Vanadium nitride preparing method
A technology of vanadium nitride and vanadium chloride, applied in the electrolysis process, electrolysis components, etc., can solve the problems of limited application fields, high content of impurity elements, high production costs, etc., to reduce production costs, lower temperatures, and strong application prospects Effect
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[0016] The preparation method of vanadium nitride of the present invention, mixes vanadium oxide and carbonaceous reductant as anode, and carbon steel bar is as cathode, implements electrolysis in alkali metal / alkaline earth metal chloride molten salt system containing low-valent vanadium chloride, Nitrogen gas is fed under the cathode, and the vanadium metal precipitated at the cathode reacts with the nitrogen gas to form vanadium nitride. The electrolyte and the vanadium nitride are separated to obtain the vanadium nitride product.
[0017] Wherein, the vanadium oxide is at least one of vanadium trioxide and vanadium pentoxide, the carbonaceous reducing agent is graphite, petroleum coke or carbon black, and the carbonaceous reducing agent and vanadium oxide are in a C / O molar ratio of 1 :1 for mixing, that is, by molar ratio, C in the carbonaceous reducing agent:O in the vanadium oxide=1:1. In order to ensure the quality of the anode, the preferred mixing method is as follo...
Embodiment 1
[0028] Weigh 100gV 2 o 5 Powder (V 2 o 5 content 95%), -320 mesh graphite 31.6g (carbon content ≥ 99%), add 3wt% PVA binder and mix, press into a Ф25 material column, dry it in an oven at 120°C for more than 12h, and use it as Anode, carbon steel rod as cathode, NaCl-KCl-VCl at 720°C 2 System (NaCl and KCl molar ratio is 1:1, VCl 2 Concentration is 4.5wt%) to implement electrolysis, electrolysis condition is voltage 2.85V, anode current density is 0.2A / cm 2 , the cathode current density is 0.1A / cm 2 , the nitrogen flow rate is 1.5L / min, after electrolysis for 2 hours, remove the cathode and anode and cool down, take out the vanadium nitride and electrolyte that sink to the bottom of the electrolytic cell, wash and remove the electrolyte, and obtain 60g of the product with a particle size of 45-75μm, refer to According to the analysis method of GB / T20567-2006, the main components are analyzed as follows: V is 78.2%, N is 21.3%, C is 0.002%, P is 0.002%, S is 0.002%, and t...
Embodiment 2
[0030] Weigh 100gV 2 o 3 Powder ((V 2 o 5 content 95%), -320 mesh carbon black 25.3g (carbon content ≥ 90%), add 2wt% PVA binder and mix, press into a material column of Ф25, dry at 120°C in an oven for more than 12h, and use its As the anode, the carbon steel rod as the cathode, at 720°C NaCl-KCl-VCl 2 System (NaCl and KCl molar ratio is 1:1, VCl 2 Concentration is 4.5wt%) to implement electrolysis, electrolysis condition is voltage 2.85V, anode current density is 0.1A / cm 2 , the cathode current density is 0.15A / cm 2 , the nitrogen flow rate is 1.5L / min, after electrolysis for 2 hours, remove the anode and cathode and cool down, take out the vanadium nitride and electrolyte that sink to the bottom of the electrolytic cell, wash with water to remove the electrolyte, and obtain 51g of the product with a particle size of 38-70μm, refer to According to the analysis method of GB / T20567-2006, the main components are as follows: V is 77.9%, N is 20.8%, C is 0.003%, P is 0.004%...
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