有机胺萃取法制备硝酸钾的工艺研究
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摘要
以硝酸以及氯化钾为原料,以二正丁胺为有机萃取剂,通过萃取法制备硝酸钾。首先将硝酸和氯化钾放入250 mL烧杯中,加入定量的水,搅拌并加热至80℃,停止加热。称取56.05 g二正丁胺,缓慢加入溶液中,反应一段时间后,生成白色细小的晶体,持续搅拌30min。将溶液静置降温至室温,抽滤分离出溶液底部的晶体,将晶体用无水乙醇洗涤3遍后,放入110℃烘箱中烘干2 h,得到产品。抽滤分离的滤液加入浓氨水,立即产生白色絮状不溶物,搅拌15min,静置分层,上层有机相即为二正丁胺,可回收循环利用。
Potassium nitrate was prepared from nitric acid and potassium chloride by extraction with dibutylamine as organic extractant. Firstly, nitric acid and potassium chloride were put into 250 mL beaker, and a certain amount of water was added. Then they were stirred and heated to 80 ℃. The heating was stopped. 56.05 g Dibutylamine was weighed and slowly added into the solution. After a period of reaction, fine white crystals were formed and stirred continuously for 30 min.The crystals at the bottom of the solution were filtered and separated. The crystals were washed three times with absolute ethanol and then dried in an oven at 110 ℃ for 2 h to obtain the product. When concentrated ammonia water was added to the filtrate, the white flocculent insoluble substance was produced immediately, it was stirred for 15 min and layered statically.The upper organic phase was di-n-butylamine which can be recycled. The effect of water consumption under experimental conditions, the amount of extractant dibutylamine and cooling methods on product yield and Cl-content was analyzed.
Potassium nitrate was prepared from nitric acid and potassium chloride by extraction with dibutylamine as organic extractant. Firstly, nitric acid and potassium chloride were put into 250 mL beaker, and a certain amount of water was added. Then they were stirred and heated to 80 ℃. The heating was stopped. 56.05 g Dibutylamine was weighed and slowly added into the solution. After a period of reaction, fine white crystals were formed and stirred continuously for 30 min.The crystals at the bottom of the solution were filtered and separated. The crystals were washed three times with absolute ethanol and then dried in an oven at 110 ℃ for 2 h to obtain the product. When concentrated ammonia water was added to the filtrate, the white flocculent insoluble substance was produced immediately, it was stirred for 15 min and layered statically.The upper organic phase was di-n-butylamine which can be recycled. The effect of water consumption under experimental conditions, the amount of extractant dibutylamine and cooling methods on product yield and Cl-content was analyzed.
引文
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[2]王恒磊,姜媛媛,刘亭,等.复分解法生产硝酸钾新工艺研究[J].无机盐工业,2017,49(11):48-49+68.
[3]王惠娥,沈瑞琪,叶迎华,等.石墨/硝酸钾的热行为及分解反应动力学研究[J].含能材料,2012,20(6):731-734.
[4]朱秀丽.浅析离子交换法制备硝酸钾工艺[J].盐科学与化工,2017,46(5):43-45.
[5]张罡,汤可攀,董朝领,等.提高硝酸钾生产中产品结晶率研究[J].山东化工,2017,46(6):38-39+42.
[6]陈坤,时爽,徐保明,等.氯化钾-硝酸铵复分解法制备硝酸钾工艺进展[J].化肥工业,2016,43(6):71-74.
[7]李树民,贾国安,吴亚洲,等.硝酸钾生产工艺及研究进展概述[J].山东化工,2016,45(15):70-72.
[8]郭举,刘美霞,杨帆,等.二甲基亚砜工业废渣制备农用硝酸钾的研究[J].无机盐工业,2018,50(10):42-44.
[9]马明德.硝酸钾生产工艺及原料技术路线[J].化工管理,2016(12):155.
[10]段正康,谢帆,张涛,等.硝酸钾生产工艺概述及复分解法存在的问题与对策[J].无机盐工业,2015,47(5):4-8.
[11]张罡.我国硝酸钾生产工艺及装置概述[J].化肥工业,2011,38(2):7-12.
[12]杨意望,陈松,李国兵.溶剂萃取法制取硝酸钾综述[J].化学工程与装备,2007(5):63-66+52.
[13]李雅芙,刘素芹.硝酸钾生产工艺综述[J].海湖盐与化工,2005(3):27-30.
[14]刘志云,孙蔓莉.中国产氯化钾在农用硝酸钾生产中的应用研究[J].无机盐工业,2005,37(2):50-51+54.
[15]张沂圭,王增平.连续式离子交换法生产硝酸钾[J].硫磷设计与粉体工程,2000(1):30-32.