V2O5-ZrO2 및 황산으로 개질된 V2O5-ZrO2의 특성

손종락; 배영일; 조성국

HWAHAK KONGHAK, Vol.31, No.6, 838-845, December, 1993

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V₂O₅-ZrO₂ 및 황산으로 개질된 V₂O₅-ZrO₂의 특성

Characterization of V₂O₅-ZrO₂ and V₂O₅-ZrO₂ Modified with H₂SO₄

손종락, 배영일, 조성국

초록

Zr(OH)₄ 분말을 NH₄VO₃ 수용액에 함침시킨 후 공기중에 소성하여 V₂O₅-ZrO₂ 촉매를 제조하였으며 또한 NH₄-VO₃로 함침된 Zr(OH)₄ 분말을 황산으로 개질한 후 소성하여 V₂O₅-ZrO₂/SO₄^2- 촉매를 제조하였다. 제조된 촉매의 특성을 FTIR, DSC-TGA, XRD 및 표면적 측정에 의하여 연구하였다. ZrO₂에 V₂O₅를 첨가하거나 황산으로 개질하면 상호작용으로 말미암아 ZrO₂의 무정형에서 tetragonal phase 및 tetragonal phase에서 monoclinic phase로 되는 상전이 온도가 높은 온도쪽으로 이동되었다. 그리고 V₂O₅ 함량이 10mol%까지는 V₂O₅가 ZrO₂ 표면에 잘 분산되어 900℃의 소성온도에서도 V₂O₅의 결정이 XRD pattern상에 나타나지 아니하였으나 V₂O₅ 함량이 15mol%에서는 700℃의 소성온도부터 V₂O₅ 결정이 나타났다.

V₂O₅-ZrO₂ catalysts were prepared by dry impregnation of powdered Zr(OH)₄ with an aqueous solution of NH₄VO₃ followed by calcining in air, and V₂O₅-ZrO₂/SO₄^2- catalysts were prepared by modifiying impregnated Zr(OH)₄ with H₂SO₄ followed by calcining in air. The characterization of prepared catalysts was performed by using FTIR, DSC-TGA, and XRD, and by the measurement of surface area. The addition of V₂O₅ to ZrO₂ and modification with H₂SO₄ shifted the phase transition of ZrO₂ from amorphous to tetragonal and from tetragonal to monoclinic to higher temperatures due to the interaction between ZrO₂ and V₂O₅(or H₂SO₄). Since V₂O₅ was dispersed on the surface of ZrO₂ up to 10mol% of V₂O₅, any crystal phase of V₂O₅ even at the calcination temperature of 900℃ was not observed on the XRD patterns. However, in the case of sample containning 15mol% of V₂O₅, V₂O₅ crystal phase appeared on XRD pattern from the calcination temperature of 700℃.

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[39] Parry EP, J. Catal., 2, 371 (1963)