蒸發(fā)溫度>攪拌線速度;較佳工藝條件為蒸發(fā)溫度94℃,攪拌線速度1.25m/s,鎢酸銨溶液初始濃度73g/L。該實驗條件下,制備所得APT四種雜質(zhì)總含量降低至39.351ppm,與響應(yīng)曲面法模型的最優(yōu)預(yù)測值的相對誤差僅為4.11%,APT純度達到4N;生成的APT晶體為伴生有少量碎晶的柱狀長方體形貌,層狀結(jié)構(gòu)明顯,粒徑分布均勻,晶粒細化明顯。"/>

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基于單因素結(jié)合Box-Behnken法的鎢酸銨蒸發(fā)結(jié)晶提純
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作者單位:

1.中南大學 材料科學與工程學院;2.中南大學 資源加工與生物工程學院;3.鄭州大學 材料科學與工程學院

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TF841.1

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國家重點研發(fā)計劃(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:

    本文采用單因素+Box-Behnken響應(yīng)曲面法對鎢酸銨溶液蒸發(fā)結(jié)晶法除雜工藝進行優(yōu)化,以制備更高純度的仲鎢酸銨(APT)。首先,以降低APT中四種雜質(zhì)(Na、K、S、Mo元素)總含量為出發(fā)點,利用單因素法初步確定結(jié)晶溫度、攪拌線速度、鎢酸銨溶液初始濃度的優(yōu)選范圍。其次,通過Box-Behnken響應(yīng)曲面法對APT的蒸發(fā)結(jié)晶除雜工藝進一步優(yōu)化,研究三種因素對APT中四種雜質(zhì)總量的相互影響。結(jié)果表明,三種因素對四種雜質(zhì)總量的影響順序為:鎢酸銨溶液初始濃度>蒸發(fā)溫度>攪拌線速度;較佳工藝條件為蒸發(fā)溫度94℃,攪拌線速度1.25m/s,鎢酸銨溶液初始濃度73g/L。該實驗條件下,制備所得APT四種雜質(zhì)總含量降低至39.351ppm,與響應(yīng)曲面法模型的最優(yōu)預(yù)測值的相對誤差僅為4.11%,APT純度達到4N;生成的APT晶體為伴生有少量碎晶的柱狀長方體形貌,層狀結(jié)構(gòu)明顯,粒徑分布均勻,晶粒細化明顯。

    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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肖來榮,李紹豪,趙小軍,王馨悅,王子豪,蔡圳陽,陸樂康,劉賽男,李慶奎.基于單因素結(jié)合Box-Behnken法的鎢酸銨蒸發(fā)結(jié)晶提純[J].稀有金屬材料與工程,,().[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
  • 錄用日期:2024-11-18
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