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成功地合成了两种新的杂多酸的过氧化合物,过氧12─钼磷杂多酸具有如下组成比例:P:MO:O2-2=1:12:10,符合于分子式:H3[PMo12O30(O2)10]xH2O(I)。过氧12─钼硅杂多酸具有如下组成比例:Si:Mo:O2-2=1:12:8,符合于分子式H4[SiMo12O32(O2)8]·xH2O(Ⅱ)。 所采取的方法是在非水介质中合成,在用通常采用的方法制备的油状的12─杂多酸乙醚络合物中加进30%H2O2溶液,颜色由杂多酸的黄色,逐渐转变成橙色的过氧杂多酸。用纯的乙醚洗涤化合物,并用通常方法分析新化合物的组成。 我们研究了它们的若干性质和红外吸收光谱。化合物(I)Mo-O-Mo伸缩振动频率在500和780cm-1处。过氧链(-O-O-)=吸收谱带的频率在920cm-1处、相当于(AmH)H2[PO2(Mo2O7·4O)2·2Am][1]的595,720与880cm-1。化合物(Ⅱ)Mo-O-Mo伸缩振动频率在520和780cm-1处。过氧链(-O-O-)=吸收谱带的频率在1090cm-1处,则是首次发现的。
Two new heteropolyacid peroxo compounds were successfully synthesized. The peroxo-12-M heteropolyphosphate has the following composition ratio: P: MO: O2-2 = 1:12:10, which is in accordance with the formula: H3 [ PMo12O30 (O2) 10] xH2O (I). The peroxy 12-molybdosilicate heteropolyacid has the following compositional ratios: Si: Mo: O2-2 = 1: 12: 8, in accordance with the formula H4 [SiMo12O32 (O2) 8] xH2O (II). The method adopted is to synthesize in non-aqueous medium, add 30% H2O2 solution to the oily 12-heteropoly acid ether complex prepared by the commonly used method, the color is gradually changed from yellow of heteropoly acid to Orange peroxopolymer. The compound was washed with pure diethyl ether and the composition of the new compound was analyzed by the usual method. We studied some of their properties and infrared absorption spectra. Compound (I) Mo-O-Mo stretching vibration frequencies at 500 and 780cm-1. The peroxy chain (-O-O -) = absorption band at 920 cm-1 corresponds to 595, 720 and 880 cm-1 of (AmH) H2 [PO2 (Mo2O7.4O) 2A2m] [1] . The stretching vibration frequency of Mo-O-Mo of compound (Ⅱ) is 520 and 780 cm-1. It was the first time that the peroxy chain (-O-O -) = absorption band at 1090 cm-1.