转盘塔内甲基异丁基酮萃取湿法磷酸实验研究

doi:10.19964/j.issn.1006-4990.2021-0106

摘要/Abstract

摘要：

溶剂萃取法是一种经济有效的湿法磷酸净化方法。在转盘塔中,以甲基异丁基酮（MIBK）为萃取剂,开展了净化湿法磷酸的实验研究。考察了搅拌转速、相比对磷酸萃取率、杂质离子选择性、洗涤效果和反萃效果的影响。研究结果表明：萃取过程适宜的相比（溶剂与磷酸的体积比）为4,搅拌转速为200~400 r/min,在此条件下磷酸萃取率为85%;洗涤过程的搅拌转速不应大于100 r/min,适宜的洗涤酸用量为溶剂相体积的10%~15%,在此条件下铁离子（Ⅲ）和镁离子脱除率均在90%以上、铝离子脱除率大于70%、硫酸根脱除率为50%~60%;反萃过程搅拌转速不应大于200 r/min,适宜的反萃水用量为溶剂相体积的9%~15%。MIBK对阳离子的脱除效果较好,但是对阴离子的脱除效果不佳。经过萃取、洗涤和反萃3个过程,磷酸收率为57.8%~70.3%,磷酸中铁离子（Ⅲ）含量可以达到工业级磷酸标准,但是硫酸根的含量无法达标,需要结合其他方法进一步脱除。

关键词: 湿法磷酸, 溶剂萃取, 甲基异丁基酮, 转盘塔

Abstract:

Solvent extraction is an economical and effective method for the purification of wet process phosphoric acid（WPA）. WPA extraction proces was carried out using methyl isobutyl ketone（MIBK） as an extractant in a rotating disc column （RDC）.The effect of rotation speed and phase ratio on the extraction rate,the selectivity coefficient of impurities,and phos-phoric acid washing and stripping was studied.The results showed that the optimum extraction ratio（volume ratio of solvent to phosphoric acid） was 4,the stirring speed was 200~400 r/min,and the extraction rate of phosphoric acid was 85%.The stir-ring speed in the washing process was limited to 100 r/min.The appropriate amount of washing acid was 10%~15% of the vol-ume of solvent phase.The removal rates of Fe³⁺ and Mg²⁺ were more than 90%.The removal rate of Al³⁺ was more than 70% and the removal rate of SO₄^2- was 50%~60%.The stirring speed of stripping process was limited to 200 r/min,and the appropriate amount of stripping water was 9%~15% of the volume of solvent phase.MIBK had good removal effect on cations,but poor re-moval effect on anions.After purification by extraction,washing and stripping,the yield of phosphoric acid was 57.8%~70.3%. The content of Fe³⁺ in phosphoric acid could meet the standard of industrial phosphoric acid,but the content of sulfate could not meet the standard,so it needs to be further removed in combination with other methods.

Key words: wet process phosphoric acid, solvent extraction, methyl isobutyl ketone, rotating disc column

中图分类号:

TQ126.35

赵远方,高有飞,杜招鑫. 转盘塔内甲基异丁基酮萃取湿法磷酸实验研究[J]. 无机盐工业, 2021, 53(12): 105-108.

ZHAO Yuanfang,GAO Youfei,DU Zhaoxin. Experimental research on purification of wet process phosphoric acid by methyl isobutyl ketone in rotating disc column[J]. Inorganic Chemicals Industry, 2021, 53(12): 105-108.

图/表 7

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参考文献 13

[1]	张俊, 韩喜超, 潘继斐, 等. 国内湿法磷酸净化技术的工业化应用[J]. 磷肥与复肥, 2020, 35(11):30-31.
[2]	王辛龙, 许德华, 钟艳君, 等. 中国磷化工行业60 年发展历程及未来发展趋势[J]. 无机盐工业, 2020, 52(10):9-17.
[3]	田文航, 张才华, 陈元辉, 等. 溶剂萃取法湿法磷酸净化技术应用现状[J]. 磷肥与复肥, 2019, 34(3):24-26.
[4]	李善华, 胡巧, 张小元. 甲基异丁酮溶剂萃取湿法磷酸净化研究进展[J]. 磷肥与复肥, 2020, 35(5):31-32.
[5]	张文静. 盐酸法湿法磷酸净化工艺研究[D]. 贵阳:贵州大学, 2019.
[6]	FEKI M, FOURATI M, CHAABOUNI M M, et al. Purification of wet process phosphoric acid by solvent extraction liquid-liquid equilib- rium at 25 ℃ and 40 ℃ of the system water-phosphoric acid-methyliso- butylketone[J]. The Canadian Journal of Chemical Engineering, 1994, 72(5):939-944. doi: 10.1002/cjce.v72:5
[7]	FEKI M, AYEDI H F. Purification of wet process phosphoric acid by solvent extraction with methyl isobutyl ketone:Systematic study of impurity distribution[J]. Separation Science and Technology, 1998, 33(16):2609-2622. doi: 10.1080/01496399808545322
[8]	FEKI M, STAMBOULI M, PAREAU D, et al. Study of the multi- component system wet process phosphoric acid-methyl isobutyl ke- tone at 40 ℃ phase equilibria and extraction performances[J]. Chemical Engineering Journal, 2002, 88(1/2/3):71-80. doi: 10.1016/S1385-8947(01)00246-7
[9]	许惕非. 湿法磷酸净化制取食品级磷酸工艺的研究[D]. 上海:华东理工大学, 2006.
[10]	张志强, 张彩棉, 孙滢博, 等. 甲基异丁基酮净化湿法磷酸的研究[J]. 无机盐工业, 2014, 46(7):20-22.
[11]	冉瑞泉, 冯云飞, 颜克春. 溶剂萃取法净化湿法磷酸萃取率的影响因素研究[J]. 磷肥与复肥, 2015, 30(8):16-17.
[12]	黄美英, 杨三可, 李军, 等. 溶剂萃取法净化湿法磷酸的工艺研究[J]. 磷肥与复肥, 2004, 19(4):9-11.
[13]	倪双林, 方晓峰, 王志刚, 等. 复合溶剂萃取净化湿法磷酸[J]. 云南化工, 2017, 44(10):42-45.

组分	质量分数/%	组分	质量分数/%
P₂O₅	50.02	Fe³⁺	0.36
SO₄^2-	4.96	Al³⁺	0.13
Mg²⁺	1.34

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