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Organic-inorganic hybrid polymolybdate crystal material and preparation method thereof

A technology of polymolybdate and crystal materials, which is applied in the growth of polycrystalline materials, chemical instruments and methods, crystal growth, etc., can solve the problems of unsatisfactory fluorescence performance, and achieve simple and easy-to-operate synthesis methods and high reaction yields high effect

Inactive Publication Date: 2016-03-23
HEFEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, current organic and organo-metallic derivative materials are not satisfactory in terms of fluorescence properties

Method used

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  • Organic-inorganic hybrid polymolybdate crystal material and preparation method thereof
  • Organic-inorganic hybrid polymolybdate crystal material and preparation method thereof
  • Organic-inorganic hybrid polymolybdate crystal material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] ①. Weigh 0.1g of molybdenum oxide, 0.12g of ammonium metavanadate, 0.05g of 1,10-phenanthroline and 0.15g of nickel acetate into a 50mL flask, add 18mL of water and 0.5mL of phosphoric acid, and place the flask under magnetic stirring Mix on mixer for 30 minutes.

[0032] ②. Transfer the uniformly mixed solution to a 25mL autoclave.

[0033] ③. Put the autoclave into an oven, heat it from room temperature to 180 °C at a rate of 1.5 °C / min, keep it at this temperature for 72 hours, and then lower it to room temperature at a rate of 5 °C / h, and the solid-liquid separation is as follows: figure 1 and figure 2 as shown, image 3 and Figure 4 The organic-inorganic hybrid polymolybdate crystal material shown in the curve has a yield of about 78%.

[0034] The crystal structure of the target product prepared in this embodiment was determined by a single crystal diffractometer, and the results were as follows:

[0035] Crystal data:

[0036]

[0037] Crystal bond len...

Embodiment 2

[0044] ①. Weigh 0.09g of molybdenum oxide, 0.13g of ammonium metavanadate, 0.04g of 1,10-phenanthroline and 0.18g of nickel acetate into a 50mL flask, add 19mL of water and 0.5mL of phosphoric acid, and place the flask under magnetic stirring Mix on mixer for 20 minutes.

[0045] ②. Transfer the uniformly mixed solution to a 25mL autoclave.

[0046] ③ Put the autoclave into an oven, heat it from room temperature to 180 °C at a rate of 1 °C / min, keep it at this temperature for 60 hours, and then cool it down to room temperature at a rate of 4 °C / h, the solid-liquid separation is as follows: figure 1 and figure 2 shown, approximately image 3 and Figure 4 The organic-inorganic hybrid polymolybdate crystal material shown in the curve has a yield of about 75%.

Embodiment 3

[0048] ①. Weigh 0.11g of molybdenum oxide, 0.11g of ammonium metavanadate, 0.06g of 1,10-phenanthroline and 0.12g of nickel acetate into a 50mL flask, add 20mL of water and 0.5mL of phosphoric acid, and place the flask under magnetic stirring Mix on mixer for 5 minutes.

[0049] ②. Transfer the uniformly mixed solution to a 25mL autoclave.

[0050] 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 80 hours, and then lower it to room temperature at a rate of 3 °C / h. The solid-liquid separation is as follows: figure 1 and figure 2 shown, approximately image 3 and Figure 4 The organic-inorganic hybrid polymolybdate crystal material shown in the curve has a yield of about 76%.

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Abstract

The invention discloses an organic-inorganic hybrid polyoxomolybdate crystal material and a preparation method thereof. The organic-inorganic hybrid polyoxomolybdate crystal material comprises a polyoxomolybdate crystal, and the chemical formula of the polyoxomolybdate crystal is [Ni(H2O)(C12H8N2)2]2(PMo12O40(VO)2].2H2O, the polyoxomolybdate crystal belongs to a triclinic system, and the space group of the polyoxomolybdate crystal is P-1. The organic-inorganic hybrid polyoxomolybdate crystal material is prepared by adopting a hydrothermal synthesis method. The preparation method of the organic-inorganic hybrid polyoxomolybdate crystal material comprises the following steps: and stirring and mixing molybdenum oxide, ammonium metavanadate, 1, 10-phenanthroline, nickel acetate, phosphoric acid and water, and then putting the mixture in a closed container, reacting for at least 1 hour at least 160 DEG C, and carrying out solid-liquid separation, thus obtaining the organic-inorganic hybrid polyoxomolybdate crystal material. When being excited by ultraviolet light with the wavelength of 310nm, the organic-inorganic hybrid polyoxomolybdate crystal material emits relatively strong fluorescence at a place with the central wavelength of 410nm, which shows that the crystal material has good fluorescence characteristic.

Description

technical field [0001] The invention belongs to the field of organic-inorganic hybrid materials and complex crystal materials, in particular to an organic-inorganic hybrid polymolybdate crystal material and a preparation method thereof. Background technique [0002] Early transition metal atoms (vanadium, niobium, tantalum, molybdenum and tungsten) can form multi-metal-oxygen clusters in their high oxidation states. These substances often have excellent electrical conductivity, magnetic properties due to their unique molecular and electronic structures. , redox, catalytic and optical nonlinear properties, and has a wide range of applications in analysis, clinical diagnosis, catalysis (including photocatalysis), biochemistry, medicine and materials science. [0003] With the development of advanced materials, the assembly of supramolecular polyoxometallates with specific compositions and functions has attracted more and more attention. With the development of inorganic polym...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/54C30B7/10
Inventor 张全争江睿张雪珂何龙中汪兴汉鲁红典
Owner HEFEI UNIV
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