Contribution to the study of the formation mechanism of ordered porous carbons from a soft-template method using the copolymer triblock (PEO140PPO39PEO140) and a phenolic resin

Abstract

Diferentes carbonos porosos foram sintetizados empregando automontagem direta de um surfactante non-iônico (PEO 140 PPO 39 PEO 140 (Pluronic ® ), PEO poli(óxido de etileno) e PPO poli(óxido de propileno)) e uma resina fenólica. Segundo experimentos de espalhamento de luz dinâmico (DLS) realizados antes da floculação, a formação de micelas híbridas cobertas (precursores de materiais mesoporosos ordenados) compete com a formação de partículas resol dependendo da concentração do surfactante. Elevada temperatura de síntese aumenta a formação de mesoporosidade. Quando monômeros (ao invés de oligômeros) são usados como precursores de resina, a mesoporosidade também é aumentada. Porém neste caso, a formação de partículas resol também é favorecida. Os materiais obtidos são principalmente microporosos, indicando que polímeros/micelas híbridas surfactantes não são estáveis o suficiente para modelar a formação de carbonos altamente mesoporosos. A interação apropriada entre micelas surfactantes e espécies precursoras de resinas, assim como o grau de polimerização da resina, é crucial para a obtenção de polímeros/micelas híbridas surfactantes que conduzam à formação de carbonos mesoporosos.Different porous carbons were synthesized using direct self-assembly of a nonionic surfactant (PEO 140 PPO 39 PEO 140 , PEO poly(ethylene oxide) and PPO poly(propylene oxide)) and a phenolic resin. According to dynamic light scattering (DLS) experiments realized before the flocculation, the formation of covered hybrid micelles (precursors of ordered mesoporous materials) competes with the formation of resol particles depending on the surfactant concentration. High synthesis temperature increases the formation of mesoporosity. When monomers (instead of oligomers) are used as resin precursors, the mesoporosity is also enhanced. However in this case, the formation of resol particles is also favored. The obtained materials are mainly microporous, indicating that the formed polymer/surfactant hybrid micelles are not stable enough to template the formation of highly mesoporous carbons. Appropriate interaction between the surfactant micelles and resin precursor species, as well as the polymerization degree of the resin, is crucial for obtaining polymer/ surfactant hybrid micelles that conduce to mesoporous carbons.

Synthesis of Highly Uniform N-Doped Porous Carbon Spheres Derived from Their Phenolic-Resin-Based Analogues for High Performance Supercapacitors

“…The peak at 1370 cm –1 is ascribed to the phenol O–H in-plane stretching band. The bands at 1266 and 1014 cm –1 represent an asymmetric stretch of phenolic C–C–OH and stretching vibration of aliphatic C–OH bonded with bis-tris, respectively. , The peak at 1144 cm –1 is due to a C–O stretching band. Furthermore, the peak at 1224 cm –1 is assigned to the stretching vibration of C–N (ternary amine) in bis-tris, which also confirms the presence of bis-tris in the sample of PS-CTAB.…”

Catalyst-free soft-template synthesis of ordered mesoporous carbon tailored using phloroglucinol/glyoxylic acid environmentally friendly precursors

“…33,41 At the same time the band between 2800 and 3000 cm −1 can also corres-pond to the stretching of the CH saturated bonds of the resin bridges. 42 Three other peaks are observed between 1900 and 1500 cm −1 . The absorption peaks at 1828 cm −1 and 1732 cm −1 are due to the CvO groups in cyclic lactones or anhydrides.…”

“…44,45 The peak from 1045 cm −1 belongs to the single bond C-O stretching vibration of resin ester or lactone bridges. 42 The peaks shown in the interval range 600-900 cm −1 are characteristic of the number of adjacent hydrogen atoms on the aromatic ring, due to the C-H vibrations out of the plane of the aromatic ring. The peak from 953 cm −1 is specific to aromatic vC-H out-of-plane deformation vibrations in the 1,2,3 trisubstituted benzene ring.…”

Hypercrosslinked Phenolic Polymers with Well‐Developed Mesoporous Frameworks

“…Thes uccessful cross-linking of aromatic 1,4-bis(chloromethyl)benzene in the polymeric matrix as molecular bridges enhances the absorbance at 1505 cm À1 ,which originates from C=Cg roups in the aromatic rings. [15] ForN MR characterization (Figure S3), the broad bands should be categorized as two carbon species,t hat is,t he aliphatic carbons assigned to methylene bridges (10-50 ppm) and the aromatic carbons contained in the phenyl rings (90-160 ppm), again indicating awell-preserved PR networks. [8b] Compared with pristine PR, the evident quenching of the CÀHs tretch from the F127 triblock copolymer at 2900 cm À1 is another indicator of the successful removal of the templates in Meso-PR-36.…”