Removal of calcium from phosphoric acid produced by the nitric acid process using solvent extraction with TCHDGA and stripping with water

IF 4.8 2区材料科学 Q1 METALLURGY & METALLURGICAL ENGINEERING

Hydrometallurgy Pub Date : 2024-07-30 DOI:10.1016/j.hydromet.2024.106379

Chengjin Xu , Miaomiao Zhang , Jianhui Su , Xiujing Peng , Xiangfeng Kong , Yanping Luo , Jiahui Sun , Yu Cui , Xuchuan Jiang , Guoxin Sun

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引用次数: 0

Abstract

The phosphoric acid produced by the nitric acid method cannot be used as an industrial-grade product as a result of the high calcium nitrate content. It can only be used for fertilizer production due to difficulty of complete removal of calcium nitrate. Herein, an efficient approach for the removal of calcium nitrate from the phosphoric acid produced by the nitric acid process was studied. The proposed process is based on solvent extraction with N, N, N′, N′-tetracyclohexyl-3-oxyglutaramide (TCHDGA). The effects of time, diluent, temperature, impurity ions, and the concentrations of extractant and nitric acid on the extraction of Ca²⁺ were considered. A series of characterization tests involving FT-IR spectroscopy, XPS analysis, slope analysis and X-ray single crystal diffracted analysis revealed that the stoichiometry of the complex is (Ca(NO₃)₂)(TCHDGA)₃. The concentration of Ca²⁺ in phosphoric acid drops below 5 mg/L a three-stage cross-current extraction process. The stripping efficiency of calcium nitrate in the organic phase by water is above 99.9%. The extraction efficiency of Ca²⁺ by TCHDGA remained above 96.8% after ten extraction-stripping cycles, realizing the efficient removal of calcium nitrate in the phosphoric acid produced by nitric acid process without changing the traditional production conditions.

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利用三氯二苯甲烷溶剂萃取和水汽提法去除硝酸法生产的磷酸中的钙

由于硝酸钙含量较高，硝酸法生产的磷酸不能用作工业级产品。由于难以完全去除硝酸钙，只能用于化肥生产。在此，研究了一种从硝酸法生产的磷酸中去除硝酸钙的有效方法。所提出的工艺基于 N，N，N′，N′-四环己基-3-氧戊二酰胺（TCHDGA）的溶剂萃取。考虑了时间、稀释剂、温度、杂质离子以及萃取剂和硝酸浓度对钙萃取的影响。通过一系列表征测试，包括傅立叶变换红外光谱、XPS 分析、斜率分析和 X 射线单晶衍射分析，发现复合物的化学计量为 (Ca(NO))(TCHDGA)。通过三级横流萃取工艺，磷酸中的钙浓度降至 5 mg/L 以下。水对有机相中硝酸钙的汽提效率高于 99.9%。经过十次萃取-剥离循环，TCHDGA 对 Ca 的萃取效率保持在 96.8%以上，在不改变传统生产条件的情况下，实现了对硝酸法生产的磷酸中硝酸钙的高效去除。

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来源期刊

Hydrometallurgy 工程技术-冶金工程

CiteScore

9.50

自引率

6.40%

发文量

144

审稿时长

3.4 months

期刊介绍： Hydrometallurgy aims to compile studies on novel processes, process design, chemistry, modelling, control, economics and interfaces between unit operations, and to provide a forum for discussions on case histories and operational difficulties. Topics covered include: leaching of metal values by chemical reagents or bacterial action at ambient or elevated pressures and temperatures; separation of solids from leach liquors; removal of impurities and recovery of metal values by precipitation, ion exchange, solvent extraction, gaseous reduction, cementation, electro-winning and electro-refining; pre-treatment of ores by roasting or chemical treatments such as halogenation or reduction; recycling of reagents and treatment of effluents.