高效制取磷酸二氢钾的优化中和法工艺研究
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摘要
以工业磷酸和碳酸钾为原料,在饱和磷酸二氢钾溶液中通过反应、蒸发、25℃结晶循环制取磷酸二氢钾产品,饱和磷酸二氢钾母液采用二氧化硅吸附剂吸附净化后重复使用。用磷钼蓝分光光度法及邻菲啰啉分光光度法分别对磷酸二氢钾产品中的磷及铁元素含量进行测定。结果表明:所得磷酸二氢钾产品具有较高的纯度以及较低的铁杂质含量;二氧化硅吸附剂的使用能够在较低的产率损耗下有效地降低产品中的杂质含量。对比传统的中和法,该方法具有流程短、操作简单、产品质量稳定、杂质含量低、耗水少、耗能低等明显的优势。
A method of the cyclical processing technology of preparing KH_2PO_4 product was proposed.Reaction,evaporation,and crystallization at 25 ℃,the whole process was carried out in medium of KH_2PO_4 saturated solution from purified industrial phosphoric acid and potassium carbonate.The saturated KH_2PO_4 solution could be reused after purification with the adsorbent of SiO_2.Phosphomolybdenum blue and phenanthroline spectrophotometries were adopted to determine the phosphorus and Fe content.Results showed that the product had high purity and low impurity content,and the SiO_2 adsorbent can effectively reduce the impurity content in the low yield loss.Compared with traditional neutralization methods,this process had less steps,simple operation,stable product quality,and low impurity content,and exhibited apparent advantages of less water and energy consumption.
A method of the cyclical processing technology of preparing KH_2PO_4 product was proposed.Reaction,evaporation,and crystallization at 25 ℃,the whole process was carried out in medium of KH_2PO_4 saturated solution from purified industrial phosphoric acid and potassium carbonate.The saturated KH_2PO_4 solution could be reused after purification with the adsorbent of SiO_2.Phosphomolybdenum blue and phenanthroline spectrophotometries were adopted to determine the phosphorus and Fe content.Results showed that the product had high purity and low impurity content,and the SiO_2 adsorbent can effectively reduce the impurity content in the low yield loss.Compared with traditional neutralization methods,this process had less steps,simple operation,stable product quality,and low impurity content,and exhibited apparent advantages of less water and energy consumption.
引文
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[24]祁极冰,刘有智,罗莹,等.邻菲啰啉分光光度法测定络合铁脱硫液中铁的含量[J].现代化工,2016,36(1):187-190.
[2]汪家铭.磷酸二氢钾生产现状与市场分析[J].上海化工,2010,35(11):31-37.
[3]谷利敏,孟新志,张燕玲,等.复分解法制备磷酸二氢钾的研究[J].河南化工,2002(10):11-12.
[4]谢英惠,刘景府,袁俊生,等.磷酸二氢钾的生产工艺[J].海湖盐与化工,2005,34(4):9-11.
[5]王东头,石香玉.磷酸二氢钾的生产方法综述[J].无机盐工业,2001,33(6):23-24.
[6]孙晓明,王新军,谢木香,等.磷酸二氢钾生产工艺研究[J].磷肥与复肥,2001,16(4):12-13.
[7]方进,周骏宏.湿法磷酸复盐结晶法制磷酸二氢钾[J].硫磷设计与粉体工程,2016(2):17-19.
[8]蒋彩丽,郑绍聪,郑远利,等.三辛胺-异戊醇有机溶剂萃取制备磷酸二氢钾[J].无机盐工业,2014,46(2):44-46.
[9]杨林,张志业,陈智勇.磷酸二氢钾的制备方法综述[J].磷肥与复肥,2004,19(1):54-56.
[10]陈路萍,樊继宽.湿法磷酸生产磷酸二氢钾新工艺[J].淮海工学院学报,2001(2):39-41.
[11]陈若愚,王国平,朱建飞,等.萃取法制备磷酸二氢钾新工艺研究[J].化工矿物与加工,2001(11):5-7.
[12]李海丽,曾波.萃取法生产磷酸二氢钾工艺[J].云南化工,2001,28(1):14-15.
[13]李春,徐世林,宿其.溶剂萃取法生产工业级磷酸二氢钾新工艺研究[J].无机盐工业,1997(3):14-16.
[14]张莉.液液离子交换法制备磷酸二氢钾过程的研究[D].上海:华东理工大学,2012.
[15]雷武.离子交换法制取磷酸二氢钾[J].磷肥与复肥,1995(3):33-34.
[16]陈红琼.磷酸二氢钾的制备方法[J].四川化工,2013,16(5):16-19.
[17]Linke W F,Seidell A.Solubility of inorganic and metal organic compounds[M].Washington:American Chemical Society,1965.
[18]孔素娟,袁菲,于旭博,等.3种磷含量测定方法的比较[J].中国生物制品学杂志,2014,27(10):1304-1308.
[19]李光明,万荣,李霞,等.饲料磷酸盐中磷含量的三种检测方法比较分析[J].饲料广角,2014(6):19-21.
[20]桑宏庆,于天宇,安乐.磷钼蓝分光光度法测定果蔬中有机磷[J].饮料工业,2011(1):30-34.
[21]桑宏庆,于天宇.磷钼蓝分光光度法测定果蔬中有机磷农药[J].饮料工业,2010(8):39-43.
[22]姚雪霞,戴存礼,李晓林,等.邻菲啰啉分光光度法测定微量铁实验条件的探讨[J].实验室研究与探索,2015,34(3):16-19.
[23]王新梅,郭然.邻菲啰啉分光光度法测定硝酸铵中铁离子含量[J].磷肥与复肥,2017,32(4):39-41.
[24]祁极冰,刘有智,罗莹,等.邻菲啰啉分光光度法测定络合铁脱硫液中铁的含量[J].现代化工,2016,36(1):187-190.