Ting Pu , Zanhong Chen , Yinliang Liu , Haodong Hu , Yong Liang
{"title":"影响通过 NaHSO4-H2O 焙烧、水/氨浸出和蒸发结晶从黑钨矿((铁、锰)WO4)精矿制备的准钨酸铵(APT)纯度的因素","authors":"Ting Pu , Zanhong Chen , Yinliang Liu , Haodong Hu , Yong Liang","doi":"10.1016/j.hydromet.2025.106467","DOIUrl":null,"url":null,"abstract":"<div><div>Traditional alkaline decomposition process for tungsten ore is facing significant challenges, including release of large amounts of hazardous waste and lengthy procedures. A previously proposed novel process for scheelite using NaHSO<sub>4</sub>·H<sub>2</sub>O roasting yielded ammonium para-tungstate (APT) of high-purity. However, the applicability of this method to wolframite ((Fe, Mn)WO<sub>4</sub>) concentrate remains uncertain. In this work, the process of wolframite decomposition by NaHSO<sub>4</sub>·H<sub>2</sub>O roasting for the preparation of APT was systematically investigated. It was found that 98.6 % of the tungsten in wolframite can be converted into WO<sub>3</sub> under the conditions of 3.0 times the stoichiometric amount of NaHSO<sub>4</sub>·H<sub>2</sub>O, a roasting temperature of 650 °C and a roasting time of 120 min. The main phases in the roasted product were WO<sub>3</sub>, MnSO<sub>4</sub>, and 3Na<sub>2</sub>SO<sub>4</sub>·Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>. Additionally, the water leaching conditions for WO<sub>3</sub> enrichment of the roasted product were investigated. At a liquid–solid ratio of 6:1 mL/g, a stirring rate of 300 rpm, a leaching time of 180 min and a leaching temperature of 25 °C, the removal efficiencies of Fe and Mn in the roasted product were 96.5 % and 99.3 %, respectively. Consequently, the concentration of WO<sub>3</sub> in the water-leaching product (residue) enriched from 25.2 % to 93.1 %. Furthermore, at an ammonia concentration of 4 mol/L, a liquid–solid ratio of 4:1 mL/g, a dissolution temperature of 80 °C, and a stirring rate of 350 rpm, the leaching efficiency of WO<sub>3</sub> in the WO<sub>3</sub> enrichment reached 98.5 % after 120 min. Subsequently, an APT product of high purity was obtained through impurity removal and evaporation crystallization. Overall, the results showed that NaHSO<sub>4</sub>·H<sub>2</sub>O roasting method has a broad range of applications in the decomposition of tungsten ore.</div></div>","PeriodicalId":13193,"journal":{"name":"Hydrometallurgy","volume":"234 ","pages":"Article 106467"},"PeriodicalIF":4.8000,"publicationDate":"2025-03-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Factors affecting purity of ammonium para-tungstate (APT) prepared from wolframite ((Fe, Mn)WO4) concentrate by NaHSO4·H2O roasting, water/ammonia leaching and evaporation crystallization\",\"authors\":\"Ting Pu , Zanhong Chen , Yinliang Liu , Haodong Hu , Yong Liang\",\"doi\":\"10.1016/j.hydromet.2025.106467\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>Traditional alkaline decomposition process for tungsten ore is facing significant challenges, including release of large amounts of hazardous waste and lengthy procedures. A previously proposed novel process for scheelite using NaHSO<sub>4</sub>·H<sub>2</sub>O roasting yielded ammonium para-tungstate (APT) of high-purity. However, the applicability of this method to wolframite ((Fe, Mn)WO<sub>4</sub>) concentrate remains uncertain. In this work, the process of wolframite decomposition by NaHSO<sub>4</sub>·H<sub>2</sub>O roasting for the preparation of APT was systematically investigated. It was found that 98.6 % of the tungsten in wolframite can be converted into WO<sub>3</sub> under the conditions of 3.0 times the stoichiometric amount of NaHSO<sub>4</sub>·H<sub>2</sub>O, a roasting temperature of 650 °C and a roasting time of 120 min. The main phases in the roasted product were WO<sub>3</sub>, MnSO<sub>4</sub>, and 3Na<sub>2</sub>SO<sub>4</sub>·Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>. Additionally, the water leaching conditions for WO<sub>3</sub> enrichment of the roasted product were investigated. At a liquid–solid ratio of 6:1 mL/g, a stirring rate of 300 rpm, a leaching time of 180 min and a leaching temperature of 25 °C, the removal efficiencies of Fe and Mn in the roasted product were 96.5 % and 99.3 %, respectively. Consequently, the concentration of WO<sub>3</sub> in the water-leaching product (residue) enriched from 25.2 % to 93.1 %. Furthermore, at an ammonia concentration of 4 mol/L, a liquid–solid ratio of 4:1 mL/g, a dissolution temperature of 80 °C, and a stirring rate of 350 rpm, the leaching efficiency of WO<sub>3</sub> in the WO<sub>3</sub> enrichment reached 98.5 % after 120 min. Subsequently, an APT product of high purity was obtained through impurity removal and evaporation crystallization. Overall, the results showed that NaHSO<sub>4</sub>·H<sub>2</sub>O roasting method has a broad range of applications in the decomposition of tungsten ore.</div></div>\",\"PeriodicalId\":13193,\"journal\":{\"name\":\"Hydrometallurgy\",\"volume\":\"234 \",\"pages\":\"Article 106467\"},\"PeriodicalIF\":4.8000,\"publicationDate\":\"2025-03-26\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Hydrometallurgy\",\"FirstCategoryId\":\"88\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0304386X25000325\",\"RegionNum\":2,\"RegionCategory\":\"材料科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"METALLURGY & METALLURGICAL ENGINEERING\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Hydrometallurgy","FirstCategoryId":"88","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0304386X25000325","RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"METALLURGY & METALLURGICAL ENGINEERING","Score":null,"Total":0}
Factors affecting purity of ammonium para-tungstate (APT) prepared from wolframite ((Fe, Mn)WO4) concentrate by NaHSO4·H2O roasting, water/ammonia leaching and evaporation crystallization
Traditional alkaline decomposition process for tungsten ore is facing significant challenges, including release of large amounts of hazardous waste and lengthy procedures. A previously proposed novel process for scheelite using NaHSO4·H2O roasting yielded ammonium para-tungstate (APT) of high-purity. However, the applicability of this method to wolframite ((Fe, Mn)WO4) concentrate remains uncertain. In this work, the process of wolframite decomposition by NaHSO4·H2O roasting for the preparation of APT was systematically investigated. It was found that 98.6 % of the tungsten in wolframite can be converted into WO3 under the conditions of 3.0 times the stoichiometric amount of NaHSO4·H2O, a roasting temperature of 650 °C and a roasting time of 120 min. The main phases in the roasted product were WO3, MnSO4, and 3Na2SO4·Fe2(SO4)3. Additionally, the water leaching conditions for WO3 enrichment of the roasted product were investigated. At a liquid–solid ratio of 6:1 mL/g, a stirring rate of 300 rpm, a leaching time of 180 min and a leaching temperature of 25 °C, the removal efficiencies of Fe and Mn in the roasted product were 96.5 % and 99.3 %, respectively. Consequently, the concentration of WO3 in the water-leaching product (residue) enriched from 25.2 % to 93.1 %. Furthermore, at an ammonia concentration of 4 mol/L, a liquid–solid ratio of 4:1 mL/g, a dissolution temperature of 80 °C, and a stirring rate of 350 rpm, the leaching efficiency of WO3 in the WO3 enrichment reached 98.5 % after 120 min. Subsequently, an APT product of high purity was obtained through impurity removal and evaporation crystallization. Overall, the results showed that NaHSO4·H2O roasting method has a broad range of applications in the decomposition of tungsten ore.
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.