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Synthesis of NiAl layered double hydroxides intercalated with aliphatic dibasic anions and their exchange with heptamolybdate
Abstract Layered double hydroxides (LDH) of general formula Ni1-x Alx(OH)2(A)x/2. mH2O were obtained by a co-precipitation method at constant pH, using succinate (C4H4O4 2−), adipate (C6H8O4 2−) and sebacate (C10H16O4 2−) as compensation anions and two x values, 0.3 and 0.5. The formation of NiAl LDH was evidenced, although in the Al-richer samples carbon analysis and solid-state 27Al NMR spectroscopy indicated the segregation of a small amount of an aluminum-containing phase. To prepare NiAlMo LDH, the original compensation anions were replaced by heptamolybdate ion using an anion exchange method. The results showed almost complete anion exchange in most samples, with small amounts of residual organic material, evidencing easy removal of the aliphatic dibasic anions as compared with terephthalate. The samples were characterized by FTIR, XRD, ICP-OES, CHN and Raman and 27Al MAS solid-state NMR spectroscopies.
Graphical abstract Display Omitted
Highlights NiAl-LDH are obtained using succinate, adipate and sebacate as compensation anions. There is no phase segregation in LDH with aluminum intralayer atom fraction = 0.3. NiAl-LDH with aluminum intralayer atom fraction >0.3 were obtained. Nearly complete exchange of aliphatic dibasic anions by heptamolybdate is achieved. Aliphatic dibasic anions are easier to replace by heptamolybdate than terephthalate.
Synthesis of NiAl layered double hydroxides intercalated with aliphatic dibasic anions and their exchange with heptamolybdate
Abstract Layered double hydroxides (LDH) of general formula Ni1-x Alx(OH)2(A)x/2. mH2O were obtained by a co-precipitation method at constant pH, using succinate (C4H4O4 2−), adipate (C6H8O4 2−) and sebacate (C10H16O4 2−) as compensation anions and two x values, 0.3 and 0.5. The formation of NiAl LDH was evidenced, although in the Al-richer samples carbon analysis and solid-state 27Al NMR spectroscopy indicated the segregation of a small amount of an aluminum-containing phase. To prepare NiAlMo LDH, the original compensation anions were replaced by heptamolybdate ion using an anion exchange method. The results showed almost complete anion exchange in most samples, with small amounts of residual organic material, evidencing easy removal of the aliphatic dibasic anions as compared with terephthalate. The samples were characterized by FTIR, XRD, ICP-OES, CHN and Raman and 27Al MAS solid-state NMR spectroscopies.
Graphical abstract Display Omitted
Highlights NiAl-LDH are obtained using succinate, adipate and sebacate as compensation anions. There is no phase segregation in LDH with aluminum intralayer atom fraction = 0.3. NiAl-LDH with aluminum intralayer atom fraction >0.3 were obtained. Nearly complete exchange of aliphatic dibasic anions by heptamolybdate is achieved. Aliphatic dibasic anions are easier to replace by heptamolybdate than terephthalate.
Synthesis of NiAl layered double hydroxides intercalated with aliphatic dibasic anions and their exchange with heptamolybdate
Aguilera, Luis Jacobo (author) / Palacio, Luz Amparo (author) / Faro Jr., Arnaldo C. (author)
Applied Clay Science ; 176 ; 29-37
2019-04-19
9 pages
Article (Journal)
Electronic Resource
English
NiAl LDH , Succinate , Adipate , Sebacate , Heptamolybdate , Anion exchange
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