一步法制备碳氮化钒的工艺优化试验

doi:10.13228/j.boyuan.issn0449-749x.20220434

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Abstract Focusing on the development of continuous,efficient and low-cost technology for the synthesis of vanadium carbonitride by one-step method,on the basis of summarizing the research on the production process of vanadium nitride,this paper takes vanadium pentoxide as the raw material,coke as reducing agent,after crushing,mixing and pressing into blocks,drying to reduce the nitride process. The optimum technological conditions for the preparation of vanadium carbonitride by one step carbothermal reduction at high temperature were investigated under high purity nitrogen atmosphere. The reduction process of vanadium pentoxide was thermodynamically analyzed and calculated,and the theoretical analysis was carried out by FactSage thermodynamic software. The single factor test analysis of reaction temperature,reaction time,nitrogen flow rate,pressure and other influencing factors was analyzed by XRD and SEM test methods. The results show that the nitriding reaction of vanadium carbide was carried out step by step,and the reaction process of vanadium carbonitride was V₂O₅→V₂O₄→V₂O₃→VC→VCN. The CO produced in the experiment will change the gas partial pressure in the furnace,which will affect the carbonization temperature and nitriding temperature. Therefore,the CO and N₂ partial pressure of the system should be strictly controlled in the reaction process. The reaction time and nitrogen flow rate had different effects on the contents of vanadium,nitrogen and carbon in the reaction products. The vanadium content and nitrogen content increased with the increase of reaction time and nitrogen flow rate,while the carbon content decreased with the increase of reaction time.The pressure determines the porosity of the reactants. On the basis of ensuring the quality of the block product,increasing the sample preparation pressure can increase the contact area between the particles and the specific surface area of the reaction,and the reduction effect is good. Considering comprehensively,setting the carbon distribution coefficient of 35%,sample preparation pressure of 20 MPa,carbothermal reduction at 900 ℃ and nitridation reaction at 1 480 ℃ for 180 min,the test can obtain (mass percent) 75.55%V,13.91%N,4.96%C of vanadium carbonitride products finally,in line with national standards.

Key words： vanadium pentoxide vanadium carbonitride direct reduction reaction temperature nitrogen

Received: 23 June 2022

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	YANG Shuang-ping
	ZHANG Tian-tian
	GAO Wen-bin
	LIU Shou-man
	SUN Hai-xing

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YANG Shuang-ping,ZHANG Tian-tian,GAO Wen-bin等. Experiment on process optimization of one-step preparation of vanadium carbonitride[J]. Iron and Steel, 2023, 58(1): 170-178.

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http://www.chinamet.cn/Jweb_gt/EN/10.13228/j.boyuan.issn0449-749x.20220434 OR http://www.chinamet.cn/Jweb_gt/EN/Y2023/V58/I1/170

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