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针对煤直接液化油渣(DCLR)，研究了采用溶剂萃取—空气焙烧—硫酸浸出—萃取剂萃取—反萃取工艺流程从中回收Mo和Fe。试验结果表明：经溶剂萃取后，DCLR上残留的有机化合物被高效脱除，得到含有残碳和灰分的煤液化油渣萃余物(ER)；再将ER在600～800℃下进行空气焙烧，可完全去除其中的残碳，使Mo和Fe富集在灰分中；对灰分用硫酸浸出，可有效浸出其中的Mo、Fe、Al等金属，Mo和Fe最高浸出率分别达93.10%和99.12%；酸浸液用三辛癸烷基叔胺(N235)萃取剂同时萃取Mo和Fe，但需加入助剂NaCl，以形成F和M等配阴离子，从而获得理想的萃取效果，优化的萃取工艺条件为NaCl添加量5%,N235∶仲辛醇∶煤油配比为3∶2∶5，氢离子浓度大于12mol/L，相比VO/VA在1/3～1/1之间，萃取时间大于2.5min，在该条件下，Mo单次萃取率最高达99.16%,Fe萃取率接近100%；用硫酸和氨水分步反萃负载有机相中的Fe和Mo，在整个萃取—反萃过程中的Fe回收率达97.90%Mo回收率达94.01%。该法可为煤直接液化催化剂中高值金属的回收提供一种可行的解决方案。
Abstract：A process of solvent extraction-air roasting-sulfuric acid leaching-extraction with extractant-stripping was studied for the recovery of Mo and Fe from direct coal liquefaction residue(DCLR).The results show that after solvent extraction,the residual organic compounds in DCLR are efficiently removed,and the coal liquefaction residue extractant residue(ER)containing residual carbon and ash is obtained.ER is then air-roasted at 600-800 ℃to completely remove the residual carbon,with Mo and Fe being enriched in the ash.The ash is leached with sulfuric acid to effectively extract Mo,Fe,Al,and other metals,with the highest leaching rates of Mo and Fe reaching 93.10%and 99.12%,respectively.The acid leaching solution is extracted with tri-n-octylamine(N235)extractant to simultaneously extract Mo and Fe,but NaCl is added to form complex anions such as Fand M,achieving an ideal extraction effect.The optimized extraction process conditions are NaCl addition of 5%,N235∶sec-octyl alcohol∶kerosene ratio of 3∶2∶5,and hydrogen ion concentration greater than 12 mol/L,phase ratio VO/V_Abetween 1/3 and 1/1,and extraction time greater than 2.5 min.Under the conditions,the single extraction rate of Mo is as high as 99.16%,and the extraction rate of Fe is close to 100%.Fe and Mo in the organic phase are sequentially stripped with sulfuric acid and ammonia,and the recovery rates of Fe and Mo in the entire extraction-stripping process are 97.90%and 94.01%,respectively.The method can provide a solution for the recovery of high-value metals in direct coal liquefaction catalysts.
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基本信息:
DOI：10.13355/j.cnki.sfyj.2026.02.014
中图分类号:TF56;TF841.2
引用信息:
[1]卢巍,单贤根,高巧利,等.煤直接液化油渣中钼铁回收技术研究[J].湿法冶金,2026,45(02):237-246.DOI:10.13355/j.cnki.sfyj.2026.02.014.
基金信息:
国家重点研发计划（2023YFB4103400）
2025-11-21
2025
2026-03-11
2026
2
2025-12-19
2025-12-19
2025-12-19