ZrO2负载12-磷钨酸催化螺[芴-9,9′-氧杂蒽]氧化溴化反应

doi:10.3724/SP.J.1095.2013.30095

摘要/Abstract

摘要： 研究了12-磷钨酸(TPA)负载量和活化温度对ZrO2固载TPA催化剂结构及催化螺[芴-9,9′-氧杂蒽](SFX)氧化溴化反应的影响。 X射线衍射和傅里叶变换红外光谱分析表明，增加TPA负载量和提高活化温度，使载体ZrO2结构的单斜相向四方相转变。 TPA质量分数为15%的催化剂样品经300 ℃活化后，具有稳定而良好的催化活性。 1H NMR表明，溴代产物中溴代位置在SFX的2位。

关键词: 磷钨酸, 二氧化锆, 氧化溴化, 螺[芴-氧杂蒽]

Abstract: A catalyst for the oxybromination of spiro[fluorene-9,9′-xanthene], 12-tungstophosphoric acid(TPA) supported on zirconia, was prepared. Effects of TPA loading and activation temperature on the structure of the catalyst and the catalytic performance for oxybromination of spiro[fluorine-9,9′-xanthene](SFX) have been investigated. The results of XRD and FTIR analysis show that the monoclinic zirconia transformed to tetragonal phase with the increase of TPA loading and calcinations temperature. A preliminary study on catalysts with 15%(mass fraction) TPA indicated that calcination at 300 ℃ could greatly enhance the stability of catalyst. The bromination position of the products was confirmed in the position of 2 of SFX from 1H NMR.

Key words: tungstophosphoric acid, zirconia, oxybromination, spiro[fluorene-xanthene]

中图分类号:

O643

任保轶, 赵阳, 李响, 冉凡鹏, 金晓丹. ZrO₂负载12-磷钨酸催化螺[芴-9,9′-氧杂蒽]氧化溴化反应[J]. 应用化学, DOI: 10.3724/SP.J.1095.2013.30095.

REN Baoyi*, ZHAO Yang, LI Xiang, RAN Fanpeng, JIN Xiaodan. Oxybromination of Spiro[fluorene-9,9′-xanthene] over 12-Tungstophosphoric Acid Supported on Zirconia[J]. Chinese Journal of Applied Chemistry, DOI: 10.3724/SP.J.1095.2013.30095.

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ZrO₂负载12-磷钨酸催化螺[芴-9,9′-氧杂蒽]氧化溴化反应

Oxybromination of Spiro[fluorene-9,9′-xanthene] over 12-Tungstophosphoric Acid Supported on Zirconia

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