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Dodeca-tungstate crystal material with two-dimensional nano pore cavity structure and preparation method of dodeca-tungstate crystal material

A technology of two-dimensional nanometer and crystalline materials, applied in the fields of polycrystalline material growth, crystal growth, chemical instruments and methods, etc. High yield, simple and easy synthesis method, and good catalytic activity

Active Publication Date: 2019-03-26
HEFEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recent studies have shown that polytungstate clusters exhibit excellent catalytic properties, but there are not many studies on organic-inorganic hybrid heteropolytungstate clusters constructed from alkali metals, especially those with two-dimensional nanopores Such crystal materials with cavity structure are rarely studied.

Method used

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  • Dodeca-tungstate crystal material with two-dimensional nano pore cavity structure and preparation method of dodeca-tungstate crystal material
  • Dodeca-tungstate crystal material with two-dimensional nano pore cavity structure and preparation method of dodeca-tungstate crystal material
  • Dodeca-tungstate crystal material with two-dimensional nano pore cavity structure and preparation method of dodeca-tungstate crystal material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] ①. Weigh 0.06g of sodium tungstate, 0.12g of tungstic acid, 0.08g of imidazole, 0.04g of ammonium chloride, and 0.03g of potassium chloride into a 50mL flask, add 18mL of distilled water, and place the flask on a magnetic stirrer to stir and mix After 20 minutes, a mixed solution was obtained.

[0023] ②. Transfer the uniformly mixed solution to a 25mL autoclave.

[0024] ③ Put the autoclave into an oven, heat it from room temperature to 160 °C at a rate of 1 °C / min, keep it at this temperature for 72 hours, and then lower it to room temperature at a rate of 0.2 °C / min to obtain a two-dimensional nanopore structure of dodecantungstate crystal material, the yield is about 72%.

[0025] The crystal structure of the target product prepared in this embodiment was determined by a single crystal diffractometer, and the results were as follows:

[0026] Crystal data:

[0027]

[0028]

[0029] Crystal structure analysis:

[0030] Please also refer to figure 1 , the ...

Embodiment 2

[0033] ①. Weigh 0.11g of sodium tungstate, 0.09g of tungstic acid, 0.07g of imidazole, 0.03g of ammonium chloride, and 0.04g of potassium chloride into a 50mL flask, add 20mL of distilled water, and place the flask on a magnetic stirrer to stir and mix After 20 minutes, a mixed solution was obtained.

[0034] ②. Transfer the uniformly mixed solution to a 25mL autoclave.

[0035] ③. Put the autoclave into an oven, heat it from room temperature to 160 °C at a rate of 1 °C / min, keep it at this temperature for 72 hours, and then lower it to room temperature at a rate of 0.26 °C / min to obtain the following: figure 1 with 2 The yield of the dodecungstate crystal material with a two-dimensional nano-cavity structure is about 73%.

Embodiment 3

[0037] ①. Weigh 0.06g of sodium tungstate, 0.12g of tungstic acid, 0.08g of imidazole, 0.04g of ammonium chloride, and 0.03g of potassium chloride into a 50mL flask, add 17mL of distilled water, and place the flask on a magnetic stirrer to stir and mix After 20 minutes, a mixed solution was obtained.

[0038] ②. Transfer the uniformly mixed solution to a 25mL autoclave.

[0039] ③. Put the autoclave into an oven, heat it from room temperature to 180 °C at a rate of 2 °C / min, keep it at this temperature for 48 hours, and then lower it to room temperature at a rate of 0.3 °C / min to obtain the following: figure 1 with 2 The yield of the dodecungungstate crystal material with a two-dimensional nano-cavity structure is about 75%.

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Abstract

The invention discloses a dodeca-tungstate crystal material with a two-dimensional nano pore cavity structure and a preparation method of the dodeca-tungstate crystal material, and belongs to the technical field of metal oxygen cluster compound materials and preparation thereof. The chemical formula of the dodeca-tungstate crystal material is (NH4)Na2K(C3H5N2)6[H2W12O42].8H2O, the dodeca-tungstatecrystal material is a triclinic system, the space group is P-1, and the cell parameters are that a=11.2454(7) Angstrom, b=11.8209(7) Angstrom, and c=11.8634(7) Angstrom, wherein alpha is equal to 82.1590(10) degrees, and beta is equal to 87.7150(10) degrees. Raw materials such as sodium tungstate, tungsten acid, imidazole and ammonium chloride are subjected to hydrothermal synthesis, then the dodeca-tungstate crystal material provided with the two-dimensional nano pore cavity structure and capable of being widely applied to the field of catalytic materials can be prepared, the dodeca-tungstate crystal material can play a catalytic role when hydrogen peroxide oxidizes cyclopentene to prepare glutaraldehyde, the productive rate of a product can reach 60% or above, and the good catalytic activity is shown.

Description

technical field [0001] The invention belongs to the technical field of metal oxygen cluster materials and their preparation, and in particular relates to a dodedotungstate crystal material with a two-dimensional nano-cavity structure and a preparation method thereof. Background technique [0002] Certain transition metals, such as vanadium, molybdenum, and tungsten, are capable of forming polymetallic oxygen clusters in their high oxidation states. Such substances usually have some excellent properties due to their unique structure, such as electrical conductivity, magnetism, and catalytic properties, and are widely used in analysis, clinical diagnosis, catalysis, biochemistry, medicine, and material science. With the development of polyoxometalate chemistry, more and more researches have been done on organic-inorganic hybrid polyoxometalates, including an important family of hybrid polytungstates. The latest challenge in this research field is how to utilize basic building...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/32C30B7/10B01J31/02B01J23/30C07C45/28C07C47/12
CPCB01J23/30B01J31/0244C07C45/28C30B7/10C30B29/32C07C47/12
Inventor 张全争梁升尹奇异鲁红典
Owner HEFEI UNIV
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