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Antimony-vanadium-oxygen cluster compound based on micromolecular nitrogen-containing ligand and synthesis method of antimony-vanadium-oxygen cluster compound

A technology of antimony vanadium oxyclusters and synthesis methods, which is applied in the fields of preparation of amino compounds, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., and can solve the problems of decomposition, generation structure, and restriction of heterogeneous catalysts application and other issues, to achieve the effect of novel structure and simple synthesis method

Inactive Publication Date: 2021-06-29
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the biggest disadvantage of this type of compound is that its structure will decompose in the air close to 300 °C, thus limiting its application as a heterogeneous catalyst.

Method used

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  • Antimony-vanadium-oxygen cluster compound based on micromolecular nitrogen-containing ligand and synthesis method of antimony-vanadium-oxygen cluster compound
  • Antimony-vanadium-oxygen cluster compound based on micromolecular nitrogen-containing ligand and synthesis method of antimony-vanadium-oxygen cluster compound
  • Antimony-vanadium-oxygen cluster compound based on micromolecular nitrogen-containing ligand and synthesis method of antimony-vanadium-oxygen cluster compound

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Embodiment 1

[0036] A kind of antimony vanadyl cluster compound based on small molecule nitrogen-containing ligand, its molecular formula is: [Cd(en) 3 ] 3 [Sb 6 V 15 o 42 (H 2 O)] 8H 2 O; wherein, en is ethylenediamine.

[0037] Above-mentioned a kind of synthesis method based on the antimony vanadyl cluster compound of small molecule nitrogen-containing ligand, specifically comprises the following steps:

[0038] Take reactant Sb 2 o 3 0.6g, NH 4 VO 3 0.6g, Cd(NO 3 ) 2 4H 2Add 0.3g of O and 2mL of en into 2ml of water in turn, stir, put into the reaction kettle, set the oven temperature at 170°C, and continue the reaction for 5 days. After the reaction is finished, black massive crystals are crystallized out, which is the above-mentioned antimony vanadium oxy-cluster compound.

Embodiment 2

[0040] A kind of antimony vanadyl cluster compound based on small molecule nitrogen-containing ligand, its molecular formula is: [Cd(en) 3 ] 3 [Sb 6 V 15 o 42 (H 2 O)] 8H 2 O; wherein, en is ethylenediamine.

[0041] Above-mentioned a kind of synthesis method based on the antimony vanadyl cluster compound of small molecule nitrogen-containing ligand, specifically comprises the following steps:

[0042] Take reactant Sb 2 o 3 0.6g, NH 4 VO 3 0.6g, Cd(NO 3 ) 2 4H 2 Add 0.3g of O and 2mL of en into 2ml of water in turn, stir, put into the reaction kettle, set the oven temperature to 160°C, and continue the reaction for 130h. After the reaction is finished, black massive crystals are crystallized out, which is the above-mentioned antimony vanadium oxy-cluster compound.

Embodiment 3

[0044] A kind of antimony vanadyl cluster compound based on small molecule nitrogen-containing ligand, its molecular formula is: [Cd(en) 3 ] 3 [Sb 6 V 15 o 42 (H 2 O)] 8H 2 O; wherein, en is ethylenediamine.

[0045] Above-mentioned a kind of synthesis method based on the antimony vanadyl cluster compound of small molecule nitrogen-containing ligand, specifically comprises the following steps:

[0046] Take reactant Sb 2 o 3 0.6g, NH 4 VO 3 0.6g, Cd(NO 3 ) 2 4H 2 Add 0.3g of O and 2mL of en into 2ml of water in turn, stir, put into the reaction kettle, set the oven temperature to 180°C, and continue the reaction for 110h. After the reaction is finished, black massive crystals are crystallized out, which is the above-mentioned antimony vanadium oxy-cluster compound.

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Abstract

The invention discloses an antimony-vanadium-oxygen cluster compound based on a micromolecular nitrogen-containing ligand. The molecular formula of the antimony-vanadium-oxygen cluster compound is [Cd(en)3]3[Sb6V15O42(H2O)]. 8H2O, wherein en is ethidene diamine. The preparation method comprises the following steps: sequentially adding Sb2O3, NH4VO3, Cd(NO3)2. 4H2O and en into water, conducing stirring, putting the formed mixture into a reaction kettle, conducing continuous reacting at 160-180 DEG C for 110-130 hours, and after the reaction is finished, performing crystallizing to separate out black blocky crystals, thereby obtaining the antimony-vanadium-oxygen cluster compound. According to the invention, the substituted vanadium-oxygen cluster compound formed by introducing main group elements or non-metallic elements into a vanadium-oxygen cluster system greatly enriches a multi-vanadium-oxygen cluster family, and promotes sustainable development of vanadium-oxygen cluster synthesis chemistry.

Description

technical field [0001] The invention relates to the technical field of compound preparation, in particular to an antimony vanadyl cluster compound based on a small molecule nitrogen-containing ligand and a synthesis method thereof. Background technique [0002] Polyoxometalates (POMs), abbreviated as polyoxometalates, are a class of multimetallic clusters with a MOM structure formed by dehydration condensation of oxoacid radicals of major elements such as Mo, W, V, Nb, and Tb. So far, polyacid chemistry has a research history of about 200 years. With the development of science and the advancement of scientific and technological means and the deepening of research, from the original Keggin (1:12) structure to various types of complex structures today. [0003] Polyacid compounds have various superior physical and chemical properties, such as new achievements in catalytic properties, drugs, magnetic properties and energy materials, etc. Scholars are paying more and more atte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/10C07C209/00B01J31/22C02F1/32C02F101/38C02F101/36C02F101/34
CPCC07C211/65C07C209/00B01J31/1805C02F1/32B01J2531/27C02F2101/38C02F2101/36C02F2101/34C02F2101/308C02F2305/10B01J35/39
Inventor 郭海洋徐昊邹永豪
Owner JIAXING UNIV