Nitrogen‐Functionalized Hydrothermal Carbon Materials by Using Urotropine as the Nitrogen Precursor

Nitrogen‐containing hydrothermal carbon (N‐HTC) materials of spherical particle morphology were prepared by means of hydrothermal synthesis with glucose and urotropine as precursors. The molar ratio of glucose to urotropine has been varied to achieve a continuous increase in nitrogen content. By raising the ratio of urotropine to glucose, a maximal nitrogen fraction of about 19 wt % could be obtained. Decomposition products of both glucose and urotropine react with each other; this opens up a variety of possible reaction pathways. The pH has a pronounced effect on the reaction pathway of the corresponding reaction steps. For the first time, a comprehensive analytical investigation, comprising a multitude of analytical tools and instruments, of a series of nitrogen‐containing HTC materials was applied. Functional groups and structural motifs identified were analyzed by means of FTIR spectroscopy, thermogravimetric MS, and solid‐state NMR spectroscopy. Information on reaction mechanisms and structural details were obtained by electronic structure calculations that were compared with vibrational spectra of polyfuran or polypyrrole‐like groups, which represent structural motifs occurring in the present samples.