钾位铈掺杂黄钾铁矾的磷吸附特性及机理研究※

doi:10.6023/A21120603

化学学报 ›› 2022, Vol. 80 ›› Issue (4): 476-484.DOI: 10.6023/A21120603 上一篇下一篇

所属专题：中国科学院青年创新促进会合辑

研究论文

钾位铈掺杂黄钾铁矾的磷吸附特性及机理研究^※

刘俊瑞^a^,^b^,^c, 陈晶琳^d, 杨杰^b^,^c, 许肖锋^b^,^c, 李若男^b^,^c, 黄有桂^b^,^c, 陈少华^d, 叶欣^d^,^*(), 王维^b^,^c^,^*()

a 福建师范大学化学与材料学院福州 350007
b 中国科学院福建物质结构研究所中国科学院功能纳米结构设计与组装重点实验室福州 350002
c 中国科学院海西研究院厦门稀土材料研究中心厦门 361021
d 中国科学院城市环境研究所中国科学院城市污染物转化重点实验室厦门 361021

投稿日期:2021-12-30 发布日期:2022-04-28
通讯作者: 叶欣, 王维
作者简介:
^※ 庆祝中国科学院青年创新促进会十年华诞.
基金资助:
中国科学院青年创新促进会专项基金(2021302); 中国科学院青年创新促进会专项基金(2021305); 中国科学院福建物质结构研究所与中国科学院城市环境研究所融合发展基金培育项目(RHZX-2019-003)

K⁺-Site Ce-Doped Jarosite for Phosphate Adsorption: a Mechanism Study^※

Junrui Liu^a^,^b^,^c, Jinglin Chen^d, Jie Yang^b^,^c, Xiaofeng Xu^b^,^c, Ruonan Li^b^,^c, You-Gui Huang^b^,^c, Shaohua Chen^d, Xin Ye^d(), Wei Wang^b^,^c()

a College of Chemistry and Materials Science, Fujian Normal University, Fuzhou 350007, China
b CAS Key Laboratory of Design and Assembly of Functional Nanostructures, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, China
c Xiamen Institute of Rare Earth Materials, Haixi Institute, Chinese Academy of Sciences, Xiamen 361021, China
d CAS Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021, China

Received:2021-12-30 Published:2022-04-28
Contact: Xin Ye, Wei Wang
About author:
^※ Dedicated to the 10th anniversary of the Youth Innovation Promotion Association, CAS.
Supported by:
Youth Innovation Promotion Association CAS(2021302); Youth Innovation Promotion Association CAS(2021305); FJIRSM&IUE Joint Research Fund(RHZX-2019-003)

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摘要/Abstract

黄钾铁矾是一种自然界常见的含铁矿物, 它对砷酸根有一定吸附作用, 但几乎不吸附同样构型的磷酸根. 为了改善黄钾铁矾的磷吸附性质, 本研究制备了铈掺杂的黄钾铁矾, 并采用X射线衍射(XRD)、电感耦合等离子发射光谱(ICP-OES)等表征手段, 构建了铈离子占据钾离子位的结构模型. 磷吸附实验结果表明, 少量铈的掺杂可将黄钾铁矾的磷吸附容量(pH=7, 24 h)从1.69 mg/g显著提升至29.33 mg/g. 同时, 初始pH和共存阴离子对其除磷效果影响较小, 说明含铈黄钾铁矾对磷酸盐的吸附具备高选择性. 进一步分析表明, 该吸附过程符合准二级动力学模型, 吸附等温线符合Freundlich等温吸附模型, 分析结果表明吸附过程可能是易进行的化学吸附. 利用XRD及阴离子交换色谱, 证实了相比于纯黄钾铁矾, 铈的掺杂提高了黄钾铁矾的反应活性, 大幅提升了吸附过程中磷酸根与硫酸根的置换. 通过X射线光电子能谱与红外光谱表征, 推测吸附过程形成稳定的Ce—O—P化学键, 实现特异性化学吸附. 这些研究结果为含磷废水的吸附治理提供了一种新的吸附材料, 并有望为黄钾铁矾的改性和资源化利用提供参考.

关键词: 黄钾铁矾, 稀土掺杂, 吸附, 磷污染, 铈

Jarosite is a common iron-containing mineral. Researchers have studied its application for removing aqueous pollutants, such as Cr(VI) and As(V). Surprisingly, it shows adsorption for arsenates, but little for the structurally similar phosphate ions. In this study, we prepare cerium doped jarosite and prove the successful doping of cerium at the K⁺ site by X-ray diffraction (XRD), inductively coupled plasma-optical emission spectrometry (ICP-OES), energy dispersive spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS). Phosphorus adsorption experiments show that the small amount of cerium doping (Ce content: 8.75×10^-5 mol/g) significantly improves the phosphate adsorption of jarosite, from 1.69 mg/g to 29.33 mg/g (pH=7, 24 h). The phosphate adsorption of Ce-doped jarosite exhibits good pH stability (from pH=3 to pH=11) and excellent selectivity, which is capable of maintaining more than 91% of its adsorption capacity in the presence of various competing anions, such as HCO₃^-, CO₃^2-, humic acid anion, SO₄^2-, NO₃^-, and SiO₃^2-. Further analysis reveals that the adsorption process obeys the pseudo-second order kinetic model while the adsorption isotherms represent the Freundlich isotherm. The analysis indicates that the adsorption may be a chemical adsorption process that is easy to proceed. To explore the mechanism of adsorption enhancement, we first characterize the Zeta-potential of the pure jarosite and Ce-doped jarosite. The result indicates similarity of the surface potential between the two samples, which rules out the electrostatic adsorption mechanism. Next, based on the result of anion exchange chromatography, we confirm that the cerium doping greatly increases the exchange between the sulfate groups in jarosite and the phosphate groups in solution, from 2.85 mg/g to 24.90 mg/g. Finally, XPS high-resolution spectroscopy reveals that the chemical environment of Ce changes after the phosphate adsorption, likely indicating the formation of Ce—O—P chemical bonds to achieve specific chemisorption. These results may provide insights for the modification and application of jarosite, as a new adsorbent material for treating phosphorus rich wastewater.

Key words: jarosite, rare-earth doping, adsorption, phosphate pollutant, cerium

引用此文

刘俊瑞, 陈晶琳, 杨杰, 许肖锋, 李若男, 黄有桂, 陈少华, 叶欣, 王维. 钾位铈掺杂黄钾铁矾的磷吸附特性及机理研究^※[J]. 化学学报, 2022, 80(4): 476-484.

Junrui Liu, Jinglin Chen, Jie Yang, Xiaofeng Xu, Ruonan Li, You-Gui Huang, Shaohua Chen, Xin Ye, Wei Wang. K⁺-Site Ce-Doped Jarosite for Phosphate Adsorption: a Mechanism Study^※[J]. Acta Chimica Sinica, 2022, 80(4): 476-484.

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图/表 12

图1. 黄钾铁矾晶体结构示意图

Figure 1. Crystal structure of jarosite

图2. 黄钾铁矾掺杂铈前后的X射线衍射图谱(XRD)

Figure 2. X-ray diffraction pattern (XRD) of jarosite before and after cerium doping

图3. 黄钾铁矾掺杂铈前后不同2θ角度的X射线衍射高分辨图谱: (a) 12.5°~20.3°、(b) 27.6°~30.4°、(c) 35.8°~44.3°、(d) 45.5°~51.0°、(e) 54.1°~54.8°

Figure 3. Jarosite doped with cerium before and after 2θ X-ray diffraction high resolution mapping of the angle: (a) 12.5°~20.3°, (b) 27.6°~30.4°, (c) 35.8°~44.3°, (d) 45.5°~51.0°, and (e) 54.1°~54.8°

序号	样品名	晶胞参数 a/nm	晶胞参数 b/nm	晶胞参数 c/nm
1	纯黄钾铁矾	0.73198	0.73198	1.70910
2	含铈黄钾铁矾	0.73082	0.73082	1.70024

表1. 掺杂前后黄钾铁矾晶胞参数

Table 1. Unit cell parameters of jarosite before and after doping

图4. 黄钾铁矾掺杂铈前(a)、后(b)扫描电镜图像(SEM); 含铈黄钾铁矾聚集体颗粒的SEM图像(c)及其铈元素EDS信号分布(d)

Figure 4. SEM images of jarosite before (a) and after (b) cerium doping; (c) the SEM image of a cerium-doped jarosite particle and (d) its corresponding Ce EDS mapping

图5. (a)初始pH对黄钾铁矾吸附性能的影响; (b)初始pH对含铈黄钾铁矾吸附性能的影响

Figure 5. (a) Effect of initial pH on the adsorption properties of jarosite; (b) effect of initial pH on the adsorption properties of Ce-doped jarosite

图6. 含铈黄钾铁矾吸附磷酸根的动力学数据及准一级、准二级动力学拟合

Figure 6. Kinetic data and quasi first-order and quasi second-order kinetic fitting of phosphate adsorption by Ce-doped jarosite

图7. 含铈黄钾铁矾磷酸根吸附等温线的Langmuir方程与Freundlich方程拟合曲线图

Figure 7. Fitting curves of Langmuir equation and Freundlich equation for the phosphate adsorption isotherm of cerium doped jarosite

图8. 共存阴离子对含铈黄钾铁矾吸附磷酸根的影响

Figure 8. The effect of coexisting anion on the phosphate adsorption of cerium doped jarosite

图9. (a)纯黄钾铁矾和(b)含铈黄钾铁矾吸附磷酸根前后的XPS全谱图; 含铈黄钾铁矾吸附磷酸根前(c)、后(d)的Ce 3d XPS高分辨谱图

Figure 9. XPS full spectra before and after phosphate adsorption (a) pure jarosite (b) cerium doped jarosite; high resolution Ce3d spectra before (c) and after (d) the phosphate adsorption by cerium doped jarosite

图10. 铈掺杂前后黄钾铁矾表面Zeta电位与pH的关系

Figure 10. Relationship between pH value and Zeta potential of jarosite before and after cerium doping

图11. 黄钾铁矾(a)与含铈黄钾铁矾(b)吸附后滤液中SO42-的沉淀; 含铈黄钾铁矾吸附磷酸根前(c)、后(d)的S 2p高分辨XPS图谱

Figure 11. Precipitation of SO42- from the filtrate after adsorption of jarosite (a) and cerium doped jarosite (b); High resolution S 2p XPS spectra of cerium doped jarosite before (c) and after (d) phosphate adsorption

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钾位铈掺杂黄钾铁矾的磷吸附特性及机理研究^※

K⁺-Site Ce-Doped Jarosite for Phosphate Adsorption: a Mechanism Study^※

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钾位铈掺杂黄钾铁矾的磷吸附特性及机理研究※

K+-Site Ce-Doped Jarosite for Phosphate Adsorption: a Mechanism Study※

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钾位铈掺杂黄钾铁矾的磷吸附特性及机理研究^※

K⁺-Site Ce-Doped Jarosite for Phosphate Adsorption: a Mechanism Study^※