Effect of curing temperature of phthalonitrile resin on the properties of resultant hierarchical porous carbon

doi:10.1016/j.cjche.2024.11.016

Chinese Journal of Chemical Engineering ›› 2025, Vol. 79 ›› Issue (3): 45-52.DOI: 10.1016/j.cjche.2024.11.016

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Effect of curing temperature of phthalonitrile resin on the properties of resultant hierarchical porous carbon

Xing Yun¹, Kewen Zhang¹, Zhaojun Chu¹, Beitao Liu¹, Yan Kou², Xigao Jian¹, Zhihuan Weng¹

1. State Key Laboratory of Fine Chemicals, Frontiers Science Center for Smart Materials Oriented Chemical Engineering, Liaoning Technology Innovation Center of High Performance Resin Materials, Department of Polymer Science & Engineering, Dalian University of Technology, Dalian 116024, China;
2. Thermochemistry Laboratory, Liaoning Province Key Laboratory of Thermochemistry for Energy and Materials, Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China

Received:2024-07-27 Revised:2024-10-31 Accepted:2024-11-17 Online:2025-01-23 Published:2025-03-28
Supported by:
This work was supported by the National Natural Science Foundation of China (51673033 and 52073038), the Fundamental Research Funds for the Central Universities (DUT22LAB605).

Effect of curing temperature of phthalonitrile resin on the properties of resultant hierarchical porous carbon

Xing Yun¹, Kewen Zhang¹, Zhaojun Chu¹, Beitao Liu¹, Yan Kou², Xigao Jian¹, Zhihuan Weng¹

1. State Key Laboratory of Fine Chemicals, Frontiers Science Center for Smart Materials Oriented Chemical Engineering, Liaoning Technology Innovation Center of High Performance Resin Materials, Department of Polymer Science & Engineering, Dalian University of Technology, Dalian 116024, China;
2. Thermochemistry Laboratory, Liaoning Province Key Laboratory of Thermochemistry for Energy and Materials, Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China

通讯作者: Yan Kou,E-mail:kouyan@dicp.ac.cn;Zhihuan Weng,E-mail:zweng@dlut.edu.cn
基金资助:
This work was supported by the National Natural Science Foundation of China (51673033 and 52073038), the Fundamental Research Funds for the Central Universities (DUT22LAB605).

Abstract

Abstract: Heteroatom-doped porous carbon materials have been widely studied due to their high specific surface area and high heteroatom content, but it is difficult to achieve high specific surface area and high heteroatom content at the same time. Herein, a simple method is introduced to prepare N/O co-doped hierarchical porous carbon materials (DNZKs). Phthalonitrile resins (DNZs) were prepared by using 1,3-bis(3,4-dicyanophenoxy)benzene as raw material and ZnCl₂/urea as composite curing agent, and then using KOH as activator to successfully prepare DNZKs with high specific surface area, developed pores and high N/O content. The porous carbon material (DNZK@400) obtained at a curing temperature of 400 ℃ has the highest N content (4.97% (mass)), a large specific surface area (2026 m²·g^-1), a high micropore proportion (0.9), a high O content (7.53% (mass)), and the best specific capacitance (up to 567 F·g^-1 at 0.1 A·g^-1), which can be attribute to the high temperature resistance of the nitrogen-containing aromatic heterocyclic structure in DNZs. When the mass ratio of resin and KOH is 1:1, the specific capacitance of the sample tested by the acid three-electrode system is obtained, and it is found that the material has high cycling stability (119% specific capacitance retention after 100,000 cycle tests). This work proposes a simple and easy-to-operate method for the preparation of multifunctional porous carbon.

Key words: Supercapacitor, Phthalonitrile resin, N/O co-doped, Porous carbon, High cycling stability

摘要： Heteroatom-doped porous carbon materials have been widely studied due to their high specific surface area and high heteroatom content, but it is difficult to achieve high specific surface area and high heteroatom content at the same time. Herein, a simple method is introduced to prepare N/O co-doped hierarchical porous carbon materials (DNZKs). Phthalonitrile resins (DNZs) were prepared by using 1,3-bis(3,4-dicyanophenoxy)benzene as raw material and ZnCl₂/urea as composite curing agent, and then using KOH as activator to successfully prepare DNZKs with high specific surface area, developed pores and high N/O content. The porous carbon material (DNZK@400) obtained at a curing temperature of 400 ℃ has the highest N content (4.97% (mass)), a large specific surface area (2026 m²·g^-1), a high micropore proportion (0.9), a high O content (7.53% (mass)), and the best specific capacitance (up to 567 F·g^-1 at 0.1 A·g^-1), which can be attribute to the high temperature resistance of the nitrogen-containing aromatic heterocyclic structure in DNZs. When the mass ratio of resin and KOH is 1:1, the specific capacitance of the sample tested by the acid three-electrode system is obtained, and it is found that the material has high cycling stability (119% specific capacitance retention after 100,000 cycle tests). This work proposes a simple and easy-to-operate method for the preparation of multifunctional porous carbon.

关键词: Supercapacitor, Phthalonitrile resin, N/O co-doped, Porous carbon, High cycling stability

Xing Yun, Kewen Zhang, Zhaojun Chu, Beitao Liu, Yan Kou, Xigao Jian, Zhihuan Weng. Effect of curing temperature of phthalonitrile resin on the properties of resultant hierarchical porous carbon[J]. Chinese Journal of Chemical Engineering, 2025, 79(3): 45-52.

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Effect of curing temperature of phthalonitrile resin on the properties of resultant hierarchical porous carbon

Effect of curing temperature of phthalonitrile resin on the properties of resultant hierarchical porous carbon

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