This research has been funded by Deutsche Forschungsgemeinschaft (DFG) within the framework of the priority program 1570: porous media with defined pore system in process engineering - modeling, application, synthesis, under grant numbers DI 696/9-1 to -3 and SCHW 478/23-1 to -3.

注意:使用前请咨询所有相关的材料安全数据表（MSDS）。几个在沸石H-ZSM-5的合成中使用的化学品是剧毒和致癌性。相比，他们的大部分对手纳米材料可能有额外的风险。进行纳米晶体的反应包括利用工程控制（通风橱，手套箱）和个人防护装备时，请使用所有适当安全守则（安全眼镜，手套，实验室外套，全长裤，封闭趾鞋）。此外，要特别注意的时候，进行吸附测量用甲醇和二甲醚，因为两者都是易燃易爆危险品。 在LCM 1沸石的合成的H-ZSM-5 <ol><li> 沸石合成混合物的制备 注意:最终合成混合物具有如下的摩尔组成如从德拉伊格莱西亚等 7适于:1的SiO 2:50 H 2 O:0.07的Na 2 O:0.024 TPA 2 O:0.005 的 Al 2 O 3。因此，该合成沸石的理论的Si / Al摩尔比的H-ZSM-5是100。 <ol><li>通过搅拌溶解在20.30克去离子含水量是0.14克氢氧化钠。可替代地，混合3.64克1 M氢氧化钠的16.8克去离子水。 </li><li>添加1.16克氢氧化四丙铵（TPAOH）溶液，直到出现明确的搅拌溶液。 </li><li>添加5.0克正硅酸乙酯（TEOS）溶液中滴加，直到出现明确的搅拌溶液。 </li><li>不断搅拌，同时加入0.09克硝酸铝九水合物（铝（NO 3）3·9H 2 O，固体）到溶液中。 </li><li>不断搅拌，直到固体九水合硝酸铝溶解。需要注意的是制备沸石合成混合物应5小时内使用，由于其老化。 </li></ol></li><li> 经由SAC 3的LCM沸石ZSM-5的合成 </st荣&gt; <ol><li> 沸石合成前清理LCM <ol><li>与去离子水彻底清洗LCM。 </li><li>把LCM与去离子水的烧杯中，并在超声浴进行清洁。 </li><li>干燥在80℃的LCM在烘箱。 </li></ol></li><li> 合成沸石 <ol><li>小心地将在LCM的中心电极上的制备的沸石合成混合物的数滴， 如图1用移液管，因为只沉积在金电极上的沸石可引起LCM 8的谐振频率偏移。此外，避免在金电极到振荡器的连接点散布在合成混合物中，由于在连接点的沸石将显著降低电导率，因而LCM的测量灵敏度。此外，沉积物等后除去该连接点的沸石晶体ñ会破坏电极。 </li><li>干燥与合成混合物中的LCM，在80℃进行2小时，得到在其上高粘性凝胶状相。 </li><li>在特氟隆内衬的高压釜（80毫升），以便在沸石合成过程中，以产生蒸汽添加的去离子水（约10毫升）量小。 </li><li>把聚四氟乙烯支架在高压釜，这在高压釜的沸石合成过程中的底部水平地支撑液态水上面的LCM。 </li><li>保持高压釜在烘箱中在150℃下48小时经由SAC方法合成的LCM沸石。 </li><li>在SAC之后，洗涂LCM与去离子水，并在80℃下使其干燥2小时。 </li><li>氧化气氛下，在高温烘箱通过煅烧除去在沸石晶体中的有机模板。程序烤箱如下:a）增加从环境温度到450℃的温度的速率3℃分钟-1; B）保持温度在450℃下进行4小时;三）降低从450℃至室温的温度以3℃分钟的速度-1。 </li><li>在0.4升去离子水溶解26.75克氯化铵（NH 4氯，固体）。在溶液中加入更多去离子水，使最终的NH 4 Cl溶液是0.5升，并具有1摩尔分米-3的浓度。 </li><li>把涂覆的LCM入一个烧杯中的 NH 4 Cl溶液（0.2升），并在20℃下2小时的离子交换涂覆在LCM中的Na-ZSM-5的晶体。重复使用0.2升新鲜的 NH 4 Cl溶液来获得的 NH 4 -ZSM-5的晶体的离子交换。 </li><li>通过使用相同的参数最终煅烧获得的H-ZSM-5如步骤1.2.2.7提及。 </li></ol></li></ol></li></ol> 2.吸附测量使用基于LCM-吸附测量装置3 注:在这项工作中，LCM无涂层和一个涂有H-ZSM-5（在最后一节的方法制备）被称为"参考LCM"和"样品LCM"，分别。此外，沸石沉积前样品LCM被称为"卸载样品LCM"。在物理化学杂志的 C 3的先前出版物中，基于LCM-吸附测定装置的详细描述可以找到。在这项工作中，气体吸附测量装置的操作，提出在该短协议和在详细视频协议。 <ol><li> 吸附测量前的准备工作 <ol><li> 上的温度和压力上在参考的共振频率之差的影响测试和卸载样品的LCM <ol><li>清洁O形环，LCM的保持器，并用丙酮样品室和加压空气。 </li><li>把参考和卸载样品的LCM中使用去离子水的烧杯中，并在一个微升清洁它们trasound洗澡。 </li><li>小心地将干净的参考和卸载样品的LCM对LCM保持器，其连接到通过耐高温电缆的振荡器。 </li><li>预测试使用振荡器来确保谐振频率可以被成功地检测到已安装的LCM。 </li><li>关闭样品室，并用真空泵抽空它。 </li><li>通过定量纯的N 2改变在样品室中的压力。 </li><li>通过温度控制器控制样品室内部的温度。 </li><li>测量参考的在所研究的温度和压力范 ​​围的谐振频率和卸载样品的LCM， 即 ，50-150℃，0-16巴，为了知道温度和压力对的谐振频率的差的影响参考和卸载样品的LCM（ <img alt="公式（2）" src="/files/ftp_upload/54413/54413eq2.jpg" />在步骤2.2.4）。的测试表明<img a所述="公式2"SRC ="/文件/ ftp_upload / 54413 / 54413eq2.jpg"/&gt;是显著受温度（1200〜3000赫兹在50〜150℃），而气体压力没有显著效果（变化<img alt="公式（2）" src="/files/ftp_upload/54413/54413eq2.jpg" />在0-16巴的压力范围小于300赫兹）。使用的确定值<img alt="公式（2）" src="/files/ftp_upload/54413/54413eq2.jpg" />在步骤2.2.4索尔布雷方程中以计算在沸石气体的吸附量。 </li></ol></li><li> 样品LCM激活 <ol><li>清洁O形环，LCM的保持器，并用丙酮样品室和加压空气。 </li><li>把基准的LCM中使用去离子水的烧杯中，并在超声浴进行清洁。 </li><li>小心放置在LCM保持器，其连接到通过耐高温电缆的振荡器的清洁参考LCM和样品LCM。 </li><li>前测解放军使用振荡器CED的LCM，以确保谐振频率可以被成功地检测到。 </li><li>关闭样品室，并用真空泵抽空它。 </li><li>激活在高温下的样本的LCM（至少50℃比吸附测量的温度，200℃在这项工作中更高）在真空条件下过夜，以确保只有可忽略的气体量被吸附在H-ZSM-5 。 </li></ol></li></ol></li><li> 吸附测量 注意:在本工作中，提出了在50℃下的 CO 2吸附测定，得到的例子。从测量（ 例如 ，谐振频率）和吸附的 CO 2在H-ZSM-5的计算质量所获得的数据可以在我们以前的出版物3的支持信息的表S1中找到。 <ol><li>调整样品室内部的温度在adsorpti的所需温度<html>上测量（ 即 ，50±0.1℃）通过一个温度控制器，在真空条件下， 即 ，只与吸附气体的一个可忽略的量。 </li><li>连接振荡器到样品LCM，并测量通过与巴特沃斯-范戴克等效电路模型拟合实验数据由振荡器的支持软件其谐振频率。 </li><li>切换振荡器的参考LCM的连接，并测量其谐振频率。 </li><li>使用样品和参考的LCM的测量谐振频率在真空条件下根据索尔布雷方程2,8确定的H-ZSM-5沉积在样品上的LCM质量（不吸附的气体）: <img alt="公式3" src="/files/ftp_upload/54413/54413eq3.jpg" /> 哪里<html> 413 / 54413eq4.jpg"/&gt;是在克质量的差异， <img alt="公式5" src="/files/ftp_upload/54413/54413eq5.jpg" />是（在该晶体被驱动谐波数在这项研究中， <img alt="公式6" src="/files/ftp_upload/54413/54413eq6.jpg" /> ） <img alt="公式7" src="/files/ftp_upload/54413/54413eq7.jpg" />是在以​​Hz参照和样品的LCM谐振频率的差， <img alt="公式（2）" src="/files/ftp_upload/54413/54413eq2.jpg" />是以Hz为单位的参考和卸载样品LCM之间的共振频率的差， <img alt="式（8）" src="/files/ftp_upload/54413/54413eq8.jpg" />是langatate晶体的密度（6.13克cm -3）的4， <img alt="公式9" src="/files/ftp_upload/54413/54413eq9.jpg" />是langatate晶体（1.9×1012克 -1秒-2）4的有效压电硬挺剪切模量，/files/ftp_upload/54413/54413eq10.jpg"/&gt;是参考LCM的共振频率， 即 ，卸载LCM， <img alt="11式" src="/files/ftp_upload/54413/54413eq11.jpg" />中，LCM的面积（1.539厘米2）3。 注意:在本工作中，H-ZSM-5的沉积在LCM中心的金电极的质量为0.502毫克，这导致在50℃下14100赫兹的谐振频率偏移。 </li><li>通过经由质量流量控制器从气体钢瓶给药纯气体（甲醇和DME，从蒸发器经由计量阀进入腔室手动地）控制的 CO 2的样品室中的气体压力，或者通过真空泵抽真空。这里，可使用0-16巴的 CO 2吸附测量的压力范 ​​围， 如图2。 </li><li>等到平衡条件和稳定的温度已达成， 例如 ，温度在50±0.1℃的变化。 </li><li>有限公司nnect振荡器到样品LCM，并测量在给定的压力接触到所述气体后的谐振频率。 </li><li>切换振荡器的参考LCM的连接，并测量在相同条件下其谐振频率。 </li><li>根据以上所示的索尔布雷方程，计算H-ZSM-5的沉积在样品上的LCM和气体该气体在压力下吸附在H-ZSM-5的总质量。减去H-ZSM-5的步骤2.2.4确定的质量（不吸附的气体），CO 2的质量，得到该气体在压力下吸附在H-ZSM-5。 </li><li>重复样品和参考的LCM谐振频率的测量，用于改变压力，为了获得CO 2的所有群众吸附于不同的气体压力的H-ZSM-5样品。 </li><li>最后，通过计算的 CO 2吸附的所有群众获得的气体吸附等温线在50℃下在0-16巴的所研究的压力范 ​​围下按照步骤2.2.9不同的气体压力下的H-ZSM-5样品。 </li><li>对于在其他温度下吸附等温线，更改使用温度控制器稳定的温度，并重复步骤2.2.1到2.2.11。 </li><li>适合具有吸附模型，如通过最小二乘法确定的吸附参数，如吸附容量，吸附焓和吸附熵朗缪尔模型吸附等温线（参见前公布3和支持信息）。 </li></ol></li></ol>

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The authors have nothing to disclose.

在这项工作中，在由SAC LCM的传感器的中心的金电极的沸石H-ZSM-5晶体的成功合成证明的， 即 ，该沸石已成功装载在LCM传感器没有覆盖的连接点金电极的振荡器。因此，沸石可以用LCM传感器一起摆动，而LCM传感器保持其良好的导电性和测量灵敏度。相比这些限制为低于80℃的常规的QCM装置，在这项工作中提出的LCM装置成功地用于在温度高达150℃， 即 ，在或接近在工业反应的温度下的吸附测量。然而，本LCM装置被限制在200℃以下。在温度高于200℃时，测量的不确定性可能会超过吸附气体的质量，因为，随着温度的升高超过150℃，则adsor的质量煤层气有显著下降，而测量的不确定性，由于温度降低控制精度显著增加。因此，在未来的实验中，应开发一种新的方法来对LCM，这将导致更多的气体吸附存入更多的沸石，而且补偿的温度和压力上的效果<img alt="公式（2）" src="/files/ftp_upload/54413/54413eq2.jpg" /> 。这可以帮助到LCM装置的应用范围扩大到更高的温度。 在实验过程中，在沸石合成中的关键步骤是步骤1.2.2.1，1.2.2.4，1.2.2.5和1.2.2.7，而在吸附测量步骤2.1.1.3，2.1.1.4，2.2.1，2.2 .5 2.2.6。在步骤1.2.2.1，避免对LCM，这将铺在金电极的连接点放置太多的合成混合物。在步骤1.2.2.4，小心地把聚四氟乙烯支架与LCM在高压釜中以确保该LCM为horizo​​ntal并在底部不接触液态水。在步骤1.2.2.5和1.2.2.7，不使用在沸石合成和煅烧一个较高的温度，因为我们以前的实验表明，它导致到LCM的降解。在吸附测量时，LCM传感器的位置对LCM传感器的连接的振荡器的显著效果，因此，对共振频率的信号的质量。因此，要特别注意步骤2.1.1.3 2.1.1.4和，其中的LCM都装上支架和预测试。所述的LCM应在它们与经由电极的连接点的振荡器连接的位置（ 图1中所示）。这是强制性的，以获得高质量的共振频率信号实现高的测量精度。此外，在步骤2.2.1和2.2.6中，确保了稳定的温度测量之前实现的，因为这也增加了测量ACCU活泼。此外，在步骤2.2.5，喂气慢，为了具有内的温度的微小变化。这有助于温度在短时间后再次变得稳定。 由于用于沸石H-ZSM-5在SAC合成方法在LCM传感器可以很容易地扩展到其他的沸石，所述基于LCM-吸附测定装置预期用于它们。而且，由于它的高精确度和低成本，这种装置可望适用于任何材料，其可以被涂覆在LCM中，为了在高温下，调查其吸附性能。

吸附性能强烈地影响催化材料的性能，这些性能，因此精确知识可以帮助表征，设计和这样的材料的最优化。然而，吸附性能通常由单组分吸附测量判断往往在室温下或甚至在液体氮的条件下，并因此延伸到实际情况可能会导致从真实行为严重偏差， 在对催化材料原位吸附测量特别是在高温和高压的条件下，仍然是一个极大的挑战。 基于石英晶体微天平（QCM）的吸附测定装置是通过在一种方式商业化的体积和重量的方法有利的是它是用于大规模的吸附应用，在受控环境中令人满意地稳定高精确度，更实惠1-2。 HoweveR，以往的QCM分析限于温度低于80℃1-2。为了克服这一限制，我们开发了基于高温高频振荡微量天平吸附测量装置（langatate体微量天平，LCM）3，其可以在温度高达200-300°实现原则上吸附测量C，由于没有结晶相转变到它的熔点（1470℃）4。在这项工作中所用的的LCM具有AT切割（ 即 ，晶体微量天平的板包含晶体的x轴，并且由35°15&#39;从z轴线倾斜）和5MHz的共振频率。此装置是在温度范围50-150℃，压力范 ​​围施加到的 CO 2的吸附测量，H 2 O，甲醇和二甲醚（DME），每个在气态状态下，在沸石H-ZSM-5 0-18条3，针对validati仿真模型的双功能核壳催化剂用于从合成气5-6一阶段生产二甲醚的优化。如何操作该设备的气体吸附测量，提出在协议部分。 之前的吸附测量，沸石H-ZSM-5的微晶（0.502毫克）在金电极在LCM由蒸汽辅助结晶（SAC）方法中心根据德拉伊格莱西亚等 7合成，在该沸石晶粒保持附着在振荡微量天平这样的方式。 如图1所示，在吸附测定装置中使用的液晶显示模块已经两面抛光，这有助于到LCM连接到一个振荡器金电极。由于在金电极的振荡器将显著降低电导率的连接点的沸石晶体（ 如图1所示），从而使LCM的的测量灵敏度，沸石H-ZSM-5的晶体沉积在经由SAC方法不覆盖这些连接点3的LCM。关于沸石H-ZSM-5上的LCM合成的细节进行了简要概括在以下方案部分和详细视频协议所示。

<table><tbody><tr><td>tetraethyl orthosilicate (TEOS), other name: tetraethoxysilane</td><td>Alfa Aesar</td><td>A14965</td><td>purity &gt; 98%, acutely toxic, inflammable and explosive</td></tr><tr><td>aluminum nitrate nonahydrate: Al(NO&lt;sub&gt;3&lt;/sub&gt;)&lt;sub&gt;3&lt;/sub&gt;&amp;#8226;9H&lt;sub&gt;2&lt;/sub&gt;O</td><td>Chempur</td><td>000176</td><td>purity &gt; 98.5%</td></tr><tr><td>tetrapropylammonium hydroxide: (TPAOH)</td><td>Sigma-Aldrich</td><td>254533</td><td>1&amp;nbsp;mol&amp;nbsp;dm&lt;sup&gt;-3&lt;/sup&gt; aqueous solution, skin corrosive</td></tr><tr><td>sodium hydroxide: NaOH</td><td>Merck</td><td>106498</td><td>purity &gt; 99%, skin corrosive</td></tr><tr><td>Ammonium chloride: NH&lt;sub&gt;4&lt;/sub&gt;Cl</td><td>Merck</td><td>101145</td><td>purity &gt; 99.8%, harmful</td></tr><tr><td>Carbon dioxide (CO&lt;sub&gt;2&lt;/sub&gt;)</td><td>Air Liquide</td><td>---</td><td>purity &gt; 99.7%</td></tr><tr><td>high-pressure stainless steel chamber</td><td>B&amp;uuml;chi AG, Uster, Switzerland</td><td>Midiclave</td><td>Volume = 300 ml, up to 200&amp;nbsp;bar, 300&amp;nbsp;&amp;deg;C</td></tr><tr><td>langatate crystal microbalance sensors</td><td>C3 Prozess- and Analysentechnik GmbH, Munich, Germany</td><td>---</td><td>Diameter: 14 mm, resonant frequency: 5&amp;nbsp;MHz</td></tr><tr><td>high-frequency oscillating microbalance</td><td>Gamry Instruments, Warminster, USA</td><td>eQCM 10M</td><td>Frequency range: 1 MHz - 10 MHz (15 MHz), resolution: 20 mHz</td></tr></tbody></table>

adsorption device based on a langatate crystal microbalance for high temperature high pressure gas adsorption in zeolite h-zsm-5

我们提出了一种基于一个高频振荡微量天平（5兆赫langatate体微量天平，LCM）的高温和高压的气体吸附测量装置和在沸石的H-ZSM-5的气体吸附测量使用。之前的吸附测量，沸石H-ZSM-5的晶体在LCM的中心的金电极合成，而不覆盖金电极的连接点到所述振荡器，由蒸汽辅助结晶（SAC）方法，以便同时保持在吸附测量LCM的良好的导电性的沸石晶体保持连接到振荡微量天平。相比传统的石英晶体微天平（QCM），其被限制在温度低于80℃时，LCM可实现在温度高达200-300℃的（ 即 ，在或接近反应温度原则上吸附测量一阶段的目标应用从合成气DME合成），由于没有结晶相转变到它的熔点（1470℃）。该系统应用到调查的 CO 2的吸附，H 2 O，甲醇和二甲醚（DME），每个在气相，在沸石H-ZSM-5中的温度和压力范 ​​围50-150℃，并0-18条，分别为。结果表明，在H-ZSM-5可以很好地通过朗缪尔型吸附等温线拟合这些气体的吸附等温线。此外，所确定的吸附参数， 即 ，吸附容量，吸附焓和吸附熵，比较以及文献资料。在这项工作中，对CO 2的结果显示为一个例子。

图1显示了照片，光学显微镜和涂覆和未涂覆的LCM传感器（左）的扫描电子显微镜（SEM）图像，以及它们的X射线衍射（XRD）图案（右）。从两者，光和扫描电子显微镜（ 图1b和c）中 ，金电极到振荡器的连接点较少覆盖有沸石晶体比LCM的中心区域。最上的LCM-传感器的顶部的沸石晶体被分离并出现舍入船形态，与（010）面为主朝上。此外，一些晶体还表现出典型的共​​生行为（"孪晶"）。此外，装载的H-ZSM-5上的langatate晶体（的Si / Al摩尔的100根据合成混合物的组成比）由X射线衍射和波长色散X射线研究（WDX）光谱3。 在图2中，与在该温度范围50-150℃，0-16巴的压力范 ​​围的LCM设备，以及单中心朗缪尔的拟合获得的H-ZSM-5沸石的 CO 2吸附等温线等温线模型的实验数据，示出以得到代表性的例子。正如图2所示， 二氧化碳的所确定的吸附等温线拟合使用单中心Langmuir等温以及图3示出了LN的图（K&#39;ⅰ）与1000 / T的CO 2从吸附等温线获得， 即 ，从吸附等温线的拟合确定吸附常数的温度依赖性。 二氧化碳的吸附焓和熵分别通过与范特霍夫方程拟合决定（见前面的出版物的支持信息3）。的模型拟合的结果表明在吸附容量，吸附焓和吸附熵为CO 2 H-ZSM-5是4.0±0.2毫摩尔克-1，15.3±0.5千焦耳摩尔-1和56.3±1.5焦耳摩尔-1 K -1，分别为3。 如图2和3中的单中心Langmuir等温和范特霍夫等式的拟合的高质量支持恒定的吸附容量的假设（ 即 ，饱和装载）和焓（ 即吸附热），以至少为的条件下使用的范围内是有效的。此外，通过基于LCM-吸附测定装置在这项工作中确定的 CO 2的吸附参数比较很好地在文献9-12， 也就是说 ，吸附容量，吸附焓和吸附熵回购报告值rted对CO 2中MFI型沸石中的2.1-3.8毫克-1，19-28.7千焦耳摩尔-1，43.7-82.7Ĵ摩尔的范围-1 K -1，分别发生变化的温度范围内的30 -200℃，0-5巴的压力范围。 <img alt="图1" src="/files/ftp_upload/54413/54413fig1.jpg" /> 图1.涂langatate体微天平传感器（左）。 （a）该涂覆和未涂覆传感器（右）的照片，（B）光镜和（c）扫描型电子显微镜图像。涂覆和未涂覆的LCM传感器（右）的X射线衍射图案。这个数字已经从以前的出版物3修改。与美国化学学会（版权2015年）的许可复制。 <a href="https://jove.unicartagenaproxy.elogim.com/files/ftp_upload/54413/54413fig1large.jpg" target="_blank">请点击此处查看大版本</a>这个数字的锡永。 <img alt="图2" src="/files/ftp_upload/54413/54413fig2.jpg" /> 在图2中的吸附等温线为CO 2 H-ZSM-5 50（ <img alt="12式" src="/files/ftp_upload/54413/54413eq12.jpg" /> ），75（ <img alt="13式" src="/files/ftp_upload/54413/54413eq13.jpg" /> ），100（ <img alt="14式" src="/files/ftp_upload/54413/54413eq14.jpg" /> ），以及150℃（ <img alt="15式" src="/files/ftp_upload/54413/54413eq15.jpg" /> ）。符号表示实验数据，误差棒表示共振频率的测量的不确定性引起的， 例如 ，温度不稳定，并如步骤2.2.4描述根据索尔布雷等式计算，而线代表的配合的单中心Langmuir等温模型的实验数据。这个数字公顷Ş已经从以前的出版物3修改。与美国化学学会（版权所有2015）的许可复制。 <a href="https://jove.unicartagenaproxy.elogim.com/files/ftp_upload/54413/54413fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图3" src="/files/ftp_upload/54413/54413fig3.jpg" /> 图3 LN（K I）与1000 / T来确定吸附焓和熵的CO 2，该图已被从先前的出版物3改性。与美国化学学会（版权所有2015）的许可复制。 <a href="https://jove.unicartagenaproxy.elogim.com/files/ftp_upload/54413/54413fig3large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

Watch this Scientific Journal Video about Adsorption Device Based on a Langatate Crystal Microbalance for High Temperature High Pressure Gas Adsorption in Zeolite H-ZSM-5 at JoVE.com

Adsorption Device Based on a Langatate Crystal Microbalance for High Temperature High Pressure Gas Adsorption in Zeolite H-ZSM-5

A protocol for high-temperature and high-pressure gas adsorption measurements on zeolite H-ZSM-5 using an adsorption measurement device based on a langatate crystal microbalance is presented. Prior to the adsorption measurements, the synthesis of zeolite H-ZSM-5 on the langatate crystal microbalance sensor by the steam-assisted crystallization (SAC) method is demonstrated.

基于一个Langatate体微天平的高温高压气体吸附在分子筛吸附器H-ZSM-5

We present a high-temperature and high-pressure gas adsorption measurement device based on a high-frequency oscillating microbalance (5 MHz langatate ...

adsorption-device-based-on-langatate-crystal-microbalance-for-high

Universidad de Cartagena UDEC

Research

JoVE Journal

Engineering

11.5K 次观看.  Karlsruhe Institute of Technology (KIT). A protocol for high-temperature and high-pressure gas adsorption measurements on zeolite H-ZSM-5 using an adsorption measurement device based on a langatate crystal microbalance is presented. Prior to the adsorption measurements, the synthesis of zeolite H-ZSM-5 on the langatate crystal microbalance sensor by the steam-assisted crystallization (SAC) method is demonstrated.

视频: Adsorption Device Based on a Langatate Crystal Microbalance for High Temperature High Pressure Gas Adsorption in Zeolite H-ZSM-5

Synthesis of Zeolites Using the ADOR (Assembly-Disassembly-Organization-Reassembly) Route

Zeolites are an important class of materials that have wide ranging applications such as heterogeneous catalysts and adsorbents which are dependent on their framework topology. For new applications or improvements to existing ones, new zeolites with novel pore systems are desirable. We demonstrate a method for the synthesis of novel zeolites using the ADOR route. ADOR is an acronym for Assembly, Disassembly, Organization and Reassembly. This synthetic route takes advantage of the assembly of a relatively poorly stable that which can be selectively disassembled into a layered material. The resulting layered intermediate can then be organized in different manners by careful chemical manipulation and then reassembled into zeolites with new topologies. By carefully controlling the organization step of the synthetic pathway, new zeolites with never before seen topologies are capable of being synthesized. The structures of these new zeolites are confirmed using powder X-ray diffraction and further characterized by nitrogen adsorption and scanning electron microscopy. This new synthetic pathway for zeolites demonstrates its capability to produce novel frameworks that have never been prepared by traditional zeolite synthesis techniques.

Synthesis of Zeolites Using the ADOR Assembly-Disassembly-Organization-Reassembly Route

A protocol for the preparation of novel zeolites by the ADOR (Assembly-Disassembly-Organization-Reassembly) synthetic route is presented.

沸石使用ADOR（汇编拆卸组织-重组）路线的合成

Zeolites are an important class of materials that have wide ranging applications such as heterogeneous catalysts and adsorbents which are dependent on ...

科研

化学

Detection and Recovery of Palladium, Gold and Cobalt Metals from the Urban Mine Using Novel Sensors/Adsorbents Designated with Nanoscale Wagon-wheel-shaped Pores

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in industrialized countries. Here, the development of optical mesosensors/adsorbents (MSAs) for efficient recognition and selective recovery of Pd(II), Au(III), and Co(II) from urban mine was achieved. A simple, general method for preparing MSAs based on using high-order mesoporous monolithic scaffolds was described. Hierarchical cubic Ia3d wagon-wheel-shaped MSAs were fabricated by anchoring chelating agents (colorants) into three-dimensional pores and micrometric particle surfaces of the mesoporous monolithic scaffolds. Findings show, for the first time, evidence of controlled optical recognition of Pd(II), Au(III), and Co(II) ions and a highly selective system for recovery of Pd(II) ions (up to ~95%) in ores and industrial wastes. Furthermore, the controlled assessment processes described herein involve evaluation of intrinsic properties (e.g., visual signal change, long-term stability, adsorption efficiency, extraordinary sensitivity, selectivity, and reusability); thus, expensive, sophisticated instruments are not required. Results show evidence that MSAs will attract worldwide attention as a promising technological means of recovering and recycling palladium, gold and cobalt metals.

Because of the importance and extensive use of palladium, gold and cobalt metals in high-technology equipment, their recovery and recycling constitute an important industrial challenge. The metal recovery system described herein is a simple, low-cost means for the effective detection, removal, and recovery of these metals from the urban mine.

检测和钯的回收，从城市矿山黄金和钴金属使用标有纳米货车车轮形的孔隙新型传感器/吸附剂

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in ...

工程学

Experimental System of Solar Adsorption Refrigeration with Concentrated Collector

To improve the performance of solar adsorption refrigeration, an experimental system with a solar concentration collector was set up and investigated. The main components of the system were the adsorbent bed, the condenser, the evaporator, the cooling sub-system, and the solar collector. In the first step of the experiment, the vapor-saturated bed was heated by the solar radiation under closed conditions, which caused the bed temperature and pressure to increase. When the bed pressure became high enough, the bed was switched to connect to the condenser, thus water vapor flowed continually from the bed to the condenser to be liquefied. Next, the bed needed to cool down after the desorption. In the solar-shielded condition, achieved by aluminum foil, the circulating water loop was opened to the bed. With the water continually circulating in the bed, the stored heat in the bed was took out and the bed pressure decreased accordingly. When the bed pressure dropped below the saturation pressure at the evaporation temperature, the valve to the evaporator was opened. A mass of water vapor rushed into the bed and was adsorbed by the zeolite material. With the massive vaporization of the water in the evaporator, the refrigeration effect was generated finally. The experimental result has revealed that both the COP (coefficient of the performance of the system) and the SCP (specific cooling power of the system) of the SAPO-34 zeolite was greater than that of the ZSM-5 zeolite, no matter whether the adsorption time was longer or shorter. The system of the SAPO-34 zeolite generated a maximum COP of 0.169.

With solar energy as the driving force, a novel adsorption refrigeration system has been developed and experimentally investigated. Water vapor and zeolite formed the working pair of the adsorption system. This manuscript describes the setup of the experimental rig, the operation procedure, and the important results.

聚光集热器太阳能吸附制冷实验系统

To improve the performance of solar adsorption refrigeration, an experimental system with a solar concentration collector was set up and investigated. The ...

环境科学

Experimental Study of the Relationship Between Particle Size and Methane Sorption Capacity in Shale

The amount of adsorbed shale gas is a key parameter used in shale gas resource evaluation and target area selection, and it is also an important standard for evaluating the mining value of shale gas. Currently, studies on the correlation between particle size and methane adsorption are controversial. In this study, an isothermal adsorption apparatus, the gravimetric sorption analyzer, is used to test the adsorption capacity of different particle sizes in shale to determine the relationship between the particle size and the adsorption capacity of shale. Thegravimetric method requires fewer parameters and produces better results in terms of accuracy and consistency than methods like the volumetric method. Gravimetric measurements are performed in four steps: a blank measurement, preprocessing, a buoyancy measurement, and adsorption and desorption measurements. Gravimetric measurement is presently considered to be a more scientific and accurate method of measuring the amount of adsorption; however, it is time-consuming and requires a strict measuring technique. A Magnetic Suspension Balance (MSB) is the key to verify the accuracy and consistency of this method. Our results show that adsorption capacity and particle size are correlated, but not a linear correlation, and the adsorptions in particles sieved into 40 - 60 and 60 - 80 meshes tend to be larger. We propose that the maximum adsorption corresponding to the particle size is approximately 250 &#181;m (60 mesh) in the shale gas fracturing.

We use an isothermal adsorption apparatus, the gravimetric sorption analyzer, to test the adsorption capacity of different particle sizes of shale, in order to find out the relationship between particle size and the adsorption capacity of shale.

页岩中粒径与甲烷吸附能力关系的实验研究

The amount of adsorbed shale gas is a key parameter used in shale gas resource evaluation and target area selection, and it is also an important standard ...

Preparation of Biomass-based Mesoporous Carbon with Higher Nitrogen-/Oxygen-chelating Adsorption for Cu(II) Through Microwave Pre-Pyrolysis

An environment-friendly technique for synthesizing biomass-based mesoporous activated carbon with high nitrogen-/oxygen-chelating adsorption for Cu(II) is proposed. Bagasse impregnated with phosphoric acid is utilized as the precursor. To pyrolyze the precursor, two separate heating modes are used: microwave pyrolysis and conventional electric-heating pyrolysis. The resulting bagasse-derived carbon samples are modified with nitrification and reduction modification. Nitrogen (N)/oxygen (O) functional groups are simultaneously introduced to the surface of activated carbon, enhancing its adsorption of Cu(II) by complexing and ion-exchange. Characterization and copper adsorption experiments are performed to investigate the physicochemical properties of four prepared carbon samples and determine which heating method favors the subsequent modification for doping of N/O functional groups. In this technique, based on analyzing data of nitrogen adsorption, Fourier transform infrared spectroscopy, and batch adsorption experiments, it is proven that microwave-pyrolyzed carbon has more defect sites and, therefore, time-saving effective microwave pyrolysis contributes more N/O species to the carbon, although it leads to a lower specific surface area. This technique offers a promising route to synthesis adsorbents with higher nitrogen and oxygen content and a higher adsorption capacity of heavy-metal ions in wastewater remediation applications.

Preparation of Biomass-based Mesoporous Carbon with Higher Nitrogen-/Oxygen-chelating Adsorption for CuII Through Microwave Pre-Pyrolysis

Here, we present a protocol to synthesize nitrogen/oxygen dual-doped mesoporous carbon from biomass by chemical activation in different pyrolysis modes followed by modification. We demonstrate that the microwave pyrolysis benefits the subsequent modification process to simultaneously introduce more nitrogen and oxygen functional groups on the carbon.

微波热解法制备了更高氮素/氧螯合吸附的生物物质基介孔碳对 cu (ii) 的研究

An environment-friendly technique for synthesizing biomass-based mesoporous activated carbon with high nitrogen-/oxygen-chelating adsorption for Cu(II) is ...

Nanostructured Ag-zeolite Composites as Luminescence-based Humidity Sensors

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high external quantum efficiencies (EQE) and spans the whole visible spectrum. It has been recently reported that the UV excited luminescence of partially Li-exchanged sodium Linde type A zeolites [LTA(Na)] containing luminescent silver clusters can be controlled by adjusting the water content of the zeolite. These samples showed a dynamic change in their emission color from blue to green and yellow upon an increase of the hydration level of the zeolite, showing the great potential that these materials can have as luminescence-based humidity sensors at the macro and micro scale. Here, we describe the detailed procedure to fabricate a humidity sensor prototype using silver-exchanged zeolite composites. The sensor is produced by suspending the luminescent Ag-zeolites in an aqueous solution of polyethylenimine (PEI) to subsequently deposit a film of the material onto a quartz plate. The coated plate is subjected to several hydration/dehydration cycles to show the functionality of the sensing film.

A protocol for the synthesis of moisture-responsive luminescent Ag-zeolite composites is described in this report.

纳米银沸石复合材料作为基于发光的湿度传感器

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high ...

Two-way Valorization of Blast Furnace Slag: Synthesis of Precipitated Calcium Carbonate and Zeolitic Heavy Metal Adsorbent

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with sufficient heavy metal adsorption capacity. To this end, blast furnace slag, a residue from iron-making, is utilized as the starting material. Calcium is selectively extracted from the slag by leaching with acetic acid (2 M CH3COOH) as the extraction agent. The filtered leachate is subsequently physico-chemically purified and then carbonated to form precipitated calcium carbonate (PCC) of high purity (&lt;2 wt% non-calcium impurities, according to ICP-MS analysis). Sodium hydroxide is added to neutralize the regenerated acetate. The morphological properties of the resulting calcitic PCC are tuned for its potential application as a filler in papermaking. In parallel, the residual solids from the extraction stage are subjected to hydrothermal conversion in a caustic solution (2 M NaOH) that leads to the predominant formation of a particular zeolitic mineral phase (detected by XRD), namely analcime (NaAlSi2O6&#8729;H2O). Based on its ability to adsorb Ni2+, as reported from batch adsorption experiments and ICP-OES analysis, this product can potentially be used in wastewater treatment or for environmental remediation applications.

A protocol for the parallel production of precipitated calcium carbonate and zeolitic material from blast furnace slag via mineral carbonation and alkaline hydrothermal conversion, respectively, is presented. The performance of the zeolitic material towards nickel adsorption is tested.

高炉矿渣的双向稳定物价:沉淀碳酸钙和沸石重金属吸附剂的合成

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with ...

Electrophoretic Crystallization of Ultrathin High-performance Metal-organic Framework Membranes

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and non-porous supports (polymer, ceramic, metal, carbon, and graphene). We developed a novel crystallization technique, which is termed the ENACT approach: the electrophoretic nuclei assembly for the crystallization of highly intergrown thin films (ENACT). This approach allows for a high density of heterogeneous nucleation of MOFs on a chosen substrate via the electrophoretic deposition (EPD) directly from the precursor sol. The growth of well-packed MOF nuclei leads to a highly intergrown polycrystalline MOF film. We show that this simple approach can be used for the synthesis of thin, intergrown zeolite imidazole framework (ZIF)-7 and ZIF-8 films. The resulting 500 nm-thick ZIF-8 membranes show a considerably high H2 permeance (8.3 x 10-6 mol m-2 s-1 Pa-1) and ideal gas selectivities (7.3 for H2/CO2, 15.5 for H2/N2, 16.2 for H2/CH4, and 2655 for H2/C3H8). An attractive performance for C3H6/C3H8 separation is also achieved (a C3H6 permeance of 9.9 x 10-8 mol m-2 s-1 Pa-1 and a C3H6/C3H8 ideal selectivity of 31.6 at 25 &#176;C). Overall, the ENACT process, owing to its simplicity, can be extended to synthesize intergrown thin films of a wide range of nanoporous crystalline materials.

A simple, reproducible, and versatile approach for the synthesis of intergrown, polycrystalline metal-organic framework membranes on a wide range of unmodified porous and non-porous supports is presented.

超薄高性能金属-有机骨架膜的电泳结晶

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and ...

Resource Recycling of Red Soil to Synthesize Fe2O3/FAU-type Zeolite Composite Material for Heavy Metal Removal

Heavy metal-polluted water is of great concern to human health and the eco-environment. In situ water remediation techniques enabled by highly efficient adsorption materials are of great importance in these circumstances. Among all the materials used in water remediation, iron-based nanomaterials and porous materials are of great interest, benefiting from their rich redox reactivity and adsorption function. Here, we developed a facile protocol to directly convert the widely spread red soil in south China to fabricate the Fe2O3/faujasite (FAU)-type zeolite composite material. 
The detailed synthesis procedure and synthesis parameters, such as reaction temperature, reaction time, and the Si/Al ratio in the raw materials, have been carefully tuned. The as-synthesized composite materials show good adsorption capacity for typical heavy metal(loid) ions. With 0.001 g/mL Fe2O3/FAU-type zeolite composite material added to different heavy metal(loid)-polluted aqueous solutions (single type of heavy metal(loid) concentration: 1,000 mg/L [ppm]), the adsorption capacity was shown to be 172, 45, 170, 40, 429, 693, 94, and 133 mg/g for Cu (II), Cr (III), Cr (VI), As (III), Cd (II), Pb (II), Zn (II), and Ni (II) removal, respectively, which can be further expanded for heavy metal-polluted water and soil remediation.

Resource Recycling of Red Soil to Synthesize Fe2O3/FAU-type Zeolite Composite Material for Heavy Metal Removal

This article presents a novel and convenient route to synthesize Fe2O3/faujasite (FAU)-type zeolite composite material from red soil. The detailed synthesis parameters have been finely tuned. The obtained composite material can be used for efficient heavy metal-contaminated water remediation, indicating its potential applications in environmental engineering.

红壤资源化循环利用合成Fe2O3/FAU型重金属去除用分子筛复合材料

Heavy metal-polluted water is of great concern to human health and the eco-environment. In situ water remediation techniques enabled by highly efficient ...

In situ FTIR Spectroscopy as a Tool for Investigation of Gas/Solid Interaction: Water-Enhanced CO2 Adsorption in UiO-66 Metal-Organic Framework

In situ infrared spectroscopy is an inexpensive, highly sensitive, and selective valuable tool to investigate the interaction of polycrystalline solids with adsorbates. Vibrational spectra provide information on the chemical nature of adsorbed species and their structure. Thus, they are very useful for obtaining molecular level understanding of surface species. The IR spectrum of the sample itself gives some direct information about the material. General conclusions can be drawn concerning hydroxyl groups, some stable surface species and impurities. However, the spectrum of the sample is &#34;blind&#34; with respect to the presence of coordinatively unsaturated ions and gives rather poor information about the acidity of surface hydroxyls, species decisive for the adsorption and catalytic properties of the materials. Furthermore, no discrimination between bulk and surface species can be made. These problems are solved by the use of probe molecules, substances that interact specifically with the surface; the alteration of some spectral features of these molecules as a result of adsorption provides valuable information about the nature, properties, location, concentration, etc., of the surface sites.
The experimental protocol for in-situ IR studies of gas/sample interaction includes preparation of a sample pellet, activation of the material, initial spectral characterization through the analysis of the background spectra, characterization by probe molecules, and study of the interaction with a particular set of gas mixtures. In this paper we investigate a zirconium terephthalate metal organic framework, Zr6O4(OH)4(BDC)6 (BDC = benzene-1,4-dicarboxylate), namely UiO-66 (UiO refers to University of Oslo). The acid sites of the UiO-66 sample are determined by using CO and CD3CN as molecular probes. Furthermore, we have demonstrated that CO2 is adsorbed on basic sites exposed on dehydroxylated UiO-66. Introduction of water to the system produces hydroxyl groups acting as additional CO2 adsorption sites. As a result, CO2 adsorption capacity of the sample is strongly enhanced.

In situ FTIR Spectroscopy as a Tool for Investigation of Gas/Solid Interaction: Water-Enhanced CO2 Adsorption in UiO-66 Metal-Organic Framework

The use of FTIR spectroscopy for investigation of the surface properties of polycrystalline solids is described. Preparation of sample pellets, activation procedures, characterization with probe molecules and model studies of CO2 adsorption are discussed.

原位FTIR 光谱作为气体/固体相互作用研究工具:UiO-66 金属-有机框架中的水增强 CO2吸附

In situ infrared spectroscopy is an inexpensive, highly sensitive, and selective valuable tool to investigate the interaction of polycrystalline solids ...

基于一个Langatate体微天平的高温高压气体吸附在分子筛吸附器H-ZSM-5

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