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Calcium vanadate microsphere material and preparation method and application thereof

A technology of micro-spheres and calcium vanadate, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., to achieve the effects of suitable mass production, mild reaction conditions, and rich materials.

Inactive Publication Date: 2016-06-29
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 preparation method and application thereof
  • Calcium vanadate microsphere material and preparation method and application thereof
  • Calcium vanadate microsphere material and preparation method and application thereof

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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 10min, with 1mol / L HNO 3 The solution adjusts the pH value of the reaction system to 10, continues to stir for 10 minutes, then transfers it into a 25mL hydrothermal reaction kettle, seals it, and places it in a constant temperature box for 12 hours of hydrothermal reaction at 180°C. After the reaction is completed, cool it to room temperature, and use Deionized water and absolute ethanol were centrifuged and washed 5 times, 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 ...

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 10min, with 1mol / L HNO 3 The solution adjusts the pH value of the reaction system to 9 and continues to stir for 10 minutes, then transfers it into a 20mL hydrothermal reaction kettle, seals it, and places it in a constant temperature box for 6 hours of hydrothermal reaction at 160°C. After the reaction is completed, cool it to room temperature, and use After deionized water and absolute ethanol were centrifuged and washed 5 times, they were 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 ...

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 distilled water, under magnetic stirring, the sodium orthovanadate solution was added dropwise to the CaCl 2 solution, stirred for 10min, with 1mol / L HNO 3 The solution adjusts the pH value of the reaction system to 10 and continues to stir for 10 minutes, then transfers it to a 20mL hydrothermal reaction kettle, seals it, and places it in a constant temperature box for hydrothermal reaction at 160°C for 48 hours. After the reaction is completed, cool it to room temperature. The resulting precipitate was washed 6 times with deionized water and then washed 5 times with absolute ethanol, and then 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 0.5-1.0μm, and the surface of each microsphere is constructed by smaller partic...

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Abstract

The invention discloses a calcium vanadate microsphere material and a preparation method thereof.The chemical constitution of the calcium vanadate microsphere material is Ca2V2O7, calcium vanadate microspheres are assembled by nanoparticles and have a three-dimensional hierarchical structure, and the diameter ranges from 0.5 micrometer to 2 micrometers.The preparation method of the calcium vanadate microsphere material comprises the steps that 1, soluble calcium salt and sodium orthovanadate are prepared into a mixed solution according to the Ca-V mole ratio of 1:(1-3); 2, the pH of the mixed solution is regulated to be 9-10 through an acid solution, uniform stirring is performed, and then reacting is performed for 2-48 h at the temperature of 140 DEG C-200 DEG C to obtain a crude product solution; 3, the crude product solution obtained in the step 2 is cooled to room temperature, and an obtained precipitate is washed and dried to obtain the calcium vanadate microsphere material.According to the preparation method, the pure-phase Ca2V2O7 microsphere material with the three-dimensional hierarchical structure is prepared for the first time.The microsphere material is synthesized through a one-step hydrothermal method and a wet method, the reacting conditions are mild, the technology is simple, controllable in condition and suitable for batched production, and a good technical foundation is laid for application research.

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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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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