H530萃取法从含镍废水中提取镍的研究

本文采用Ｎ５３０溶剂萃取法成功地从硬化油催化剂工业排出的含镍废水中提取镍。通过对废水进行氧化除铁后，直接萃取，用稀Ｈ＿２ＳＯ＿４反萃，反萃液经蒸发浓缩结晶，获得了ＡＲ级硫酸镍产品。     

用新癸酸萃取剂从P507萃余液中提纯浓缩制备电池级硫酸镍

研究了用新癸酸萃取剂从硫酸钴萃余液中萃取分离镍镁制得高纯硫酸镍,考察了萃取体系pH、萃取相比、萃取平衡时间、反萃过程硫酸浓度对萃取率的影响。结果表明:当有机相为45%新癸酸萃取剂+55%磺化煤油、皂化率为50%、与水相混合振荡萃取、控制V_O/V_A=1∶3、萃取时间为3 min时,单级萃取率达81.2%,四级萃取率达99%。反萃液控制pH在2～3,镍总回收率为99%,反萃液中镍总质量浓度大于90 g·L~(-1),浓缩结晶后可制备得到电池级硫酸镍。     

3-羟基丙酸稀溶液的络合萃取

以三辛胺为萃取剂,分别用正辛醇、二氯甲烷、乙酸乙酯、4-甲基-2-戊酮、正己烷、环己烷为稀释剂对3-羟基丙酸稀溶液进行络合萃取,分析了稀释剂对萃取的影响,讨论了温度、溶液p H、相比及络合剂体积分数对络合萃取相平衡分配系数的影响,利用傅立叶红外光谱仪测定了负载有机相中萃合物的结构,对三辛胺络合萃取3-羟基丙酸的机理进行了探讨.结果表明,正辛醇作稀释剂萃取效果最好,平衡分配系数高达4.46.以Na OH溶液进行反萃,3-羟基丙酸的反萃率为99.6%.     

磷的一种间接测定方法

研究了醋酸丁酯萃取磷钼杂多酸铬合物的最佳条件,选用乙醇的稀硫酸溶液洗涤进入有机相中的钼酸盐,用氨水反萃有机相中与磷结合的钼,以硫氰酸钾为显色剂,吐温-20进行胶束增溶测定钼,从而间接测定磷含量.     

化学镀镍废液中镍的萃取及综合利用

利用二－ （２－ 乙基己基）磷酸作为萃取剂萃取化学镀镍废液中的镍,萃余液用硫酸反萃取,生产工业级硫酸镍,达到治理环境,废物利用的目的。     

碱熔-氟硅酸钾容量法测定硅锰合金中硅含量

对氟硅酸钾容量法测定硅锰合金中硅的条件进行研究,建立一种测定硅锰合金中硅含量的简单方法。通过氢氧化钾熔融分解,在硝酸介质中,沉淀硅酸根离子,经过过滤,洗涤,中和残余酸,水解,用氢氧化钠标准溶液滴定生成的氢氟酸,计算出硅的含量。方法应用于硅锰合金标准物质中硅的测定,测定值与标准值一致。对样品进行精密度试验,三种硅锰合金标准物质中硅含量测定结果的标准偏差(RSD)均不大于0. 6%(n=8)。     

微量硫氰酸根的测定

本方法基于季胺氯仿溶液萃取硫氰酸根,再用0.1N 高氯酸溶液反萃于水相中,可使硫氰酸根与大量镍、钴分离。异烟酸—吡唑啉酮比色法测定。     

铜镍混合盐的溶剂萃取分离

从废氢化触媒中获得的硫酸铜和硫酸镍混合盐还含有Fe、Ca、Mg等金属离子及各种机械杂质,经氧化和沉淀Fe(OH)_3后,混合盐得到初步净化。在pH值为3.3～3.5的条件下用一定皂化度的脂肪酸萃取铜,萃取铜后的水相再用皂化后的脂肪酸萃取镍。这时铜镍得以分离,且能除去Ca~(2+)、Mg~(2+)离子。用稀H_2SO_4进行反萃取,反萃水相经幕发结晶即可得到合乎工业品要求的硫酸铜和硫酸镍产品。     

草酸-酸亚硅钼蓝光度法检测钢铁及合金中硅的含量

试样用稀酸溶解,在微酸性溶液中,硅酸与钼酸铵生成硅钼杂多酸,在草酸存在下,用硫酸亚铁铵还原成硅钼蓝,测其吸光度.与钼酸盐形成杂多酸的硅必须以正硅酸状态存在,所以在试样溶解过程中必须避免硅酸的聚合.在溶液中硅酸较易于聚合,其聚合程度与溶液的酸度、溶解时加热的程度和时间以及最终溶液中正硅酸离子的浓度有关     

用溶剂萃取法从ITO膜蚀刻废液中回收金属铟的实验研究

文章对ITO膜蚀刻废液中锱的回收进行了研究。首先采用TBP萃取蚀刻废液,在实验的最优条件下经两次萃取,钢的萃取率可达到96.2％。然后用水反萃TBP有机相,不仅反萃了金属铟,并实现了铟、锡分离。使用P2O4对反萃液萃取及盐酸反萃富集,所得的富钢溶液由NaOH调节pH,用铝片置换,成功回收海绵钢。     

Simultaneous solvent extraction of cobalt and magnesium in the presence of nickel from sulfate solutions by Ionquest 801

The simultaneous extraction of Co(II) and Mg(II) from nickel sulfate solutions has been carried out using the organophosphonic extractant Ionquest 801 diluted in Exxsol D‐80. Statistical design and analysis of experiments were used in order to determine the main effects and interactions of the solvent extraction parameters, which were the extraction pH at equilibrium, the temperature, the extractant concentration and the organic/aqueous phase ratio. A statistically designed experiment was also carried out to study the stripping of the Ionquest 801 organic phase loaded with cobalt and magnesium by sulfuric acid solution. The number of stages required for both extraction and stripping processes of cobalt and magnesium was evaluated. The results of continuous counter‐current mini‐plant tests demonstrated the simultaneous recovery of cobalt and magnesium from nickel sulfate solution. Copyright © 2005 Society of Chemical Industry     

碱融分光光度法测定钛铁中二氧化硅

本法采用氢氧化钠在高温炉中对钛铁样品进行熔融,使钛铁中的硅在碱性环境中能完全熔解,熔解后熔块经硝酸酸化处理,其溶液中可溶性硅酸与钼酸铵作用,用硫酸亚铁还原为硅钼蓝,根据硅钼蓝的深浅,以吸光度法测出硅的含量。     

静态溶液聚合法合成SA-IP-SPS型高吸水性树脂

采用氯磺酸磺化法制备了聚乙烯醇硫酸钠（SPS）,以工业级丙烯酸和SPS为原料采用静态溶液聚合法合成了具有良好吸水、吸盐水性能及较高热稳定性的聚丙烯酸（盐）-聚乙烯醇硫酸钠互穿网络型高吸水性树脂（SA-IP-SPS）,红外光谱、热重分析、硫含量分析结果表明了SA-IP-SPS互穿网络结构的形成.对SPS含量、PVA分子量的考察结果表明：PVA相对分子质量在90000～124000,SPS含量在3%左右时得到的SA-IP-SPS高吸水性树脂吸附性能最高（吸水900g·g^-1,吸0.9%食盐水97 g·g^-1）.     

Separation of cobalt and nickel from acidic sulfate solutions using mixtures of di(2‐ethylhexyl)phosphoric acid (DP‐8R) and hydroxyoxime (ACORGA M5640)

DP‐8R and ACORGA M5640 extractants diluted in Exxsol D100 were used to co‐extract cobalt and nickel from aqueous acidic sulfate media. The influences of equilibration time, temperature, equilibrium pH and reagent concentrations on the extraction of both metals have been studied. It was observed that both cobalt and nickel extraction are slightly sensitive to temperature but are pH dependent. Metal extraction equilibria are reached within about 5 min contact time. In addition, cobalt extraction depends on the extractant concentration in the organic phase. For a solution containing 0.5 g dm^?3 each of cobalt and nickel and an initial pH of 4.1, conditions were established for the co‐extraction of both metals and selective stripping (with H₂SO₄) of cobalt and nickel. Using the appropriate reagent concentrations the yield (extraction stage) for both metals exceeded 90%, and stripping of cobalt and nickel was almost quantitative. Copyright © 2004 Society of Chemical Industry     

硅钼蓝光度法测定钼铁中硅含量方法的条件优化设计

建立了钼蓝分光光度法测定钼铁中硅的方法.通过溶样方法的比较、基体影响、杂质离子的影响确定了样品的溶解方法;同时研究了钼酸铵用量、硫酸亚铁铵用量、波长等对硅测定的影响.在优化条件下对4个不同级别试样进行了测定,RSD＜ 10％,回收率在96.8％～103.1％之间.能够满足GB/T 3649-2008标准的要求,适用于0...     

硫酸肼标准溶液浊度的影响因素研究

对影响硫酸肼标准溶液稳定性的因素,如存放时间、温度、配制方式等因素。结果表明：标准溶液放置时间长达15d,正常使用温度在5℃以上,温度对吸光度影响很小,配制方式对吸光度无影响。硫酸肼标准液吸光度在pH=6.2～10.2范围内稳定性较好。     

Separation of Co(II) and Ni(II) from thiocyanate media by hollow fiber supported liquid membrane containing Alamine300 as carrier — investigation on polarity of diluent and membrane stability

The separation of cobalt(II) and nickel(II) ions by HFSLM has been presented. The feed solution is 0.5M thiocyanate containing 300 ppm each of cobalt(II) and nickel(II) ions, whereas extractant is Alamine300 and the stripping solution is ammonia. Cobalt(II) is more preferable with Alamine300 than nickel(II). The effects of pH, Alamine300 concentration and ammonia concentration were investigated. Seven diluents were used: hexane, decanol, chlorobenzene, benzene, dichloromethane, ethylene dichloride and chloroform with different polarity indexes, from 0.1–4.1. Nickel(II) ion which is unpreferable with Alamine300 was used as a tracer to determine the membrane stability. The polarity of the diluents was found to be the main factor influencing the extraction performance and stability of a liquid membrane. The decreasing of polarity of the diluent can prolong the membrane stability, but the percentages of extraction and stripping decreased. The longest lifetime, 200 minutes, was obtained by using hexane as a diluent with the polarity index of 0.1.     

不同pH值下制备的镍-磷化学镀层相结构及热稳定性

在硫酸镍体系中,pH值为4.5、5.5和6.5的情况下分别制备出3种镍-磷化学镀层,目的在于研究pH值变化对镀层微观结构、内应力水平及热稳定性的影响。采用激光弯曲（LC）应力测量方法对3种镍-磷镀层的应力值进行测量;用电感耦合等离子质谱（ICPM）测量镀层中的磷含量;用扫描电镜（SEM）和配备能量散射谱的透射电镜（TEM/EDS）对镀层的表面形貌及内部相结构进行观测;用差热分析仪（DSC）对镍-磷镀层在高温下的相变规律及热稳定性进行研究。结果表明,pH值为4.5和6.5时制备的镍-磷镀层分别为完整的非晶态和纳米晶结构;pH值为5.5时制备的镍-磷镀层为部分非晶态与纳米晶的混合结构,并且该镀层具有介于前两种镀层之间的P含量及内应力水平。pH值为5.5时制备的镍-磷镀层在经历250℃热处理时发生明显的开裂,TEM测试表明微裂纹起源于Ni/Ni-P相界面;而pH值为4.5和6.5时镍-磷镀层所表现出的高热稳定性分别在于前者更低的拉应力水平及后者的充分的纳米晶结构。pH值为6.5时制备的镍-磷镀层虽然有最高的拉应力值,但其内部充分细小的纳米晶结构会有效避免局部应力集中的发生。此外镀层中可能存在的“反Hall-Petch效应”也是其耐热性能好的原因之一。     

Selective transport of cobalt (II) from ammoniacal solutions containing cobalt (II) and nickel (II) by emulsion liquid membranes using 8-hydroxyquinoline

The selective transport of cobalt (II) from ammoniacal solutions containing nickel (II) and cobalt (II) by emulsion liquid membranes (ELMs) using 8-hydroxyquinoline (8-HQ) as extractant has been presented. Membrane solution consists of a diluent (kerosene), a surfactant (ECA 4360J), and an extractant (8-HQ). Very dilute sulphuric solution buffered at pH 5.0 has been used as a stripping solution. The ammoniacal feed solution pH was adjusted to 9.0 with hydrochloric acid. The important variables governing the permeation of cobalt (II) have been studied. These variables are membrane composition, pH of the feed solution, cobalt (II) and nickel (II) concentrations of the feed solution, stirring speed, surfactant concentration, extractant concentration, complexing agent concentration and pH of the stripping solution, and phase ratio. After the optimum conditions had been determined, it was possible to selectively transport 95.0% of cobalt (II) from ammoniacal feed solution containing Co²⁺ and Ni²⁺ ions. The separation factors of cobalt (II) with respect to nickel (II), based on initial feed concentration, have experimentally found to be of as high as 31 for equimolar Co(II)–Ni(II) feed solution.     

选择性络合滴定法测定伪劣钛白粉中二氧化钛含量

不法企业在钛白粉中常掺入碳酸钙、立德粉、高岭土等违法添加物。针对此现状,建立了钛含量的选择性络合滴定法。方法采用浓硫酸、硫酸铵分解试料,丙三醇作为TiO2+的水解抑制剂,试样溶液pH为2.0～4.0,用过量的乙二胺四乙酸二钠（EDTA）络合TiO2+及其他金属离子,建立以二甲酚橙（XO）-甲基百里酚蓝（MTB）-十二烷基硫酸钠（SDS）为混合指示剂三元体系,用氯化锌标准溶液回滴过量的EDTA,酒石酸钾钠选择性分解TiO-EDTA,再用氯化锌标准溶液滴定释放的EDTA。该方法的加标回收率为98.78%～100.18%、相对标准偏差（RSD）为0.10%～ 0.78%。该方法操作简便,终点变化清晰且敏锐,适用于伪劣钛白粉中二氧化钛含量的测定。