NaVO_(3)-NH_(4)Cl-H_(2)O体系下NH_(4)VO_(3)溶析结晶工艺  

Anti⁃solvent crystallization process of NH_(4)VO_(3) in NaVO_(3)-NH_(4)Cl-H_(2)O solution system

作　　者：李春丽 张焕焕 程卓 汤秀华 张峰榛 叶宇玲 LI Chunli;ZHANG Huanhuan;CHENG Zhuo;TANG Xiuhua;ZHANG Fengzhen;YE Yuling(School of Chemical Engineering,Sichuan University of Science&Engineering,Zigong 643000,China)

机构地区：[1]四川轻化工大学化学工程学院,四川自贡643000

出　　处：《无机盐工业》2024年第5期39-44,共6页Inorganic Chemicals Industry

基　　金：国家自然科学基金资助项目(21868014);四川省科技厅项目(2022YFG0134)。

摘　　要：针对NH_(4)VO_(3)冷却结晶过程中存在结晶诱导期长、结晶收率低等问题,提出了NH_(4)VO_(3)溶析结晶工艺。以乙醇为溶析剂、NH_(4)Cl为沉淀剂,在单因素实验基础上采用响应曲面法考察了乙醇-浸取液体积比、NH_(4)Cl初始浓度和温度3个因素对产品收率的影响,并得到预测产品收率的回归方程。研究结果表明:回归方程能较好地预测产品收率;3个因素中只有乙醇-浸取液体积比和NH_(4)Cl初始浓度之间存在显著的交互作用;3个因素对产品收率影响程度从高到低的顺序依次为乙醇-浸取液体积比、NH_(4)Cl初始浓度、温度;在结晶时间为150 min、NH_(4)Cl初始浓度为0.68 mol/L、温度为278.15~288.15 K、乙醇-浸取液体积比为(1.5∶1)^(2∶1)条件下可获得收率大于95%的NH_(4)VO_(3)产品,产品形貌为花簇状结构,尺寸为5~10μm。The anti-solvent crystallization technology of NH_(4)VO_(3)was proposed to deal with the problems of long induction period and low product yield in the process of NH_(4)VO_(3) cooling crystallization.By using ethanol as anti-solvent and NH_(4)Cl as precipitator,the effects of volume ratio of ethanol-leaching solution,NH_(4)Cl initial concentration and temperature on the product yield were investigated by response surface methodology based on single factor experiment and the regression equa-tion for predicting the product yield was obtained.The results showed that the regression equation could predict the product yield well.There was only a significant interaction between the volume ratio of ethanol-leaching solution and the initial con-centration of NH_(4)Cl.The influence of three factors on the product yield from high to low was volume ratio of ethanol-leaching solution,initial concentration of NH_(4)Cl,temperature.The NH_(4)VO_(3) products with yield greater than 95%were prepared un-der the conditions of crystallization time of 150 min,NH_(4)Cl initial concentration of 0.68 mol/L,temperature of 278.15~288.15 K and volume ratio of ethanol-leaching solution of(1.5∶1)~(2∶1).The product morphology was flower-like structure with the size of 5~10µm.

关 键 词：溶析结晶 响应曲面法 偏钒酸铵 乙醇 

分 类 号：TQ420.6[化学工程]