Diethylenetriamine vanadium (Ⅲ)-tungsten (vi)-vanadium (iv)-oxygen cluster compound and its synthesis method
A technology of diethylenetriamine vanadium and diethylenetriamine, which is applied in the field of diethylenetriamine vanadium-tungsten-vanadium-oxygen clusters and their synthesis, can solve problems such as unstable structures and limited applications, and achieve synthetic methods Simple, high-yield, high-reliability results
Active Publication Date: 2019-10-22
欧阳明亮
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[0003] However, despite their excellent catalytic performance, polyoxometallates are inherently unstable due to the high electronegative nature of polyanions, the basic inorganic structural unit, and their large water solubility, Limit its application in some specific fields (such as liquid phase catalysis)
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Embodiment 1
[0029]First, synthesis of diethylenetriamine vanadium (III) complex: all operations were carried out in a glove box under an inert atmosphere. Under constant stirring, 20.0 mL of distilled water, 1.200 g of partial After the ammonium vanadate and 1.8mL phosphorous acid are completely mixed, 2.5mL diethylenetriamine is slowly added dropwise. After the addition of diethylenetriamine is completed, the resulting mixture is heated to 70°C and stirred for 2 hours to obtain a mixed solution A; add 20.0mL distilled water, 6.515g sodium tungstate and 0.5mL phosphorous acid to a 50mL Erlenmeyer flask in turn and stir to obtain a mixed solution B; quickly take out the mixed solution A from the glove box and press the mixed solution B Stir and mix at a volume ratio of 1:2, then quickly pipette 20mL of the mixed solution into a 25mL polytetrafluoroethylene stainless steel reactor, place the sealed reactor in an oven at 160°C for 7 days, and cool naturally Cool down to room temperature, ope...
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The invention provides a DETA (diethylenetriamine) vanadium (III)-tungsten (VI)-vanadium (IV)-oxygen cluster and a synthetic method thereof. The molecular formula of the DETA vanadium (III)-tungsten (VI)-vanadium (IV)-oxygen cluster is as follows: (H3DETA)3(DETA)(NA(VIII(DETA)2(WVI8VIV4O36(PO4)))2).2H2O, wherein DETA is diethylenetriamine, the crystal of the cluster belongs to the monoclinic system, the space group is C2 / c, and the cell parameters are as follows: a=21.8135, b=13.0499, c=37.5978 and V=10,666.3. Synthesis can be realized with a stepwise self-assembly method, phosphorous acid, ammonium metavanadate and DETA are mixed in distilled water in an inert atmosphere, the mixture is heated and stirred, and a mixed solution A is obtained; sodium tungstate and phosphorous acid are mixed in the distilled water and stirred, and a mixed solution B is obtained; the mixed solution A and the mixed solution B are mixed and then transferred to a reaction kettle, the mixture reacts under a hydrothermal condition and then is cooled filtered and washed, and the DETA vanadium (III)-tungsten (VI)-vanadium (IV)-oxygen cluster is obtained.
Description
technical field [0001] The invention belongs to the field of metal-oxygen clusters, in particular to diethylenetriamine vanadium (III)-tungsten (VI)-vanadium (IV)-oxygen clusters and a synthesis method thereof. Background technique [0002] Polyoxometalates, as functional materials with great development value, not only have a wide range of applications in the fields of light, electricity, magnetism, biology, medicine, etc., but also their natural and excellent catalytic properties are attracting the attention of researchers. The cage-like structural characteristics and high negative charge, strong acid, strong oxidation and pseudo-liquid properties of polyoxometalates are the reasons for their particularly excellent catalytic performance. As a class of environment-friendly catalysts, oxometalates also have the advantages of good thermal stability, high conversion rate, good selectivity, non-corrosion equipment and reproducibility, and have been widely used in homogeneous an...
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IPC IPC(8): C07F19/00
Inventor 陈武华胡志彪张著森丘则海黄田富袁秋兰
Owner 欧阳明亮