MXene改性材料的制备及其吸附除Sr<sup>2+</sup>性能

张鹏丽; 武莉娅; 杨宗政; 吴志国; 曹井国

MXene改性材料的制备及其吸附除Sr²⁺性能

天津科技大学　化工与材料学院, 天津 300457

基金项目: 天津市卤水化工与资源生态化利用重点实验室开放基金资助项目(BCERE201902)；国家科技重大项目子项目(2017 ZX07107-001)；天津市教委科研计划项目(自然科学)(2019 KJ225)

详细信息

通讯作者:
曹井国，博士，副教授，硕士生导师，研究方向为水污染防治技术　E-mail：cjg@tust.edu.cn

中图分类号: O647.33
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出版历程
- 收稿日期: 2022-10-21
- 修回日期: 2022-11-29
- 录用日期: 2022-12-10
- 网络出版日期: 2022-12-27

Preparation of modified MXene material and its adsorption performance for Sr²⁺

College of Chemical Engineering and Materials Science, Tianjin University of Science and Technology, Tianjin 300457, China

Funds: The Foundation of Tianjin Key Laboratory of Brine Chemical Engineering and Resource Eco-utilization (No. BCERE201902); Sub project of National Science and Technology Major Projects (No. 2017 ZX07107-001); Scientific Research Program of Tianjin Municipal Education Commission (Natural Science) (No. 2019 KJ225)

摘要

摘要: 目的本文选择以四元TiAlCN MAX为原相，对多层TiCNT MXene进行改性制备处理，并评估其对模拟放射性废水中Sr的吸附性能。方法借助有机小分子四甲基氢氧化铵(TMAOH)作插层剂，对多层TiCNT MXene进行改性制备处理，优化产物TiCNT/TMAOH的合成条件，并采用SEM-EDS、XRD、BET和FTIR等对改性前后的样品进行表征分析。结果复合材料TiCNT/TMAOH及其对模拟废水中Sr的吸附性能体现在①插层剂TMAOH将多层TiCNT的层间距由1.22 nm增大到1.48 nm，比表面积提高到3.154 m·g，同时提高了材料表面的氧官能团含量；②改性后的TiCNT/TMAOH对Sr的吸附去除率由原来的56.38%提高到99.78%，且可在弱酸性和碱性条件下(5~11)有效吸附除Sr；③在Na和K的质量浓度为500 mg∙L，具有较强的抗干扰能力，对Sr的去除率为64.54%~75.44%，竞争离子的抑制顺序为CaMgKNaCs；④ TiCNT/TMAOH在吸附除Sr中具有超快动力学(10 min，去除率为99.28%)，吸附过程符合准二级动力学模型(1.00≥≥0.9986)，化学吸附是主要的速控步骤；⑤吸附等温线符合R-P(0.999≥≥0.991)模型，产生吸附效果的动态点位于特定的位置，升温有利于吸附过程的进行；⑥经过四次的循环再生后，对Sr的去除率为69.56%，具有一定的再生性能；⑦在以自来水和湖水为背景配制的模拟含Sr废水中，可分别去除93.80%和68.49%的Sr；⑧TiCNT/TMAOH对Sr的吸附机制可能包括以下个方面：1)-N=与Sr、C-N与Sr、Ti-N与Sr、Ti-F与Sr以及Ti-O与Sr之间的螯合作用；2)负的表面电荷与Sr之间的静电作用；3)Ti-OH上的H与Sr之间的离子交换作用；4)层间截留作用。结论插层剂TMAOH的引入，使得改性后的多层TiCNT/TMAOH能够有效去除模拟废水中的Sr，在pH为6，温度为313 K时，对Sr的最大吸附容量为41.91 mg∙g，其吸附容量有待进一步提高。
- MXene /
- 四甲基氢氧化铵 /
- 改性材料 /
- 吸附 /
- Sr²⁺
Abstract: Ti₃CNT_x/TMAOH was prepared when tetramethylammonium hydroxide(TMAOH) was selected as the intercalating agent. Adsorption performance of Ti₃CNT_x/TMAOH on Sr²⁺ in simulated radioactive wastewater was evaluated. The synthesized Ti₃CNT_x/TMAOH was characterized by SEM-EDS, XRD, BET and FTIR. In the batch experiment, the effects of the dosage of adsorbent Ti₃CNT_x/TMAOH, time, pH and competitive ions on Sr²⁺ removal were investigated. The results show that the removal rate of Sr²⁺ is 99.28% when the dosage is 1.0 g·L⁻¹, pH is 6, and the time is 10 min. The inhibition order of competitive ions is Ca²⁺$ \text{ > > } $Mg²⁺$ \text{ > } $K⁺$ \text{ > } $Na⁺$ \text{ > } $Cs⁺. After four adsorption-desorption cycles, the Sr²⁺ removal rate is 69.56%. The adsorption is consistent with the pseudo-second-order kinetic. The adsorption isotherm data conforms to the R-P model. 93.80% and 68.49% Sr²⁺ can be removed in tap water and lake water, respectively. Sr²⁺ is adsorbed by Ti₃CNT_x/TMAOH via ion exchange, surface chelation, electrostatic adsorption and interlayer interception.
- MXene /
- tetramethylammonium hydroxide /
- modified materials /
- adsorption /
- Sr²⁺

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图 1 Ti₃CNT_x插层改性前表面(a)和断面(c)，以及改性后表面(b)和断面(d)的SEM图

Figure 1. SEM of surface (a) and cross section (c) before Ti₃CNT_x modification, and surface (b) and cross section (d) after modification

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图 2 Ti₃CNT_x(a)和Ti₃CNT_x/TMAOH(b)的N₂吸脱附及孔径图

Figure 2. N₂ adsorption-desorption and pore size of Ti₃CNT_x (a) and Ti₃CNT_x/TMAOH (b)

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图 3 Ti₃CNT_x(a)和Ti₃CNT_x/TMAOH(b)的EDS光谱

Figure 3. EDS spectra of Ti₃CNT_x (a) and Ti₃CNT_x/TMAOH (b)

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图 4 Ti₃CNT_x和Ti₃CNT_x/TMAOH的红外光谱

Figure 4. Infrared spectra of Ti₃CNT_x and Ti₃CNT_x/TMAOH

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图 5 Ti₃CNT_x和Ti₃CNT_x/TMAOH的XRD光谱

Figure 5. XRD spectra of Ti₃CNT_x and Ti₃CNT_x/TMAOH

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图 6 TMAOH用量对吸附剂Ti₃CNT_x/TMAOH去除Sr²⁺的影响

Figure 6. The effect of TMAOH dosage on Sr²⁺ removal by adsorbent Ti₃CNT_x/TMAOH

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图 7 Ti₃CNT_x和Ti₃CNT_x/TMAOH对Sr²⁺的去除效果

Figure 7. The removal effect of Ti₃CNT_x and Ti₃CNT_x/TMAOH for Sr²⁺

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图 8 pH值对Ti₃CNT_x/TMAOH吸附Sr²⁺的效果(a)和zeta电位(b)的影响

Figure 8. The effect of pH on Sr²⁺ adsorption effect (a) and zeta potential (b) of Ti₃CNT_x/TMAOH

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图 9 共存离子浓度对Ti₃CNT_x/TMAOH吸附Sr²⁺去除率的影响

Figure 9. The effect of coexisting ion concentration on Sr²⁺ removal by Ti₃CNT_x/TMAOH

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图 10 时间对Ti₃CNT_x/TMAOH去除Sr²⁺: (a)吸附容量和(b)去除率的影响; (c)拟一级和(d)拟二级动力学模型

Figure 10. The effect of contact time on Sr²⁺: (a) adsorption capacity and (b) removal rate of Ti₃CNT_x/TMAOH; (c) Pseudo-first-order and (d) pseudo-second-order kinetic model

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图 11 Ti₃CNT_x/TMAOH吸附Sr²⁺:(a)Langmuir、(b)Freundlich和(c)R-P吸附等温线(C_e为平衡状态下Sr²⁺的质量浓度)

Figure 11. Adsorption isotherms for Sr²⁺ : (a) Langmuir, (b) Freundlich, and (c) R-P on Ti₃CNT_x/TMAOH (C_e is the mass concentration of Sr²⁺ in equilibrium)

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图 12 Ti₃CNT_x/TMAOH吸附去除Sr²⁺的lnK_C与T⁻¹的线性拟合

Figure 12. Linear fit of lnK_C vs T⁻¹ for adsorption Sr²⁺ on Ti₃CNT_x/TMAOH

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图 13 Ti₃CNT_x/TMAOH吸附Sr²⁺的的再生实验

Figure 13. Regeneration experiment of Ti₃CNT_x/TMAOH for adsorption Sr²⁺

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图 14 Ti₃CNT_x/TMAOH吸附去除Sr²⁺前后的XPS和FTIR

Figure 14. XPS and FTIR before and after adsorption of Ti₃CNT_x/TMAOH for Sr²⁺

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图 15 Ti₃CNT_x/TMAOH吸附Sr²⁺的机制图

Figure 15. Mechanism diagram of Sr²⁺ adsorption by Ti₃CNT_x/TMAOH

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图 16 不同水环境下Ti₃CNT_x/TMAOH对Sr²⁺的去除率

Figure 16. Sr²⁺ removal rate of Ti₃CNT_x/TMAOH in various water environments

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表 1 Ti₃CNT_x和Ti₃CNT_x/TMAOH的比表面积、孔容和孔径数据

Table 1. The surface area, pore volume, and pore diameter of Ti₃CNT_x and Ti₃CNT_x/TMAOH

Material	Surface area/ (m²·g⁻¹)	Pore volume/ (cm³·g¹)	Pore diameter/ nm
Ti₃CNT_x	1.215	0.0044	38.01
Ti₃CNT_x/TMAOH	3.154	0.0029	16.13

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表 2 Ti₃CNT_x/TMAOH吸附Sr²⁺的动力学模型参数

Table 2. The parameters of adsorption kinetics model of Sr²⁺ adsorption on Ti₃CNT_x/TMAOH

kinetic model		5.5/(mg∙L⁻¹)	10/(mg∙L⁻¹)	30/(mg∙L⁻¹)	50/(mg∙L⁻¹)
Pseudo-first-order	q_e/(mg∙g⁻¹)	25.02	22.80	10.49	8.061
	k₁×10⁻⁴/(min⁻¹)	0.01869	5.540	34.50	127.10
	R²	0.1065	0.6222	0.6940	0.9302
Pseudo-second-order	q_e/(mg∙g⁻¹)	4.988	8.829	24.16	29.83
	k₂/(g∙mg⁻¹∙min⁻¹)	0.1573	0.08457	0.01053	0.00587
	R²	1.00	0.9986	0.9999	0.9998
Notes: q_e is the adsorption capacity at equilibrium time; k₁ and k₂ are reaction rate constants of pseudo-first-order and pseudo-second-order equations, respectively; R² is the correlation coefficient.

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表 3 Ti₃CNT_x/TMAOH吸附Sr²⁺的吸附等温线拟合参数

Table 3. Fitting parameters of adsorption isotherm for Sr²⁺ on Ti₃CNT_x/TMAOH

t/℃		Langmuir			Freundlich			R-P
t/℃	q_max/(mg∙g⁻¹)	K_L/(L∙mg⁻¹)	R²	K_F/(mg∙g⁻¹)	n	R²	A/(L∙g⁻¹)	B	g	R²
20	25.04	0.033	0.996	2.90	3	0.970	10.7	13	0.89	0.999
30	37.47	0.036	0.974	3.37	2	0.886	11.9	16	0.96	0.991
40	41.91	0.038	0.990	4.98	3	0.917	12.5	18	0.99	0.999
Notes: t is the reaction temperature; q_max represents the maximum adsorption capacity of Langmuir; K_L is Langmuir adsorption constant; K_F is the Freundlich adsorption constant, and n is the constant related to the adsorption strength; A and B are constants related to the adsorption capacity, and the index g is an empirical constant between 0 and 1.

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表 4 不同吸附剂对Sr²⁺的吸附去除效果对比

Table 4. Comparison of adsorption and removal effects of different adsorbents for Sr²⁺

Adsorbents	q_max/(mg∙g⁻¹)	C₀/(mg∙L⁻¹)	t/min	pH	References
Mn_xO_y-Sb_mO_n	30.20	4.4	~30	3.0-9.0	[25]
ZrO₂-MnO₂	30.86	100	~100	4.0-8.0	[26]
GO	23.83	7.4	—	6.5-11.0	[27]
M/GO	9.81	4.0	360	1.7-11.8	[28]
Commercial AC	7.58	50	—	8.0-11.0	[29]
Ti₃CNT_x/TMAOH	41.91	5.5	~120	5-11	This study
Notes: C₀ is the initial Sr²⁺ concentration of, t is the adsorption equilibrium time.

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表 5 Ti₃CNT_x/TMAOH吸附Sr²⁺的热力学参数Table 5 Thermodynamic parameter for adsorption Sr²⁺ on Ti₃CNT_x/TMAOH

ΔG/(kJ∙mol⁻¹)			ΔH/ (kJ∙mol⁻¹)	ΔS/ (J∙K⁻¹∙mol⁻¹)
293 K	303 K	313 K	ΔH/ (kJ∙mol⁻¹)	ΔS/ (J∙K⁻¹∙mol⁻¹)
−25.34	−26.39	−27.41	4.95	103.42
Notes: ΔG is Gibbs free energy change; ΔH is enthalpy change; ΔS is entropy change.

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表 6 Ti₃CNT_x/TMAOH在不同水环境下去除Sr²⁺前后的主要水质参数

Table 6. The main water quality parameters after Sr²⁺ removal by Ti₃CNT_x/TMAOH in different water environments

	pH	Na⁺/ (mg∙L⁻¹)	K⁺/ (mg∙L⁻¹)	Mg²⁺/ (mg∙L⁻¹)	Ca²⁺/ (mg∙L⁻¹)	Sr²⁺/ (mg∙L⁻¹)
TW	6.23	8.230	3.382	9.823	45.46	5.500
1.0/(g∙L⁻¹)		8.129	2.999	7.777	23.38	1.572
3.0/(g∙L⁻¹)		7.895	2.861	3.772	7.616	0.3411
LW	7.12	23.2	39.98	44.33	98.57	5.982
1.0/(g∙L⁻¹)		228.1	38.00	41.39	80.69	3.347
3.0/(g∙L⁻¹)		216.1	33.86	35.93	56.65	1.885
Notes: TW and LW represent tap water and lake water, respectively.

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