巯基/铁基功能化蒙脱土对土壤镉的钝化行为研究

doi:10.16258/j.cnki.1674-5906.2023.07.013

生态环境学报 ›› 2023, Vol. 32 ›› Issue (7): 1301-1312.DOI: 10.16258/j.cnki.1674-5906.2023.07.013

巯基/铁基功能化蒙脱土对土壤镉的钝化行为研究

李治梅(), 安娅, 李梅, 王室苹, 秦好丽^*()

贵州师范大学化学与材料科学学院，贵州贵阳 550025

收稿日期:2023-04-11 出版日期:2023-07-18 发布日期:2023-09-27
通讯作者: * 秦好丽。E-mail: hollyqin@126.com
作者简介:李治梅（1995年生），女，硕士研究生，主要从事土壤重金属钝化材料。E-mail: 1639129523@qq.com
基金资助:
贵州省自然科学基金项目(20201Y182);国家自然科学基金项目(41967003)

Study on Passivation Behavior for Cadmium with Sulfhydryl/iron-based Functionalized Montmorillonite in Soil

LI Zhimei(), AN Ya, LI Mei, WANG Shiping, QIN Haoli^*()

School of Chemistry and Materials Science, Guizhou Normal University, Guiyang 550025, P. R. China

Received:2023-04-11 Online:2023-07-18 Published:2023-09-27

摘要/Abstract

摘要：

土壤镉（Cd）的迁移和富集严重威胁国家粮食安全和损害人体健康。通过整合有机/无机改性方法制备了新型的巯基/铁基复合功能化蒙脱土（SH-Fe-Mont），用于Cd的高效去除和钝化。利用FTIR、XRD、BET、SEM及XPS等表征手段证实了钝化剂被成功制备，且在没有改变蒙脱土（Mont）基本层状结构的基础上拥有丰富的孔隙结构及更大的比表面积。通过系列水溶液吸附实验和土壤有效态Cd及赋存形态变化考察钝化剂对重金属Cd的去除率和钝化效果。等温吸附实验结果证明在293-323 K温度范围内，钝化剂吸附行为均符合Langmuir模型。在303 K时，SH-Fe-Mont和单改性的铁基功能化蒙脱土（Fe-Mont）的理论最大饱和吸附量分别为55.3、42.7 mg·g^-1，分别是Mont的46.9、36.2倍。吸附动力学实验的结果显示，初始质量浓度分别为20、50、100 mg·L^-1时，钝化剂对Cd(Ⅱ)的吸附过程均符合伪二级模型，更快的吸附动力学使SH-Fe-Mont在40 min内达到吸附平衡（Mont：80 min；Fe-Mont：50 min）。更重要的是，SH-Fe-Mont对Cd的去除率超过99.0%（Cd的初始质量浓度20 mg·L^-1）。酸雨模拟实验证明了SH-Fe-Mont对镉吸附后的高稳定性，仅有0.31%的镉解吸和0.22 mg·kg^-1的镉浸出，远低于原始Mont（41.2%，11.7 mg·kg^-1）和Fe-Mont（4.58%，1.67 mg·kg^-1）。利用XPS研究了SH-Fe-Mont对镉的吸附机制，结果表明，Cd能被SH-Fe-Mont以一种复杂的络合状态-S-Cd和FeOOCd⁺固化。与对照组相比，施加2% SH-Fe-Mont后有效态镉含量降低71.2%，且活性高的可交换态和碳酸盐结合态之和由83.8%降低至47.4%，而稳定性较强的铁锰氧化结合态、有机结合态和残渣态之和由16.2%增加至52.6%，从而有效降低了镉的生物活性，进而减弱土壤中镉迁移的风险。该研究结果可为土壤和水中镉污染的钝化修复提供理论依据。

关键词: 蒙脱土, 功能化, 复合钝化剂, 镉, 钝化修复

Abstract:

Soil contamination by cadmium (Cd) is one of the major environmental hazards recognized in the world, and its migration and enrichment severely threaten national food security and harm human health. A novel sulfhydryl/iron composite functionalized montmorillonite (SH-Fe-Mont) prepared by rational integration of organic/inorganic modification methods and used for efficient removal and passivation of Cd. FTIR, XRD, BET, SEM and XPS were used to confirm that the passivators were successfully prepared and possessed a rich porosity and larger specific surface area without changing the basic layered structure of montmorillonite (Mont). The removal rate and passivation effect of passivators on Cd were examined through a series of aqueous solution adsorption experiments and morphological changes of Cd in soil. The isothermal adsorption experiments were carried out to demonstrate that the adsorption behavior of the passivator was consistent with the Langmuir model over the temperature range of 293-323 K. The theoretical maximum saturated adsorption capacity of Cd onto SH-Fe-Mont and single-modified iron-based functionalized montmorillonite (Fe-Mont) were 55.3 and 42.7 mg·g^-1, which were 46.9 and 36.2 times higher than that of Mont, respectively. The results of the adsorption kinetics experiments showed that the adsorption of Cd(II) by the passivators at the initial concentrations of 20, 50, and 100 mg·L^-1 were in accordance with the pseudo-secondary model, and the faster adsorption kinetics led to the adsorption equilibrium of SH-Fe-Mont within 40 min (Mont: 80 min; Fe-Mont: 50 min). More importantly, the removal rate for Cd could exceed 99.0% (initial Cd concentration 20 mg·L^-1). Acid rain simulation experiments demonstrated only 0.31% Cd desorption and 0.22 mg·kg^-1 Cd leaching after Cd adsorption by SH-Fe-Mont, which was much lower than that of pristine Mont (41.2%, 11.7 mg·kg^-1) and Fe-Mont (4.58%, 1.67 mg·kg^-1). The adsorption mechanism of SH-Fe-Mont on Cd was investigated by XPS, and the results showed that Cd could be immobilized by SH-Fe-Mont in a complex state of -S-Cd and FeOOCd⁺. After the application of 2% SH-Fe-Mont, the available Cd content was reduced by 71.2%, and the sum of the highly active exchangeable and carbonate-bound states was reduced from 83.8% to 47.4%, while the sum of the more stable Fe-Mn oxidized-bound, organically-bound, and residue-bound states was increased from 16.2% to 52.6%, which effectively reduced the Cd bioactivity, and thus reduced the risk of Cd migration and enrichment in soil. The results of this study can provide a theoretical basis for the passivation remediation of Cd-contaminated soils and water.

Key words: montmorillonite, functionalization, compound passivator, cadmium, passivation repair

中图分类号:

李治梅, 安娅, 李梅, 王室苹, 秦好丽. 巯基/铁基功能化蒙脱土对土壤镉的钝化行为研究[J]. 生态环境学报, 2023, 32(7): 1301-1312.

LI Zhimei, AN Ya, LI Mei, WANG Shiping, QIN Haoli. Study on Passivation Behavior for Cadmium with Sulfhydryl/iron-based Functionalized Montmorillonite in Soil[J]. Ecology and Environment, 2023, 32(7): 1301-1312.

图/表 14

表1 Tessier法重金属提取步骤

Table 1 Tessier process for extraction of heavy metals

提取步骤	提取试剂	提取形态
1	氯化镁 (1 mol·L^-1)	可交换态
2	乙酸钠和醋酸 (1 mol·L^-1)	碳酸盐结合态
3	盐酸羟胺 (0.04 mol·L^-1) 和20%醋酸	铁锰氧化结合态
4	硝酸 (0.02 mol·L^-1) 和30%过氧化氢	有机结合态
5	硝酸、过氧化氢和氢氟酸	残渣态

图1 不同钝化剂的红外光谱图和X射线衍射图

Figure 1 FTIR spectra and XRD patterns of different passivators

图2 不同钝化剂的N2吸附-脱附等温线

Figure 2 N2 adsorption-desorption isotherms of different passivators

表2 不同钝化剂的比表面积和孔径分布

Table 2 The surface area and pore size distribution of different passivators

样品	比表面积/(m²·g^-1)	平均孔径/nm	总孔体积/(cm³·g^-1)
Mont	46.6	6.96	0.11
Fe-Mont	71.5	7.67	0.14
SH-Fe-Mont	169	4.95	0.24

图3 不同钝化剂的扫描电镜图（a）蒙脱土；（b）铁基功能化蒙脱土；（c）巯基/铁基功能化蒙脱土

Figure 3 SEM images of different passivators

图4 不同钝化剂对Cd(II)的吸附等温线（a）Mont对Cd(II)的吸附等温线；（b）Fe-Mont对Cd(II)的吸附等温线；（c）SH-Fe-Mont对Cd(II)的吸附等温线

Figure 4 Adsorption isotherms of different passivators on Cd(II)

表3 Cd(II)在不同钝化剂上的吸附等温线参数

Table 3 Adsorption isotherm parameters of different passivators on Cd(II)

样品	温度/ K	Langmuir			Freundlich
样品	温度/ K	q_m/ (mg·g^-1)	K_L/ (L·mg^-1)	r²	K_F/ (L·g^-1)	n	r²
Mont	293	0.97	0.069	0.980	0.167	0.362	0.988
	303	1.18	0.112	0.996	0.278	0.305	0.939
	313	1.56	0.088	0.995	0.314	0.336	0.956
	323	2.05	0.071	0.997	0.351	0.363	0.952
Fe-Mont	293	37.7	0.003	0.990	0.806	0.516	0.983
	303	42.7	0.003	0.996	1.422	0.465	0.970
	313	58.1	0.003	0.992	1.230	0.511	0.972
	323	61.6	0.004	0.998	2.021	0.468	0.963
SH-Fe-Mont	293	38.8	0.003	0.992	1.088	0.484	0.986
	303	55.3	0.003	0.991	1.297	0.505	0.971
	313	58.2	0.004	0.993	2.017	0.460	0.956
	323	68.5	0.004	0.992	2.239	0.468	0.947

表4 其他报道的钝化剂对Cd(Ⅱ)吸附能力对比

Table 4 Comparison of other reported passivators on Cd(II) adsorption capacity

钝化剂	温度/K	pH	时间/h	q_e/(mg·g^-1)	参考文献
巯基改性海泡石	298	8.0	24	8.87	符云聪等, 2018
十二烷基二甲基甜菜碱改性蛭石	298	5.5	4	19.72	Yang et al., 2020
巯基改性凹凸棒石	298	6.5	2	22.71	Fu et al., 2021
羟基铁柱撑蒙脱石	298	5.0	-	25.7	Wu et al., 2009
生物炭负载纳米级零价铁	298	5.5	2	33.8	Yang et al., 2020
两性表面活性剂活化蒙脱土	303	5.0	-	41.73	Liu et al., 2016
石墨烯类生物炭负载纳米零价铁	298	7.0	2	46.4	Liu et al., 2020

图5 不同钝化剂对Cd(II)的吸附动力学曲线（a）Cd(II)对反应时间作图（Mont）；（b）Cd(II)对反应时间作图（Fe-Mont）；（c）Cd(II)对反应时间作图（SH-Fe-Mont）

Figure 5 Adsorption kinetics of different passivators on Cd(II)

表5 不同钝化剂对Cd(II)的吸附动力学参数

Table 5 Adsorption kinetic parameters of different passivators on Cd(II)

样品	浓度/ (mg·L^-1)	伪一级动力学			伪二级动力学
样品	浓度/ (mg·L^-1)	q_e/(mg·g^-1)	k₁	r²	q_e/(mg·g^-1)	k₂	r²
Mont	20	0.72	0.092	0.958	0.79	0.171	0.988
	50	0.92	0.092	0.965	1.03	0.129	0.992
	100	1.03	0.092	0.940	1.15	0.118	0.981
Fe-Mont	20	3.19	0.221	0.984	3.36	0.125	0.998
	50	7.27	0.252	0.983	7.64	0.066	0.999
	100	8.94	0.236	0.977	9.45	0.046	0.997
SH-Fe-Mont	20	3.94	0.185	0.982	4.18	0.082	0.996
	50	9.96	0.548	0.998	10.1	0.238	0.999
	100	12.9	0.298	0.984	13.4	0.047	0.998

图6 pH对Cd(II)在不同钝化剂上解吸的影响

Figure 6 Effect of pH on Cd(II) desorption on different passivators

图7 不同钝化剂对土壤有效态镉和浸出镉质量分数的影响

Figure 7 Effects of different passivators on mass fraction of available Cd and leached Cd in soil

图8 不同钝化剂对土壤中镉形态分布的影响

Figure 8 Effect of different passivators on the morphological distribution of cadmium in soil

图9 SH-Fe-Mont吸附Cd(II)前后XPS全谱；O 1s、S 2p和Cd 3d的高分辨率XPS谱

Figure 9 XPS survey spectra; high-resolution XPS spectra of O 1s, N 1s, and S 2p of SH-Fe-Mont before and after adsorption of Cd(II)

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巯基/铁基功能化蒙脱土对土壤镉的钝化行为研究

Study on Passivation Behavior for Cadmium with Sulfhydryl/iron-based Functionalized Montmorillonite in Soil

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