Effect and mechanism of removing chlorophenolic pollutants from water by refinery residual activated sludge pyrolytic carbon

doi:10.19965/j.cnki.iwt.2025-0011

Abstract

Abstract:

Sludge pyrolytic carbon(SPC) was prepared by one-step pyrolysis of residual activated sludge from refineries, and its structure was characterized. It was used to adsorb 4-chlorophenol(4-CP) to investigate its adsorption performance for 4-CP. The results showed that the SPC prepared at pyrolysis temperature of 600 ℃, residence time of 1.5 h, and heating rate of 10 ℃/min had an irregular surface with sheet-like particle stacking structure and a large number of mesopores. At the optimal dosage (3.75 g/L) in the experiment, the adsorption capacity for 4-CP was 11.79 mg/g, and the adsorption capacity remained stable within pH range of 3-11. The adsorption process of 4-CP by SPC followed the Weber-Morris intraparticle diffusion model, indicating that the rate limiting step of the adsorption process was diffusion within mesopores and micropores, and there was pore filling phenomenon. In addition, the Dubinin-Radushkevich(D-R) model also had a high degree of fit with adsorption, indicating that there were both physical and chemical interactions in the adsorption process. The —OH, C $̿$ O, and π-π structures of sp²-C were the main reaction sites of SPC, which adsorbed 4-CP through hydrophobic, π-π, and hydrogen bonding interactions, and then generated ¹O₂ through C $̿$ O and defected sites to slowly oxidize 4-CP. After 4 fixed bed cycle experiments, SPC showed stable adsorption performance for 4-CP and 2-chlorophenol, and had the potential to be used as a chlorophenol adsorbent.

Key words: sludge pyrolytic carbon, adsorption, 4-chlorophenol, fixed bed, adsorption mechanism

摘要：

通过一步热解法热解炼厂剩余污泥制备污泥热解炭（Sludge pyrolytic carbon，SPC），对其结构进行表征，并将其用于吸附4-氯苯酚（4-CP），探究其对4-CP的吸附性能。研究结果表明，在热解温度600 ℃、热解停留时间1.5 h、升温速率10 ℃/min下制得的SPC表面不规整，具有片状颗粒堆积结构和大量介孔，其在实验的最佳投加量（3.75 g/L）下对4-CP的吸附量为11.79 mg/g，且吸附量在pH处于3~11的范围内保持稳定。SPC对4-CP的吸附过程较为遵循Weber-Morris颗粒内扩散模型，表明吸附过程的限速步骤是介孔和微孔内扩散，存在孔隙填充现象，此外Dubinin-Radushkevich（D-R）模型与吸附也具有较高拟合度，表明吸附过程同时存在物理和化学作用。—OH、C $̿$ O和sp²-C的π-π结构是SPC的主要反应位点，SPC通过疏水作用、π-π作用、氢键作用吸附4-CP，进而通过C $̿$ O和缺陷位点生成¹O₂使4-CP缓慢氧化。SPC经4次固定床循环实验后对4-CP、2-氯酚的吸附性能稳定，具有作为氯酚类吸附剂的应用潜力。

关键词: 污泥热解炭, 吸附, 4-氯苯酚, 固定床, 吸附机制

CLC Number:

X705

Yuntao HU, Yue CAO, Zhuoyu LI, Yali ZHAN, Qinghong WANG, Chunmao CHEN. Effect and mechanism of removing chlorophenolic pollutants from water by refinery residual activated sludge pyrolytic carbon[J]. Industrial Water Treatment, 2025, 45(6): 61-72.

胡昀涛, 曹越, 李琢宇, 詹亚力, 王庆宏, 陈春茂. 炼厂剩余污泥热解炭去除水中氯酚类污染物的效果与机制[J]. 工业水处理, 2025, 45(6): 61-72.

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URL: https://www.iwt.cn/EN/10.19965/j.cnki.iwt.2025-0011

https://www.iwt.cn/EN/Y2025/V45/I6/61

Figures/Tables 17

Fig.1 Schematic diagram of the fixed bed device

Fig.2 XRD of SPC prepared at different pyrolysis temperatures

Fig.3 Raman spectra of SPC prepared at different pyrolysis temperatures

Fig.4 XPS （C 1s） of SPC prepared at different pyrolysis temperatures

Fig.5 Adsorption kinetics curves of 4-CP by SPC prepared under different pyrolysis temperatures（a），pyrolysis residence times（b）， and heating rates （c）

Fig.6 The effect of SPC dosage（a） and pH（b） on SPC adsorption of 4-CP

Table 1 Fitting parameters of kinetic models for SPC adsorption of 4-CP

吸附剂	q _exp/（mg·g^-1）	准一级吸附动力学模型		准二级吸附动力学模型		颗粒内扩散模型
吸附剂	q _exp/（mg·g^-1）	q _e/（mg·g^-1）	R ²	q _e/（mg·g^-1）	R ²	R $12$	R $22$	R $32$
SPC-600 ℃-1.5 h-10 ℃/min	12.47	10.79	0.806	11.21	0.885	0.898	0.947	0.957
SPC-400 ℃-1.5 h-10 ℃/min	5.91	5.04	0.702	5.31	0.829	0.920	0.929	0.963
SPC-800 ℃-1.5 h-10 ℃/min	10.67	8.95	0.842	9.13	0.875	0.856	0.988	0.887
SPC-600 ℃-0.5 h-10 ℃/min	10.41	9.06	0.835	9.37	0.906	0.886	0.882	0.997
SPC-600 ℃-2.5 h-10 ℃/min	9.13	7.63	0.779	7.95	0.864	0.900	0.964	0.949
SPC-600 ℃-0.5 h-5 ℃/min	11.57	9.91	0.826	10.24	0.894	0.899	0.954	0.989
SPC-600 ℃-0.5 h-20 ℃/min	10.67	9.13	0.795	9.51	0.884	0.890	0.965	0.956

Table 1 Fitting parameters of kinetic models for SPC adsorption of 4-CP

吸附剂	q _exp/（mg·g^-1）	准一级吸附动力学模型		准二级吸附动力学模型		颗粒内扩散模型
吸附剂	q _exp/（mg·g^-1）	q _e/（mg·g^-1）	R ²	q _e/（mg·g^-1）	R ²	R $12$	R $22$	R $32$
SPC-600 ℃-1.5 h-10 ℃/min	12.47	10.79	0.806	11.21	0.885	0.898	0.947	0.957
SPC-400 ℃-1.5 h-10 ℃/min	5.91	5.04	0.702	5.31	0.829	0.920	0.929	0.963
SPC-800 ℃-1.5 h-10 ℃/min	10.67	8.95	0.842	9.13	0.875	0.856	0.988	0.887
SPC-600 ℃-0.5 h-10 ℃/min	10.41	9.06	0.835	9.37	0.906	0.886	0.882	0.997
SPC-600 ℃-2.5 h-10 ℃/min	9.13	7.63	0.779	7.95	0.864	0.900	0.964	0.949
SPC-600 ℃-0.5 h-5 ℃/min	11.57	9.91	0.826	10.24	0.894	0.899	0.954	0.989
SPC-600 ℃-0.5 h-20 ℃/min	10.67	9.13	0.795	9.51	0.884	0.890	0.965	0.956

Fig.7 Particle size distribution of SPC

Fig.8 EPR of SPC

Fig.9 The concentration change of Cl^- in the systems

Fig.10 SEM images of SPC

Fig.11 N₂ adsorption-desorption isotherms and pore size distribution of SPC before and after adsorbing 4-CP

Table 3 Specific surface area and pore parameters of SPC before and after adsorbing 4-CP

项目

总比表面积/

（m²·g^-1）

微孔比表面积/

（m²·g^-1）

外比表面积/

（m²·g^-1）

总孔容/

（cm³·g^-1）

平均孔径/

Fig.12 XPS spectra of SPC-600 ℃ after adsorption of 4-CP

Fig.13 FT-IR spectra of SPC before and after adsorbing 4-CP

Fig.14 The speculated mechanism of SPC removing 4-CP

Fig.15 Recycling experiments

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