Experimental study on precipitation of ammonium metavanadate in NaVO3-H2O system by ammonium bicarbonate and ammonium carbonate
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摘要: 针对钒渣钠法提钒得到的NaVO3-H2O溶液体系,利用碳酸氢铵/碳酸铵作为铵盐,考察了沉淀pH值、沉淀温度、结晶时间、加铵系数对偏钒酸铵结晶效果的影响。结果表明:在一定范围内提高溶液的pH值(9.1~9.5),可以改善偏钒酸铵的结晶率;在温度15~27 ℃、结晶时间>3 h、加铵系数不小于2.9条件下,可实现偏钒酸铵结晶率>85%,经煅烧获得的五氧化二钒纯度>99.3%,满足YB/T 5304—2017质量标准要求。Abstract: For the NaVO3-H2O solution system obtained by extracting vanadium from vanadium slag by sodium method, the effects of precipitation pH value, precipitation temperature, crystallization time, ammonium addition coefficient on the crystallization of ammonium metavanadate were investigated using ammonium bicarbonate and ammonium carbonate as ammonium salt. The results show that the crystallization rate of ammonium metavanadate can be improved by increasing the pH value of the solution (9.1–9.5) in a certain range. Under the conditions of temperature 15–27 ℃, crystallization time >3 h and ammonium addition coefficient no less than 2.9, the crystallization rate of ammonium metavanadate is higher than 85%, and the purity of vanadium pentoxide obtained by calcination ammonium metavanadate is higher than 99.3%, meeting the requirements of YB/T 5304—2017 quality standard.
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表 1 沉钒原液主要成分
Table 1. Main components of vanadium precipitation solution
g/L V P Si Na 34.07 0.067 0.019 44.40 表 2 主要试验设备
Table 2. Main test equipment
设备 型号 厂家 智能数显恒温水浴锅 HH-5L 郑州长城科工贸有限公司 循环水式真空泵 SBH-3 郑州科泰实验设备有限公司 电动搅拌器 H2010-G 上海梅颖浦仪器仪表制造有限公司 贝意克马弗炉 MF-1100C 安徽贝意克设备技术有限公司 精密电子秤 MW-2002C 上海沪士电子有限公司 实验室pH计 PHSJ-3F 上海仪电科学仪器股份有限公司 表 3 pH沉钒试验偏钒酸铵主要成分
Table 3. Main components of ammonium metavanadate in pH vanadium precipitation test
样品名称 碳酸铵占比 w/% P NH4VO3 Si Na S 偏钒酸铵 0.0 <0.01 98.50 0.017 0.038 0.008 偏钒酸铵 0.2 <0.01 98.92 0.012 0.034 0.007 偏钒酸铵 0.4 <0.01 98.58 0.015 0.025 0.007 偏钒酸铵 0.6 <0.01 99.29 0.012 0.032 0.006 偏钒酸铵 0.8 <0.01 99.29 0.014 0.029 0.008 偏钒酸铵 1.0 <0.01 98.92 0.013 0.035 0.006 表 4 沉钒时间试验五氧化二钒主要成分
Table 4. Main components of vanadium pentoxide in vanadium precipitation time test
样品名称 沉钒时间 /h P /% Si /% Na /% S /% V2O5 /% 五氧化二钒 1.5 <0.01 0.031 0.048 0.011 99.42 五氧化二钒 2.0 <0.01 0.030 0.044 0.012 99.30 五氧化二钒 2.5 <0.01 0.033 0.043 0.014 99.53 五氧化二钒 3.0 <0.01 0.033 0.054 0.010 99.30 五氧化二钒 3.5 <0.01 0.031 0.062 0.011 99.53 五氧化二钒 4.0 <0.01 0.032 0.060 0.011 99.30 五氧化二钒 4.5 <0.01 0.030 0.046 0.013 99.44 五氧化二钒 5.0 <0.01 0.031 0.072 0.012 99.30 表 5 沉钒温度试验五氧化二钒主要成分
Table 5. Main components of vanadium pentoxide in temperature precipitation test
样品名称 沉钒温度 /℃ P /% Si /% Na /% S /% V2O5 /% 五氧化二钒 15 <0.01 0.033 0.064 0.014 99.42 五氧化二钒 18 <0.01 0.030 0.050 0.011 99.30 五氧化二钒 21 <0.01 0.033 0.039 0.010 99.76 五氧化二钒 24 <0.01 0.031 0.052 0.010 99.76 五氧化二钒 27 <0.01 0.034 0.044 0.015 99.64 五氧化二钒 30 <0.01 0.032 0.034 0.014 99.76 五氧化二钒 33 <0.01 0.031 0.029 0.012 99.53 五氧化二钒 36 <0.01 0.035 0.028 0.010 99.53 表 6 沉钒加铵系数试验五氧化二钒主要成分
Table 6. Main components of vanadium pentoxide in vanadium precipitation test with different ammonium addition
样品名称 加铵系数 P /% Si /% Na /% S /% V2O5 /% 五氧化二钒 1.7 <0.01 0.032 0.050 0.013 99.42 五氧化二钒 2.0 <0.01 0.034 0.052 0.016 99.64 五氧化二钒 2.3 <0.01 0.033 0.045 0.010 99.30 五氧化二钒 2.6 <0.01 0.035 0.042 0.012 99.76 五氧化二钒 2.9 <0.01 0.032 0.053 0.013 99.53 五氧化二钒 3.2 <0.01 0.035 0.046 0.011 99.53 -
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