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Iron-dysprosium heterometallic antimony tungstate frame material with binary organic carboxylic acid and its preparation method and application

A technology of binary organic carboxylic acid and metal antimony tungstate, which is applied in the field of iron-dysprosium heterometal antimony tungstate frame material and its preparation, can solve the problems of active center destruction and poor electrochemical cycle stability, and achieve Sensitive detection, accurate and sensitive detection, and low preparation cost

Active Publication Date: 2020-12-25
HENAN UNIVERSITY
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  • Abstract
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  • Application Information

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Problems solved by technology

Although some of them have been used to detect small molecular compounds like dopamine, folic acid, L-tyrosine, L-tryptophan (see Z. Wang, Q. Han, J. Xia, et al. J. Electroanal. Chem. 2014, 726 , 107–111), but polyoxometalate biosensors that can be used to detect biomacromolecules such as proteins, nucleic acids, and DNA have not been reported
In this research field, the main problem is that the polyoxometalate material with isolated structure has good solubility in the reaction system, which destroys the active center during the detection process, and then presents a poor electrochemical cycle. Stability (see J.-S. Qin, D.-Y. Du, W. Guan, et al. J. Am. Chem. Soc. 2015, 137 , 7169–7177)

Method used

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  • Iron-dysprosium heterometallic antimony tungstate frame material with binary organic carboxylic acid and its preparation method and application
  • Iron-dysprosium heterometallic antimony tungstate frame material with binary organic carboxylic acid and its preparation method and application
  • Iron-dysprosium heterometallic antimony tungstate frame material with binary organic carboxylic acid and its preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of iron-dysprosium heterometallic antimony tungstate frame material participated by binary organic carboxylic acid, its chemical formula is: [Dy(H 2 O) 6 ] 2 [Fe 4 (H 2 L) 4 (B-β-SbW 9 o 33 ) 2 ]∙50H 2 O(H 2 L = 2,5-pyridinedicarboxylic acid).

[0026] The iron-dysprosium heterometal antimony tungstate frame material participated by the above-mentioned binary organic carboxylic acid is obtained by a step-by-step assembly method, and its preparation method specifically includes the following steps:

[0027] 0.700 g Na 9 [B-α-SbW 9 o 33 ]∙19.5H 2 O (0.245 mmol), 0.080 g Dy(NO 3 ) 3 ∙6H 2 O (0.175 mmol) and 0.160 g of 2,5-pyridinedicarboxylic acid (0.957 mmol) were dissolved in 10 mL of distilled water (555.1 mmol). After stirring for 30 min, use 1 mol∙L –1 HCl to adjust the pH of the reaction system to 2.0, then add 0.150 g FeCl 3 ∙6H 2 O (0.555 mmol). After stirring for 30 min, use 2 mol∙L –1 The pH of the reaction system was adjusted to 2.0 ...

Embodiment 2

[0029] A kind of iron-dysprosium heterometallic antimony tungstate frame material participated by binary organic carboxylic acid, its chemical formula is: [Dy(H 2 O) 6 ] 2 [Fe 4 (H 2 L) 4 (B-β-SbW 9 o 33 ) 2 ]∙50H 2 O, (H 2 L = 2,5-pyridinedicarboxylic acid).

[0030] The iron-dysprosium heterometal antimony tungstate frame material participated by the above-mentioned binary organic carboxylic acid is obtained by a step-by-step assembly method, and its preparation method specifically includes the following steps:

[0031] 0.700 g Na 9 [B-α-SbW 9 o 33 ]∙19.5H 2 O (0.245 mmol), 0.090g Dy(NO 3 ) 3 ∙6H 2 O (0.197 mmol) and 0.160 g of 2,5-pyridinedicarboxylic acid (0.957 mmol) were dissolved in 10 mL of distilled water (555.1 mmol). After stirring for 30 min, use 1 mol∙L –1 HCl to adjust the pH of the reaction system to 2.0, then add 0.150 g FeCl 3 ∙6H 2 O (0.555 mmol). After stirring for 30 min, use 2 mol∙L –1 The pH of the reaction system was adjusted to 2.0...

Embodiment 3

[0033] A kind of iron-dysprosium heterometallic antimony tungstate frame material participated by binary organic carboxylic acid, its chemical formula is: [Dy(H 2 O) 6 ] 2 [Fe 4 (H 2 L) 4 (B-β-SbW 9 o 33 ) 2 ]∙50H 2 O, (H 2 L = 2,5-pyridinedicarboxylic acid).

[0034] The iron-dysprosium heterometal antimony tungstate frame material participated by the above-mentioned binary organic carboxylic acid is obtained by a step-by-step assembly method, and its preparation method specifically includes the following steps:

[0035] 0.650 g Na 9 [B-α-SbW 9 o 33 ]∙19.5H 2 O (0.227 mmol), 0.080g Dy(NO 3 ) 3 ∙6H 2 O (0.175 mmol) and 0.160 g of 2,5-pyridinedicarboxylic acid (0.957 mmol) were dissolved in 10 mL of distilled water (555.1 mmol). After stirring for 30 min, use 1 mol∙L –1 HCl to adjust the pH of the reaction system to 2.10, then add 0.150 g FeCl 3 ∙6H 2 O (0.555 mmol). After stirring for 30 min, use 2 mol∙L –1 The pH of the reaction system was adjusted to 2....

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Abstract

The invention relates to an organic dicarboxylic acid participated iron-dysprosium dissimilar metal antimoniotungstate frame material. A chemical formula of the organic dicarboxylic acid participatediron-dysprosium dissimilar metal antimoniotungstate frame material is [Dy(H2O)6]2[Fe4(H2L)4(B-beta-SbW9O33)2]-502HO; and in the formula, H2L is 2,5-pyridinedicarboxylic acid. The organic dicarboxylicacid participated iron-dysprosium dissimilar metal antimoniotungstate frame material belongs to a hexagonal system and the space group is R-3, and unit cell parameters are as follows: a being equal to42.8411(12) angstrom, b being equal to 42.8411(12) angstrom, c being equal to 20.4129(12) angstrom, alpha being equal to 90.00 degrees, beta being equal to 90.00 degrees, gamma being equal to 120.00degrees, V being equal to 32446(2) angstrom<3>, Z being equal to 9, R1 being equal to 0.0519, and wR2 being equal to 0.1226. Synthesis of the organic dicarboxylic acid participated iron-dysprosium dissimilar metal antimoniotungstate frame material adopts a strategy of stepwise assembly, and the organic dicarboxylic acid participated iron-dysprosium dissimilar metal antimoniotungstate frame material is prepared by utilizing prepared precursors Na9[B-alpha-SbW9O33]-19.5H2O, 2,5-pyridinedicarboxylic acid, FeCl3-6H2O and Dy(NO3)3-6H2O under the hydrothermal condition. Discovered through researches, the organic dicarboxylic acid participated iron-dysprosium dissimilar metal antimoniotungstate frame material can be used an electrode material in an electrochemical biosensor, and the electrochemical biosensor can realize precision detection on the content of mucin in human serum.

Description

technical field [0001] The invention belongs to the technical field of preparation of polyoxometalate chemical materials, and specifically relates to an iron-dysprosium heterometallic antimony tungstate framework material participated in by binary organic carboxylic acid, its preparation method and its application in the field of electrochemical biosensing . Background technique [0002] In recent years, with the growing demand for rapid and ultrasensitive detection of biomolecules in chemical analysis, medical diagnosis, health care, and environmental monitoring, the design and fabrication of electrochemical biosensors with excellent performance has received great attention. , which are inseparable from their advantages of low price, convenient operation and good reproducibility (see S. Mao, J. Chang, H. Pu, et al . Chem. Soc. Rev. 2017, 46 , 6872–6904). It is well known that the performance of electrochemical biosensors greatly depends on the physical and chemical prop...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 陈利娟赵俊伟刘雅洁陈艳红
Owner HENAN UNIVERSITY
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