Silicophosphates containing SiO<sub>6</sub>octahedra – anhydrous synthesis under ambient conditions

Jähnigen, Sandra; Brendler, Erica; Böhme, Uwe; Heide, G.; Kroke, Edwin

doi:10.1039/c3nj00721a

Cited by 25 publications

(25 citation statements)

References 46 publications

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“…Several other examples should also be mentioned in this context. Silicophosphates were prepared from anhydrous phosphoric acid and tetraalkoxysilanes by Jähningen et al [197,198] and Tokuda et al [199]. Hybrid silicophosphates with various organic groups were prepared by solventless condensations of anhydrous phosphoric acid with alkyl-and arylchlorosilanes by the Takahashi group [200][201][202][203].…”

Section: New Compositionsmentioning

confidence: 99%

The Power of Non-Hydrolytic Sol-Gel Chemistry: A Review

et al. 2017

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This review is devoted to non-hydrolytic sol-gel chemistry. During the last 25 years, non-hydrolytic sol-gel (NHSG) techniques were found to be attractive and versatile methods for the preparation of oxide materials. Compared to conventional hydrolytic approaches, the NHSG route allows reaction control at the atomic scale resulting in homogeneous and well defined products. Due to these features and the ability to design specific materials, the products of NHSG reactions have been used in many fields of application. The aim of this review is to present an overview of NHSG research in recent years with an emphasis on the syntheses of mixed oxides, silicates and phosphates. The first part of the review highlights well known condensation reactions with some deeper insights into their mechanism and also presents novel condensation reactions established in NHSG chemistry in recent years. In the second section we discuss porosity control and novel compositions of selected materials. In the last part, the applications of NHSG derived materials as heterogeneous catalysts and supports, luminescent materials and electrode materials in Li-ion batteries are described.

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Section: New Compositionsmentioning

confidence: 99%

The Power of Non-Hydrolytic Sol-Gel Chemistry: A Review

et al. 2017

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“…It was expected that both catalysts used would be observable through two clear absorption bands; one band at 1650 cm −1 , noted for hydrated phosphates POH and corresponding to OH stretching and OH deformation vibrations and second band between 1300 and 900 cm −1 that is characteristic of PO and CO vibrations . In this reaction, these absorption bands cannot be independently isolated as both bands coincide with the phenolic resin bands at 1594 cm −1 , corresponding to the absorption of CC of phenyl rings, and bands 1100 cm −1 , which are the characteristic of the CH flexural of phenyl rings.…”

Section: Resultsmentioning

confidence: 97%

Optimizing size and distribution of voids in phenolic resins through the choice of catalyst types

Hamad

Farr

Teng

et al. 2019

J of Applied Polymer Sci

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Phenolics are widely used for over a century in different industries due to their chemical resistance and thermomechanical properties. However, the presence of voids in phenolic resins has negative effects on the mechanical properties and a conventional approach is to avoid these by utilizing very long cure cycles. Our alternative approach investigates the tailoring of void size and distribution to achieve a better balance between processing time and mechanical properties. Therefore, we produced phenolic resin with a void-free microstructure by a long cure cycle as a reference. To alter the void size and distributions, we utilized different catalysts and a short cure cycle to obtain phenolic resins and test their flexural properties with respect to the reference. We investigated the fracture surfaces of all materials by SEM, FTIR and compared results to finite element modeling that confirmed the effects of different void size and distributions on the mechanical properties.

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“…In the present study, different types of silicophosphate oligomers with different network structures (such as cyclic and cage oligomers) and terminal groups (P-OH and/or Si-Cl) were prepared by changing the reaction temperature and molar ratio of the precursors. Although various types of molecular silicophosphates, such as cyclic and cage oligomers, have been reported so far [22][23][24][25][26], this is the first report on the synthesis of silicophosphates oligomers which contain organic moieties in inorganic main chains. The organic moieties incorporated in the inorganic chains of silicophosphates can increase the surface area as reported in silicophosphate xerogels prepared from bridged acetoxysilanes and phosphoryl reagents [27].…”

Section: Silicophosphate Hybrid Network Formation From Phosphoric Acimentioning

confidence: 91%

Preparation of Silicophosphate Alternating Hybrid Copolymers via Nonaqueous Acid-Base Reactions of Phosphoric Acid and Organo-Bridged Bis(chlorosilane)

et al. 2019

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A design of atomic and oligomer level structure in organic-inorganic hybrid materials is highly important for various applications. Nonaqueous acid-base reaction allows us to prepare silicophosphates with controlled inorganic networks (-(O-P-O-Si) n ) at atomic level because phosphorous and silicon-based precursors can react directly, resulting in an alternating copolymer network. Organic functionalization in those materials has been realized so far by using organic-modified phosphorous acid and/or organo-chlorosilane as precursors.In the present study, silicophosphate oligomers exhibiting inorganic-organic hybrid chains of (-(O-P-O-Si-R-Si) n ) (R: bridging organic functional groups), are prepared from phosphoric acid and organo-bridged bis(chlorosilane). The 1, 2-bis(chlorodimethylsilyl)ethane ((C 2 H 4 )(Me 2 SiCl) 2 ) and 1, 4-bis(chlorodimethylsilyl)benzene ((C 6 H 4 )(Me 2 SiCl) 2 ) were used as organo-bridged bis(chlorosilane). Different types of silicophosphate oligomers with different network structures and terminal groups (P-OH and/or Si-Cl) were prepared by changing the reaction temperature and molar ratio of precursors. The formation of low molecular weight oligomers of ring and cage morphologies (ring tetramer, cage pentamer, and ring hexamer) is suggested in the product prepared from phosphoric acid and (C 6 H 4 )(Me 2 SiCl) 2 molecule at 150 • C. Those silicophosphate hybrid oligomers are expected to be used as building blocks of hybrid materials with well-defined network structures for desired functionalities.

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Silicophosphates containing SiO₆octahedra – anhydrous synthesis under ambient conditions

Cited by 25 publications

References 46 publications

The Power of Non-Hydrolytic Sol-Gel Chemistry: A Review

The Power of Non-Hydrolytic Sol-Gel Chemistry: A Review

Optimizing size and distribution of voids in phenolic resins through the choice of catalyst types

Preparation of Silicophosphate Alternating Hybrid Copolymers via Nonaqueous Acid-Base Reactions of Phosphoric Acid and Organo-Bridged Bis(chlorosilane)

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Silicophosphates containing SiO6octahedra – anhydrous synthesis under ambient conditions

Cited by 25 publications

References 46 publications

The Power of Non-Hydrolytic Sol-Gel Chemistry: A Review

The Power of Non-Hydrolytic Sol-Gel Chemistry: A Review

Optimizing size and distribution of voids in phenolic resins through the choice of catalyst types

Preparation of Silicophosphate Alternating Hybrid Copolymers via Nonaqueous Acid-Base Reactions of Phosphoric Acid and Organo-Bridged Bis(chlorosilane)

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Silicophosphates containing SiO₆octahedra – anhydrous synthesis under ambient conditions