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Synthesis Strategies Towards Amorphous Porous Carbons with Selective Oxygen Functionalization for the Application as Reference Material
Carbon ( IF 10.5 ) Pub Date : 2021-01-01 , DOI: 10.1016/j.carbon.2020.09.030
Felix Herold , Oliver Leubner , Philipp Pfeifer , Dina Zakgeym , Alfons Drochner , Wei Qi , Bastian J.M. Etzold

Abstract Manipulation of carbon surface functionalization and especially of oxygen surface groups has been demonstrated to be key for obtaining high performance materials in a multitude of applications. Although control of carbon surface chemistry offers large potential in many technical relevant applications, qualitative and quantitative analysis of surface oxides for amorphous and porous carbons remains challenging. In this study, we attempt selective, organic chemistry-based functionalization of a polymer-derived porous model carbon featuring high oxygen loadings, with the aim to establish analytical standards for temperature programmed desorption (TPD) and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). In this context, quantitative chemical reduction of an oxidized carbon material with lithium aluminum hydride (LiAlH4) is utilized as the key for the synthesis of carbon materials with defined ensembles of oxygen surface groups (hydroxyl groups and ethers). Based on this reduction strategy, selective LiAlH4 reduction based on protection group chemistry leads to aldehydes, ketones and quinones as surface functional groups and chemical grafting is studied for the selective introduction of phenyl esters, methyl ethers and carboxylic acids. All materials are evaluated with respect to the applicability as analytical standard by DRIFT spectroscopy, TPD, X-ray photoelectron spectroscopy and titration methods.

中文翻译:

具有选择性氧功能化的无定形多孔碳作为参考材料的合成策略

摘要 碳表面官能化,尤其是氧表面基团的操纵已被证明是在众多应用中获得高性能材料的关键。尽管碳表面化学的控制在许多技术相关应用中提供了巨大的潜力,但对无定形和多孔碳的表面氧化物进行定性和定量分析仍然具有挑战性。在这项研究中,我们尝试对具有高氧负载量的聚合物衍生多孔模型碳进行选择性的、基于有机化学的功能化,目的是建立程序升温脱附 (TPD) 和漫反射红外傅立叶变换光谱 (DRIFTS) 的分析标准. 在这种情况下,使用氢化铝锂 (LiAlH4) 对氧化的碳材料进行定量化学还原被用作合成具有定义的氧表面基团(羟基和醚)集合的碳材料的关键。基于这种还原策略,基于保护基化学的选择性 LiAlH4 还原导致醛、酮和醌作为表面官能团,并研究了化学接枝以选择性引入苯酯、甲基醚和羧酸。通过 DRIFT 光谱、TPD、X 射线光电子能谱和滴定方法,就作为分析标准的适用性对所有材料进行了评估。基于这种还原策略,基于保护基化学的选择性 LiAlH4 还原导致醛、酮和醌作为表面官能团,并研究了化学接枝以选择性引入苯酯、甲基醚和羧酸。通过 DRIFT 光谱、TPD、X 射线光电子能谱和滴定方法,就作为分析标准的适用性对所有材料进行了评估。基于这种还原策略,基于保护基化学的选择性 LiAlH4 还原导致醛、酮和醌作为表面官能团,并研究了化学接枝以选择性引入苯酯、甲基醚和羧酸。通过 DRIFT 光谱、TPD、X 射线光电子能谱和滴定方法,就作为分析标准的适用性对所有材料进行了评估。
更新日期:2021-01-01
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