从氨性溶液中萃取分离铜、钴的研究

研究了不同萃取剂从氨性溶液中分离铜、钴的过程。采用LIX984N作萃取剂,经一级萃取,溶液中铜的萃取率大于99%;用180g/L硫酸溶液对负载有机相进行反萃,经二级逆流反萃,铜的反萃率达99%以上。采用LIX54-100作萃取剂,经过四级逆流萃取铜的萃取率达到99 53%;用30g/L硫酸溶液对负载有机相进行反萃,经一级反萃,铜的反萃率大于99 9%。在上述萃取过程中,钴均不被萃取。     

用N235从大洋多金属结核萃铜余液中萃取钴

研究了用N235从大洋多金属结核熔炼-锈蚀-萃取工艺中所产出的萃铜余液中萃取分离钴的方法。实验结果表明, N235萃取钴效果明显, 负载有机相中的钴能被稀酸反萃完全。采用N235萃取和稀酸反萃方法可以把Co(Ⅱ)、Ni(Ⅱ)分离开。从含钴0.85 g/L的料液中, 按相比V_O/V_A= 1/2, 经四级逆流萃取, 二级反萃可将钴富集到15.20 g/L, 萃余液中含钴0.0055 g/L, 萃余液中Ni/Co高达1 838, 反萃液中Co/Ni =1 520, 产品质量符合优质工业氯化钴质量要求, 钴镍萃取分离效果甚佳, 钴的回收率大于98%。     

富钴结壳浸出液中钴镍的N235萃取分离

对大洋富钴结壳硫酸活化浸出液经萃取分离铜、锌、锰后得到的镍钴富集溶液，用N235萃取分离镍钴。钴镍氯化物溶液用N235萃取分离的最佳的萃取工艺条件为室温，相比（O／A）=2～3：1。混合时间0．5min。经四级逆流萃取、洗涤与反萃。钴萃取率达99．99％，反萃率达99．81％，反萃液钴镍比达10^6。萃取分离后得到的氯化钴和氯化镍溶液纯度高，既可满足电解沉积金属的要求，又适于生产高纯化工产品。     

Cyanex272在镍钴分离中的应用

研究黑镍除钴渣酸溶后溶液用Cyanex272萃取钴,实现钴、镍的深度分离,并介绍其工业生产应用.试验结果表明混合时间3rnin,Co的萃取率可达98%以上;经2级萃取溶液中的Co2+由4.5降至0.01g/L以下;负载有机相经三级洗涤[Co]/[Ni]达到529.20;通过三级萃取,三级洗涤,钴的萃取率达99.90%以上,镍钴分离系数βCo/Ni为2.50×105;两级反萃使有机相含Co2+降至0.020g/L以下;采用去离子水二级洗涤,Cl-几乎100%被洗掉,不会进入硫酸镍溶液中循环积累.工业实践中黑镍除钴渣酸溶后溶液经P204萃取除铜、铁-Cyanex272萃取分离镍钴-氯化钴溶液草酸沉淀-草酸钴煅烧,产出的精制氧化钴粉达到国家Y1级标准,产出的硫酸镍溶液完全满足生产1#电镍的要求.     

高冰镍浸出液萃取净化流程

本文用一种新的磷类萃取剂５７０９对高冰镍硫酸选择性浸出液中的镍和钴、铜、铁、铅、锌等萃取性能进行了研究，确定了萃取净化分离的工艺条件。水相料液经过萃取后，萃余液达到１号电镍新液标准，镍收率大于９９％；负载钴等金属的有机相先用低酸反萃钴、铜、锌、铅镍后，再用３ｍｏｌ／Ｌ硫酸反萃除铁；除去金属后的有机相再用ＮａＯＨ溶液皂化复用。有机相在１０台φ２０ｍｍ离心萃取器组成的萃取回路试验中复用了７４次，证明性能稳定。     

用LIX 622从含砷铜／锌混合精矿加压浸出液中萃取铜

研究采用LIX622从含砷铜／锌混合精矿加压浸出液中萃取铜的工艺过程。含Cu10～15g／L，pH=1．0～1．2的加压浸出料液，采用22．58％LIX622-煤油体系，经过3级萃取、3级洗涤和3级反萃，萃余液中含铜可降到0．3～0．6g／L，平均铜萃取率达95．40％，反萃液满足电积工艺要求。     

P204/4PC协同萃取分离镍钴与镁钙的研究

采用新型协同萃取剂P204/4PC从含少量镍钴钙的硫酸镁溶液中选择性萃取镍和钴, 考察了萃取剂浓度、平衡pH值等因素对萃取分离效果的影响, 绘制了萃取、反萃取等温线, 并进行了串级模拟萃取-反萃取全流程实验。研究结果表明: P204/4PC协同萃取剂能从硫酸镁溶液中选择性萃取镍钴, 实现镍钴与钙镁的高效分离以及镍钴的高倍富集回收。模拟串级全流程实验结果显示, 对于含镍1.68 g/L、钴0.10 g/L、镁15.68 g/L和钙0.11 g/L的料液, 采用组成为0.25 mol/L P204+0.5 mol/L 4PC+磺化煤油的有机相经5级逆流萃取-1级洗涤-6级反萃取, 萃余液中镍和钴含量均小于0.01 g/L, 镍和钴萃取率均达到99.5%以上;反萃液中镍和钴浓度分别达到40.4 g/L和1.8 g/L, 杂质钙和镁浓度分别为0.02 g/L和0.09 g/L, 全流程钙镁除去率分别达到99.97%和99.36%。     

废电池合金制备氯化镍溶液的工艺研究

对用废旧电池熔铸的含镍废合金制备氯化镍溶液的工艺进行了研究.采用的工艺流程为:盐酸体系膜电解→化学沉淀法除杂→萃取除杂.通过该工艺流程获得的三级萃余液中镍含量大于30 g/L、铁为痕量、钴为0.51 g/L、铜含量小于0.0183 mg/L,该溶液可直接用于电镍生产.     

铜锌铁溶液萃取分离铜的试验研究

采用国产萃取剂N902从铜锌铁多金属矿浸出液中萃取分离Cu2+,考察了萃取剂体积浓度、萃取相比、振荡时间、萃取温度对铜萃取率的影响。在试验获得的较佳条件下对H2SO4含量为20.18g/L、30.38g/L的铜锌铁溶液分别进行3级逆流萃取,铜的萃取率分别为98.65%、96.50%,铜与锌、铁分离效果良好;以模拟电积后液为反萃原液进行四级逆流反萃,铜的反萃率约为88%,获得的反萃液可满足铜电积的要求。      

废旧三元锂电池正极材料回收镍、钴和锂

以废旧三元锂电池正极材料为原料,经湿法浸出、化学沉淀、萃取分离等工序,有效回收了废旧三元锂电池正极材料中的镍、钴和锂。首先考察了H2SO4和H2O2体系各因素对浸出效果的影响,通过单因素条件试验结果分析,确定了浸出最佳浸出条件为：浸出温度90℃,酸料比2:1,双氧水/料（mL/g）1.33,液固比（mL/g）10:1,浸出时间1h。在此条件下渣率低,镍、钴、锰和锂浸出率都能达到99%以上。浸出液用30%的NaOH溶液进行中和沉淀,时间2h,温度90℃,终点pH值3.7,除铁后液中铁的含量小于0.005g/L,镍、钴损失1%以下。除铁后液经P204萃取除锰-P507镍钴分离- P204萃镍制备镍、钴产品,萃余后的硫酸锂溶液经浓缩后再进行碳酸钠沉锂。     

Recovery of nickel and cobalt from leach solutions of nickel laterites using a synergistic system consisting of Versatic 10 and Acorga CLX 50

A direct solvent extraction (DSX) process to recover nickel and cobalt from laterite leach solutions is potentially more cost effective compared to the traditional precipitation and re-leaching method. A synergistic solvent extraction (SSX) system consisting of Versatic 10 and Acorga CLX 50 in ShellSol 2046 was studied for DSX nickel and cobalt recovery from a synthetic solution using semi-continuous tests. The effect of pH on the metal distribution profile and metal separation were investigated. It was found that the SSX system can effectively recover nickel and cobalt and separate them from manganese, calcium and magnesium. Over 99% of Ni and Co was extracted using four stages of semi-continuous extraction from the synthetic laterite solution at pH 6.3 and an A/O flowrate ratio of 1:1. More than 80% of the manganese was rejected to the raffinate. The co-extraction of calcium was less than 5% and the co-extraction of magnesium was negligible under these conditions. The co-extracted manganese and calcium were readily scrubbed in three stages semi-continuous scrubbing. The loaded strip liquor with a high concentration of nickel (71.3 g/L Ni) was obtained after two-stage continuous stripping. The final strip solution pH of 3 would be suitable for nickel electrowinning. A conceptual DSX process flowsheet using the SSX system to recover nickel and cobalt from laterite leach solutions after iron removal has been proposed.     

硫酸镍钴溶液中萃取除镉的试验研究

研究用萃取法从硫酸镍钴溶液中脱除镉。实验采用10 %N235 + 5 %TBP+85 %煤油的油相为萃取剂，稀硫酸为洗涤剂，氢氧化钠溶液为反萃剂。实验结果表明，萃取的最佳条件是：添加氯化钠的量为18 g/L，油水比为1:2、常温萃取5 min，三级逆流萃取率达99.4 %。反萃的最佳条件是：氢氧化钠溶液浓度为120 g/L、油水比为4:1、常温反萃5 min，反萃率达到98.0 %，实现了镉从硫酸镍钴溶液中脱除的目的。     

Cyanex 272萃取分离硫酸钴溶液中镍钴的试验研究

采用Cyanex 272萃取剂从硫酸钴溶液中分离去除镍,在有机相组成为25%Cyanex 272+75%航空煤油(用30%NaOH皂化,皂化率75%)、萃原液pH值4.5～5.0、温度25～35 ℃、相比1.5～2条件下,经5级逆流萃取,混合萃取时间5 min,然后用1 mol/L硫酸溶液4级反萃取获得反萃取液,钴直收率达99.86%,Ni去除率达95.20%,钴镍分离效果较好。反萃取后的硫酸钴溶液中杂质含量很低,Co/Ni比达368 95,可以满足生产精制CoSO₄·7H₂O和电钴的要求。     

从硫化镍矿浸出液中萃取分离铜的试验研究

对萃取方法从硫化镍矿浸出液中萃取分离铜进行了试验研究。结果表明:选取N902作萃取剂,经过两级萃取,铜萃取率平均为98.65%,镍萃取率平均为0.44%;用硫酸反萃,铜反萃率平均为99.54%;铜的回收率较高,可达98.20%。     

电镀污泥中铜的浸出和溶剂萃取回收研究

采用硫酸浸出-萃取-反萃工艺流程回收电镀污泥中的铜。运用MATLAB拟合了1 mol/L硫酸体系中铜的浸出动力学模型,表明该浸出过程为扩散和表面反应共同控制。在硫酸浓度1 mol/L、液固比15∶1条件下浸出10 min,铜浸出率达到90%。采用萃取-反萃取的方式回收浸出液中的Cu²⁺,以Mextral^® 984H为萃取剂、Mextral^® DT100为稀释剂,在溶液pH=2、萃取时间30 min、O/L相比1∶1、萃取剂浓度10%条件下萃取,铜萃取率可达99%;O/L相比1∶1、反萃取时间30 min,用25%的硫酸溶液进行反萃取,铜反萃取率可达95%。此工艺流程铜总回收率可达85%,实现了铜的高效回收。     

硅胶-聚合胺树脂在模拟硫酸镍电解液中深度净化除铜

用离子交换柱在Ni2+70g/L,Cu2+0.5～2.0g/L,pH=1～4,温度20℃～60℃的模拟硫酸镍电解液中研究硅胶-聚合胺树脂从硫酸镍电解液中深度净化除铜的过程.用H2SO4浓度分别为1.0,1.5,2.0mol/L的解析液考察树脂的解析性能.结果表明,随料液pH增大以及温度升高,树脂对铜的交换容量增大,料液Cu2+浓度对交换容量影响不大.最佳吸附条件为料液pH=4,吸附接触时间30min,温度60℃.最佳解析条件为H2SO42mol/L,解析接触时间40min.最佳工艺条件下,树脂的铜穿漏及饱和交换容量分别为0.378和0.496 mmol/mL-湿树脂,铜解析液峰值浓度可达38g/L以上.     

Recovery of copper,nickel and cobalt from acidic pressure leaching solutions of low-grade sulfide flotation concentrates

Recovery of copper, nickel and cobalt from the acidic pressure leaching solutions of Jinbaoshan (YN Province, PRC) low-grade sulfide flotation concentrates was investigated. The proposed technique includes four major steps: (1) the acidity adjustment of the acidic pressure leaching solutions; (2) solvent extraction (SX) separation of copper by organic reagent XD5640, and then stripped from the loaded organic phase by H₂SO₄ solution for copper recovery; then (3) iron in raffinates after copper extracting is selectively removed by high-temperature hydrolysis precipitation in an autoclave; and lastly (4) nickel and cobalt are selectively precipitated by Na₂S from the final solutions after removing iron. The experimental results for treating 1 L acidic leaching solutions per batch by this new technique were reported, and some evaluation and further comparisons with previous investigations were also carried out. It was reported that the total percent recovery of Cu could reach 95% or more, and that of Ni and Co were all more than 99%. In the processing, the percent removal of impurities, such as Fe, Mg and Ca, were all also near to 99%.     

Selective extraction of nickel from ammoniacal solutions containing nickel and cobalt by emulsion liquid membrane using 5,7-dibromo-8-hydroxyquinoline (DBHQ) as extractant

The selective extraction and concentration of nickel from ammoniacal solutions containing nickel and cobalt by an emulsion liquid membrane (ELM) technique using 5,7-dibromo-8-hydroxyquinoline (DBHQ) as extractant has been presented. ELM consists of a diluent (kerosene), a surfactant (Span 80), an extractant (DBHQ), a modifier (tributyl phosphate), and a stripping solution (very dilute sulfuric acid solution containing EDTA as complexing agent, buffered at pH 4.25). Cobalt (II) in feed solution with 6 mol/L ammonia was oxidised to Cobalt (III) by H₂O₂ and pH of this ammoniacal solution was adjusted to 10.0 with the addition of hydrochloric acid (HCl). The important variables governing the permeation of nickel and their effect on the separation process have been studied. These variables were membrane composition, ammonia concentration in the feed solution, mixing speed, surfactant concentration, extractant concentration, pH of the feed and the stripping solutions, complexing agent concentration in the stripping solution, and phase ratio. After the optimum conditions had been determined, it was possible to selectively extract 99% of nickel from the ammoniacal solutions containing Ni and Co. The separation factors of nickel with respect to cobalt, based on initial feed concentration, have experimentally found to be of as high as 88.1 for about equimolar Co–Ni feed solutions.