A kind of method for synthesizing manganese vanadate nanometer material

A technology for synthesizing nanometer and nanometer manganese vanadate, which is applied in the directions of nanotechnology, nanotechnology, chemical instruments and methods to achieve the effects of low temperature controllable preparation, controllable conditions and pure product

Active Publication Date: 2016-10-05
SHIJIAZHUANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] So far, about Mn 6.87 (OH) 3 (VO 4 ) 3.6 (V 2 o 7 ) 0.2 The research on nano-micro-materials has not been reported at home and abroad. However, for nano-materials, their composition, morphology and preparation methods are closely related to their performance, which is of great significance to the diversification of materials and potential functional diversification. It can be seen that , the development of manganese vanadate materials with different compositions and morphologies is in urgent need of a breakthrough in the field of materials

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  • A kind of method for synthesizing manganese vanadate nanometer material
  • A kind of method for synthesizing manganese vanadate nanometer material
  • A kind of method for synthesizing manganese vanadate nanometer material

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Embodiment 1

[0022] At room temperature, 2 mmol of sodium orthovanadate was dissolved in 6 mL of distilled water, and 1 mmol of MnSO 4 ·H 2 O was dissolved in 8 mL distilled water, and the sodium orthovanadate solution was added dropwise to the MnSO 4 solution, stirred for 10 min, with 1mol / L H 2 SO 4 The solution adjusted the pH value of the reaction system to 7, continued to stir for 10 min, then transferred it into a 20 mL hydrothermal reaction kettle, sealed it and placed it in a constant temperature box for 6 hours of hydrothermal reaction at 160 °C, and cooled to room temperature after the reaction , washed three times with deionized water and absolute ethanol respectively, centrifuged, and placed the resulting precipitate in an oven at 60 °C for 16 hours in vacuum to obtain manganese vanadate Mn 6.87 (OH) 3 (VO 4 ) 3.6 (V 2 o 7 ) 0.2 Material. The above product was analyzed by X-ray diffraction (XRD) and scanning electron microscope, and the results were as follows: figur...

Embodiment 2

[0024] At room temperature, 0.2 mmol of sodium orthovanadate was dissolved in 6 mL of distilled water, and 0.1 mmol of MnCl 2 Dissolved in 8mL distilled water, under the action of magnetic stirring, the sodium orthovanadate solution was added dropwise to the MnCl 2 solution, stirred for 10 min, adjusted the pH value of the reaction system to 8 with 1mol / L HCl solution, continued to stir for 10 min, then transferred to a 20 mL hydrothermal reactor, sealed and placed in a constant temperature box Hydrothermal reaction at 180 °C for 4 hours, after the reaction was completed, cool to room temperature, wash with deionized water and absolute ethanol for 5 times, centrifuge, and place the resulting precipitate in an oven for 8 hours at 80 °C to obtain manganese vanadate Mn 6.87 (OH) 3 (VO 4 ) 3.6 (V 2 o 7 ) 0.2 The nanoparticle material is a spherical particle with a diameter of 30-60nm.

Embodiment 3

[0026] At room temperature, 2 mmol of sodium orthovanadate was dissolved in 6 mL of distilled water, and 2 mmol of MnCl 2 Dissolved in 8mL distilled water, under magnetic stirring, the sodium orthovanadate solution was added dropwise to the MnCl 2 solution, stirred for 10 min, with 1mol / L HNO 3 The solution adjusted the pH value of the reaction system to 8 and continued to stir for 10 min, then transferred it into a 20 mL hydrothermal reaction kettle, sealed it, and placed it in a thermostat for 22 h at 180 °C for hydrothermal reaction. After the reaction was completed, it was cooled to At room temperature, wash five times with deionized water and absolute ethanol respectively, centrifuge, and place the obtained precipitate in an oven at 80°C for 8 hours in vacuum to obtain manganese vanadate Mn 6.87 (OH) 3 (VO 4 ) 3.6 (V 2 o 7 ) 0.2 Material. The above product was analyzed by XRD analysis and scanning electron microscope, and the results were as follows: image 3 , ...

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Abstract

The invention discloses a manganese vanadate nano-micro material and a synthetic method and application thereof, belonging to the field of inorganic non-metallic materials. The composition of the nano-micro manganese vanadate material is Mn6.87(OH)3(VO4)3.6(V2O7)0.2, and the material is in the form of nanoparticle, microrod or microtube. The synthetic method comprises the following steps: preparing a mixed solution from sodium orthovanadate and manganese salt according to a mol ratio of V to Mn of 1-3: 1; adjusting the pH value of the mixed solution to be 7 to 8, carrying out stirring for 10 min, then transferring the mixed solution into a reaction vessel and carrying out a reaction at a temperature of 160 to 260 DEG C for 1 to 24 h so as to obtain the solution of a crude product; and cooling the solution of the crude product to room temperature and carrying out cooling and drying so as to obtain the manganese vanadate Mn6.87(OH)3(VO4)3.6(V2O7)0.2 nano-micro material. The invention has the following beneficial effects: the nano-micro material is synthesized by using a one-step hydrothermal method and a wet method, low-temperature controllable preparation of manganese vanadate is realized, and energy consumption is low; no surfactant or organic template is needed in the process of synthesis, so the synthetic method is friendly to the environment and the produced nano-micro material is pure and has excellent crystallization property; the nano-micro material has uniform morphology and size; and the synthetic method is simple, can be realized under controllable conditions, is suitable for batch production and lays a good foundation for application and research.

Description

technical field [0001] The invention belongs to the field of inorganic non-metallic materials, and in particular relates to a method for synthesizing manganese vanadate nano-micron materials. Background technique [0002] Manganese vanadate is an important inorganic material. According to the different proportions of manganese, vanadium and oxygen, manganese vanadate has many different compositions and structures. Such materials have good application prospects in electrical devices, optical devices and lithium-ion batteries due to their good electrical, optical and electrochemical properties. The traditional synthetic method of manganese vanadate is mainly high-temperature solid-state reaction, manganese vanadate powder with irregular shape can be prepared by high-temperature solid-phase method, the reaction process consumes a lot of energy, and the cycle is long, and the product is usually a block Bulk material, large and uneven in size. In recent years, with the continuo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G45/00H01M4/131H01M4/1391B82Y30/00
CPCY02E60/10
Inventor 张绍岩次立杰李中秋
Owner SHIJIAZHUANG UNIVERSITY
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