磁性聚氨基噻唑吸附剂脱除水体Hg2+性能

doi:10.11949/0438-1157.20240134

化工学报 ›› 2024, Vol. 75 ›› Issue (6): 2283-2298.DOI: 10.11949/0438-1157.20240134

磁性聚氨基噻唑吸附剂脱除水体Hg²⁺性能

王岩¹(), 周佳文¹, 孙培亮², 陈勇¹(), 齐元红³, 彭冲²()

^1.临港石油天然气储运技术国家地方联合工程研究中心，浙江海洋大学石油化工与环境学院，浙江舟山 316022
^2.大连理工大学化工学院，精细化工国家重点实验室，辽宁大连 116024
^3.新特能源股份有限公司，新疆乌鲁木齐 830000

收稿日期:2024-01-29 修回日期:2024-04-11 出版日期:2024-06-25 发布日期:2024-07-03
通讯作者: 陈勇,彭冲
作者简介:王岩（1998—），女，硕士研究生，wangyan040321@163.com
基金资助:
舟山市定海区科技项目(2021C31002);大连理工大学基本科研业务项目(DUT23RC(3)044)

Removal of Hg²⁺ from water by magnetic polyaminothiazole adsorbent

Yan WANG¹(), Jiawen ZHOU¹, Peiliang SUN², Yong CHEN¹(), Yuanhong QI³, Chong PENG²()

^1.National & Local Joint Engineering Research Center of Harbor Oil & Gas Storage and Transportation Technology, School of Petrochemical Engineering & Environment, Zhejiang Ocean University, Zhoushan 316022, Zhejiang, China
^2.State Key Laboratory of Fine Chemicals, School of Chemical Engineering, Dalian University of Technology, Dalian 116024, Liaoning, China
^3.Xinte Energy Co. , Ltd. , Urumchi 830000, Xinjiang, China

Received:2024-01-29 Revised:2024-04-11 Online:2024-06-25 Published:2024-07-03
Contact: Yong CHEN, Chong PENG

摘要/Abstract

摘要：

聚多巴胺（PDA）辅助负载聚氨基噻唑（PAT）法制备了磁性颗粒吸附剂Fe₃O₄@SiO₂@PDA-PAT。对吸附剂进行了XRD、VSM、TG、SEM、XPS、EDS和Zeta电位等表征分析，考察了吸附剂对Hg²⁺的吸附性能。结果表明，Fe₃O₄@SiO₂@PDA-PAT具有超顺磁性，在pH小于2时Zeta电位为正，pH大于2时Zeta电位为负。在303 K和Hg²⁺浓度为50 mg/L模拟废水中，当pH为1.3和5.0时，Hg²⁺的平衡吸附量分别为121.9 mg/g和153.1 mg/g。在强酸（如pH 1.3）和弱酸（如pH 5.0）环境下Fe₃O₄@SiO₂@PDA-PAT吸附Hg²⁺的过程均是自发过程，且符合二级动力学模型和Langmuir等温吸附模型。强酸环境下（如pH 1.3）Fe₃O₄@SiO₂@PDA-PAT吸附Hg²⁺是焓驱动的放热过程，弱酸（如pH 5.0）环境下是熵驱动的吸热过程。用2 mol/L混酸（盐酸和硝酸摩尔比为1∶1）作为解吸液可使Hg²⁺解吸率达91%以上。在303 K、pH 1.3、Hg²⁺浓度20 mg/L条件下，当Na⁺、K⁺、Mg²⁺、Ca²⁺、Cu²⁺、Zn²⁺、Ni²⁺质量浓度为Hg²⁺的20倍时，Fe₃O₄@SiO₂@PDA-PAT的Hg²⁺平衡吸附量分别下降了33.2%、32.1%、20.6%、26.7%、21.2%、29.6%、17.8%。在模拟海水下，Hg²⁺吸附量下降40.9%。Fe₃O₄@SiO₂@PDA-PAT具有较好的Hg²⁺选择性，具有净化海水脱除重金属的应用潜力。

关键词: 聚氨基噻唑, 磁性吸附剂, 四氧化三铁, 含Hg²⁺废水

Abstract:

In this study, magnetic particle adsorbent Fe₃O₄@SiO₂@PDA-PAT was prepared by using polydopamine (PDA) assisted loading polyaminothiazole (PAT) method. The adsorbent was characterized by XRD, VSM, TG, SEM, XPS, EDS, and Zeta potential analysis, and the adsorption performance of the adsorbent for mercury was investigated. The results showed that Fe₃O₄@SiO₂@PDA-PAT exhibited super paramagnetic behavior, and its Zeta potential was positive at pH<2 and negative at pH>2. At 303 K and a mercury ion concentration of 50 mg/L in simulated wastewater, the equilibrium adsorption capacities of Fe₃O₄@SiO₂@PDA-PAT were 121.9 mg/g and 153.1 mg/g at pH 1.3 and pH 5.0, respectively. The adsorption process of mercury ions by Fe₃O₄@SiO₂@PDA-PAT was a spontaneous process and followed the second-order kinetic model and Langmuir isotherm model at 303 K, as well as in strong acid (pH 1.3) and weak acid (pH 5.0) environments. The adsorption of mercury ions by Fe₃O₄@SiO₂@PDA-PAT in strong acid environment (pH 1.3) was an exothermic process driven by enthalpy, while in weak acid environment (pH 5.0) it was an endothermic process driven by entropy. The use of 2 mol/L mixed acid (hydrochloric acid and nitric acid in a molar ratio of 1∶1) as the desorption solution could achieve a mercury desorption rate of more than 91%. Under the conditions of 303 K, pH 1.3, and Hg²⁺ concentration 20 mg/L, when the mass concentration of Na⁺, K⁺, Mg²⁺, Ca²⁺, Cu²⁺, Zn²⁺, and Ni²⁺ were 20 times that of Hg²⁺, the Hg²⁺ equilibrium adsorption capacities of Fe₃O₄@SiO₂@PDA-PAT for mercury ions decreased by 33.2%, 32.1%, 20.6%, 26.7%, 21.2%, 29.6%, and 17.8%, respectively. In simulated seawater, the mercury adsorption capacity decreased by 40.9%. Fe₃O₄@SiO₂@PDA-PAT exhibited good mercury adsorption selectivity and had the potential to be used for purifying seawater and removing heavy metals.

Key words: polyaminothiazole, magnetic adsorbent, ferric oxide, wastewater containing Hg²⁺

中图分类号:

TH 3

王岩, 周佳文, 孙培亮, 陈勇, 齐元红, 彭冲. 磁性聚氨基噻唑吸附剂脱除水体Hg²⁺性能[J]. 化工学报, 2024, 75(6): 2283-2298.

Yan WANG, Jiawen ZHOU, Peiliang SUN, Yong CHEN, Yuanhong QI, Chong PENG. Removal of Hg²⁺ from water by magnetic polyaminothiazole adsorbent[J]. CIESC Journal, 2024, 75(6): 2283-2298.

图/表 21

图1 吸附剂制备简图

Fig.1 Adsorbent preparation diagram

图2 Fe3O4@SiO2@PAT、Fe3O4@SiO2@PDA-PAT和PAT的Hg2+平衡吸附量（实验条件：pH 为1.3和Hg2+浓度为50 mg/L的废水100 ml，20 mg吸附剂在303 K下吸附24 h）

Fig.2 The Hg2+ equilibrium adsorption capacity of Fe3O4@SiO2 @PAT, Fe3O4@SiO2@PDA-PAT, PAT (experimental conditions: 100 ml of wastewater with pH of 1.3 and Hg2+ concentration of 50 mg/L was absorbed by 20 mg adsorbent at 303 K for 24 h)

图3 样品的表征分析图1—Fe3O4;2—Fe3O4@SiO2;3—Fe3O4@SiO2@PAT;4—Fe3O4@SiO2@PDA-PAT

Fig.3 Characterization analysis diagram of samples

图4 样品的SEM和TEM图

Fig.4 SEM and TEM images of the sample

图5 Fe3O4@SiO2@PDA-PAT的EDS谱图(a)和XPS谱图(b)

Fig.5 EDS spectra (a) and XPS spectra (b) of Fe3O4@SiO2@PDA-PAT

表1 Fe3O4@SiO2@PDA-PAT的XPS元素含量

Table 1 Fe3O4@SiO2@PDA-PAT XPS elements content

元素	峰值/eV	元素含量/%
Hg 4f	103.18	—
N 1s	399.71	5.52
S 2p	163.91	1.25
C 1s	284.6	92.33
Cu 2p	932.73	0.53

图6 Fe3O4@SiO2@PDA-PAT颗粒结构示意图

Fig.6 Schematic diagram of Fe3O4@SiO2@PDA-PAT particle structure

图7 Fe3O4@SiO2@PDA-PAT的Zeta电位与pH关系

Fig.7 Relationship between pH and Zeta potential of Fe3O4@SiO2@PDA-PAT

图8 吸附时间和pH对Fe3O4@SiO2@PDA-PAT吸附Hg2+的影响（实验条件：pH为1.3和Hg2+浓度为50 mg/L的废水100 ml，20 mg吸附剂在303 K下吸附24 h）

Fig.8 Effect of adsorption time and pH on Hg2+ adsorption by Fe3O4@SiO2@PDA-PAT (experimental conditions: 100 ml of wastewater with pH of 1.3 and Hg2+ concentration of 50 mg/L was absorbed by 20 mg adsorbent at 303 K for 24 h)

图9 温度和Hg2+浓度对Fe3O4@SiO2@PDA-PAT吸附性能的影响（实验条件：pH为1.3或pH为5.0和Hg2+浓度为50 mg/L的废水100 ml，20 mg吸附剂在303 K下吸附24 h）

Fig.9 Effect of temperature and Hg2+ concentration on the adsorption properties of Fe3O4@SiO2@PDA-PAT (experimental conditions: 100 ml wastewater with pH of 1.3 or pH of 5.0 and Hg2+ concentration of 50 mg/L was adsorbed by 20 mg adsorbent at 303 K for 24 h)

图10 不同pH时Fe3O4@SiO2@PDA-PAT的Hg2+吸附时间与吸附量的关系（实验条件：pH为1.3或5.0和Hg2+浓度为50 mg/L的废水100 ml，20 mg吸附剂）

Fig.10 Relationship between mercury adsorption time and adsorption capacity of Fe3O4@SiO2@PDA-PAT at different pH (experimental conditions: 100 ml of wastewater with pH 1.3 or pH 5.0 and Hg2+ concentration of 50 mg/L, 20 mg of adsorbent)

图11 Fe3O4@SiO2@PDA-PAT对Hg2+的吸附动力学拟合

Fig.11 Fe3O4@SiO2@PDA-PAT adsorption kinetics fitting of Hg2+

表2 Fe3O4@SiO2@PDA-PAT吸附Hg2+的动力学参数

Table 2 Kinetic parameters of adsorption of Hg2+ by Fe3O4@SiO2@PDA-PAT

pH	T/K	准一级吸附动力学			准二级吸附动力学			内扩散吸附动力学
pH	T/K	Q_e/(mg/g)	k₁/min^-1	R²	Q_e/(mg/g)	k₂/(g/(mg·min))	R²	k_in	C	R²
1.3	297	98.99	0.0105	0.9602	119.8	6.26×10^-5	0.9893	5.469	-10.03	0.9789
	303	84.95	0.0089	0.9513	135.9	1.29×10^-4	0.9845	5.632	20.21	0.9744
	309	109.2	0.0051	0.9686	138.5	2.17×10^-4	0.9987	7.253	24.20	0.9052
5.0	297	56.42	0.0060	0.9553	86.43	1.59×10^-4	0.9948	3.591	9.681	0.9007
	303	134.8	0.0065	0.9539	179.5	7.97×10^-5	0.9975	8.383	-8.289	0.9684
	309	122.6	0.0048	0.9502	204.5	3.12×10^-5	0.9929	7.253	24.20	0.9052

图12 不同pH时Fe3O4@SiO2@PDA-PAT的Hg2+初始浓度与平衡吸附量的关系（实验条件：pH为1.3或5.0的废水100 ml，20 mg吸附剂吸附24 h）

Fig.12 The relationship between the initial Hg2+ concentration of Fe3O4@SiO2@PDA-PAT and the equilibrium adsorption capacity at pH 1.3 and 5.0 (experimental conditions: 100 ml of wastewater with pH 1.3 or pH 5.0 was absorbed by 20 mg adsorbent for 24 h)

图13 Fe3O4@SiO2@PDA-PAT对Hg2+的吸附等温线拟合

Fig.13 Fe3O4@SiO2@PD-PAT adsorption isotherm fitting for Hg2+

表3 Fe3O4@SiO2@PDA-PAT吸附Hg2+的等温吸附模型

Table 3 Fe3O4@SiO2@PDA-PAT isotherm adsorption model for Hg2+ adsorption

pH	T/K	Langmuir等温吸附模型			Freundlich等温吸附模型
pH	T/K	Q_m/(mg/g)	K_L/(L/mg)	R²	1/n	K_F/(mg/g)	R²
1.3	297	92.42	0.7723	0.9989	0.2233	44.95	0.7599
	303	131.9	0.4446	0.9999	0.4246	35.22	0.7760
	309	159.7	0.3110	0.9996	0.3951	45.54	0.9426
5.0	297	83.26	0.3099	0.9825	0.2487	33.01	0.9528
	303	163.1	0.5104	0.9926	0.3120	62.69	0.8851
	309	176.7	1.018	0.9884	0.2899	73.89	0.9658

图14 Fe3O4@SiO2@PDA-PAT吸附Hg2+的吸附热力学参数lnK与1/T的关系图

Fig.14 Plot of lnKvs 1/T for estimation of thermodynamic parameters for the adsorption of mercury onto Fe3O4@SiO2@PDA-PAT

表4 Fe3O4@SiO2@PDA-PAT吸附Hg2+的热力学参数

Table 4 Thermodynamic parameters of adsorption of Hg2+ by Fe3O4@SiO2@PDA-PAT

pH	T/K	R²	ΔH/(kJ/mol)	ΔS/(J/(mol·K))	ΔG/(kJ/mol)
1.3	297	0.9876	-57.91	-95.89	-29.51
	303				-28.71
	309				-28.36
5.0	297	0.9892	75.52	345.8	-27.25
	303				-29.06
	309				-31.41

图15 Fe3O4@SiO2@PDA-PAT吸附废水中重金属汞的示意图

Fig.15 Fe3O4@SiO2@PDA-PAT schematic diagram of adsorption of heavy metal mercury in wastewater

图16 常见金属阳离子(a)以及Na+浓度(b)对Fe3O4@SiO2 @PDA-PAT吸附Hg2+的影响（实验条件：pH 1.3、Hg2+为20 mg/L和400 mg/L的模拟废水100 ml，20 mg吸附剂在303 K下吸附24 h）

Fig.16 Effect of common metal cations (a) and Na+ (b) on the adsorption of mercury ions by Fe3O4@SiO2@PDA-PAT(experimental conditions: 100 ml of simulated wastewater with pH 1.3, Hg2+ at 20 mg/L and 400 mg/L, 20 mg adsorbent at 303 K for 24 h)

图17 Fe3O4@SiO2@PDA-PAT的解吸效率（实验条件：20 mg饱和吸附后的吸附剂加入50 ml解吸液中，在303 K下解吸24 h）

Fig.17 Desorption efficiency of Fe3O4@SiO2@PDA-PAT(experimental conditions: the adsorbent after 20 mg saturation adsorption was added into 50 ml desorption solution and desorbed at 303 K for 24 h)

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磁性聚氨基噻唑吸附剂脱除水体Hg²⁺性能

Removal of Hg²⁺ from water by magnetic polyaminothiazole adsorbent

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