A study of inorganic ion exchangers. XI. The hydrothermal reactions of ZrOCl2 and M(H2PO4)2 (M=Mg, Ca, Sr, Ba).
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概要
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The possibility of the hydrothermal synthesis of layered zirconium phosphates containing various alkaline earth metals (abbreviated as ZrMP; M=Mg, Ca, Sr, Ba) has been studied from ZrOCl<SUB>2</SUB> and M(HPO<SUB>4</SUB>)<SUB>2</SUB>, and their characteristics have been investigated. The optimum conditions for the synthesis of a highly crystalline product were as follows; the molar ratio of the starting materials of Ca(H<SUB>2</SUB>PO<SUB>4</SUB>)<SUB>2</SUB> and ZrOCl<SUB>2</SUB> was Ca/Zr=3, and the temperature of the hydrothermal reaction was in the range of 200–270 °C. By the hydrothermal reaction of ZrOCl<SUB>2</SUB> and Mg(H<SUB>2</SUB>PO<SUB>4</SUB>)<SUB>2</SUB>, a new compound of ZrMg<SUB>0.5</SUB>H(PO<SUB>4</SUB>)<SUB>2</SUB>·H<SUB>2</SUB>O with a layer-spacing of 11.94 Å was obtained. Layered phosphate (ZrMP) was not obtained by the hydrothermal reaction of ZrOCl<SUB>2</SUB> and Ba(H<SUB>2</SUB>PO<SUB>4</SUB>)<SUB>2</SUB>. The temperature range of the inter-layer dehydration of the layered phosphates (ZrMgP, ZrCaP, and ZrSrP) was similar to that of α-zirconium(IV) bis(hydrogenphosphate) (α-ZrP); i.e. the water in the interlayer was lost at 130–240 °C, and dehydro-condensation took place at a higher temperature above 340 °C. Zirconium phosphate containing Mg<SUP>2+</SUP> or Ba<SUP>2+</SUP> was not obtained by the ion exchange of the protons in α-ZrP with the alkaline earth metal cations (M<SUP>2+</SUP>) in MCl<SUB>2</SUB>, while Ca<SUP>2+</SUP> and Sr<SUP>2+</SUP> were exchanged with the protons. These alkaline earth metal ions except for Ba<SUP>2+</SUP> were easily exchanged with H<SUP>+</SUP> in α-ZrP, when NaOH was added. The layer-spacing of the Mg<SUP>2+</SUP>-exchanged zirconium phosphate was 9.6 Å, which was different from that of the hydrothermal product. The layer distances of Ca<SUP>2+</SUP>- or Sr<SUP>2+</SUP>-exchanged products were similar to those of the hydrothermal products.
- 公益社団法人 日本化学会の論文
著者
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Kobayashi Etsuro
National Chemical Laboratory for Industry
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Okabe Kiyomi
National Chemical Laboratory for Industry
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