铵离子交换材料的制备、表征及应用研究
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摘要
氨氮是水质指标中引起水体富营养化和水生生物毒性提高的一种重要污染物。随着污水处理技术的发展,目前去除氨氮的方法很多,各种方法都有其利弊及限制因素。离子交换法以其特有的优点成为近年来研究较多的去除氨氮的新型方法。
本研究以广州茂名高岭土为原料,通过对其改性制备高性能铵离子交换材料,并通过不同改性方法对比,得到最佳改性方法。本文研究了不同因素对铵离子交换容量的影响:高岭土与改性剂的质量比、改性温度、煅烧升温速率、保温时间等。通过铵离子交换容量(CEC)测定,所制备材料的铵离子交换容量大于75 mg/g,可用于水处理过程中氨氮的脱除。
本文通过XRD、SEM、NMR、IR及XPS等表征手段对高岭土的改性过程和改性产物的作用机理进行了探讨分析。XRD结果表明,改性过程改变了高岭土原土的结构,由原来的层状结构变为立方结构;从SEM谱图可以看出高岭土的表观形貌在改性前后发生了很大变化,高岭土原土表观形貌大,呈层片状结构,而改性材料层片状结构消失,颗粒细小,呈分散状态;NMR测定数据显示,样品中骨架Al在改性前后的化学环境发生很大的变化,27Al中大部分六配位变为四配位;29Si在改性前后变化不大,只有少量的层状和枝状硅氧四面体变为链中间硅氧四面体。
本文对材料离子交换过程中影响因素、离子交换动力学过程和离子交换热力学特性进行了研究。从结果可以看出,Langmuir模型与Freundlich模型相比更能反映离子交换规律;准二级动力学模型可以准确的描述铵离子交换材料交换NH_4~+的过程。
由于改性粉体材料直接用于水处理脱除氨氮,会导致固液分离困难,增加处理水的水头损失,不利于工业应用。为了提高材料的实际应用性能,本研究将医药用挤出-滚圆机引入实验,将粉体材料制备成一定粒径的球形多孔颗粒,以方便应用于工业和生活氨氮废水的处理。在颗粒成型工艺中,本文研究了造孔剂种类选择、造孔剂加入量、煅烧升温速率、煅烧温度、保温时间、退火降温速率等对颗粒成型及离子交换性能影响。
Ammonia nitrogen is an important contamination in the index of water quality which can promote eutrophication in receiving waters and increased toxicity to aquatic life. With the development of sewage treatment technology, a number of methods are now available for the elimination of ammonia nitrogen. Due to its unique advantages, ion exchange method has become the topic of many recent researches.
In this paper, kaolin produced in Maoming of Guangzhou Province is used as the raw material and modified to prepare a high-performance ammonium ion-exchange material. We got the best method according to the comparing of different methods and this modified method was optimized. The effect of different factors on ammonium removal efficiency of the material is studied, including the mass ratio between kaolin and alkali, modified temperature, heating rate and holding time. According to cation exchange capacity (CEC) measurement, the prepared ammonium ion exchange material has an ammonium ion exchange capacity greater than 75 mg /g and can be used to remove ammonia nitrogen in water treatment.
XRD, SEM, NMR, IR and XPS analysis are used to discuss and analyze the modification process of kaolin and the modification results of an ammonia ion exchange material. The measurement result of XRD show the samdwich of Kaolin material has changed during modified, layer space was smaller than before. The measurement result of SEM show apparent appearance of Kaolin before modified and after has been changed a lot, the former samdwich become small granule product. NMR data indicates that 27Al is mainly converted from hexa-coordinated Al to tetra-coordinated Al during the modification. Compared with that of the original kaolin, 29Si in the modified kaolin does not have obvious change in the average chemical environment except that a small part of the laminated and dendritic silicon-oxygen tetrahedrons are turned into inter-chain silicon-oxygen tetrahedrons.
Then we discussed the adsorption process, kinetics, thermodynamics and desorption conditions. A comparison of the data with Langmuir and Freundlich isotherm models shows a good correlation the Langmuir model describes the process more accurately. And the adsorption process of ammonia nitrogen in water with the ammonium ion exchange material closely matches the pseudo-second-order reaction.
However, when the modified powder material is directly used in water treatment to remove ammonia nitrogen, it will cause difficulty in solid-liquid separation and more head loss of treated water, which are unfavorable for industrial application. In order to improve actual performance of the material in application, a pharmaceutical extruder-rounder is used to turn the powder material into spherical grains of a certain grain size in order to facilitate its application in the treatment of industrial and domestic ammonia nitrogen wastewater.
本研究以广州茂名高岭土为原料,通过对其改性制备高性能铵离子交换材料,并通过不同改性方法对比,得到最佳改性方法。本文研究了不同因素对铵离子交换容量的影响:高岭土与改性剂的质量比、改性温度、煅烧升温速率、保温时间等。通过铵离子交换容量(CEC)测定,所制备材料的铵离子交换容量大于75 mg/g,可用于水处理过程中氨氮的脱除。
本文通过XRD、SEM、NMR、IR及XPS等表征手段对高岭土的改性过程和改性产物的作用机理进行了探讨分析。XRD结果表明,改性过程改变了高岭土原土的结构,由原来的层状结构变为立方结构;从SEM谱图可以看出高岭土的表观形貌在改性前后发生了很大变化,高岭土原土表观形貌大,呈层片状结构,而改性材料层片状结构消失,颗粒细小,呈分散状态;NMR测定数据显示,样品中骨架Al在改性前后的化学环境发生很大的变化,27Al中大部分六配位变为四配位;29Si在改性前后变化不大,只有少量的层状和枝状硅氧四面体变为链中间硅氧四面体。
本文对材料离子交换过程中影响因素、离子交换动力学过程和离子交换热力学特性进行了研究。从结果可以看出,Langmuir模型与Freundlich模型相比更能反映离子交换规律;准二级动力学模型可以准确的描述铵离子交换材料交换NH_4~+的过程。
由于改性粉体材料直接用于水处理脱除氨氮,会导致固液分离困难,增加处理水的水头损失,不利于工业应用。为了提高材料的实际应用性能,本研究将医药用挤出-滚圆机引入实验,将粉体材料制备成一定粒径的球形多孔颗粒,以方便应用于工业和生活氨氮废水的处理。在颗粒成型工艺中,本文研究了造孔剂种类选择、造孔剂加入量、煅烧升温速率、煅烧温度、保温时间、退火降温速率等对颗粒成型及离子交换性能影响。
Ammonia nitrogen is an important contamination in the index of water quality which can promote eutrophication in receiving waters and increased toxicity to aquatic life. With the development of sewage treatment technology, a number of methods are now available for the elimination of ammonia nitrogen. Due to its unique advantages, ion exchange method has become the topic of many recent researches.
In this paper, kaolin produced in Maoming of Guangzhou Province is used as the raw material and modified to prepare a high-performance ammonium ion-exchange material. We got the best method according to the comparing of different methods and this modified method was optimized. The effect of different factors on ammonium removal efficiency of the material is studied, including the mass ratio between kaolin and alkali, modified temperature, heating rate and holding time. According to cation exchange capacity (CEC) measurement, the prepared ammonium ion exchange material has an ammonium ion exchange capacity greater than 75 mg /g and can be used to remove ammonia nitrogen in water treatment.
XRD, SEM, NMR, IR and XPS analysis are used to discuss and analyze the modification process of kaolin and the modification results of an ammonia ion exchange material. The measurement result of XRD show the samdwich of Kaolin material has changed during modified, layer space was smaller than before. The measurement result of SEM show apparent appearance of Kaolin before modified and after has been changed a lot, the former samdwich become small granule product. NMR data indicates that 27Al is mainly converted from hexa-coordinated Al to tetra-coordinated Al during the modification. Compared with that of the original kaolin, 29Si in the modified kaolin does not have obvious change in the average chemical environment except that a small part of the laminated and dendritic silicon-oxygen tetrahedrons are turned into inter-chain silicon-oxygen tetrahedrons.
Then we discussed the adsorption process, kinetics, thermodynamics and desorption conditions. A comparison of the data with Langmuir and Freundlich isotherm models shows a good correlation the Langmuir model describes the process more accurately. And the adsorption process of ammonia nitrogen in water with the ammonium ion exchange material closely matches the pseudo-second-order reaction.
However, when the modified powder material is directly used in water treatment to remove ammonia nitrogen, it will cause difficulty in solid-liquid separation and more head loss of treated water, which are unfavorable for industrial application. In order to improve actual performance of the material in application, a pharmaceutical extruder-rounder is used to turn the powder material into spherical grains of a certain grain size in order to facilitate its application in the treatment of industrial and domestic ammonia nitrogen wastewater.
引文
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