A series of microporous carbons (chars) containing various amounts of magnetic Ni nanoparticles were prepared using a simple procedure. The resorcinol–formaldehyde polymers containing nickel(II) acetate was carbonized to produce chars (labelled as Ni/C-20, Ni/C-35 and Ni/C-50). All chars were characterized by X-ray diffraction, Raman spectroscopy, nitrogen adsorption and scanning electron microscopy methods. The formation of Ni crystallites (18 nm in size) occurs in carbon spheres measuring 1–2 μm in diameter. The Raman spectra show that the content of Ni influences the carbon structure. Dye-separation performance by Ni/C was investigated using methylene blue. The adsorption capacity was 26.6, 20.8 and 15.1 mg/g for Ni/C-20, Ni/C-35 and Ni/C-50, respectively.
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