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Dawson type phosphotungstic heteropolyacid salt constructed by mixed-valence tetracarboxylic acid binuclear ruthenium and synthesis method for Dawson type phosphotungstic heteropolyacid salt

A technology of phosphotungstic heteropolyacid salt and synthesis method, which is applied in the field of Dawson type phosphotungstic heteropolyacid salt and its synthesis, and can solve the problem that polyoxometalate has not been reported in literature and the like

Active Publication Date: 2020-03-31
XI'AN PETROLEUM UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, there are no reports in the literature on the formation of polyoxometalates containing dinuclear ruthenium tetracarboxylic acids and Dawson-type heteropolyacids.

Method used

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  • Dawson type phosphotungstic heteropolyacid salt constructed by mixed-valence tetracarboxylic acid binuclear ruthenium and synthesis method for Dawson type phosphotungstic heteropolyacid salt
  • Dawson type phosphotungstic heteropolyacid salt constructed by mixed-valence tetracarboxylic acid binuclear ruthenium and synthesis method for Dawson type phosphotungstic heteropolyacid salt
  • Dawson type phosphotungstic heteropolyacid salt constructed by mixed-valence tetracarboxylic acid binuclear ruthenium and synthesis method for Dawson type phosphotungstic heteropolyacid salt

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Embodiment 1

[0018] Dawson-type phosphotungstic heteropolyacid salt constructed by dinuclear ruthenium of mixed valent tetracarboxylic acid, molecular formula K 2 [Ru 2 (CH 3 COO) 4 (H 2 O) 2 ] 2 [H 2 P 2 W 18 o 62 ]·22H 2 O, molecular weight 5788.23, belongs to monoclinic crystal system, space group P2(1) / c, unit cell parameters β=106.20(2)°, D. c =3.81g cm -3 , the number of molecules in the unit cell Z = 4, the weight factor is 0.972, and the consistency factor of the diffraction points is final R 1 =0.0858, the consistency factor wR of the diffraction spots 2 = 0.1743.

[0019] The synthetic method of the Dawson type phosphotungstic heteropolyacid salt constructed by mixed valent tetracarboxylic acid dinuclear ruthenium, the steps are as follows:

[0020] (1) Weighing Na with a weight of 50g 2 WO 4 2H 2 O was dissolved in 175mL of distilled water, heated to boiling, and then 75mL of H with a mass concentration of 85% was added 3 PO 4 , the solution turned yellow-...

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Abstract

The invention discloses Dawson type phosphotungstic heteropolyacid salt constructed by mixed-valence tetracarboxylic acid binuclear ruthenium and a synthesis method for the Dawson type phosphotungsticheteropolyacid salt. The Dawson type phosphotungstic heteropolyacid salt has a chemical formula of K2[Ru2(CH3COO)4(H2O)2]2[H2P2W18O62].22H2O and a molecular weight of 5788.23, and belongs to a monoclinic system; and the space group of the phosphotungstic heteropolyacid salt is P2(1) / c. The cell parameters of the phosphotungstic heteropolyacid salt are that a is equal to 25.18(3)angstrom; b is equal to 18.25(2)angstrom; c is equal to 22.16(3)angstrom; beta is equal to 106.20(2)angstrom; V is equal to 9782.4(19)angstrom<3>; D<c> is equal to 3.81 g cm<-3>; and Z is equal to 4. The preparation method comprises the following steps: (1) weighing Na2WO4.2H2O, dissolving the Na2WO4.2H2O into distilled water, carrying out heating to boil, adding H3PO4, carrying out boiling reflux, carrying out cooling to a room temperature, adding a KCl solid so as to obtain alpha-K6[P2W18O62].16H2O, and dissolving the alpha-K6[P2W18O62].16H2O into distilled water so as to obtain a solution I; and dissolving [Ru2(CH3COO)4Cl] into distilled water so as to prepare a solution II, dropwise adding the solution II into the solution I, and carrying out a reaction so as to obtain a final product. The Dawson type phosphotungstic heteropolyacid salt provided by the invention is synthesized by adopting a conventional aqueous solution method; the reaction temperature is controlled to be 60 DEG C; the pH value is controlled to be 3.0-3.5; and the compound prepared by using the preparation method provided by the invention is clear in composition and structure and has potential application value in the aspect ofcatalytic materials.

Description

technical field [0001] The invention belongs to the technical field of inorganic polyoxometalate chemistry, and in particular relates to a Dawson type phosphotungstic heteropolyacid salt constructed by mixed valent tetracarboxylic acid dinuclear ruthenium and a synthesis method thereof. Background technique [0002] The noble metal ruthenium is a transition element located in the d-block of the periodic table, and it is easy to lose 2, 3 or 4 electrons in the outermost layer to form Ru 2+ 、Ru 3+ and Ru 4+ . Due to the rich valence changes of metal ruthenium, it has rich physical and chemical properties. Ruthenium has a strong coordination ability, and it is easy to coordinate with C, N, O, P, etc. to form a coordination compound. In the complex, metal ruthenium often exists in a single valence state of +2 or +3, and often in + Mixed valence states of 2 and +3 exist. Common metal ruthenium complexes used as precursors are Ru 2 (O 2 CCH 3 ) 4 Cl, Ru(bpy) 3 Cl 2 , ci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/10C07C51/41C07C51/43B01J31/22B01J27/188
CPCC07C53/10B01J31/2239B01J27/188B01J2531/821C07B2200/13
Inventor 刘雪梅孟祖超孙妩娟李慧敏韦海龙
Owner XI'AN PETROLEUM UNIVERSITY