功能化三维石墨烯复合气凝胶对U(VI)的吸附行为

王子鸣; 赵家印; 秦凯文; 张爽; 王英财; 刘云海; 柳玉辉

doi:10.13801/j.cnki.fhclxb.20230113.001

功能化三维石墨烯复合气凝胶对U(VI)的吸附行为

doi: 10.13801/j.cnki.fhclxb.20230113.001

1.
东华理工大学　核科学与工程学院，南昌 330013
2.
东华理工大学　化学生物与材料科学学院，南昌 330013

基金项目: 国家自然科学基金委员会地区科学基金项目(22266003)；江西省科技厅青年基金项目(20212BAB213005 )

详细信息

通讯作者:
刘云海，博士，教授，博士生导师，研究方向为放射性核素吸附分离与污染治理　E-mail：yhliu@ecut.edu.cn；

柳玉辉，博士，副教授，硕士生导师，研究方向为放射性核素吸附分离与污染治理、乏燃料干法后处理　E-mail：liuyuhui@ecut.edu.cn

中图分类号: TB33；X703.1
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出版历程
- 收稿日期: 2022-11-18
- 修回日期: 2022-12-16
- 录用日期: 2022-12-31
- 网络出版日期: 2023-01-14
- 刊出日期: 2023-11-01

Adsorption behavior of U(VI) on functionalized three-dimensional graphene composite aerogel

1.
School of Nuclear Science and Engineering, East China University of Technology, Nanchang 333013, China
2.
School of Chemical Biology and Materials Science, East China University of Technology, Nanchang 333013, China

Funds: National Regional Science Foundation of China (22266003); Youth Fund Project of Jiangxi Provincial Department of Science and Technology (20212BAB213005)

摘要

摘要: 核工业循环链中产生的大量含铀废水会对人类健康及生态环境造成损害，因此高效处理含铀废水是保障核工业可持续发展及人类生态安全的重要一环。以氧化石墨烯为前驱体自组装合成了聚乙烯亚胺(PEI)功能化的复合气凝胶(MGO/PEI)，并用于去除水溶液中的U(Ⅵ)。通过探究不同PEI投放量、稳定性、pH值、时间、U(Ⅵ)浓度及温度对U(VI)的去除影响。结果表明：在298 K、pH=6时，最大吸附量为1027.01 mg·g⁻¹，符合准二级动力学模型和Langmuir等温吸附模型。热力学常数表明MGO/PEI对U(Ⅵ)的吸附是一个自发吸热的过程。XPS分析表明去除机制主要是由于氨基及含氧官能团与U(VI)的表面络合。
- 石墨烯 /
- 气凝胶 /
- 聚乙烯亚胺 /
- 吸附 /
- 铀
Abstract: A large amount of uranium-containing wastewater produced in the nuclear industry circulation chain will cause damage to human health and ecological environment. Therefore, efficient treatment of uranium-containing wastewater is an important part of ensuring the sustainable development of the nuclear industry and human ecological security. Polyethyleneimine (PEI) functionalized composite aerogel (MGO/PEI) was synthesized by self-assembly of graphene oxide as a precursor and used to remove U(VI) from aqueous solution. The effects of different PEI dosage, stability, pH value, time, U(VI) concentration and temperature on the removal of U(VI) were investigated. The results showed that the adsorption behavior was accorded with the pseudo-second-order kinetic model and the Langmuir isothermal adsorption model at 298 K and pH=6, and the maximum adsorption capacity was 1027.01 mg·g⁻¹. The thermodynamic constants indicated that the adsorption of U(VI) by MGO/PEI was a spontaneous endothermic process. XPS analysis showed that the removal mechanism was mainly due to the surface complexation of amino and oxygen-containing functional groups with U(VI).
- graphene /
- aerogel /
- polyethyleneimine /
- adsorption /
- uranium

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图 1 氧化石墨烯/聚乙烯亚胺复合气凝胶(MGO/PEI)的制备流程示意图

GO—Graphene oxide; MCC—Microcrystalline cellulose

Figure 1. Schematic for the preparation process of graphene oxide/polyethyleneimine composite aerogel (MGO/PEI)

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图 2 MGO/PEI复合气凝胶可能的合成机制

Figure 2. Possible synthesis mechanism of MGO/PEI composite aerogel

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图 3 GO/PEI (a)、MGO/PEI1 (b)、MGO/PEI2 (c)、MGO/PEI3 (d)、MGO/PEI4 (e) 的SEM图像和MGO/PEI3 (f) 的横截面

Figure 3. SEM images of GO/PEI (a), MGO/PEI1 (b), MGO/PEI2 (c), MGO/PEI3 (d), MGO/PEI4 (e) and intersecting surface image of MGO/PEI3 (f)

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图 4 MGO/PEI1 (a)、MGO/PEI2 (b)、MGO/PEI3 (c) 的TEM及Mapping图像

Figure 4. TEM and Mapping images of MGO/PEI1 (a), MGO/PEI2 (b), MGO/PEI3 (c)

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图 5 (a) GO和MGO/PEI的XRD图谱；(b) GO、MCC、GO/PEI及MGO/PEI的FTIR图谱；(c) MGO/PEI的Raman图谱

I_D/I_G—Intensity ratio of peak D to peak G

Figure 5. (a) XRD patterns of GO and MGO/PEI; (b) FTIR spectras of GO, MCC, GO/PEI and MGO/PEI; (c) Raman spectras of MGO/PEI

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图 6 (a) MGO/PEI的TG曲线；(b) 不同负荷对MGO/PEI的压缩过程；(c) MGO/PEI3的亲水接触角；(d) MGO/PEI3在U(VI)溶液中的时间稳定性

Figure 6. (a) TG curves of MGO/PEI; (b) Digital images of the compression process of MGO/PEI when loaded by different mass; (c) Water contact angel images of MGO/PEI3; (d) Time stability digital images of MGO/PEI3 in U(VI) solution

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图 7 (a) pH值对MGO/PEI吸附U(VI)的影响；(b) U(VI)在不同pH下的物种形态(C₀=50 mg·L⁻¹，P_CO2=38.5035 Pa)；(c)接触时间对MGO/PEI吸附U(VI)的影响；(d)接触时间对MGO/PEI去除U(VI)的影响

Figure 7. (a) Effect of pH on the adsorption of U(VI) by MGO/PEI; (b) Species morphology of U(VI) at different pH (C₀=50 mg·L⁻¹, P_CO2=38.5035 Pa); (c) Effect of contact time on the adsorption of U(VI) by MGO/PEI; (d) Effect of contact time on the removal rate of U(VI) by MGO/PEI

q_e—Equilibrium adsorption capacity; t—Adsorption time; C₀—Initial concentration; Pco₂—Atmospheric pressure of dioxide in the air

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图 8 准一级动力学模型 (a)、准二级动力学模型 (b)、Elovich模型 (c)、粒子内扩散模型 (d)

Figure 8. Pseudo-first order kinetics model (a), Pseudo-second order kinetics model (b), Elovich model (c), Internal diffusion model (d)

q_t—Adsorption capacity at time t

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图 9 MGO/PEI对U(VI)的Langmuir和Freundlich吸附等温模型

Figure 9. Langmuir and Freundlich adsorption isothermal models of U(VI) on MGO/PEI

C_e—Concentration at adsorption equilibrium

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图 10 温度对MGO/PEI吸附U(VI)的影响

Figure 10. Effect of temperature on the adsorption of U(VI) by MGO/PEI

K_d—Distribution coefficient; T—Kelvin temperature

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图 11 吸附前后MGO/PEI的XPS谱图对比：(a)全谱；(b) U4f精细谱；(c) C1s精细谱；(d) N1s精细谱；(e) O1s精细谱

Figure 11. XPS spectra of MGO/PEI before and after adsorption: (a) Survey scan; High resolution scans of U4f (b), C1s (c), N1s (d), O1s (e)

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图 12 吸附后MGO/PEI的SEM图像及EDS能谱图

Figure 12. SEM image and EDS of MGO/PEI after adsorption

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图 13 MGO/PEI对U(VI)的洗脱性能 (a) 和循环利用性能 (b)

Figure 13. Elution performance (a) and recycling performance (b) of MGO/PEI on U(VI)

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图 14 MGO/PEI在混合溶液下的吸附量 (a)、去除率及分配系数K_d(b)

Figure 14. Adsorption capacity (a), removal rate and distribution coefficient K_d (b) of MGO/PEI in mixed solution

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表 1 不同吸附剂的PEI掺杂量

Table 1. PEI doping amount of different adsorbents

Adsorbent	Doping mass ratio
Adsorbent	MCC	GO	PEI
GO/PEI	–	1	1
MGO/PEI1	1	1	1
MGO/PEI2	1	1	3
MGO/PEI3	1	1	5
MGO/PEI4	1	1	7

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表 2 MGO/PEI的Mapping元素含量

Table 2. Mapping element content of MGO/PEI

Adsorbent	Elements content/at%
Adsorbent	C	N	O
MGO/PEI1	87.81	6.75	5.44
MGO/PEI2	85.47	8.71	5.72
MGO/PEI3	84.64	9.56	5.80

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表 3 MGO/PEI对U(VI)的准一级、准二级和Elovich动力学参数

Table 3. Pseudo-first order kinetic, Pseudo-second order kinetic and Elovich kinetic parameters of U(VI) on MGO/PEI

Adsorbent	q_{e, exp.}/ (mg·g⁻¹)	Pseudo-first order model			Pseudo-second order model			Elovich model
Adsorbent	q_{e, exp.}/ (mg·g⁻¹)	q_e,cal./(mg·g⁻¹)	k₁/min⁻¹	R²	q_e,cal./(mg·g⁻¹)	k₂/(g·mg⁻¹·min⁻¹)	R²	α/(mg·g⁻¹·min⁻¹)	β/(mg·g⁻¹)	R²
MGO/PEI1	104.38	93.64	1.51×10⁻¹	0.94	102.58	1.76×10⁻³	0.97	5.36×10¹	5.89×10⁻²	0.95
MGO/PEI2	246.57	240.54	4.55×10⁻¹	0.95	250.60	3.15×10⁻³	0.99	2.02×10⁵	4.55×10⁻²	0.70
MGO/PEI3	249.47	246.70	5.71×10⁻¹	0.96	251.58	4.18×10⁻³	0.98	2.24×10⁵	5.48×10⁻²	0.69
Notes: q_{e, exp.}—Experimental equilibrium adsorption capacity; q_{e, cal.}—Calculated equilibrium adsorption capacity; k₁—Rate constants of Pseudo-first-order model; k₂—Rate constants of Pseudo-second-order model; α—Initial adsorption rate of Elovich model; β—Desorption constant of Elovich model; R²—Fitting constant.

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表 4 MGO/PEI对U(VI)离子内扩散动力学参数

Table 4. Internal diffusion kinetic parameters of U(VI) on MGO/PEI

Adsorbent	Intraparticle diffusion model
Adsorbent	k_i₁ /(mg·g⁻¹·min^1/2)	R²	k_i2 /(mg·g⁻¹·min^1/2)	R²
MGO/PEI1	18.92	0.84	2.36	0.88
MGO/PEI2	35.49	0.86	0.43	0.85
MGO/PEI3	31.72	0.74	0.04	0.36
Note: k_i—Rate constants of Webber-Morris model.

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表 5 MGO/PEI对U(VI)的吸附等温模型参数

Table 5. Adsorption isothermal model parameters of U(VI) on MGO/PEI

Adsorbent	Langmuir model			Freundlich model
Adsorbent	q_m/(mg·g⁻¹)	k_L/(L·mg⁻¹)	R²	k_F/((mg·g⁻¹)·(mg·L⁻¹)^−1/n)	n	R²
MGO/PEI1	179.53	0.02	0.95	18.26	2.43	0.84
MGO/PEI2	537.29	0.84	0.91	269.05	6.25	0.89
MGO/PEI3	1027.01	0.40	0.97	392.98	4.54	0.78
Notes: q_m—Constants for adsorption capacity of Langmuir model; k_L—Constants for affinity of Langmuir model; k_F—Constant of Freundlich model; n—Favorability factor of the adsorption.

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表 6 MGO/PEI对U(VI)的热力学参数

Table 6. Thermodynamics parameters of U(VI) on MGO/PEI

Adsorbent	ΔH^ο/(kJ·mol⁻¹)	ΔS^ο/(kJ·mol⁻¹)	ΔG^ο/(kJ·mol⁻¹)
Adsorbent	ΔH^ο/(kJ·mol⁻¹)	ΔS^ο/(kJ·mol⁻¹)	298 K	308 K	318 K	328 K	338 K
MGO/PEI1	5.07	30.48	−33.40	−35.91	−38.47	−41.00	−43.53
MGO/PEI2	0.87	20.53	−43.65	−45.36	−47.07	−48.77	−50.48
MGO/PEI3	0.94	21.90	−46.47	−48.29	−50.11	−51.93	−53.75
Notes: ΔH^ο—Heat of the adsorption; ΔS^ο—Standard entropy change; ΔG^ο—Gibbs free energy of adsorption.

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表 7 不同气凝胶复合吸附剂对U(VI)的吸附性能比较

Table 7. Comparison of U(VI) adsorption performance of different aerogel composite adsorbents

Adsorbent	pH	Adsorption time/min	Adsorption capacity/(mg·g⁻¹)	Adsorption mechanism	Refs.
CNFs aerogels	5.0	100	440.60	Carboxyl coordination complex	[38]
GONRs aerogels	4.5	60	430.60	Oxygen functional groups chemical adsorption	[39]
CS-PTADMA3 aerogels	6.0	480	160.00	Coordination and electrostatic adsorption	[40]
MgO-N aerogels	4.0	100	1061.80	Electrical interaction and surface complexation	[41]
GO@PDA/CS aerogels	6.0	50	415.90	Coordination of nitrogen and oxygen functional groups	[42]
IAA-CTSA aerogels	6.5	360	847.50	Cation-π interaction, surface complexation and electrostatic interaction	[43]
Pr₂O₃ aerogels	7.0	240	770.60	Inner-sphere surface complexation	[44]
MGO/PEI aerogels	6.0	40	1027.01	Complexation of amide carbonyl and hydroxyl function groups	This work
Notes: CNFs aerogels—Cellulose nanofibers aerogels; GONRs aerogels—Graphene oxide nanoribbons aerogels; CS-PTADMA3 aerogels—Chitosan-based aerogels; GO@PDA/CS aerogels—Chitosan crosslinked dopamine modified graphene oxide aerogels; IAA-CTSA aerogels—Indole-modified cross-linked chitosan aerogel.

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