吸附材料的制备及其对重金属离子和染料吸附性能研究
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摘要
随着经济的快速发展，近代工业也取得了长足的发展，而由此引发的环境问题也变的日益严重。尤其是重金属和有机染料的污染引起了人们的广泛关注，这是由于重金属离子不能够分解，在生物体内易累积，再通过食物链进入到人体中，会危害人类的健康。由于有机染料废水中含有大量有毒的有机残留物、酸、碱及无机物而毒害环境，其中有些染料中的对二胺联苯类的有毒化学物质可能会引发癌症和诱导有机突变，有机染料废水排放到水体中不仅会影响水体的美观，而且会降低阳光的透射率从而导致光合作用的减少。因此，能够有效地去除重金属离子和染料变得非常有必要。
油页岩又称为干酪根，是分布在岩石中的一种沉积岩，由碳氢有机化合物构成的固体物质。油页岩被认为是世界上最大的能源之一。近年来,由于石油价格的上升，油页岩被看作是石油的替代能源。然而,在油页岩的燃烧过程中会产生大量的副产品油页岩灰渣，这些灰渣会产生严重的环境问题。因此，非常有必要对灰渣进行妥善处理和利用。目前，一些研究人员致力于使用石油页岩灰作为一种低成本且有效的吸附剂材料来去除废水中的重金属离子。
本文以油页岩灰渣作为原料成功地合成了Na-A沸石，并以合成的沸石作为吸附剂去除水溶液中的重金属离子和有机染料；还以油页岩灰渣中的铝作为铝源，成功地制备了疏水的氧化铝气凝胶。这些工作为油页岩灰渣的综合利用提供了新的方向，具有很大的理论和现实意义。本论文主要进行了以下几方面的工作：
1.以油页岩灰渣为原料成功的制备了Na-A沸石，并对合成的沸石中NaOH/OSA的质量比进行了探索和优化，确定了NaOH/OSA最佳质量比的比值为1.6。并对合成的产品进行了表征，合成的沸石具有立方体结构，平均粒径在2μm左右，由孔径分析表明合成的沸石属于介孔材料，合成沸石的比表面积比油页岩灰渣提高一倍，由此表明此沸石具有作为高效吸附材料的潜力。
2.以合成的Na-A沸石与油页岩灰渣去除水溶液中的重金属离子Cu2+，探讨了吸附剂的浓度及溶液的pH值对吸附的影响，同时也研究了吸附等温线、动力学和热力学，实验结果表明：合成Na-A沸石在去除Cu2+离子溶液时，pH值在5-6最佳；吸附等温线研究表明吸附的过程符合Langmuir吸附等温线，Na-A沸石吸附效果远高于油页岩灰渣吸附效果，Na-A沸石对Cu2+最大吸附量为156.7mg/g，油页岩灰渣的仅为38.9mg/g；动力学结果表明吸附过程符合拟二级动力学过程；热力学数据分析表明ΔG值为负， Δ H值为正，表明吸附过程为自发的吸热过程。
3.以合成的Na-A沸石作为吸附剂去除水溶液中的亚甲基蓝和刚果红，研究了影响吸附的各种因素。通过对吸附等温线的拟合，发现吸附过程符合Langmuir吸附等温方程，计算得到了沸石对亚甲基蓝和刚果红理论的最大吸附量分别为18.73mg/g和31.05mg/g。对实验数据进行拟一级动力学方程和拟二级动力学方程拟合后，计算得到各种参数及相关系数。结果表明：吸附的过程倾向于符合拟二级动力学方程。
4.以油页岩灰渣中的铝作为铝源成功地制备了疏水的氧化铝气凝胶。使用了三甲氧基甲基硅烷(MTMS)和正硅酸乙酯(TEOS)作为改性剂对气凝胶进行疏水改性，且对改性后的性质进行了研究。与未改性前相比，使用MTMS和TEOS改性后的接触角分别为54°和110°。此性能利于其作为吸附剂载体及吸附剂在水处理方面的应用。MTMS及TEOS改性后的气凝胶作为吸附剂去除水溶液中的亚甲基蓝吸附量分别达到了22.36mg/g和24.31mg/g。在去除废水方面有一定应用的潜力。
5.本文还合成了磁性壳聚糖复合材料，并研究了该材料对重金属离子Cu2+和Pb2+的吸附性能，对于Cu2+和Pb2+去除的最佳pH值分别为5.0和6.0，符合Langmuir吸附等温线，最大吸附量分别为64.35mg/g和224.21mg/g。动力学符合拟二级动力学过程，热力学过程属于放热过程。
With the rapid development of economy, the modern industry has made greatdevelopment, and the resulting environmental problems have become increasinglyserious. Especially the contamination of heavy metals and organic dye caused theattention of people because the heavy metal ions can't decompose and introduce thepotential danger of bioaccumulation, which may eventually affect man through thefood chain. Dyes can cause hazards to the environment due to the presence of a largenumber of contaminants like toxic organic residues, acids, bases and inorganiccontaminants. Some of the dyes are carcinogenic and mutagenic because they wereformerly made by hazardous chemicals such as benzidine, metals, etc.. The dischargeof colored wastes into the receiving water bodies not only affects their aestheticnature but also interferes with the transmission of sunlight and therefore reduces thephotosynthetic activity. Therefore, it is very necessary to remove effectively heavymetal ions and dyes from waterbodies.
Oil shale, called kerogen, is a kind of sedimentary rock containing varying amountsof a solid, waxy mixture of hydrocarbon compounds and disseminates throughout the rock. The oil shale is considered one of the largest energy resources in the world. Inrecent years, oil shale has been widely used as an alternative source of energy with theincrease of oil price. However,(the) large quantities of oil shale ash (OSA)(which isa by-product ash) are generated due to the direct combustion process of oil shale. Thiskind of ash is considered a serious environmental problem. Therefore, it is necessaryto make a proper strategy for ash handling, disposal and utilization. At present, someresearchers are focusing on using oil shale ash as a low cost, promising and efficientadsorbent material for the removal of heavy metals and dyes from wastewater.
In the paper, Na-A zeolite was successfully synthesized based on the oil shale ashas raw materials and used as an adsorbent to remove heavy metal ions and dyes fromaqueous solution. Hydrophobic alumina aerogel was also prepared using oil shale ashas aluminum source. This work provided a new direction for the comprehensiveutilization of oil shale ash and had great theoretical and practical significance. Thedetailed novelties of this thesis can be categorized as following:
1. The Na-A zeolite was successfully synthesized by the alkaline fusion methodusing oil shale ash as raw materials. The effect of weight ratio of NaOH/OSA onthe preparation of zeolite was studied. The optimum weight ratio of NaOH/OSAfor synthesizing zeolite is1.6. The synthesized zeolite was characterized by analysis techniques. SEM image shows that the as-synthesized zeolite is cube andits average diameter is about2μm. Pore size distributions reveal that zeolitebelongs to the mesoporous material. The surface area of the synthesized zeolite iscomparatively twice higher than that of the oil shale ash, indicating that the zeolitehas great potential as an efficient adsorption material.
2. The synthesized Na-A zeolite and oil shale ash were used to remove Cu2+ionsfrom aqueous solution. Effects of initial concentration and pH value on theadsorption have been discussed. The adsorption isotherm, kinetics andthermodynamics have also been investigated. The results showed that the optimalpH value for removing Cu2+was about5-6. The adsorption data were fitted withLangmuir model. The maximum adsorption capacities of the obtained zeolite andoil shale ash from Langmuir adsorption isotherm were found to be156.7mg/g and38.9mg/g for Cu2+, respectively. The batch kinetic data fitted with thepseudo-second order equation better. The negative ΔG and positive Δ Hatdifferent temperatures confirmed that the adsorption processes were spontaneousand endothermic.
3. The prepared Na-A zeolite was used to remove methylene blue and congo redfrom aqueous solution. The effects of various factors on adsorption have beenstudied. The experimental data were correlated with the Langmuir model. Themaximum adsorption capacities of methylene blue and congo red were18.73mg/gand31.05mg/g, respectively. Adsorption kinetics data were correlated to thepseudo-first-order and pseudo-second-order equation. The batch kinetic data fittedwith the pseudo-second order equation better.
4. Hydrophobic alumina aerogels were successfully prepared using oil shale ash asalumina source. The effects of methyltrimethoxysilane (MTMS) andtetraethylorthosilicate (TEOS) used as surface modifying agents on thephysicochemical properties of the alumina aerogels were investigated. Comparedwith the unmodified aerogels, the water contact angles of alumina aerogelsfunctionalized with TEOS and MTMS were54°and110°, respectively. Thesurface area of the modified aerogels was higher than that of unmodified aerogels,which has great potential as efficient adsorption material. The maximumadsorption capacities of the modified aerogels and modified with MTMS andTEOS from Langmuir adsorption isotherm were found to be22.36mg/g and24.31mg/g for methylene blue.
5. Magnetic–chitosan composites were synthesized, characterized and were used forthe adsorption Pb2+and Cu2+ions from aqueous solution. The optimum pH value is5.0for Cu2+and6.0for Pb2+.The maximum adsorption capacities of Pb2+and Cu2+ions based on the Langmuir isotherm model were224.21mg/g and64.35mg/g,respectively. Adsorption kinetics data fitted with the pseudo-second orderequation better. The thermodynamic results demonstrated that the adsorptionprocess was exothermic under natural conditions.
油页岩又称为干酪根，是分布在岩石中的一种沉积岩，由碳氢有机化合物构成的固体物质。油页岩被认为是世界上最大的能源之一。近年来,由于石油价格的上升，油页岩被看作是石油的替代能源。然而,在油页岩的燃烧过程中会产生大量的副产品油页岩灰渣，这些灰渣会产生严重的环境问题。因此，非常有必要对灰渣进行妥善处理和利用。目前，一些研究人员致力于使用石油页岩灰作为一种低成本且有效的吸附剂材料来去除废水中的重金属离子。
本文以油页岩灰渣作为原料成功地合成了Na-A沸石，并以合成的沸石作为吸附剂去除水溶液中的重金属离子和有机染料；还以油页岩灰渣中的铝作为铝源，成功地制备了疏水的氧化铝气凝胶。这些工作为油页岩灰渣的综合利用提供了新的方向，具有很大的理论和现实意义。本论文主要进行了以下几方面的工作：
1.以油页岩灰渣为原料成功的制备了Na-A沸石，并对合成的沸石中NaOH/OSA的质量比进行了探索和优化，确定了NaOH/OSA最佳质量比的比值为1.6。并对合成的产品进行了表征，合成的沸石具有立方体结构，平均粒径在2μm左右，由孔径分析表明合成的沸石属于介孔材料，合成沸石的比表面积比油页岩灰渣提高一倍，由此表明此沸石具有作为高效吸附材料的潜力。
2.以合成的Na-A沸石与油页岩灰渣去除水溶液中的重金属离子Cu2+，探讨了吸附剂的浓度及溶液的pH值对吸附的影响，同时也研究了吸附等温线、动力学和热力学，实验结果表明：合成Na-A沸石在去除Cu2+离子溶液时，pH值在5-6最佳；吸附等温线研究表明吸附的过程符合Langmuir吸附等温线，Na-A沸石吸附效果远高于油页岩灰渣吸附效果，Na-A沸石对Cu2+最大吸附量为156.7mg/g，油页岩灰渣的仅为38.9mg/g；动力学结果表明吸附过程符合拟二级动力学过程；热力学数据分析表明ΔG值为负， Δ H值为正，表明吸附过程为自发的吸热过程。
3.以合成的Na-A沸石作为吸附剂去除水溶液中的亚甲基蓝和刚果红，研究了影响吸附的各种因素。通过对吸附等温线的拟合，发现吸附过程符合Langmuir吸附等温方程，计算得到了沸石对亚甲基蓝和刚果红理论的最大吸附量分别为18.73mg/g和31.05mg/g。对实验数据进行拟一级动力学方程和拟二级动力学方程拟合后，计算得到各种参数及相关系数。结果表明：吸附的过程倾向于符合拟二级动力学方程。
4.以油页岩灰渣中的铝作为铝源成功地制备了疏水的氧化铝气凝胶。使用了三甲氧基甲基硅烷(MTMS)和正硅酸乙酯(TEOS)作为改性剂对气凝胶进行疏水改性，且对改性后的性质进行了研究。与未改性前相比，使用MTMS和TEOS改性后的接触角分别为54°和110°。此性能利于其作为吸附剂载体及吸附剂在水处理方面的应用。MTMS及TEOS改性后的气凝胶作为吸附剂去除水溶液中的亚甲基蓝吸附量分别达到了22.36mg/g和24.31mg/g。在去除废水方面有一定应用的潜力。
5.本文还合成了磁性壳聚糖复合材料，并研究了该材料对重金属离子Cu2+和Pb2+的吸附性能，对于Cu2+和Pb2+去除的最佳pH值分别为5.0和6.0，符合Langmuir吸附等温线，最大吸附量分别为64.35mg/g和224.21mg/g。动力学符合拟二级动力学过程，热力学过程属于放热过程。
With the rapid development of economy, the modern industry has made greatdevelopment, and the resulting environmental problems have become increasinglyserious. Especially the contamination of heavy metals and organic dye caused theattention of people because the heavy metal ions can't decompose and introduce thepotential danger of bioaccumulation, which may eventually affect man through thefood chain. Dyes can cause hazards to the environment due to the presence of a largenumber of contaminants like toxic organic residues, acids, bases and inorganiccontaminants. Some of the dyes are carcinogenic and mutagenic because they wereformerly made by hazardous chemicals such as benzidine, metals, etc.. The dischargeof colored wastes into the receiving water bodies not only affects their aestheticnature but also interferes with the transmission of sunlight and therefore reduces thephotosynthetic activity. Therefore, it is very necessary to remove effectively heavymetal ions and dyes from waterbodies.
Oil shale, called kerogen, is a kind of sedimentary rock containing varying amountsof a solid, waxy mixture of hydrocarbon compounds and disseminates throughout the rock. The oil shale is considered one of the largest energy resources in the world. Inrecent years, oil shale has been widely used as an alternative source of energy with theincrease of oil price. However,(the) large quantities of oil shale ash (OSA)(which isa by-product ash) are generated due to the direct combustion process of oil shale. Thiskind of ash is considered a serious environmental problem. Therefore, it is necessaryto make a proper strategy for ash handling, disposal and utilization. At present, someresearchers are focusing on using oil shale ash as a low cost, promising and efficientadsorbent material for the removal of heavy metals and dyes from wastewater.
In the paper, Na-A zeolite was successfully synthesized based on the oil shale ashas raw materials and used as an adsorbent to remove heavy metal ions and dyes fromaqueous solution. Hydrophobic alumina aerogel was also prepared using oil shale ashas aluminum source. This work provided a new direction for the comprehensiveutilization of oil shale ash and had great theoretical and practical significance. Thedetailed novelties of this thesis can be categorized as following:
1. The Na-A zeolite was successfully synthesized by the alkaline fusion methodusing oil shale ash as raw materials. The effect of weight ratio of NaOH/OSA onthe preparation of zeolite was studied. The optimum weight ratio of NaOH/OSAfor synthesizing zeolite is1.6. The synthesized zeolite was characterized by analysis techniques. SEM image shows that the as-synthesized zeolite is cube andits average diameter is about2μm. Pore size distributions reveal that zeolitebelongs to the mesoporous material. The surface area of the synthesized zeolite iscomparatively twice higher than that of the oil shale ash, indicating that the zeolitehas great potential as an efficient adsorption material.
2. The synthesized Na-A zeolite and oil shale ash were used to remove Cu2+ionsfrom aqueous solution. Effects of initial concentration and pH value on theadsorption have been discussed. The adsorption isotherm, kinetics andthermodynamics have also been investigated. The results showed that the optimalpH value for removing Cu2+was about5-6. The adsorption data were fitted withLangmuir model. The maximum adsorption capacities of the obtained zeolite andoil shale ash from Langmuir adsorption isotherm were found to be156.7mg/g and38.9mg/g for Cu2+, respectively. The batch kinetic data fitted with thepseudo-second order equation better. The negative ΔG and positive Δ Hatdifferent temperatures confirmed that the adsorption processes were spontaneousand endothermic.
3. The prepared Na-A zeolite was used to remove methylene blue and congo redfrom aqueous solution. The effects of various factors on adsorption have beenstudied. The experimental data were correlated with the Langmuir model. Themaximum adsorption capacities of methylene blue and congo red were18.73mg/gand31.05mg/g, respectively. Adsorption kinetics data were correlated to thepseudo-first-order and pseudo-second-order equation. The batch kinetic data fittedwith the pseudo-second order equation better.
4. Hydrophobic alumina aerogels were successfully prepared using oil shale ash asalumina source. The effects of methyltrimethoxysilane (MTMS) andtetraethylorthosilicate (TEOS) used as surface modifying agents on thephysicochemical properties of the alumina aerogels were investigated. Comparedwith the unmodified aerogels, the water contact angles of alumina aerogelsfunctionalized with TEOS and MTMS were54°and110°, respectively. Thesurface area of the modified aerogels was higher than that of unmodified aerogels,which has great potential as efficient adsorption material. The maximumadsorption capacities of the modified aerogels and modified with MTMS andTEOS from Langmuir adsorption isotherm were found to be22.36mg/g and24.31mg/g for methylene blue.
5. Magnetic–chitosan composites were synthesized, characterized and were used forthe adsorption Pb2+and Cu2+ions from aqueous solution. The optimum pH value is5.0for Cu2+and6.0for Pb2+.The maximum adsorption capacities of Pb2+and Cu2+ions based on the Langmuir isotherm model were224.21mg/g and64.35mg/g,respectively. Adsorption kinetics data fitted with the pseudo-second orderequation better. The thermodynamic results demonstrated that the adsorptionprocess was exothermic under natural conditions.
引文
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