Abstract
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 ((C2H4)(Me2SiCl)2) and 1, 4-bis(chlorodimethylsilyl)benzene ((C6H4)(Me2SiCl)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 (C6H4)(Me2SiCl)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.
Highlights
Organic-inorganic hybrid materials have attracted attention because of the unique properties derived from both organic and inorganic moieties
We have reported silicate-phosphate and silicate-phosphite alternating copolymers (–(O–P–O–Si)n ) by a direct reaction of phosphoric acid and organically modified chlorosilane [9,10,11,12]
The silicophosphate hybrid oligomers were synthesized by a nonaqueous acid-base reaction between phosphoric acid and organo-bridged bis(chlorosilane) ((C2 H4 )(Me2 SiCl)2 or (C6 H4 )(Me2 SiCl)2 )
Summary
Organic-inorganic hybrid materials have attracted attention because of the unique properties derived from both organic and inorganic moieties. The properties of the hybrid materials are mostly determined by the chemistry of the organic and inorganic components, their arrangements, and the microstructures [1,2]. These hybrid materials are widely synthesized via an alkoxide-derived sol-gel method because the low temperature process prevents the decomposition of the organic component [3,4,5]. Molecules 2020, 25, 127 and inorganic components is hardly controllable by the alkoxide-derived sol-gel method because the hydrolysis and condensation reactions of inorganic moieties of organically modified alkoxides take place competitively, which results in different nucleation-growth processes. The network formation process involved a nonaqueous acid-base reaction as follows: P–OH + Si–Cl → P–O–Si
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