Preparation and Characterization of Aminated Carbon from a Single-Step Reaction

Abstract

The paper describes a single-step procedure by which linear terminal diamines are directly anchored onto activated carbon in sizable amounts (∼5%). Evidence for the formation of real amide bonds is provided by using a range of spectroscopic and "in situ" electrochemical determinations (X-ray photoelectron spectroscopy, Brunauer-Emmett-Teller, Fourier transform infrared, Boehm titrations, and potentiometric acid-base titrations). Results on the reaction stoichiometry are also given, showing that diamines and surface carboxyls react in a close to 1:1 molar ratio. Terminal -NH 2 groups not engaged in amide bonds are free to react further and, in the present conditions, show well-defined proton adsorption behavior.

Hybrid Inorganic‐Organic Materials Carrying Tertiary Amine and Thiourea Residues Tethered on Mesoporous Silica Nanoparticles: Synthesis, Characterization, and Co‐Operative Catalysis

“…[11] Spectra were acquired on a Spectrum One FTIR Spectrophotometer Table 5. Relative concentrations of T n and Q n silicon groups (in %), surface coverage (SC, in %), molecular concentrations of organic functionalities (MC, in mmol g [3a ,7] (Perkin-Elmer) in the range 4000-450 cm À1 (transmittance mode).…”

“…This technique was used both to assess the presence of the functional groups on the surface of the nanoparticles and to determine their relative concentration. [11] Comparison of the FTIR spectra ( Figure 4) of bifunctional catalyst 1 and monofunctional material 7, both containing the thiourea residue, (Figure 1) allowed us to assign the signal at 1555 cm À1 to the C=S double bond stretching of this group, the signal at 1388 cm À1 to the Ar À N bond stretching, and the signal at 1282 cm À1 to the C À F bond stretching; together with other signals at 847, 700, and 682 cm À1 the latter signal was considered diagnostic of the meta substitution pattern on the aromatic ring. As expected, all of these signals were absent in the spectrum of the dimethylamino-functionalized material 6 ( Figure 1).…”

Surface chemical modifications induced on high surface area graphite and carbon nanofibers using different oxidation and functionalization treatments

“…For example, the immobilization of transition metal complexes on carbon has been carried out by using coupling agents to link the metal complexes to the carbon surface groups [12]. Also, the electrochemical or chemical reduction of aryldiazonium salts, with different groups at the para position, can form covalent CAC bonds with the carbon surface [13,14] A promising route and simple derivatization strategy to obtain N-modified carbons is the formation of surface amide bonds by means of molecules with two amine groups [15,16]. If one of these amine groups remains free, it could react further or make the anchoring of transition metal complexes onto carbon surface possible.…”

Low-temperature intermediates to oxygen reduction reaction catalysts based on amine-modified metal-loaded carbons. An XPS and ss-NMR investigation

“…A detailed picture was obtained on these products by a combination of high resolution XPS and solid state 15 N and 13 C NMR (ss-NMR). Also aided by similar results on an auxiliary model compound the direct NMR data are of special interest in that the amineecarbon bond is clearly established as iminic, in this also allowing a restatement of previous results [47] where this bond was considered amidic relying on less direct experimental evidence.…”