Preparation method of supramolecular crystal material based on crown ether-Keggin type polyacid

A technology of supramolecular crystals and crown ethers, applied in organic chemistry methods, 6/16 group organic compounds without C-metal bonds, organic chemistry, etc., can solve the problems of difficulty in maintaining structural stability, easy dissociation, and weak force and other problems, to achieve the effect of high yield, simple preparation and stable crystal structure

Active Publication Date: 2021-06-11

YANGZHOU UNIV

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Problems solved by technology

[0005] Judging from the current technical means, the supramolecular crystal materials constructed by crown ethers and polyacids are mostly dominated by intermolecular forces, which...

Method used

Fig. 1 and Fig. 2 are the molecular structure figure that prepares crown ether-Keggin type multi-acid novel supramolecular crystal material in embodiment 1,...

Abstract

The invention discloses a preparation method of a supramolecular crystal material based on crown ether-Keggin type polyacid, and belongs to the technical field of preparation of polyoxometallate compounds. The preparation method comprises the steps of dissolving Keggin type polyoxometallate in an acetonitrile solution, then adding an alkali metal element, heating to the temperature of 60-80 DEG C, then adding supramolecular crown ether for reaction, filtering after the reaction is finished, taking filtrate, volatilizing a solvent to obtain crystals, and then carrying out suction filtration, washing and drying to obtain the supramolecular crystal material based on crown ether-Keggin type polyacid. The preparation method is simple, the yield is high, and most importantly, a stable crystal structure is formed.

Application Domain

Organic chemistry methodsGroup 6/16 organic compounds without C-metal linkages

Technology Topic

Polymer chemistryCrown ether +6

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Examples

Experimental program(2)
Comparison scheme(1)

Example Embodiment

[0038] Example 1:

[0039] 455 mg (0.25 mmol) of Keggin-type heteropolyacid H 4 [SiMo 12 O 40 ] dissolved in 125 mL of CH 3 CN, and the temperature of the system was heated to 70 °C through a water bath, and the 4 [SiMo 12 O 40 ] After complete dissolution, 145 mg (1.5 mmol) of KAc and 330 mg (1.25 mmol) of 18-crown-6 were added sequentially. The mixed liquid was stirred for 30 minutes, filtered while hot, and slowly volatilized with the solution at room temperature to obtain yellow-green massive crystals.

[0040] Then through suction filtration, after fully washing with a large amount of deionized water, the crystals were collected and placed in an oven at 60 °C and dried for 24 h to obtain {[K(H 24 C 12 O 6 )] 2 [K(H 24 C 12 O 6 )(CH 3 EN)] 2 [SiMo12 O 40 ]} 0.559g, referred to as crystal material 1 , Yield: 71.7% (based on Mo)

Example Embodiment

[0041] Example 2:

[0042] 720 mg (0.25 mmol) of Keggin-type heteropolyacid H 4 [SiW 12 O 40 ] dissolved in 120 mL of CH 3 CN, and the temperature of the system was heated to 70 °C through a water bath, and the 4 [SiW 12 O 40 ] After complete dissolution, 110 mg (1.5 mmol) of KCl and 330 mg (1.25 mmol) of 18-crown-6 were added sequentially. The mixed liquid was stirred for 30 minutes, filtered while hot, and slowly volatilized with the solution at room temperature to obtain colorless and transparent bulk crystals.

[0043] Suction filtration, fully washed with a large amount of deionized water, then filtered with suction, washed with a large amount of deionized water, collected the crystals in an oven at 60 °C, and dried for 24 h to obtain {[K(H 24 C 12 O 6 )] 2 [K(H 24 C 12 O 6 )(CH 3 EN)] 2 [SiW 12 O 40 ]} 0.845g, referred to as crystal material 2 , Yield: 81% (based on W).

[0044] The crystallographic parameters of the crystalline materials prepared in the above two examples are shown in the following table:

[0045] Crystallographic parameters Crystal material 1

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Preparation method of supramolecular crystal material based on crown ether-Keggin type polyacid

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