Synthesis of inorganic-organic layered compounds using immiscible liquid-liquid systems under the distribution law

Sara Inoue, Shinobu Fujihara

Research output: Contribution to journalArticle

17 Citations (Scopus)

Abstract

A method for synthesizing inorganic-organic layered compounds is proposed using a biphasic liquid-liquid system in one pot. Layered basic zinc benzoate (LBZB) compounds were chosen, and their formation was investigated starting from a xylene-water system. In a typical synthesis, a xylene phase dissolving benzoic acid was allowed to stand in contact with an equal amount of an aqueous phase dissolving zinc nitrate hexahydrate and urea. A role of urea is to supply OH- gradually by hydrolysis at an elevated temperature. The biphasically separated solutions were maintained at 80 °C, and then LBZB was obtained in the aqueous phase. Two kinds of layered structures with a basal spacing of 27.14 and 14.77 Å were formed by changing a C6H 5COOH/Zn molar ratio. Chemical compositions of the 27.14 and the 14.77 Å layered phases were estimated to be Zn(OH)1.74(C 6H5COO)0.260.29H2O and Zn(OH) 1.12(C6H5COO)0.880.21H2O, respectively. The 27.14 Å phase could also be deposited as a film on substrates by heterogeneous nucleation. The film consisted of standing platelike particles and exhibited a two-dimensional structure, which could be converted to ZnO by heating. The relationship between the initial solution compositions and the final solid products was systematically examined on the basis of distribution law for benzoic acid in the xylene-water system.

Original languageEnglish
Pages (from-to)15938-15944
Number of pages7
JournalLangmuir
Volume26
Issue number20
DOIs
Publication statusPublished - 2010 Oct 19

Fingerprint

Xylenes
xylene
Xylene
organic compounds
Benzoic Acid
Benzoic acid
Benzoates
benzoic acid
ureas
Urea
dissolving
Liquids
Zinc
synthesis
liquids
zinc
Zinc compounds
zinc compounds
Water
Chemical analysis

ASJC Scopus subject areas

  • Electrochemistry
  • Condensed Matter Physics
  • Surfaces and Interfaces
  • Materials Science(all)
  • Spectroscopy

Cite this

Synthesis of inorganic-organic layered compounds using immiscible liquid-liquid systems under the distribution law. / Inoue, Sara; Fujihara, Shinobu.

In: Langmuir, Vol. 26, No. 20, 19.10.2010, p. 15938-15944.

Research output: Contribution to journalArticle

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abstract = "A method for synthesizing inorganic-organic layered compounds is proposed using a biphasic liquid-liquid system in one pot. Layered basic zinc benzoate (LBZB) compounds were chosen, and their formation was investigated starting from a xylene-water system. In a typical synthesis, a xylene phase dissolving benzoic acid was allowed to stand in contact with an equal amount of an aqueous phase dissolving zinc nitrate hexahydrate and urea. A role of urea is to supply OH- gradually by hydrolysis at an elevated temperature. The biphasically separated solutions were maintained at 80 °C, and then LBZB was obtained in the aqueous phase. Two kinds of layered structures with a basal spacing of 27.14 and 14.77 {\AA} were formed by changing a C6H 5COOH/Zn molar ratio. Chemical compositions of the 27.14 and the 14.77 {\AA} layered phases were estimated to be Zn(OH)1.74(C 6H5COO)0.260.29H2O and Zn(OH) 1.12(C6H5COO)0.880.21H2O, respectively. The 27.14 {\AA} phase could also be deposited as a film on substrates by heterogeneous nucleation. The film consisted of standing platelike particles and exhibited a two-dimensional structure, which could be converted to ZnO by heating. The relationship between the initial solution compositions and the final solid products was systematically examined on the basis of distribution law for benzoic acid in the xylene-water system.",
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