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从废钯催化剂中回收钯的绿色工艺研究 总被引:1,自引:0,他引:1
以双氧水-盐酸混合溶液浸出废催化剂中钯,经离子交换树脂脱出氯钯酸后,循环使用;pH8-9的氢氧化钠和氯化铵溶液为洗脱液。研究了双氧水、盐酸浓度、浸出温度和时间及浸出液循环次数对浸出率的影响,结果表明,最佳浸出条件为:盐酸、双氧水的浓度分别为:1.7,1.1moL/L,72℃反应7h,80℃反应2h,钯平均浸出率98.3%,单程总回收率90.2%;由于浸出液与洗脱液能循环使用,解决了浸出液深度脱钯问题,并避免排放大量废酸液,实现了绿色化生产。 相似文献
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为了更准确地测定土壤中的铂、钯,在体积分数为5%的盐酸介质中,选用不同试剂为络合剂,改性活性炭为吸附剂,电感耦合等离子体质谱法测定土壤中的铂、钯。实验研究表明:经盐酸羟胺改性的活性炭富集,铂、钯的回收率为92.3%~102.4%;8-羟基喹啉为络合剂时,铂的回收率为86.4%~104.9%,钯的回收率为91.7%~100.0%;抗坏血酸为络合剂时,铂的回收率为82.6%~100.9%,钯的回收率为86.2%~98.3%;硫脲为络合剂时,铂的回收率为78.2%~105.1%,钯的回收率为81.9%~95.3%。方法检出限:铂为0.017 ng/mL,钯为0.021 ng/mL。该方法操作简便,分析速度快,灵敏度高,具有良好的测定精密度和准确度,适用于超痕量铂、钯的分析。 相似文献
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三烷基氧膦络合萃取一元有机羧酸 总被引:3,自引:0,他引:3
络合萃取法对极性有机物稀溶液的分离具有高效性和高选择性。选择甲酸、乙酸、丙酸、丁酸为分离对象 ,三烷基氧膦 (TRPO)为络合剂 ,煤油为稀释剂 ,进行了系统的萃取相平衡实验 ,测定了络合剂浓度、稀释剂组成等因素对萃取平衡分配系数的影响。实验结果表明 ,溶质的亲油性对络合萃取平衡影响起主导作用 ;随TRPO浓度增大 ,萃取平衡分配系数呈增大趋势 ;随溶质初始浓度增大 ,有机相的溶质浓度向饱和萃取量接近 ;饱和萃取量随络合剂浓度的增大而增大。对相平衡分配系数进行拟合 ,精度令人满意。 相似文献
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钯的二苄基硫醚固相萃取分离研究 总被引:1,自引:0,他引:1
基于二苄基硫醚与钯的配合反应,建立了一种高选择性固相萃取吸附钯的方法。在0.1 mol/L的盐酸介质中,钯可以被二苄基硫醚树脂吸附富集并形成1∶2稳定配合物,该配合物可用20 g/L酸性硫脲洗脱,洗脱液经处理后用分光光度法测定,柱可以再生和重复使用,且萃取剂流失少。二苄基硫醚对钯的吸附是配位萃取机理;方法用于吸附分离钯选择性高,钯的回收率达95%以上。 相似文献
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试验样品经HCl-H_2O_2-KClO_3高效湿法分解体系分解后,采用活性炭-717阴离子交换树脂混合吸附剂进行分离富集矿石中微量的的铂、钯、金,建立了以盐酸为介质电感耦合等离子体发射光谱测定矿石样品中铂、钯、金的方法。通过国家标准物质验证本方法,结果与标准值相符。方法中铂、钯、金的检出限分别为0.021、0.020、0.0050μg/g,测定下限分别为0.050、0.040和0.017μg/g。按照实验方法测定地质标准样品中铂、钯、金,测定结果的相对标准偏差(RSD,n=10)均小于6.7%,相对误差(RE,n=10)均小于3%,可满足地球化学样品中微量铂、钯、金的检测要求。 相似文献
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《Reactive and Functional Polymers》2001,46(3):283-291
New resins, with a functional group based on triisobutyl phosphine sulphide and containing different spacer arms between the polymeric matrix and the functional group, are evaluated in order to determine and characterise the mechanism of the metal adsorption process. These polymers are selective towards gold and palladium from other noble (Pt, Rh and Ir) and base (Fe, Cu, Ni and Zn) metals. Selectivity is higher in the case of gold (2.8 mmol Au/g resin for polymer 3 and 6.5 for polymer 4) than for palladium (0.5 mmol Pd/g resin for polymer 3 and 0.7 for polymer 4). The application of the Langmuir model to the data permits the determination of the adsorption mechanism, which we found to be a chelating process. The result shows that spacer heteroatoms become involved in the adsorption process. The kinetics of the adsorption is faster for palladium than for gold. The elution of these two metals is accomplished by the use of sodium nitrite and thiourea as eluting compounds. 相似文献
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ABSTRACT The separation of gold and palladium ions in hydrochloric acid solutions by strong anion Type II exchange resins is studied in batch and column operations. Increases in the hydrochloric acid concentration and the temperature of the adsorption process have the effect of decreasing the adsorption capacity and the separation factor of both metals. A faster kinetics of the adsorption process of both ions results from temperature increase and this effect is higher for gold ions as a result of greater changes in its diffusivity. Although the adsorption capacity of palladium ions is lower at equilibrium conditions, the adsorption isotherms obtained suggest that they are more strongly retained by the polymers. The high capacities of these resins for both metals permits their use in the preconcentration of gold and palladium but their application in quantitative separation is restricted by the co-elution of up to% of the interfering ion during the desorption process. The best method for ion desorption is sequential elution with% ammonia for palladium recovery followed by 0·5M thiourea in HCI 1M for the recovery of gold. 相似文献
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Yulia. S. Petrova Alexandr. V. Pestov Maria. K. Usoltseva Elena I Kapitanova Ludmila K. Neudachina 《分离科学与技术》2019,54(1):42-50
In this paper, we report methods for correction of selectivity of sorbents based on N-(2-sulfoethyl)chitosan towards platinum(IV) and palladium(II) in HCl solutions. The common method for correction of selectivity of the sorbents is variation of their modification degree with complexing groups. An increase in the degree of sulfoethylation of the chitosan leads to the significant increase in selectivity of sorption of palladium(II) over platinum(IV). Application of the N-(2-sulfoethyl)chitosan with the highest degree of sulfoethylation allows for selective separation palladium(II) from platinum(IV) (рН = 5.0). Palladium is quantitatively desorbed from the surface of the N-(2-sulfoethyl)chitosans by 3.5 mol/dm3 solution of HCl. 相似文献
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《分离科学与技术》2012,47(11):2533-2553
Abstract Cyanex 301‐immobilized material (prepared by immobilization into an alginate matrix) was tested for Pd sorption in 1 M HCl solutions with a special attention to sorption isotherms and uptake kinetics. This immobilized extractant had great affinity for Pd, as shown by the initial slope of the sorption isotherms. Sorption capacities as high as 150 mg Pd g?1 were obtained in 1 M HCl solutions. However, kinetics was slow, compared to conventional resins. The main limiting step in the process is the diffusion of metal ions into the matrix. The influence of parameters such as HCl concentration, NaCl addition, presence of Pt (as a competitor metal) has been checked. It appeared that sorption performance of Cyanex 301‐immobilized material was hardly influenced by the addition of NaCl and by HCl concentration (below 2.5 M). The resin was remarkably selective for Pd, versus Pt, especially at 1 M HCl concentration. Loaded resins can be desorbed using thiourea solutions. 相似文献
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《分离科学与技术》2012,47(10):1497-1506
The adsorption and separation of platinum(IV) and palladium(II) chlorido species ([PtCl6]2? and [PdCl4]2?) on silica-based microparticles functionalized with ammonium centers based on ethylenediamine (EDA), diethylenetriamine (DETA), triethylenetriamine (TETA) and tris-(2-aminoethyl)amine (TAEA) were investigated. The functionalized sorbent materials were characterized using SEM, XPS, BET, and FTIR. The sorbents were used in the batch and column study for adsorption and selective separation of [PtCl62? and PdCl4]2?. The adsorption model for both [PtCl6]2? and [PdCl4]2? on the different sorbent materials fitted the Freundlich isotherm with R2 values > 0.99. The S-TETA sorbent material was palladium(II) specific. Pd(II) loaded on the silica column was recovered using 3% m/v thiourea solution as the eluting agent. Separation of platinum and palladium was achieved by selective stripping of [PtCl6]2? with 0.5 M of NaClO4 in 1.0 M HCl while Pd(II) was eluted with 0.5 M thiourea in 1.0 M HCl. The separation of palladium (Pd) from a mixture containing platinum (Pt), iridium (Ir), and rhodium (Rh) was successful on silica functionalized with triethylenetriamine (TETA) showing specificity for palladium(II) and a loading capacity of 0.27 mg/g. S-TETA showed potential for use in the recovery of palladium from platinum group metals such as from solutions of worn out automobile emission control catalytic convertors and other secondary sources. 相似文献
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《分离科学与技术》2012,47(17-18):2607-2620
Abstract A batch analysis method has been developed for evaluation of metal salt sorption by crown ether polymers. Selectivity in competitive alkali-metal chloride sorption by a series of formaldehyde condensation polymers of dibenzocrown ethers is influenced by the relationship between the crown ether cavity size and metal ion diameter, as well as the degree of hydration of the metal salt. Effective and selective sorption of KCl from the other alkali-metal chlorides was obtained with a dibenzo-18-crown-6 resin. Excellent sorption selectivity for the monovalent metal chlorides was noted for competitive ion-pair sorption of NaCl, KCl, MgCl2, and CaCl2 by this resin. This resin was examined as a stationary phase for selective column separation of KCl from alkali-metal chlorides and of KCl and NaCl from alkali-metal and alkaline-earth chloride mixtures in 80% methanol—20% water. 相似文献
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J. E. Terrazas-Rodríguez S. Gutiérrez-Granados M. A. Alatorre-Ordaz C. Ponce de León F. C. Walsh 《Journal of Applied Electrochemistry》2011,41(1):89-97
The reduction of palladium, rhodium and neodymium ions at concentrations of 0.94, 0.97 and 0.69 mol dm−3, respectively was studied in 1 mol dm−3 HNO3 or 1 mol dm−3 HCl, at a stainless steel and a vitreous carbon electrode, at 25 °C. At a vitreous carbon electrode in a solution containing
rhodium and palladium ions in 1 mol dm−3 HCl electrolyte, the reduction of metal ions occurred at a similar potential to the formation of hydrogen gas, which impeded
the selective separation of the two metals. At a stainless steel cathode in 1 mol dm−3 HNO3, palladium deposition occurred at a potential ≈0.35 V less negative than that of rhodium allowing the selective recovery
of palladium. Neodymium ions were not electroactive in acidic chloride or nitrate media at pH 0. Using a solution obtained
from a catalytic converter manufacturer containing palladium, rhodium and neodymium ions in 1 mol dm−3 HNO3, palladium ions were preferentially removed at 0.15 V versus SHE at an average cumulative current efficiency of 57%. 相似文献
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负载型钯酞菁能有效催化CCl2F2的选择性加氢脱氯反应,在氟化物为载体的钯酞菁催化剂上,CCl2F2转化成CH2F2的选择性可达75%以上.对比研究表明,负载型钯酞菁催化剂上CCl2F2选择性加氢脱氯的稳态催化活性要高于普通的负载型金属钯催化剂.在钯活性中心引入环状酞菁配体能有效提高催化剂在高腐蚀性反应条件下的稳定性.红外光谱、X射线衍射和紫外-可见光谱表征揭示了负载型钯酞菁催化剂具有良好催化活性和催化稳定性的可能原因. 相似文献
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Thiourea–formaldehyde (TF) and urea–formaldehyde (UF) chelating resins were synthesized and these resins were used in the separation of gold(III) ions from copper(II) and zinc(II) base metal ions. In the experimental studies, the effect of acidity on gold(III) uptake and gold(III) adsorption capacities by batch method, and loading and elution profiles of gold(III) ions, gold(III), copper(II), and zinc(II), dynamic adsorption capacities and the stability tests of TF and UF resins by column method were examined. By batch method, the optimum acidities were found as pH 2 and 0.5M HCl, and gold(III) adsorption capacities in the solutions including copper(II) and zinc(II) ions were obtained as 0.088 and 0.151 meq Au(III)/g for UF and TF resins, respectively. On the other hand, by column method, the dynamic adsorption capacities were calculated as 0.109 meq Au(III)/g with TF, 0.023 meq Au(III)/g with UF, 0.015 meq Cu(II)/g with TF, 0.0057 meq Cu(II)/g with UF, and under 6.1 × 10?5 meq Zn(II)/g with TF or UF. TF resin was more effective in the separation and the concentration of gold(III) ions from copper(II) and zinc(II) ions than UF resin. It was seen that sulfur atoms contributed the gold(III) adsorption comparing with oxygen atoms. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009 相似文献
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采用普通阴离子交换树脂(Purolite A 300E)和硝酸盐选择性离子交换树脂(Purolite A 520E)处理受硝酸盐污染的模拟地下水,通过树脂床层的水流速度越慢,相应的穿透体积越大;用氯化钠水溶液再生饱和的离子交换树脂时,需要的再生液体积随氯化钠浓度的下降而增加,但实际消耗的氯化钠量却随其浓度的下降而减少,氯化钠适宜浓度在3%左右;当地下水中硫酸盐含量较高时,应采用硝酸盐选择性离子交换树脂,但该树脂比普通树脂难再生;树脂再生过程中产生的废液可用SBR工艺进行反硝化脱氮,硝态氮浓度为550m#L的再生废液在SBR池中搅拌反应10h,就能实现完全反硝化。 相似文献