Value-added long-chain aliphatic compounds obtained through pyrolysis of phosphorylated chitin.

In this work, chitin, as a biobased polymer, is used as a precursor to obtain a phosphorylated derivatives. The influence of the different degree of phosphorylation in chitin on pyrolysis pattern was investigated. In order to understand the pyrolysis mechanism and the potential application of phosphorylated chitins, the samples were pyrolyzed at different temperatures and analyzed by FTIR, SEM, and Py-GC/MS analysis. Moreover, the thermal degradation and the evolved gases during chitin degradation and its derivatives were measured. The results showed that phosphorylation of chitin decreased the thermal stability of biopolymer and significantly changed the pattern of pyrolysis compared to neat chitin. The production of long-chain hydrocarbons was detected during pyrolysis of phosphorylated chitin, whereas this was not the case with raw chitin. Those two effects were more pronounced as the degree of phosphorylation increased. Chitin with the degree of phosphorylation (DS 1.35) exhibited the highest selectivity (91 %) towards production of long-chain hydrocarbons (C12-C17) at 500 °C. Moreover, the obtained results allowed to propose, for the first time, the mechanism of pyrolysis of phosphorylated chitin.

Experimental protocol for the study of One-pot amination of Cyclohexanone-to-secondary amines over Carbon-supported Pd.

The validation of protocols for carrying out the experimental analysis of amination reactions is of paramount importance to enhance the scientific knowledge and reproducibility of results. Accordingly, in the present paper, a protocol has been proposed for the study of the amination of cyclohexanone-to-secondary amines (Diphenylamine and N-Cyclohexylaniline) over heterogeneous catalysts. The results of activity and selectivity, and the elucidation of a plausible reaction pathway were described in a parent paper. Therefore, the purpose of this document is to inform about the details of the experimental setups, the methods, and the analytical techniques to identify and quantify the reaction products. Finally, some practical and safety considerations are also included.•One-pot catalytic amination of cyclohexanone with aniline was performed efficiently in liquid phase on Pd/C.•Stirring, He atmosphere and temperature control were critical to achieve reproducible activity results.•Ultra-High Performance Liquid Chromatography allows identifying products and reaction intermediates, while nonane performed well as internal standard for GC-FID quantification.

The reduction of Fe-bearing copper slag for its use as a catalyst in carbon oxide hydrogenation to methane. A contribution to sustainable catalysis.

Reduction of Fe-phases in a slag from the copper smelting process is studied for its use as a catalyst in methanation of carbon oxide (CO). This material contains 36.4 wt% Fe and the main Fe-phases in its fresh and reduced forms were identified and quantified. Chemical analysis and X-ray diffraction (XRD) for crystalline phase detection and determination of Fe dispersion were carried out. Reducibility of Fe-oxides was studied by thermal programmed reduction (TPR) under H2 at 650 and 800 °C using 0.5 and 2 h soak time. In the fresh slag, iron was found to be in the form of Fe3O4 (17.4 wt%) and fayalite, Fe2SiO4 (43.4 wt%). The composition was experimentally determined and verified by stoichiometric balances and thermogravimetric analysis (TGA). Upon reduction at 800 °C and 2 h soak time, 87 % of the Fe-phases were reduced, leaving an activated catalyst with a 35.2 % Fe0, which is the active phase for CO hydrogenation to methane. An expression was derived to determine the Fe0 concentration in the reduced slag based on the composition of the fresh slag and its reduction degree. The catalytic activity of the reduced slag during CO hydrogenation was evaluated in a fixed bed differential reactor. The selectivity to methane, at 300 °C, was 87 %, thus confirming its catalytic activity for the selected reaction.