作者感谢荷兰科学研究组织（NWO）的财政支持（授予杰克·范·希恩德尔023.007.020）。

1. 绿色克诺维纳格尔凝结注射器醛对西纳皮尼奇酸与 5 摩尔% 碳酸氢铵
<ol><li>将马洛尼克酸（20.81 克，200.0 mmol）与注射器醛 （36.4 克， 200.0 mmol） 一起加入 250 mL 圆底烧瓶中。溶解两个成分在20.0 mL乙酸乙酸乙酸酯，并添加碳酸氢铵（790毫克，10.0毫米醇）到烧瓶。 注:为确保完全完成凝结反应，旋转蒸发器可用于蒸馏乙酸乙酸乙酯并浓缩反应混合物，从而产生无溶剂反应。</li>
	<li>将反应混合物在 90 °C 的开放烧瓶中保持 2 小时，而无需搅拌以完全转化为西纳皮尼酸。 注:在此反应期间，观察到一些形态变化。反应混合物从密集的灰色混合物变为溶解的黄色混合物，原因是水在反应的凝结步骤中形成。冷凝水蒸发后，反应混合物再次凝固，表示完全转换。</li>
	<li>在合成酶酸产品的处理中，将饱和的 NaHCO3溶液的残留物溶解在 100 mL 中。将溶液转移到烧饼上，然后使用 6 M HCl 将其酸化为 2 的 pH 值。 注:在添加饱和的AHCO3溶液时，原油产品溶解缓慢，需要一些时间和手动刮擦才能完全溶解。一旦完全溶解并转移到烧瓶中，6 M HCl 的酸性溶液就会被添加到滴中。西纳皮尼酸会迅速沉淀，CO2 气体的释放会导致产品发泡。</li>
	<li>通过真空过滤分离产生的残留物，然后用非盐化水清洗。 注意:此时，HPLC 可以分析产品的纯度。如果产品出现污染，则必须应用下一个净化步骤（例如再装层）。</li>
	<li>在水乙醇混合物（4:1，v/v）中重新安装后，通过真空过滤分离晶体。在真空烤箱中将残留物在 60 °C 下干燥，产生 42.56 克纯西纳平酸。 注:通过熔点分析和HPPC测量西纳皮尼酸的纯度。</li>
</ol>2. 将西纳平酸氢化为二氢酸与拉尼TM 镍。
<ol><li>用西纳平酸（33.6克，150 mmol）给450mL烧瓶（使用加氢装置）充电。将西纳平酸溶解在 300 mL 的 2 M NaOH 溶液中，在将烧瓶安装到设备之前加入 1.5 克镍浆（参见 材料表）。 注:反应混合物的颜色因添加碱性溶液而改变。新浪酸的晶体形式为黄色，但当基质脱质时，溶液的颜色将变为红色。镍的加入会使颜色变黑。</li>
	<li>用三巴氢气给反应堆加压，在80°C下机械地摇动反应三个小时。</li>
	<li>将反应堆冷却至室温，慢慢减压。用磁铁回收大部分镍催化剂，然后在减压下过滤溶液。 注:反应混合物应从红色变为绿色，过滤后可见。显著的颜色变化是因为结合系统被双键的加氢中断。</li>
	<li>用 4 M HCl 溶液将溶液酸化为 2 pH 值。随后，用乙酸酯（4倍50ml）进行萃取。在MgSO4干燥后，在减压下取出溶剂。在真空烤箱中将固体产品二氢酸干燥至 60 °C。 注:从理论上讲，多聚变反应可以在二氢酸上处理，但也有一些实际的缺点。由于分子结构，二氢酸升华在熔点以上。乙酰化反应可以执行，以防止升华和提高反应性。</li>
</ol>3. 乙酰酸乙酰化对乙酰化单体和寡聚体（聚合物）。
<ol><li>在 250 mL 圆底烧瓶中加入二氢酸（22.6 克，100 mmol），然后是醋酸氢化物（14.2 mL、150 mmol）和醋酸钠（0.82 克、10 mmol）。 注:二氢酸在室温下不会完全溶解在醋酸中。</li>
	<li>将溶液加热至 90 °C，同时搅拌一小时，将二氢酸完全转化为 4-乙氧二氢平酸及其乙酰化寡聚物。 注:所有产品仍溶解在醋酸氢化物中。为了增加4-乙氧二氢酸的总降水量，下一步添加少量水溶性溶剂。</li>
	<li>溶解25mL丙酮的固体，沉淀（溶剂-非溶剂）到250 mL的0.1M HCl，同时大力搅拌，并在真空下过滤。 注:最好的结果显示完全沉淀的白色，粘性固体。如果将产品溶液添加到 HCl 溶液中的速度过快，则产品仍作为棕色液体留在酸性溶液的底部。在这种情况下，用乙酸酯（4 倍 50 mL）提取整个产品溶液。在MgSO4上干燥后，在减压下取出乙酸乙酸乙酯。该产品是4-乙酰氧二氢酸和聚合物。</li>
</ol>4. 乙酰化单体和寡聚物的聚合。
<ol><li>加入单体，4-乙酰氧二氢酸（20.8克，100mmol），和前聚合物到100ml圆底烧瓶，并添加精细粉末NaOH（400毫克，10.0毫米醇）。在开放烧瓶中设定的温度为 140 °C 时加热反应混合物三小时，同时在 100 rpm 时搅拌。 注:在此反应期间，水和醋酸从开放的烧瓶凝结。可以测量蒸汽的pH值，以确认醋酸的凝结。反应产品的形态从熔融状态转变为紧凑的浅棕色产品。设置受氮流，以促进冷凝水的蒸发和防止氧化。由于混合物的粘度很高，这种反应通常用机械搅拌器搅拌。但是，磁搅拌器的使用已经足够了，在这个尺度上，这种差异可以忽略不计的。</li>
	<li>通过在烧瓶中加入锌（II）醋酸（180毫克，1 mmol）和25.0 mL的1，2-xylene，建立溶剂辅助聚合。将设定温度提高到 160 °C。 注:将设定温度提高到 160 °C，以确保 1，2-xylene 的回流和聚合的完全反应性。由于1，2-二甲苯的沸点，反应本身的温度保持在144°C。</li>
	<li>使用 Dean-Stark 头在 144 °C 下倒流混合物三小时，使用恒水和醋酸去除。 注:在加入1，2-xylene并将反应瓶加热到所需的温度后，试剂形成粘度较低的棕色泥浆。这种较低的粘度被认为有利于聚合物末组的移动性，促进反应性。</li>
	<li>冷却反应混合物，通过使用真空（<10mbar）去除1，2-xylene。 注:反应混合物在蒸发溶剂时凝固，变成白色固体。</li>
	<li>在聚合的最后阶段将温度提高到 240 °C，并应用高真空< 1 mbar 30 分钟。 注:在此步骤中，只有少量的冷凝水蒸发，因为在聚合阶段，只需要少量的冷凝剂来大幅提升链条长度。</li>
	<li>将聚合物聚S冷却至室温，并用甲醇清洗，以消除4-乙酰氧-二氢酸酸和前聚合物。获得的产品是浅棕色固体。 注:在此过程之后，GPC 和 DSC 将调查聚酯的链条长度和热性能。</li>
</ol>5. 1 M Naoh 中聚氨酯去聚合的代表程序:
<ol><li>将聚S精细研磨并筛成小于180μm的颗粒，以测量水解降解。 注:要将颗粒研磨到所需的大小，请使用砂浆和液氮冷却多 S，然后采用机械筛分步骤。</li>
	<li>装载多个试管，20毫克多S，并添加1.0 mL的1M NaOH溶液。在三种不同的温度（RT、50 和 80 °C）下孵育管子，使用受控环境孵化器摇床搅拌 500 rpm。 注意:使用具有多个条目的加热块/摇床进行此反应，以确保所有反应均在完全相同的（热）条件下发生。</li>
	<li>以 1.0 mL 的 0.5 M H2SO4 定期中和试管，冷却后加入 2.0 mL 甲醇。 注:少量的多S和只有1.0 mL的1M NaOH被使用，因为这些浓度，在添加甲醇后，可以直接注射到HPPL，不需要任何进一步稀释。</li>
	<li>使用 0.45 μm PTFE 注射器过滤器过滤所有样品，然后使用自动采样器在 HPLC 上注射 （20 μL）。监测 ±254 nm 的吸收量，并计算已知二氢酸标准溶液校准曲线的浓度。 注:校准曲线的标准溶液应与去聚合后的工作用同一溶剂混合物制成。</li>
</ol>

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LC-copolyesters of 3-(4-hydroxyphenyl) propionic acid and 4-hydroxy benzoic acids.</a> Journal of Polymer Science Part A: Polymer Chemistry. 25 (2), 489-504 (1987).</li><li>Chen, Y., Tan, L., Chen, L., Yang, Y., Wang, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Study+on+biodegradable+aromatic/aliphatic+copolyesters.">Study on biodegradable aromatic/aliphatic copolyesters.</a> Brazilian Journal of Chemical Engineering. 25 (2), 321-335 (2008).</li><li>Han, X., 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=A+Change+in+Mechanism+from+Acidolysis+to+Phenolysis+in+the+Bulk+Copolymerization+of+4-Acetoxybenzoic+Acid+and+6-Acetoxy-2-naphthoic+Acid.">A Change in Mechanism from Acidolysis to Phenolysis in the Bulk Copolymerization of 4-Acetoxybenzoic Acid and 6-Acetoxy-2-naphthoic Acid.</a> Macromolecules. 29 (26), 8313-8320 (1996).</li><li>Lu, X. F., Hay, J. N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Isothermal+crystallization+kinetics+and+melting+behaviour+of+poly(ethylene+terephthalate).">Isothermal crystallization kinetics and melting behaviour of poly(ethylene terephthalate).</a> Polymer. 42 (23), 9423-9431 (2001).</li><li>S&#225;nchez, M. E., Mor&#225;n, A., Escapa, A., Calvo, L. F., Mart&#237;nez, O. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Simultaneous+thermogravimetric+and+mass+spectrometric+analysis+of+the+pyrolysis+of+municipal+solid+wastes+and+polyethylene+terephthalate.">Simultaneous thermogravimetric and mass spectrometric analysis of the pyrolysis of municipal solid wastes and polyethylene terephthalate.</a> Journal of Thermal Analysis and Calorimetry. 90 (1), 209-215 (2007).</li></ol>

作者没有什么可透露的。

当二氢酸在反应容器中加热时，启动材料的升华发生，当应用真空时，这种效果得到增强。乙酰化已对二氢酸进行，以避免升华。克里切多夫等人12日、27日承认，不仅乙酰化，而且类似的二寡聚化也发生了。然而，这些酯化单体和寡聚物不再升华，适合作为单体熔化聚合物28。此外，从4-乙氧二氢酸的预聚合物的形成证实了假设反应机...

与聚合物废物的焚烧相比，化学回收提供了回收单体的可能性。化学回收是聚合物材料技术寿命结束时的一个合乎逻辑的选择，因为这些聚合物材料是化学1生产的。有两种方法可以化学地回收聚合物材料，热解和分子回收2。通过热解，聚合物材料通过极端条件3、4转化为高价值产品。分子回收是利用去聚合回收起始材料的有效方法。去聚合后，单体单元可再聚合成处女聚合材料5。需要有合适的单体来大规模地应用分子回收。目前的塑料问题决定了社会需要坚固耐用的聚合物材料。同时，也更希望同样的聚合物材料易于回收利用，在环境中不耐用。电流聚合物材料具有良好的热和机械性能，不容易去聚合。
利格宁，常见于血管植物，占世界天然碳含量的30%，是仅次于纤维素的第二大生物聚合物。褐金具有复杂的无定形结构，似乎是替代从化石材料中提取的芳香剂的合适替代品。木质素的三维结构为木材提供强度和刚度，以及抗降解。从化学上讲，木质素是一种非常复杂的多酚热集。它由三种不同的甲氧化苯丙烷结构的不同组成组成。西林吉尔、瓜亚基和p-羟基苯基（通常分别缩写为S、G和H）来自单利尼诺西纳皮尔醇、针叶醇和p-库马里尔酒精7。这些单位的分布不同，每个生物质类型，软木，例如，主要包括瓜亚基单位和硬木的瓜亚基和注射器单位8，9。可再生的天然资源，如树木和植物，是生产重新设计的单体创新聚合物材料10的理想。这些单体，从天然来源分离和合成，聚合到所谓的生物基聚合物11。
芳香性碳酸是几个数量级比同等的药化碳酸少12。各种商业聚酯使用芳香的碳酸，而不是药酸。因此，聚酯纺织品中由聚（乙烯四甲酸酯）纤维制成的纤维在洗涤过程中几乎对水解麻木不仁，例如，雨13。当需要聚酯分子回收时，建议在聚合物的积累中使用脂肪酯。
对于上述原因，我们已研究了用4-羟基-3，5-二氧二氢辛酸制造聚酯的可能性。克里切尔多夫15号、迈尔16号和米勒17号、18号先前的研究表明，使用4-羟基-3，5-二氧-二氢辛酸制造聚合物是具有挑战性的。脱卡和交联阻碍了聚合，因此限制了这些合成器的成功。此外，多聚变的机制仍然不清楚。论文描述了聚酯聚（二氢酸）可以定期合成和高产的条件，从而为使用分子可回收的半芳香聚酯铺平了道路。
我们开发了一种绿色和高效的方法，利用注射器醛和恶性酸19，20之间的凝结反应合成西纳皮尼酸。在此绿色克诺维纳格尔之后，氢化产生二氢酸，适用于可逆多聚化。本出版物可视化分子可回收聚合物聚（二氢酸）的合成步骤，指木质素的基础单位，称为聚S。在分析聚合物材料后，聚氨酯在相对有利的条件下去聚聚到单体二氢酸中，并反复再聚。

<table>
	<tbody>
		<tr>
			<td>Reaction 1: Green Knoevenagel condensation</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Ammonium bicarbonate</td>
			<td>Sigma Aldrich</td>
			<td>&#62;99%</td>
			<td></td>
		</tr>
		<tr>
			<td>Ethanol</td>
			<td>Boom</td>
			<td>Technical grade</td>
			<td></td>
		</tr>
		<tr>
			<td>Ethyl acetate</td>
			<td>Macron</td>
			<td>99.8%</td>
			<td></td>
		</tr>
		<tr>
			<td>Hydrochloric acid</td>
			<td>Boom</td>
			<td>37%</td>
			<td></td>
		</tr>
		<tr>
			<td>Malonic acid</td>
			<td>Sigma Aldrich</td>
			<td>99%</td>
			<td>used as received</td>
		</tr>
		<tr>
			<td>Sodium bicarbonate</td>
			<td>Sigma Aldrich</td>
			<td>&#62;99.7%</td>
			<td></td>
		</tr>
		<tr>
			<td>Syringaldehyde</td>
			<td>Sigma Aldrich</td>
			<td>98%</td>
			<td>used as received</td>
		</tr>
		<tr>
			<td>Reaction 2: Hydrogenation</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Magnesium sulfate</td>
			<td>Macron</td>
			<td>99%</td>
			<td>dried</td>
		</tr>
		<tr>
			<td>Raney&#8482; nickel</td>
			<td>Sigma Aldrich</td>
			<td>&#62;89%</td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium hydroxide</td>
			<td>Boom</td>
			<td>Technical grade</td>
			<td>dissolved</td>
		</tr>
		<tr>
			<td>Reaction 3: Acetylation</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Acetic anhydride</td>
			<td>Macron</td>
			<td>&#62;98%</td>
			<td></td>
		</tr>
		<tr>
			<td>Acetone</td>
			<td>Macron</td>
			<td>&#62;99.5%</td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium acetate</td>
			<td>Sigma Aldrich</td>
			<td>&#62;99%</td>
			<td></td>
		</tr>
		<tr>
			<td>Reaction 4A: Polymerisation</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>1,2-xylene</td>
			<td>Macron</td>
			<td>&#62;98%</td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium hydroxide</td>
			<td>Boom</td>
			<td>Technical grade</td>
			<td>finely powdered</td>
		</tr>
		<tr>
			<td>Zinc(II)acetate</td>
			<td>Sigma Aldrich</td>
			<td>99.99%</td>
			<td></td>
		</tr>
		<tr>
			<td>Reaction 4B: Depolymerisation</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium hydroxide</td>
			<td>Boom</td>
			<td>Technical grade</td>
			<td>dissolved</td>
		</tr>
		<tr>
			<td>Sulfuric acid</td>
			<td>Macron</td>
			<td>100%</td>
			<td></td>
		</tr>
		<tr>
			<td>Analysis</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>CDCl3</td>
			<td>Cambride Isotope Laboratories, Inc.</td>
			<td>99.5%</td>
			<td></td>
		</tr>
		<tr>
			<td>CF3COOD</td>
			<td>Cambride Isotope Laboratories, Inc.</td>
			<td>98%</td>
			<td></td>
		</tr>
		<tr>
			<td>Dimethylformamide</td>
			<td>Macron</td>
			<td>&#62;99.9%</td>
			<td></td>
		</tr>
		<tr>
			<td>Hexafluoro-2-propanol</td>
			<td>TCI Chemicals</td>
			<td>&#62;99%</td>
			<td></td>
		</tr>
		<tr>
			<td>Methanol</td>
			<td>Macron</td>
			<td>&#62;99.8%</td>
			<td></td>
		</tr>
		<tr>
			<td>Tetrahydrofuran</td>
			<td>Macron</td>
			<td>&#62;99.9%</td>
			<td></td>
		</tr>
	</tbody>
</table>

designed for molecular recycling: a lignin-derived semi-aromatic biobased polymer

化学可回收生物聚合物的发展为追求循环经济提供了机遇。化学可回收生物聚合物在使用阶段后的处置阶段积极努力解决聚合物材料问题。本文对生物基半芳烃聚酯的生产进行了描述和可视化，这种聚酯完全可以从木质素等生物量中提取。本文中描述的聚合物聚氨酯具有与某些常用塑料（如 PET）相似的热性能。我们开发了一种绿色克诺维纳格尔反应，它可以有效地产生芳香醛和马洛尼克酸的单体。这种反应已被证明是可扩展的，并且具有非常低的计算电子因子。这些以利格诺植物化学物质为起点的聚酯显示出高效的分子回收利用，损失最小。聚酯聚（二氢酸）（聚S）是这些半芳香聚酯的示例，并描述了聚合、去聚合和再聚合。

西纳皮尼酸是使用绿色克诺维纳凝结剂从注射器醛中高纯度和高产量（>95%）合成的。（支持信息:图S1）电子因子表示废物产生，其中较高的数字表示更多的废物。电子因子的计算方法是获取总材料投入，减去所需最终产品的量，并将整个产品除以最终产品的量。这种绿色克诺维纳格尔凝结物的电子因子为1.0， 可以计算: [（29.81 克马洛尼克酸 = 36.4 克注射器醛 = 0.790 克碳酸氢铵 = 18.04 ?...

Watch this Scientific Journal Video about Designed for Molecular Recycling: A Lignin-Derived Semi-aromatic Biobased Polymer at JoVE.com

Designed for Molecular Recycling: A Lignin-Derived Semi-aromatic Biobased Polymer

这里介绍了对循环材料经济采取闭环方法的一个例子。整个可持续循环由生物基半芳烃聚酯设计，通过聚合、去聚合，然后重新聚合，其产量或最终特性仅略有变化。

专为分子回收而设计:一种褐宁衍生的半芳烃生物基聚合物

The development of chemically recyclable biopolymers offers opportunities within the pursuit of a circular economy. Chemically recyclable biopolymers make ...

designed-for-molecular-recycling-lignin-derived-semi-aromatic

Research

Education

JoVE Core

JoVE Journal

Organic Chemistry

Chemistry

Unit 1

&alpha;-Carbon Chemistry: Enols, Enolates, and Enamines

SCIENTISTS IN ACTION

3.4K 次观看.  Avans University of Applied Science. 这里介绍了对循环材料经济采取闭环方法的一个例子。整个可持续循环由生物基半芳烃聚酯设计，通过聚合、去聚合，然后重新聚合，其产量或最终特性仅略有变化。

视频: Designed for Molecular Recycling: A Lignin-Derived Semi-aromatic Biobased Polymer

Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, have high porosity, high surface-to-volume and strength-to-weight ratio. Unfortunately, common approaches for preparation of metallic nanostructures render materials with highly disordered architecture, which might have an adverse effect on their mechanical properties. Block copolymers have the ability to self-assemble into ordered nanostructures and can be applied as templates for the preparation of well-ordered metal nanofoams. Here we describe the application of a block copolymer-based supramolecular complex - polystyrene-block-poly(4-vinylpyridine)(pentadecylphenol) PS-b-P4VP(PDP) - as a precursor for well-ordered nickel nanofoam. The supramolecular complexes exhibit a phase behavior similar to conventional block copolymers and can self-assemble into the bicontinuous gyroid morphology with two PS networks placed in a P4VP(PDP) matrix. PDP can be dissolved in ethanol leading to the formation of a porous structure that can be backfilled with metal. Using electroless plating technique, nickel can be inserted into the template&#39;s channels. Finally, the remaining polymer can be removed via pyrolysis from the polymer/inorganic nanohybrid resulting in nanoporous nickel foam with inverse gyroid morphology.

This article describes the preparation of well-ordered nickel nanofoams via electroless metal deposition onto nanoporous templates obtained from self-assembled diblock copolymer based supramolecules.

Gyroid镍纳米结构的嵌段共聚物超分子

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, ...

科研

化学

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

对磷酸增强富集制备高度多孔配位聚合物涂层的孔聚合物石柱的

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous solution. In a carbon nanotube/PEO105-PPO70-PEO105 (poloxamer 407) aqueous solution, the amphiphilic poloxamer 407 adsorbs onto the carbon nanotube surfaces and self-assembles into continuous layers, driven by intermolecular interactions between constituent molecules. The addition of 5-methylsalicylic acid changes the self-assembled structure from spherical-micellar to a cylindrical morphology. The fabricated poloxamer 407/carbon nanotube hybrid particles exhibit thermo-responsive structural features so that the density and thickness of poloxamer 407 layers are also reversibly controllable by varying temperature. The detailed structural properties of the poloxamer 407/carbon nanotube particles in suspension can be characterized by small-angle neutron scattering experiments and model fit analyses. The distinct curve shapes of the scattering intensities depending on temperature control or addition of aromatic additives are well described by a modified core-shell cylinder model consisting of a carbon nanotube core cylinder, a hydrophobic shell, and a hydrated polymer layer. This method can provide a simple but efficient way for the fabrication and in-situ characterization of carbon nanotube-based nano particles with a structure-tunable encapsulation.

A method for the functionalization of carbon nanotubes with structure-tunable polymeric encapsulation layers and structural characterization using small-angle neutron scattering is presented.

单壁碳纳米管与热可逆嵌段共聚物及表征功能化小角度中子散射

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous ...

The Preparation and Properties of Thermo-reversibly Cross-linked Rubber Via Diels-Alder Chemistry

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ethylene-propylene rubber, grafted with maleic anhydride, is thermo-reversibly cross-linked in two steps. The pending anhydride moieties are first modified with furfurylamine to graft furan groups to the rubber backbone. These pendant furan groups are then cross-linked with a bis-maleimide via a Diels-Alder coupling reaction. Both reactions can be performed under a broad range of experimental conditions and can easily be applied on a large scale. The material properties of the resulting Diels-Alder cross-linked rubbers are similar to a peroxide-cured ethylene/propylene/diene rubber (EPDM) reference. The cross-links break at elevated temperatures (&#62; 150 &#176;C) via the retro-Diels-Alder reaction and can be reformed by thermal annealing at lower temperatures (50-70 &#176;C). Reversibility of the system was proven with infrared spectroscopy, solubility tests and mechanical properties. Recyclability of the material was also shown in a practical way, i.e., by cutting a cross-linked sample into small parts and compression molding them into new samples displaying comparable mechanical properties, which is not possible for conventionally cross-linked rubbers.

A simple two-step approach involving rubber modification and cross-linking yields fully reworkable, elastic rubber products.

热可逆交联橡胶通过的Diels-Alder反应的化学制备与性能

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ...

Direct Imaging of Laser-driven Ultrafast Molecular Rotation

We present a method for visualizing laser-induced, ultrafast molecular rotational wave packet dynamics. We have developed a new 2-dimensional Coulomb explosion imaging setup in which a hitherto-impractical camera angle is realized. In our imaging technique, diatomic molecules are irradiated with a circularly polarized strong laser pulse. The ejected atomic ions are accelerated perpendicularly to the laser propagation. The ions lying in the laser polarization plane are selected through the use of a mechanical slit and imaged with a high-throughput, 2-dimensional detector installed parallel to the polarization plane. Because a circularly polarized (isotropic) Coulomb exploding pulse is used, the observed angular distribution of the ejected ions directly corresponds to the squared rotational wave function at the time of the pulse irradiation. To create a real-time movie of molecular rotation, the present imaging technique is combined with a femtosecond pump-probe optical setup in which the pump pulses create unidirectionally rotating molecular ensembles. Due to the high image throughput of our detection system, the pump-probe experimental condition can be easily optimized by monitoring a real-time snapshot. As a result, the quality of the observed movie is sufficiently high for visualizing the detailed wave nature of motion. We also note that the present technique can be implemented in existing standard ion imaging setups, offering a new camera angle or viewpoint for the molecular systems without the need for extensive modification.

We present a protocol for creating a real-time movie of a molecular rotational wave packet using a high-resolution Coulomb explosion imaging setup.

激光驱动的超快分子旋转直接成像

We present a method for visualizing laser-induced, ultrafast molecular rotational wave packet dynamics. We have developed a new 2-dimensional Coulomb ...

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 ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

电化学阻抗谱作为电化学速率常数估计的一种工具

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

Time-resolved Photophysical Characterization of Triplet-harvesting Organic Compounds at an Oxygen-free Environment Using an iCCD Camera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables the acquisition of photoluminescence spectra covering the time regime from nanoseconds up to 0.1 s. This enables us to follow the changes in the intensity (decay) and emission of the spectra over time. Using this method, it is possible to study diverse photophysical phenomena, such as the emission of phosphorescence, and the contributions of prompt and delayed fluorescence in molecules showing thermally activated delayed fluorescence (TADF). Remarkably, all spectra and decays are obtained in a single experiment. This can be done for solids (thin film, powder, crystal) and liquid samples, where the only limitations are the spectral sensitivity of the camera and the excitation wavelength (532 nm, 355 nm, 337 nm, and 266 nm). This technique is, thus, very important when investigating the excited state dynamics in organic emitters for their application in organic light-emitting diodes and other areas where triplet harvesting is of paramount importance. Since triplet states are strongly quenched by oxygen, emitters with efficient TADF luminescence, or those showing room temperature phosphorescence (RTP), must be correctly prepared in order to remove any dissolved oxygen from solutions and films. Otherwise, no long-lived emission will be observed. The method of degassing solid samples as presented in this work is basic and simple, but the degassing of liquid samples creates additional difficulties and is particularly interesting. A method of minimizing solvent loss and changing the sample concentration, while still enabling to remove oxygen in a very efficient and a repeatable manner, is presented in this work.

Here, we present a method of the spectroscopic characterization of organic molecules by means of time-resolved photoluminescence spectroscopy on the nanosecond-to-millisecond timescale in oxygen-free conditions. Methods to efficiently remove oxygen from the samples and, thus, limit luminescence quenching are also described.

利用 iccd 摄像机对无氧环境下的三重收集有机化合物进行光物理表征

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables ...

Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. Conductive polymers, poly(3,4-ethylenedioxythiophene) (PEDOT) and poly(3,4-propylenedioxythiophene) (PProDOT), and a semiconducting polymer, poly(thieno[3,2-b]thiophene) (PTT), were deposited on unconventional highly-disordered and textured substrates with high surface areas, such as paper, towels and fabrics. This reported deposition chamber is an improvement of previous vapor reactors because our system can accommodate both volatile and nonvolatile monomers, such as 3,4-propylenedioxythiophene and thieno[3,2-b]thiophene. Utilization of both solid and liquid oxidants are also demonstrated. One limitation of this method is that it lacks sophisticated in situ thickness monitors. Polymer coatings made by the commonly used solution-based coating methods, such as spin-coating and surface grafting, are often not uniform or susceptible to mechanical degradation. This reported vapor phase deposition method overcomes those drawbacks and is a strong alternative to common solution-based coating methods. Notably, polymer films coated by the reported method are uniform and conformal on rough surfaces, even at a micrometer scale. This feature allows for future application of vapor deposited polymers in electronics devices on flexible and highly textured substrates.

This paper presents a protocol for reactive vapor deposition of poly(3,4-ethylenedioxythiophene), poly(3,4-propylenedioxythiophene), and poly(thieno[3,2-b]thiophene) films on glass slides and rough substrates, such as textiles and paper.

任意基底上共轭聚合物薄膜的反应气相沉积

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. ...

Light-driven Molecular Motors on Surfaces for Single Molecular Imaging

The design and synthesis of a synthetic system that aims for the direct visualization of a synthetic rotary motor at the single molecule level on surfaces are demonstrated. This work requires careful design, considerable synthetic effort, and proper analysis. The rotary motion of the molecular motor in solution is shown by 1H NMR and UV-vis absorption spectroscopy techniques. In addition, the method to graft the motor onto an amine-coated quartz is described. This method helps to gain more insight into molecular machines.

The manuscript describes how to synthesize and graft a molecular motor on surfaces for single molecular imaging.

表面光驱动分子电机的单分子成像

The design and synthesis of a synthetic system that aims for the direct visualization of a synthetic rotary motor at the single molecule level on surfaces ...