Method for preparing flake-shaped NH4V3O8 microcrystalline with microwave-ultrasonic method
A flaky, microwave technology, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve problems such as side reactions, low product purity, and difficult reactions, and achieve short reaction cycles, high purity, and improved The effect of electrochemical performance
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Embodiment 1
[0026] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in an appropriate amount of deionized water at 50°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate, and prepared NH 4 + The concentration is 0.10mol / L of NH 4VO 3 Solution, denoted as A solution;
[0027] 2) Use 4mol L -1 The hydrochloric acid solution adjusts the pH value of A solution to be 4.0, obtains B solution;
[0028] 3) Pour solution B into a four-neck round-bottom flask, then put the four-neck round-bottom flask into a microwave-ultraviolet-ultrasonic trinity synthesis extraction reaction apparatus, and fix it, and use direct temperature measurement (platinum resistance measurement) Temperature); the microwave-ultrasonic synthesis mode is used to make microwave and ultrasonic wave act on the solution simultaneously, wherein the power of microwave is controlled at 200W, and the power of ultrasonic wave is controlled at 600W. Select the temperature-time working mod...
Embodiment 2
[0031] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 60°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate, and prepared into NH 4 + The concentration is 0.20mol / L of NH 4 VO 3 Solution, denoted as A solution;
[0032] 2) Use 3mol L -1 The hydrochloric acid solution adjusts the pH value of A solution to be 4.5, obtains B solution;
[0033] 3) Pour solution B into a four-neck round-bottom flask, then put the four-neck round-bottom flask into a microwave-ultraviolet-ultrasonic trinity synthesis extraction reaction apparatus, and fix it, and use direct temperature measurement (platinum resistance measurement) temperature); the microwave-ultrasonic synthesis mode is used to make microwave and ultrasonic wave act on the solution at the same time, wherein the power of microwave is controlled at 300W, and the power of ultrasonic wave is controlled at 400W. Select the temperature-time working mode, turn on the mi...
Embodiment 3
[0039] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 55°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate, and prepared into NH 4 + The concentration is 0.12mol / L of NH 4 VO 3 Solution, denoted as A solution;
[0040] 2) Use 3mol L -1 The hydrochloric acid solution adjusts the pH value of A solution to be 5.0, obtains B solution;
[0041] 3) Pour solution B into a four-neck round-bottom flask, then put the four-neck round-bottom flask into a microwave-ultraviolet-ultrasonic trinity synthesis extraction reaction apparatus, and fix it, and use direct temperature measurement (platinum resistance measurement) temperature); the microwave-ultrasonic synthesis mode is used to make the microwave and ultrasonic wave act on the solution at the same time, wherein the power of the microwave is controlled at 300W, and the power of the ultrasonic wave is controlled at 300W. Select the temperature-time working mode, tu...
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