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A kind of preparation method of polymolybdophosphoric acid-nitrogen heterocyclic salt supramolecular compound

A technology of supramolecular compounds and nitrogen heterocycles, applied in organic chemistry methods, chemical instruments and methods, 6/16 group organic compounds without C-metal bonds, etc., can solve complex immobilization procedures and key operating conditions and costs High, long time required for detection, etc.

Inactive Publication Date: 2019-12-13
UNIV OF JINAN
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Existing electrochemical sensors generally rely on biological enzymes and soluble redox mediators, but enzyme-based electrochemical sensors have poor stability and high cost; at the same time, they also have complex immobilization procedures and key operating conditions. Therefore, the use of enzyme-based electrochemical sensors When chemical sensors are used for detection, the detection takes a long time, and the requirements for the detection operating environment and personnel are high

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  • A kind of preparation method of polymolybdophosphoric acid-nitrogen heterocyclic salt supramolecular compound
  • A kind of preparation method of polymolybdophosphoric acid-nitrogen heterocyclic salt supramolecular compound
  • A kind of preparation method of polymolybdophosphoric acid-nitrogen heterocyclic salt supramolecular compound

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[0046] The invention provides a kind of preparation method of polymolybdophosphoric acid-nitrogen heterocyclic salt supramolecular compound, and described preparation method comprises the following steps:

[0047] step one:

[0048] Weigh the polymolybdenum phosphate and nitrogen heterocyclic rings, place them in the reaction solution, stir to make them fully dispersed, add an acid regulator dropwise to adjust the pH of the reaction solution to 1.0-5.0, and continue stirring to completely dissolve the reaction materials.

[0049] The polymolybdenum phosphate refers to a metal phosphate containing multiple molybdenum atoms, such as hexamolybdenum tetraphosphate, dodecamolybdenum phosphate, octadecyl molybdenum diphosphate, octadecademolybdenum hexaphosphate or pentamolybdenum diphosphate Salt;

[0050] Preferred are octadecyl molybdenum diphosphate and octadecadeca molybdenum hexaphosphate;

[0051] It is more preferred to use octadecyl molybdenum diphosphate, the anion in th...

Embodiment 1

[0160] (1) Preparation of octadecadectamolybdenum diphosphate di(4,4') bipyridine hexaammonium salt;

[0161] 0.4g (NH 4 ) 6 P 2 Mo 18 o 62 2H 2 O, 0.043g C 10 h 8 N 2 (4,4'-Bipyridine) was added to a mixed solution of 5mL distilled water and 3mL absolute ethanol, stirred until uniformly dispersed, adjusted the pH of the solution to 2.0 with dilute nitric acid, and stirred for 1 hour to completely dissolve; then the reaction solution was placed in Seal it in a stainless steel reaction kettle with a filling degree of 50%; place the sealed stainless steel reaction kettle in an oven with a temperature of 150°C, heat it for 4 days, and obtain block crystals after cooling at room temperature, wash with distilled water and dry at room temperature to obtain the compound 1, 0.195 g, yield 44.1%.

[0162] (2) Preparation of compound 1 and graphene oxide mixture modified electrode;

[0163] Select the bare glassy carbon electrode as the base electrode, first polish the bare gl...

Embodiment 2

[0172] (1) Preparation of octadecadectamolybdenum diphosphate tetrapyridinium hexammonium salt;

[0173] 0.4g (NH 4 ) 6 P 2 Mo 18 o 62 2H 2 O. Add 0.043g of pyridine to the mixed solution of 5mL of distilled water and 3mL of absolute ethanol, stir until uniformly dispersed, adjust the pH of the solution to 1.5 with dilute nitric acid, and stir for 1.5 hours to completely dissolve it; then place the reaction solution in a stainless steel reactor Internally sealed, the filling degree is 45%; the sealed stainless steel reaction kettle is placed in an oven with a temperature of 160°C, heated for 4 days, cooled at room temperature to obtain blocky crystals, washed with distilled water and dried at room temperature to obtain compound 1, which is 0.187 g, the yield was 42.3%.

[0174] (2) Preparation of compound 1 and graphene oxide mixture modified electrode;

[0175] The method is the same as that in Example 1(2).

[0176] (3) Preparation of compound 1-polypyrrole-graphene ...

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Abstract

The invention provides a preparation method of a polymolybdophosphate-N-heterocyclic salt supramolecular compound. The method comprises the following steps: 1, weighing polymolybdophosphate and N-heterocycle; adding to reaction liquid; stirring to fully disperse; dropwise adding an acid conditioner to condition the pH of the reaction liquid to be 1.0-5.0; and continuously stirring until the reacting raw materials are completely dissolved; 2, sealing all reacting substances into a reaction kettle after the stirring is finished; heating and reacting until the reaction is finished; and cooling toobtain blocky crystals; and 3, post-processing the obtained blocky crystals to obtain the polymolybdophosphate-N-heterocyclic salt supramolecular compound. The method is simple in preparation processes, easy to obtain raw materials, low in cost, and high in yield.

Description

technical field [0001] The present invention relates to a kind of polyoxometalate, especially the preparation method of polymolybdenum phosphate; Specifically, relate to a kind of preparation method of polymolybdophosphoric acid-nitrogen heterocyclic salt supramolecular compound, and this compound is used for modifying electrode Improving the electrochemical properties of electrodes and making them selective. Background technique [0002] Polyoxometallates are rich in structure, and have acidity, alkalinity and redox properties. The research on the synthesis, structure and properties of polyoxometalates provides a theoretical and experimental basis for practical applications, and also promotes the development of chemical science. Research and development of its adjacent disciplines in catalysis, biomedicine, and functional materials development. [0003] In organisms, hydrogen peroxide is not only a by-product under the action of enzymes, but also a second signal transmitte...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F11/00G01N27/30
CPCC07B2200/13C07F11/005G01N27/308
Inventor 高广刚孙浩浩刘红张玉琢宋朝宇
Owner UNIV OF JINAN