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Calcium vanadate microsphere material and its preparation method and application

A technology of microspheres and calcium vanadate, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., to achieve the effects of strong ultraviolet-visible light absorption, rich material fields, and mild reaction conditions

Inactive Publication Date: 2018-01-12
SHIJIAZHUANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In recent years, with the rapid development of nanotechnology, three-dimensional hierarchical structure nano / micro materials composed of low-dimensional nano-sized units have shown more excellent physical and chemical properties due to the coupling benefits and synergistic benefits generated by a single combination of nanostructures. characteristics, gradually attracted extensive attention of researchers, making it an important frontier research field in the world, however, the prior art has not reported the Ca with three-dimensional hierarchical structure 2 V 2 o 7 microsphere

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  • Calcium vanadate microsphere material and its preparation method and application
  • Calcium vanadate microsphere material and its preparation method and application
  • Calcium vanadate microsphere material and its preparation method and application

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Embodiment 1

[0027] At room temperature, 2 mmol of sodium orthovanadate was dissolved in 10 mL of distilled water, and 1 mmol of CaCl 2 Dissolved in 8mL distilled water, under magnetic stirring, the sodium orthovanadate solution was added dropwise to the CaCl 2 solution, stirred for 10 min, with 1mol / L HNO 3 The solution adjusted the pH value of the reaction system to 10, continued to stir for 10 min, then transferred it into a 25 mL hydrothermal reaction kettle, sealed it and placed it in a constant temperature box for 12 hours of hydrothermal reaction at 180 °C, and cooled to room temperature after the reaction , were centrifuged and washed 5 times with deionized water and absolute ethanol, and the resulting precipitate was dried in an oven at 80 °C for 8 hours to obtain Ca 2 V 2 o 7 microsphere material. The above product was subjected to X-ray diffraction (XRD) analysis, figure 1 It is an XRD spectrum, and the result shows that the product diffraction peak is related to Ca 2 V 2...

Embodiment 2

[0029] At room temperature, 2 mmol of sodium orthovanadate was dissolved in 7 mL of distilled water, and 1 mmol of CaCl 2 Dissolve in 9mL distilled water, and add sodium orthovanadate solution dropwise to CaCl under magnetic stirring 2 solution, stirred for 10 min, with 1mol / L HNO 3 The solution adjusts the pH value of the reaction system to 9 and continues to stir for 10 min, then transfers it into a 20 mL hydrothermal reaction kettle, seals it, and places it in a thermostat for 6 hours of hydrothermal reaction at 160 °C, and cools to room temperature after the reaction is completed , were centrifuged and washed five times with deionized water and absolute ethanol, and then dried in an oven at 80 °C for 12 hours to obtain Ca 2 V 2 o 7 microsphere material. XRD spectrum ( image 3 ) results show that the product diffraction peaks are closely related to Ca 2 V 2 o 7 match. SEM analysis was performed at a higher magnification ( Figure 4 ) indicates that the product ha...

Embodiment 3

[0031] At room temperature, 1 mmol of sodium orthovanadate was dissolved in 7 mL of distilled water, and 1 mmol of CaCl 2 Dissolved in 7mL of distilled water, under the action of magnetic stirring, the sodium orthovanadate solution was added dropwise to the CaCl 2 solution, stirred for 10 min, with 1mol / L HNO 3 The solution adjusted the pH value of the reaction system to 10 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 48 h at 160 °C for hydrothermal reaction. After the reaction was completed, it was cooled to At room temperature, the obtained precipitate was washed 6 times with deionized water and then washed 5 times with absolute ethanol, and then the obtained precipitate was placed in an oven at 80 °C for 8 h in vacuum to obtain Ca 2 V 2 o 7 microsphere material. SEM analysis ( Figure 5 ) indicates that the diameter of the microsphere is 0.5-1.0 μm, and the surface of each ...

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Abstract

The invention discloses a calcium vanadate microsphere material and a preparation method thereof. The chemical composition of the calcium vanadate microsphere is Ca2V2O7. The calcium vanadate microsphere is assembled from nanoparticles, has a three-dimensional hierarchical structure, and has a diameter of 0.5 to 2 μm. Its preparation method includes: 1. soluble calcium salt and sodium orthovanadate are formulated into a mixed solution according to the Ca:V molar ratio of 1:1~3; React at 200°C for 2 to 48 hours to obtain a solution of the crude product; ③cool the solution of the crude product obtained in step ② to room temperature, wash and dry the obtained precipitate to obtain the calcium vanadate microsphere material. The present invention has prepared pure-phase Ca2V2O7 microsphere materials with a three-dimensional hierarchical structure for the first time. The present invention adopts one-step hydrothermal method and wet method synthesis, with mild reaction conditions, simple process, controllable conditions, and suitable for mass production, laying a good foundation for application research. technical foundation.

Description

technical field [0001] The invention belongs to the field of inorganic nanometer materials and preparation methods thereof, and in particular relates to a calcium vanadate microsphere material with a three-dimensional hierarchical structure, a preparation method and application thereof. Background technique [0002] Calcium vanadate is an inorganic compound with excellent chemical stability, heat resistance and good crystallization properties. The application prospect has aroused people's extensive research interest. According to the different ratios of Ca, V, and O in the material, a variety of calcium vanadate materials with different compositions and structures can be obtained. At present, the research on calcium vanadate materials mainly includes CaV 2 o 6 , Ca 2 V 2 o 7 , Ca 10 V 6 o 25 Wait. Among them, about Ca 2 V 2 o 7 There are few research reports on nano and micro materials, only a small amount about Ca 2 V 2 o 7 The high-temperature solid-phase m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/00
CPCC01G31/00C01P2002/72C01P2002/84C01P2004/03C01P2004/32C01P2004/50C01P2004/61C01P2004/62
Inventor 张绍岩侯梦华候玲玲
Owner SHIJIAZHUANG UNIVERSITY
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