表面氨基高密度化介孔氧化硅的合成及其高效去除酸性橙7

以月桂酸为阴离子表面活性剂,3-胺丙基三乙氧基硅烷(APTES)为共结构导向剂,合成了高含量氨基功能化介孔氧化硅材料(AFMS)。以AFMS为吸附剂对溶液中酸性橙7(AO7)进行吸附,对影响AO7吸附效率的相关因素进行了详细研究,结果表明,溶液pH值及温度影响较大。吸附动力学表明,本研究中合成的AFMS对AO7的吸附速率极快。Sips吸附模型对吸附等温线模拟效果最好,从中可知AO7在样品D(由3.0 mL正硅酸乙酯及1.4 mL APTES合成)上的最大吸附量为1.26 mmol·g^-1,远远高于相关文献报道的值。此外,通过吸-脱附循环实验证明,样品D具有良好的稳定性。     

加热方式及原料配比对介孔CeO_2结构及其光催化性能的影响

以P123(聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物)为模板剂,Ce(NO_3)_3为反应原料,通过考察加热方式、加热温度、原料配比等因素,合成了结构性能较好、表面羟基含量较高的介孔CeO_2材料。利用XRD,N_2吸附-脱附,TEM,Raman,FT-IR等技术对合成样品的结构性能进行了表征,结果表明,当P123与Ce(NO_3)_3物质的量之比为1∶10,在110℃水热下合成的CeO_2结构性能最好。以酸性橙7(AO7)为探针分子,对合成介孔CeO_2的光催化性能进行评价。光催化结果证明,由于表面羟基含量较高、介孔及氧缺位的形成,所合成结构性能较好的CeO_2,利用可见光可彻底催化降解溶液中的AO7。     

顺丁烯二酸-co-苯乙烯微球对Cd(Ⅱ)的吸附行为研究

以火焰原子吸收光谱法(FAAS)为检测手段,研究了本实验室合成的顺丁烯二酸-苯乙烯共聚物微球对Cd(Ⅱ)的静态吸附性能,考察了影响吸附率的相关因素以及不同浓度的各种解吸剂对Cd(Ⅱ)的解吸效果.溶液pH为6、吸附时间为2h时吸附基本达到平衡,吸附率可达到95%以上.以3 mol/,L的HCI溶液作为解吸剂对Cd(Ⅱ)进...     

氨丙基硅三烷改性介孔二氧化硅及对痕量镉(Ⅱ)的分离富集性能研究

以氨丙基硅三烷作为改性剂,对介孔二氧化硅表面进行修饰,制备了氨基化介孔二氧化硅吸附材料,采用透射电镜和傅立叶红外光谱仪对其进行表征,并用于水样中痕量镉的富集,建立了氨基化介孔二氧化硅分离预富集/火焰原子吸收光谱法测定痕量镉的方法。考察了溶液pH值、样品流速、洗脱剂类型、干扰离子和吸附容量等对痕量镉分离富集的影响,以及该吸附材料对痕量镉(Ⅱ)的吸附性能。结果表明,溶液pH 7.0,样品流速8 m L/min时镉离子能被制备材料高效吸附,吸附的镉(Ⅱ)用5.0 m L 2 mol/L HNO_3完全洗脱,火焰原子吸收法测定。在最佳实验条件下,方法的线性范围为0.6~20 ng/m L,定量下限为0.5 ng/m L,富集倍数为50倍,对10 ng/m L Cd2+测定的相对标准偏差(n=11)为0.92%,加标回收率为98.8%~104.5%。该方法的抗干扰能力较好,富集柱可循环使用12次以上,可用于环境水样中镉(Ⅱ)的测定。     

杯芳烃修饰玻碳电极吸附溶出伏安法测定微量铅

研究了以杯芳烃衍生物修饰玻碳电极,以其吸附溶出伏安法测定微量铅。对富集时间、铅的浓度、支持电解质、样品溶液pH值及部分离子干扰等进行了实验。实验发现以氢氧化钠溶液处理修饰电极可提高测定灵敏度,经过优化处理后,线性范围和检出限分别为5.0×10-7～1.0×10-5mol/L和1.0×10-8mol/L。应用本法对合成水样进行了测定,结果满意。本文还对吸附溶出机理进行了讨论。     

聚乙烯吡啶树脂对间苯二酚的吸附性能研究

通过悬浮聚合法,合成了一种聚乙烯吡啶树脂(PVP)。以大孔弱碱树脂D301和大孔吸附树脂XAD-4作为参照,研究了PVP树脂对间苯二酚的吸附性能,探讨了溶液的p H值及无机盐对树脂吸附间苯二酚的影响。结果表明,溶液pH值为6.02时,PVP树脂对间苯二酚的吸附量达到134mg/g,无机盐对PVP吸附间苯二酚几乎无影响。Freundlich等温吸附方程能够很好地拟合PVP树脂吸附间苯二酚的等温线,且间苯二酚在PVP树脂上的吸附为放热过程,能够自发进行。     

β-环糊精/Fe3O4水基磁流体的制备表征及其对中性红的吸附行为

采用化学共沉淀方法合成了柠檬酸化β-环糊精(CA-β-CD)修饰的水基磁流体。运用红外光谱(FTIR)、透射电子显微镜(TEM)、热重分析(TGA)、X射线衍射(XRD)和振动样品磁强计(VSM)对其结构、形貌、组成成分和磁性能进行了表征。结果显示,磁流体粒子分散性良好,粒径分布在(7±2)nm范围;磁流体具有超顺磁性,CA-β-CD修饰前后的饱和磁化值分别为62和43 A·m2/Kg。将磁流体用于染料中性红(NR)的吸附,考察了吸附时间、NR初始浓度及溶液pH值对吸附作用的影响。结果显示,磁流体在中性条件下对NR的吸附效果最佳,最大吸附量为244 mg/g,吸附效率最高可达99.8%。     

交联聚丙烯酸固载化氧化β-环糊精的合成及其对尿素的吸附性能

大孔交联聚丙烯酸树脂(D151和D152)用氯化亚砜转化为酰氯后,通过成酯反应固载β-环糊精,再进一步用高碘酸钠氧化,合成出具有环状多醛结构的交联聚丙烯酸固载化氧化β-环糊精。系统研究了反应条件对β-环糊精固载化反应的影响,发现摩尔投料比(—COC1/β-CD)为1.5—1/1、温度80℃、时间24 h为最佳固载反应条件。探讨交联聚丙烯酸固载化氧化β-环糊精对尿素的吸附性能,阐明了吸附时间、溶液中尿素浓度、及介质pH值等对吸附量的影响。在尿素浓度130 mg/dL、吸附时间4h、介质pH 7、温度25℃时,交联聚丙烯酸固载化氧化β-环糊精对尿素呈现出最大吸附量82.13 mg/g。     

桉树遗态Fe/C复合材料对水中磷的动态吸附研究

以桉树遗态Fe/C复合材料为吸附剂,溶液初始p H值、吸附剂粒径、流速、含P(V)模拟废水初始浓度、吸附剂投加量和温度为影响因素,开展了对P(V)的动态吸附行为研究。研究表明,吸附剂粒径(20~40mesh到100mesh)和吸附剂投加量(1~4g)越大、流速(3.43~15.41m L/min)和初始浓度(5~30mg/L)越小,桉树遗态Fe/C复合材料对目标污染物的吸附效果越好;溶液的p H值为3时吸附效果最佳;温度对吸附效果的影响不大。桉树遗态Fe/C复合材料吸附初始浓度为10mg/L的P(V)溶液所得到的平衡吸附量为6.61mg/g。Thomas模型和Yoon-Nelson模型均能很好地描述桉树遗态Fe/C复合材料对P(V)的动态吸附行为,获得的拟合值和实验值基本吻合。     

D301大孔树脂吸附钒(V)的性能研究

研究了D301大孔树脂对钒的吸附性能.结果表明,pH值对D301树脂吸附钒的影响很大,与钒在溶液中的赋存状态有关,且在pH=2时吸附效果最好:测得吸附热力学参数分别为:△H=8.97kJ/mol,△G_(313)=-5.69kJ/mol,△G_(303)=-5.2kJ/mol,△G_(293)=-4.9kJ/mol,△S=46.84J/mol·K.等温吸附服从Freundlich经验式;考察了溶液浓度、搅拌速率对交换过程的影响,并对实验数据运用相关理论模型进行拟合,结果显示钒(V)在D301树脂上吸附交换过程控制步骤为颗粒扩散控制,反应级数n为0.2391.     

Adsorption properties of amidoximated porous acrylonitrile/methyl acrylate copolymer beads for Ag (I)

Porous a crylonitrile (AN)/methyl acrylate (MA) copolymer beads were synthesized by suspended emulsion polymerization and amidoximated for the purpose of Ag⁺ adsorption. Optimum amidoximation temperature and time were determined by following the adsorption capacity for Ag⁺. The results showed that amidoximated AN/MA (AO AN/MA) with the amidoximation temperature 70°C and amidoximation time 20 hr had a relatively higher adsorption capacity for Ag⁺. The effect of pH on adsorption for Ag⁺ was studied; the highest adsorption capacity presented at pH 5.0. Adsorption kinetics and isotherms of AO AN/MA copolymer beads for Ag⁺ were also investigated. The kinetics data indicated that the adsorption process was governed by the film diffusion and followed both pseudo‐first‐order and pseudo‐second‐order rate model. The isotherms indicated that adsorption capacities increased with equilibrium concentration and temperature. The Langmuir model and Sips model could describe the isothermal process. Thermodynamic analysis revealed that the adsorption behaviors of Ag⁺ ions on AO AN/MA could be considered as endothermic and physical sorption process. Copyright © 2010 John Wiley & Sons, Ltd.     

Fabrication of a magmolecule using nanoparticle and evaluation of its adsorption capacity for selenium ions from nuclear wastewater

The purpose of present study is to fabrication of a magmolecule (amino-functionalized magnetite nanoparticles) and evaluation of its adsorption capacity for selenite (SeO₃ ^2?) ions from nuclear wastewater. To accomplish this, synthesized magnetite nanoparticles is coated with a layer of SiO₂ in order to be chemically stable and then functionalized with 3-aminopropyl triethoxysilane (APTES) to be more effective. Adsorption of SeO₃ ^2? ions was investigated in batch technique. The effect of parameters such as solution pH, presence of competing anions using sulfuric acid and nitric acid (NO₃ ^?, HSO₄ ^? and SO₄ ^2?) and temperature were studied. Maximum adsorption occurred at pH 2.4 for magnetite (naked nanoparticle) and 1.7 for functionalized nanoparticles, while the dose of adsorbent was 1 g/L and selenite ion concentration was 50 mg/L. sulfuric acid was selected as the better acidic agent for controlling pH of solution. Thermodynamic parameters were also calculated and it has been found that the adsorption was endothermic. The obtained result showed that the naked particles had more adsorption capacity but it has been suggested usage of functionalized particles in the magmolecule process duo to stability and reusable capability.     

Preparation of a Chelating Polymeric Membrane and Application to Uphill Transport

Abstract

Modification of an anion-exchange membrane by (1-(2-arsono-phenylazo))-2-hydroxy-3,6-naphthalenedisulfonic acid (thoron) results in a membrane that can chelate metals. The high affinity of the disulfonate for the anion-exchange sites together with molecular adsorption of the aromatic thoron onto the polymers yields a system that is stable in strong acids at or below 1 M. By employing a relatively high pH sample (5-9) in conjunction with an acidic stripping solution (0.2 - 1.0 M HCl), uphill transport of Cu(II) and Zn(II) was accomplished. The transport rate was increased by means (lower chelating capacity and the use of a chelate-forming aid on in the stripping solution) of promoting the volume diffusion mechanism of membrane transport. With a 0.05 mmol per dry gram chelating capacity and a 0.1 M EDTA stripping solution (pH 6.5), an enrichment factor of 16 was observed in a one-hour experiment with a 200 mL sample, 11 cm² membrane, and 5 mL stripping solution. This value compares favorably with those obtained by other uphill transport modes under the same conditions.     

Sorption-spectroscopic determination of selenium using a PANV-AV-17 fibrous ion-exchanger

The possibility of determining selenium on the solid phase of polyacrylonitrile fibers impregnated by an AV-17 anion-exchanger ([PANV-AV-17]) were examined by virtue of diffuse reflectance spectroscopy. Reactions of a complex formation between selenium(IV) and organic reagents on solid phase as well as the formation of an elemental selenium sol both on the solid phase and in solution followed by absorption were studied. The best analytical parameters were achieved in the adsorption of selenium sol formed in solution upon the addition of ascorbic acid. The comparison of the batch and dynamic adsorption modes revealed greater advances of the dynamic one. The optimal conditions for determining selenium were proved as follows: the formation of a selenium sol in a 1% ascorbic acid solution at pH 2 and dynamic adsorption at a flow rate of 5 mL/min. A procedure was developed for determining selenium with a limit of detection of 0.1 mg/L. The procedure was validated by the added-found method in the analysis of river and well natural waters and also the standard specimen OSO-200-90, which also contained As, Bi, Sb, and PO₄³⁻. The duration of analysis for 5–6 samples of the volume 100 mL was 30 min approximately, RSD < 20%.     

Highly efficient adsorption of Cr(VI) from aqueous solution by Fe3+ impregnated biochar

Biochar (BC) has been widely used as a low-cost adsorbent for the removal of contaminants from water and soil. However, the adsorption ability of BC towards heavy metal oxyanions (e.g., Cr(VI)) is relatively low due to the negatively charged surface of BC. In this study, pristine BC was impregnated with Fe³⁺ to improve its Cr(VI) adsorption capability. Fe³⁺-impregnated BC (Fe³⁺-BC) was successfully synthesized by a simple impregnation method and used for the removal of Cr(VI) from aqueous solution. Various factors affecting the adsorption, such as impregnation ratio, pH, adsorbent dosage, contact time, temperature, and the presence of humic acid, were investigated in detail. Results showed that Fe³⁺-BC had strong adsorption ability to Cr(VI) with a maximum adsorption capacity of 197.80 mg/g, which were not only significantly higher than that of the pristine BC, but also were superior to many previously reported adsorbents. It was favorable for Cr(VI) adsorption under the condition of acidic and high temperature. The adsorption data obeyed Sips and Langmuir isotherms and the kinetic data were well described by the pseudo-first-order kinetic model. The results herein revealed that the Fe³⁺-impregnated BC had a good potential as a highly efficient material for adsorption of Cr(VI) from aqueous solution.     

Structural and adsorption behaviour of ZnO/aminated SWCNT-COOH for malachite green removal: face-centred central composite design

In this study, an effective adsorbent was synthesized to remove malachite green (MG), which is one of the toxic dyes. Firstly, single walled carbon nanotube with carboxylated acid (SWCNT-COOH) was functionalized with diethylenetriamine and a new nanocomposite was obtained using nano zinc oxide (ZnO) powder. The effects of pH (3–7), the amount of adsorbent (5–15 mg) and the initial concentration (10–50 mg L^–1) of the solution on the adsorption uptake were investigated. The optimal parameters that maximize the adsorption uptake according to the specified working range are found to be 4.63 for pH, 49.94 mg L^–1 for initial concentration, 5.25 mg for the adsorbent dose, and the maximum adsorption capacity has been found as 52.26 mg g^–1. The excellent fitting of the pseudo-second kinetic model with (R² = 0.9912) was fitted the experimental data. The Freundlich isotherm model gave a clue about the type of adsorption. Furthermore, thermodynamic results showed that adsorption process was endothermic.     

Preconcentration of beryllium via octadecyl silica gel microparticles doped with aluminon, and its determination by flame atomic absorption spectrometry

A simple and sensitive method is presented for solid phase extraction (SPE) and preconcentration of trace quantities of beryllium using octadecyl silica gel modifed with aurin tricarboxylic acid (aluminon). Beryllium is then determined by flame atomic absorption spectroscopy. Parameters affecting SPE such as pH, sample solution and eluent flow rate, type, concentration and volume of eluent, interfering ions and breakthrough volume, were investigated. Under optimal conditions, the beryllium ions were retained on the sorbent at pH 6–6.7, while 3.0 mL of 0.05 mol L^?1 HNO₃ is sufficient to elute the ions. The limit of detection (LOD) based on 3σ was 0.8 µg L^?1 for 250 mL sample solution and 5 mL 0.05 mol L^?1 HNO₃ as eluent. The LOD can reach 0.1 µg L^?1 for 1 L sample solution and 3 mL of 0.05 mol L^?1 HNO₃. The accuracy and precision (RSD %) of the method is >90% and <10%, respectively. The method was applied to the determination of beryllium in aqueous samples.     

一个具有eea拓扑和高甲烷存储量的金属有机骨架材料

合成了含有2个羧基和1个N配位点的双官能团有机配体5-（quinolin-6-yl）isophthalic acid （H₂L）,并成功制得一个新的三维的多孔金属-有机骨架{[CuL]·x（Solvent）}_n （1）。金属-有机骨架1具有eea拓扑的网络结构,点（Schläfli）符号为{4².6}₂{4⁴.6².8⁶.10³}。值得一提的是,除去溶剂分子的1还表现出较大的CH₄吸附焓,在298 K和高压下对CH₄有高的吸附量。     

一个具有eea拓扑和高甲烷存储量的金属有机骨架材料

合成了含有2个羧基和1个N配位点的双官能团有机配体5-（quinolin-6-yl）isophthalic acid （H₂L）,并成功制得一个新的三维的多孔金属-有机骨架{[CuL]·x（Solvent）}_n （1）。金属-有机骨架 1具有eea拓扑的网络结构,点（Schläfli）符号为{4².6}₂{4⁴.6².8⁶.10³}。值得一提的是,除去溶剂分子的1还表现出较大的CH₄吸附焓,在298 K和高压下对CH₄有高的吸附量。