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Polyoxometalate cluster organic amine salt and preparation method thereof

A technology of polymetallic oxygen clusters and organic amine salts, which is applied in the preparation of organic compounds, organic chemistry, preparation of amino compounds, etc., can solve the problem of single cation structure, achieve broad application prospects, expand the scope of application, and simple preparation methods Effect

Inactive Publication Date: 2014-10-29
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] For the cation structure of the existing tetrabutylammonium polymetallic oxygen cluster is too single, the force between the anion and the cation is only electrostatic, and the applicable catalytic system still has certain limitations. One of the purposes of the present invention It is to provide a polymetallic oxygen cluster organic amine salt. The polymetallic oxygen cluster organic amine salt increases the type of interaction between anion and cation, that is, on the basis of the original electrostatic interaction, the interaction between the two is increased. Hydrogen bonding; the second purpose is to provide a preparation method of polymetallic oxygen cluster organic amine salt, the preparation method is low in cost and simple to operate

Method used

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  • Polyoxometalate cluster organic amine salt and preparation method thereof
  • Polyoxometalate cluster organic amine salt and preparation method thereof
  • Polyoxometalate cluster organic amine salt and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0052] Cyclohexylamine phosphotungstate ((C 6 H 14 N) 3 PW 12 O 40 ) Preparation method:

[0053] (1) Fully dissolve 0.4 mmol cyclohexylamine in 10 mL deionized water, adjust pH=2 with 2 mol / L hydrochloric acid solution, and obtain a concentration of 4.0×10 -2 mol / L cyclohexylamine solution;

[0054] (2) Fully dissolve 0.1 mmol phosphotungstic acid in 10 mL deionized water to obtain a concentration of 1.0×10 -2 mol / L phosphotungstic acid solution;

[0055] (3) Add the cyclohexylamine solution dropwise to the phosphotungstic acid solution under stirring, react for 20 minutes, centrifuge, wash twice with distilled water, and dry in the air in the dark to obtain a solid composite;

[0056] (4) Dissolve the solid composite in acetonitrile and recrystallize at 20°C to obtain crystal 1;

[0057] by figure 1 It can be seen that crystal 1 is at 700-1100 cm -1 H appears in the wave number interval 3 PW 12 O 40 The corresponding characteristic absorption peak (Introduction to Polyacid Chemistry...

Embodiment 2

[0061] Morpholine phosphotungstate ((C 4 H 10 NO) 3 PW 12 O 40 ) Preparation method:

[0062] (1) Fully dissolve 0.45 mmol morpholine in 10 mL deionized water, adjust pH=3 with 2 mol / L hydrochloric acid solution, and obtain a concentration of 4.5×10 -2 mol / L morpholine solution;

[0063] (2) Fully dissolve 0.1 mmol phosphotungstic acid in 10 mL deionized water to obtain a concentration of 1.0×10 -2 mol / L phosphotungstic acid solution;

[0064] (3) Add the morpholine solution dropwise to the phosphotungstic acid solution under stirring, react for 30 minutes, centrifuge, wash 3 times with distilled water, and dry in the air in the dark to obtain a solid composite of morpholine phosphotungstate;

[0065] (4) The solid composite was dissolved in acetonitrile, and recrystallized at 22°C to obtain crystal 2;

[0066] by Figure 4 It can be seen that crystal 2 is at 700-1100 cm -1 H appears in the wave number interval 3 PW 12 O 40 The corresponding characteristic absorption peak (Introductio...

Embodiment 3

[0070] Triethanolamine phosphotungstate ((C 6 H 16 NO 3 ) 3 PW 12 O 40 ) Preparation method:

[0071] (1) Fully dissolve 0.45 mmol triethanolamine in 10 mL deionized water, adjust pH=3 with 2.5 mol / L hydrochloric acid solution, and obtain a concentration of 4.5×10 -2 mol / L triethanolamine solution;

[0072] (2) Fully dissolve 0.11 mmol phosphotungstic acid in 10 mL deionized water to obtain a concentration of 1.1×10 -2 mol / L phosphotungstic acid solution;

[0073] (3) Add the triethanolamine solution dropwise to the phosphotungstic acid solution under stirring, react for 30 minutes, centrifuge, wash 3 times with distilled water, and dry in the air in the dark to obtain a solid composite;

[0074] (4) The solid composite was dissolved in acetonitrile, and recrystallized at 22°C to obtain crystal 3;

[0075] by Figure 7 It can be seen that crystal 3 is at 700-1100 cm -1 H appears in the wave number interval 3 PW 12 O 40 The corresponding characteristic absorption peak (Introduction to ...

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Abstract

The invention discloses polyoxometalate cluster organic amine salt and a preparation method thereof, belonging to the field of chemical technology of inorganic polyoxometalate clusters. A molecular formula of the polyoxometalate cluster organic amine salt is (Q)Mxm12O40. The preparation method comprises the following steps: dropwise adding an organic amine salt solution into a polyoxometalate cluster solution, reacting for a period of time, centrifuging, washing, drying, and re-crystallizing to obtain the polyoxometalate cluster organic amine salt. The preparation method is easy and convenient to operate; all raw materials are obtained from the market and are low in cost. According to the prepared novel polyoxometalate cluster organic amine salt, organic amine positive ions with certain spatial structures are introduced, the types of acting forces between negative ions and positive ions are enriched, the acting intensity of the negative and positive ions is increased, the application range of a polyoxometalate cluster catalyst is conveniently expanded, and the application prospects are wide.

Description

Technical field [0001] The invention relates to a polymetallic oxygen cluster organic amine salt and a preparation method thereof, belonging to the chemical technical field of inorganic polymetallic oxygen clusters. Background technique [0002] Polyoxometalates (POMs) are a kind of homopoly and heteropolymetallic oxygen with a certain structure and a skeleton structure with a size between 0.5 nm and 5 nm rich in transition elements such as molybdenum, tungsten, vanadium, niobium, and tantalum. Cluster compound. Polymetallic oxygen clusters have diverse topological structures and rich physical and chemical properties, so they have shown great application potential in the fields of optical, electrical and magnetic functional materials, medicine and catalysis. Among the various functional characteristics of polymetallic oxygen clusters, the catalytic properties are the most extensive and in-depth research. One of the representative ones is the catalysis of polymetallic oxygen clus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/35C07C211/38C07C209/00C07C213/08C07C215/12C07D295/027C07D295/088C07D295/023C07D487/18B01J31/18B01J31/16
Inventor 曹洁贾巧地徐冲胡长文
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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