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Characterization Study of CO2, CH4, and CO2/CH4 Hydroquinone Clathrates Formed by Gas–Solid Reaction
The Journal of Physical Chemistry C ( IF 3.3 ) Pub Date : 2017-10-10 00:00:00 , DOI: 10.1021/acs.jpcc.7b07378
Romuald Coupan 1 , Eve Péré 2 , Christophe Dicharry 1 , Frédéric Plantier 3 , Joseph Diaz 1 , Abdel Khoukh 2 , Joachim Allouche 2 , Stephane Labat 2 , Virginie Pellerin 2 , Jean-Paul Grenet 2 , Jean-Marc Sotiropoulos 2 , Pascale Senechal 4 , Fabrice Guerton 4 , Peter Moonen 1, 4 , Jean-Philippe Torré 1
The Journal of Physical Chemistry C ( IF 3.3 ) Pub Date : 2017-10-10 00:00:00 , DOI: 10.1021/acs.jpcc.7b07378
Romuald Coupan 1 , Eve Péré 2 , Christophe Dicharry 1 , Frédéric Plantier 3 , Joseph Diaz 1 , Abdel Khoukh 2 , Joachim Allouche 2 , Stephane Labat 2 , Virginie Pellerin 2 , Jean-Paul Grenet 2 , Jean-Marc Sotiropoulos 2 , Pascale Senechal 4 , Fabrice Guerton 4 , Peter Moonen 1, 4 , Jean-Philippe Torré 1
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Hydroquinone (HQ) is known to form organic clathrates with some gaseous species such as CO2 and CH4. This work presents spectroscopic data, surface and internal morphologies, gas storage capacities, guest release temperatures, and structural transition temperatures for HQ clathrates obtained from pure CO2, pure CH4, and an equimolar CO2/CH4 mixture. All analyses are performed on clathrates formed by direct gas–solid reaction after 1 month’s reaction at ambient temperature conditions and under a pressure of 3.0 MPa. A collection of spectroscopic data (Raman, FT-IR, and 13C NMR) is presented, and the results confirm total conversion of the native HQ (α-HQ) into HQ clathrates (β-HQ) at the end of the reaction. Optical microscopy and SEM analyses reveal morphology changes after the enclathration reaction, such as the presence of surface asperities. Gas porosimetry measurements show that HQ clathrates and native HQ are neither micro- nor mesoporous materials. However, as highlighted by TEM analyses and X-ray tomography, α- and β-HQ contain unsuspected macroscopic voids and channels, which create a macroporosity inside the crystals that decreases due to the enclathration reaction. TGA and in situ Raman spectroscopy give the guest release temperatures as well as the structural transition temperatures from β-HQ to α-HQ. The gas storage capacity of the clathrates is also quantified by means of different types of gravimetric analyses (mass balance and TGA). After having been formed under pressure, the characterized clathrates exhibit exceptional metastability: the gases remain in the clathrate structure at ambient conditions over time scales of more than 1 month. Consequently, HQ gas clathrates display very interesting properties for gas storage and sequestration applications.
中文翻译：
气固反应生成CO 2，CH 4和CO 2 / CH 4对苯二酚包合物的表征研究
已知氢醌（HQ）与某些气态物质（例如CO 2和CH 4）形成有机包合物。这项工作介绍了从纯CO 2，纯CH 4和等摩尔CO 2 / CH 4混合物获得的HQ包合物的光谱数据，表面和内部形态，储气量，客体释放温度和结构转变温度。所有分析都是在环境温度条件下，在3.0 MPa的压力下，反应1个月后，通过直接气固反应形成的笼形物进行的。光谱数据的集合（拉曼光谱，傅立叶变换红外光谱和13结果显示，天然HQ（α-HQ）完全转化为HQ笼形物（β-HQ）。光学显微镜和SEM分析揭示了包封反应后的形态变化，例如表面凹凸不平的存在。气孔法测量表明，总部包合物和天然总部既不是微孔材料也不是中孔材料。但是，正如TEM分析和X射线断层扫描所突出显示的那样，α-和β-HQ包含了未预料到的宏观空隙和通道，这些空隙和通道在晶体内部产生了大孔隙，该孔隙由于包封反应而降低。TGA和原位拉曼光谱给出了客体释放温度以及从β-HQ到α-HQ的结构转变温度。包合物的储气量也通过不同类型的重量分析（质量平衡和TGA）进行定量。在压力下形成后，表征的包合物表现出卓越的亚稳性：在环境条件下，气体在超过1个月的时间范围内仍保留在包合物结构中。因此，总部气体包合物在气体储存和封存应用中显示出非常有趣的特性。
更新日期：2017-10-10
中文翻译：
气固反应生成CO 2，CH 4和CO 2 / CH 4对苯二酚包合物的表征研究
已知氢醌（HQ）与某些气态物质（例如CO 2和CH 4）形成有机包合物。这项工作介绍了从纯CO 2，纯CH 4和等摩尔CO 2 / CH 4混合物获得的HQ包合物的光谱数据，表面和内部形态，储气量，客体释放温度和结构转变温度。所有分析都是在环境温度条件下，在3.0 MPa的压力下，反应1个月后，通过直接气固反应形成的笼形物进行的。光谱数据的集合（拉曼光谱，傅立叶变换红外光谱和13结果显示，天然HQ（α-HQ）完全转化为HQ笼形物（β-HQ）。光学显微镜和SEM分析揭示了包封反应后的形态变化，例如表面凹凸不平的存在。气孔法测量表明，总部包合物和天然总部既不是微孔材料也不是中孔材料。但是，正如TEM分析和X射线断层扫描所突出显示的那样，α-和β-HQ包含了未预料到的宏观空隙和通道，这些空隙和通道在晶体内部产生了大孔隙，该孔隙由于包封反应而降低。TGA和原位拉曼光谱给出了客体释放温度以及从β-HQ到α-HQ的结构转变温度。包合物的储气量也通过不同类型的重量分析（质量平衡和TGA）进行定量。在压力下形成后，表征的包合物表现出卓越的亚稳性：在环境条件下，气体在超过1个月的时间范围内仍保留在包合物结构中。因此，总部气体包合物在气体储存和封存应用中显示出非常有趣的特性。
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