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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 are relatively weak to covalent bonds. For example, the force is weak, it is not easy to maintain the stability of its structure, and it is easy to dissociate in various solvents

Method used

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

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Experimental program
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Effect test

Embodiment 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 by a water bath, and the H 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 sequentially added. The mixed liquid was stirred for 30 minutes and then filtered while hot. At room temperature, the solution slowly volatilized to obtain yellow-green massive crystals.

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

Embodiment 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 by a water bath, and the H 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 sequentially added. The mixed liquid was stirred for 30 minutes and then filtered while hot. At room temperature, the solution was slowly volatilized to obtain colorless transparent block crystals.

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

[0044] The crystallographic parameters of the crystal materials prepared in the above...

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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.

Description

technical field [0001] The invention belongs to the technical field of preparation of polyoxometalate complexes. Background technique [0002] With the in-depth study of supramolecular chemistry, supramolecular chemistry has already become a new interdisciplinary subject. The development of macrocycle chemistry and the coordination and specific recognition of metal ions by some host macrocycles have not only pushed chemists' enthusiasm for supramolecular research to the peak, but also pushed supramolecular host-guest chemistry to a broader stage. . [0003] As the main body of the first generation of supramolecular macrocycles, crown ethers have developed rapidly in the field of supramolecular chemistry. Crown ethers had been prepared by C.J. Pederson in the mid-1960s, and by 1967 Pederson had prepared 49 crown ether compounds. Excitingly, Pederson reported at the International Symposium on Coordination Chemistry that year that these crown ether compounds have a strong co...

Claims

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Application Information

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IPC IPC(8): C07F19/00
CPCC07F11/005C07B2200/13
Inventor 刁国旺张红旭倪鲁彬王牌查俊杰吕曾想章瀚之吴若
Owner YANGZHOU UNIV
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