Layered double hydroxides (LDHs) with the compositions (Cs+/NH4+)0.111[M2+0.667Al0.333(OH)2.0 (SO4)0.222] (M2+ = Mn, Zn) and basal distance of ca. 11 Å were obtained by co-precipitating Mn/Al and Zn/Al sulfate salts with aqueous NH3, using excess of Cs2SO4. [Mn0.667Al3+0.333(OH)2]Cl0.333.nH2O and [M2+0.667Al3+0.333(OH)2](NO3)0.333.nH2O (M2+ = Mn, Zn) were also synthesized by co-precipitation, presenting respective basal distances of 8.92 and 7.92 Å. After applying exchange reactions with excess of Cs2SO4, materials with basal distances of ca. 11 Å were obtained, indicating the exchange of chloride and nitrate with sulfate, without incorporation of Cs+. When Na+0.111[M2+0.667Al0.333(OH)2.0(SO4)0.222](M2+ = Mn, Zn) obtained by co-precipitation and having basal distances of ca. 11 Å was exchanged with excess of Cs2SO4, the content of sulfate remained constant and Na+ was partially replaced with Cs+, but the amount was lower, indicating the probable composition (Na+/Cs+)y[M2+0.667Al0.333(OH)2-y(SO4)y/2(SO4)0.222-(y/2)](M2+ = Mn, Zn), where some of the hydroxide anions were replaced with grafted SO42-.

Layered double hydroxides (LDHs) of Cu:Al in the molar ratio of 2:1, intercalated with sulfate, sulfate/(Li+, Na+, K+ or NH4+), NO3- and CO32-, were synthesized by co-precipitation with increasing pH. The materials were submitted to exchange reactions using B2SO4 (B = Li+, Na+, K+, NH4+) solutions in an attempt to replace previously intercalated cations or incorporated cations without removing intercalated sulfate. X-ray diffraction (XRD) patterns and Fourier transform infrared (FTIR) spectra were consistent with the expected intercalated species and scanning electron microscopy (SEM) images indicated submicrometric platelet-like particles, typical of LDHs. The chemical compositions of all phases were confirmed by inductively coupled plasma optical emission spectrometry (ICP OES) and thermogravimetric analyses (TGA). In the exchange reactions, only in [Cu6Al3(OH)18][Na(H2O)6(SO4)2]·6H2O the sodium cations were almost totally replaced with lithium, potassium and ammonium, without removing the intercalated sulfate.