NaVO3-NH4Cl-H2O体系下NH4VO3溶析结晶工艺
Anti-solvent crystallization process of NH4VO3 in NaVO3-NH4Cl-H2O solution system
李春丽 1张焕焕 1程卓 1汤秀华 1张峰榛 1叶宇玲1
作者信息
- 1. 四川轻化工大学化学工程学院,四川自贡 643000
- 折叠
摘要
针对NH4VO3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NH4VO3溶析结晶工艺.以乙醇为溶析剂、NH4Cl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、NH4Cl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NH4Cl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、NH4Cl初始浓度、温度;在结晶时间为150 min、NH4Cl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NH4VO3产品,产品形貌为花簇状结构,尺寸为5～10 µm.
Abstract
The anti-solvent crystallization technology of NH4VO3was proposed to deal with the problems of long induction period and low product yield in the process of NH4VO3 cooling crystallization.By using ethanol as anti-solvent and NH4Cl as precipitator,the effects of volume ratio of ethanol-leaching solution,NH4Cl 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 NH4Cl.The influence of three factors on the product yield from high to low was volume ratio of ethanol-leaching solution,initial concentration of NH4Cl,temperature.The NH4VO3 products with yield greater than 95%were prepared un-der the conditions of crystallization time of 150 min,NH4Cl 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 5～10 µm.
关键词
溶析结晶/响应曲面法/偏钒酸铵/乙醇Key words
anti-solvent crystallization/response surface methodology/ammonium metavanadate/ethanol引用本文复制引用
基金项目
国家自然科学基金资助项目(21868014)
四川省科技厅项目(2022YFG0134)
出版年
2024
NETL
NSTL
万方数据