高纯钴制备工艺研究

目前制备99.999%以上金属高纯钴的制备方法很多,主要制备工艺有萃取法,膜分离法,离子交换法,电解法,区域熔炼法等方法.但单一的提纯方法很难达到99.999%以上高纯钴.研究络合-P507萃取工艺与P507萃取工艺分离钴中镍及金属杂质,考察酸度、盐酸、硫酸体系对萃取分离影响.采用20%P507磺化煤油有机相单级萃取提纯钴,钴中Ni%为0.4%,提纯钴中Ni%可达到0.003%～0.004%;不能达99.999%要求,选择1.8%的络合剂Dmege按Co料液中所含Ni的量计算加入,得到络合后的Co溶液.采用同样萃取剂及条件,一次络合萃取分离可使金属钴的Ni%降到≤0.002%;经二次络合萃取分离可使金属钴的Ni%降到0.001%,其他金属杂质含量在检测下限.因此二次络合-萃取-电积工艺,用市售的金属钴料和普通分析纯试剂制备出纯度达99.9999%的高纯金属钴,该工艺采取单级萃取,流程短,操作简单,易控制,Co回收率高,运转费用,生产成本低,易实现工业化生产.为制备高纯金属钴提供简单、合理工艺流程.     

高纯锌的制备及检测技术研究进展

高纯锌是制备化合物半导体材料、精密铸件、还原剂、高纯金属盐和高纯金属有机化合物的重要材料。高纯锌的重要应用依赖于制备和检测技术的发展。围绕超高纯锌产品和高纯锌化学分析两个行业标准，重点介绍了高纯锌的电解法、真空蒸馏法和区域熔炼法等制备方法以及辉光放电质谱法(GD-MS)、电感耦合等离子体质谱法(ICP-MS)、极谱法、氢化物发生-原子荧光光谱法(HG-AFS)、电感耦合等离子体原子发射光谱法(ICP-AES)、原子吸收光谱法(AAS)、分光光度法等检测方法。高纯锌的制备需要逐级提纯，包括电解法初级提纯、真空蒸馏法提纯、区域熔炼精炼和超纯化。高纯锌中的杂质元素检测主要采用辉光放电质谱法和电感耦合等离子体质谱法，并辅以极谱法、氢化物发生-原子荧光光谱法、电感耦合等离子体原子发射光谱法等方法作为验证手段和补充。文章可以为高纯锌制备和检测方法的研究者提供相关借鉴和指导。高纯锌制备和检测技术的发展也促进了材料应用领域的拓展，目前高纯锌越来越多在电子信息、生物医药等高新技术领域得到应用。     

电解质水溶液中钴、镍分离、提纯研究进展

高浓度、高纯度钴盐电解质水溶液是电解或电解精炼生产高纯乃至超高纯金属钴的关键.钴、镍离子深度地分离是制备该种电解质水溶液的核心任务.研究发现目前主要的分离、提纯方法包括:离子交换法、萃取色层法、膜分离法和溶剂萃取法等.研究对象主要集中在含高镍、低钴的硫酸盐水溶液体系.离子交换法、萃取色层法是实现两者深度分离的有效手段，溶剂萃取法则更易实现规模化.研究主要针对有机萃取剂和吸附材料的研发、改性、组合和分离提取工艺的改进等展开.文中对含钴、镍电解质水溶液中钴、镍分离研究进展进行总结评述，并对其发展进行展望.      

真空蒸馏技术在低熔点金属提纯中的应用

真空蒸馏方法以其流程短、消耗少、对环境无污染等优点,成为高纯金属,特别是低熔点金属的研究热点和工业生产中的最主要的方法之一.综述了真空蒸馏技术在高纯金属提纯方面的现状与前景,详细介绍了真空蒸馏技术的分馏机理和影响因素,包括饱和蒸气压、分离系数和蒸发速率3个方面对真空蒸馏提纯效果和效率的影响.介绍了真空蒸馏技术在高纯金属铋、锑、铟3种低熔点金属制备中的应用,并探讨了采用多种方法联合提纯获得超高纯金属的可行性,通过真空蒸馏与区域熔炼两种方法相结合制备了纯度大于99.999 9 %的超高纯铋.      

高纯金属钪锭的制备

在理论分析的基础上,以3N级金属钪为原料,对金属钪真空蒸馏提纯过程进行了研究,并通过真空蒸馏—电弧熔炼制备高纯金属钪锭。结果表明,在自行设计制作的蒸馏塔中,采用1 500℃预蒸馏、1 560℃蒸馏的工艺条件下,经过一次真空蒸馏、电弧熔炼即可获得纯度达99.995%的高纯金属钪锭。     

高纯碳酸锂制备研究进展

高纯碳酸锂已被广泛应用到电池、医药、军工、航天等领域,是制备其他高纯锂盐的原料,高纯碳酸锂的制备已成为近年来研究的热点之一,目前高纯碳酸锂的制备方法主要分为直接合成法和粗碳酸锂提纯法两类,本文详述了各种制备高纯碳酸锂方法的机理、现状及存在问题,其中氢化-离子交换法操作性强、回收率高、产品纯度高,是目前高纯碳酸锂制备的有效方法。本文还对高纯碳酸锂未来制备发展进行了展望:在制备高纯碳酸锂过程中,应根据不同的用途提取不同物性的产品;产量更大、操作性更强、纯度更高、效率更高是高纯碳酸锂制备技术的发展目标;超纯(5N)碳酸锂是碳酸锂制备的发展方向。     

高纯稀土化合物制备的现状与发展

综述了近年来离子交换法、溶剂萃取法和萃取色层法在制备高纯稀土化舍物上的应用现状与发展，总结了三种方法在提取高纯稀土化合物上的优缺点，并提出了C272萃取色层制备单一、高纯稀土的设想。     

钨中的金属杂质在化学法和熔炼法精炼过程中的行为

本文研究了从工业级的钨化合物中除去各种金属杂质和气体的方法,文中介绍了两种精炼法的试验研究。第一种是化学精炼法,此方法包括溶剂萃取法、离子交换法和结晶法;第二种是真空熔炼法,亦称电子束熔炼法。通过试验发现,化学精炼法能很容易地除去碱金属、碱土金属以及过渡元素;电子束熔炼法能蒸发掉和除去各种气体与挥发性的元素。为了得到高纯钨金属产品,研究各种精炼方法的特点是很重要的。     

离子交换法深度除杂制备高纯钴的研究

选用弱碱性阴离子树脂201和D301深度除杂净化电解液,考查了树脂对电解液中离子的吸附情况,以及在钴电解精炼过程中,温度、电流密度、pH等电解工艺参数对纯CoCl2·6H2O体系电解液中主要杂质Fe,Ni,Cu,Zn,Pb的去除影响,电沉积钴经过辉光放电质谱法(GD-MS)全元素(73个元素)分析,得到纯度为99.9995%的高纯钴。只通过离子交换树脂和电解精炼串联提纯,就可以稳定制备高纯钴,实现高纯钴的工业化生产。     

高纯碲的制备

高纯碲根据其纯度可用于制作红外探测器材料，温差发电，潮汐发电和太阳能电池材料，静电复印机硒鼓感光材料和致冷材料等。由于其应用领域不同，对碲纯度要求也不同。本文简述了高纯碲的制备方法，并采用真空蒸馏和区域熔炼法制备出了纯度为９９．９９９９９５％的高纯碲。     

Development and Assimilation of Technology of Obtaining Electrolytic Cobalt from Industrial Products

At Norilsk Mining and Metallurgical plant up to now electrolytic cobalt K-0 has been obtained from commodity cobalt hydroxide. This hydroxide was dissolved in hydrochloric acid and was purified from Fe, Cu, and Ni by extraction with sodium salts of synthetic monocarboxylic acids.

A new technology has been developed to use the industrial product of the main cobalt production, i.e., the solution after purification from manganese, instead of commodity hydroxide. This solution contains sulphate and chloride ions. For obtaining electrolytic cobalt from this solution it is necessary to convert the sulphates to chlorides. This is conducted by extraction of cobalt (and heavy metals impurities) with sodium salts of SMA and then by stripping with hydrochloric acid. This procedure allows obtaining the concentrated cobalt chloride solutions and separate light metals. After the conversion the obtained solution is purified from copper by extraction with the cobalt salt of SMA and from nickel by extraction with a mixture of non-chelating aldoximes and SMA. This mixture of extractants provides an effective purification of cobalt solutions. The separation coefficient pN/c is 25-30.

Use of this technology at the Norilsk Mining and Metallurgical plant has allowed the reduction of the reagent expenses and improved the purification from nickel. In addition extraction equipment has been decreased more than two times at the same productivity. The suggested procedure of conversion allows the use of solutions of practically any anion composition for obtaining cobalt.     

Extraction and Refining of High Purity Terbium Metal From Rare Earth Resources

Terbium metal finds applications in the phosphor industry such as in fluorescent lighting and television tubes, and in the electronic industry for the production of magneto-optical recording media for computer storage discs, and in the production of specialty alloys. There are no direct high grade ores of terbium, rather it occurs as a very minor constituent in ores of the rare-earth minerals. For example, terbium oxide constitutes only 0.01% of California's bastnaesite. 0.05-0.16% of Florida' s monazite. and in the order of 1.00% in the Malaysian xenotime. Currently, the chief rare-earth bearing minerals of commercial importance are bastnaesite (California), monazite (Florida, Australia. India and China) and xenotime( Malaysia).

Extraction of high purity terbium metal involves several major steps. These are

(1) Recovery of rare earth minerals from ores into (REO)concentrates

(2)Leaching of rare earth metals (REM) into leach solutions. This step is often preceded by a roasting step and a mild leaching to remove associated carbonates

(3)Separation or concentration of the rare earth metals into groups or individual metal solutions by either solvent extraction and/ or ion-exchange. Terbium is precipitated out from the solvent extraction solution as oxalate or carbonate compounds, which are converted to terbium oxide upon heating in air

(4)Production and refining of terbium from terbium oxide. These involve conversion of terbium oxide to terbium fluoride, followed by a metallothermic reduction step to the terbium metal, using calcium metal reductant. 3N (99.9%) and 4N (99.99%) purity terbium metal can be obtained by vacuum remelting and sublimation (distillation) of the crude metal, respectively.

In this article, modern practices for extraction and refining of high purity terbium metal is reviewed and reported.     

不同冶炼方法生产1Cr12Ni3MoVN性能对比

1Cr12Ni3MoVN（S/SJ2）合金是一种含有12%Cr的变形低碳马氏体耐热钢,因使用环境的特殊性,所以对材料的成分、纯净度、组织性能等要求较高。综合性能要求高,需要严格控制杂质元素和气体元素含量,以往采用真空感应＋电渣冶炼方式生产来保证产品质量,为进一步提高产品在市场上的竞争力,采用电炉＋电渣冶炼方法进行生产。采用统计学方法,探讨了冶炼方式对材料化学成分的控制、纯净度、性能及产品质量稳定性的影响。结果表明：电炉＋电渣法生产的材料,完全满足技术指标要求。     

高铜硫化镍阳极电解工艺中阳极液净化工艺研究

采用萃取除铜,沉淀法联合除去铁、部分铅及砷,萃取法除钴,离子交换法深度除铅工艺处理高铜硫化镍阳极电解的阳极液。结果表明,该工艺流程短,原料适应性强,铜、镍、钴金属分离彻底,金属回收率高,可得到合格的镍阴极液。     

六氟化钨净化工艺研究

工业制备的初级六氟化钨含有大量杂质气体和金属杂质,必须进行净化,其过程首先采用化学试剂置换去除杂质气体中沸点与六氟化钨接近的氟化氢,然后将反应后的六氟化钨蒸馏至精馏釜中进行低温固化,再利用真空系统抽真空排出其他杂质气体,初步净化后的六氟化钨检测合格,可直接进行精馏去除金属杂质。经过多步净化后,成品六氟化钨的纯度可达99.999%以上。     

稀土金属脱除氧杂质的新技术及驱动机制研究进展

介绍了活泼金属除气法、等离子体熔炼法和固溶氢原子除气法等稀土金属脱除氧杂质的新方法,详细归纳了将氧杂质含量限制在5×10-5以下的工艺条件.重点介绍新方法中引入活泼金属、氢等离子体、活性固溶氢原子等各种外部驱动因素的设计思想,提出提纯新技术的同时探究了痕量杂质的迁移规律及去除机制,深化对杂质存在形式、行为规律及提纯机理的认识.采用FAST-2D与Stefan数值模拟技术、18O₂示踪同位素标记技术、CALPHAD相图数据库模拟计算技术对稀土金属高纯化的新工艺提供理论指导与评价,加深对提纯驱动机制的理解.      

大口径连轧管机限动芯棒坯的研制

利用宝钢特钢现有装备条件,运用相图分析、纯净化与夹杂物控制、组织形态控制、锻造过程温降控制等技术,采用炉外精炼、真空脱气、电渣重熔以及高温均质化、多向锻造、球化退火工艺成功试制了380大直径限动芯棒坯,制成的成品芯棒,显微组织均匀,横向V型缺口冲击功≥17J,使用寿命达到2500支以上,满足生产要求。     

Use of mixed-metals isotherm and log–log McCabe Thiele's diagram in solvent extraction—A case study

Nickel and cobalt are invariably associated with other transition element impurities like copper, zinc, iron, etc. It is essential to remove these impurities in order to attain the high standards of purity required for specific applications. Solvent extraction is a well-tested route for this purpose. The present paper describes the application of two novel concepts, viz. mixed-metals isotherm and log–log McCabe Thiele's (MT) diagram in solvent extraction. Mixed-metals isotherms can be applied to a system in which two metal ions compete for a single extractant. If these two metal ions are required to be extracted as a group, mixed-metals isotherms can precisely predict their behavior. Log–log MT diagrams are useful in determining the requirement of the number of stages in counter current extraction, especially when the feed and raffinate concentrations differ by several orders of magnitude. The two concepts have been successfully applied to develop a process for the separation of high purity cobalt and nickel from ocean nodules leach liquor.     

Molybdenum Metallurgy Review: Hydrometallurgical Routes to Recovery of Molybdenum from Ores and Mineral Raw Materials

With the vigorously growing demand of the steel industry, oil and gas industry, corrosion resistance alloys, cast iron, and catalyst industries, high-grade molybdenum ores are being exhausted gradually in the world. Thus, much attention have been drawn to the recovery of molybdenum from low-grade molybdenum ores in recent years. With the increasingly stringent environmental requirements, the shortcomings due to SO₂ emission in the roasting process of traditional technology becomes obvious. This review outlines metallurgical processes for molybdenum production from various resources, particularly focusing on recent developments in direct hydrometallurgical and recovery processes to identify potential sources of molybdenum products and by-products such as uranium which can be economically produced.

Several methods have been extensively reviewed for molybdenum separation and purification from solution which are potentially applicable to leach solutions of molybdenum ores and raw materials. The main methods include solvent extraction, ion exchange, membrane-based separation, and precipitation. Solvent extraction is highly selective for recovery of molybdenum and the most promising method recommended for future research and development. Membrane-based separation is the next preferred method for selective extraction of molybdenum, purification of molybdenum solutions, or co-recovery of other valuable metals. Ion exchange offers useful means for purification and/or co-recovery of other base metal impurities, although the scale of application of ion exchange in the industry is limited.