| P—W系杂多阴离子柱水滑石的制备及表征 |
| STUDY ON PREPARATION AND CHARACTERIZATION OF HYDROTALCITES PILLARED WITH TRI-ATOMIC HETEROPOLY ANIONS OF P-W SYSTEM |
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| 摘要: 本文采用微波法,首次制备了第四周期系过渡金属取代三元杂多阴离子(PZW11)柱水滑石。经XRD、DTA、IR、UV-DRS和ESR表征,结果表明插入层间的柱高约为1.0nm,进入水滑石层间的杂多阴离子与其盐的IR振动类型和振动频率很相近,并且在水滑石层间PW12基因不能稳定存在,可能已部分发生降解,而PZW11则能稳定的存在于水滑石层间。UV结果表明,进入水滑石层间的杂多阴离子的桥氧与钨(Ob/Oc→W)的荷移跃迁变化不大,而由于水滑石层板的影响,过渡金属的d-d跃迁能级发生较大的紫移。ESR结果显示PCuW11进入水滑石层间后Cu2+更加趋向于5配位的立方锥场之中。DTA结果表明,杂多阴离子进入水滑石层间后其热稳定性有所提高,元素分析结果表明微波场中交换进行得彻底,杂多阴离子交换量在90%以上。 |
| 关键词: 水滑石 杂多阴离子 制备 表征 |
| 基金项目: |
| Abstract: The preparation of hydrotalcs pillared with triatomic heteropoly compound PZW11,whichZ represented the 4th period transition metal first by microwave method by the charactcrizationof XRD,DTA,IR, UV-DRS and ESR was reported. The state of hcteropoly compoundexisting in the layered region of heterotalcite was investigated. The heteropoly anion(pillarheight)was about 0.97-1.00nm from XRD results. The data of iR spcctra exhibit that the vibration frequency of heteropoly anion existing in the layered region of hydrotalc was similar tothat of parent heteropoly acid salt. The anion of PW12 may be dissociated into the anion ofPW11 form which was stable in the layered region. The UV-DRS results show that there wasless change of charge jump for the bond of bridge oxygen atom to tungstcr atom(Ob / Oc→W).meanwhile there was greater change of d-d electron jump which resulted in the violet shift.The ESR results indicated that the symmetry of heteropoly anion has some change after introducedinto the layered region of hydrotalcite and Cu2+ ion may be exist in a cubic cone field withPentadentate.The data of DTA show that thermal stability of pillared hydrotalc was 300℃ higher than that of the parent hydrotalc.The element analysis results exhibit that the anion exchange capacity of hydrotalc was above 90 percent in microwave field. |
| Keywords: hydrotalcite heteropoly anion preparation characterization |
| 投稿时间：1993-07-15 |
| 摘要点击次数: 1308 |
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| 贺鹤鸣,孙铁,蒋大振.P—W系杂多阴离子柱水滑石的制备及表征[J].无机化学学报,1994,10(3):272-277. |
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