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首页> 外文期刊>Environmental Science & Technology >Characterization of a Mixture of CO_2 Adsorption Products in Hyperbranched Aminosilica Adsorbents by ~(13)C Solid-State NMR
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Characterization of a Mixture of CO_2 Adsorption Products in Hyperbranched Aminosilica Adsorbents by ~(13)C Solid-State NMR

机译：〜（13）C固态NMR表征超支化氨基二氧化硅吸附剂中CO_2吸附产物的混合物。

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摘要

Hyperbranched amine polymers (HAS) grown from the mesoporous silica SBA-1S (hereafter "SBA-1S-HAS") exhibit large capacities for CO, adsorption. We have used static in situ and magic-angle spinning (MAS) ex situ ~(13)C nuclear magnetic resonance (NMR) to examine the adsorption of CO_2 by SBA-15-HAS. ~(13)C NMR distinguishes the signal of gas-phase ~(13)CO_2 from mat of the chemisorbed species. HAS polymers possess primary, secondary, and tertiary amines, leading to multiple chemisorption reaction outcomes, including carbamate (RnNCOO~-), carbanuc add (RnNCOOH), and bicarbonate (HCO_3~-) moieties. Carbamates and bicarbonate fall within a small ~(13)C chemical shift range (162-166 ppm), and a mixture was observed including carbamic add and carbamate, the former disappearing upon evacuation of the sample By examining the ~(13)C-~(1+)N dipolar coupling through low-field (B_0 = 3 T) ~(13)C{~1H} cross-polarization MAS NMR, carbamate is confirmed through splitting of the ~(13)C resonance. A third spedes that is either bicarbonate, or a second carbamate is evident from bimodal T_2 decay times of the ～163 ppm peak, Indicating the presence of two spedes comprising mat single resonance. The mixture of products suggests that (1) the presence of amines and water leads to bicarbonate being present and/or (2) the multiple types of amine sites in HAS permit formation of chemically distinct carbamates.
机译：由中孔二氧化硅SBA-1S（以下称为“ SBA-1S-HAS”）生长的超支化胺聚合物（HAS）表现出大的CO吸附能力。我们已经使用静态原位和幻角旋转（MAS）异位〜（13）C核磁共振（NMR）来研究SBA-15-HAS对CO_2的吸附。 〜（13）C NMR从化学吸附物质的垫层中区分出气相〜（13）CO_2的信号。 HAS聚合物具有伯胺，仲胺和叔胺，从而导致多种化学吸附反应结果，包括氨基甲酸酯（RnNCOO-），碳酸钠添加（RnNCOOH）和碳酸氢盐（HCO_3-）部分。氨基甲酸酯和碳酸氢盐在一个很小的〜（13）C化学位移范围内（162-166 ppm），观察到包括氨基甲酸酯添加物和氨基甲酸酯的混合物，前者在抽空样品后消失，方法是检查〜（13）C-通过低场（B_0 = 3 T）〜（13）C {〜1H}交叉极化MAS NMR进行〜（1+）N偶极耦合，通过拆分〜（13）C共振确认了氨基甲酸酯。从〜163 ppm峰的双峰T_2衰减时间可以明显看出，第三种碳酸氢盐或第二种氨基甲酸盐，表明存在两个具有单共振的离子。产物的混合物表明（1）胺和水的存在导致存在碳酸氢盐和/或（2）HAS中多种类型的胺位点允许形成化学上不同的氨基甲酸酯。

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  • 来源
    《Environmental Science & Technology》 |2015年第22期|13684-13691|共8页
  • 作者

    Jeremy K. Moore; Miles A. Sakwa-Novak; Watcharop Chaikittisilp; Anil K. Mehta; Mark S. Conradi; Christopher W. Jones; Sophia E. Hayes;

  • 作者单位

    Department of Chemistry, Washington University, One Brookings Drive, Saint Louis, Missouri 63130, United States;

    School of Chemical & Biomolecular Engineering, Georgia Institute of Technology, 311 Ferst Drive, Atlanta, Georgia 30332, United States;

    School of Chemical & Biomolecular Engineering, Georgia Institute of Technology, 311 Ferst Drive, Atlanta, Georgia 30332, United States;

    Department of Chemistry, Emory University, 1515 Dickey Drive, Atlanta, Georgia 30322, United States;

    Department of Chemistry, Washington University, One Brookings Drive, Saint Louis, Missouri 63130, United States ,Department of Physics, Washington University, One Brookings Drive, Saint Louis, Missouri 63130, United States;

    School of Chemical & Biomolecular Engineering, Georgia Institute of Technology, 311 Ferst Drive, Atlanta, Georgia 30332, United States;

    Department of Chemistry, Washington University, One Brookings Drive, Saint Louis, Missouri 63130, United States;

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