Name: preparation of expanded chitin foams and their use in the removal of aqueous copper
Uploaded: 2021-02-27T15:00:00
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这项研究由作战能力发展指挥部陆军研究实验室（合作协议编号W911NF-15-2-0020）赞助。本材料中表达的任何意见、发现和结论或建议都是作者的意见，并不一定反映陆军研究实验室的观点。
我们感谢蒙大拿理工大学高级材料处理中心 （CAMP） 使用本研究所需的一些专用设备。我们还感谢加里·怀斯、南希·奥耶、里克·拉杜瑟尔、约翰·柯特利和凯瑟琳·佐德罗的技术援助和有益的讨论。

1. 准备扩大的辣椒
<ol><li>准备一个 250 mL 溶液 5 wt% LiCl 在二甲基乙酰胺 （DMAc） 警告：溶剂 DMAc 是一种易燃刺激物，可能会损害生育能力并导致出生缺陷。使用防化手套和护目镜在烟雾罩中处理 DMAc，以避免与皮肤和眼睛接触。<ol>
<li>加入 15 克 LiCl 和 285 克 （268 mL） 的 DMAc 到 500 mL Erlenmeyer 烧瓶中，然后放置 50 mm 聚酯氟乙烯 （PTFE） 衬里磁搅拌棒。</li>
		<li>用橡胶隔膜盖上烧瓶，放在加热搅拌...

<ol>
	<li>Rinaudo, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chitin+and+chitosan:+Properties+and+applications.">Chitin and chitosan: Properties and applications.</a> Progress in Polymer Science. 31 (7), 603-632 (2006).</li><li>Percot, A., Viton, C., Domard, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Optimization+of+chitin+extraction+from+shrimp+shells.">Optimization of chitin extraction from shrimp shells.</a> Biomacromolecules. 4 (1), 12-18 (2003).</li><li>Austin, P. 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L., Cunha, J. M., Calgaro, C. O., Tanabe, E. H., Bertuol, D. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+modification+of+chitin+using+ultrasound-assisted+and+supercritical+CO2+technologies+for+cobalt+adsorption.">Surface modification of chitin using ultrasound-assisted and supercritical CO2 technologies for cobalt adsorption.</a> Journal of Hazardous Materials. 295, 29-36 (2015).</li><li>Phongying, S., Aiba, S., Chirachanchai, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+chitosan+nanoscaffold+formation+via+chitin+whiskers.">Direct chitosan nanoscaffold formation via chitin whiskers.</a> Polymer. 48 (1), 393-400 (2007).</li><li>Tan, T. S., Chin, H. Y., Tsai, M. L., Liu, C. 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建议的奇丁泡沫制造方法允许生产这种泡沫，而无需专门的设备或技术。奇廷泡沫的生产依赖于奇丁醇凝胶内氢化钠的悬浮。与大气中的水接触通过分解氢化钠诱导气质基质的凝胶和氢气的演化。因此，制备的关键步骤是（1）形成溶胶，（2）在无水条件下引入氢化钠，（3）大气水与奇丁醇凝胶和氢化钠悬浮剂的反应。
第三步有两个重要的限制。首先，该过程扩展得很差。?...

奇廷是一种机械坚固和化学惰性生物聚合物，仅次于天然丰度1中的纤维素。它是节肢动物外骨骼和真菌和酵母2细胞壁的主要成分。奇丁与纤维素相似，但每个单体的羟基组被乙酰胺组（图1A，B）所取代。这种差异增加了相邻聚合物链之间的氢粘结强度，并赋予奇丁其特有的结构弹性和化学惰性2，3。由于其特性和丰富性，奇廷吸引了巨大的工业和学术兴趣。它已被研究为组织生长的支架4，5，6，作为复合材料的成分7，8，9，10，11，并作为支持吸附剂和催化剂11，12，13，14。其化学稳定性，特别是使奇丁吸引吸附应用，涉及条件不适宜常见的吸附剂14。此外，丰富的胺组使奇丁对金属离子15的有效吸附。然而，酸性条件下胺组的质子会降低奇丁16的金属吸附能力。一个成功的策略是引入更耐质子17，18的吸附位点。相反，这里描述了一个简单的方法来增加特定的表面积，因此，在奇廷吸附点的数量。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/62301/62301fig01.jpg"> 图1。化学结构。（A）纤维素， （B）奇廷， （C）奇托桑。<a href="https://www.jove.com/files/ftp_upload/62301/62301fig01large.jpg" target="_blank">请点击这里查看这个数字的更大版本。</a>
尽管它有许多潜在的用途，但奇丁的利用不足。奇廷加工具有挑战性，因为它在大多数溶剂中的溶解性较低。其在催化和吸附中的使用的主要限制是其低特异性表面积。而典型的碳和金属氧化物支架有特定的表面积在顺序102-103 m2/g，商业辣椒片有表面积在10米2/克19，20，21的顺序。将辣椒素扩展到泡沫的方法是存在的，但它们总是依赖于高温高压、强酸和碱基，或代表重大进入屏障的专用设备，这些设备代表着重要的进入屏障5、21、22、23、24、25。此外，这些方法倾向于去乙酰丁，形成甲壳素（图1C）- 一种更可溶性和反应性生物聚合物5，25，26。
其中，介绍了一种将奇丁扩展到固体泡沫、增加其特定表面积和吸附能力以及保持其化学完整性的方法。该方法依赖于气体从奇廷凝胶内的快速演化，不需要专门的设备。扩大的辣椒素的吸附能力增加，用水Cu2+证明 - 当地地下水26中的常见污染物。
<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always"><tbody>
<tr>
<td></td>
			<td>单位</td>
			<td>整洁的弗莱克</td>
			<td>烤泡沫</td>
			<td>嗜血泡沫</td>
		</tr>
<tr>
<td>结晶</td>
			<td>%</td>
			<td>88</td>
			<td>74</td>
			<td>58</td>
		</tr>
<tr>
<td>晶体大小</td>
			<td>纳米</td>
			<td>6.5</td>
			<td>4.4</td>
			<td>4.4</td>
		</tr>
<tr>
<td>表面积</td>
			<td>m2/g</td>
			<td>12.6 ± 2.1</td>
			<td>43.1 ± 0.2</td>
			<td>73.9 ± 0.2</td>
		</tr>
<tr>
<td>库塔克</td>
			<td>毫克/克</td>
			<td>13.8 ± 2.9</td>
			<td>48.6 ± 1.9</td>
			<td>73.1 ± 2.0</td>
		</tr>
<tr>
<td>库塔克</td>
			<td>原子/纳米2
</td>
			<td>10.5 ± 2.8</td>
			<td>10.7 ± 0.4</td>
			<td>9.4 ± 0.3</td>
		</tr>
</tbody></table>表1。材料属性摘要。 与整洁的奇丁片相比，奇廷泡沫的晶体度和晶体大小较低。然而，奇丁泡沫的特定表面积和Cu吸收量比整齐的奇丁片高。

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>Ammonium bicarbonate</td>
			<td>Sigma-Aldrich</td>
			<td>9830</td>
			<td>NH4HCO3, &#8805;99.5 %</td>
		</tr>
		<tr>
			<td>Chitin</td>
			<td>Sigma-Aldrich</td>
			<td>C7170</td>
			<td>Pandalus borealis, practical grade</td>
		</tr>
		<tr>
			<td>Colorimeter</td>
			<td>Hanna Instruments</td>
			<td>HI83399-01</td>
			<td>Photometer for wastewater analysis</td>
		</tr>
		<tr>
			<td>Copper High Range Checker</td>
			<td>Hanna Instruments</td>
			<td>HI702</td>
			<td>Bicinchoninate colorimetric titration</td>
		</tr>
		<tr>
			<td>Copper nitrate hydrate&#160;</td>
			<td>Sigma-Aldrich</td>
			<td>223395</td>
			<td>Cu(NO3)2 &#183; 2.5 H2O, 98 %</td>
		</tr>
		<tr>
			<td>Dimethylacetamide (DMAc)</td>
			<td>Sigma-Aldrich</td>
			<td>271012</td>
			<td>Anhydrous, 99.8 %</td>
		</tr>
		<tr>
			<td>IR Spectrophotometer</td>
			<td>Thermo Nicolet</td>
			<td>Nexus 670</td>
			<td>Fitted with an ATR cell</td>
		</tr>
		<tr>
			<td>Lithium chloride</td>
			<td>Sigma-Aldrich</td>
			<td>310468</td>
			<td>LiCl, &#8805;99 %</td>
		</tr>
		<tr>
			<td>N2 Physisorption Apparatus</td>
			<td>Micromeritics</td>
			<td>Tristar II</td>
			<td></td>
		</tr>
		<tr>
			<td>Nitric acid</td>
			<td>BDH</td>
			<td>BDH7208-1</td>
			<td>HNO3, 0.1 N</td>
		</tr>
		<tr>
			<td>Scanning electron microscope</td>
			<td>Zeiss LEO</td>
			<td>1430 VP</td>
			<td>15 kV, secondary electron detector, 29-31 mm working distance</td>
		</tr>
		<tr>
			<td>Sodium hydride</td>
			<td>Sigma-Aldrich</td>
			<td>223441</td>
			<td>NaH, packed in mineral oil, 90 %</td>
		</tr>
		<tr>
			<td>Thermogravimetric analyzer</td>
			<td>TA Instruments</td>
			<td>Q500</td>
			<td>100 ml/min N2, 10 &#176;C/min to 800 &#176;C</td>
		</tr>
		<tr>
			<td>Water Purification System</td>
			<td>Millipore</td>
			<td>Milli-Q</td>
			<td>Type A water (18 M&#937;)</td>
		</tr>
		<tr>
			<td>X-Ray Diffractometer</td>
			<td>Rigaku</td>
			<td>Ultima IV</td>
			<td>Cu K-&#945; radiation, 8.04 keV</td>
		</tr>
	</tbody>
</table>

preparation of expanded chitin foams and their use in the removal of aqueous copper

奇廷是一种开发不足、自然丰富、机械坚固、耐化学的生物聚合物。这些品质在吸附剂中是可取的，但奇丁缺乏必要的特定表面积，其修改涉及专门的技术和设备。这里描述了一种新的化学程序，将来自虾壳废物的辣椒片膨胀成表面积较高的泡沫。这个过程依赖于H2 气体的进化，从水的反应与NaH被困在一个奇丁凝胶。制备方法不需要专用设备。粉末X射线衍射和N2-物理吸收表明晶体大小从6.6纳米减少到4.4纳米，特定表面积从12.6±2.1米2/g增加到73.9±0.2米2/克。然而，红外光谱学和热重力学分析表明，这个过程不会改变奇廷的化学特性。扩大的奇丁的特定Cu吸附能力与特定表面积成正比，从13.8±2.9毫克/克增加到73.1±2.0毫克/克。然而，Cu吸附能力作为表面密度保持相对恒定，平均为10.1±0.8原子/nm2，这再次表明甲酰丁的化学特性没有变化。这种方法提供了在不牺牲其理想特性的情况下将奇丁转化为更高表面积材料的方法。虽然这里的奇丁泡沫被描述为吸附剂，但它可以设想为催化剂支撑、热绝缘体和结构材料。

无论干燥方法如何，扩展的奇廷都表现出相同的形态。图3显示整齐的奇丁片（图3A1），烤箱干膨胀的奇丁（图3B1）和利血性扩大奇丁（图3C3）的图像。虽然整洁的薄片有粗砂的外观，但膨胀的辣椒泡沫有弹出玉米的核状外观。扫描电子显微图在较小的尺度上也显示出类似的变化。虽然整洁的奇丁片（<stro...

Watch this Scientific Journal Video about Preparation of Expanded Chitin Foams and their Use in the Removal of Aqueous Copper at JoVE.com

Preparation of Expanded Chitin Foams and their Use in the Removal of Aqueous Copper

这项研究描述了一种通过不需要专门设备的化学技术将奇丁扩展成泡沫的方法。

准备扩大的奇廷泡沫及其用于去除水中的铜

Chitin is an underexploited, naturally abundant, mechanically robust, and chemically resistant biopolymer. These qualities are desirable in an adsorbent, ...

该协议允许奇廷，一种大容量的废料，这是出了名的难以与之合作的新的物理转换。该技术的主要优点是处理方法简单。因为它不需要专门的材料。只有化学实验室中常见的基本设备。我们用奇丁演示了这种方法，但这项技术可以修改，以创建其他聚合物和生物聚合物的扩展版本，形成凝胶。在这种技术的最简单版本中，如所示。耐心很重要。日差率会随着湿度的每日和季节性变化而变化。在准备扩大的辣椒素的前一天，在80摄氏度的烤箱中至少干燥1.2克辣椒片24小时。第二天早上，在烟雾罩和戴着防化学手套和护目镜，加入15克氯化锂到285克D-MAc，在一个500毫升的Erlenmeyer烧瓶中，含有50毫升PTFE线磁搅拌棒。用橡胶隔膜盖上烧瓶，放在加热搅拌盘上。放置时，通过隔膜对混合物进行温度探针，在 80 摄氏度下以每分钟 400 次旋转搅拌混合物，持续约 4 小时。当所有的氯化锂溶解后，在 5% 氯化锂 D-MAc 溶液中加入 1 克烤箱干辣椒片。并将产生的溶液转移到 500 毫升圆形底部烧瓶中，其中含有 50 毫升 PTFE 衬里磁搅拌棒。将带橡胶隔膜的烧瓶盖放在搅拌热块上。用针刺穿隔膜，使烧瓶在80摄氏度下通风和加热溶液，以每分钟400次旋转搅拌24至48小时。当所有的奇丁溶解后，让由此产生的奇丁醇凝胶冷却到室温约一小时，搅拌。一旦溶液达到室温，将烧瓶放入冰浴中，持续搅拌约20分钟，直到温度稳定下来。准备100毫升的氢化钠和D-MAc泥浆。戴着防化手套和护目镜，在烟气罩中清洗从矿物油储存中取出的大约1克氢化钠。3 次，每次洗涤 10 毫升六烷。将0.82克洗涤钠氢化物加入新鲜的250毫升Erlenmeyer烧瓶中，在PTFE线磁搅拌棒中含有100毫升D-MAc，并旋转混合物，产生氢化钠D-MAc浆料。要形成气凝胶，请将整个体积的氢化钠泥浆添加到冷却的溶胶中，同时大力搅拌凝胶溶液。然后更换盖子，继续以每分钟400次旋转搅拌混合物，直到凝胶形成。凝胶形成后，在烟气罩中将 100 毫升的去离子水加入烧瓶中，并从烧瓶中取出膨胀的奇丁泡沫，如有必要，将泡沫分解成碎片。将泡沫与1000毫升的去离子水一起放入足够大的结晶盘中，以容纳泡沫。将分离的凝胶冲洗3次，每次洗涤500毫升的去离子水，然后浸泡在1000毫升的去离子水中，500毫升甲醇和1000毫升新鲜的去离子水中，每次浸泡24次。最后一次去离子水洗后，让凝胶干燥24至48小时。然后，在环境空气或嗜热剂的照热器下，在烤箱中干燥48小时，零下43摄氏度，压力0.024毫巴，干燥48小时。当形成固体气质泡沫时，使用砂浆和砂浆将泡沫研磨成细粉末。干燥前，揉合辣椒片，表现出核心沙的外观。干燥后，无论方法如何，膨胀的奇丁形态都类似于爆米花的内核。扫描电子显微图显示，揉合奇丁是一种紧凑的密集结构，而膨胀的奇丁，类似于皱褶的纸张或皱纹的床单。在X射线衍射研究中，揉合奇丁显示一个与晶体平面相对应的19.3度的强峰值。烘烤后强度降低，或嗜血。建议干燥改变奇丁的晶体指数。测量从氮物理吸收等温体获得的特定表面积，显示最大的吸收量，为扩大的泡沫。确认这些样品的更开放和多孔结构。尽管这些形态的变化，膨胀过程似乎并不影响奇廷的化学结构。正如这些具有代表性的红外光谱中观察到的。在热重力分析之后，也注意到了类似的观测结果。随着所有三个样品的热分解的开始，在260摄氏度下发生，而最大分解率发生在较高温度下的奇丁片，由于其形态更紧凑。特定表面积的增加伴随着奇廷最大铜吸收量的预期增加。然而，当铜吸收由表面积正常化时，吸收中的这些差异就会消失。重要的是要记住，D-MAc和NAH是危险化学品，必须小心处理。始终在烟罩中工作，并佩戴相应的个人防护装备。我们收集的有限氮吸附等温，只能提供特定的表面积。全氮吸收等温，可以提供孔隙信息，这是确定大小选择应用的有用性的关键。

Research

JoVE Journal

Chemistry

Preparation and Use of Samarium Diiodide (SmI2) in Organic Synthesis: The Mechanistic Role of HMPA and Ni(II) Salts in the Samarium Barbier Reaction

Preparation and Use of Samarium Diiodide SmI2 in Organic Synthesis: The Mechanistic Role of HMPA and NiII Salts in the Samarium Barbier Reaction

二碘化钐的制备和使用（SMI<sub&gt; 2</sub&gt;）在有机合成中：HMPA和镍（II）盐的钐巴尔比耶反应的机理作用

Although initially considered an esoteric reagent, SmI2 has become a common tool for synthetic organic chemists. SmI2 is generated through the addition of ...

科研

化学

Preparation of Hydrophobic Metal-Organic Frameworks via Plasma Enhanced Chemical Vapor Deposition of Perfluoroalkanes for the Removal of Ammonia

增强型氟烷烃的化学气相沉积等离子通过疏水金属 - 有机骨架的制备氨的去除

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high ...

Exfoliation of Egyptian Blue and Han Blue, Two Alkali Earth Copper Silicate-based Pigments

埃及蓝色和汉蓝，两碱地球铜硅酸盐类颜料剥落

In a visualized example of the ancient past connecting with modern times, we describe the preparation and exfoliation of CaCuSi4O10 and BaCuSi4O10, the ...

Amide Coupling Reaction for the Synthesis of Bispyridine-based Ligands and Their Complexation to Platinum as Dinuclear Anticancer Agents

酰胺偶联反应为双吡啶基配体及其络合合成，以白金为双核抗癌药物

Amide coupling reactions can be used to synthesize bispyridine-based ligands for use as bridging linkers in multinuclear platinum anticancer drugs. ...

Preparation and Use of Carbonyl-decorated Carbenes in the Activation of White Phosphorus

羰基饰卡宾的白色磷的活化制备方法和用途

Here we present a protocol for the synthesis of two distinct carbonyl-decorated carbenes. Both carbenes can be prepared using nearly identical procedures ...

Preparation of a Corannulene-functionalized Hexahelicene by Copper(I)-catalyzed Alkyne-azide Cycloaddition of Nonplanar Polyaromatic Units

Preparation of a Corannulene-functionalized Hexahelicene by CopperI-catalyzed Alkyne-azide Cycloaddition of Nonplanar Polyaromatic Units

一个碗烯官能Hexahelicene的铜（Ⅰ）制备催化的非平面多环芳烃单位炔叠氮化物环加成

The main purpose of this video is to show 6 reaction steps of a convergent synthesis and prepare a complex molecule containing up to three nonplanar ...

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

蛋白质生物缀合物的合成<em&gt;通过</em&gt;半胱氨酸马来酰亚胺化学

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the ...

Visualization of Ambient Mass Spectrometry with the Use of Schlieren Photography

环境质谱可视化纹影摄影的使用

This manuscript outlines how to visualize mass spectrometry ambient ionization sources using schlieren photography. In order to properly optimize the mass ...

Synthesis of Cyclic Polymers and Characterization of Their Diffusive Motion in the Melt State at the Single Molecule Level

环状聚合物的合成及其在熔融状态扩散运动的表征在单分子水平

We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single ...

A Convenient Method for Extraction and Analysis with High-Pressure Liquid Chromatography of Catecholamine Neurotransmitters and Their Metabolites

用高压液相色谱法提取和分析儿茶酚胺神经递质及其代谢物的简便方法

The extraction and analysis of catecholamine neurotransmitters in biological fluids is of great importance in assessing nervous system function and ...