磷酸脲母液制备工业级磷酸二氢铵工艺研究
收稿日期: 2019-10-14
网络出版日期: 2020-04-22
Process study on preparation of industrial grade ammonium dihydrogen phosphate from urea phosphate mother liquor
Received date: 2019-10-14
Online published: 2020-04-22
湿法磷酸制备磷酸脲过程中会副产大量磷酸脲母液,母液含有金属杂质及五氧化二磷含量较高。采用溶剂萃取法回收磷酸脲母液中五氧化二磷制备工业级磷酸二氢铵(MAP),分别考察了包括萃取、洗涤、中和、精制、结晶等工艺流程对产品收率及纯度的影响,确定了最佳工艺条件:萃取相比(有机相与水相体积比)=3:1,萃取时间为5 min,萃取温度为50 ℃,洗涤相比(有机相与洗涤剂体积比)=10:1,中和pH为4.5,复合酸性萃取剂PO8皂化率为20%,精制相比(萃取剂与水相体积比)=1:1,浓缩比为1.36,结晶温度为30 ℃。在该条件下制备的工业级MAP纯度可达99.45%,母液中五氧化二磷回收率为85.34%。该工艺对环境友好,原料中五氧化二磷回收率高,具有较高的经济效益。
廖晓婷 , 李军 , 陈明 . 磷酸脲母液制备工业级磷酸二氢铵工艺研究[J]. 无机盐工业, 2020 , 52(4) : 79 -83 . DOI: 10.11962/1006-4990.2019-0333
In the process of preparing urea phosphate by wet process phosphoric acid,a large amount of urea phosphate moth-er liquor was by-produced,in which metal impurities and P2O5 were relatively high. Industrial grade MAP was prepared by us-ing the P2O5 recovered from the urea phosphate mother liquor through solvent extraction method.The effects of technological process including extraction,washing,neutralization,refining and crystallization on the yield and purity of product were in-vestigated.The optimum process conditions were confirmed: the extraction ratio(volume ratio of organic phase to aqueous phase)was 3:1,the extraction time was 5 min,the extraction temperature was 50 ℃,the washing ratio(volume ratio of organic phase to detergent)was 10:1,the neutralization pH=4.5,the saponification rate of compound acid extractant PO8 was 20%,the refining ratio(volume ratio of extract phase to aqueous phase) was 1:1,the concentration ratio was 1.36 and the crystalliza-tion temperature was 30 ℃.Under the optimum condition,industrial grade MAP with the purity of 99.45% was obtained and the P2O5 recovery rate in the mother liquor was 85.34%.The method had high economic benefits as its process was environmentally friendly,and the P2O5 recovery rate of raw materials and economic benefits were high.
Key words: urea phosphate; solvent extraction method; neutralization; crystallization; MAP
[1] | 罗珍 . 湿法磷酸溶剂萃取副产萃余酸制磷酸脲和磷镁肥实验研究[D]. 昆明:昆明理工大学, 2015. |
[2] | 周兆安, 唐瑜钟, 慎义勇 , 等. 化学抛光废磷酸处理方法和磷酸一铵的制备方法:中国, 107089650A[P]. 2017-08-25. |
[3] | 林晶, 党亚固, 费德君 , 等. 磷酸二氢铵结晶介稳区的研究[J]. 无机盐工业, 2007,39(10):21-23. |
[4] | Chen Ming, Li Jun, Jin Yang , et al. Efficient solvent extraction of phosphoric acid with dibutyl sulfoxide[J]. Journal of Chemical Tech-nology & Biotechnology, 2018,93(2):467-475. |
[5] | 杨楠, 李军 . 胺类萃取剂萃取湿法磷酸中硫酸根的研究[J]. 无机盐工业, 2019,51(3):41-44. |
[6] | 陈遵逵, 丁一刚, 龙秉文 , 等. 萃余酸制备工业级磷酸一铵的工艺优化[J]. 化学与生物工程, 2015,32(8):63-66. |
[7] | 李军, 金央, 罗建洪 , 等. 用湿法磷酸制工业磷酸二氢铵工艺综述[J]. 磷肥与复肥, 2016,31(5):17-18,43. |
[8] | 赵治华, 姜晓丽, 胡刚 . HEH[EHP]酸性络合萃取剂固体皂化性能研究[J]. 稀土, 2016,37(6):90-94. |
[9] | 陈德清, 王娜, 张敏 , 等. 湿法磷酸净化生产工业磷酸一铵研究[J]. 无机盐工业, 2016,48(1):38-40. |
[10] | 党亚固, 费德君, 林晶 . 湿法磷酸生产精细磷酸一铵结晶改善剂[J]. 无机盐工业, 2010,42(4):49-51. |
/
〈 |
|
〉 |