锆改性凹凸棒石及锆/铝/铈体系复合除氟材料的制备及其除氟性能研究
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摘要
氟在阻止人体骨骼及一些器官疾病方面有着重要的作用。然而过量摄入氟会导致牙齿和骨骼疾病。世界卫生组织的标准规定,饮用水中氟离子浓度应不超过1.5mg/L,中国安全饮用水中氟离子浓度规定要小于1.0mg/L。在众多除氟方法中,吸附法因简单、方便而成为应用最广泛的方法之一。然而,现有的吸附剂大多数存在吸附量低、吸附缓慢以及最优pH值范围较窄等问题,虽然价格低廉,但依旧限制了它们的应用。因此,研究开发具有较高吸附容量、较快吸附速率以及较宽最优pH值范围的吸附剂成为一个亟待解决的问题。为解决上述这些技术问题,本文使用简单易行的方法制备了锆改性凹凸棒石(Zr-A)和锆／铝／铈体系(Zr-A1-Ce)两种复合除氟材料。通过大量实验,研究了其制备工艺条件,结合其结构及性能的表征,获得了较常规吸附剂具有更好吸附性能的除氟材料。
使用XRD、FT-IR、SEM以及EDAX对锆改性凹凸棒石复合材料进行分析。结果表明,改性过程中,凹凸棒石的结构被破坏到一定的程度,纳米氧化锆粒子成功进入到凹凸棒石的层间或者表面。Zr-A吸附剂的除氟性能大大优于凹凸棒石原土的除氟性能,这主要是由Zr-A吸附剂表面电性的改变以及生成大量羟基离子造成的。溶液pH值控制了氟离子在固-液界面的吸附,因此对氟离子的吸附具有重要意义。氟离子通过离子交换吸附到吸附剂表面。
Zr-A吸附剂对氟离子的吸附平衡数据较好地符合Langmuir吸附模型。溶液pH值为4.13,50℃下,按此模型计算出的最大吸附量为24.55mg/g。吸附过程符合准二级动力学模型。磷酸根离子、硫酸根离子以及碳酸氢根离子对吸附氟离子效果具有一定的影响,但是氯离子和硝酸根离子对吸附效果没有影响。该材料再生利用六次后,依然具有较高的吸附量。吸附及重复利用实验表明,Zr-A吸附剂可以成为一种有潜力的饮用水除氟剂。
从实际应用角度出发,对Zr-A吸附剂进行了造粒和固定床吸附实验。Zr-A颗粒吸附剂的最佳制各条件为,粘结剂浓度为10wt.%,热处理温度为70℃C。实验结果表明,固定床进水流量越小,穿透吸附量越大；初始氟离子浓度越大,穿透吸附量越大。Zr-A颗粒吸附剂经过五次再生和重复利用后,仍具有较好的吸附效果。
XRD和ζ电位分析结果表明,Zr-Al-Ce复合材料不是Zr02、A1203和Ce02的简单复合。FT-IR分析表明吸附剂表面的羟基离子参与到了反应中；XPS分析证明,参与反应的羟基离子来自于吸附剂表面与金属相结合的-OH而并非是归属于油酸的C-OH。
Zr-Al-Ce吸附剂对氟离子的吸附平衡数据符合Langmuir吸附模型。溶液pH值为6.80±0.20,30℃C下,按照Langmuir吸附模型计算出的最大吸附量为250.0mg/g,说明该吸附剂具有很高的吸附容量。
热力学研究表明,Zr-Al-Ce吸附剂对氟离子吸附过程为自发、吸热过程。吸附过程符合准二级动力学模型。共存阴离子对Zr-Al-Ce吸附剂除氟效果的影响按以下顺序递减,P043->HC03->S042->N03->C1-。Zr-Al-Ce吸附剂再生利用三次后,依然具有较高的吸附量。吸附和重复利用实验表明,Zr-Al-Ce吸附剂可以成为一种较有潜力的饮用水除氟剂。
造粒实验表明,Zr-Al-Ce颗粒吸附剂的最佳制备条件为,Zr-Al-Ce和凹凸棒石的质量比为1：2,粘结剂浓度为15wt.%,热处理温度为80℃。固定床吸附实验证明,固定床进水流量越小,穿透吸附量越大；初始氟离子浓度越大,穿透吸附量越大。Zr-Al-Ce颗粒吸附剂经过再生和重复利用后,穿透吸附量只下降了8%,说明所制备的Zr-Al-Ce颗粒吸附剂具有较强的吸附性能,可以成为一种较有潜力的饮用水除氟剂。
Excess fluoride in bodies of water can lead to dental, skeletal, and nonskeletal forms of endemic public health problem. According to the WHO standards, the permissible limit of fluoride ions in drinking water is1.5mg/L. Chinese drinking water standard for it has been amended to lowering fluoride content in the in drinking water to less than1.0mg/L. Among some treatment technologies, adsorption because of its simplicity and conveniency, is still one of the most extensively used methods. Unfortunately, low adsorption capacities, slow adsorption processes and narrow optimum pH ranges of the most materials, though cheap, limit their practical applications. Therefore, an adsorbent with high fluoride adsorption capacity, fast adsorption processes and wide some optimum pH ranges is desired. In order to solve the above-mentioned technique problems, in the present paper, zirconium modified attapulgite (Zr-A) and Zr/Al/Ce system (Zr-Al-Ce) adsorbents were prepared by simple methods. The optimization preparation processes were carried out and the results showed that the Zr-A and Zr-Al-Ce adsorbents showed higher adsorption capacities in comparision with other adsorbents.
The Zr-A composite adsorbent was characterized by XRD, FT-IR, SEM and ED AX analyses showed that the structure of attapulgite was destroyed to some extent during the modification process and the ZrO2nanoparticles were formed in the interlayers of attapulgite or on the surface of attapulgite. The fluoride adsorption capacity of the Zr-A adsorbent was higher in comparison with attapulgite, which was due to the changes of the surface charge of the adsorbent and the generation of abundant hydroxyl ions. The solution pH is very important for fluoride adsorption, which controls the adsorption of fluoride at the absorbent-water interface. Fluoride was adsorbed on the adsorbent via the ion-exchange mechanism.
The adsorption data were better represented by the Langmuir isotherm than the Freundlich isotherm. A Langmuir maximum adsorption capacity of24.55mg/g was obtained at an initial pH of3.14and temperature of30℃. The adsorption process followed the pseudo-second-order model for fluoride. The fluoride adsorption was influenced by the phosphate, sulfate and bicarbonate ions, but not by the chloride and nitrate ions. After six regeneration and reuse cycles, the Zr-A adsorbent still showed high adsorption capacity. The results of adsorption and reuse experiments indicated that the Zr-A adsorbent could be employed as a promising adsorbent for fluoride adsorption from drinking water.
From a practical perspective, the Zr-A adsorbent granulation and fixed-bed adsorption experiments were carried out. The optimal preparation conditions of the granular Zr-A adsorbent were as follows, the concentration of the caking agent was10wt.%and the heating temperature was70℃. The fixed-bed adsorption results indicated that the breakthrough capacity of the granular Zr-A adsorbent increased with the decrease of the water discharge and the increase of the initial fluoride concentration. After five regeneration cycles, the Zr-A adsorbent still showed high adsorption capacity.
XRD and ζ analysis indicated that the Zr-Al-Ce composite was not a simple mixture of the ZrO2, Al2O3and CeO2. FT-IR analysis indicated that the hydroxyl groups on the adsorbent surface were involved in the fluoride adsorption. XPS analysis demonstrated that the hydroxyl groups bonded to metal (M-OH) were involved in fluoride adsorption but not the hydroxyl groups attributed to oleic acid (C-OH).
The fluoride adsorption data on the Zr-Al-Ce adsorbent agreed well with the Langmuir mode. A Langmuir maximum adsorption capacity of250.0mg/g was obtained at an initial pH of6.80±0.20and temperature of30℃, which indicates that the Zr-Al-Ce adsorbent has a high fluoride adsorption capacity. The thermodynamic studies indicated that the adsorption process was spontaneous and endothermic. The adsorption process followed the pseudo-second-order model for fluoride. The effects of co-existing anions on the sorption of fluoride followed the decreasing order of PO43-> SO42-> HCO3-> NO3-> CI-. The Zr-Al-Ce adsorbent still showed high adsorption capacity after three regeneration and reuse cycles. The results of adsorption and reuse experiments indicated that the Zr-Al-Ce adsorbent could be employed as a promising adsorbent for fluoride adsorption from drinking water.
The granulation experiments indicated that the optimal preparation conditions of the Zr-Al-Ce granular adsorbent were as follows, the mass ratio of the Zr-Al-Ce adsorbent to attapulgite was1:2, the concentration of the caking agent was15wt.%, and the heating temperature was80℃. The fixed-bed adsorption results indicated that the breakthrough capacity of the granular Zr-Al-Ce adsorbent increased with the increase of the initial fluoride concentration and the decrease of the water discharge. After regeneration and reuse experiments, the breakthrough capacity of the granular Zr-Al-Ce adsorbent was just decreased about8%, which indicated that the granular Zr-Al-Ce adsorbent had a good adsorption property and could be employed as a promising adsorbent for fluoride adsorption from drinking water.
使用XRD、FT-IR、SEM以及EDAX对锆改性凹凸棒石复合材料进行分析。结果表明,改性过程中,凹凸棒石的结构被破坏到一定的程度,纳米氧化锆粒子成功进入到凹凸棒石的层间或者表面。Zr-A吸附剂的除氟性能大大优于凹凸棒石原土的除氟性能,这主要是由Zr-A吸附剂表面电性的改变以及生成大量羟基离子造成的。溶液pH值控制了氟离子在固-液界面的吸附,因此对氟离子的吸附具有重要意义。氟离子通过离子交换吸附到吸附剂表面。
Zr-A吸附剂对氟离子的吸附平衡数据较好地符合Langmuir吸附模型。溶液pH值为4.13,50℃下,按此模型计算出的最大吸附量为24.55mg/g。吸附过程符合准二级动力学模型。磷酸根离子、硫酸根离子以及碳酸氢根离子对吸附氟离子效果具有一定的影响,但是氯离子和硝酸根离子对吸附效果没有影响。该材料再生利用六次后,依然具有较高的吸附量。吸附及重复利用实验表明,Zr-A吸附剂可以成为一种有潜力的饮用水除氟剂。
从实际应用角度出发,对Zr-A吸附剂进行了造粒和固定床吸附实验。Zr-A颗粒吸附剂的最佳制各条件为,粘结剂浓度为10wt.%,热处理温度为70℃C。实验结果表明,固定床进水流量越小,穿透吸附量越大；初始氟离子浓度越大,穿透吸附量越大。Zr-A颗粒吸附剂经过五次再生和重复利用后,仍具有较好的吸附效果。
XRD和ζ电位分析结果表明,Zr-Al-Ce复合材料不是Zr02、A1203和Ce02的简单复合。FT-IR分析表明吸附剂表面的羟基离子参与到了反应中；XPS分析证明,参与反应的羟基离子来自于吸附剂表面与金属相结合的-OH而并非是归属于油酸的C-OH。
Zr-Al-Ce吸附剂对氟离子的吸附平衡数据符合Langmuir吸附模型。溶液pH值为6.80±0.20,30℃C下,按照Langmuir吸附模型计算出的最大吸附量为250.0mg/g,说明该吸附剂具有很高的吸附容量。
热力学研究表明,Zr-Al-Ce吸附剂对氟离子吸附过程为自发、吸热过程。吸附过程符合准二级动力学模型。共存阴离子对Zr-Al-Ce吸附剂除氟效果的影响按以下顺序递减,P043->HC03->S042->N03->C1-。Zr-Al-Ce吸附剂再生利用三次后,依然具有较高的吸附量。吸附和重复利用实验表明,Zr-Al-Ce吸附剂可以成为一种较有潜力的饮用水除氟剂。
造粒实验表明,Zr-Al-Ce颗粒吸附剂的最佳制备条件为,Zr-Al-Ce和凹凸棒石的质量比为1：2,粘结剂浓度为15wt.%,热处理温度为80℃。固定床吸附实验证明,固定床进水流量越小,穿透吸附量越大；初始氟离子浓度越大,穿透吸附量越大。Zr-Al-Ce颗粒吸附剂经过再生和重复利用后,穿透吸附量只下降了8%,说明所制备的Zr-Al-Ce颗粒吸附剂具有较强的吸附性能,可以成为一种较有潜力的饮用水除氟剂。
Excess fluoride in bodies of water can lead to dental, skeletal, and nonskeletal forms of endemic public health problem. According to the WHO standards, the permissible limit of fluoride ions in drinking water is1.5mg/L. Chinese drinking water standard for it has been amended to lowering fluoride content in the in drinking water to less than1.0mg/L. Among some treatment technologies, adsorption because of its simplicity and conveniency, is still one of the most extensively used methods. Unfortunately, low adsorption capacities, slow adsorption processes and narrow optimum pH ranges of the most materials, though cheap, limit their practical applications. Therefore, an adsorbent with high fluoride adsorption capacity, fast adsorption processes and wide some optimum pH ranges is desired. In order to solve the above-mentioned technique problems, in the present paper, zirconium modified attapulgite (Zr-A) and Zr/Al/Ce system (Zr-Al-Ce) adsorbents were prepared by simple methods. The optimization preparation processes were carried out and the results showed that the Zr-A and Zr-Al-Ce adsorbents showed higher adsorption capacities in comparision with other adsorbents.
The Zr-A composite adsorbent was characterized by XRD, FT-IR, SEM and ED AX analyses showed that the structure of attapulgite was destroyed to some extent during the modification process and the ZrO2nanoparticles were formed in the interlayers of attapulgite or on the surface of attapulgite. The fluoride adsorption capacity of the Zr-A adsorbent was higher in comparison with attapulgite, which was due to the changes of the surface charge of the adsorbent and the generation of abundant hydroxyl ions. The solution pH is very important for fluoride adsorption, which controls the adsorption of fluoride at the absorbent-water interface. Fluoride was adsorbed on the adsorbent via the ion-exchange mechanism.
The adsorption data were better represented by the Langmuir isotherm than the Freundlich isotherm. A Langmuir maximum adsorption capacity of24.55mg/g was obtained at an initial pH of3.14and temperature of30℃. The adsorption process followed the pseudo-second-order model for fluoride. The fluoride adsorption was influenced by the phosphate, sulfate and bicarbonate ions, but not by the chloride and nitrate ions. After six regeneration and reuse cycles, the Zr-A adsorbent still showed high adsorption capacity. The results of adsorption and reuse experiments indicated that the Zr-A adsorbent could be employed as a promising adsorbent for fluoride adsorption from drinking water.
From a practical perspective, the Zr-A adsorbent granulation and fixed-bed adsorption experiments were carried out. The optimal preparation conditions of the granular Zr-A adsorbent were as follows, the concentration of the caking agent was10wt.%and the heating temperature was70℃. The fixed-bed adsorption results indicated that the breakthrough capacity of the granular Zr-A adsorbent increased with the decrease of the water discharge and the increase of the initial fluoride concentration. After five regeneration cycles, the Zr-A adsorbent still showed high adsorption capacity.
XRD and ζ analysis indicated that the Zr-Al-Ce composite was not a simple mixture of the ZrO2, Al2O3and CeO2. FT-IR analysis indicated that the hydroxyl groups on the adsorbent surface were involved in the fluoride adsorption. XPS analysis demonstrated that the hydroxyl groups bonded to metal (M-OH) were involved in fluoride adsorption but not the hydroxyl groups attributed to oleic acid (C-OH).
The fluoride adsorption data on the Zr-Al-Ce adsorbent agreed well with the Langmuir mode. A Langmuir maximum adsorption capacity of250.0mg/g was obtained at an initial pH of6.80±0.20and temperature of30℃, which indicates that the Zr-Al-Ce adsorbent has a high fluoride adsorption capacity. The thermodynamic studies indicated that the adsorption process was spontaneous and endothermic. The adsorption process followed the pseudo-second-order model for fluoride. The effects of co-existing anions on the sorption of fluoride followed the decreasing order of PO43-> SO42-> HCO3-> NO3-> CI-. The Zr-Al-Ce adsorbent still showed high adsorption capacity after three regeneration and reuse cycles. The results of adsorption and reuse experiments indicated that the Zr-Al-Ce adsorbent could be employed as a promising adsorbent for fluoride adsorption from drinking water.
The granulation experiments indicated that the optimal preparation conditions of the Zr-Al-Ce granular adsorbent were as follows, the mass ratio of the Zr-Al-Ce adsorbent to attapulgite was1:2, the concentration of the caking agent was15wt.%, and the heating temperature was80℃. The fixed-bed adsorption results indicated that the breakthrough capacity of the granular Zr-Al-Ce adsorbent increased with the increase of the initial fluoride concentration and the decrease of the water discharge. After regeneration and reuse experiments, the breakthrough capacity of the granular Zr-Al-Ce adsorbent was just decreased about8%, which indicated that the granular Zr-Al-Ce adsorbent had a good adsorption property and could be employed as a promising adsorbent for fluoride adsorption from drinking water.
引文
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