Nitrogen-containing porous carbon materials by twin polymerization

Schliebe, Christian; Noll, Julian; Scharf, Sebastian; Gemming, Thomas; Seifert, Andreas; Spange, Stefan; Lehmann, Daniel; Zahn, Dietrich R. T.; Fiedler, Benjamin; Friedrich, Joachim; Blaudeck, Thomas; Lang, Heinrich

doi:10.1007/s00396-017-4254-y

Cited by 5 publications

(38 citation statements)

References 79 publications

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“…Solid‐state 13 C{ 1 H} cross‐polarization magic angle spinning NMR measurements confirmed the polymeric structure typical of salicylic alcohol‐based twin polymers [49,51] . SEM/EDX and HAADF‐STEM/EDX studies revealed homogeneously distributed MgO domains within the hybrid materials as characteristic for twin polymerization processes [48,56,65] . The carbonization and calcination behavior of HM_1 and HM_2 was explored by TG and the thus obtained porous magnesium oxides MgO_1 and MgO_2 were analyzed by BET, PXRD, IR, SEM/EDX and TEM studies.…”

Section: Discussionmentioning

confidence: 79%

“…[49,51] SEM/EDX and HAADF-STEM/EDX studies revealed homogeneously distributed MgO domains within the hybrid materials as characteristic for twin polymerization processes. [48,56,65] The carbonization and calcination behavior of HM_1 and HM_2 was explored by TG and the thus obtained porous magnesium oxides MgO_1 and MgO_2 were analyzed by BET, PXRD, IR, SEM/EDX and TEM studies. Their surface area was determined to 400 m 2 g À 1 for MgO_2 and 200 m 2 g À 1 for MgO_1.…”

Section: Discussionmentioning

confidence: 99%

“…[49,52] Carbonization followed by careful oxidation of the organic phase resulted in mainly meso-porous SiO 2 in solid or foam-like textures. [48,49,51] When instead of furfuryl alcohol the respective thiophene or pyrrole derivatives are used, then sulfur-, [53][54][55] or nitrogen-doped [56] carbon materials are obtained. Addition of transition metal carboxylates, such as [Ag(2-OCH 2 -c C 4 H 3 S)(PPh 3 )] [57] or [Co(O 2 CCH 2 (OCH 2 CH 2 ) 3 OMe) 2 ] [58] to the twin monomer led to highly dispersed metal or metal oxide nanoparticle-loaded porous carbon and silica materials, respectively.…”

Section: Introductionmentioning

confidence: 99%

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Porous Magnesium Oxide by Twin Polymerization: From Hybrid Materials to Catalysis

et al. 2023

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Twin monomers [Mg(2‐OCH2‐cC6H4O)][L]0.8 (2, L=diglyme) and [Mg(2‐OCH2‐cC6H4O)][L]0.66 (3, L=tmeda) form by their thermal polymerization interpenetrating organic‐inorganic hybrid materials in a straightforward manner. Carbonization (Ar) followed by calcination gave porous MgO (2: surface area 200 m2 g−1, 3: 400 m2 g−1), which showed in catalytic studies towards Meerwein‐Ponndorf‐Verley reductions excellent yields and complete conversions for cyclohexanone and benzaldehyde. However, with crotonaldehyde a mixture of C4–C8 compounds was obtained. When MgO was exposed to air then primarily crotyl alcohol was formed. The range of applications could be easily extended by twin polymerization of 3 in presence of [Cu(O2CCH2O(CH2CH2O)2Me)2] (4) or [Ag(O2CCH2‐cC4H3S)(PPh3)] (5), resulting in the formation of nanoparticle‐decorated porous CuO@MgO or Ag@MgO materials, which showed high catalytic reactivity towards the reduction of methylene blue.

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Section: Discussionmentioning

confidence: 79%

Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Porous Magnesium Oxide by Twin Polymerization: From Hybrid Materials to Catalysis

et al. 2023

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“…These values are the lowest temperatures observed for thermally-induced TP so far. [100] TG-MS (= Thermogravimetry -Mass Spectrometry) investigations confirmed that at these temperatures a temperature-induced condensation reaction occurred.…”

Section: Figurementioning

confidence: 68%

“…In 2018, our group prepared nitrogen-containing porous carbon materials by applying the TP procedure. [100] In addition, the reaction path of CÀ C and CÀ N linking for 2M and 2M2A models were reported with BP86-D3/SVP and COSMO (ɛ = 2. b).…”

Section: Figurementioning

confidence: 99%

Twin Polymerization: A Unique Strategy towards Versatile Functional Materials

Scharf,

Notz,

Lang

2023

Eur J Inorg Chem

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Twin polymerization (=TP), a non‐aqueous synthetic methodology for the preparation of inorganic‐organic hybrid materials, by using, for example, salicylic‐ or furfurylic‐functionalized main‐group elements and/or transition metal‐based twin monomers, results in the formation of interpenetrating phase (nano)domains in a single step. The chemical, analytical and physical properties including theoretical studies of the (co)polymerization process of the respective twin monomers, polymers and the as‐generated hybrid and composite materials are described. Furthermore, the synthesis of hierarchical materials such as carbon hollow spheres as well as the encapsulation of nanoparticles (=NPs) within them by applying TP is envisaged. TP gives access to a wide range of applications (e. g., coatings for a variety of substrates, textile functionalization, carbon materials for Li−S or redox‐flow batteries) which will be discussed herein. The use of NP‐decorated hybrid and composite materials and nanoparticular MgO as catalysts in heterogeneous catalysis is reported as well.

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Synthesis and Twin Polymerization of Si(OCH₂py)₄ for Nitrogen‐containing Carbon Materials

Scharf,

Notz,

Pfefferkorn

et al. 2024

Eur J Inorg Chem

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The synthesis and twin polymerization (TP) of Si(OCH2py)4 (3 a, py=2‐cC5H4N; 3 b, py=3‐cC5H4N; 3 c, py=4‐cC5H4N) is discussed. The solid state structures of 3 b, c were confirmed by single‐crystal X‐ray crystallography showing non‐conventional H‐bonding, forming 2D chains (3 b) or 3D networks (3 c). Thermally induced TP of 3 a–c and their simultaneous polymerization with 2,2‘‐spiro‐bi[4H‐1,3,2‐benzodioxasiline] (4) is described. The resulting hybrid materials were characterized by 1H, 13C{1H}, and 29Si{1H} CP MAS NMR spectroscopy confirming the transformation of the SiOCH2 moieties into CH2 groups enabling the formation of the respective polymers. These results were supported by HAADF‐STEM studies, displaying micro‐structuring. Nitrogen‐containing porous carbon materials C_1–C_3 show surface areas of 1300 and 1700 m2 g−1, large pore volumes between 0.6–1.2 cm3 g−1, and nitrogen contents of up to 3.1 at‐%. X‐ray photoemission spectroscopy reveal that pyrrolic, pyridine, and pyridone nitrogen atoms are present. If equimolar amounts of 3 a–c and 4 are simultaneously polymerized in the presence of [Pd(OAc)2] (5), then the Pd nanoparticle‐decorated material Pd@C_3 (900 m2 g−1) was obtained, which showed k values of −0.083 and −0.066 min−1 in the reduction of methylene blue and methyl orange, proving the accessibility of the Pd NPs.

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Nitrogen-containing porous carbon materials by twin polymerization

Cited by 5 publications

References 79 publications

Porous Magnesium Oxide by Twin Polymerization: From Hybrid Materials to Catalysis

Porous Magnesium Oxide by Twin Polymerization: From Hybrid Materials to Catalysis

Twin Polymerization: A Unique Strategy towards Versatile Functional Materials

Synthesis and Twin Polymerization of Si(OCH₂py)₄ for Nitrogen‐containing Carbon Materials

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Nitrogen-containing porous carbon materials by twin polymerization

Cited by 5 publications

References 79 publications

Porous Magnesium Oxide by Twin Polymerization: From Hybrid Materials to Catalysis

Porous Magnesium Oxide by Twin Polymerization: From Hybrid Materials to Catalysis

Twin Polymerization: A Unique Strategy towards Versatile Functional Materials

Synthesis and Twin Polymerization of Si(OCH2py)4 for Nitrogen‐containing Carbon Materials

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Synthesis and Twin Polymerization of Si(OCH₂py)₄ for Nitrogen‐containing Carbon Materials