摘要
聚丙烯酸钠和富羧基碳化合物表面均含有大量羧基官能团,对重金属及放射性核素有良好的吸附性能,有望在放射性废物的处理中得到应用。近年来,利用磁性纳米材料具有尺寸小、比表面积大、表面活性位点多和在外加磁场作用下快速响应等特性,研究其吸附分离废液中的重金属离子,已受到人们的极大关注。本文制备了磁性聚丙烯酸钠改性有机膨润土纳米复合物(PSA/O-BT-Fe3O4),探讨了该磁性纳米复合物的制备及表征,研究了U(Ⅵ)、Th(Ⅳ)和Eu(Ⅲ)在该复合物上的吸附性能及吸附机理,考察了平衡时间、吸附剂用量、pH、离子强度、腐殖质(富里酸和胡敏酸)和温度等对吸附的影响,通过解吸和再生实验考察了该吸附剂的循环利用性能。本文又制备了磁性富羧基碳复合材料(10ACA-C/Fe3O4),并研究了其对Pb(Ⅱ)、Ni(Ⅱ)、Hg(Ⅱ)和U(Ⅵ)的吸附性能。
第一章介绍了本工作的研究背景以及国内外水凝胶和磁性纳米材料的研究现状与最新进展。
第二章采用共沉淀法制备了磁性有机膨润纳米颗粒(O-BT-Fe3O4),并将其在聚丙烯酸钠溶液中共聚合制备得到磁性聚丙烯酸钠改性有机膨润土纳米复合物(PSA/O-BT-Fe3O4).采用扫描电子显微镜(SEM)、红外光谱分析(FTIR、X射线衍射(XRD)、热重差热分析(TGA)、振动样品磁强计(VSM)、 zeta电位分析以及元素分析等手段对磁性聚丙烯酸钠改性有机膨润土纳米复合物的形貌、磁性、组成、结构以及表面电荷特性等进行了表征,结果表明所合成的材料磁响应性良好,具有良好的热稳定性,表面为强酸性位点。采用溶胀动力学实验测定了该纳米复合物的溶胀动力学,纳米复合物在去离子水和0.2%NaCl溶液中均在60分钟内达到溶胀平衡,纳米复合物在去离子水中的溶胀倍率要远远大于在0.2%NaCl溶液中。
Th(IV)在PSA/OBT-Fe3O42#表面的吸附随固液比的增大而增大；吸附动力学符合准二级动力学模型：pH强烈影响吸附,受离子强度影响较弱,可以推测在低pH值时主要以外层配合作用和/或离子交换作用为主,在较高pH值时主要以内层配合作用和／或表面沉淀为主；HA/FA的存在与否均对Th(Ⅳ)的吸附没有影响；升高温度有利于Th(IV)在PSA/OBT-Fe3O42#上吸附,吸附足吸热过程,吸附反应是自发进行的；具有优良的重复利用性能,从经济性考虑使用0.1mol/L HC1作为洗脱剂最佳,经5次吸附-解吸实验后吸附容量依然高达3.6mmol/g。
U(VI)在PSA/OBT表面上的吸附受pH值、离子强度影响显著,离子强度对U(VI)在PSA/OBT表面上的吸附有促进效应,可以推测U(VI)在PSA/OBT表面以内层配合形式吸附；固液比显著影响吸附,吸附百分数随固液比的增大先增大后减小再增大,吸附量随固液比增大而减小；升高温度有利于U(VI)在PSA/OBT上吸附,吸附是吸热过程,吸附反应自发进行,且吸附等线符合Langmuir模型。吸附前后的红外谱图证实了内层配合物的形成足PSA/OBT作为吸附剂吸附去除U(VI)的主要机理。
Eu(Ⅲ)在PSA/OBT-Fe3O42#上的吸附量随Eu(Ⅲ)初始浓度的增加而增加直到到达最大洗发量,吸附百分数随初始浓度增加而降低,且吸附等温线符合Langmuir模型。
第三章采用水热法合成了富羧基碳(10ACA-C),进一步采用共沉淀法合成了不同配比的磁性富羧基碳复合材料(10ACA-C/Fe3O4)。采用TEM、FTIR、 VSM、XRD、TGA、zeta电位分析及BET等手段读磁性富羧基碳复合材料的形貌、磁性、组成、结构以及表面电荷特性等进行了表征。结果表明所合成的材料磁响应性良好,具有良好的热稳定性,10ACA-C和10ACA-C/Fe3O4在pH大于3.0时表面总体表现为电负性。采用静态法研究了Pb(Ⅱ)、Ni(Ⅱ)、Hg(Ⅱ)和U(Ⅵ)仆磁性富羧基碳复合材料的吸附性能。Pb(Ⅱ)、Ni(Ⅱ)、Hg(Ⅱ)和U(Ⅵ)在：10ACA-C上的吸附容量要高于在10ACA-C/Fe3O42#上。该吸附剂是重金属污水和放射性废液处理领域中极具发展前景的吸附材料。
上述研究结果表明,磁性富羧基碳复合物对金属离子及放射性核素具有吸附速率快、吸附容量大、可循环利用,并且在外加磁场下可以实现与净化介质有效分离等优点,在重金属污水及放射性废液处理等方面具有良好的应用前景。
Poly(sodium acrylate) and carboxylate-rich carbonaceous materials contain carboxylic groups, which has endowed sorbents with very high sorption capacities to heavy metal ions and radionuclides. The application of these carboxylate-rich materials as sorbents for the safety and reasonable treatment of radio-waste is expected. An innovative technology is the use of magnetic materials for magnetic separation of pollutants from effluents rapidly. The unique and attractive property of magnetic carrier materials, is small size, great specific surface area, high surface activity and readily be collected from sample solutions using an external magnetic field. In this work, poly(sodium acrylate)/organo-bentonite-Fe3O4(PSA/OBT-Fe3O4) magnetic superabsorbent nanocomposites were prepared and characterized. The effects on sorption (such as contact time, solid content, pH, ion strengthen, humic substances, temperature etc.) and desorption (the kind and concentration of desorbing agent, recyclability) of U(Ⅵ), Th(Ⅳ) and Eu(Ⅲ) on magnetic nanocomposites was investigated to discuss the sorption behavior and mechanism. Magnetically modified carboxylate-rich carbonaceous composite materials (10ACA-C/Fe3O4) were also prepared, characterized and applied to study the sorption capacities of Pb(Ⅱ), Ni(Ⅱ), Hg(Ⅱ) and U(Ⅵ).
In the first chapter, the curren situation and the latest progress in research of hydrogels and magnetic nanoparticles were briefly reviewed.
In the second chapter, the organo-bentonite-Fe3O4magnetic nanoparticles (O-BT-Fe3O4) were prepared by using co-precipitation technique, then a series of poly(sodium acrylate)/organo-bentonite-Fe3O4(PSA/OBT-Fe3O4) magnetic superabsorbent nanocomposites were prepared by copolymerization reaction of partially neutralized acrylic acid (SA) and organo-bentonite/Fe3O4(OBT-Fe3O4). The morphology, paramagnetic properties, contents, structures and surface charge properties of PSA/OBT-Fe3O4have been characterized by using SEM, FT-IR, XRD, TGA, VSM, zeta potential and ICP-AES. The experimental results showed that the nanocomposites were well responded to magnetic fields, thermodynamic stabilized and strong acid sites on surface. Swelling kinetic of the nanocomposites was measured. The water absorbency sharply increased and the equilibrium swelling was achieved after60min in distilled water and0.2%NaCl, and the higer swelling was obtained in distilled water than0.2%NaCl.
The sorption percentage of Th(Ⅳ) on PSA/OBT-Fe3O42#increases with increasing adsorbent content. Sorption processes can be described accurately by the pseudo-second order rate model. The sorption of Th(Ⅳ) is affected strongly by pH and weakly by sodium ions, which indicated that the ion exchange and/or outer-sphere complexes were the main sorption species at low pH, and inner-sphere and/or surface precipitation complexes dominated at high pH range. The presence of humic substances (HA/FA) have no effect on the soption of Th(Ⅳ). Th(Ⅳ) sorption on PSA/OBT-Fe3O42#is promoted at higher temperature and sorption processes were spontaneous and endothermic. Furthermore, the PSA/OBT-Fe3O4superabsorbent could be regenerated through the desorption of Th(Ⅳ) using0.1mol/L HCI solution and the sorption capacity is still higher than3.6mmol/g after five consecutive sorption-desorption processes.
The sorption of U(Ⅵ) on PSA/OBT was strongly dependent on pH and ionic strength. U(Ⅵ) sorption amount is increasing with salinity growing, inner-sphere complexes dominated U(Ⅵ) sorption on PSA/OBI. The sorption processes were strongly affected by solid-to-liquid ratio (m/V), the sorption percentage increases, decreases and then increase with solid-to-liquid ratio increases, U(Ⅵ) sorption amount is decreasing with solid-to-liquid ratio increases. IJ(Ⅵ) sorption on PSA/OBT is promoted at higher temperature and sorption processes were spontaneous and endothermic. Sorption Isotherms can be fitted accurately by the Langmuir model. FTIR spectra of before and after sorption confirmed that inner-sphere complexes formation is the major mechanism for U(VI) sorption on PSA/OBT.
The sorption amount is increasing with initial Eu(Ⅲ) concentration increases until equilibrium soption was achieved, the sorption percentage of Eu(Ⅲ) on PSA/OBT-Fe3O42#decreases with initial concentration increases. Sorption isotherms can be described by the Langmuir model.
In the third chapter, Carboxylate-rich carbonaceous materials were prepared using hydrothermal, followed by co-precipitation method to obtain magnetic carboxylate-rich carbons. The morphology, paramagnetic properties, contents, structures and surface charge properties of10ACA-C/Fe3O4have been characterized by TEM, FT-IR, VSM, XRD, TGA, zeta potential and BET. The experimental results showed that the composites were thermodynamic stabilized and well magnetic responsiveness. The surface charge of10ACA-C and10ACA-C/Fe3O4is negative at pH>3.0. The sorption behavior of Pb(Ⅱ), Ni(Ⅱ), Hg(Ⅱ) and U(Ⅵ) from aqueous solution to10ACA-C and10ACA-C/Fe3O4was investigated by batch experiment. The sorption capacity of Pb(Ⅱ), Ni(Ⅱ), Hg(Ⅱ) and U(Ⅵ) on10ACA-C is higher than10ACA-C/Fe3O4, and the sorption capacity of Pb(Ⅱ) and Hg(Ⅱ) on10ACA-C and10ACA-C/Fe3O4is higher than Ni(Ⅱ). Magnetic carboxylate-rich carbon is a promising sorption material for water treatment of heavy metal ions and radionuclides.
The results of the present thesis confirmed that magnetic carboxylate-rich composites provides sorbent materials with many advantages like fast response, high capacity, reusability and readily be collected from sample solutions using an external magnetic field for the removal of heavy metal ions and radionuclides from aqueous solution, which indicated that magnetic carboxylate-rich composites have a good prospect in the heavy metal containing sewage as well as nuclear waste treatment.
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