Deep Purification of Zinc Ammoniacal Leaching Solution by Cementation with Zinc Dust

Deep purification of zinc ammoniacal leaching solution by cementation using zinc dust was studied.The effects of relative amount of metallic impurities,dosage of zinc dust,purification time,temperature,pH value and total ammonia concentration in the solution on the purification of the solution were investigated.The results indicate that total ammonia concentration in the solution had no effect on the purification,but relative amount of metallic impurities,dosage of zinc dust,purification time,temperature and pH value of the solution were the main factors influencing the purification.Keeping appropriate molar ratio of copper to cadmium or nickel to cadmium was beneficial to the cementation of cadmium.Nevertheless,the presence of cobalt went against the cementation of cadmium and cobalt.All metallic impurities could be decreased to acceptable levels under the optimized conditions of 2 g/L of zinc dust dosage,1 h of purification time,35℃,pH value 9.03 of zinc ammoniacal leaching solution.The deeply purified zinc ammoniacal solution obtained by one-stage purification meets the requirements of zinc electrowinning.     

Synthesis of well-aligned ZnO nanorod arrays from mixed sulfide-oxide lead and zinc ore

A novel process of recovery of zinc from mixed sulfide-oxide lead and zinc ore was presented in this paper. ZnO nanorod arrays (ZNRAs) on FTO substrate pre-coated with a layer of ZnO seeds was synthesized successfully from the mixed ore via the oxidative ammoniacal leaching process and a two-step process including precipitation and hydrothermal synthesis. The characterization results from the XRD, SEM and UV–vis spectrophotometer analysis showed that the as-prepared ZNRAs was well-aligned, large-scale, perpendicular to the FTO substrate and had a reduced band gap energy of 3.03 eV. XPS analysis indicated that the grown ZNRAs were doped by a small quantity of carbon and did not contain any other impurities particularly Fe and Pb. The total zinc extraction can reach 92.4% after the oxidative ammoniacal leaching process and the precipitation process. The elimination of conventional purification process in zinc production was achieved due to the efficient and selective oxidative ammoniacal leaching process.     

用氨配合法从含锌废催化剂中回收锌

针对氧化锌易溶于氨-碳酸氢铵混合溶液中生成锌氨配合物这一特点,采用含锌废催化剂为原料,经化浆、高剪切分散后加入氨-碳酸氢铵溶液浸取,通过沉淀除杂、锌粉置换和热解蒸氨得到碱式碳酸锌。考察了高剪切分散机剪切速率、反应温度、浸取剂pH和浸取时间对锌浸出率的影响。结果表明,在剪切速率为25 000 r/min、反应温度为328 K、浸取剂pH=7.5、浸取时间为2 h的条件下,锌浸出率可达90%以上,制备的碱式碳酸锌优于HG/T 2523—2007《工业碱式碳酸锌》标准要求。该研究综合利用了含锌废催化剂,无二次污染产生,符合清洁生产和资源合理利用的要求。     

氨法浸出锌冶金渣尘提锌工艺及动力学研究

锌冶金渣尘作为一种重要的锌二次资源,来源广、储量大、具有较高的综合回收利用价值。以NH₃-CH₃COONH₄-H₂O为浸出体系,考察粒度、反应时间、搅拌速度、液固比、总氨浓度、NH₃与NH₄⁺物质的量比和温度对锌浸出率的影响,结果表明：控制浸出温度为25 ℃、总氨浓度为5 mol/L、液固体积质量比为5 mL/g、n（NH₃）/n（NH₄⁺）=1:1、搅拌速度为300 r/min、浸出时间为60 min,在此条件下锌的浸出率可达84%。含锌冶金渣尘浸出动力学分析显示,浸出反应表观活化能为22.66 kJ/mol,锌浸出过程的浸出速率受固体膜层扩散及界面化学反应共同控制,并获得了浸出锌的动力学速率方程。     

Influence de l'antimoine et du cuivre sur la cementation du cobalt par le zinc

Zinc sulphate solution (160g/l Zn²⁺) used for zinc electrowinning is purified for cobalt by cementation with metallic zinc powder. Industrial practice shows that considerable acceleration of this operation is achieved by the presence of trace impurities in solution. Eventually, CuSO₄ and Sb₂O₃ are deliberately added to the solution. The aim of this work is to elucidate the mechanism of action of those impurities.Zn²⁺ ions present in the solution are responsible for the slow speed of cobalt deposition (160g/l Zn²⁺; 10 mg/l Co²⁺).The cathodic part of the cementation reaction was simulated on a flat electrode through potentiostatic deposits at ?730 mV/ENH (potential at zero current of metallic zinc in the solution). The deposits were studied by anodic dissolution, radioactive tracers, X-ray diffraction and fluorescence, atomic absorption spectrophotometry, optical and electronic microscopy (transmission and scanning). The results were compared with cementation on zinc plate and zinc powder.Antimony and copper are deposited together with cobalt and form alloys with reduced cobalt activity. Total voltage available to overcome the inhibitor effect of zinc ions is thus increased and the reduction of cobalt ions accelerated. Antimony, copper and cobalt triple alloys resist particularly well to corrosion with hydrogen evolution. Copper has a higher accelerating effect on cobalt cementation than antimony, but the latter stabilizes the deposit very effectively.The electrochemical methods used and the knowledge of the mechanism of action of the impurities open new trends for industrial practice.     

用含锌烟尘制备活性氧化锌的工艺研究

以含锌烟尘为原料，用酸法制得了活性氧化锌，产品达部颁标准。考察了硫酸浓度、固液比、温度及时间对浸出率的影响。在优惠条件下，实验浸出率可达９８％左右。三段控温添加锌粉除杂以及氨水与碳酸氢铵复配作为沉淀剂是技术关键。     

Cementation-induced recovery of self-assembled ultrafine copper powders from spent etching solutions of printed circuit boards

Ultrafine copper powders have been recovered from spent etching solutions of printed circuit boards by cementation on helical-form iron scrap chips. The tested solution is an ammoniacal copper solution containing 135 g/l copper with minor impurities. The influences of contact time, temperature, pH, initial copper concentration and Fe stoichiometry on the yield, purity and grain size and shape of the precipitated copper powders were studied. Ultrafine self-assembled copper nanocubes with high purity of about > 99% was obtained at temperature 25 °C, time 20 min, pH 2, Fe stoichiometry 1X and initial copper concentration 20 g/l Cu. It was proposed that the precipitation of copper from the solution involved two main processes: (1) adsorption of copper ions on the surface of the iron chips due to the iron oxides present on it and (2) cementation of copper ions onto the metallic iron contained in the chips. Scrap iron chips is seen to be an effective material for copper powder recovery from spent etching solutions in a pure and fine form.     

Recovery of cadmium from a zinc hydrometallurgical leachate using reactive emulsion liquid membrane technology

A new emulsion liquid membrane process using 3,5‐diisopropylsalicylic acid (DIPSA) and triisobutylphosphine sulfide (TIBPS) as carriers, and ammonium sulfide (NH₄)₂S as precipitant is described. The reactive nature of sulfide ions with extracted cadmium ions in the internal aqueous phase significantly increases cadmium recovery and minimizes zinc impurities. The new process is applied to the enrichment of a low concentration of cadmium ions from a solution containing a high concentration of zinc ions. Under optimum operating conditions, a single stage process produced a cadmium recovery of 98% at a cadmium sulfide content of 99.6%. The results are encouraging for potential applications in zinc hydrometallurgy for recovery of cadmium from sulfuric acid leaching solution of zinc ores. Copyright © 2004 Society of Chemical Industry     

低品位氧化锌矿氨-碳酸氢铵浸出制备氧化锌工艺的研究

采用氨-碳酸氢铵溶液从低品位氧化锌矿中浸出制备氧化锌。研究结果表明,在氨水浓度7mol/L、碳酸氢铵浓度0.62mol/L、浸出温度50℃、氧化锌矿粉粒度为177μm、液固比5:1、浸出时间3h的条件下,锌一段浸出率为87.2%,经过二段浸出,锌总收率可提高至95.9%;浸出液采用足量锌粉还原除杂后,净化液中铜为0.51mg/L,铬为0.18mg/L,铅可降至0.10mg/L以下;净化液经过蒸氨和焙烧制得的氧化锌含量为99.53%(以氧化锌计)。该方法具有工艺简单、能耗低、浸出率较高、浸出过程对环境较友好等优点。     

氨法制取纳米氧化锌的粒径控制研究

为有效控制氨法制取纳米氧化锌的粒径,在蒸氨前将浸出原液用一定量的纯净水稀释,可增加初期沉淀生成的晶核数,使沉淀粒径更加均匀和细化,同时发现蒸氨残液不可以作为浸出原液的稀释剂回用.蒸氨的加热方式对纳米氧化锌的粒径也有影响,选择蒸汽直接加热,当溶液含锌质量浓度小于0.3 g/L时,所制取的纳米氧化锌粒径满足GB/T 19589-2004纳米氧化锌的要求 .     

电磁屏蔽导电涂料用镀银铜粉的制备

采用置换反应法制备镀银铜粉时,铜粉还原银氨溶液中的Ag+生成的Cu2+与NH3形成络合物[Cu(NH3)4]2+,它吸附于铜粉表面而阻碍还原反应的继续进行,使制备的镀银铜粉表层的银含量降低。用氨水提高银氨溶液的pH,可增加制备的镀银铜粉表层的银含量,提高其抗氧化性能。当用氨水调节银氨溶液的pH至11.50时,可制得表层银的质量分数高达47.91%且具有常温抗氧化性能的镀银铜粉。研究了pH、AgNO3用量、AgNO3浓度和反应温度对镀银铜粉的抗氧化性能的影响。     

Extraction of zinc(II) from ammoniacal solution into hydrophobic ionic liquids

BACKGROUND: Separation and recovery of zinc from ammoniacal solutions with solvent extraction is very important in the hydrometallurgical industry. Ionic liquids (ILs) have considerable potential for the separation of metal ions. The extraction behaviour of zinc from ammoniacal solution into three hydrophobic ILs was investigated using β‐diketone as the extractant. RESULTS: The extraction efficiency of zinc for three ILs reached a maximum at pH 7.5 and subsequently decreased with increase of pH and it also decreases with increase of the total ammonia concentration. The overall extraction process is exothermic. The extractability decreases in the IL order: [BMIM]NTf₂ > [OMIM]PF₆ > [OMIM]NTf₂. The results of X‐ray absorption spectra indicate that the coordination number of the extracted zinc complexes decreases with increase in the hydrophobicity of the ILs. The results of five recycling experiments indicate that the three hydrophobic ILs are more stable than [BMIM]PF₆ for the extraction of zinc in ammoniacal solutions. CONCLUSION: Hydrophobic ILs combined with β‐diketone can be used to extract zinc from ammoniacal solutions. The extraction of zinc is dependent on the zinc species in ammoniacal solutions and the hydrophobicity of ILs. Moreover, the latter affects both the extractability of extraction systems and the structure of the extracted complexes. © 2012 Society of Chemical Industry     

阴离子交换色谱法分离含钴溶液中锌、镉、铜等杂质

采用阴离子交换色谱法,研究了某锌厂冶炼废渣的硫酸化焙砂浸出液中钴与锌、镉、铜等杂质离子的分离工艺,确定了最佳工艺参数：将料液配制成含2 mol/L Cl–1和0.1 mol/L Na2SO3的溶液,调节pH值为 4.5,搅拌数分钟,料液pH值降低至 4.0后,用201?7阴离子交换色谱柱进行分离,柱后流出液中锌、镉、铜等杂质的含量达到钴冶金工艺要求,钴的损失为0.7%左右.     

氨配合法制活性氧化锌除杂净化过程研究

本文对氨水－碳酸氨作浸取液以粗氧化锌为原料制活性氧化锌的除杂净化过程进行了研究。氨配合法生产活性氧化锌深度除杂净化中，以H2O2作氧化剂深度除锰，以（NH4）2S为沉淀除杂剂深度除铜，使低品位的原料浸取液得以净化。     

低品位氧化锌矿堆浸实验研究

对含锌11.49%的低品位氧化锌矿以自然粒度筑堆,堆高1 m,浓酸熟化、板结后,采用间歇式喷淋(1/3闲置),喷淋强度10~12 L/(m2×h),堆浸温度20~32℃,堆浸浸出液终点pH值控制在1.0~1.5,经过13周的堆浸后,2 t规模低品位氧化锌矿的锌堆浸浸出率大于93%. 堆浸渣石灰乳处理以消除其可能的环境污染. 低品位氧化锌矿堆浸浸出工艺在技术上是可行的.     

锌浮渣制备活性氧化锌

利用熔锌浮渣制取活性氧化锌。实验表明熔锌浮渣经湿法硫酸浸出后,溶液经过除铁、铅、镉、铜等杂质后再用15%～20%的碳酸铵溶液沉淀锌,经烘干、煅烧可制取高纯度活性氧化锌。     

水解沉淀法制备超细碱式碳酸锌的试验研究

以碳酸氢铵和氨水浸出锌灰,然后经除杂净化得到高纯锌氨溶液,以高纯锌氨溶液为原料,采用加热水解沉淀法合成超细碱式碳酸锌,碱式碳酸锌经煅烧得到超细氧化锌。研究了加热水解沉淀工艺条件对碱式碳酸锌的粒径分布的影响。结果表明,最佳工艺条件为：搅拌速度为300 r/min、蒸氨温度为90 ℃、锌氨溶液中锌质量浓度为75 g/L、负压为-2 kPa。最佳工艺条件下得到的碱式碳酸锌的D50为0.77 μm,颗粒近似球形;煅烧后的氧化锌为六方晶系纤锌矿结构,D50为0.69 μm。     

Radiological Waste Processing for the Recovery of Silver through Cementation with Zinc Powder

Abstract

The recovery of silver from silver-thiosulphate-fixer solutions of radiological wastes has been studied by cementation in batch-stirred reactors using zinc powder as the cementing agent. Silver is efficiently recovered from the solutions. The silver recovery rate and the total silver recovery increased with pH. Metallic silver was the product for cementation in deoxygenated solutions at all pH studied. With non-deoxygenated solutions and at low pH values, metallic silver cemented first, followed by silver sulfide. At high pH values, metallic silver was the cementation product. Electrochemical reactions are proposed for the cementation process in the presence and absence of oxygen.     

常规湿法炼锌净化钴渣再利用的研究与应用

介绍了某湿法炼锌企业利用二段净化钴渣部分替代锌粉,对贫镉液进行沉钴操作的技术改造情况.二段净化钴渣中残余锌粉较多,含锌质量分数达45%~55%.技术人员将二段净化钴渣从钴渣浆化槽送入贫镉液沉钴槽,对贫镉液进行沉钴操作,并控制沉钴后液中钴质量浓度低于0.03 g/L.技术改造后,该厂锌粉单耗降低2.23 kg/t,每年可节约锌粉费用为121.39万元.     

硅酸锌加压硫酸浸出的热力学分析与实验研究

计算绘制了Zn-Si-H2O系ET-pH图,分析了硅酸锌硫酸浸出和原硅酸高温脱硅的热力学可行性. 通过人工合成硅酸锌的加压酸浸实验,考察了始酸浓度、终点pH值、铁含量、硫酸铝添加量、浸出温度对硅酸锌酸浸和硅酸凝聚的影响. 结果表明,升高浸出温度能有效降低硅溶胶的稳定性且有利于原硅酸的高温脱硅过程,进而改善矿浆的过滤性能;硫酸铝能促使硅溶胶凝结析出,可降低硅酸浓度;控制恰当的矿浆终点pH值和Si/Fe及Si/Al质量比均有助于硅析出. 在浸出温度120℃、浸出时间0.5 h、液固比8 mL/g及H2SO4浓度120 g/L的优化条件下,锌、硅浸出率分别约为98%和1%.