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Green Supercritical CO 2 Ion-Exchange Strategy for Cation Engineering in Polyheptazine Imides Towards Efficient Photoreduction CO 2 to C 2 H 4.

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Title: Green Supercritical CO 2 Ion-Exchange Strategy for Cation Engineering in Polyheptazine Imides Towards Efficient Photoreduction CO 2 to C 2 H 4.
Authors: Peng, Xin1 (AUTHOR), Du, Lina2 (AUTHOR) fugl@hhstu.edu.cn, Fu, Gaoliang1,2 (AUTHOR), Zhang, Shouren2 (AUTHOR), Ma, Junying1 (AUTHOR) majy379@163.com
Source: Nanomaterials (2079-4991). Apr2026, Vol. 16 Issue 8, p489. 13p.
Subjects: Supercritical carbon dioxide, Ion exchange (Chemistry), Coupling reactions (Chemistry), Photoreduction, Photocatalysts, Ethylene synthesis
Abstract: Photocatalytic reduction of carbon dioxide (CO2) into high-value multicarbon products, such as ethylene (C2H4), remains a significant challenge due to the difficult C-C coupling process. Potassium poly(heptazine imide) (K-PHI) is a promising photocatalyst, yet efficiently exchanging its interlayer cations to tune catalytic selectivity without causing structural degradation is difficult. Herein, an efficient and green supercritical CO2 (SC CO2) assisted ion-exchange strategy was developed to successfully prepare a series of mono-/di-/trivalent cation-doped M-PHI photocatalysts (M = H+, Na+, Sr+, Ca2+, Co2+, Fe3+). Systematic characterizations confirmed that the SC-CO2 treatment successfully achieved in-depth cation substitution without destroying the intrinsic heptazine framework, effectively regulating the interlayer structure and significantly optimizing the photoelectrochemical charge separation. Among the prepared samples, H-PHI exhibited the optimal photocatalytic CO2 reduction performance with an outstanding selectivity toward C2H4 generation. Under simulated sunlight irradiation for 3 h, the yields of CO, CH4, and C2H4 C2H4 C2H4 reached 3564.87, 807.32, and 40.00 μmol·g−1, respectively, significantly outperforming pristine K-PHI and other metal-doped samples. Crucially, isotope-tracing experiments utilizing a SC CO2-DCl treatment detected deuterated CH4 and C2H4 products, providing direct evidence that the hydrogen in the carbon products originates from the introduced protons, thereby elucidating the precise reaction pathway for C-C coupling. This study provides a green and efficient supercritical CO2 ion exchange strategy for the cation engineering of crystalline carbon nitride, and also offers new ideas and methods for designing high-activity photocatalysts for photocatalytic CO2 reduction. [ABSTRACT FROM AUTHOR]
Copyright of Nanomaterials (2079-4991) is the property of MDPI and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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  Label: Title
  Group: Ti
  Data: Green Supercritical CO 2 Ion-Exchange Strategy for Cation Engineering in Polyheptazine Imides Towards Efficient Photoreduction CO 2 to C 2 H 4.
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  Data: <searchLink fieldCode="AR" term="%22Peng%2C+Xin%22">Peng, Xin</searchLink><relatesTo>1</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Du%2C+Lina%22">Du, Lina</searchLink><relatesTo>2</relatesTo> (AUTHOR)<i> fugl@hhstu.edu.cn</i><br /><searchLink fieldCode="AR" term="%22Fu%2C+Gaoliang%22">Fu, Gaoliang</searchLink><relatesTo>1,2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Zhang%2C+Shouren%22">Zhang, Shouren</searchLink><relatesTo>2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Ma%2C+Junying%22">Ma, Junying</searchLink><relatesTo>1</relatesTo> (AUTHOR)<i> majy379@163.com</i>
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  Data: <searchLink fieldCode="JN" term="%22Nanomaterials+%282079-4991%29%22">Nanomaterials (2079-4991)</searchLink>. Apr2026, Vol. 16 Issue 8, p489. 13p.
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  Data: <searchLink fieldCode="DE" term="%22Supercritical+carbon+dioxide%22">Supercritical carbon dioxide</searchLink><br /><searchLink fieldCode="DE" term="%22Ion+exchange+%28Chemistry%29%22">Ion exchange (Chemistry)</searchLink><br /><searchLink fieldCode="DE" term="%22Coupling+reactions+%28Chemistry%29%22">Coupling reactions (Chemistry)</searchLink><br /><searchLink fieldCode="DE" term="%22Photoreduction%22">Photoreduction</searchLink><br /><searchLink fieldCode="DE" term="%22Photocatalysts%22">Photocatalysts</searchLink><br /><searchLink fieldCode="DE" term="%22Ethylene+synthesis%22">Ethylene synthesis</searchLink>
– Name: Abstract
  Label: Abstract
  Group: Ab
  Data: Photocatalytic reduction of carbon dioxide (CO2) into high-value multicarbon products, such as ethylene (C2H4), remains a significant challenge due to the difficult C-C coupling process. Potassium poly(heptazine imide) (K-PHI) is a promising photocatalyst, yet efficiently exchanging its interlayer cations to tune catalytic selectivity without causing structural degradation is difficult. Herein, an efficient and green supercritical CO2 (SC CO2) assisted ion-exchange strategy was developed to successfully prepare a series of mono-/di-/trivalent cation-doped M-PHI photocatalysts (M = H+, Na+, Sr+, Ca2+, Co2+, Fe3+). Systematic characterizations confirmed that the SC-CO2 treatment successfully achieved in-depth cation substitution without destroying the intrinsic heptazine framework, effectively regulating the interlayer structure and significantly optimizing the photoelectrochemical charge separation. Among the prepared samples, H-PHI exhibited the optimal photocatalytic CO2 reduction performance with an outstanding selectivity toward C2H4 generation. Under simulated sunlight irradiation for 3 h, the yields of CO, CH4, and C2H4 C2H4 C2H4 reached 3564.87, 807.32, and 40.00 μmol·g−1, respectively, significantly outperforming pristine K-PHI and other metal-doped samples. Crucially, isotope-tracing experiments utilizing a SC CO2-DCl treatment detected deuterated CH4 and C2H4 products, providing direct evidence that the hydrogen in the carbon products originates from the introduced protons, thereby elucidating the precise reaction pathway for C-C coupling. This study provides a green and efficient supercritical CO2 ion exchange strategy for the cation engineering of crystalline carbon nitride, and also offers new ideas and methods for designing high-activity photocatalysts for photocatalytic CO2 reduction. [ABSTRACT FROM AUTHOR]
– Name: AbstractSuppliedCopyright
  Label:
  Group: Ab
  Data: <i>Copyright of Nanomaterials (2079-4991) is the property of MDPI and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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        Value: 10.3390/nano16080489
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      – Code: eng
        Text: English
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        PageCount: 13
        StartPage: 489
    Subjects:
      – SubjectFull: Supercritical carbon dioxide
        Type: general
      – SubjectFull: Ion exchange (Chemistry)
        Type: general
      – SubjectFull: Coupling reactions (Chemistry)
        Type: general
      – SubjectFull: Photoreduction
        Type: general
      – SubjectFull: Photocatalysts
        Type: general
      – SubjectFull: Ethylene synthesis
        Type: general
    Titles:
      – TitleFull: Green Supercritical CO 2 Ion-Exchange Strategy for Cation Engineering in Polyheptazine Imides Towards Efficient Photoreduction CO 2 to C 2 H 4.
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            NameFull: Peng, Xin
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            NameFull: Du, Lina
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            NameFull: Fu, Gaoliang
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            NameFull: Zhang, Shouren
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            NameFull: Ma, Junying
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              M: 04
              Text: Apr2026
              Type: published
              Y: 2026
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