Poly(4-sodium styrene sulfonate-co-4-acryloylmorpholine). Synthesis,Characterization, and Metal Ion Retention Properties

Abstract

A novel resin poly(sodium 4-styrene sulfonate-co-4-acryloyl morpholine) was synthesized through a radical solution polymerization in solution and studied as an adsorbent under uncompetitive and competitive conditions by batch and column equilibrium procedures for the following divalent metal ions Cd(II), Zn(II), Pb(II), and Hg(II), and trivalent Cr(III). For all metal ions, the adsorption was strongly influenced by the pH. The maximum retention capacity, 3.29 mmol of metal ion/g, was obtained for Zn(II) at pH 5 by batch equilibrium procedure. For both the batch and column procedures, the retention behavior was similar for Cd(II), Cr(III), Zn(II), and Pb(II).     

Synthesis,Characterization, and Applications of a New Chelating Resin Containing 4-2-(Thiazolylazo) Resorcinol (TAR)

A new phenol–formaldehyde based chelating resin containing 4-(2-thiazolylazo) resorcinol (TAR) functional groups has been synthesized and characterized by Fourier transform infrared spectroscopy and elemental analysis. Its adsorption behavior for Cu(II), Pb(II), Ni(II), Co(II), Cd(II), and Mn(II) has been investigated by batch and column experiments. The chelating resin is highly selective for Cu(II) in the pH range 2 ～ 3, whereas alkali metal and alkaline earth metal ions such as Na(I), Mg(II), and Ca(II) are not adsorbed even at pH 6. Quantitative recovery of most metal ions studied in this work except Co(II) is achieved by elution with 2M HNO₃ at a flow rate of 0.2 mL min^?1. A similar trend is observed for distribution coefficient values. The quantitative separations achieved on a mini-column of chelating resin include Cd(II) – Cu(II), Mn(II) – Pb(II), Co(II) – Cu(II), Mn(II) – Ni(II), and Mn(II) – Co(II) – Cu(II). The recovery of copper(II) is quantitative (98.0–99.0%) from test solutions (10–50 mg/L) by 1 mol/L HNO₃-0.01 mol/L EDTA. The chelating resin is stable in acidic solutions below 2.5 M HNO₃ or HCl as well as in alkaline solution below pH 11. The adsorption behavior of the resin towards Cu(II) was found to follow Langmuir isotherm and second order rate.     

强酸性阳离子交换树脂在模拟含镍废水处理中的应用研究

以模拟镍废水作原料,001×7强酸性阳离子交换树脂作为吸附剂,采用正交试验法研究得出强酸性阳离子交换树脂-镍溶液体系中分配系数的最佳条件是:树脂用量60 mL,模拟镍废液用量为15 mL,硫酸用量10 mL,其中影响最大的因素是溶液用量,其次是树脂用量,影响最小的是硫酸用量.采用单因素实验法得出:交换系数及交换容量与平...     

腐植酸树脂处理含重金属离子废水可行性探讨

利用泥炭为原料制备腐植酸树脂。在动态条件下,研究了腐植酸树脂对重金属离子Zn2+、Ni2+的吸附效果及吸附条件并探讨了吸附与解吸再生机理:主要吸附形式为离子交换吸附和络合吸附。实验结果表明,在20℃,流速为4mL/min,pH值为5.0～7.0条件下,含Zn2+、Ni2+质量浓度均为70mg/L的废水,经腐植酸树脂处理后,Zn2+、Ni2+去除率可达98%以上,且处理后废水近中性。含Zn2+、Ni2+质量浓度分别为32.5mg/L和29.4mg/L,pH值为5.9的电镀废水,经腐植酸树脂处理后,废水中Zn2+、Ni2+含量显著低于国家排放标准允许值。     

Synthesis,Ion Exchange Properties,and Applications of Amorphous Cerium(III) Tungstosilicate

Abstract

A novel hetropolyacid-based cation exchanger cerium(III) tungstosilicate was synthesized in amorphous form by mixing tungstosilisic acid (TSA) solutions to cerium(III) nitrate solutions at different Ce:TSA ratios. The materials were precipitated from the liquid phase by raising the pH of the solutions using sodium hydroxide. The produced ion exchange powders were characterized using powder X-ray diffractometry, thermogravimetry, infrared spectrometry, inductively coupled plasma and atomic absorption elemental analysis. The materials which were dried at 50°C were found to be stable in water, dilute acids, alkaline solutions, and high temperature up to 1000°C. The Ion exchange properties of the synthesized samples were studied by measuring the distribution coefficients (K_d) for 29 metal ions in demineralized water and nitric acid media. On the basis of K_d values, some quantitative separations such as Co²⁺-Pb²⁺, Cr³⁺-Zr⁴⁺, and Mo⁶⁺- W⁶⁺ are achieved on their columns.     

水处理中离子交换树脂再生时酸碱耗的降低

为了降低水处理中离子交换树脂再生时的酿碱耗，根据生产上对水质要求，水处理的设备、工艺条件等情况，采用逆流再生双层床工艺，通过调整试验确定最优酸碱耗，酸耗＜40-45g／mo1；碱耗63．85g／mo1。提高了总平均工作交换容量，取得了较好的经济效益。     

强酸性离子交换树脂催化合成5-乙氧羰基-4-苯基-6-甲基-3,4-二氢嘧啶-2(H)-酮

在732型强酸性离子交换树脂催化下,以苯甲醛、乙酰乙酸乙酯与尿素为原料,一步合成了5-乙氧羰基-4-苯基-6-甲基-3,4-二氢嘧啶-2(H)-酮.优化的反应条件如下:苯甲醛、乙酰乙酸乙酯与尿素的摩尔比为1:3:2,732树脂用量为0.6 g,乙醇为溶剂,反应温度为80～84℃,反应时间为2 h.此时目标产物的收率为97.96%.     

高效液相色谱法同时测定工业废水中的2,4-二叔丁基酚和2,6-二叔丁基酚

采用高效液相色谱法同时测定工业废水中的2,4-二叔丁基酚和2,6-二叔丁基酚的含量。色谱条件为ZORBAX -XDB-C8色谱柱（4.6 mm×150 mm,5μm）,流动相为水：甲醇：异丙醇（25＋60＋15）混合液,流量为1.0 mL·min-1,进样量20μL,调节检测波长为270 nm。在该方法下2,4-二叔丁基酚和2,6-二叔丁基酚的线性范围为0.005~0.5 mg·mL-1（相关系数分别为0.9999, n=5;0.9999, n=5）。加标回收率分别在98.3%~101.8%和98.5%~101.0%之间,相对标准偏差（n=8）分别为1.35%和1.07%。所用的方法准确简便、重复性好,可作为2,4-二叔丁基酚和2,6-二叔丁基酚含量测定的有效方法。     

Adsorptive Removal of Nitrate and Phosphate from Water by a Purolite Ion Exchange Resin and Hydrous Ferric Oxide Columns in Series

Elevated concentrations of nitrate and phosphate in surface and ground waters can lead to eutrophication, and nitrate can also cause health hazards to humans. The adsorption process is generally considered to be an efficient technique in removing these ions provided that the adsorbent is highly selective for these ions. Removal of nitrate and phosphate from a synthetic water (50 mg N/L as nitrate, 15 mg P/L as phosphate) and a wastewater (12.9 mg N/L as nitrate, 5.9 mg P/L as phosphate) using a Purolite A500P anion exchange resin and a hydrous ferric oxide (HFO) columns (60 cm height, 2 cm diameter, flow rate 1 m/h) in series containing 1–10% (w/w) of these adsorbents and the remainder anthracite (90–99%) were studied. Data from batch adsorption experiment at various concentrations of adsorbents satisfactorily fitted to Langmuir adsorption isotherm for nitrate and phosphate on Purolite with adsorption maxima of 64 mg N/g and 7 mg P/g and only for phosphate on HFO with adsorption maxima of 14 mg P/g. Both batch and column experiments showed that Purolite selectively removed nitrate and HFO selectively removed phosphate. The Purolite column BTC time was greater for nitrate than for phosphate. At the highest percentage by weight of Purolite almost all nitrate was removed in batch study and up to 1000 min in column study, but it was not able to remove a comparatively high percentage of phosphate. However, when the effluent from the Purolite column was passed through the HFO column almost all phosphate was removed. The two columns when set up in series also removed almost all nitrate and phosphate from the wastewater.     

Recent Developments in the Synthesis, Characterization and Applications of Zirconium(IV) Based Composite Ion Exchangers

This article provides a review in the area of zirconium(IV) based organic–inorganic composite ion exchange materials used in analytical, pharmaceutical and environmental protection processes. It focuses on the synthesis, characterization and electroanalytical applications of various Zr(IV)-based composite ion exchangers in detail. The results obtained in different studies have also been critically reviewed. Also reviewed are the various composite cation exchange materials used as electroactive materials for the fabrication of ion-selective membrane electrodes. The ion exchange kinetic parameters of Zr(IV) based composite ion exchangers have been discussed, which provide the preliminary idea before the selection of the material for a particular application.     

Synthesis,Characterization, and Analytical Applications of a New Composite Cation Exchange Material Acetonitrile Stannic(IV) Selenite: Adsorption Behavior of Toxic Metal Ions in Nonionic Surfactant Medium

A composite cation exchange material acetonitrile stannic(IV) selenite was prepared under different experimental conditions. The ion exchange capacity of the material was improved from 0.75 to 1.83 meq g^?1 in comparison to its inorganic counterpart, stannic selenite. The material was characterized on the basis of X-ray, TGA, FTIR, and SEM studies. Ion-exchange capacity, pH titration, elution behavior, and distribution studies were also carried out to determine the preliminary ion-exchange properties of the material. Furthermore, it was investigated that this ion exchange material has a good reusability after 8 times regeneration. The sorption behavior of metal ions was studied in nonionic surfactants namely triton x-100 and tween. On the basis of distribution coefficient studies, several binary separations of metal ions viz- Pb²⁺-Th⁴⁺, Ni²⁺-Th⁴⁺, Ni²⁺-Zn²⁺, Cu²⁺-Ce⁴⁺, Al³⁺-Bi³⁺, and Al³⁺Zn²⁺ was achieved on the packed column of this ion exchange material. The practical applicability of this cation-exchanger was demonstrated in the separation of Th⁴⁺ from a synthetic mixture of Th⁴⁺, Ca²⁺, Sr²⁺, Ni²⁺, and Mg²⁺ as well as Cu²⁺ and Zn²⁺ from a brass alloy sample. Thus, all the studies suggest that acetonitrile stannic(IV) selenite has excellent potential for the removal of metal ionic pollutant species from aqueous media effectively.     

Levels,Sources, and Risk Assessment of Polychlorinated Biphenyls (PCBs) in Soils from Industrial Areas: A Case Study from Saudi Arabia

ABSTRACT

The objective of this study was to assess the pollution levels, sources, and human health risk of polychlorinated biphenyls (PCBs) in soils of industrial areas of the central and eastern regions of Saudi Arabia. Therefore, the surface soil samples from industrial areas (cement kiln, oil refinery, electric power plant, steel industry, and desalination plant) were collected and analyzed by High-Resolution Gas Chromatography-Mass Spectrometry/Mass Spectrometry-Time of Flight (HRGC-MS/MS-TOF) to quantify the levels of 26 PCBs (including 12 dioxin-like PCBs and 14 indicator-PCBs). The investigated 26 PCBs were detected in all soil samples. The total PCBs concentration (from tri-CBs to hepta-CBs) ranged from 171 to 4892 pg g^?1 with an average of 1369 pg g^?1 in soils of the central region and of 142–1231 pg g^?1 with an average of 302 in soils of the eastern region, showing higher values at cement factory and/or oil refinery sites. Overall, the indicator-PCBs were the main congeners and contributed dominantly to the total mass of PCBs in comparison with the dioxin-like PCB congeners, with the most abundant for PCB-180 in the soil samples of the central region. Among individual dioxin-like PCBs, PCB-126 had the highest average value of the toxicity equivalence (TEQ). The TEQ values of ∑12dioxin-like PCBs did not exceed the Canadian soil quality guidelines of dioxin (4 pg TEQ g^?1). Based on human health risk assessment via ingestion, dermal contact, and inhalation, low adverse effects of PCBs could be expected as indicated by lower values of cancer risk (≤10^?6). The principal component analysis indicated that there is a different source of PCBs with similar or different PCB profiles.     

Preparation and Characterization of Titanium Dioxide (TiO2) from Sludge produced by TiCl4 Flocculation with FeCl3, Al2(SO4)3 and Ca(OH)2 Coagulant Aids in Wastewater

Abstract

In this study, TiCl₄ coagulant together with coagulant aids such as FeCl₃, Al₂(SO₄)₃, and Ca(OH)₂ were investigated to improve the photoactivity of titanium dioxide (TiO₂) produced from sludge and to increase the resulting low pH value. After TiCl₄ flocculation with three coagulant aids, the settled floc (sludge) was incinerated at 600°C to produce TiO₂ doped with Fe, Al, and Ca elements. Fe-, Al-, and Ca-doped TiO₂ was characterized in terms of structural, chemical, and photo-electronic properties. All the coagulant aids used together with Ti-salt flocculation effectively increased the pH values. The surface area of TiO₂-WO (without any coagulant aids), Fe/TiO₂, Al/TiO₂, and Ca/TiO₂ was 122 m²/g, 77 m²/g, 136 m²/g and 116 m²/g, respectively. The TiO₂-WO, Fe/TiO₂, Al/TiO₂, and Ca/TiO₂ was found to be of anatase phase. The XRD pattern on the Fe/TiO₂ included an additional peak of hematite (α-Fe₂O₃). The majority of gaseous acetaldehyde with TiO₂-WO and Ca/TiO₂ for photocatalytic activity was completely removed within 40 minutes under UV irradiation.     

Synthesis,Characterization, and Glass Reinforcement of Flame Retardant Acrylated Poly(Ester-Amide) and Flame Retardant Poly(Ester-Imide) Resins Based on Brominated Epoxy Resin

Bisphthalamic acids were prepared by reaction of phthalic anhydride and aliphatic diamines. Flame retardant poly(ester-amide)s were prepared by reaction of brominated epoxy resin with bisphthalamic acids and post reaction was carried out with acryloyl chloride to obtained acrylated flame retardant poly(ester-amide) resins. Bismaleimides were prepared by reaction between aromatic diamines and maleic anhydride. Carboxy terminated bismaleimides were prepared by Michael addition reaction of bismaleimides and 4-amino benzoic acid. Flame retardant poly(ester-imide)s were prepared by reaction between carboxy terminated bismaleimides and brominated epoxy resin. All the obtained products were characterized and analyzed by making composites.     

Synthesis and characterization of Co5Cr2(P2O7)4 - New pyrophosphate as a colouring substance

A new pyrophosphate(V) of the formula Co₅Cr₂(P₂O₇)₄ was obtained in the system Co₂P₂O₇–Cr₄(P₂O₇)₃ as a result of solid-state reactions taking place between different reactants. The new compound crystallizes in the orthorhombic system and belongs to the family of pyrophosphates of the general formula M₅²⁺M₂³⁺(P₂O₇)₄ and is probably isostructural with Fe₅²⁺Fe₂³⁺(P₂O₇)₄. Powder diffraction pattern, infrared spectrum and SEM image of the new compound were presented. As a new potential inorganic pigment, Co₅Cr₂(P₂O₇)₄ was tested for its thermal stability, particle size distribution and colour properties, which were studied both for powder and after introduction into organic matrix and leadless ceramic glaze. The colour of Co₅Cr₂(P₂O₇)₄ powder was defined as deep grey with the colour coordinates L*/a*/b* = 60.63/-1.42/-3.41 and according to the hue angle (h° = 247.39°) it belongs to the blue region. Co₅Cr₂(P₂O₇)₄, with its relatively high thermal stability (t _m = 1230 ± 10 °C) and appropriate colour properties, is a good candidate to be used as inorganic pigment for colouring of acrylic paints. In the case of leadless glaze, the obtained compound acts as a dye.     

新型4-甲基邻苯二草胺酸合Cu（Ⅱ）、Co（Ⅱ）、Ni（Ⅱ）单核配合物的合成与表征

合成了 4 甲基邻苯二草胺酸的 3种单核配合物Na2 〔M (Meopba)〕·3H2 O〔M =Cu(Ⅱ )、Co(Ⅱ )、Ni(Ⅱ ) ;Meopba 4 methyl N ,N’ 1,2 phenylenebis(oxamato)〕。通过红外光谱、紫外光谱、元素分析和摩尔电导等手段对其结构和物理化学性质进行了表征 ,并初步研究了它们的催化氧化性能     

Li4+xMxSi1-xO4(M＝Fe,Cr)离子导电材料的制备与电导性能研究

采用溶胶凝胶法制备了Li4+xMxSi1-xO4(M=Fe,Cr)离子导体材料,并对样品的结构及其电导率用TG-DTA、XRD和交流阻抗仪进行了观察和测试。结果表明,采用该方法可大大降低材料的合成温度,且M(M=Fe,Cr)的掺入有利于提高材料的离子电导性。     

Synthesis,Characterization, and Combustion Catalytic Activities of Copper(II) and Lead(II) Salts of p‐Nitrocalix[n]arenes (n=4, 6, 8)

Six copper(II) and lead(II) salts of p‐nitrocalix[n]arene (n=4, 6, 8) were synthsized and characterized. The DSC curves of all salts showed exothermic decomposition. Sensitivity studies revealed that all the salts with the exception of the lead salt of p‐nitrocalix[6]arene (NCPb6) are relatively insensitive materials. Investigations of the catalytic activities showed that most of the salts displayed high activities in thermal decomposition of NC‐NG and RDX. As evaluated in this work, the salts enhanced the burning rates of both double base (DB) and RDX‐component modified double base propellants. The best catalytic effect was obtained with NCPb6, which increased the burning rate of the DB propellant to the order of about 200 % (2–6 MPa) and 103–198 % (8–20 MPa) while decreasing the pressure index (n) to 0.22 (20–22 MPa).     

Nanoparticles of a New Potassium(I) Coordination Polymer from Thermal Treatment with Oleic Acid: Syntheses, Characterization, Thermal, Structural and Solution Studies

Nanoparticles of a new potassium two-dimensional coordination polymer, {[K₂(μ₄-L)₂(μ-H₂O)₄]_n·nH₂O} (1), HL = 3-{[(4-nitrophenyl)methylen]amino}benzoic acid} were synthesized from thermal treatment of compound 1 with oleic acid at 523 K. The nanoparticles were characterized by scanning electron microscopy and FT-IR spectroscopy. Compound 1 was structurally characterized by single-crystal X-ray diffraction. The crystal structure of this compound indicates that the coordination number for the potassium ions is seven. A hydrogen bonding network and π-π stacking interactions result in more stability of compound 1 crystal packing. The thermal stability of compound 1 was studied by thermal gravimetric (TG) and differential thermal analyses (DTA). The results of stoichiometry studies and formation of compound 1 in MeCN solution were found to be in support of its solid state stoichiometry and show the 1:1 complex formation between the L⁻ and K⁺ ion in MeCN solution.