Formation of Hierarchically Porous Metal Oxide and Metal Monoliths by Nanocasting into Silica Monoliths

Smått, Jan‐Henrik; Sayler, Franchessa M.; Grano, Amy J.; Bakker, Martin G.

doi:10.1002/adem.201100355

Cited by 35 publications

(12 citation statements)

References 87 publications

(119 reference statements)

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“…The SiO2 template monoliths were synthesized according to the procedure described by Smått et al [8]. In summary: polyethylene glycol (PEG, MW = 35,000 g/mol), 30% v/v HNO3, tetraethyl orthosilicate (TEOS) and octadecyltrimethylammonium bromide (C18TAB) were mixed with molar ratios of 5.5 × 10 −4 :2.5 × 10 −1 :14.5:1:0.12, respectively.…”

Section: Synthesis Of the Sio2 Monolith Templatementioning

confidence: 99%

“…When fabricated as monoliths, i.e., as single pieces, they are particularly attractive as continuous flow microreactors, providing superior mass diffusion and increasing the accessibility of the fluids (reactants and products) during organic transformations [4]. A wide variety of hierarchically porous monoliths [5], such as hierarchically porous zeolites (SiO2/Al2O3, aluminophosphate (AlPO), silico-aluminophosphate SAPO) [6], hierarchically porous metal oxides (SiO2 [7][8][9][10], Co3O4 [8][9][10], NiO [8][9][10], ZnO [11], TiO2 [12]) and hierarchically porous carbon-based catalysts [13,14], have been studied.…”

Section: Introductionmentioning

confidence: 99%

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Ag/SiO2- and Ag/Co3O4-Based Monolithic Flow Microreactors for Hydrogenation of Dyes: Their Activity and Stability

2015

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Silver nanoparticles supported on hierarchically porous silica and cobalt oxide monoliths have previously been shown to be catalytically active for the hydrogenation of common organic dyes in batch studies. This work presents a detailed investigation of the activity and stability of these monoliths during the hydrogenation of eosin-Y in a continuous flow microreactor. The silver-containing monoliths showed excellent catalytic activity that reached a plateau after a period of approximately 6 h. From SEM particle size distribution studies of the catalysts before and after water and hexane were flowed through them, it was determined that under reaction conditions, silver was removed both by washing off of particles and by dissolution of silver.

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Section: Synthesis Of the Sio2 Monolith Templatementioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Ag/SiO2- and Ag/Co3O4-Based Monolithic Flow Microreactors for Hydrogenation of Dyes: Their Activity and Stability

2015

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“…The Wet Impregnation (WI) method of a metal salt on a ceramic surface is one of the procedures that allows for the direct incorporation of metal nanoparticles on ceramic supports. Although different examples of impregnation of amorphous ceramic surfaces with metal salts have been reported, the efficient WI of palladium on micro/mesoporous sintered silica monoliths and their catalytic evaluation in metal catalyzed cross‐coupling reactions via solution phase chemistry has not been addressed yet.…”

Section: Introductionmentioning

confidence: 99%

Integrating Reactors and Catalysts through Three‐Dimensional Printing: Efficiency and Reusability of an Impregnated Palladium on Silica Monolith in Sonogashira and Suzuki Reactions

et al. 2020

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For this work, an integrated system composed of a polypropylene reactor and a palladium on silica monolithic catalyst was designed and manufactured by 3D‐printing. These devices are able to perform solution phase chemistry in a robotic orbital shaker. The capped reactor was obtained in its entirety by 3D‐printing, using polypropylene and fused deposition modeling. The monolithic catalyst was also obtained by 3D‐printing ‐robocasting‐ of a silica support, sintering and subsequent palladium deposition through the wet impregnation method. The catalytic efficiency in Sonogashira or Suzuki reactions as well as the recyclability of the entire system – catalyst+reactor – were studied. The strong electrostatic adsorption (SEA) of the palladium on sintered silica and the reduced mechanical stress produced by the convenient adjustment of the catalyst into the polypropylene reactor makes the catalytic system reusable without significant loss of catalytic activity.

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“…Various synthetic methods have been developed to synthesize MMOs. One promising route is nanocasting method, which depends on the usage of mesoporous silica, mesoporous carbon, or polymer as hard templates to provide the desired mesoporous structure and subsequent removal of templates by etching or calcination to finally obtain MMOs. However, the application of this method suffers from some limitations, for instance, the mesoporous characteristics of such oxides are completely relied on the framework of hard templates.…”

Section: Introductionmentioning

confidence: 99%

A Polymer‐Oriented Self‐Assembly Strategy toward Mesoporous Metal Oxides with Ultrahigh Surface Areas

Xiong

Gao

et al. 2019

Advanced Science

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Mesoporous metal oxides (MMOs) have attracted comprehensive attention in many fields, including energy storage, catalysis, and separation. Current synthesis of MMOs mainly involve use of surfactants as templates to generate mesopores and organic reagents as solvents to hinder hydrolysis and condensation of inorganic precursors, which is adverse to adjusting the interactions between surfactants and inorganic precursors. The resulting products have uncontrollable pore structure, crystallinity, and relatively lower surface areas. Here, a facile and general polymer‐oriented self‐assembly strategy to synthesize a series of MMOs (e.g., TiO 2 , ZrO 2 , NbO 5 , Al 2 O 3 , Ta 2 O 5 , HfO 2 , and SnO 2 ) by using cationic polymers as porogens and metal alkoxides as metal oxide precursors in a robust aqueous synthesis system are reported. Nitrogen adsorption analysis and transmission electron microscopy confirm that the obtained MMOs have ultrahigh specific surface areas and large pore volumes (i.e., 733 m 2 g −1 and 0.485 cm 3 g −1 for mesoporous TiO 2 ). Moreover, the structural parameters (surface area, pore size, and pore volume) and crystallinity can be readily controlled by tuning the interactions between cationic polymers and precursors. The as‐synthesized crystalline mesoporous TiO 2 exhibits promising performance in photocatalytic water splitting of hydrogen production and a high hydrogen production rate of 3.68 mol h −1 g −1 .

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Formation of Hierarchically Porous Metal Oxide and Metal Monoliths by Nanocasting into Silica Monoliths

Cited by 35 publications

References 87 publications

Ag/SiO2- and Ag/Co3O4-Based Monolithic Flow Microreactors for Hydrogenation of Dyes: Their Activity and Stability

Ag/SiO2- and Ag/Co3O4-Based Monolithic Flow Microreactors for Hydrogenation of Dyes: Their Activity and Stability

Integrating Reactors and Catalysts through Three‐Dimensional Printing: Efficiency and Reusability of an Impregnated Palladium on Silica Monolith in Sonogashira and Suzuki Reactions

A Polymer‐Oriented Self‐Assembly Strategy toward Mesoporous Metal Oxides with Ultrahigh Surface Areas

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