New Synthetic Routes to Hydrotalcite-Like Compounds − Characterisation and Properties of the Obtained Materials

Hydrotalcite-like anionic clays of general formula [M(II)1–xM(III)x(OH)2]x+[CO32–x/2]x– · m H2O with M(III) = Al and M(II) = Mg, Ni, Zn have been prepared by precipitation of the hydroxycarbonates from the “homogeneous” solution after the thermally induced hydrolysis of urea. The effect of the temperature of precipitation, of the total metal cations concentration, of the molar fraction M(III)/M(III) + M(II) and of the molar fraction urea/M(II) + M(III) in solution on the composition and on the crystallinity degree of the samples has been investigated. The optimum conditions are reported to obtain micro-crystalline powders with a narrow distribution of particle size in a short time with a simple procedure. The compounds obtained have been characterised for chemical composition, thermal behaviour, particle-size distribution and BET-surface area. In addition, the crystal structure of Mg0.67Al0.33(OH)2 (CO3)0.165 · 0.4 H2O has been refined by X-ray diffraction powder methods. The carbonate form has been converted into the chloride form by letting gaseous HCl flow over the hydrotalcite-like compounds, heated at 150 °C. The exchange of Cl– anions with some alkoxide anions in the presence of the respective alkanols has been investigated. The exchange reaction was driven by the segregation of NaCl crystals poorly soluble in alkanols and led to the co-intercalation of the alkoxide ions together with the alkanol with the formation of a bi-layer of extended alkyl chain in the interlayer region of the Mg-Al hydrotalcite. The intercalation compound, washed with water, produces a hydrotalcite with Cl– and OH– as balancing anions.