这项研究是由国防威胁减少局 (DTRA BA08PRO015) 和美国海军研究局通过海军研究实验室基地基金发起的。这里所表达的观点是作者的意见, 并不代表美国海军、美国国防部或美国政府。

1. 微波启动
<ol><li>用10毫升的氢氧化铵 (28-30%) 与184毫升异丙醇在玻璃烧杯中混合, 用一个在 150 rpm 上的磁力搅拌棒来制备初始溶液。将6毫升的四乙基硅酸 (TEOS) 加入氢氧化铵溶液5。 注意: 氢氧化铵是一种碱溶液, 在接触眼睛和皮肤时会引起刺激和燃烧危险, 吸入或摄取时也会产生毒性。 注意: 四乙基硅酸是易燃和有毒的。</li>
	<li>要启动样品, 将织物的基质完全浸入 TEOS 混合物中, 取出玻璃、微波安全盘。 注意: 这里使用的布料是重量轻, 未漂白的棉花从一个特殊工艺品和织品零售商获得。所述工艺适用于范围广泛的织物, 限制其必须有可用的羟基或胺类5。这道菜的尺寸不重要, 只要布料能平躺在里面。<ol>
<li>微波饱和织物样品使用 1200 W 三十年代。 注意: 面料的样品和菜将是热的后续治疗。微波样品有足够的透气性, 避免吸入产生的蒸气。</li>
		<li>重复浸泡和微波处理共三个周期。 注: TEOS 混合物随着降水的发生而迅速变多云。立即使用。</li>
		<li>干燥处理的织物在100°c 30 分钟在烘干烤箱。一旦干燥, 织物可以储存在环境条件下。 注: 在这里使用的烤箱是一个重力烤箱, 但任何足够大小的烤箱适合干燥的材料。</li>
	</ol>
</li>
</ol>2. 镀膜用溶胶的制备
<ol><li>为制备溶胶, 在室温15、16、17、18、20 的塑料瓶中混合1.9 克 Pluronic P123、0.5 克均三甲苯和2.12 克 12-双 (trimethyoxysilyl) 乙烷 (BTE)。 ,21。 注意:12-双 (trimethyoxysilyl) 乙烷是易燃和有毒的。避免皮肤接触和吸入。均三甲苯是易燃和有毒的。避免皮肤接触和吸入。<ol>
<li>加入2.0 克甲醇和一个磁力搅拌棒。密封容器, 搅拌150转。 注意: 甲醇是易燃和有毒的, 可能会带来其他健康危害。避免皮肤接触和吸入。 注: 在这种沉积物的变化中, 乙醇可以代替本议定书的甲醇。在讨论中提供了其他信息。</li>
		<li>当搅拌溶液出现均匀时, 加入6.07 克的0.1 米 HNO3滴状。 注意: 硝酸是腐蚀性的, 会引起皮肤、眼睛和呼吸系统的刺激。避免皮肤接触和吸入。</li>
		<li>继续搅拌6小时的混合物。 注: 在这一点上, 混合物在一夜之间是稳定的, 但只有在没有蒸发的情况下。如果甲醇在贮存过程中蒸发, 会发生对溶胶凝胶的改变。</li>
	</ol>
</li>
</ol>3. 浸渍涂布
<ol><li>以150毫米/分钟的速率将 TEOS 处理过的织物浸入所制备的溶胶中。 注: 更快的速度高达270毫米/分钟可以使用, 并没有负面影响的结果材料。在这里, 任何设备达到倾角和绘制率之间的150和270毫米/分钟是合适的。<ol>
<li>将样品转移到60摄氏度烤箱中晾干24小时。</li>
		<li>继续固化在80摄氏度额外的24小时。 注意: 在这一点上可以接受120摄氏度以上的固化温度。固化后, 织物可以储存在室温下, 允许以后提取。</li>
	</ol>
</li>
	<li>将织物样品浸泡在超过65摄氏度的乙醇中, 以提取表面活性剂。 注意: 乙醇是易燃的。 注: 确保容器能耐受必要的温度。<ol>
<li>用额外的乙醇冲洗织物。</li>
	</ol>
</li>
	<li>在 60-65 摄氏度处过夜。一旦干燥, 织物可以储存在环境条件下。</li>
</ol>4. 涂层织物的卟啉功能化
<ol><li>为了 functionalize 主要胺基团的吸附剂材料, 在0.5% 体积/体积15,16的情况下, 在甲苯中制备 3-aminopropyltriethoxy 硅烷 (APS) 溶液。 注意: 3-Aminopropyltriethoxy 硅烷具有腐蚀性和毒性。避免皮肤接触和吸入。甲苯是易燃、有毒和已知的致癌物质。避免皮肤接触和吸入。<ol>
<li>浸泡在溶液中的织物和孵化1小时, 覆盖。</li>
		<li>用甲苯彻底冲洗样品。</li>
		<li>干燥织物样品隔夜在100°c。</li>
	</ol>
</li>
	<li>为制备次卟啉 IX 24 双乙二醇 (迪克斯) 的铜络合物, 在2毫升二甲基亚砜22中溶解20毫克卟啉。 注意: 卟啉可能存在健康危害;遵循建议的预防程序。<ol>
<li>将卟啉溶液添加到100毫升水中, 用12.8 毫克的氯化铜在圆底烧瓶中加入。 注意: 氯化铜具有腐蚀性、毒性, 并对水生环境构成危害。避免皮肤接触和吸入。</li>
		<li>一夜之间回流解决方案。</li>
		<li>使用旋转蒸发将总试样体积减少到5毫升。 注: 卟啉可以用更大的数量制备, 供以后使用。制备的卟啉应在室温下储存在黑暗中。</li>
	</ol>
</li>
	<li>将所制备的卟啉溶液添加到15毫升的0.1 米 2-(n-吗啉代) ethansulfonic 酸 (MES) 缓冲 pH 值5.5。<ol>
<li>在溶液中加入5毫克 1-乙基 3-(3-dimethylaminopropyl) carbodiimide (EDC), 立即将织物样品浸泡。</li>
		<li>覆盖样品和孵化过夜。</li>
		<li>用清水冲洗样品。</li>
		<li>干燥织物样品隔夜在100°c。</li>
	</ol>
</li>
</ol>5. 织物的特性
<ol><li>根据制造商的协议, 使用任何商业上可用的氮气吸附特性系统来表征织物样品的孔隙度。 注: 在这里, 氮气吸附分析完成 77 k 根据所使用的系统, 可能需要权衡样品或德加在≥65°c 之前分析。<ol>
<li>使用布鲁诺尔 (下注) 法测定表面积。</li>
		<li>使用巴雷特-乔伊纳-Halenda (BJH) 法测定等温线吸附支路的孔隙大小。</li>
		<li>用单点法测定相对压力下的孔隙体积 (p/p0) 0.97。</li>
	</ol>
</li>
	<li>通过对 2-氯乙基硫化物 (塞斯·弗林特曼) 通过织物样品的渗透特性, 遵循试验操作程序 (顶部) 8-2-501 的指导, 通过化学试剂或模拟剂 (色板试验) 对材料进行渗透试验 (样本测试)23 ,24。 注意: 2-氯乙基乙硫醚易燃、耐腐蚀、有毒, 并对健康构成危害。避免皮肤接触和吸入。 注: 在本研究中, 采用内部探头驱动加热器, 控制了自定义环境中的温度。使用探头驱动的质量流量控制器解决了进入本会议厅的潮湿空气比。不锈钢气溶胶-蒸气-液体评估组 (AVLAG) 单元与 O 形环密封水平保持样品。扩散渗透试验使用氮气流。该色板上方的顶空, 其中的目标放置, 是停滞的, 没有压力差在色板之上和下方。样品在两个实心支持盘之间支持与被排列的 0.64 cm2圆的开头。该组件放置在 AVLAG 单元格中, 湿度为2小时平衡, 使用重复分配器将目标作为液滴引入。一个专用的氢裂允许连续监测目标浓度。</li>
	<li>遵循 ASTM E96 提供的指导, 水蒸气运输: 直立开杯法表征水汽输送通过织物样品4,24,25。<ol>
<li>修改孵化器以提供25摄氏度的此分析的外壳。</li>
		<li>用16.9 毫升去离子水填充闪烁瓶 (20 毫升)。把样品材料密封在这个瓶子上, 然后称量瓶子。使用干燥剂在孵化器中驱动湿度差异, 并使干氮气流保持在样品表面 (0.25 升/分钟) 的流动。</li>
		<li>用分析天平测量30到45分钟的样品盖瓶的重量。</li>
	</ol>
</li>
</ol>

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作者声明他们没有竞争的财政利益。

在这里, 我们已经表明, 微波引发的沉积 TEOS 可用于制备织物, 随后沉积的多孔 organosilicate 吸附剂。方法导致布料的装载与 1.12 g 吸附剂每 m2织品表面。用氮吸附法对涂层织物进行分析, 表明在充分处理的材料与所启动的织物之间存在显著差异的多孔涂层的沉积。然而, 表面面积比作为一个整体合成的类似组合材料所观察到的要少。单独的吸附剂降低了85% 塞斯·弗林特曼运输的速度。加入卟啉功能化对支持的吸附剂进一步减少运输 (93% 总减少)。卟啉官能化处理织物的初步突破发生在2分钟;初步突破棉织物为0.6 分钟。这种化学渗透的减少对织物的水汽输送影响不大。
所沉积的吸附剂不是连续薄膜。该方法产生的涂层, 更紧密的保形, 以纱线的面料。因此, 减少渗透是有限的织物编织。在这里, 用轻质棉布作为支撑材料。微波启动适用于其它提供胺类或羟基的织物进行改性。更密的梭织织物, 如美国陆军战斗制服使用的尼龙和棉混纺 (针灸), 将产生更大的减少目标运输简单的基础上的空隙空间内的编织。作为遮蔽材料使用的密被编织的织物将提供类似的优势。忆及吸附剂的处理不限于织物的表面, 也可望提供某种深度的羊毛或重针织织物的材料, 从而产生更多的渗透减少。这一概念也适用于空气过滤用的三维折叠材料。
此处概述的治疗不限于在传统织物上使用。它提供了可能修改的纸张, 分层和褶积材料更典型地应用于过滤方法和非织造纺织品。在某些情况下, 此处描述的条件可能需要温和, 以保持支持材料的完整性。减少碱的浓度 (氢氧化铵) 可能是必要的, 如聚乙烯织物的情况。缩短微波周期的时间可能是必要的, 以避免灼热 (纸张材料)。一些合成纤维, 例如聚丙烯, 需要减少使用的干燥温度。应避免对溶胶时效温度和持续时间的变化, 因为这些条件对产生的吸附剂的形貌有重大影响。
在浸渍涂层溶胶中, 乙醇可以取代甲醇。这在放大合成和使用更大体积的溶胶时是鼓励的, 因为乙醇对健康危害较小。溶胶可以相当稀释与酒精,例如, 4 到12克乙醇, 而不是2克甲醇), 以准备一个更大的体积的混合物, 没有比例增加 BTE, Pluronic P123, 均三甲苯和酸。相对量的反应物和溶剂也可以乘以以制备溶胶, 以生成更大的涂层材料样品。溶胶的稀释程度或浓度可能会影响到特定织物上的吸附剂材料的大量加载。多循环的浸入溶胶混合物也应导致总负荷的变化。
目前正在对其他支持材料的沉积方法进行优化。改性的针刺尼龙和棉混纺织物是特别感兴趣的日常磨损解决方案提供基线化学保护, 因为是泽西针织材料。其他吸附剂材料的沉积也正在探索中。例如, 为捕获杀虫剂目标而开发的苯桥吸剂, 使用与此处描述的17、20、27和催化不同的溶胶制备方法。卟 啉。最后, 对织物支持材料进行了对气溶胶、液体和蒸气目标的评估。

目前, 美国国防部 (DoD) 使用的化学防护服, 要么提供一个完整的屏障, 一级的化学防护服, 例如, 或使用多层织物保护, 如在联合服务轻量级综合套装技术 (JSLIST)。全垒服给用户造成了很大的负担。由于没有水蒸气通过材料输送, 热调节受到阻碍。因此, 使用期限 (任务长度) 受到限制;该服装适用于范围有限的方案。另一方面, JSLIST 在壳织物和舒适层之间使用一层碳吸附剂。由此造成的用户负担减少, 但没有消除, 并减少了防护能力相比, 屏障西装。除热负荷外, JSLIST 套装仅适用于连续使用24小时。这两种技术都不适合在长期的日常服装中提供基线保护能力。基线保护将用于低危险环境, 适用于 MOPP 0 至2的条件 (MOPP 以任务为导向的保护姿态) 和其他低风险条件。除了国防部的关注之外, 基线保护对于那些可能进入受污染环境但没有事先警告的急救人员是有用的。
寻求改进国防部防护服装的研究正在进行中, 连续1,2,3,4。以前的努力确定了微波启动过程的潜力, 以沉积 heptadecafluoro-11, 22-tetrahydrodecyl) 三氯织物, 以产生憎油行为5。目的是生产一种可以增强 JSLIST 服装外壳层的织物。虽然这种 oleophobicity 可以提高层状服装的耐化学性, 但它不会解决该套装所施加的热量负担。还有其他正在进行的工作侧重于吸附剂和催化剂的捕获和/或分解化学威胁6,7,8,9,10, 11,12,13,14。最近描述的方法使用多孔 organosilicate 吸附剂结合卟啉捕获和降解光气, 并使用类似的材料捕获有毒的工业化合物 (抽搐) 以及杀虫剂模拟剂和 nitroenergetics15 ,16,17,18,19,20。这些粉状材料虽然前景看好, 但并不直接适用于服装技术。
Organosilicate 系统广泛应用于浸渍和自旋涂层方法, 通常在玻璃和硅片上。上述微波沉积技术为这些材料在织物上的应用提供了一种机制。在这里, 我们使用所描述的过程与 tetraethylorthosilicate 结合, 以准备织物。然后通过浸渍涂层方法对其进行多孔吸附剂处理。形态学表征表明了多孔吸附剂在织物上的存在。对 2-氯乙基硫醚 (塞斯·弗林特曼) 在织物上的渗透和不经过这种处理, 对靶材的运输有很大的影响。

<table><tbody><tr><td>unbleached 100% cotton fabric</td><td>JOANN Stores</td><td>N/A</td><td>Protocol is suitable for use on a variety of fabrics</td></tr><tr><td>ammonium hydroxide</td><td>Aldrich</td><td>32,014-5</td><td></td></tr><tr><td>tetraethyl orthosilicate</td><td>Aldrich</td><td>13,190-3</td><td></td></tr><tr><td>Pluronic P123</td><td>Aldrich</td><td>435465</td><td></td></tr><tr><td>mesitylene</td><td>Sigma-Aldrich</td><td>M7200</td><td></td></tr><tr><td>1,2-bis(trimethoxysilyl)ethane</td><td>Aldrich</td><td>447242</td><td></td></tr><tr><td>methanol</td><td>Fisher Chemical</td><td>A454SK-4</td><td></td></tr><tr><td>nitric acid</td><td>Sigma-Aldrich</td><td>438073</td><td>Prepare 0.1 M aqueous solution</td></tr><tr><td>3-aminopropyltriethoxysilane</td><td>Gelest</td><td>SIA0603.4</td><td></td></tr><tr><td>toluene</td><td>Sigma-Aldrich</td><td>650579</td><td></td></tr><tr><td>Deuteroporphyrin IX bis ethylene glycol</td><td>Frontier Scientific</td><td>D630-9</td><td></td></tr><tr><td>dimethyl sulfoxide</td><td>Sigma-Aldrich</td><td>276855</td><td></td></tr><tr><td>copper chloride</td><td>Sigma-Aldrich</td><td>256528</td><td></td></tr><tr><td>2-(N-morpholino)ethansulfonic acid</td><td>Sigma-Aldrich</td><td>M3671</td><td>Prepare 0.1M buffer at pH 5.5</td></tr><tr><td>1-ethyl-3-(3-dimethylaminopropyl)carbodiimide</td><td>Sigma-Aldrich</td><td>E6383</td><td></td></tr><tr><td>ethyl alcohol</td><td>Warner-Graham</td><td>64-17-5</td><td></td></tr><tr><td>Drierite</td><td>Sigma-Aldrich</td><td>737828</td><td></td></tr><tr><td>Microwave</td><td>Daewoo</td><td>KOR-630A</td><td></td></tr><tr><td>Nitrogen adsorption instrument</td><td>Micromeritics</td><td>&amp;nbsp;TriStar II Plus&amp;nbsp;</td><td></td></tr><tr><td>Environmental chamber</td><td>custom part</td><td>N/A</td><td>Here, a modified Thermolyne incubator, Compact Series 5000 was used</td></tr><tr><td>Flame ionization detector (FID)</td><td>SRI Instruments</td><td>8690-0010</td><td>Model 110</td></tr><tr><td>Humidity probe</td><td>Vaisala</td><td>HMT3303E0A193BCAC100A0CCABEA1</td><td></td></tr><tr><td>AVLAG Cell</td><td>custom part</td><td>N/A</td><td>AERO-Space Tooling and Machining, P/N RS0010 Permeation cell</td></tr><tr><td>Computer controlled heater</td><td>World Precision Instruments</td><td>AIRTHERMY-ATX</td><td></td></tr><tr><td>Mass flow controller</td><td>MKS Instruments</td><td>1179A01312CS</td><td></td></tr><tr><td>Dipper mechanism Type D1L</td><td>NIMA Technology Ltd</td><td>D1L</td><td></td></tr><tr><td>Gravity oven</td><td>Fisher Scientific</td><td>15-103-0520</td><td></td></tr><tr><td>Stirring hotplate</td><td>Fisherbrand</td><td>S28482</td><td></td></tr><tr><td>Octagon spinbar, magnetic stirring bar</td><td>Fisherbrand</td><td>14-513-82</td><td></td></tr><tr><td>PSI-Plot version 9.5</td><td>Poly Software International, Inc</td><td>N/A</td><td></td></tr><tr><td>Microsoft Office Professional Plus - Excel 2013 32-bit</td><td>Microsoft</td><td>N/A</td><td></td></tr><tr><td>MicroActive TriStar II Plus Software</td><td>Micromeritics</td><td>packaged with the TriStar II nitrogen adsorption instrument</td><td></td></tr></tbody></table>

deposition of porous sorbents on fabric supports

烷的微波沉积技术, 以前被描述为生产的憎油织物, 是为了提供一种织物支持材料, 可随后处理的浸渍涂层。采用溶胶制备的浸渍涂层在织物上提供了受支持的多孔层。在这种情况下, 多孔层是一种卟啉功能性吸附剂系统, 其基础是一种粉末材料, 此前已经证明了对光气的捕获和转化。在10毫克/克的负载水平上, 有代表性的涂层适用于棉织物。这种涂层对通过织物 (93% 的支撑织物速率) 的水汽输送影响极小, 同时通过材料 (7% 的支持织物率) 显著减少了 2-氯乙基硫醚 (塞斯·弗林特曼) 的运输。所述方法适用于其他提供胺类和羟基的织物进行改性, 可与其他溶胶制剂结合使用, 以产生不同的功能。

采用氮气吸附法对浸渍涂层工艺后的织物进行了评价。如图 1所示, 为多孔涂层获得了预期的等温线。这与未处理的织品和为微波开始的织品注意的行为对比。仅对织物和微波处理后的织物进行了可忽略的氮吸附。没有确定孔隙大小。多孔涂层产生的表面积为3.39 米2/克, 孔隙体积0.013 厘米3/克。该仪器报告的 BJH 吸附孔径为76Å, 但在孔隙大小分布上没有明显的特征。图 2提供了涂层过程中每个阶段的织物图像。根据样品在沉积前的差重和最终干燥后的重量, 从原来的织物中增重 1%, 在棉花支护上沉积的吸附剂的平均质量确定为0.01 克/克。如果测量的表面积和孔隙体积被改正, 只占材料的吸附剂质量分量, 则吸附剂的表面积为339米2/克, 孔隙体积1.3 厘米3/克。为比较, 当这个吸附剂被合成作为一个整体在一个闭合的反应器, 氮气压表明了赌注表面面积 1143年 m2/g 与孔容量 1.01 m2/g 和孔直径76Å26。观察了这种材料具有显著滞后的 IV. 型等温线 (图 3)。在培养皿中固化镀膜溶胶, 并根据涂层织物样品的处理工艺, 制备了厚薄膜试样。氮气压表示一个赌注表面面积 968 m2/g 与孔容量 0.78 cm3/g 和孔直径39Å为这材料 (图 3)。
用两个腔室细胞4、24、25对所处理织物的水蒸气传输 (WVT) 速率进行了评估。该评价使用了一个圆形织物样品, 总暴露面积为1.65 厘米2。如图 4所示, 与未经处理的棉花相比, 这种织物的微波起动引起的水汽输送略有减少。在吸附剂沉积或功能化与卟啉之后, 没有注意到水蒸气输送的额外变化。棉织物的 WVT 率定为121克/小时/米2。在微波启动时, WVT 率降低到112克/小时/米2 。WVT 率为113克/小时/米2被确定为完全卟啉功能治疗。
2-氯乙基硫醚 (塞斯·弗林特曼) 被用作模拟, 以确定是否沉积的多孔处理导致化学运输性能的变化的织物。塞斯·弗林特曼通常被用作模拟硫磺芥末, 一种化学战剂。这里使用的吸附剂材料由乙烷桥接组组成, 并具有铜次卟啉 IX 24 双乙二醇 (CuDIX) 卟的功能。这反映了以前用来捕获光气15,16的吸附剂系统的特性。化学气相输送是用气溶胶-蒸气-液体评估组 (AVLAG) 细胞23,24确定的。该方法在受控温度 (40 °c) 和相对湿度 (50%) 的情况下, 利用连续流进行火焰电离检测 (FID), 使总暴露面积为0.64 厘米2。图 5提供了与时间相关的 FID 响应。当对纯棉织物进行评估时, 注意到67克/小时/米2的峰值率没有保留目标 (214 µg)。多孔处理的结果大大降低了运输高峰期 (9.6 克/小时/米2) 和目标通过织物的总运输。最初应用的214µg 塞斯·弗林特曼中只有78µg 在83小时内恢复。卟啉功能化多孔处理进一步降低了峰值的运输到4.5 克/小时/米2 , 总运输39µg 塞斯·弗林特曼超过 83 h 实验。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/57331/57331fig1.jpg"> 图 1: 织物的形态表征.这里显示的是代表性的氮吸附等温线 (a) 和孔隙大小分布 (B) 为典型的织物色板 (红色), 一个类似的样本后, 微波启动过程 (蓝色), 织物后应用的吸附剂 (绿色), 和织物以下应用的全吸附剂系统 (黑色)。<a href="/files/ftp_upload/57331/57331fig1large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/57331/57331fig2.jpg"> 图 2: 织物的照片.这里的照片显示了微波启动, 吸附剂涂层材料 (A), CuDIX 卟啉单独在棉花 (B), 和一个完整的卟啉功能涂层的棉花 (C)。处理过的色板覆盖在未经治疗的棉织物上。<a href="/files/ftp_upload/57331/57331fig2large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 3" class="xfigimg" src="/files/ftp_upload/57331/57331fig3.jpg"> 图 3: 不受支持的吸附剂的形态学表征.这里显示的是代表性的氮气吸附等温线 (A) 和孔隙大小分布 (B) 的吸附剂当合成为一个整体 (黑色), 当合成为厚膜 (红色)26。<a href="/files/ftp_upload/57331/57331fig3large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 4" class="xfigimg" src="/files/ftp_upload/57331/57331fig4.jpg"> 图 4: 水蒸气渗透.本文给出了全 CuDIX 卟啉功能化吸附剂 (黑色) 的水蒸气渗透分析结果。棉织物仅 (红色) 和棉织物以仅吸附剂组分 (蓝色) 被提供比较。<a href="/files/ftp_upload/57331/57331fig4large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 5" class="xfigimg" src="/files/ftp_upload/57331/57331fig5.jpg"> 图 5: 塞斯·弗林特曼的渗透.本文介绍了塞斯·弗林特曼在棉织物上的完全卟啉功能性吸附剂涂层 (黑色) 的渗透。织物仅 (红色) 和织品与仅吸附剂组分 (蓝色) 被提供比较。该插图为三材料的初始突破期提供了一个放大的视图。<a href="/files/ftp_upload/57331/57331fig5large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>

Watch this Scientific Journal Video about Deposition of Porous Sorbents on Fabric Supports at JoVE.com

Deposition of Porous Sorbents on Fabric Supports

本报告详细介绍了微波启动的方法, 以沉积卟啉功能性多孔 organosilicate 吸附剂在棉织物, 并表明减少 2-氯乙基硫醚 (塞斯·弗林特曼) 运输通过织物由此产生的治疗。

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 ...

deposition-of-porous-sorbents-on-fabric-supports

Nanyang Technological University

Research

JoVE Journal

Chemistry

6.5K 次观看.  Naval Research Laboratory. 本报告详细介绍了微波启动的方法, 以沉积卟啉功能性多孔 organosilicate 吸附剂在棉织物, 并表明减少 2-氯乙基硫醚 (塞斯·弗林特曼) 运输通过织物由此产生的治疗。

视频: Deposition of Porous Sorbents on Fabric Supports

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

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high surface area microporous materials, such as metal-organic frameworks (MOFs), unique challenges present themselves for PECVD treatments. Herein the protocol for development of a MOF that was previously unstable to humid conditions is presented. The protocol describes the synthesis of Cu-BTC (also known as HKUST-1), the treatment of Cu-BTC with PECVD of perfluoroalkanes, the aging of materials under humid conditions, and the subsequent ammonia microbreakthrough experiments on milligram quantities of microporous materials. Cu-BTC has an extremely high surface area (~1,800 m2/g) when compared to most materials or surfaces that have been previously treated by PECVD methods. Parameters such as chamber pressure and treatment time are extremely important to ensure the perfluoroalkane plasma penetrates to and reacts with the inner MOF surfaces. Furthermore, the protocol for ammonia microbreakthrough experiments set forth here can be utilized for a variety of test gases and microporous materials.

Herein the procedures for plasma enhanced chemical vapor deposition of perfluoroalkanes on microporous materials such as metal-organic frameworks to enhance their stability and hydrophobicity are described. Furthermore, breakthrough testing of milligram quantities of samples is described in detail.

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 ...

科研

化学

Characterization and Application of Passive Samplers for Monitoring of Pesticides in Water

Five different water passive samplers were calibrated under laboratory conditions for measurement of 124 legacy and current used pesticides. This study provides a protocol for the passive sampler preparation, calibration, extraction method and instrumental analysis. Sampling rates (RS) and passive sampler-water partition coefficients (KPW) were calculated for silicone rubber, polar organic chemical integrative sampler POCIS-A, POCIS-B, SDB-RPS and C18 disk. The uptake of the selected compounds depended on their physicochemical properties, i.e., silicone rubber showed a better uptake for more hydrophobic compounds (log octanol-water partition coefficient (KOW) &#62; 5.3), whereas POCIS-A, POCIS-B and SDB-RPS disk were more suitable for hydrophilic compounds (log KOW &#60; 0.70).

A protocol about the characterization and application of five different passive sampling devices is presented.

表征和被动采样的应用在农药水监测

Five different water passive samplers were calibrated under laboratory conditions for measurement of 124 legacy and current used pesticides. This study ...

环境科学

Air Filter Devices Including Nonwoven Meshes of Electrospun Recombinant Spider Silk Proteins

Based on the natural sequence of Araneus diadematus Fibroin 4 (ADF4), the recombinant spider silk protein eADF4(C16) has been engineered. This highly repetitive protein has a molecular weight of 48kDa and is soluble in different solvents (hexafluoroisopropanol (HFIP), formic acid and aqueous buffers). eADF4(C16) provides a high potential for various technical applications when processed into morphologies such as films, capsules, particles, hydrogels, coatings, fibers and nonwoven meshes. Due to their chemical stability and controlled morphology, the latter can be used to improve filter materials. In this protocol, we present a procedure to enhance the efficiency of different air filter devices, by deposition of nonwoven meshes of electrospun recombinant spider silk proteins. Electrospinning of eADF4(C16) dissolved in HFIP results in smooth fibers. Variation of the protein concentration (5-25% w/v) results in different fiber diameters (80-1,100 nm) and thus pore sizes of the nonwoven mesh.
Post-treatment of eADF4(C16) electrospun from HFIP is necessary since the protein displays a predominantly &alpha;-helical secondary structure in freshly spun fibers, and therefore the fibers are water soluble. Subsequent treatment with ethanol vapor induces formation of water resistant, stable &beta;-sheet structures, preserving the morphology of the silk fibers and meshes. Secondary structure analysis was performed using Fourier transform infrared spectroscopy (FTIR) and subsequent Fourier self-deconvolution (FSD).
The primary goal was to improve the filter efficiency of existing filter substrates by adding silk nonwoven layers on top. To evaluate the influence of electrospinning duration and thus nonwoven layer thickness on the filter efficiency, we performed air permeability tests in combination with particle deposition measurements. The experiments were carried out according to standard protocols.

Spider silk fibers display extraordinary mechanical properties. Engineered Araneus diadematus Fibroin 4 (eADF4) can be processed into nonwoven meshes using electrospinning. Here, the eADF4 nonwoven meshes are used to improve the performance of air filtering devices.

空气过滤设备，包括非织造网格静电重组蜘蛛丝蛋白

Based on the natural sequence of Araneus diadematus Fibroin 4 (ADF4), the recombinant spider silk protein eADF4(C16) has been engineered. This highly ...

生物工程

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 ...

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven effective in gas adsorption, separations, and catalysis. MOFs are most commonly synthesized as bulk powder, requiring additional processes to adhere them to functional devices and fabrics that risk decreasing the powder porosity and adsorption capacity. Here, we demonstrate a method of first coating fabrics with metal oxide films using atomic layer deposition (ALD). This process creates conformal films of controllable thickness on each fiber, while providing a more reactive surface for MOF nucleation. By submerging the ALD coated fabric in solution during solvothermal MOF synthesis, the MOFs create a conformal, well-adhered coating on the fibers, resulting in a MOF-functionalized fabric, without additional adhesion materials that may block MOF pores and functional sites. Here we demonstrate two solvothermal synthesis methods. First, we form a MIL-96(Al) layer on polypropylene fibers using synthetic conditions that convert the metal oxide to MOF. Using initial inorganic films of varying thicknesses, diffusion of the organic linker into the inorganic allows us to control the extent of MOF loading on the fabric. Second, we perform a solvothermal synthesis of UiO-66-NH2 in which the MOF nucleates on the conformal metal oxide coating on polyamide-6 (PA-6) fibers, thereby producing a uniform and conformal thin film of MOF on the fabric. The resulting materials can be directly incorporated into filter devices or protective clothing and eliminate the maladroit qualities of loose powder.

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

Metal-organic frameworks are effective in gas storage and heterogeneous catalysis, but typical synthesis methods result in loose powders that are difficult to incorporate into smart materials. We demonstrate a method of first coating fabrics with ALD metal oxides, resulting in conformal films of MOF on the fabrics during solvothermal synthesis.

溶剂热合成 MIL-96 和 UiO-66-NH2在纤维垫上原子层沉积金属氧化物涂层上的合成

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven ...

Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) with a 4.6 nm pore size, and ordered silica porous matrix, SBA-15, with a 5.3 nm pore size. This work describes the surface properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the differently ordered porous materials with similar pore sizes. For this purpose, OMC and SBA-15 with highly ordered nanoporous structures are synthesized via impregnation of the silica matrix by applying a carbon precursor and by the sol-gel method, respectively. The porous structure of investigated systems is characterized by an N2 adsorption-desorption analysis at 77 K. To determine the electrochemical character of the surface of synthesized materials, potentiometric titration measurements are conducted; the obtained results for OMC shows a significant pHpzc shift toward the higher values of pH, relative to SBA-15. This suggests that investigated OMC has surface properties related to oxygen-based functional groups. To describe the surface properties of the materials, the contact angles of liquids penetrating the studied porous beds are also determined. The capillary rise method has confirmed the increased wettability of the silica walls relative to the carbon walls and an influence of the pore roughness on the fluid/wall interactions, which is much more pronounced for silica than for carbon mesopores. We have also studied the melting behavior of D2O confined in OMC and SBA-15 by applying the dielectric method. The results show that the depression of the melting temperature of D2O in the pores of OMC is about 15 K higher relative to the depression of the melting temperature in SBA-15 pores with a comparable 5 nm size. This is caused by the influence of adsorbate/adsorbent interactions of the studied matrices.

Here we report the synthesis and characterization of ordered nanoporous carbon (with a 4.6 nm pore size) and SBA-15 (with a 5.3 nm pore size). The work describes the surface and textural properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the materials.

合成纳米碳和二氧化硅矩阵的表面性能

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) ...

Synthesis of Hydrogels with Antifouling Properties As Membranes for Water Purification

Hydrogels have been widely utilized to enhance the surface hydrophilicity of membranes for water purification, increasing the antifouling properties and thus achieving stable water permeability through membranes over time. Here, we report a facile method to prepare hydrogels based on zwitterions for membrane applications. Freestanding films can be prepared from sulfobetaine methacrylate (SBMA) with a crosslinker of poly(ethylene glycol) diacrylate (PEGDA) via photopolymerization. The hydrogels can also be prepared by impregnation into hydrophobic porous supports to enhance the mechanical strength. These films can be characterized by attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) to determine the degree of conversion of the (meth)acrylate groups, using goniometers for hydrophilicity and differential scanning calorimetry (DSC) for polymer chain dynamics. We also report protocols to determine the water permeability in dead-end filtration systems and the effect of foulants (bovine serum albumin, BSA) on membrane performance.

This paper reports practical methods to prepare hydrogels in freestanding films and impregnated membranes and to characterize their physical properties, including water transport properties.

水凝胶的合成与防污性能作为膜的净水

Hydrogels have been widely utilized to enhance the surface hydrophilicity of membranes for water purification, increasing the antifouling properties and ...

A Simple and Scalable Fabrication Method for Organic Electronic Devices on Textiles

Today, wearable electronics devices combine a large variety of functional, stretchable, and flexible technologies. However, in many cases, these devices cannot be worn under everyday conditions. Therefore, textiles are commonly considered the best substrate to accommodate electronic devices in wearable use. In this paper, we describe how to selectively pattern organic electroactive materials on textiles from a solution in an easy and scalable manner. This versatile deposition technique enables the fabrication of wearable organic electronic devices on clothes.

In this paper, we present a protocol to selectively deposit organic materials on textiles, which allows for the direct integration of organic electronic devices with wearables. The fabricated devices can be fully integrated in textiles, respecting their mechanical appearance and enabling sensing capabilities.

关于纺织品有机电子设备的简单和可扩展的制作方法

Today, wearable electronics devices combine a large variety of functional, stretchable, and flexible technologies. However, in many cases, these devices ...

胺化化合物的浸渍和接枝到二氧化硅基材上

A Synthetic Methodology for Preparing Impregnated and Grafted Amine-Based Silica Composites for Carbon Capture

Recently, there has been a significant effort towards reducing or mitigating CO2 emissions through the use of carbon capture materials for point source or direct air capture (DAC) methods. This work focuses on amine-functionalized CO2 adsorbents for DAC. These materials show promise for CO2 removal because they have low regeneration energy consumption and high adsorption capacity. The incorporation of amine species into a porous substrate combines the advantages of the amine species&#39; affinity to CO2 with the large pore volumes and surface areas of the porous substrate. There are three methods commonly used to prepare amine-based CO2 sorbents, depending on the selection of the amine species, material support, and preparation method. These methods are impregnation, grafting, or chemical synthesis. Silica is a prevalent choice of substrate material because of its adjustable pore size, moisture tolerance, temperature stability, and ability to adsorb CO2 in low concentrations for DAC applications. Typical synthetic procedures and primary attributes of both impregnated and grafted amine-silica composites are described herein.

作者聚焦:胺基二氧化硅复合材料作为直接空气捕获的 CO2 吸附剂的标准化开发 

This work aims to facilitate the development of standardized techniques for impregnating or grafting aminated compounds onto silica substrates, which are often broadly described in the literature. Specific amounts of solvent, substrate, amines, and the values of other important experimental parameters will be discussed in detail.

一种制备浸渍接枝胺基二氧化硅复合材料的合成方法

Recently, there has been a significant effort towards reducing or mitigating CO2 emissions through the use of carbon capture materials for point source or ...

织物支架上多孔吸附剂的沉积

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此视频中的章节

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

表征和被动采样的应用在农药水监测

空气过滤设备，包括非织造网格静电重组蜘蛛丝蛋白

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

溶剂热合成 MIL-96 和 UiO-66-NH₂在纤维垫上原子层沉积金属氧化物涂层上的合成

合成纳米碳和二氧化硅矩阵的表面性能

水凝胶的合成与防污性能作为膜的净水

关于纺织品有机电子设备的简单和可扩展的制作方法

一种制备浸渍接枝胺基二氧化硅复合材料的合成方法

一种制备浸渍接枝胺基二氧化硅复合材料的合成方法