磁性聚氨基噻唑吸附剂脱除水体Hg2+性能

doi:10.11949/0438-1157.20240134

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，大于2时Zeta电位为负。在303K和Hg²⁺浓度为50mg/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121.9mg/g和153.1mg/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2M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303K、pH 1.3、Hg²⁺浓度20mg/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%、20.7%、26.7%、21.2%、29.7%、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 using polydopamine (PDA) assisted loading polyamino-thiazole (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 superparamagnetic behavior, and its Zeta potential was positive at pH<2 and negative at pH>2. At 303K and a mercury ion concentration of 50mg/L in simulated wastewater, the equilibrium adsorption capacities of Fe₃O₄@SiO₂@PDA-PAT were 121.9mg/g and 153.1mg/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 303K, 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 2M 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%. When the mass concentration ratios of other metal cations Na⁺, K⁺, Mg²⁺, Ca²⁺, Cu²⁺, Zn²⁺, and Ni²⁺ were 20 times that of mercury ions at a mercury ion concentration of 20mg/L and pH 1.3, the equilibrium adsorption capacities of Fe₃O₄@SiO₂@PDA-PAT for mercury ions decreased by 33.2%, 32.1%, 20.7%, 26.7%, 21.2%, 29.7%, 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: polyamino-thiazole, magnetic adsorbent, ferric oxide, wastewater containing Hg²⁺

中图分类号:

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, DOI: 10.11949/0438-1157.20240134.

Yan WANG, Jiawen ZHOU, Peiliang SUN, Yong CHEN, Hongyuan QI, Chong PENG. Removal of Hg²⁺ from water by magnetic polyaminothiazole adsorbent[J]. CIESC Journal, DOI: 10.11949/0438-1157.20240134.

图/表 21

图1 吸附剂制备简图

Fig.1 Adsorbent preparation diagram

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

Fig.2 (a)Hg2+ equilibrium adsorption capacity,Fe3O4@SiO2@PAT (b)Hg2+ equilibrium adsorption capacity,Fe3O4@SiO2@PDA-PAT (c)Hg2+ equilibrium adsorption capacity,PATExperimental conditions: 100 ml of wastewater with pH of 1.3 and Hg2+ concentration of 50mg/L was absorbed by 20mg adsorbent at 303 3k for 24h

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图注:(a) Fe3O4@SiO2@PDA-PAT, SEM (b)Fe3O4@SiO2,TEM (c) Fe3O4@SiO2@PDA-PAT,TEM

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

图6 Fe3O4@SiO2@PDA-PAT颗粒结构示意图

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

表1 Fe3O4@SiO2@PDA-PAT的XPS元素含量

Table 1 Fe3O4@SiO2@PDA-PAT XPS content

元素	峰值/eV	元素含量%
Hg4f	103.18	—
N1s	399.71	5.52
S2p	163.91	1.25
C1s	284.6	92.33
Cu2p	932.73	0.53

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（a）和pH（b）对Fe3O4@SiO2@PDA-PAT吸附Hg2+的影响注:Experimental conditions: 100 ml of wastewater with pH of 1.3 and Hg2+ concentration of 50mg/L was absorbed by 20mg adsorbent at 303 3k for 24h实验条件: pH为1.3和Hg2+浓度为50mg/L的废水100 ml,20mg吸附剂在303K下吸附24h

Fig.8 Effect of adsorption time(a) and pH (b) on Hg2+ adsorption by Fe3O4@SiO2@PDA-PAT

图9 温度（a）和Hg2+浓度（b）对Fe3O4@SiO2@PDA-PAT的吸附性能影响注:Experimental conditions: 100 ml wastewater with pH of 1.3 or pH of 5.0 and Hg2+ concentration of 50mg/L was adsorbed by 20mg adsorbent at 303 3k for 24h实验条件: pH为1.3或pH为5.0和Hg2+浓度为50mg/L的废水100 ml,20mg吸附剂在303K下吸附24h

Fig.9 Effects of temperature (a) and Hg2+ concentration (b) on the adsorption properties of Fe3O4@SiO2@PDA-PAT

图10 pH为1.3（a）和5.0（b）时Fe3O4@SiO2@PDA-PAT的Hg2+吸附时间与吸附量的关系注:Experimental conditions: 100 ml of wastewater with pH 1.3 or pH 5.0 and Hg2+ concentration of 50mg/L, 20mg of adsorbent实验条件: pH为1.3或pH为5.0和Hg2+浓度为50mg/L的废水100 ml,20mg吸附剂

Fig.10 Relationship between mercury adsorption time and adsorption capacity of Fe3O4@SiO2@PDA-PAT at pH 1.3 (a) and 5.0 (b)

图11 Fe3O4@SiO2@PDA-PAT对Hg2+的吸附动力学拟合 (a)准一级吸附动力学拟合,pH=1.3 (b)准一级吸附动力学拟合,pH=5.0 (c)准二级吸附动力学拟合,pH=1.3 (d)准二级吸附动力学拟合,pH=5.0 (e)内扩散吸附动力学拟合,pH=1.3 (f)内扩散吸附动力学拟合,pH=5.0

Fig.11 Fe3O4@SiO2@PDA-PAT adsorption kinetics fitting of Hg2+ at (a) quasi-first-order adsorption kinetics fitting at pH=1.3 (b) quasi-first-order adsorption kinetics fitting at pH=5.0 (c) quasi-second-order adsorption kinetics fitting at pH=1.3 (d) quasi-second-order adsorption kinetics fitting at pH=5.0 (e) Internal diffusion adsorption kinetics fitting,pH=1.3 (f) Internal diffusion adsorption kinetics fitting,pH=5.0

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^-1•min^-1)	R²	k_in	C	R²
1.3	297	98.99	0.0105	0.9602	119.8	6.26E-05	0.9893	5.469	-10.03	0.9789
	303	84.95	0.0089	0.9513	135.9	1.29E-04	0.9845	5.632	20.21	0.9744
	309	109.2	0.0051	0.9686	138.5	2.17E-04	0.9987	7.253	24.20	0.9052
5.0	297	56.42	0.0060	0.9553	86.43	1.59E-04	0.9948	3.591	9.681	0.9007
	303	134.8	0.0065	0.9539	179.5	7.97E-05	0.9975	8.383	-8.289	0.9684
	309	122.6	0.0048	0.9502	204.5	3.12E-05	0.9929	7.253	24.20	0.9052

图12 pH为1.3（a）和5.0（b）时Fe3O4@SiO2@PDA-PAT的Hg2+初始浓度与平衡吸附量的关系注:Experimental conditions: 100 ml of wastewater with pH 1.3 or pH 5.0 was absorbed by 20mg adsorbent for 24h实验条件: pH为1.3或pH为5.0的废水100 ml, 20mg吸附剂吸附24h

Fig.12 The relationship between the initial Hg2+ concentration of Fe3O4@SiO2@PDA-PAT and the equilibrium adsorption capacity at pH 1.3 (a) and 5.0 (b)

图13 Fe3O4@SiO2@PDA-PAT对Hg2+的吸附等温线拟合：(a)Langmuir吸附模型拟合,pH=1.3 (b)Langmuir吸附模型拟合,pH=5 (c)Freundlich吸附模型拟合,pH=1.3 (d)Freundlich吸附模型拟合,pH=5

Fig.13 Fe3O4@SiO2 @PD-PAT adsorption isotherm fitting for Hg2+ : (a)Langmuir adsorption model fitting,pH=1.3 (b)Langmuir adsorption model fitting,pH=5 (c)Freundlich adsorption model fitting,pH=1.3 (d)Freundlich adsorption model fitting,pH=5

表3 Fe3O4@SiO2@PDA-PAT吸附Hg2+的吸附等温线

Table 3 Fe3O4@SiO2@PDA-PAT adsorption isotherm 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^-1)	KL/（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	∆H/(kJ·mol^-1)	∆S/(J·mol^-1·K^-1)	∆G/(kJ·mol^-1)
1.3	297	0.9876	-57.91	-95.89	-29.51
	303				-28.71
	309				-28.36
5	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（a）pH 1.3的废水;（b）pH 5.0的废水

Fig.15 Fe3O4@SiO2@PDA-PAT schematic diagram of adsorption of heavy metal mercury in wastewater (a) wastewater at pH 1.3; (b) wastewater at pH 1.3

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

Fig.16 Effects of common metal cations (a) and Na+ (b) on the adsorption of mercury ions by Fe3O4@SiO2@PDA-PAT

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

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

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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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