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Polyoxometalate cluster organic amine salt and preparation method thereof

A technology of polymetallic oxygen clusters and organic amine salts, applied in the preparation of organic compounds, organic chemistry, preparation of amino compounds, etc., can solve the problem of single cation structure, achieve wide application prospects, expand application scope, and enhance the strength of action. Effect

Inactive Publication Date: 2015-06-10
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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
Comparison scheme
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 compound;

[0056] (4) dissolving the solid complex in acetonitrile and recrystallizing at 20°C to obtain crystal 1;

[0057] Depend on 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 (Int...

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 complex of morpholine phosphotungstate;

[0065] (4) Dissolving the solid complex in acetonitrile and recrystallizing at 22°C to obtain crystal 2;

[0066] Depend on 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 absor...

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 with distilled water for 3 times, and dry in the air in the dark to obtain a solid compound;

[0074] (4) Dissolving the solid complex in acetonitrile and recrystallizing at 22°C to obtain crystal 3;

[0075] Depend on 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 abso...

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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 class of isopoly and heteropolyoxometalates rich in transition elements such as molybdenum, tungsten, vanadium, niobium, and tantalum in a framework structure with a definite structure and a size between 0.5 nm and 5 nm. cluster compounds. Polymetallic oxygen clusters have diverse topological structures and rich physical and chemical properties, so they show great application potential in the fields of optical, electrical, and magnetic functional materials, medicine, and catalysis. Among the functional properties of polymetallic oxygen clusters, the catalytic properties are the most widely and deeply studied, and the representative one is the catalytic effect of polymetallic oxygen clusters, which can b...

Claims

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Application Information

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Patent Type & Authority Patents(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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