A study of inorganic ion-exchangers. VIII. The synthesis of the crystalline Zr(RNH)xH2-x(PO4)2yH2O and their characteristics(R=(CnH2n+1)3 and C5H5, n=1-6).
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The synthesis of microcrystalline compounds with the formula of Zr(RNH)<I><SUB>x</SUB></I>H<SUB>2−<I>x</I></SUB>(PO<SUB>4</SUB>)<SUB>2</SUB>·<I>y</I>H<SUB>2</SUB>O (R=(C<I><SUB>n</SUB></I>H<SUB>2<I>n</I>+1</SUB>)<SUB>3</SUB>, C<SUB>5</SUB>H<SUB>5</SUB>, <I>n</I>=1–6, <I>x</I>=0.1–0.6, <I>y</I>=1–3) and their characteristics have been investigated. The compounds were formed by means of a hydrothermal reaction between RNH·H<SUB>2</SUB>PO<SUB>4</SUB> and ZrOCl<SUB>2</SUB> in the mole ratio of 4:1 at 130–180 °C. The layer-spacings of the trimethyl-, triethyl-, tripropyl-, tributyl-, tripentyl-, trihexylamine, and pyridine phosphates were 9.9, 13.0, 13.6, 17.0, 16.5, 18.4, and 10.9 Å respectively. In the thermal decomposition of each phosphate, the water of crystallization was eliminated at 105–130 °C. The organic base group in the alkylamine phosphates was burned in the presence of air at 330–360 °C, but this combustion was imperfect in the case of pyridine phosphate. The phosphates condensed at 400–450 °C. Zr(RNH)<I><SUB>x</SUB></I>H<SUB>2−<I>x</I></SUB>(PO<SUB>4</SUB>)<SUB>2</SUB>·<I>y</I>H<SUB>2</SUB>O was also obtained by means of an ion-exchange reaction between γ-Zr(HPO<SUB>4</SUB>)<SUB>2</SUB>·2H<SUB>2</SUB>O and the corresponding tertiary amine. In these products, the layer-spacings of the trimethyl-, triethyl-, tripropyl-, tributyl-, tripentyl-, and trihexylamine phosphates were 17.6, 16.4, 16.7, 21.0, 21.5, and 23.2 Å respectively, while those of pyridine and piperidine phosphates were 12.4 and 18.4 Å respectively. The layer-spacings of the products increased roughly with the size of the guest molecules. When Zr(RNH)<I><SUB>x</SUB></I>H<SUB>2−<I>x</I></SUB>(PO<SUB>4</SUB>)<SUB>2</SUB>·<I>y</I>H<SUB>2</SUB>O was treated with HCl, the products from the hydrothermal reaction changed to α-Zr(HPO<SUB>4</SUB>)<SUB>2</SUB>·H<SUB>2</SUB>O, while the products from the ion-exchange reaction returned to γ-Zr(HPO<SUB>4</SUB>)<SUB>2</SUB>·2H<SUB>2</SUB>O the raw material.
- 公益社団法人 日本化学会の論文
著者
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Shin Shigemitsu
National Chemical Laboratory for Industry
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Kobayashi Etsuro
National Chemical Laboratory for Industry
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