NaVO3-NH4Cl-H2O体系下NH4VO3溶析结晶工艺
收稿日期: 2023-07-13
网络出版日期: 2024-05-15
基金资助
国家自然科学基金资助项目(21868014);四川省科技厅项目(2022YFG0134)
Anti-solvent crystallization process of NH4VO3 in NaVO3-NH4Cl-H2O solution system
Received date: 2023-07-13
Online published: 2024-05-15
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。
李春丽 , 张焕焕 , 程卓 , 汤秀华 , 张峰榛 , 叶宇玲 . NaVO3-NH4Cl-H2O体系下NH4VO3溶析结晶工艺[J]. 无机盐工业, 2024 , 56(5) : 39 -44 . DOI: 10.19964/j.issn.1006-4990.2023-0371
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 equation 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 concentration 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 under 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.
| 1 | BARAN R， MILLOT Y， AVERSENG F，et al.Vanadium incorporation from aqueous NH4VO3 solution into siliceous Beta zeolite determined by NMR with formation of V-single site zeolite catalysts for application in SCR of NO［J］.Applied Catalysis A：General，2020，606：117830. |
| 2 | MAHTAB M， DAVOOD H， MEHDI B，et al.ZrCl4 or NH4VO3 as a versatile catalyst for the capable synthesis of xanthenediones and their corresponding theoretical studies［J］.Inorganic Chemistry Communications，2022，141：109582. |
| 3 | 官清，王远望，彭荣华，等.用偏钒酸铵制备偏钒酸钠工艺研究［J］.无机盐工业，2016，48（9）：57-60. |
| GUAN Qing， WANG Yuanwang， PENG Ronghua，et al.Study on preparation technology of sodium metavanadate with ammonium metavanadate［J］.Inorganic Chemicals Industry，2016，48（9）：57- 60. | |
| 4 | DENG Rongrui， XIAO Hao， XIE Zhaoming，et al.A novel method for extracting vanadium by low temperature sodium roasting from converter vanadium slag［J］.Chinese Journal of Chemical Engineering，2020，28（8）：2208-2213. |
| 5 | LI Hongyi， WANG Chengjie， LIN Minmin，et al.Green one-step roasting method for efficient extraction of vanadium and chromium from vanadium-chromium slag［J］.Powder Technology，2020，360：503-508. |
| 6 | 杜小旺，仲剑初，王孝天.高硅水镁石钠化焙烧法除硅工艺研究［J］.无机盐工业，2020，52（10）：92-95. |
| DU Xiaowang， ZHONG Jianchu， WANG Xiaotian.Study on removal of silicon from high-silicon brucite by sodium roasting method［J］.Inorganic Chemicals Industry，2020，52（10）：92-95. | |
| 7 | MENG Yuqi， WANG Xuewen， YANG Minge，et al.Recovery of Cr from vanadium-containing chromate solution with copper salt precipitation after V separation［J］.Hydrometallurgy，2019，188：157- 160. |
| 8 | LI Hailong， FENG Yali， WANG Hongjun，et al.Separation of V（Ⅴ） and Mo（Ⅵ） in roasting-water leaching solution of spent hydrodesulfurization catalyst by co-extraction using P507-N235 extractant［J］.Separation and Purification Technology，2020，248：117135. |
| 9 | ZHANG Yutao， ZHAO Ruzhen， ZHANG Xiaohuan，et al.A novel technology for producing high-purity V2O5 from hazardous vanadium-containing solutions using precipitation and solvent extraction［J］.Process Safety and Environmental Protection，2023，173：567-578. |
| 10 | YING Ziwen， HUO Manxing， WU Guixuan，et al.Recovery of vanadium and chromium from leaching solution of sodium roasting vanadium slag by stepwise separation using amide and EHEHPA［J］.Separation and Purification Technology，2021，269：118741. |
| 11 | 张焕焕，杜光文，吴然昊，等.Aliquat 336萃取提钒性能研究［J］.应用化工，2022，51（10）：2855-2858. |
| ZHANG Huanhuan， DU Guangwen， WU Ranhao，et al.Study on extraction properties of vanadium for Aliquat 336［J］.Applied Chemical Industry，2022，51（10）：2855-2858. | |
| 12 | WOLOWICZ A， HUBICKI Z.Removal of vanadium by ion exchange resins from model and real solutions from spent V2O5 catalyst［J］.Hydrometallurgy，2022，211：105871. |
| 13 | LI Hongyi， LI Cui， ZHANG Meng，et al.Removal of V（Ⅴ） from aqueous Cr（Ⅵ）-bearing solution using anion exchange resin：Equilibrium and kinetics in batch studies［J］.Hydrometallurgy，2016，165：381-389. |
| 14 | WANG Xuewen， WANG Mingyu， SHI Lihua，et al.Recovery of vanadium during ammonium molybdate production using ion exchange［J］.Hydrometallurgy，2010，104（2）：317-321. |
| 15 | 郭雪梅，王少娜，杜浩，等.碳酸氢铵溶液中偏钒酸铵的冷却结晶［J］.化工进展，2018，37（3）：853-860. |
| GUO Xuemei， WANG Shaona， DU Hao，et al.Cooling crystallization of ammonium metavanadate from ammonium bicarbonate solution［J］.Chemical Industry and Engineering Progress，2018，37（3）：853-860. | |
| 16 | 张峰榛，张焕焕，程卓，等.一种高纯偏钒酸铵晶体及制备方法：中国，114162865A［P］.2022-03-11. |
| 17 | 李锐，姜永华，张燕玲，等.基于响应曲面法优化硫酸铵结晶［J］.硅酸盐学报，2022，50（3）：782-790. |
| LI Rui， JIANG Yonghua， ZHANG Yanling，et al.Optimisation of ammonium sulphate crystallization based on response surface methodology［J］.Journal of the Chinese Ceramic Society，2022，50（3）：782-790. |
/
| 〈 |
|
〉 |
