Dtg 60 instrument

Scanning Electron Microscopy (SEM) micrographs have been obtained using a Cambridge 90 instrument, equipped with an energy dispersive X-ray microanalysis (EDX) facility. Fourier Transform IR (FTIR) analysis was performed by a PerkinElmer Spectrum 100 spectrometer, at room temperature, from 4000 to 650 cm⁻¹, with a resolution of 2.0 cm⁻¹. A universal Attenuated Total Reflectance (ATR) sampling accessory was used for the measurements, which were made directly on samples, without any preliminary treatment. ThermoGravimetric Analyses (TGA) have been carried out by a Shimadzu model DTG-60 instrument. TGA curves have been recorded at a heating rate of 10 °C min⁻¹, under static air atmosphere, from 35 to 700 °C. Analyzed sample mass varied between 8.0 and 11.0 mg.

Aldehydes, triazine, benzene-1,3-disulfonyl chloride, 2-aminopyridine, malononitrile, chlorosulfonic acid, and solvents were purchased from Sigma-Aldrich Company. Also, the thin-layer chromatography (TLC) of the commercial plates (silica gel 60 F254), were purchased from Merck Company. FT-IR spectra were recorded in a spectrophotometer (PerkinElmer 781). To investigate the surface morphology of the catalyst FE-SEM images and EDX analyses provided by a Sigma ZEISS, Oxford Instruments Field Emission Scanning Electron Microscope. The morphology of prepared catalysts was investigated using TEM by a Philips CM 120, Netherlands and microscope with an accelerating voltage of 150 kV. X-ray diffraction was performed using a Philips X'pert MPD diffractometer with a Cu operating at a current of 100 mA and a voltage of 45 kV, with the Cu-Kα radiation (λ = 0.154056 nm) at the 2q range of 10–80 and scanning at the speed of 0.05° per minute. Thermogravimetric analysis (TGA) was carried out using Shimadzu DTG-60 instrument at 25 to 600 °C. The pore volume and pore size distribution were resulted from the desorption profiles of the isotherms using the Barrett–Joyner–Halenda (BJH) method. NMR spectra (Bruker 400 MHz) were used to confirm product structure by DMSO-d6 as a solvent on a Bruker DRX-400 spectrometer.

The reagents and solvents used in this project were purchased from various chemical companies and were used directly without additional purification. The reactions were monitored by thin-layer chromatography (TLC) over gel-60 F₂₅₄ plates. Chromatography columns were packed using 63–200 mesh ASTM silica gel. Melting points were measured via an electrothermal 9100 apparatus. FT-IR spectroscopy was done using KBr disks in a AABFT-IR (FTLA 2000) spectrophotometer. ¹H NMR (300 and 600) and ¹³C NMR (75 MHz) spectra were recorded with a Bruker spectrometer. High-resolution mass spectra of the products were recorded with an Agilent quadrupole time-of-flight liquid chromatography/mass spectrometry system. XRD spectroscopy patterns of as-prepared samples were obtained by an XPert Pro Panalytical setup. The morphology and size of particles were recorded using a scanning electron microscope (Zeiss-SIGMA VP). TEM images were obtained by a Zeiss EM10C (100 kV) system. The specific surface area and pore size of the synthesized nano-catalyst were determined by N₂ sorption–desorption. The TGA curves of samples were obtained using a Shimadzu DTG-60 instrument. The copper content of the nanocatalyst was determined ICP-OES. The elemental analysis of the catalyst was achieved by EDX using a Zeiss SIGMA VP system.