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zn 2 (oh) 3 vo 3 Preparation method of microspheres

A technology of microspheres and mixed liquids, applied in chemical instruments and methods, inorganic chemistry, vanadium compounds, etc., can solve the problems of high energy consumption, no literature reports on microspheres, and difficult control of product shape, etc., and achieve low energy consumption , Excellent luminous performance, easy to control the shape of the effect

Inactive Publication Date: 2017-03-22
BOHAI UNIV
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Problems solved by technology

[0003] Zn with different morphology 3 (VO 4 ) 2 and Zn 3 (OH) 2 V 2 o 7 2H 2 There have been some reports on O micro / nano materials, such as Pei Lizhai "A method for preparing zinc vanadate nanorods (ZL201310074973.5), Guo Hongxu, etc. "Preparation and application of zinc pyrovanadate hollow microspheres" (ZL201210512067. 4), Li Chunsheng et al. "A Method for Synthesizing Zinc Vanadate Micro / Nanowire Materials by Hydrothermal Method" (ZL201110038566.X), Qin Xinying et al. "(Zn 3 (VO 4 ) 2 Preparation of microspheres and their light absorption properties” (Acta Synthetic Crystallography, 2014, 43 (4): 875-879), and about Zn 2 (OH) 3 VO 3 However, there are few reports on the synthesis and fluorescence properties of Zn, Kou Junjiao et al. 2 (OH) 3 VO 3 :Eu 3+ Hydrothermal synthesis and luminescent properties of nanocrystals" (Materials Review, 2015, 29 (5) 14-17) Using zinc nitrate and sodium metavanadate as raw materials, Zn nanocrystals doped with europium ions were synthesized by hydrothermal method. 2 (OH) 3 VO 3 Nanocrystalline
These preparation methods have problems such as the need to continue high-temperature heat treatment after hydrothermal treatment, high energy consumption, and difficult control of product morphology, especially due to the structural diversity of vanadate, the synthesis of Zn with controllable morphology. 2 (OH) 3 VO 3 Micro-nano materials are of great significance
[0004] Zinc metavanadate Zn 2 (OH) 3 VO 3 There is no relevant literature report for microspheres

Method used

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preparation example Construction

[0028] The present invention proposes a kind of preparation method of spherical zinc metavanadate, it is characterized in that: the method step is as follows:

[0029] (1) At room temperature, prepare 0.1 mol -0.3 mol / L NaVO respectively 3 and Zn(NO 3 ) 2 Aqueous solution; this setting can avoid the low yield of less than 0.1 mol / L, and more than 0.3 mol / L is likely to cause product impurity due to local overconcentration.

[0030] (2) According to the ratio of material mass ratio of n(Zn):n(V)=2:1, take NaVO 3 and Zn(NO 3 ) 2 solution, mixed and stirred to obtain a mixed solution.

[0031] (3) According to the ratio of water to ethylene glycol volume ratio of 1:2, add ethylene glycol to the mixed solution, and adjust the pH value of the above reaction system to 4-6 to obtain a precursor solution; set the pH to 4 -6 can get a spherical product, otherwise it is a flake product.

[0032] (4) Transfer the precursor solution obtained in step (3) to a reaction kettle and se...

Embodiment 1

[0037] At room temperature, prepare 0.1 mol / L NaVO 3 and Zn(NO 3 ) 2 Aqueous solution; take a certain amount of NaVO according to the mass ratio of n(Zn):n(V)=2:1 3 and Zn(NO 3 ) 2 Solution, mixed and stirred to obtain a mixed solution, according to the water / ethylene glycol volume ratio of 1:2, add ethylene glycol to the mixed solution. And use 1mol / l HCl solution or 1mol / L NaOH solution to adjust the pH value of the above reaction system to 4, transfer the precursor solution obtained above to a reactor with a filling degree of 80%, and react at 150°C for 48h. After the reactor was cooled to room temperature, the obtained precipitate was washed three times with distilled water, and then dried in an oven at 80 °C to obtain Zn particles with a diameter of about 8 μm. 2 (OH) 3 VO 3 Microspheres, whose Scanning Electron Microscope (SEM) image is shown in figure 2 shown.

Embodiment 2

[0039] At room temperature, prepare 0.3 mol / L NaVO 3 and Zn(NO 3 ) 2 Aqueous solution; take a certain amount of NaVO according to the mass ratio of n(Zn):n(V)=2:1 3 and Zn(NO3 ) 2 Solution, mixed and stirred to obtain a mixed solution, according to the water / ethylene glycol volume ratio of 1:2, add ethylene glycol to the mixed solution. And use 1mol / l HCl solution or 1mol / L NaOH solution to adjust the pH value of the above reaction system to 5, transfer the precursor solution obtained above to a reactor with a filling degree of 80%, and react at 170°C for 24h. After the reactor was cooled to room temperature, the obtained precipitate was washed three times with distilled water, and then dried in an oven at 80 °C to obtain Zn particles with a diameter of about 3.5 μm. 2 (OH) 3 VO 3 Microspheres, whose Scanning Electron Microscope (SEM) image is shown in image 3 shown.

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Abstract

The invention relates to a preparation method of Zn2(OH)3VO3 microspheres. The method uses NaVO3 and Zn(NO3)2 as raw materials, ethylene glycol as solvent, adjusts the pH value of the precursor solution to 4~6, and reacts for 16~48h under solvothermal conditions of 150~220°C to prepare Zn2(OH)3VO3 microspheres with a diameter of about 4-8μm. The method of the invention has the advantages of simple equipment, mild conditions of the solvothermal method, simple operation, controllable composition and purity, etc., and conforms to the new idea of ​​green chemistry. Eu3+-doped Zn2(OH)3VO3 microspheres have a strong emission peak at 610-620 nm under excitation at a wavelength of 295 nm, and have excellent luminescence properties. They are good light-converting materials for ultraviolet light excitation and visible light emission.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic functional micro-nano materials, and mainly relates to a preparation method of spherical zinc metavanadate, especially Zn 2 (OH) 3 VO 3 Solvothermal synthesis method of microsphere luminescent material. Background technique [0002] Zinc vanadate micro / nano materials have gradually attracted the attention of researchers due to their good fluorescence and photocatalytic properties, and they are photoluminescent and photocatalytic materials with potential application value. [0003] Zn with different morphology 3 (VO 4 ) 2 and Zn 3 (OH) 2 V 2 o 7 2H 2 There have been some reports on O micro / nano materials, such as Pei Lizhai "A method for preparing zinc vanadate nanorods (ZL201310074973.5), Guo Hongxu, etc. "Preparation and application of zinc pyrovanadate hollow microspheres" (ZL201210512067. 4), Li Chunsheng et al. "A Method for Synthesizing Zinc Vanadate Micro / Nanowire Materials...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/00C09K11/69
CPCC01G31/00C01P2002/72C01P2004/03C01P2004/32C01P2004/61C09K11/693
Inventor 刘连利寇俊娇刘玉静王莉丽崔岩张帆
Owner BOHAI UNIV