用P204和P507脱除含钴废料中的杂质生产高纯度氯化钴

采用硫酸溶解预先焙烧的钐钴粉 ,化学中和法除稀土、铁和钙镁后用P2 0 4萃取铜、锰、锌等杂质 ,再用P5 0 7萃取分离镍和钴 ,制得的氯化钴溶液用来制备高纯氯化钴。钴回收率大于 90 %。     

多金属结核氨浸液中镍钴铜的萃取分离

采用LIX84从氨性溶液中萃取分离镍、钴、铜。首先采用 5级逆流共萃铜、镍 ,钴留在萃余液中 ,含铜、镍的负载有机相经二级洗涤氨 ;用镍电解废液进行 7级逆流选择性反萃镍 ,实现镍与铜的初步分离 ;然后从含铜有机相中反萃铜得到纯净的硫酸铜溶液 ,选择性反萃镍得到含有少量铜的粗镍液 ,该液仍采用LIX84萃取脱铜 ,并回收铜 ,从而将铜、镍彻底分离 ,实现了用一种萃取剂分离氨浸液中的镍、钴、铜。联动连续运转试验结果表明 ,采用本研究确定的萃取工艺流程和萃取设备处理氨浸液 ,萃取分离效果好 ,试验结果稳定、可靠。金属回收率高 ,萃取回收率分别为 ( %) :Ni 99 0 ,Co 99 7,Cu 99 9。     

从钴镍废料电溶液中分离回收钴镍

研究了从钴镍废料电溶液中回收钴、镍，采用的流程为电溶液-针铁矿法除铁-P204萃取除杂-7401萃取分离钴镍-碳酸盐沉淀钴、镍。试验结果表明，采用该方法，可将溶液中的钴和镍有效分离并回收，钴、镍回收率均达99％。无有毒废气、废水产生，废渣少量，可直接外排。     

从含氨溶液中分离铜、镍和钴

从含氨溶液中分离铜、镍和钴印度处理含铜、镍和钻的氨－硫酸铵溶液以分离有价金属。用ＬＩＸ６４Ｎ煤油溶液处理溶液使铜与镍共萃取，而钴留在萃余液中。用５％ＬＩＸ６４Ｎ煤油液研究了ｐＨ和硫酸铵浓度对铜和镍萃取效率的影响。确定了从含１．７６Ｋｇ／ｍ￣３铜，１７...     

硫酸镍电解液净化除杂工艺研究

对硫酸镍电解液的萃取净化除杂进行了系统的研究。实验采用M5640对铜离子进行除杂,实验条件为:pH值为3.0,相比为1∶1,萃取剂体积浓度为15%,振荡时间5min,在此实验条件下铜离子的萃取率大于99.83%,其含量小于0.1mg·mL-1,已达到5N镍电解液标准。去除铜离子之后,采用P507对电解液进行除杂,在实验条件pH为4.0,相比为1∶1,萃取剂体积浓度为15%,振荡时间5min下,二价铁离子、锌离子、铅离子的萃取率分别为:99.93%,99.75%,84.01%,其含量分别为:0.10,0.21,0.30mg·mL-1,已达到5N镍电解液标准。在此之后再采用P507对电解液中钴离子进行去除,实验条件为:用氢氧化钠溶液均相制皂75%,提高待萃液当中钴离子的含量至4.19g.L-1,即Co/Ni为1/10。实验采取四级萃取,控制水相pH值在4～5之间。钴离子萃取率为74.92%,含量为14.88mg·mL-1,已达到5N镍电解液标准。     

矿石中铜钴镍铅锌镉的方波极谱测定

铜、钴、镍、铅、锌、镉极谱分析,难点在于钴和锌的测定。在多种底液中,钴和锌半波电位相当接近,不能连续测定。文献成功地分开了钴、锌和镍波。文献利用钴波的不可逆性,逆向电压扫描测定锌。有人以萃取—反萃取方式将铜、钴、镍和铅、锌、镉分成两组实施测定。 本工作试验了用萃取—反萃取法分离,极谱测定红土矿中铜、钴、镍、铅、锌、镉六元素。     

从大洋多金属结核氨浸液中萃取分离铜,镍,钴

用ＬＩＸ８４的煤油溶液作萃取剂，从大洋多金属结核的催化还原氨浸溶液中选择性共萃铜和镍，而钴等留在萃余液中，然后选择反萃镍和铜，再生有机相循环使用，铜和镍溶液可用电积回收铜和镍。本工艺只需一种萃取剂便可有效地将铜、镍、钴三者彼此分离，操作简便，可用于处理大洋多金属结核或其它含铜、镍、钴的复杂矿     

废高温镍钴合金浸出液净化试验研究

在"苏打焙烧-碱浸出-氯气浸出-TBP萃取除铁-中和水解除铬-P204萃取除微量杂质-N235萃取分离镍、钴"处理废高温镍钴合金工艺的基础上,重点研究了废高温镍钴合金浸出液的净化工艺,确定了废高温镍钴合金浸出液净化的较优工艺技术参数。采用该净化工艺条件可将浸出液中的杂质元素有效地脱除,处理后所得镍、钴溶液成份满足某公司镍、钴产品生产的要求。     

以5,7-二溴磷-8-羟基喹啉(DBHQ)作萃取剂用乳状液膜法从含镍和钴的氨溶液中选择性萃取镍

R．A．Kumbasar研究了以5,7-二溴磷-8-羟基喹啉（DBHQ）作萃取剂用乳状液膜法（ELM）从含镍和钴的氨溶液中选择性萃取和浓缩镍。乳状液膜由稀释剂（煤油）、表面活性剂（Span80）、萃取剂（DBHQ）、改性剂（磷酸三丁酯）和反萃取液（很稀的硫酸溶液,含有EDTA络合剂,缓冲pH为4．25）组成。料液中氨浓度6mol／L,其中的钴（Ⅱ）用H2O2氧化成钴（Ⅲ）,pH用盐酸调整到10．0。研究了控制镍萃取的变量及其对分离工艺的影响。这些变量是膜的组成,料液中氨浓度,混合速度,表面活性剂浓度,     

高镍、钴合金中锌的极谱测定

极谱法测定锌在岩石矿物分析中得到广泛应用,但在含有大量镍、钴、铬、钒、钨等元素的体系中测定低含量锌时,则需要采取一些分离手续,才能进行锌的测定。分离镍或钴中微量锌多采用有机试剂萃取分离,或用氰化物掩蔽钴、镍等干扰元素,手续繁琐复杂。本文用氨性底液示波极谱法测定上述体系中的锌,着重研究了铬、钴、镍、钒对测锌的干扰情况和消除干扰的方法。在氨性底液中,镍、钴、锌均产生清晰的还原波、它们的E_(1/2)均靠近,共存时,很难测定锌。锌具有两性性质,在强碱性溶液中不沉淀,以Fe(Ⅲ)作载体时,加氯化钠、氢氧化钠沉淀,     

氨法制备低铁锌工艺研究

采用NH3-NH4Cl-H2O体系浸出锌焙砂,经过锌粉两段净化,再电积出低铁金属锌。浸出时Fe、Ge、Si、As、Sb、Pb均进入浸出渣,而Zn、Cu、Cd等进入浸出液中。锌的平均浸出率90.8%,总回收率89.5%。得到的电锌产品中杂质元素Cu、Cd、Sb、As、Ni、Co、Pb和Fe含量≤0.0002%。     

从氧化钴矿石中提取钴的试验研究

研究了从氧化钴矿石中回收钴.通过两段浸出,浸出渣中钴质量分数小于0.5%,钴浸出率达99%.通过黄钾铁钒法除铁,氟化钠法除钙、镁,亚硫酸钠法除铜,P204串级萃取法进一步去除杂质Fe、Ca、Mg、Cu、Zn、Mn、Pb、As等,P507萃取分离钴镍,最后通过沉淀得草酸钴产品,产品纯度符合要求.     

Extraction of nickel,cobalt and other metals [Cu,Zn, Fe(III)] with a commercial β-diketone extractant

The extraction of nickel, cobalt, copper and zinc from ammoniacal solutions of ammonium carbonate or ammonium sulphate by solutions of Hostarex DK-16 in kerosene has been investigated as a function of phase contact time, aqueous-phase pH and organicphase reagent concentration. Besides copper, Hostarex DK-16 also partially extracts iron (III) from moderately acidic solutions whereas nickel, cobalt(II), copper and zinc are extracted from neutral or ammoniacal ammonium sulphate and ammonium carbonate solutions. Extraction decreases in the following order of metals: Cu > Co > Ni > Zn. Cobalt(III) is not extracted, but the complex of cobalt(II) with Hostarex DK-16 is slowly oxidized to a cobalt(III) complex which cannot be stripped even when 10 N sulphuric acid is used. Absorption spectra for cobalt complexes with Hostarex DK-16 (purified by preparative thin-layer chromatography) in benzene also suggest oxidation of cobalt(II) to cobalt(III) in the organic phase. Nickel, cobalt(II), zinc and copper can be stripped easily from organic solution with dilute solutions of sulphuric acid. Hostarex DK-16 extracts iron very slowly, nickel moderately rapidly and copper, cobalt(II) and zinc rapidly. Slope analysis and extraction isotherms suggest that the complexes CuR₂, NiR₂ ·HR and CoR₂·HR are present in the organic phase. Nickel can easily be separated from cobalt by extraction with Hosterex DK-16 after oxidation of cobalt in aqueous ammoniacal solution by hydrogen peroxide; however, LIX 64N seems to be a more promising extractant owing to the higher extraction of nickel under analogous conditions and the poorer extraction of zinc in comparison with Hostarex DK-16.     

Processing of nickel- and cobalt-containing leach liquors obtained from different raw materials

Acidic as well as ammoniacal leach liquors obtained from three different raw materials, namely, lateritic nickel ores, copper converter slag and Indian Ocean manganese nodules, were treated for removal of impurities and separation of copper, nickel and cobalt. Precipitation and solvent extraction techniques were used for these purposes. Iron and silica impurities from acidic solutions were removed by lime precipitation. In ammoniacal medium, iron was coprecipitated with manganese. Manganese was removed as manganese dioxide by oxidative precipitation from both media; this removal also results in some loss of cobalt due to its adsorption on the manganese dioxide matrix. From sulphate solutions, copper was extracted using LIX 64N^®1 followed by nickel-cobalt coextraction using di-2-ethylhexylphosphoric acid (D2EHPA). From the loaded solvent, nickel and cobalt were separated by the crowding technique. From ammoniacal solution, both copper and nickel were coextracted with LIX 64N and separated by selective stripping from the loaded organic phase. Cobalt was recovered either by sulphide precipitation or by adsorption on lignite followed by desorption with sulphuric acid/spent electrolyte.     

连续光源火焰原子吸收光谱法测定氧化镍中钴铜锌铁钙镁

采用盐酸溶解样品,选择Co 240.72nm、Cu 324.75nm、Zn 213.86nm、Fe 248.33nm、Ca 422.67nm、Mg 202.58nm作为分析谱线,钴、铜、锌、铁选择3个像素点,钙、镁选择9个像素点,建立了连续光源原子吸收光谱法(CS-AAS)同时测定氧化镍中的钴、铜、锌、铁、钙、镁的方法。实验表明:在100mL测定液中加入2mL 200g/L氯化锶溶液,可消除测定介质(体积分数为2%的盐酸)对待测元素的影响;基体镍对测定的干扰可忽略。在优化的实验条件下,钴、铜、锌、铁、钙、镁的校准曲线相关系数均不低于0.999 0,且其方法检出限在0.002~0.092μg/mL之间。按照实验方法对氧化镍样品中钴、铜、锌、铁、钙、镁分别平行测定11次,钙和镁的测定值在0.1%~0.4%之间,其对应的相对标准偏差(RSD)不大于2%;钴、铜、锌、铁的测定值在0.003%~0.04%之间,其对应的相对标准偏差均小于10%。将实验方法应用于电真空镍光谱标准样品(该标样为氧化镍状态)中上述各元素的测定,结果与认定值基本一致。     

镍溶液提纯方法研究现状

相继更新的硫酸镍、氯化镍等镍盐产品标准对镍盐中杂质含量提出了更严格的要求。镍溶液中常见金属杂质离子有铁、铜、锌、钙、镁、钠等,介绍了去除这些杂质的方法及研究现状,并指出今后的发展趋势。     

粗硫酸镍中铁钴钙镁深度脱除的工艺研究

研究了以臭氧和氟化钠为脱杂试剂,采用"溶解造液--强氧化除铁钴--氟化除钙镁--结晶析出"为主干的工艺处理粗硫酸镍,深度脱除其中的铁、钴、钙、镁杂质的工艺可行性及最佳工艺条件。试验结果表明,以臭氧为强氧化剂,可深度脱除粗硫酸镍中的铁钴杂质,最佳反应条件为:反应温度80℃,时间8h,终点pH值4.5~5.0,反应终点溶液中铁、钴浓度小于0.005g/L;以氟化钠做添加剂,可深度脱除粗硫酸镍中的钙镁杂质,最佳反应条件为:反应温度90℃,时间2h,pH值5.5,氟化钠添加系数1.5,反应终点溶液中钙0.007g/L,镁0.005g/L;将"强氧化除铁钴"与"氟化钠除钙镁"工序相结合,可获得更好的除杂效果。     

锌精矿化学成分差异对湿法炼锌主要技术指标的影响

本文简要介绍了炼锌原料中硅、铜、铅、镉、钴、镍等杂质含量变化对锌湿法生产及锌粉消耗的影响,重点针对锌精矿主品位变化以及含铁差异对电锌产量、锌总回收率、加工成本的影响进行分析,并为完成10万t电锌产能、回收率达到94.3%的目标,提出了原料要求。     

Zinc electrowinning from flue dusts at a secondary copper smelter and connected adhesion problems of the metal deposits

The secondary copper smelter “Metallhütte Carl Fahlbusch” (MCF), Rastatt, Federal Republic of Germany is discussed, with particular consideration of the MCF zinc electrowinning process from low-grade, chloride-containing flue dusts. The investigations performed were focussed on the adhesion of zinc deposits on the aluminium cathodes. With laboratory tests using the tankhouse electrolyte and an apparatus for measuring the adhesion force, the influence of the electrolyte impurities lead, cadmium, cobalt, nickel, tin and antimony on the adhesion behaviour and on the current efficiency have been determined. Field tests to affect the adhesion of the zinc deposits on aluminium cathodes by dip pretreatment of the cathodes with glue or sodium resinate reveal that with only small sodium resinate additions in the dipping bath better stripping can be achieved.