High-nuclear cobalt cluster substituted silicotungstate nano-cluster compound as well as preparation method and application thereof

A technology of silicotungstate and high-nuclear cobalt clusters, which is applied in the direction of cobalt compounds, chemical instruments and methods, and measuring devices, can solve the problem of electrolysis of silicotungstate nano-clusters that have not yet been seen with more than 20 multi-nuclear cobalt clusters. Reports on chemical biosensing applications and other issues, to achieve good electrochemical activity, high yield, and good application prospects

Active Publication Date: 2020-09-01
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] According to the literature survey, there are no reports on the preparation of 20 polynuclear cob

Method used

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  • High-nuclear cobalt cluster substituted silicotungstate nano-cluster compound as well as preparation method and application thereof
  • High-nuclear cobalt cluster substituted silicotungstate nano-cluster compound as well as preparation method and application thereof
  • High-nuclear cobalt cluster substituted silicotungstate nano-cluster compound as well as preparation method and application thereof

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preparation example Construction

[0039] Another aspect of the embodiments of the present invention also provides a method for preparing the high-nuclear cobalt cluster-substituted silicotungstate nanoclusters, which includes: mixing silicotungstate, cobalt salts, and bipyridine derivatives in a solvent Mix well, and then solidify at 110-130°C for 56-88 hours to obtain purple massive crystals, which are the high-nuclear cobalt cluster-substituted silicotungstate nanoclusters, in which silicotungstate, cobalt salt and The molar ratio of bipyridine derivatives is 1:7:3˜1:9:5.

[0040] Further, the molar ratio of the silicotungstate, cobalt salt and bipyridine derivatives is (0.03~0.05):(0.21~0.45):(0.09~0.25), specifically, the silicotungstate, The amounts of the cobalt salt and the bipyridine derivatives are 0.03-0.05 mmol, 0.21-0.45 mmol and 0.09-0.25 mmol, respectively.

[0041] Further, the cobalt salt includes cobalt chloride hydrate, preferably cobalt chloride hexahydrate, but not limited thereto.

[004...

Embodiment 1

[0056] Example 1: Preparation of high-nuclear cobalt cluster substituted silicotungstate nanoclusters

[0057] Na 10 [α-SiW 9 o 34 ]·18H 2 O (111.2mg, 0.04mmol), CoCl 2 ·6H 2 O (78.0mg, 0.33mmol) and 4,4'-bipyridine-N,N'-dioxide (30.0mg, 0.16mmol) were added to 6.0mL of water, and 1mol·L –1 Adjust the pH of the system with HCl to 5.0, stir at room temperature for 30 minutes, then add the above suspension into a 25mL polytetrafluoroethylene reactor, solidify at 120°C for 72 hours, and finally cool to room temperature to obtain purple Blocky crystals were washed 3 times with acetonitrile and dried at room temperature. The yield was about 31%.

Embodiment 2

[0058] Example 2: Preparation of high-nuclear cobalt cluster substituted silicotungstate nanoclusters

[0059] Na 10 [α-SiW 9 o 34 ]·18H 2 O (139.0 mg, 0.05 mmol), CoCl 2 ·6H 2 O (49.6mg, 0.21mmol) and 4,4'-bipyridine-N,N'-dioxide (16.9mg, 0.09mmol) were added to a mixed solvent of 6.0mL water and 0.5mL acetonitrile, and 1mol·L –1 Adjust the pH of the system with HCl to 5.4, stir at room temperature for 25 minutes, then add the above suspension into a 25mL polytetrafluoroethylene reactor, solidify at 110°C for 88 hours, and finally cool to room temperature to obtain a purple color Blocky crystals were washed 3 times with acetonitrile and dried at room temperature. The yield was about 37%.

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Abstract

The invention discloses a high-nuclear cobalt cluster substituted silicotungstate nano-cluster compound as well as a preparation method and application thereof. The high-nuclear cobalt cluster substituted silicotungstate nano-cluster compound has the following chemical formula: Na18[Co(H2O)6]2{[Na(H2O)4]2[Na(H2O)2]2[Co(H2O)3]2[Co21(H2O)4(OH)12] (SiW10O37)6} 24H2O. The high-core cobalt cluster substituted silicotungstate nano-cluster compound is crystallized in a triclinic system, and the space group is P-1. An electrochemical biosensor based on the high-nuclear cobalt cluster substituted silicotungstate nano-cluster compound is simple and convenient when being used for detecting dichlorvos, and has the advantages of high selectivity, good repeatability, good stability, low detection limitand the like.

Description

technical field [0001] The invention specifically relates to a high-nuclear cobalt cluster substituted silicotungstate nano-cluster and its preparation method, as well as the application of an electrochemical biosensor based on the nano-cluster in food safety detection, which belongs to the preparation of new chemical materials and Field of application technology. Background technique [0002] Polyoxometalates (Polyoxometalates, POMs) are a class of nanoscale metal-oxygen clusters formed by high oxidation state transition metal ions such as Mo, W, V, Nb, Ta, etc. connected through oxygen atoms. Lacking POMs are considered as inorganic, multidentate ligands that are ideal candidates for encapsulating a wide variety of polynuclear metal–oxygen fragments. In particular, nanoclusters constructed from high-nuclear transition metal-oxygen fragments and vacant POMs not only exhibit novel nanostructures, but also have diverse applications in the fields of single-molecule magnets, h...

Claims

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Application Information

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IPC IPC(8): C01G51/00G01N27/327
CPCC01G51/006G01N27/3278C01P2002/72C01P2002/84C01P2002/80
Inventor 史岽瑛崔超杰王思佳孙晨一聂周缓
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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