One-pot strategy for synthesis of open-cage silsesquioxane monomers

Katoh, Ryoichi; Imoto, Hiroaki; Naka, Kensuke

doi:10.1039/c9py00036d

Cited by 30 publications

(22 citation statements)

References 57 publications

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“…−68 ppm for T type Si atoms (see Supplementary Materials, Figure S1b). It is in accordance with the data of compounds described by Naka et al [11]. Additionally, the important aspect of the synthetic procedure to ensure effective product formation was the proper cooling of the reaction mixture in an ice bath and the sequence of chlorosilane and amine addition.…”

Section: Resultssupporting

confidence: 89%

“…On the other hand, open-cage silsesquioxanes, i.e., not-completely condensed systems have recently attracted much attention. The silsesquioxane trisilanol precursors enable the introduction of three reactive substituents to the Si-O-Si core by means of stoichiometric (hydrolytic condensation), but also catalytic (e.g., hydrosilylation, arylation, O-silylation), processes using functional groups that are already attached to the SQ core [8][9][10][11][12][13][14][15][16]. The symmetry of their trifunctional T 7 open-cage derivatives is changed due to the lack of one vertex in the structure, which affects their physical properties (i.e., changes in molecular packing, melting points) [9,[17][18][19][20].…”

Section: Introductionmentioning

confidence: 99%

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Preparation of Tri(alkenyl)functional Open-Cage Silsesquioxanes as Specific Polymer Modifiers

et al. 2020

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The scientific reports on polyhedral oligomeric silsesquioxanes are mostly focused on the formation of completely condensed T8 cubic type structures and recently so-called double-decker derivatives. Herein, we report on efficient synthetic routes leading to trifunctionalized, open-cage silsesquioxanes with alkenyl groups of varying chain lengths from -vinyl to -dec-9-enyl and two types of inert groups (iBu, Ph) at the silsesquioxane core. The presented methodology was focused on hydrolytic condensation reaction and it enabled obtaining titled compounds with high yields and purity. A parallel synthetic methodology that was based on the hydrosilylation reaction was also studied. Additionally, a thorough characterization of the obtained compounds was performed, also in terms of their thermal stability, melting and crystallization temperatures (TGA and DSC) in order to show the changes in the abovementioned parameters dependent on the type of reactive as well as inert groups at Si-O-Si core. The presence of unsaturated alkenyl groups has a profound impact on the application potential of these systems, i.e., as modifiers or comonomers for copolymerization reaction.

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Section: Resultssupporting

confidence: 89%

Section: Introductionmentioning

confidence: 99%

Preparation of Tri(alkenyl)functional Open-Cage Silsesquioxanes as Specific Polymer Modifiers

et al. 2020

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“…The EP-POSS resin was home-made in the laboratory; it was prepared by a condensation reaction with isopropanol (IPA), 5% tetramethylammonium hydroxide (TMAH) aqueous solution and γ-(2,3-glycidoxy) propyltrimethoxysilane (KH560), the specific preparation method is referred to in previous research [ 23 ]. The molecular structure of POSS is shown in Figure 1 .…”

Section: Methodsmentioning

confidence: 99%

The Effect of Graphene Nanofiller on the Surface Structure and Performance of Epoxy Resin–Polyhedral Oligomeric Silsesquioxane (EP-POSS)

Fang

Wang

Sun³

et al. 2021

Nanomaterials

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Epoxy resin–polyhedral oligomeric silsesquioxane (EP-POSS) has excellent mechanical properties and hydrophobic properties. In order to adapt for application in sensor and photovoltaic fields, graphene, nano-SiO2 and nano-ZnO were used to modify EP-POSS. FTIR was used to characterize changes on the surface structure after introducing nanoparticles. The change of hydrophobicity was measured using a contact angle test. TEM test results showed that nanoparticles were successfully inserted between the graphene sheets. However, the content of Si on the surface was low, as the cage structure of POSS in the molecular chain was coated by epoxy groups. XRD tests indicated that nanoparticles facilitated the dispersion of graphene in EP-POSS. XPS characterized the chemical state and content of the elements, confirming that the addition of graphene can induce the enrichment of Si on the surface of EP-POSS, which had a shielding effect on the main chain and improved the hydrophobicity. Wear resistance and adhesion tests showed that, after the introduction of nanoparticles, the EP-POSS coating film met the requirements of graphene materials.

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“…[21][22][23] T7 can undergo corner-capping reaction with equal amount of R 0 SiX 3 which offers target functional groups, and finally generate mono-functional POSS. [24][25][26] This synthesis method ( Figure 3) has been widely used in the preparation of mono-functional POSS molecules. But the synthetic product of this method is mostly a mixture of various derivatives containing silicon hydroxyl groups, as well as diverse by-products, so it is difficult to separate and purify T7.…”

Section: Corner-capping Reactionmentioning

confidence: 99%

Biomass/polyhedral oligomeric silsesquioxane nanocomposites: Advances in preparation strategies and performances

Wang

Zhang

et al. 2020

J of Applied Polymer Sci

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Polyhedral oligomeric silsesquioxane (POSS) as an organic–inorganic hybrid at a molecular level, has excellent mechanical properties, thermodynamic properties, dielectric properties and so on. In recent decades, POSS has been extensively used in modification of various polymers to prepare nanocomposites with enhanced comprehensive performances. Biomass materials such as chitosan, cellulose, silk protein, collagen fibers and gelatin have excellent biocompatibility and biodegradability, which have been widely used in the fields such as biomedical, innovative environmental protection and so on. However, deficiencies including insufficient mechanical properties and rapid rate of biodegradation hampered their application. This paper briefly introduced the principal methods to synthesize POSS nanoparticles, and then focused on technologies for preparing biomass‐based composites utilizing diverse functional POSSs. Finally, put forward the prospects of POSS modification technology and its future application direction. This article will have a positive guiding role for the further research and development of biomass/POSS nanocomposites.

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One-pot strategy for synthesis of open-cage silsesquioxane monomers

Cited by 30 publications

References 57 publications

Preparation of Tri(alkenyl)functional Open-Cage Silsesquioxanes as Specific Polymer Modifiers

Preparation of Tri(alkenyl)functional Open-Cage Silsesquioxanes as Specific Polymer Modifiers

The Effect of Graphene Nanofiller on the Surface Structure and Performance of Epoxy Resin–Polyhedral Oligomeric Silsesquioxane (EP-POSS)

Biomass/polyhedral oligomeric silsesquioxane nanocomposites: Advances in preparation strategies and performances

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