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基于单因素结合Box-Behnken法的钨酸铵蒸发结晶提纯
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作者单位:

1.中南大学 材料科学与工程学院;2.中南大学 资源加工与生物工程学院;3.郑州大学 材料科学与工程学院

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TF841.1

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国家重点研发计划(2022YFC2904900)


Ammonium tungstate evaporation crystallization purification based on single factor combined with Box-Behnken method
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1.School of Materials Science and Engineering,Central South University;2.School of Resource Processing and Bioengineering,Central South University;3.School of Materials Science and Engineering,Zhengzhou University

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    摘要:

    本文采用单因素+Box-Behnken响应曲面法对钨酸铵溶液蒸发结晶法除杂工艺进行优化,以制备更高纯度的仲钨酸铵(APT)。首先,以降低APT中四种杂质(Na、K、S、Mo元素)总含量为出发点,利用单因素法初步确定结晶温度、搅拌线速度、钨酸铵溶液初始浓度的优选范围。其次,通过Box-Behnken响应曲面法对APT的蒸发结晶除杂工艺进一步优化,研究三种因素对APT中四种杂质总量的相互影响。结果表明,三种因素对四种杂质总量的影响顺序为:钨酸铵溶液初始浓度>蒸发温度>搅拌线速度;较佳工艺条件为蒸发温度94℃,搅拌线速度1.25m/s,钨酸铵溶液初始浓度73g/L。该实验条件下,制备所得APT四种杂质总含量降低至39.351ppm,与响应曲面法模型的最优预测值的相对误差仅为4.11%,APT纯度达到4N;生成的APT晶体为伴生有少量碎晶的柱状长方体形貌,层状结构明显,粒径分布均匀,晶粒细化明显。

    Abstract:

    The single factor + Box-Behnken response surface method was used to optimize the impurity removal process of ammonium tungstate solution evaporation crystallization method to prepare higher purity ammonium paratungstate (APT). Firstly, in order to reduce the total content of four impurities (Na, K, S, Mo elements) in APT, the preferred range of crystallization temperature, stirring speed and initial concentration of ammonium tungstate solution was preliminarily determined by single factor method. Secondly, the evaporation crystallization impurity removal process of APT was further optimized by Box-Behnken response surface method, and the mutual influence of three factors on the total amount of four impurities in APT was studied. The results show that the order of influence of three factors on the total amount of four impurities is : initial concentration of ammonium tungstate solution > evaporation temperature > stirring speed ; the optimum process conditions were as follows : evaporation temperature 94 °C, stirring speed 1.25 m/s, initial concentration of ammonium tungstate solution 73 g/L. Under the experimental conditions, the total content of the four impurities in the prepared APT was reduced to 39.351 ppm, and the relative error with the optimal prediction value of the response surface method model was only 4.110 %, and the purity of APT reached 4N. The generated APT crystal is a columnar cuboid morphology with a small amount of broken crystals. The layered structure is obvious, the particle size distribution is uniform, and the grain refinement is obvious.

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肖来荣,李绍豪,赵小军,王馨悦,王子豪,蔡圳阳,陆乐康,刘赛男,李庆奎.基于单因素结合Box-Behnken法的钨酸铵蒸发结晶提纯[J].稀有金属材料与工程,,().[Xiao Lairong, Li Shaohao, Zhao Xiaojun, Wang Xinyue, Wang Zihao, Cai Zhenyang, Lu ekang, Liu Sainan, Li Qingkui. Ammonium tungstate evaporation crystallization purification based on single factor combined with Box-Behnken method[J]. Rare Metal Materials and Engineering,,().]
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  • 收稿日期:2024-09-23
  • 最后修改日期:2024-11-14
  • 录用日期:2024-11-18
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