Thermal pretreatment of willow branches impacts yield and pore development of activated carbon in subsequent activation with ZnCl2 via modifying cellulose structure

doi:10.1016/j.cjche.2024.01.014

中国化学工程学报 ›› 2024, Vol. 69 ›› Issue (5): 227-237.DOI: 10.1016/j.cjche.2024.01.014

Thermal pretreatment of willow branches impacts yield and pore development of activated carbon in subsequent activation with ZnCl₂ via modifying cellulose structure

Linghui Kong¹, Chao Li¹, Runxing Sun¹, Shu Zhang², Yi Wang³, Jun Xiang³, Song Hu³, Dong Wang⁴, Chuanjun Leng⁴, Xun Hu¹

1. School of Material Science and Engineering, University of Jinan, Jinan 250022, China;
2. Joint International Research Laboratory of Biomass Energy and Materials, College of Materials Science and Engineering, Nanjing Forestry University, Nanjing 210037, China;
3. State Key Laboratory of Coal Combustion, Huazhong University of Science and Technology, Wuhan 430074, China;
4. Shandong BASAN Graphite New Material Plant, Zibo 255311, China

收稿日期:2023-10-13 修回日期:2024-01-04 出版日期:2024-05-28 发布日期:2024-07-01
通讯作者: Xun Hu,E-mail:Xun.Hu@outlook.com
基金资助:
This work was supported by the National Natural Science Foundation of China (52276195), Program for Supporting Innovative Research from Jinan (202228072); Program of Agricultural Development from Shandong (SD2019NJ015).

Thermal pretreatment of willow branches impacts yield and pore development of activated carbon in subsequent activation with ZnCl₂ via modifying cellulose structure

Linghui Kong¹, Chao Li¹, Runxing Sun¹, Shu Zhang², Yi Wang³, Jun Xiang³, Song Hu³, Dong Wang⁴, Chuanjun Leng⁴, Xun Hu¹

1. School of Material Science and Engineering, University of Jinan, Jinan 250022, China;
2. Joint International Research Laboratory of Biomass Energy and Materials, College of Materials Science and Engineering, Nanjing Forestry University, Nanjing 210037, China;
3. State Key Laboratory of Coal Combustion, Huazhong University of Science and Technology, Wuhan 430074, China;
4. Shandong BASAN Graphite New Material Plant, Zibo 255311, China

Received:2023-10-13 Revised:2024-01-04 Online:2024-05-28 Published:2024-07-01
Contact: Xun Hu,E-mail:Xun.Hu@outlook.com
Supported by:
This work was supported by the National Natural Science Foundation of China (52276195), Program for Supporting Innovative Research from Jinan (202228072); Program of Agricultural Development from Shandong (SD2019NJ015).

摘要/Abstract

摘要： Development of pore structures of activated carbon (AC) from activation of biomass with ZnCl₂ relies on content and structure of cellulose/hemicellulose in the feedstock. Thermal pretreatment of biomass could induce dehydration and/or aromatization to change the structure of cellulose/hemicellulose. This might interfere with evolution of structures of AC, which was investigated herein via thermal pretreatment of willow branch (WB) from 200 to 360 ℃ and the subsequent activation with ZnCl₂ at 550 ℃. The results showed that thermal pretreatment at 360 ℃ (WB-360) could lead to substantial pyrolysis to form biochar, with a yield of 31.9%, accompanying with nearly complete destruction of cellulose crystals and remarkably enhanced aromatic degree. However, cellulose residual in WB-360 could still be activated to form AC-360 with specific surface area of 1837.9 m²·g^-1, which was lower than that in AC from activation of untreated WB (AC-blank, 2077.8 m²·g^-1). Nonetheless, the AC-200 from activation of WB-200 had more developed pores (2113.9 m²·g^-1) and superior capability for adsorption of phenol, due to increased permeability of ZnCl₂ to the largely intact cellulose structure in WB-200. The thermal pretreatment did increase diameters of micropores of AC but reduced the overall yield of AC (26.8% for AC-blank versus 18.0% for AC-360), resulting from accelerated cracking but reduced intensity of condensation. In-situ infrared characterization of the activation showed that ZnCl₂ mainly catalyzed dehydration, dehydrogenation, condensation, and aromatization but not cracking, suppressing the formation of derivatives of cellulose and lignin in bio-oil. The thermal pretreatment formed phenolic -OH and CO with higher chemical innerness, which changed the reaction network in activation, shifting morphology of fibrous structures in AC-blank to “melting surface” in AC-200 or AC-280.

关键词: Thermal pretreatment, Activation with ZnCl₂, Willow branch, Activated carbon, Biochar

Abstract: Development of pore structures of activated carbon (AC) from activation of biomass with ZnCl₂ relies on content and structure of cellulose/hemicellulose in the feedstock. Thermal pretreatment of biomass could induce dehydration and/or aromatization to change the structure of cellulose/hemicellulose. This might interfere with evolution of structures of AC, which was investigated herein via thermal pretreatment of willow branch (WB) from 200 to 360 ℃ and the subsequent activation with ZnCl₂ at 550 ℃. The results showed that thermal pretreatment at 360 ℃ (WB-360) could lead to substantial pyrolysis to form biochar, with a yield of 31.9%, accompanying with nearly complete destruction of cellulose crystals and remarkably enhanced aromatic degree. However, cellulose residual in WB-360 could still be activated to form AC-360 with specific surface area of 1837.9 m²·g^-1, which was lower than that in AC from activation of untreated WB (AC-blank, 2077.8 m²·g^-1). Nonetheless, the AC-200 from activation of WB-200 had more developed pores (2113.9 m²·g^-1) and superior capability for adsorption of phenol, due to increased permeability of ZnCl₂ to the largely intact cellulose structure in WB-200. The thermal pretreatment did increase diameters of micropores of AC but reduced the overall yield of AC (26.8% for AC-blank versus 18.0% for AC-360), resulting from accelerated cracking but reduced intensity of condensation. In-situ infrared characterization of the activation showed that ZnCl₂ mainly catalyzed dehydration, dehydrogenation, condensation, and aromatization but not cracking, suppressing the formation of derivatives of cellulose and lignin in bio-oil. The thermal pretreatment formed phenolic -OH and CO with higher chemical innerness, which changed the reaction network in activation, shifting morphology of fibrous structures in AC-blank to “melting surface” in AC-200 or AC-280.

Key words: Thermal pretreatment, Activation with ZnCl₂, Willow branch, Activated carbon, Biochar

Linghui Kong, Chao Li, Runxing Sun, Shu Zhang, Yi Wang, Jun Xiang, Song Hu, Dong Wang, Chuanjun Leng, Xun Hu. Thermal pretreatment of willow branches impacts yield and pore development of activated carbon in subsequent activation with ZnCl₂ via modifying cellulose structure[J]. 中国化学工程学报, 2024, 69(5): 227-237.

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Thermal pretreatment of willow branches impacts yield and pore development of activated carbon in subsequent activation with ZnCl₂ via modifying cellulose structure

Thermal pretreatment of willow branches impacts yield and pore development of activated carbon in subsequent activation with ZnCl₂ via modifying cellulose structure

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