溶剂萃取法分离锌锰金属离子的实验研究

以软锰矿和锌精矿同槽酸浸取得到硫酸锌、硫酸锰混合液,研究了从混合溶液中萃取分离锌离子、锰离子的萃取剂的选择以及适宜的萃取条件.实验结果表明,磷酸二(2-乙基己基)酯(P204)萃取锌的能力优于磷酸三丁酯(TBP),在室温、相比A/O=2∶ 1、萃取时间10 min、萃取级数5级、溶液pH为4.0,P204的体积分数为40%时,萃取率达到95%,萃取相锌质量浓度为27.15 g/L.反萃液为0.8 mol/L的稀硫酸,4级反萃,反萃液锌质量浓度可达到89.9 g/L,在此基础上提出了从软锰矿和锌精矿同槽酸浸取液中用P204萃取锌的工艺.     

TBP对LIX84由Cu2+-NH3-Cl——H2O系萃取铜及氨的影响

以Cu2+-NH3-Cl--H2O氨性溶液为被萃水相,在LIX84中添加磷酸三丁酯(TBP),考察了有机相中TBP浓度、被萃水相铜离子浓度、总氨浓度和pH值及相比、LIX84浓度对铜萃取率、共萃氨量的影响. 结果表明,随LIX84中TBP浓度升高,铜萃取率变化不大,负载有机相的共萃氨量明显降低. 有机相中TBP浓度为0.1 mol/L、LIX84浓度为40%、被萃水相铜离子浓度25 g/L、总氨浓度3 mol/L及pH值9.1、相比1:1、萃取时间30 min时,铜萃取率约为81%,与未添加TBP时基本一致,而负载有机相的共萃氨量由未添加TBP时的260 mg/L降至添加TBP后的85 mg/L.     

从铜熔炼烟灰浸出液中萃取分离铜的试验研究

以铜熔炼烟灰浸出液为研究对象，采用N902萃取剂从中分离回收铜，并将铜元素进行富集。研究了萃取剂浓度、相比(O/A)、溶液pH值、振荡时间对铜萃取分离的影响，以及反萃剂浓度、相比、振荡时间对铜反萃率的影响。试验结果表明，在萃取剂质量分数12%、相比(O)/(A)=1∶2、溶液pH值为2.0、振荡时间6 min的萃取条件下，通过两级逆流萃取，铜、锌、铁的萃取率分别为98.26%、1.29%、2.28%;铜与铁、锌的分离系数分别达到4346和2425,实现了铜与铁、锌的有效分离。在选定反萃剂硫酸铜浓度为2.5 mol/L、相比(O)/(A)=2∶1、振荡时间6 min的条件下，通过两级逆流反萃，铜的反萃率为94.68%,反萃后铜质量浓度达到7.04 g/L,相较于浸出液中铜离子质量浓度提高了约3.72倍，实现了铜离子的富集，得到的硫酸铜溶液可用于电积铜生产。     

由锌锰硫酸溶液三相萃取锌锰离子

以P204煤油溶液(油相,O)、PEG 10000水溶液(水相1,W1)及锌锰离子的硫酸铵盐溶液(水相2,W2)构建三相萃取体系(O-W1-W2),将其对锌锰离子的萃取效率与传统溶剂萃取[O-W'2(锌锰硫酸溶液)]和双水相萃取(W1-W2)作了比较. 结果表明,加入KSCN后,三相体系能有效地一步分离锌锰离子. 将SCN-/Zn2+摩尔比由10增大至60,W1相只富集Zn2+,且Zn2+总的萃取率(90%)高于O-W'2(52.8%)和W1-W2(86.2%),O相对Mn2+的萃取率(28%)高于O-W1(10.2%).     

从电镀污泥浸出液中选择性萃取铜的研究

采用M5640-磺化煤油作为萃取剂,H2SO4为反萃剂,对电镀污泥浸出液中的铜进行选择性萃取实验,确定了萃取铜及反萃的最佳工艺参数。结果表明,实验采用二级萃取,萃取剂浓度为5％,VO/VA=1：1,混合时间为2min时,铜的萃取率可达到9996以上,另外采用已优化的反萃工艺参数,铜的反萃率可达99％以上。同时,萃取剂对Ni、Zn的共萃率较低,表明M5640-磺化煤油体系对电镀污泥液中铜的萃取选择能力较高,可以达到与溶液中Ni、Zn有较好的分离效果。     

N-乙基-N-丁基吗啉离子液体双水相体系萃取分离蛋白质

研究了新型离子液体N-乙基-N-丁基吗啉四氟硼酸盐([Nebm]BF4)和KH2PO4形成的双水相体系对牛血清白蛋白(BSA)的萃取行为,考察了盐的加入量、离子液体浓度、溶液pH值、蛋白质浓度等因素对萃取率的影响。结果表明:当KH2PO4的加入量为85 g/L、离子液体浓度在200~250 g/L、BSA的浓度60~120 mg/L、溶液酸度在pH4.5~7.0时,其萃取率达98.0%以上。该双水相体系对α-淀粉酶的萃取率也达98.5%。     

超临界CO_2萃取辣椒精中辣椒碱的工艺研究

采用辣椒总碱含量10%的辣椒精为原料进行单因素实验,考察了萃取温度、萃取压力、萃取时间、夹带剂浓度及流量、CO2流量等因素对超临界萃取过程的影响,得到了适宜的萃取条件:萃取温度45~55℃,萃取压力23~33Mpa,夹带剂为浓度80%的乙醇,夹带剂流量0.04~0.07 m L/min,CO2流量1.5~2.5 L/min,萃取时间1.5 h。     

二-(2-乙基己基)磷酸酯与单烷基磷酸酯协同萃取湿法磷酸中铁离子的研究

以二-(2-乙基己基)磷酸酯(P204)与单烷基磷酸酯(P538)作为协同萃取剂、磺化煤油为稀释剂,从模拟湿法磷酸溶液中萃取Fe3+,研究萃取时间、萃取剂浓度、萃取相比、萃取温度对Fe3+萃取效果的影响.结果表明,当萃取时间为25 min、萃取剂浓度为2 mol/L、萃取相比为2:1、萃取温度为25℃时,铁的单级萃取率...     

硫酸体系中P507对铟锌锰的萃取分离研究

根据软锰矿和闪锌矿在酸性条件下同槽浸出所得浸出液特点(含铟、锌、锰离子),用P507萃取浸出液中的铟,分离出锌和锰。考察了平衡水相酸度(氢离子浓度)、萃取剂体积分数、萃取温度、有机相与水相体积比、萃取时间等因素对铟萃取率的影响。研究结果表明:在室温下,在平衡水相酸度为2.5 mol/L、P507体积分数为30%(30%P507+70%磺化煤油)、有机相与水相体积比为1∶1、萃取时间为10 min条件下,铟的一级萃取率在99%以上,锌和锰一级萃取率在1.20%以下,铟与锌和锰的分离达到最佳效果;负载有机相经水洗,锌和锰洗涤率为99%,铟洗涤率为0;用2.0 mol/L盐酸进行反萃,铟反萃率在98%以上,达到了富集铟分离锌和锰的目的。     

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。     

Separation and recovery of copper from waste printed circuit boards leach solution using solvent extraction with Acorga M5640 as extractant

Waste printed circuit boards (WPCBs) have received extensive attention in recent years because of its harmfulness and resource. In this work, two-step leaching process was carried out by using steel pickling waste liquor (SPWL) as the leaching agent. The leaching solution contains a variety of metals, especially iron, which will have an effect on the recovery of copper. Acorga M5640 (M5640) extractant with a kerosene diluent was used to recover copper from WPCBs leach solution, and the separation factor is adopted to analyze the effects of these metal ions. The effect of different parameters such as pH of aqueous phase, phase ratio (O/A), M5640 concentration, contact time as well as the concentration of H₂SO₄ as stripping reagent were investigated. Over 90.0% copper was extracted with pH 1.1, phase ratio (O/A) 1/1, M5640 concentration 16%, contact time 3 min at room temperature. For the stripping process, the 60 s contact time and 2.5 mol/L H₂SO₄ concentration are suitable with 90.0% stripping percentage of copper. Copper extraction isotherm accords with Langmuir isotherm equation and the results show that iron is the most influential metal ion for copper extraction, which will reduce the theoretical saturation of the extractant. The extractant M5640 has excellent reuse performance and can be recycled more than 10 times, which demonstrated M5640 has the industrial application value in the extraction of copper from WPCBs leach solution.     

湿法炼锌中性浸出液中铜、镉的萃取分离无渣净化工艺

用ＡｃｏｒｇａＭ５６４０萃取剂对硫酸锌浸出液优先萃取分离铜．用二（２－乙基己基）二硫代磷酸（Ｄ２ＥＨＤＴＰＡ）和三辛胺（ＴＯＡ）协萃体系进行锌、镉分离．应用Ｄ２ＥＨＤＴＰＡ－甲苯体系时,镉完全萃取,但有机相中的镉很难反萃．应用Ｄ２ＥＨＤＴＰＡ－ＴＯＡ协萃体系时,镉能从硫酸锌溶液中选择性萃取,也能很容易地从有机相中反萃,实现镉与锌的分离．提出了从硫酸锌中性浸出液萃取分离铜、镉的无渣净化新工艺．     

Liquid-Liquid Extraction of Zinc with Aliquat 336-S-Br from Aqueous Bromide Solutions

Abstract

A new solvent extraction system has been developed for zinc in aqueous bromide solution using Aliquat 336-S-Br-xylene solution as an extractant. A 1 mg/ml zinc solution is extracted essentially quantitatively with an equal volume of 5% Aliquat 336-S-Br-xylene solution in 15 sec. The extracted zinc can be stripped from the nonaqueous layer with a series of aqueous solutions including Na₂SO₃ (≥m 1.0 M) NaOH (≥m 0.5 M), NH₃ (≥m 0.5 M), ethylenediamine (≥m 0.3%), and EDTA (≥m0.5%). The extraction is quantitative only from acidic solutions. High aqueous to organic phase ratios can be utilized without loss of extraction efficiency.     

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.     

采用N235从含Mo,Mn酸浸液中萃取回收Mo

基于软锰矿的强氧化性和辉钼矿的还原性及资源的综合利用,开发出软锰矿与辉钼矿共同焙烧新工艺,焙砂的处理及Mo, Mn分离是该新工艺的关键. 采用N235(20%)+仲辛醇(10%)+磺化煤油(70%)作为萃取剂,从含Mn, Mo焙砂酸浸液中萃取回收Mo,实验得出优化工艺条件为：萃取温度室温(25℃),相比O/W 1:2,错流萃取级数3级,水相中硫酸浓度CH2SO4≤100 g/L;反萃时先用70 g/L的硫酸溶液对萃取有机相进行洗涤,反萃剂采用17%的氨水,反萃温度为室温,相比O/W为1:2,萃取级数为3,此条件下Mo的萃取率及反萃率分别达到99.9%和99.4%.     

Deep Purification of Zinc Ammoniacal Leaching Solution

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.     

锌灰制备活性氧化锌工艺的研究

以冶炼厂废锌灰为原料,经硫酸浸取,考察了不同工艺条件对锌的浸出率的影响。实验结果表明:锌灰在50℃下浸取,pH值为1.5时,可使锌灰中锌的溶出率达93.5%。碱式碳酸锌最佳水解温度为40℃,水解时间为2 h,pH值为7.5时,溶液中锌含量为12 g/L,得到96%以上的水解率。     

用P507从硫酸体系中萃取分离镓与铁锌离子

采用P507萃取剂对硫酸体系中的Ga3+与Fe2+, Zn2+进行萃取分离,考察了料液酸度、萃取剂浓度、时间、温度对萃取的影响,绘制萃取等温线;通过比较负载有机相中3种离子用不同浓度HCl和H2SO4反萃的效果及规律,提出用HCl洗脱Fe2+和Zn2+后,再用H2SO4反萃Ga3+的分离方案,并绘制反萃等温线. 结果表明,以40%(j) P507+磺化煤油为有机相,在相比O/A=1:1、温度25℃、时间20 min条件下,经过4级逆流萃取,Ga3+萃取率可达98.48%,同时19.56%的Fe2+和38.42%的Zn2+共萃进入有机相. 负载有机相用6 mol/L HCl洗涤3次可完全洗脱Fe2+和Zn2+而不损失Ga3+,除Fe2+和Zn2+后的负载有机相用100 g/L H2SO4按O/A=4:1、25℃、10 min,经过4级逆流反萃,Ga3+反萃率达97.64%.