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1.
《分离科学与技术》2012,47(5):1079-1092
Abstract

A novel monolithic column containing large interconnected pores was simply prepared from epoxy resin and triethylenetetramine (TETA) and pore‐forming reagent (polyethylene glycol, PEG‐1000) by in‐situ polymerization. PEG‐1000 was both solvent at the initial stage and phase‐separation reagent at the later stage of polymerization reaction. Its structure was characterized by Fourier transform‐infrared spectra (FTIR) and scanning electron microscopy (SEM), respectively. The results showed that the pore characteristics of monoliths depended strongly on the amount of PEG‐1000. A column method has been established for the preconcentration and determination of copper(II) combined with inductively coupled plasma atomic emission spectroscopy (ICP‐AES), using a simple glass‐tipped tube. The adsorption‐desorption characteristics of the monoliths for Cu(II) in aqueous solution were investigated in detail. The ion concentrations in batch adsorption experiments were determined by ICP‐AES. Copper ions could form complexes with the amino groups of the monoliths, and be quantitatively retained in the pH ranges of 5.0–9.0. The uploaded column was eluted by 1.0 mol L?1 HNO3 and recovery of Cu(II) was more than 97%.  相似文献   

2.
The synthesis of a water-insoluble adsorbent resin was carried out by radical polymerization of [2-(methacryloyloxy)ethyl] trimethyl ammonium chloride by using ammonium peroxydisulfate as initiator and N,N′-methylene-bis-acrylamide (MBA) as crosslinking reagent. The adsorbent was characterized by elemental analyses, and FT-IR spectroscopy. The thermal stability was studied in the presence of Hg(II). The ability to bind Hg(II), Cd(II), Zn(II), Pb(II), Cu(II), Cr(III), and U(VI) as well as the maximum adsorption capacity, and elution of the Hg(II) from the loaded resin was studied. At pH 2 the adsorbent retained 95% of Hg(II) from an aqueous solution containing 1 g/L in Hg(II). The retention of other metal ions was lower than 15%. Sorption selectivity from the binary mixtures Hg(II)-Cd(II), Hg(II)-Zn(II), Hg(II)-Pb(II), and Hg(II)-Cr(III) was studied at the optimum sorption pH value. Received: 20 April 1997/Revised: 24 July 1997/Accepted: 6 August 1997  相似文献   

3.
A novel Hg(II) ion‐imprinted resin based on thiourea‐modified melamine was manufactured for selective elimination of Hg2+ from aqueous solutions. The polymerizable thiourea–melamine ligand together with its Hg(II) complex were extensively investigated using elemental analysis, Fourier transform infrared (FTIR) and 1H NMR spectroscopies. The Hg(II) complex was used in a condensation polymerization in the presence of formaldehyde crosslinker and then the Hg(II) ions were leached out from the crosslinked polymeric network to finally leave the ion‐imprinted Hg‐PMTF resin. Both ion‐imprinted Hg‐PMTF and non‐imprinted resins were examined utilizing scanning electron microscopy and FTIR spectroscopy. The potential of the prepared resin for selective separation of Hg(II) ions from aqueous solutions was then evaluated by performing a series of batch experiments. Hg‐PMTF displayed an obvious rapid removal of Hg(II) ions with a pseudo‐second‐order kinetic pattern. In addition, the Langmuir adsorption isotherm model exhibited the best fit with the experimental data with comparatively high maximum adsorption capacity (360.5 mg g?1). © 2015 Society of Chemical Industry  相似文献   

4.
A resin containing 3‐(dimethylamine)propyl acrylate and 4‐vinylpyridine was synthesized by radical polymerization (in 1:1 mole ratio). Ammonium persulfate (0.5 mol %) and N,N′‐methylene‐bis‐acrylamide (2 mol %) were used as initiator and crosslinking reagents, respectively. The resin was characterized by Fourier transform infrared (FTIR) and ultraviolet‐visible (UV‐Vis) spectroscopy. The ability to bind Hg(II), Cd(II), Zn(II), Pb(II), Cu(II), and Cr(III) as well as the maximum adsorption capacity and elution of Hg(II) ions from the loaded resin was studied. Sorption selectivity from ternary mixture Hg(II), Cd(II), and Zn(II) was studied at the optimum sorption pH value. At pH 2 the adsorbent retained 98% of Hg(II); the retention of the other metal ions was lower than 20%. The elution assay was made in HClO4 solutions. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 85: 2559–2563, 2002  相似文献   

5.
A novel chelating resin anchoring 2‐amino‐pyridine on macroporous crosslinked polystyrene beads via a sulfur‐containing spacer (PVBS‐AP) has been synthesized and its structures were characterized by FTIR, scanning electron microscopy, porous structure analysis, and elementary analysis. The results of scanning electron microscopy and pores analysis demonstrated that PVBS‐AP resin had meso‐macro porous structure. Its adsorption properties for Hg(II), Pd(II), Ni(II), Cu(II), Zn(II), Pb(II), and Cd(II) were investigated. Some factors affecting the adsorption of PVBS‐AP resin for Hg(II), such as temperature, contact time, ion concentration, and pH were also studied. The results showed that the increasing of temperature was beneficial to adsorption and Langmuir model was much better than Freundlich model to describe the isothermal process. PVBS‐AP resin had good adsorption selectivity for Hg(II). It could selective adsorb Hg(II) from such binary ions system as Hg(II)‐Ni(II), Hg(II)‐Zn(II), and Hg(II)‐Pb(II), their selective coefficients are αHg/Ni = ∞, αHg/Zn = 28.1, αHg/Pb = ∞, respectively. Five adsorption–desorption cycles demonstrate that this resin were suitable for reuse without considerable change in adsorption capacity. POLYM. ENG. SCI., 47:721–727, 2007. © 2007 Society of Plastics Engineers.  相似文献   

6.
The water‐insoluble resin poly(2‐acrylamido‐2‐methyl‐1‐propanosulfonic acid‐co‐4‐vinyl pyridine), through a radical polymerization solution, was synthesized with ammonium persulfate as an initiator and N,N‐methylene bisacrylamide as a crosslinking reagent. The metal‐ion‐retention properties were studied by batch and column equilibrium procedures for the following metal ions: Hg(II), Cu(II), Cd(II), Zn(II), Pb(II), and Cr(III). These properties were investigated under competitive and noncompetitive conditions. The effects of the pH, maximum retention capacity, and regeneration capacity were studied. The resin showed a high retention ability for Hg(II) ions at pH 2.0. The retention of Hg(II) ions from a mixture of ions was greater than 90%. The resin showed a high selectivity for Hg(II) with respect to other metal ions. The Hg(II)‐loaded resin was able to be recovered with 4M HClO4. The retention capacity was kept after four cycles of adsorption and desorption. The retention properties for Hg(II) were very similar with the batch and column methods. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 3556–3562, 2003  相似文献   

7.
Silica aerogel surface modifications with chelating agents for adsorption/removal of metal ions have been reported in recent years. This investigation reported the preparation of silica aerogel (SA) adsorbent coupled with metal chelating ligands of 4-amino-5-methyl-1,2,4-triazole-3(4H)-thion (AMTT) and its application for selective adsorption of Hg(II) ion. The adsorbent was characterized by Fourier transform infrared spectra (FTIR) and thermo gravimetric analysis (TGA) measurements, nitrogen physisorption and scanning electron microscope (SEM). Optimal experimental conditions including pH, temperature, adsorbent dosage and contact time have been established. Langmuir and Freundlich isotherm models were applied to analyze the experimental data. The best interpretation for the experimental data given by the Langmuir isotherm equation and the maximum adsorption capacity of the modified silica gel and silica aerogel was 142.85 and 17.24mgg?1, respectively. Thermodynamic parameters such as Gibbs free energy (ΔG o ), standard enthalpy (ΔH o ) and entropy change (ΔS o ) were investigated. The adsorbed Hg(II) on the SA-AMTT adsorbents could be completely eluted by 1.0M KBr solution and recycled at least four times without the loss of adsorption capacity. The results of the present investigation illustrate that modified silica aerogel with AMTT could be used as an adsorbent for the effective removal of Hg(II) ions from aqueous solution.  相似文献   

8.
A novel chelating resin bearing amidinothiourea (ADTU) moieties was prepared by chloroethyl crosslinked polystyrene (CMPS) with ADTU in the presence of a phase transfer catalyst. Fourier transform infrared spectra (FT-IR) and scanning electron microscopy (SEM) were used to characterized the resulting chelating resin. The saturated adsorption capacity of Hg(II) ions estimated from the Langmuir model was up to 1215 mg g?1at 313 K. Furthermore, the resin was able to selectively separate Hg(II) from multicomponent solutions with Cd(II), Co(II), Cu(II), Zn(II), Mg(II) and Pb(II). The desorption process showed the mercury recovery reached to 99.2% under eluting condition of 1 M HCl + 8% thiourea.  相似文献   

9.
BACKGROUND: Hg(II) is one of the most toxic metals and has received particular attention in environmental pollution. Hg(II) pollution is common in water sources, so rapid and efficient methods must be developed for its removal from water samples. Mesoporous silica (MS) is an ideal adsorbent due to its high surface area and biocompatibility. The efficiency and selectivity of MS adsorbents can be improved by surface modification. RESULTS: A new sorbent for trace Hg(II) removal was developed by grafting 1‐(3‐carboxyphenyl)‐2‐thiourea (CPTU) onto SBA‐15 mesoporous silica. The optimum pH range for Hg(II) adsorption was 3‐7 and the maximum static adsorption capacity was 64.5 mg g?1. An enrichment factor of 150 was obtained with a relative standard deviation < 1.5% (n = 8). Common coexisting ions did not interfere with the adsorption of Hg(II) under optimal conditions. Quantitative recovery was achieved by stripping with a mixed solution of 1 mol L?1 HCl and 5% CS(NH2)2. Efficient adsorption capacity of the recycled material could still be maintained at a level of 95% at the 7th cycle. CONCLUSION: 1‐(3‐carboxyphenyl)‐2‐thiourea functionalized SBA‐15 mesoporous silica was synthesized and applied for Hg(II) removal from water samples with high efficiency and selectivity. Copyright © 2012 Society of Chemical Industry  相似文献   

10.
A new chelating resin is prepared by coup‐ling Amberlite XAD‐2 with salicylic acid (SAL) through an azo spacer. Then the polymer support was coupled with iminodiacetic acid (IDA). The resulting sorbent has been characterized by FT‐IR, elemental analysis, thermogravimetric analysis (TGA), and scanning electron microscopy (SEM) and studied for the preconcentration and determination of trace Pb (II) ion from human biological fluid and environmental water samples. The optimum pH value for sorption of the metal ion was 5. The sorption capacity of functionalized resin is 67 mg g−1. The chelating sorbent can be reused for 20 cycles of sorption–desorption without any significant change in sorption capacity. A recovery of 95% was obtained for the metal ion with 0.5M nitric acid as eluting agent. The profile of lead uptake on this sorbent reflects good accessibility of the chelating sites in the Amberlite XAD‐2‐SAL/IDA. Scatchard analysis revealed that the homogeneous binding sites were formed in the polymers. The equilibrium adsorption data of Pb (II) on modified resin were analyzed by Langmuir, Freundlich, Temkin, and Redlich‐Peterson models. Based on equili‐brium adsorption data the Langmuir, Freundlich, and Temkin constants were determined 0.428, 20.99, and 7 × 10−12 at pH 5 and 20°C. The method was successfully applied for determination of lead ions in human plasma and sea water sample. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011  相似文献   

11.
A chelating resin is produced by coupling a dye calcein blue to Amberlite XAD-2 through an azo spacer. The resulting resin has been characterized by FT-IR, elemental analysis, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM) studied for the preconcentration and determination of trace Cu(II) from solution samples. The optimum pH for adsorption of copper ions was 6. The sorption capacity of functionalized resin is 27 mg·g−1. The chelating resin can be reused for 10 cycles without any significant changes in sorption capacity. A recovery of 100% was obtained for Cu(II) when eluted with 0.5 M nitric acid. Scatchard analysis revealed that homogeneous binding sites were formed in the resin. The equilibrium adsorption data of Cu(II) on modified resin were analyzed by Langmuir, Freundlich and Temkin models. Based on equilibrium adsorption data the Langmuir, Freundlich and Temkin constants were determined 0.036, 2.196 and 0.348 at pH 6 and 20 °C, respectively. The method was applied for Cu(II) assay in environmental samples.  相似文献   

12.
《分离科学与技术》2012,47(14):2963-2986
Abstract

For the functional enhancement of chelating resins containing carboxylic acids, copolymer beads were prepared by suspension polymerization of styrene (St), methyl methacrylate (MMA), and divinylbenzene (DVB) in the presence of toluene as diluent. The phenyl rings of the beads were directly chloromethylated, and the carboxylic ester groups of the beads were converted into hydroxymethyl groups by reduction followed by chlorination to give chloromethyl groups, respectively. The chelating resins containing a pair of neighboring carboxylic acid groups (NCAGs) were obtained by the alkylation of chloromethyl groups in copolymer beads with diethyl malonate in the presence of sodium hydride followed by hydrolysis using aqueous alkali solution. Accordingly, the structural effects of the resins on the adsorption of heavy metal ions were investigated. Poly(St‐co‐DVB)‐based chelating resin containing NCAGs showed adsorption abilities toward heavy metal ions like Pb2+, Cd2+, and Cu2+, whereas poly(MMA‐co‐DVB)‐based chelating resin containing NCAGs showed adsorption abilities toward heavy metal ions like Cu2+, Cd2+, and Co2+. On the other hand, poly(St‐co‐MMA‐co‐DVB)‐based chelating resin containing NCAGs showed adsorption abilities toward heavy metal ions like Pb2+, Cd2+, Hg2+, Co2+, and Cu2+: a synergistic effect on the adsorption of heavy metal ions like Pb2+, Cd2+, Hg2+, and Co2+ was observed. The adsorption ability of poly(St‐co‐MMA‐co‐DVB)‐based chelating resin among three kinds of chelating resins was relatively good.  相似文献   

13.
《分离科学与技术》2012,47(2):376-388
Abstract

Melamine‐formaldehyde‐thiourea (MFT) chelating resin were prepared using melamine (2,4,6‐triamino‐1,3,5‐triazine), formaldehyde, and thiourea and this resin has been used for separation and recovery of silver(I) ions from copper(II) and zinc(II) base metals and calcium(II) alkaline‐earth metal in aqueous solution. The MFT chelating resin was characterized by elemental analysis and FT‐IR spectra. The effect of pH, adsorption capacity, and equilibrium time by batch method and adsorption, elution, flow rate, column capacity, and recovery by column method were studied. The maximum uptake values of MFT resin were found as 60.05 mg Ag+/g by batch method and 11.08 mg Ag+/g, 0.052 mg Zn2+/g, 0.083 mg Cu2+/g and 0.020 mg Ca2+/g by column method. It was seen that MFT resin showed higher uptake behavior for silver(I) ions than base and earth metals due to chelation.  相似文献   

14.
Thiourea‐formaldehyde (TUF), a well‐known chelating resin, has been synthesized and it was used in the adsorption, selective separation, and concentration of Pd(II) ions from Fe(III), Co(II) Ni(II), and Cu(II) base metal ions. The composition of the synthesized resin was determined by elemental analysis. The effect of initial acidity/pH and the adsorption capacity for Pd(II) ions were studied by batch technique. The adsorption and separation of Pd(II) were then examined by column technique. FTIR spectra and SEM/EDS analysis were also recorded before and after the adsorption of Pd(II). The optimum pH was found to be 4 for the adsorption. The adsorption data fitted well to the Langmuir isotherm. The maximum adsorption capacity of the TUF resin for Pd(II) ions was found to be 31.85 mg g−1 (0.300 mmol g−1). Chelating mechanism was effective in the adsorption. Pd(II) ions could be separated efficiently from Fe(III), Cu(II), Ni(II), and Co(II) ions using TUF resin. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011  相似文献   

15.
Crosslinked poly[3‐(methacryloylamino)propyl]dimethyl(3‐sulfopropyl)ammonium hydroxide‐co‐2‐acrylamido glycolic acid [P(MAAPDSA‐co‐AGCO)] was synthesized by radical polymerization and tested as an adsorbent under competitive and noncompetitive conditions for Cu(II), Cd(II), Hg(II), Zn(II), Pb(II), and Cr(III) by batch and column equilibrium procedures. The resin–metal ion equilibrium was achieved before 1 h. The resin showed a maximum retention capacity value for Hg(II) at pH 2 of 1.084 meq/g. The recovery of the resin was investigated at 20°C under different concentrations of HNO3 and HClO4. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 91: 3679–3685, 2004  相似文献   

16.
Graft copolymerization of acrylamide onto coconut husk (CH), initiated by the ferrous ammonium sulfate/H2O2 redox initiator system, was studied. To determine the optimum conditions of grafting, the effect of the concentrations of ferrous ammonium sulfate, the monomer, and H2O2 and the time and temperature on percentage of the graft yield was studied. A new adsorbent media having a carboxylate functional group was synthesized by the surface modification of polymer‐grafted coconut husk (PGCH COOH). The mechanism of graft polymerization and surface functionalization is proposed. The material exhibits a very high adsorption potential for Hg(II). The sorption of Hg(II) was found to be dependent on the contact time, concentration, pH, and temperature. Maximum removal of 99.4% with 2 g/L of the sorbent was observed at 125 μmol L−1 Hg(II) concentration at pH 6.0. The slow step which determines the rate of exchange of Hg(II) ions is diffusion through the adsorbent particles. The diffusion coefficients, energy of activation, and entropy of activation were calculated and used to determine the theoretical behavior of the sorption process. The applicability of the Langmuir isotherm established the endothermic character of the adsorption. Acid regeneration was tried for several cycles with a view to recover the adsorbed metal ions and also to restore the sorbent to its original state. The adsorbent efficiency toward Hg(II) removal was tested using synthetic and chloralkali industry wastewaters. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 75: 1261–1269, 2000  相似文献   

17.
A new fibrous adsorbent was prepared by grafting acrylic acid/acryl amide (AA/AAm) comonomers onto poly (ethylene terephthalate) (PET) fibers. The resulting sorbent has been characterized by Fourier transform infrared (FT‐IR), elemental analysis, thermogravimetric analysis (TGA), FT‐Raman, and scanning electron microscopy (SEM) and studied for the preconcentration and determination of trace Pb (II) ion from human biological fluid and environmental water samples. The optimum pH value for sorption of the metal ion was 8. The sorption capacity of functionalized resin is 44.1 mg g?1. The chelating sorbent can be reused for 20 cycles of sorption–desorption without any significant change in sorption capacity. A recovery of 100.2% was obtained for the metal ion with 0.5M nitric acid as eluting agent. Effect of grafting yield, shaking time, shape of sorbent, and pH of the medium on adsorption of the metal ion were investigated. Scatchard analysis revealed that the homogeneous binding sites were formed in the polymers. The equilibrium adsorption data of Pb (II) on modified fiber were analyzed by Langmuir, Freundlich, Temkin, and Redlich‐Peterson models. Based on equilibrium adsorption data, the Langmuir, Freundlich, and Temkin constants were determined as 0.236, 10.544, and 9.497 at pH 8 and 20°C, respectively. The method was applied for lead ions determination from human plasma and sea water sample. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011  相似文献   

18.
An ICP‐AES method using a new spherical macroporous epoxy–polyamide chelating resin to enrich and separate trace Ga(III), In(III), Bi(III), V(V), Cr(III), and Ti(IV) ions from solution samples is established. The results show that the analyzed ions can be enriched quantitatively by 0.1 g of the resin at pH 4, with recoveries > 98%. The ions can be desorbed quantitatively with 10 mL of 2M HCl from the resin column with recoveries > 96%, and 100–1000‐fold excesses of Ca(II), Mg(II), Fe(III), Cu(II), Zn(II), Al(III), Ni(II), and Mn(II) cause little interference in the determination of these ions by ICP‐AES. The chelating resin is reused for ten times; the recoveries of these ions are still over 95%. The relative standard deviations for enrichment and determination of 100 ng ml?1 Ga(III), In(III), and Bi(III), 10 ng ml?1 V(V), Cr(III), and Ti(IV) are in the range 0.6–2.3%. The concentration of each ion found in the real wastewater sample and alloy sample is in good agreement with the values provided by the plant. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 2330–2334, 2005  相似文献   

19.
The present investigation was undertaken to evaluate the effectiveness of a new adsorbent prepared from coconut coir pith (CP), a coir industry‐based lignocellulosic residue in removing metal ions from aqueous solutions. The adsorbent (PGCP‐COOH) having a carboxylate functional group at the chain end was prepared by grafting polyacrylamide onto CP using potassium peroxydisulphate as an initiator and in the presence of N,N′‐methylenebisacrylamide as a crosslinking agent. The adsorbent was characterized by infrared (IR) spectroscopy, thermogravimetry (TG), X‐ray diffraction (XRD) patterns, scanning electron microscopy (SEM), and potentiometric titration. The adsorbent exhibits very high adsorption potential for the removal of Pb(II), Hg(II), and Cd(II) ions from aqueous solutions. The optimum pH range for metal ion removal was found to be 6.0–8.0. The adsorption process follows a pseudo‐second‐order kinetic model. The adsorption capacities for Hg(II), Pb(II), and Cd(II) calculated using the Langmuir isotherm equation were 254.52, 189.49, and 63.72 mg g?1, respectively. Adsorption isotherm experiments were also conducted for comparison with a commercial carboxylate form cation exchanger. Different industry wastewater samples were treated by the PGCP‐COOH to demonstrate its efficiency in removing heavy metals from wastewater. The reusability of the PGCP‐COOH was also demonstrated using 0.2M HCl. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 3670–3681, 2007  相似文献   

20.
Melamine–formaldehyde–diethylenetriaminepentaacetic acid (MF–DTPA) resin was prepared as a new adsorbent for removing heavy metals from wastewater effluents. The resin was synthesised by anchoring the chelating agent diethylenetriaminepentaacetic acid (DTPA) to melamine via amide covalent bond during melamine–formaldehyde condensation reaction in an acidic aqueous medium. The effects of reaction parameters (temperature, acidity, and water content) on resin characteristics (water regain, rigidity, DTPA functionality, and porosity) were monitored to specify the best synthesis conditions. The resin was chemically characterized using infrared spectroscopy (FTIR), elemental analysis (EA), thermal programmed decomposition-mass spectrometry (TPD-MS), solid-state 13C NMR and 15N NMR, and was morphologically characterized using N2 gas adsorption/desorption (BET analysis) and field emission-scanning electron microscopy (FE-SEM). The water regain factor was also calculated to determine hydrophilic character of the resin. The simultaneous adsorption performance of MF–DTPA resin towards selected heavy metals, Co(II), Cd(II), Zn(II), and Cu(II), was discussed. Quantitative analysis for adsorption was conducted using atomic absorption to investigate the kinetics, adsorption isotherm and thermodynamics of the removal process considering pH, initial concentration, temperature, and contact time as controlling parameters. The mechanism of adsorption was suggested based on experimental results. This work shows the potential application of the MF–DTPA resin for removing heavy metals from wastewaters.  相似文献   

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