木质素表面功能化MXene纳米片的制备及其对U(VI)的吸附性能

李仕友; 乔记帅; 杨宇彪; 熊芷毓; 王国华

木质素表面功能化MXene纳米片的制备及其对U(VI)的吸附性能

李仕友^{1, 2},
乔记帅¹,
杨宇彪¹,
熊芷毓¹,
王国华^{1, 2, ,}

1.
南华大学　土木工程学院, 湖南衡阳 421001
2.
南华大学　污染控制与资源化技术湖南省重点实验室, 湖南衡阳 421001

基金项目: 湖南省自然科学基金项目(2022JJ30490)；国家自然科学基金项目(51904155)

详细信息

通讯作者:
王国华，博士，副教授，硕士生导师，研究方向为放射性污染治理与资源化　E-mail: wghcsu@163.com

中图分类号: TB333
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- 被引次数: 0
出版历程
- 收稿日期: 2023-11-16
- 修回日期: 2023-12-20
- 录用日期: 2023-12-23
- 网络出版日期: 2024-01-18

Preparation of lignin surface-functionalized MXene nanosheets and its U(VI)adsorption properties

Li Shiyou^{1, 2},
Qiao Jishuai¹,
Yang Yubiao¹,
Xiong Zhiyu¹,
Wang Guohua^{1, 2
, ,}

1.
School of Civil Engineering, University of South China, Hengyang 421001, China
2.
Hunan Provincial Key Laboratory of Pollution Control and Recycling Technology, University of South China, Hengyang 421001, China

Funds: The Natural Science Foundation of Hunan Province (2022JJ30490); The National Natural Science Foundation of China(51904155)

摘要

摘要: 为了进一步改善MXene纳米材料对模拟放射性废水中U(Ⅵ)的吸附性能，利用天然资源酶水解木质素(EHL)作为生物表面活性剂对MXene进行表面功能化处理，采用SEM-EDS、XRD及FTIR对改性前后的材料进行了表征分析，并在吸附实验中探究了pH、温度、反应时间、干扰离子及不同初始U(Ⅵ)浓度等因素对除U(Ⅵ)效果的影响。结果表明，EHL阻止了MXene纳米片的聚集堆叠，并且引入了大量活性官能团，提高了EHL功能化MXene纳米片的吸附性能。在MXene与EHL的质量比为1∶5、投加量为0.1 g·L⁻¹、pH为5、温度为303 K时，对U(VI)的最大吸附容量为231.95 mg·g⁻¹。此外，吸附动力学和等温线分析表明，拟二阶动力学模型和Frendlich等温线模型能很好的拟合此吸附过程，热力学分析表明其吸附过程是自发吸热的。经历5次循环再生后，对U(VI)的去除率仍在80%以上。表征分析结果表明，MX/EHL与U(VI)之间相互作用机制包括离子交换、静电吸引以及与含氧官能团之间的络合作用。基于此研究，MX/EHL作为一种环境友好型吸附材料，对去除废水中的U(VI)具有巨大潜力。
- MXene /
- 木质素 /
- 纳米材料 /
- U(VI) /
- 吸附性能
Abstract: In order to further improve the adsorption performance of MXene nanomaterials on U(Ⅵ) in simulated radioactive wastewater, the surface functionalization of MXene was carried out by using natural resources of enzymatically hydrolyzed lignin (EHL) as a biosurfactant, and the materials before and after the modification were characterized and analyzed by using SEM-EDS, XRD, and FTIR, and the effects of pH, temperature, and the adsorption experiments were explored, reaction time, interfering ions and different initial U(VI) concentrations on the effect of U(VI) removal. The results show that EHL prevents the re-stacking of MXene nanosheets and introduces a large number of active functional groups, which improves the adsorption performance of EHL-functionalized MXene nanosheets. The maximum adsorption capacity for U(VI) is 231.95 mg·g⁻¹ at the mass ratio of MXene to EHL of 1∶5, the dosage of 0.1 g·L⁻¹, pH = 5, and the temperature of 303 K. In addition, the adsorption kinetic and isotherm analyses show that the proposed second-order kinetic model and the Frendlich isotherm model fit this adsorption process well, and the thermodynamic analyses indicate that its adsorption process is spontaneous heat absorption. After five cycles of regeneration, the removal rate of U(VI) is still above 80%. Characterization results reveals that the interaction mechanisms between MX/EHL and U(VI) involve ion exchange, electrostatic attraction, and complexation with oxygen-containing functional groups. Based on this study, MX/EHL has great potential as an environmentally friendly adsorbent material for the removal of U(VI) from wastewater.
- MXene /
- lignin /
- nanomaterials /
- U(VI) /
- adsorption performance

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图 1 Ti₃C₂T_x(MX)/酶水解木质素(EHL)的主要制备步骤

Figure 1. The main preparation processes of Ti₃C₂T_x (MX)/ enzymatically hydrolyzed lignin (EHL)

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图 2 MX(a、b)和MX/EHL(c、d)的SEM图；MX(e)和MX/EHL(f)的EDS能谱

Figure 2. SEM images of MX(a、b) and MX/EHL(c、d);EDS patterns of MX(e) and MX/EHL(f)

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图 3 MAX(Ti₃AlC₂)、MX和MX/EHL的XRD光谱(a)；MX和MX/EHL的N₂吸脱附及孔径图(b)

Figure 3. XRD spectra of MAX(Ti₃AlC₂)、MX and MX/EHL(a); N₂ adsorption-desorption and pore size of MX and MX/EHL (b)

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图 4 MX、EHL和MX/EHL吸附前后的FTIR图谱

Figure 4. FTIR spectra of MX、EHL and MX/EHL before and after adsorption

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图 5 不同配比MX/EHL吸附剂对U(VI) 的吸附效率对比

Figure 5. Comparison of adsorption efficiency of different ratios of MX/EHL adsorbents on U(VI)

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图 6 不同MX/EHL投加量对吸附U(VI) 的影响

Figure 6. Effect of different MX/EHL dosage on adsorption of U(VI)

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图 7 (a)不同pH值下U(VI) 的形态分布曲线图；(b)不同pH值对MX/EHL吸附U(VI)性能的影响

Figure 7. (a) Morphological distribution curves of U(VI) at different pH values; (b) Effect of different pH values on the adsorption performance of U(VI) by MX/EHL

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图 8 (a)接触时间对MX/EHL吸附U(VI)的影响；(b)拟一级动力学；(c)拟二级动力学；(d)颗粒内扩散模型

Figure 8. (a) Effect of contact time on U(VI) adsorption by MX/EHL; (b) Pseudo-first-order; (c) Pseudo-second-order; (d) Intraparticle diffusion model

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图 9 MX/EHL吸附U(VI)的Langmuir(a)、Freundlich(b)和Dubinin-Radushkevich(c)等温吸附模型拟合曲线；(d)lnK⁰与1/T的线性拟合

Figure 9. Fitting curve of Langmuir(a)、 Freundlich (b) and Dubinin‒Radushkevich (c) isothermal adsorption model of U(VI) adsorption by MX/EHL; (d) Linear fit of lnK⁰ versus 1/T

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图 10 不同种类竞争离子对MX/EHL吸附U(VI)的影响

Figure 10. effect of different competitive ions on adsorption of U(VI) on MX/EHL

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图 11 MX/EHL吸附剂循环再生试验

Figure 11. MX/EHL adsorbent cycle regeneration experiment

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图 12 (a)吸附前后MX/EHL全谱图；(b)U 4 f光谱图；(c、d)O 1 s光谱图；(e、f)C 1 s光谱图；

Figure 12. (a)full spectrum of MX/EHL before and after adsorption; (b) U 4 f spectrum; (c、d) O 1 s spectrum; (e、f) C 1 s spectrum

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表 1 MX和MX/EHL的孔隙结构参数

Table 1. Pore structure parameters of MX and MX/EHL

Material	Surface area/ (m²·g⁻¹)	Pore volume/ (cm³·g⁻¹)	Pore diameter/ nm
MX	3.8297	0.0100	10.4628
MX/EHL	8.7751	0.0455	20.7320

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表 2 MX/EHL对U(VI)的吸附动力学参数

Table 2. The adsorption kinetic parameters of U(VI) on MX/EHL

Kinetic model	Name of sample	MX	MX/EHL(1∶4)	MX/EHL(1∶5)
Kinetic model	q_e,exp/(mg·g⁻¹)	35.22	46.92	48.24
Pseudo-first-order	k₁/min⁻¹	0.017	0.017	0.018
	q_e,cal/(mg·g⁻¹)	3.487	2.737	2.502
	R²	0.882	0.949	0.930
Pseudo-second-order	k₂/min⁻¹	0.021	0.027	0.030
	q_e,cal/(mg·g⁻¹)	35.51	47.13	48.43
	R²	0.999	0.999	0.999
Intraparticle diffusion	k_p1/(mg·(g·min^0.5)⁻¹)	0.688	0.282	0.338
	C₁	29.782	43.819	45.002
	R₁²	0.973	0.958	0.981
Intraparticle diffusion	k_p2/(mg·(g·min^0.5)⁻¹)	0.406	0.324	0.303
	C₂	31.266	43.568	45.243
	R₂²	0.989	0.986	0.994
	k_p3/(mg·(g·min^0.5)⁻¹)	0.015	0.058	0.035
	C₃	35.029	46.175	47.794
	R₃²	0.804	0.653	0.615
Notes: q_e,exp is the actual adsorption capacity at adsorption equilibrium; q_e,cal is the calculated adsorption capacity at adsorption equilibrium; k₁ and k₂ are the adsorption rate constants of the pseudo-first and pseudo-second, respectively ; R² is the correlation coefficient; k_p1, k_p2, k_p3 are the adsorption rate constants of intraparticle diffusion.

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表 3 Langmuir、Freundlich和Dubinin‒Radushkevich吸附等温线模型的相关参数

Table 3. Parameters associated with Langmuir, Freundlich and Dubinin-Radushkevich adsorption isotherm models

T/K	Langmuir			Freundlich			Dubinin‒Radushkevich
T/K	q_max/(mg·g⁻¹)	K_L/(L∙mg⁻¹)	R²	K_F	1/n	R²	q_DR	E	R²
293 K	205.493	0.164	0.890	48.175	0.399	0.982	115.99	1.879	0.554
298 K	217.057	0.221	0.925	58.802	0.378	0.989	129.09	2.077	0.607
303 K	231.947	0.251	0.924	65.565	0.379	0.997	138.33	2.337	0.627
Notes: q_max is the maximum adsorption capacity; K_L is the Langmuir adsorption equilibrium constant; K_F and n are the constants that are related to the adsorption capacity and the adsorption intensity, respectively; R is the universal gas constant (8.312 J·mol⁻¹·K⁻¹), T is the temperature (K); E is the average free energy of adsorption.

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表 5 不同吸附剂对U(VI)的吸附去除效果对比

Table 5. Comparison of adsorption and removal effects of different adsorbents on U(VI)

Adsorbent	pH	T/K	q_max/(mg·g⁻¹)	Reference
C-TC	5	308	165.43	[20]
MXene/SA	4	298	126.82	[34]
C-TC-CS	6	313	141.96	[36]
PANI/Ti₃C₂T_x	5	298	102.8	[37]
PAO/Ti₃C₂T_x	4	298	98.04	[38]
Ti₃C₂-AO-PA	8.3	298	81.1	[47]
MX/EHL	5	303	231.95	This work
Notes: C-TC is Chloroacetic acid modified-Ti₃C₂T_x; MXene/SA is MXene composite sodium alginate gel microsphere; C-TC-CS is chloroacetic acid-modified MXene-CS gel microspheres; PANI/Ti₃C₂T_x is polyaniline modified Mxene composites; PAO/Ti₃C₂T_x is Polyamidoxime functionalized MXene composite; Ti₃C₂-AO-PA is polyamide enhanced amidoxime-functionalized Ti₃C₂ nanosheet; T is the reaction temperature; q_max is the maximum adsorption capacity.

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表 4 MX/EHL吸附U(VI)的热力学参数

Table 4. Thermodynamic parameters of MX/EHL adsorption of U(VI)

T/K	lnK⁰	ΔG⁰/(kJ·mol⁻¹)	ΔH⁰/(kJ·mol⁻¹)	ΔS⁰/(J·(mol·K)⁻¹)
293 K	4.69	−11.43	38.89	175.26
298 K	5.00	−12.39
303 K	5.23	−13.18
Notes: T is the thermodynamic temperature; K⁰ is the equilibrium constant at different temperatures; ΔH⁰ is the standard enthalpy change; ΔG⁰ is the standard free energy change; ΔS⁰ is the standard entropy change.

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