Synthesis and Characterization of Heteropolytungstosilicate Complexes with the Lanthanide Elements

Lanthanide heteropoly compounds K15[Ln(HSiW9O34)2]·28H2O(Ln = La, Ce, Nd), denoted as Ln(SiW9)2, were synthesized and characterized by element analysis, TG-DTA, IR, UV, XPS and XRD. The results show that partial oxygen in Ln(SiW9)2 was coordinated with Ln3- , where Ln-3 was in the inner side of the heteropoly anions, while the fundamental structure of SiW9 had little change. The result was supported by ion exchange experiment.

Thermal Behaviour of Some New Polyoxometalate Complexes of Ciprofloxacin with Keggin-type Heteropoly Acids

Four polyoxometalate complexes, (CPFX·HCl)_3H_4SiW_~12 O_~40 , (CPFX·HCl)_3H_3PW_~12 O_~40 , (CPFX·HCl)_3H_3PMo_~12 O_~40 and (CPFX·HCl)_4H_4SiMo_~12 O_~40 , were prepared from ciprofloxacin hydrochloride(CPFX·HCl) reacting with H_nXM_~12 O_~40 ·nH_2O(X=P,Si; M=W,Mo) in an aqueous solution, and characterized by elemental analysis, IR spectrometry and TG-DTA. The IR spectrum confirms the presence of Keggin-type anions of heteropoly acids and the characteristic functional groups of ciprofloxacin. The TG/DTA curves show that their thermal decomposition is a multi-step process including simultaneous collapse of the Keggin-type structure. At first, these compounds had a mass loss of water molecules, then several other mass losses occured due to the decomposition of ciprofloxacin hydrochloride and its fragments with the degradation of Keggin anions. The end product of decomposition is the mixture of WO_3(or MoO_3) and SiO_2(or P_2O_5), identified by X-ray diffraction and IR spectroscopy. The possible thermal decomposition mechanisms of these complexes are proposed. This study exemplified that the thermal stability of the complexes containing tungsten is much better than that of the complexes containing molybdenum.

Synthesis and Characterization of Heteropoly Complexes of Indium with Metal-centred Undecatungstate Ligands

New indium heteropoly undecatungstometalate complexes of general formula K_n In( H_2O) MW_(11)O_(39) .xH_2O (M = Cr(Ⅲ) , Fe( Ⅲ ), Co(Ⅱ) or Zn( Ⅱ) ) were prepared by the stepwise acidification and the stepwise addition of materials. The products were characterized by elemental analysis, ion-exchange, IRspectra, UV spectra, X-ray powder diffraction and thermal analysis. The results show that the structure ofthe products derives from the Keggin structure. Their themial stability is higher than that of the homolo-gous dedecatungstometalates .

Synthesis and Properties of Heteropoly Complexes LnHSiW_(12)O_(40)·xH_2O

The present paper covers seven rare earth-containing tungstosilicate heteropoly complexes LnHSiW_(12)O_(40)·xH_2O with Keggin structure(Ln=La,Ce,Pr,Nd,Sm,Eu and Gd)snythesized by double decomposition reaction.The synthesized heteropoly complexes were characterized by ICP,^(29)Si-NMR,XPS, XRD,IR,UV,polarogram,CV and TG-DTA.The relationship between the structure of the synthesized heteropoly complexes and their properties is discussed.

Magnetic Properties of Heteropoly Complexes α-Na_(m)H_(n)[GaW_(9)M_(3)(H_(2)O)_(3)O_(37)]·16H_(2)O(M=Co(Ⅱ),Mn(Ⅱ),Cr(Ⅲ))

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A Study of Heteropoly Complexes of Rare Earths as Catalyst Promoter in the Synthesis of Ethyl Acetate

The capability of the synthesized heteropoly complexes of rare earths {K10 [(O39W11Si) Ln(Gly)3Ln(SiW11O39)]?H2O (Ln=La, Pr, Nd, Sm, Eu, Gd, Tb, Dy)} as the catalyst promoter in the synthesis of the ethyl acetate was studied. The results showed that the quantity of H2SO4 used for synthesizing the ethyl acetate can be reduced by 75% and the yield reached 98% at the optional condition.

Synthesis and Characterization 9-tungstosilicate Complexes with Transition Metal

The title complexes KaHb[M(SiW9O34)2]?mH2O(M=Ni,Cu,Zn,Fe or Mn) were synthesized by SiW9O34 10? with transition metal respectively and their structure were characterized by mean of elemental analysis, TG-DTA, IR spectra and, UV spectra. In addition, their redox properties in solution were investigated using polarographic and cyclic voltammographic methods. Experimental results indicated that the complexes have Keggin structure and that the heteropolyanions underwent two-step, two-electron tungsten reduction processes.

Study on Rare Earth Co-Permeation and Conductivity of Complex K_7[BNi(OH_2)W_(11)O_(39)]·11H_2O

The title compound was synthesized by means of direction. Its composition was determined by TG and ICP. The studies of IR and XRD indicate that the compound has the Keggin structure. The rare earth chemical thermal diffusion of the complex also was studied. The results show that the rare earth element Gd can permeate into the surface, interface and the body cavity of the prepared material. The results of TG-DTA show that the stable temperature is improved and the conductivity of the permeated sample is 3.05 S·cm -1, which is 4.67×106 times higher than that of the parent K_7[BNi(OH_2)W_ 11O_ 39]·11H_2O.

Syntheses, Characterizations and Catalytic Activities of Rare Earth Derivatives of Molybdotungstovanado-Phosphoric Heteropoly Acid

Seven new-type pentabasic heteropoly complexes with the general molecular formula K 10H 5[Ln(PMo 5W 4V 2O 39) 2]·nH 2O(Ln=La, Ce, Pr, Nd, Eu, Gd, Dy) were synthesized. The results of IR, UV, 31P, 51V NMR and X-ray powder diffraction pattern demonstrate that the product still maintains Keggin structure. The thermal stability studied by water solubility test, TG-DTA, XRD and IR at various temperature shows that the range of pyrolysis temperature is from 500～550 ℃. The catalytic action varies according to the contents of rare earths which are used to catalyze the decomposition of hydrogen peroxide.

取代型钨镓杂多配合物的导电性及其磁性

合成了过渡金属取代的钨镓杂多配合物α－Na7[GaW11Co（H2O）O39]·16H2O（简写为GaW11Co，其它类同）、α－Na7H2[GaW10Co2（H2O）2O39]·16H2O和α－NanHm[GaW9M3（H2O）3O37]·16H2O[M＝Co（Ⅱ），Ni（Ⅱ），V（Ⅴ）]，通过红外、紫外、ICP、TG－DTA、EPR、XPS、183WNMR、极谱等手段进行了表征．在室温下，α－GaW9Co3的电导率。值可达10－3S·cm－1，343K时可达10-2S·cm-1，表明是一类新型高质子导体．磁分析表明，GaW11Co、GaW9V3具有顺磁性，GaW9Ni3具有反铁磁性．

钼钨钒磷杂多酸稀土衍生物的合成、表征及催化性质

报道了通式为K1 0 H5[Ln(PMo5W4V2 O3 9) 2 ]·nH2 O (Ln =La ,Ce ,Pr ,Nd ,Eu ,Gd ,Dy)的 7种五元新型杂多配合物的合成方法。从IR ,UV ,3 1 P ,51 VNMR ,X射线粉末衍射证实产物仍保持Keggin结构 ,借助TG DTA、变温IR、XRD和水溶性实验考察了新配合物热解性质 ,得出了热稳定的温度范围为 5 0 0～ 5 5 0℃。该系列配合物对H2 O2 的分解具有一定的催化作用 ,且不同稀土配合物对H2 O2

Keggin结构稀土钼钒磷四元杂多配合物的合成、表征及苯酚羟化制苯二酚的催化活性

合成了 5种通式为 ( NH4) 1 5 [RE( PMo9V2 O39) 2 ]· x H2 O( RE=La3+ ,Ce3+ ,Gd3+ ,Y3+ ,Yb3+ )的稀土钼钒磷四元杂多配合物 ,并用 IR,UV,XRD,ICP,TG-DTA和 CV等手段对其结构和性能进行了表征 .催化活性实验表明 。

钼钨铌磷杂多化合物的研究(Ⅰ)——杂多酸的合成和表征

提出了分步酸化一分步加料合成[PNb_2Mo_xW_(10-x)O_(40)]^(5-)(x=0,2,4,6)系列杂多酸的方法,给出了最佳配料比和生成反应的pH值,并进行了红外、紫外、极谱、电位滴定及热稳定性研究。

镧系元素钨硼杂多酸盐的合成及性质研究

钨硼杂多配合是一类性能良好的催化剂，它还具有抗病毒作用，也可用于乳糖酶分离、纤维素光解剂及用于制造耐热油漆等，本文报道了K_(15)[Ln(BW_(11)O_(39))

钇磷钨三元杂多配合物的合成及其稀土多元渗与导电性的研究

合成了未见报道的标题配合物。通过化学分析、ICP和TG曲线确定了其化学式为K_8H_3[Y(PW_(11)O_(39))_2]·25H_2O;利用IR、UV、XRD、^(183)W-NMR、循环伏安等手段对其结构进行了表征,结果表明杂多阴离子为β_2型Keggin结构。采用稀土多元渗的方法对配合物进行了气相热扩渗,经ICP和XPS测试表明:微量的稀土元素La和Ce可以渗入到配合物的体相,并与组份元素存在键合作用。扩渗后化合物的化学式为K_8H_6YLa_(0.11)Ce_(0.18)P_2W_4~ⅤW_(18)~ⅥO_(78)·15H_2O,其晶体属单斜晶系,晶胞参数:a=6.3775nm,b=3.6771nm,c=3.7727nm,β=90.192°,V=88.47326nm^3;导电性的测试结果表明:室温时,扩渗后试样的电导率提高了约10~3倍,且热稳定范围变宽,523K时的电导率为1.33×10^(-2)S·cm^(-1),有望成为实用化的导电材料;~1H MAS NMR测试结果表明其存在三种质子,其导电机理可能是质子导电。

磷钼杂多酸-罗丹明S体系的共振散射光谱研究

在0.14mol·dm^(-3)H_2SO_4介质中,PO_4^(3-),MoO_4^(2-)与罗丹明S形成磷钼杂多酸-罗丹明S三元缔合物,在610nm处产生一灵敏的共振散射(即瑞利散射)光谱峰,磷浓度在0.2～20μg·dm^(-3)范围内与共振散射光强度呈良好线性关系.实验结果表明,本法具有灵敏度高、选择性好等特点,用于水和茶叶试样中磷酸根的测定,结果与示波极谱法的测定结果一致.

希土元素钼钨硅多元杂多配合物的合成、结构和性质研究

本文报道了标题系列配合物K_(10)H_3[Ln(SiMo_(11-n)W_nO_(39))_2]·mH_2O(n=2、4;Ln=La^(3+)、Ce^(3+)、Pr^(3+)、Nd^(3+)、Sm^(3+)、Eu^(3+)、Gd^(3+)、Dy^(3+)、Yb^(3+))的合成、热解性质、氧化还原性以及某些波谱特性。测定了K_(10)H_3[La(SiMo_9W_2O_(39)_2]·27H_2O的单晶结构:a=17.224(6)(?),b=26.952(11)(?),c=21.158(7)(?),β=103.76(3)°,Z=4,V=9540.17(6)(?)~3,F(000)=8663,此晶体属于单斜晶系,P2_1/n空间群。

镧系元素钨硅杂多配合物异构体的合成与表征

关于[Ln(XM_(11)O_(39))_2]^(n-)类配合物合成有一些报道,但它们均未指出其中配体及所得配合物的构型,本文以α-和β_2-SiW_(11)O_(39)^(8-)为配体,首次合成了双-(11-钨硅酸根)合镧系元素钾盐的异构体并进行了结构表征。 1 实验部分 1.1 仪器和试剂 pHS-2型酸度计;883型笔录式极谱仪,384B型极谱分析仪。

镝的钼硅杂多配合物的合成、结构和振动光谱

合成了镝的钼硅杂多配合物K_(10)H_3[Dy(SiMo_(11)O_(39))_2]·20H_2O,用X射线单晶结构分析,确定其空间群为P2_1/n,晶胞参数.结果表明:SiMo_(11)O_(39)^(8-)作为四齿配体与Dy配位,Dy与8个氧原子配位,形成四方反棱柱.K离子的配位数有6、7、8、和94种.讨论了该配合物的振动光谱.

K_(10)H_3[Ln(SiMo_(11-n)W_nO_(39))_2]·mH_2O(n=5,7,9)的合成、结构和性质研究

研究了K_(10)H_3[Ln(SiMo_(11-n)W_nO_(39)_2]·mH_2O(n=5,7,9;Ln=La^(3+),Ce^(3+),Pr^(3+),Nd^(3+),Sm^(3+),Eu^(3+),Gd^(3+),Dy^(3+),Yb^(3+))的合成方法。测定了K_(10)H_3[Pr(SiMo_6W_5O_(39))_2]·30H_2O的晶体结构,P2_1/n空间群,晶胞参数:a=1.7134(3)nm,b=2.6896(5)nm,c=2.1232(3)nm,β=103.60(3)°,Z=4.讨论了所合成配合物的IR光谱、电子光谱和X射线扮末衍射的特征。热分解性质研究结果表明,不同系列的配合物的分解温度范围:n=5,250～300℃;n=7,300～350℃;n=9,350～400℃。