Solvent-Mediated and Mechanochemical Methods for Anion Exchange of Carbonate from Layered Double Hydroxides Using Ammonium Salts.

Deintercalation of carbonate from layered double hydroxides (LDH) followed by intercalation of another anion (decarbonative intercalation) is a good method for the synthesis of crystalline LDH with different intercalated anions. We have carried out decarbonative intercalation of halides, nitrate, acetate, and sulfate by refluxing the carbonate-LDH with the corresponding ammonium salt in 1-butanol to obtain ordered LDH incorporating the desired anion. The crystallinity of the precursor LDH is retained in the anion-exchanged products, making this reaction a useful tool to prepare ordered LDH containing various anions. In addition, the morphology of the LDH is also retained after the exchange, making the reaction morphotactic. As the reaction is facilitated by the weak acidity of the ammonium salt, just grinding the carbonate-LDH with the ammonium salt of the desired anion also results in anion exchange. However, while the crystallinity of the LDH is retained, the morphology changes possibly due to breaking up of the crystals during the reaction.