聚合物的提取

To evaluate and develop methodologies for the extraction of gel-forming extracellular polymeric substances (EPS), EPS from aerobic granular sludge (AGS) ...

科研

环境科学

Highly Stable, Functional Hairy Nanoparticles and Biopolymers from Wood Fibers: Towards Sustainable Nanotechnology

Nanoparticles, as one of the key materials in nanotechnology and nanomedicine, have gained significant importance during the past decade. While metal-based nanoparticles are associated with synthetic and environmental hassles, cellulose introduces a green, sustainable alternative for nanoparticle synthesis. Here, we present the chemical synthesis and separation procedures to produce new classes of hairy nanoparticles (bearing both amorphous and crystalline regions) and biopolymers based on wood fibers. Through periodate oxidation of soft wood pulp, the glucose ring of cellulose is opened at the C2-C3 bond to form 2,3-dialdehyde groups. Further heating of the partially oxidized fibers (e.g., T = 80 &#176;C) results in three products, namely fibrous oxidized cellulose, sterically stabilized nanocrystalline cellulose (SNCC), and dissolved dialdehyde modified cellulose (DAMC), which are well separated by intermittent centrifugation and co-solvent addition. The partially oxidized fibers (without heating) were used as a highly reactive intermediate to react with chlorite for converting almost all aldehyde to carboxyl groups. Co-solvent precipitation and centrifugation resulted in electrosterically stabilized nanocrystalline cellulose (ENCC) and dicarboxylated cellulose (DCC). The aldehyde content of SNCC and consequently surface charge of ENCC (carboxyl content) were precisely controlled by controlling the periodate oxidation reaction time, resulting in highly stable nanoparticles bearing more than 7 mmol functional groups per gram of nanoparticles (e.g., as compared to conventional NCC bearing &#60;&#60; 1 mmol functional group/g). Atomic force microscopy (AFM), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) attested to the rod-like morphology. Conductometric titration, Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), dynamic light scattering (DLS), electrokinetic-sonic-amplitude (ESA) and acoustic attenuation spectroscopy shed light on the superior properties of these nanomaterials.

Synthesis schemes to prepare highly stable wood fiber-based hairy nanoparticles and functional cellulose-based biopolymers have been detailed.

高稳定性，功能性毛纳米粒子和木纤维生物聚合物:迈向可持续纳米技术

Nanoparticles, as one of the key materials in nanotechnology and nanomedicine, have gained significant importance during the past decade. While ...

化学

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, ...

Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables the silk proteins to be compact and ordered by shearing and elongation forces. Here, a biomimetic microfluidic channel was designed to mimic the specific geometry of the spinning duct of the silkworm. Regenerated silk fibroin (RSF) spinning doped with high concentration, was extruded through the microchannel to dry-spin fibers at ambient temperature and pressure. In the post-treated process, the as-spun fibers were drawn and stored in ethanol aqueous solution. Synchrotron radiation wide-angle X-ray diffraction (SR-WAXD) technology was used to investigate the microstructure of single RSF fibers, which were fixed to a sample holder with the RSF fiber axis normal to the microbeam of the X-ray. The crystallinity, crystallite size, and crystalline orientation of the fiber were calculated from the WAXD data. The diffraction arcs near the equator of the two-dimensional WAXD pattern indicate that the post-treated RSF fiber has a high orientation degree.

A protocol for the microfluidic spinning and microstructure characterization of regenerated silk fibroin monofilament is presented.

微流控干纺及再生丝素纤维的表征

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables ...

Manufacturing Of Robust Natural Fiber Preforms Utilizing Bacterial Cellulose as Binder

A novel method of manufacturing rigid and robust natural fiber preforms is presented here. This method is based on a papermaking process, whereby loose and short sisal fibers are dispersed into a water suspension containing bacterial cellulose. The fiber and nanocellulose suspension is then filtered (using vacuum or gravity) and the wet filter cake pressed to squeeze out any excess water, followed by a drying step. This will result in the hornification of the bacterial cellulose network, holding the loose natural fibers together.
Our method is specially suited for the manufacturing of rigid and robust preforms of hydrophilic fibers. The porous and hydrophilic nature of such fibers results in significant water uptake, drawing in the bacterial cellulose dispersed in the suspension. The bacterial cellulose will then be filtered against the surface of these fibers, forming a bacterial cellulose coating. When the loose fiber-bacterial cellulose suspension is filtered and dried, the adjacent bacterial cellulose forms a network and hornified to hold the otherwise loose fibers together.
The introduction of bacterial cellulose into the preform resulted in a significant increase of the mechanical properties of the fiber preforms. This can be attributed to the high stiffness and strength of the bacterial cellulose network. With this preform, renewable high performance hierarchical composites can also be manufactured by using conventional composite production methods, such as resin film infusion (RFI) or resin transfer molding (RTM). Here, we also describe the manufacturing of renewable hierarchical composites using double bag vacuum assisted resin infusion.

We present a novel method of manufacturing rigid and robust short natural fiber preforms using a papermaking process. Bacterial cellulose acts simultaneously as the binder for the loose fibers and provides rigidity to the fiber preforms. These preforms can be infused with a resin to produce truly green hierarchical composites.

制造业的鲁棒天然纤维预制体的利用细菌纤维素为粘结剂

A novel method of manufacturing rigid and robust natural fiber preforms is presented here. This method is based on a papermaking process, whereby loose ...

生物工程

Deposition of Porous Sorbents on Fabric Supports

A microwave deposition technique for silanes, previously described for production of oleophobic fabrics, is adapted to provide a fabric support material that can be subsequently treated by dip coating. Dip coating with a sol preparation provides a supported porous layer on the fabric. In this case, the porous layer is a porphyrin functionalized sorbent system based on a powdered material that has been demonstrated previously for the capture and conversion of phosgene. A representative coating is applied to cotton fabric at a loading level of 10 mg/g. This coating has minimal impact on water vapor transport through the fabric (93% of the support fabric rate) while significantly reducing transport of 2-chloroethyl ethyl sulfide (CEES) through the material (7% of support fabric rate). The described approaches are suitable for use with other fabrics providing amine and hydroxyl groups for modification and can be used in combination with other sol preparations to produce varying functionality.

This report details a microwave-initiated approach for deposition of porphyrin functionalized porous organosilicate sorbents on a cotton fabric and demonstrates reduction in 2-chloroethyl ethyl sulfide (CEES) transport through the fabric resulting from this treatment.

织物支架上多孔吸附剂的沉积

A microwave deposition technique for silanes, previously described for production of oleophobic fabrics, is adapted to provide a fabric support material ...

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 ...

Reactive Inkjet Printing and Propulsion Analysis of Silk-based Self-propelled Micro-stirrers

In this study, a protocol for using reactive inkjet printing to fabricate enzymatically propelled silk swimmers with well-defined shapes is reported. The resulting devices are an example of self-propelled objects capable of generating motion without external actuation and have potential applications in medicine and environmental sciences for a variety of purposes ranging from micro-stirring, targeted therapeutic delivery, to water remediation (e.g., cleaning oil spills). This method employs reactive inkjet printing to generate well-defined small-scale solid silk structures by converting water soluble regenerated silk fibroin (silk I) to insoluble silk fibroin (silk II). These structures are also selectively doped in specific regions with the enzyme catalase in order to produce motion via bubble generation and detachment. The number of layers printed determines the three-dimensional (3D) structure of the device, and so here the effect of this parameter on the propulsive trajectories is reported. The results demonstrate the ability to tune the motion by varying the dimensions of the printed structures.

This protocol demonstrates the ability to utilize reactive inkjet printing to print self-motile biocompatible and environmentally friendly micro-stirrers for use in biomedical and environmental applications.

基于丝绸的自行式微搅拌器的反应式喷墨打印及推进分析

In this study, a protocol for using reactive inkjet printing to fabricate enzymatically propelled silk swimmers with well-defined shapes is reported. The ...

Fabricating Degradable Thermoresponsive Hydrogels on Multiple Length Scales via Reactive Extrusion, Microfluidics, Self-assembly, and Electrospinning

While various smart materials have been explored for a variety of biomedical applications (e.g., drug delivery, tissue engineering, bioimaging, etc.), their ultimate clinical use has been hampered by the lack of biologically-relevant degradation observed for most smart materials. This is particularly true for temperature-responsive hydrogels, which are almost uniformly based on polymers that are functionally non-degradable (e.g., poly(N-isopropylacrylamide) (PNIPAM) or poly(oligoethylene glycol methacrylate) (POEGMA)). As such, to effectively translate the potential of thermoresponsive hydrogels to the challenges of remote-controlled or metabolism-regulated drug delivery, cell scaffolds with tunable cell-material interactions, theranostic materials with the potential for both imaging and drug delivery, and other such applications, a method is required to render the hydrogels (if not fully degradable) at least capable of renal clearance following the required lifetime of the material. To that end, this protocol describes the preparation of hydrolytically-degradable hydrazone-crosslinked hydrogels on multiple length scales based on the reaction between hydrazide and aldehyde-functionalized PNIPAM or POEGMA oligomers with molecular weights below the renal filtration limit. Specifically, methods to fabricate degradable thermoresponsive bulk hydrogels (using a double barrel syringe technique), hydrogel particles (on both the microscale through the use of a microfluidics platform facilitating simultaneous mixing and emulsification of the precursor polymers and the nanoscale through the use of a thermally-driven self-assembly and cross-linking method), and hydrogel nanofibers (using a reactive electrospinning strategy) are described. In each case, hydrogels with temperature-responsive properties similar to those achieved via conventional free radical cross-linking processes can be achieved, but the hydrazone cross-linked network can be degraded over time to re-form the oligomeric precursor polymers and enable clearance. As such, we anticipate these methods (which may be generically applied to any synthetic water-soluble polymer, not just smart materials) will enable easier translation of synthetic smart materials to clinical applications.

Protocols are described for the fabrication of degradable thermoresponsive hydrogels based on hydrazone cross-linking of polymeric oligomers on the bulk scale, microscale, and nanoscale, the latter for preparation of both gel nanoparticles and nanofibers.

通过反应挤出、微流体、自组装和电纺丝制备多长尺度可降解 Thermoresponsive 水凝胶

While various smart materials have been explored for a variety of biomedical applications (e.g., drug delivery, tissue engineering, bioimaging, etc.), ...

利用 Gracilaria gracilis:可持续创新的生物活性潜力

Valorization of the Red Seaweed Gracilaria gracilis Through a Biorefinery Approach

The interest in seaweeds as an abundant feedstock to obtain valuable and multitarget bioactive ingredients is continuously growing. In this work, we explore the potential of Gracilaria gracilis, an edible red seaweed cultivated worldwide for its commercial interest as a source of agar and other ingredients for cosmetic, pharmacological, food, and feed applications.
G. gracilis growth conditions were optimized through vegetative propagation and sporulation while manipulating the physicochemical conditions to achieve a large biomass stock. Green extraction methodologies with ethanol and water were performed over the seaweed biomass. The bioactive potential of extracts was assessed through a set of in vitro assays concerning their cytotoxicity, antioxidant, and antimicrobial properties. Additionally, dried seaweed biomass was incorporated into pasta formulations to increase food&#39;s nutritional value. Pigments extracted from G. gracilis have also been incorporated into yogurt as a natural colorant, and their stability was evaluated. Both products were submitted to the appreciation of a semi-trained sensorial panel aiming to achieve the best final formulation before reaching the market.
Results support the versatility of G. gracilis whether it is applied as a whole biomass, extracts and/or pigments. Through implementing several optimized protocols, this work allows the development of products with the potential to profit the food, cosmetic, and aquaculture markets, promoting environmental sustainability and a blue circular economy.
Moreover, and in line with a biorefinery approach, the residual seaweed biomass will be used as biostimulant for plant growth or converted to carbon materials to be used in water purification of the in-house aquaculture systems of MARE-Polytechnic of Leiria, Portugal.

作者聚焦:探索海藻的生物活性化合物以促进工业的可持续创新 

Here, we describe several protocols aiming at an integrated valorization of Gracilaria gracilis: wild species harvesting, in-house growth, and extraction of bioactive ingredients. The extracts&#39; antioxidant, antimicrobial, and cytotoxic effects are evaluated, along with the nutritional and stability assessment of food enriched with whole seaweed biomass and pigments.

通过生物精炼方法对红海藻 gracilaria gracilis 进行增值

The interest in seaweeds as an abundant feedstock to obtain valuable and multitarget bioactive ingredients is continuously growing. In this work, we ...