Eu（Ⅲ）和Am（Ⅲ）在红壤及膨润土上的吸附行为研究
摘要
在核能利用的过程中,不仅要考虑到如何提高核能利用效率,还要充分考虑核燃料利用后的高放废物处置问题和放射性核素对环境可能造成的风险问题,因此研究放射性核素在粘土及缓冲回填材料上的吸附-迁移行为,就成为核能利用和核能安全领域重要的基础性课题。
本文将作为核能利用重点地区之一的中国南方地区红壤和高放废物处置建设中的重要缓冲回填材料——膨润土作为研究对象,通过制备不同组成成分和类型的固体吸附剂,研究吸附过程中不同组分对吸附的影响,揭示吸附的一般规律；重点考察吸附过程中的影响因素——pH、离子强度、腐殖酸(HA)、温度等——对吸附的影响,探讨了吸附行为的特点；讨论了两种核素在不同吸附体系的形态分布对吸附行为的影响,以形态分布研究建立起宏观与微观的联系。
(1)采集并制备三种红壤样品,分别对天然红壤、去氧化铁成分红壤、去有机质红壤吸附Eu(Ⅲ)的行为进行研究。以SEM、XRD等分析手段对吸附反应前后的样品进行表征,考察各样品的元素组成、矿物结构和表面形貌等。
(2)制备Na基膨润土,并对其吸附Am(Ⅲ)的特性进行研究；制备Ca基膨润土,对其吸附Eu(Ⅲ)的特点进行研究。分别以SEM、XRD、EDS等对两种膨润土在吸附反应后的样品进行表征,考察不同类型膨润土的吸附特性。
(3)研究了pH、离子强度对核素吸附的影响。结果表明,Eu(Ⅲ)在三种红壤样品上的吸附受pH值和离子强度影响较大,在pH<7时,吸附随pH值的升高而增强,且在pH>7后基本维持不变；同一pH下,随着溶液中离子强度增加,Eu(Ⅲ)的吸附率会逐渐降低,即高离子强度抑制吸附进行；Am(Ⅲ)在Na基膨润土上的吸附,及Eu(Ⅲ)在Ca基膨润土上的吸附规律与上述结果基本相同,只是在低离子强度下,两种膨润土吸附核素的pH边界会显著降低至pH2～4。
(4)研究了接触时间对核素吸附的影响。Eu(Ⅲ)在红壤上的吸附达到吸附-解吸平衡的时间约为4-12小时,其中去氧化铁成分红壤能够最快达到吸附平衡,而其在25℃的准二级吸附反应速率常数k2’和吸附量qe也最大。Am(Ⅲ)在Na基膨润土及Eu(Ⅲ)在Ca基膨润土上吸附平衡时间均较短,约为4小时,其反应速率常数k2’均为负值,说明吸附反应在初始阶段较快,随着时间推移,反应速率反而有所下降。以上吸附反应动力学可以被准二级动力学模型所描述。
(5)研究了腐殖酸对核素吸附的影响。在较低pH下,HA对核素吸附基本上都能起到促进作用,而在较高pH下,HA对Eu(Ⅲ)在红壤上的吸附促进作用相对有限,而对Am(Ⅲ)和Eu(Ⅲ)在膨润土上的吸附却起到抑制作用,特别是较高pH下Am(Ⅲ)在Na基膨润土上的吸附在pH7-7.5存在一个低点,说明Am(Ⅲ)与Eu(Ⅲ)在HA存在下的吸附形态有所不同,进一步说明核素存在形态对吸附有显著影响。
(6)研究了温度对核素吸附的影响,绘制了Eu(Ⅲ)与Am(Ⅲ)在不同温度下在不同吸附剂上的吸附等温线,并计算了各体系的热力学函数△G0、△S0和△H0。由热力学函数计算结果,可见核素在吸附剂上的吸附一般是吸热且自发的过程,即高温有利于吸附反应进行,只是Eu(Ⅲ)在三种红壤上的吸附随着温度的升高存在放热的过程,即在一定区间高温反而不利于吸附反应进行。上述过程吸附等温线符合Freundlich吸附模型。
The safe disposal of radioactive waste is paid more and more attention in worldwide, so it is very important to study the sorption activity of radioactive nuclides on clays and buffer/backfill materials.
High level radioactive wastes have the characters of long half-life, high toxicity, complex chemical behavior, make the study of sorption and transference on these transuraniums in natural medium be more important. As a clay mineral, red earth has many sorption characteristics such as ion exchange capability, expanding capacity, highly capable of adsorbing pollutants and self-purification functions, therefore clay minerals have the capacity for controlling environmental pollution. Bentonite is the first choice for buffer/backfill materials, so the investigation of sorption of radionuclides on bentonite is nonnegligible. This research put the focus on the speciation of radionuclides sorption on red earth and bentonite, and the effect factors of sorption such as pH, ionic strength, humic acid(HA), temperatures and so on. The main research contents are:
(1) Prepared three red earth samples:natural red earth(NRE), inorganic components removed red earth(ICRRE) and organic matter removed red earth(OMRRE), studied the sorption of Eu(Ⅲ) on red earth samples, and characterized these samples using XRD, SEM etc, investigated the chemical compositions, mineral structures and surface morphology of the samples.
(2) Prepared two different type of bentonite:Na-bentonite and Ca-bentonite, characterized these samples using XRD, SEM, EDS etc, and studied sorption of Am(Ⅲ) on Na-bentonite and sorption of Eu(Ⅲ) on Ca-bentonite.
(3) Investigated sorption of radionuclides on red earth and bentonite samples as a function of pH and ionic strength. The results showed that the sorption of radionuclides is strongly depended on the pH and ionic strength. The sorption increases with increasing pH values at pH<7, and then maintains a high level at pH>7. Ion exchange or outer-sphere surface complexation may be the main sorption mechanism of Am(Ⅲ) on bentonite at pH<7, whereas inner-sphere surface complexation may be the main sorption mechanism at pH>7.
(4) Researched sorption of radionuclides on red earth and bentonite samples as a function of contact time. The sorption was quickly to achieve the sorption equilibration, and the time to achieve the sorption equilibrium was about4～12hours; The sorption of Eu(Ⅲ) on ICRRE was fastest to achieve equilibrium in the three red earth samples and its adsorption capacity was the largest. The kinetic sorption of radionuclides on red earth and bentonite samples could be described well by a pseudo-second-order model.
(5) Studied the influence of HA for the sorption of radionuclides on red earth and bentonite samples. The presence of HA enhances the sorption of radionuclides on the adsorbents at low pH values, and reduces the sorption at high pH values, while there was a valley at pH7～7.5in the sorption progress of Am(Ⅲ) on Na-bentonite. This result suggests that the sorption is significantly influenced by the speciation of radionuclides.
(6) Studied sorption of radionuclides on adsorbents as a function of temperature and calculated thermodynamic parameters (△G0,△S0, and△H0). The sorption of radionuclides on adsorbents was an endothermic and spontaneous process, and an endothermic process in lower temperature range and exothermic process in higher temperature range for the red earth samples. The sorption isotherms of radionuclides could be described by Freundlich model.
本文将作为核能利用重点地区之一的中国南方地区红壤和高放废物处置建设中的重要缓冲回填材料——膨润土作为研究对象,通过制备不同组成成分和类型的固体吸附剂,研究吸附过程中不同组分对吸附的影响,揭示吸附的一般规律；重点考察吸附过程中的影响因素——pH、离子强度、腐殖酸(HA)、温度等——对吸附的影响,探讨了吸附行为的特点；讨论了两种核素在不同吸附体系的形态分布对吸附行为的影响,以形态分布研究建立起宏观与微观的联系。
(1)采集并制备三种红壤样品,分别对天然红壤、去氧化铁成分红壤、去有机质红壤吸附Eu(Ⅲ)的行为进行研究。以SEM、XRD等分析手段对吸附反应前后的样品进行表征,考察各样品的元素组成、矿物结构和表面形貌等。
(2)制备Na基膨润土,并对其吸附Am(Ⅲ)的特性进行研究；制备Ca基膨润土,对其吸附Eu(Ⅲ)的特点进行研究。分别以SEM、XRD、EDS等对两种膨润土在吸附反应后的样品进行表征,考察不同类型膨润土的吸附特性。
(3)研究了pH、离子强度对核素吸附的影响。结果表明,Eu(Ⅲ)在三种红壤样品上的吸附受pH值和离子强度影响较大,在pH<7时,吸附随pH值的升高而增强,且在pH>7后基本维持不变；同一pH下,随着溶液中离子强度增加,Eu(Ⅲ)的吸附率会逐渐降低,即高离子强度抑制吸附进行；Am(Ⅲ)在Na基膨润土上的吸附,及Eu(Ⅲ)在Ca基膨润土上的吸附规律与上述结果基本相同,只是在低离子强度下,两种膨润土吸附核素的pH边界会显著降低至pH2～4。
(4)研究了接触时间对核素吸附的影响。Eu(Ⅲ)在红壤上的吸附达到吸附-解吸平衡的时间约为4-12小时,其中去氧化铁成分红壤能够最快达到吸附平衡,而其在25℃的准二级吸附反应速率常数k2’和吸附量qe也最大。Am(Ⅲ)在Na基膨润土及Eu(Ⅲ)在Ca基膨润土上吸附平衡时间均较短,约为4小时,其反应速率常数k2’均为负值,说明吸附反应在初始阶段较快,随着时间推移,反应速率反而有所下降。以上吸附反应动力学可以被准二级动力学模型所描述。
(5)研究了腐殖酸对核素吸附的影响。在较低pH下,HA对核素吸附基本上都能起到促进作用,而在较高pH下,HA对Eu(Ⅲ)在红壤上的吸附促进作用相对有限,而对Am(Ⅲ)和Eu(Ⅲ)在膨润土上的吸附却起到抑制作用,特别是较高pH下Am(Ⅲ)在Na基膨润土上的吸附在pH7-7.5存在一个低点,说明Am(Ⅲ)与Eu(Ⅲ)在HA存在下的吸附形态有所不同,进一步说明核素存在形态对吸附有显著影响。
(6)研究了温度对核素吸附的影响,绘制了Eu(Ⅲ)与Am(Ⅲ)在不同温度下在不同吸附剂上的吸附等温线,并计算了各体系的热力学函数△G0、△S0和△H0。由热力学函数计算结果,可见核素在吸附剂上的吸附一般是吸热且自发的过程,即高温有利于吸附反应进行,只是Eu(Ⅲ)在三种红壤上的吸附随着温度的升高存在放热的过程,即在一定区间高温反而不利于吸附反应进行。上述过程吸附等温线符合Freundlich吸附模型。
The safe disposal of radioactive waste is paid more and more attention in worldwide, so it is very important to study the sorption activity of radioactive nuclides on clays and buffer/backfill materials.
High level radioactive wastes have the characters of long half-life, high toxicity, complex chemical behavior, make the study of sorption and transference on these transuraniums in natural medium be more important. As a clay mineral, red earth has many sorption characteristics such as ion exchange capability, expanding capacity, highly capable of adsorbing pollutants and self-purification functions, therefore clay minerals have the capacity for controlling environmental pollution. Bentonite is the first choice for buffer/backfill materials, so the investigation of sorption of radionuclides on bentonite is nonnegligible. This research put the focus on the speciation of radionuclides sorption on red earth and bentonite, and the effect factors of sorption such as pH, ionic strength, humic acid(HA), temperatures and so on. The main research contents are:
(1) Prepared three red earth samples:natural red earth(NRE), inorganic components removed red earth(ICRRE) and organic matter removed red earth(OMRRE), studied the sorption of Eu(Ⅲ) on red earth samples, and characterized these samples using XRD, SEM etc, investigated the chemical compositions, mineral structures and surface morphology of the samples.
(2) Prepared two different type of bentonite:Na-bentonite and Ca-bentonite, characterized these samples using XRD, SEM, EDS etc, and studied sorption of Am(Ⅲ) on Na-bentonite and sorption of Eu(Ⅲ) on Ca-bentonite.
(3) Investigated sorption of radionuclides on red earth and bentonite samples as a function of pH and ionic strength. The results showed that the sorption of radionuclides is strongly depended on the pH and ionic strength. The sorption increases with increasing pH values at pH<7, and then maintains a high level at pH>7. Ion exchange or outer-sphere surface complexation may be the main sorption mechanism of Am(Ⅲ) on bentonite at pH<7, whereas inner-sphere surface complexation may be the main sorption mechanism at pH>7.
(4) Researched sorption of radionuclides on red earth and bentonite samples as a function of contact time. The sorption was quickly to achieve the sorption equilibration, and the time to achieve the sorption equilibrium was about4～12hours; The sorption of Eu(Ⅲ) on ICRRE was fastest to achieve equilibrium in the three red earth samples and its adsorption capacity was the largest. The kinetic sorption of radionuclides on red earth and bentonite samples could be described well by a pseudo-second-order model.
(5) Studied the influence of HA for the sorption of radionuclides on red earth and bentonite samples. The presence of HA enhances the sorption of radionuclides on the adsorbents at low pH values, and reduces the sorption at high pH values, while there was a valley at pH7～7.5in the sorption progress of Am(Ⅲ) on Na-bentonite. This result suggests that the sorption is significantly influenced by the speciation of radionuclides.
(6) Studied sorption of radionuclides on adsorbents as a function of temperature and calculated thermodynamic parameters (△G0,△S0, and△H0). The sorption of radionuclides on adsorbents was an endothermic and spontaneous process, and an endothermic process in lower temperature range and exothermic process in higher temperature range for the red earth samples. The sorption isotherms of radionuclides could be described by Freundlich model.
引文
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3. M. S. Murali, J. N. Mathur.:Sorption characteristics of Am(Ⅲ), Sr(Ⅱ) and Cs(Ⅰ) on bentonite and granite. Journal of Radioanalytical and Nuclear Chemistry,254 (2002):129-136
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5. Q. H. Fan, D. D. Shao, Y, Lu, W. S. Wu, X. K. Wang.:Effect of pH, ionic strength, temperature and humic substances on the sorption of Ni (Ⅱ) to Na-attapulgite. Chemical Engineering Journal,150(2009):188-195
6.张茂林,杨子谦,吴王锁.：Eu(Ⅲ)和Am(Ⅲ)在凹凸棒石上的吸附行为.核化学与放射化学,30(2008)：120-124
7. S. Palagyi, H. Vodickova, J. Landa, J. Palagyiova, A. Laciok.:Migration and sorption of 137Cs and 152,154Eu in crushed crystalline rocks under dynamic conditions. Journal of Radioanalytical and Nuclear Chemistry,279 (2009):431-441
8. X. K. Wang, Y. X. Chen, Y. C. Wu.:Sorption and desorption of radiostrontium on powdered bentonite:Effect of pH and fulvic acid. Journal of Radioanalytical and Nuclear Chemistry, 261 (2004):497-500
9. Z. J. Guo, J. Xu, K. L Shi, Y. Q. Tang, W. S. Wu, Z. Y. Tao.:Eu(Ⅲ) adsorption/desorption on Na-bentonite:Experimental and modeling studies. Colloids and Surfaces A: Physicochemical and Engineering Aspects,339 (2009):126-133
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12. Q. H. Fan, M. L. Zhang, Y. Y. Zhang, K. F. Ding, Z. Q. Yang, W. S. Wu.:Sorption of Eu (Ⅲ) and Am(III) on attapulgite:effect of pH, ionic strength and fulvic acid. Radiochimica Acta, 98(2010):19-25
13. D. Humelnicu, G. Drochioiu, M. I. Sturza, A. Cecal, K. Popa.:Kinetic and thermodynamic aspects of U(Ⅵ) and Th(Ⅳ) sorption on a zeolitic volcanic tuff. Journal of Radioanalytical and Nuclear Chemistry,270 (2006):637-640