Abstract
Interaction of 3-aminopropyltriethoxysilane RNH 2 [R = (EtO) 3 SiCH 2 CH 2 CH 2 ] with triphenylphosphate (PhO) 3 P=O proceeds at temperature 180–200 о С and leads to formation of quaternary ammonium salt of phenylphosphoric acid [PhOP(O)O 2 ] 2- [PhH 2 NR] 2+ , which turns into liquid silicon-containing oligoamidophosphates RNH[P(O)(OPh)NR] n P(O)(OPh)NHR and phenol at high temperature. The latter transesterifies the original 3-aminopropyltriethoxysilane and the obtained products. With the use of high-temperature vacuum rectification liquid oligomers and the solid cross-linked polymer have been isolated. Heating of the solid polymer up to 1000 о С in inert atmosphere results in the amorphous phase, containing SiO 2 and NPO. The reactions of 3-aminopropyltriethoxysilane with triphenylphosphate and trimethylphosphate have been compared.
Highlights
Molecules of triethoxysilylpropylamidophosphates (EtO)3SiCH2CH2CH2NRP(O)X2 (R = H, All; X = OR, NR2) contain the hydrolyzed group (EtO)3Si and the amidophosphate fragment NRP(O)X2, which can form coordination compounds with d- and f-elements
Ability of sol-gel polymerization and forming coordination compounds offers a way to obtain metal-containing gels, films [1], transparent glasses [2] on their basis. Target syntheses of such compounds are based on the reaction of 3-aminoprolyltriethoxysilane (EtO)3SiCH2CH2CH2NН2 (APTES) with the derivatives of phosphorous oxychloride ClP(O)X2 (X = OPh, NR2)
The alternative way of synthesis involves the reaction of two industrial products: APTES and triorganophosphates (RO)3P=O, which can lead to substitution of RO groups at the phosphorus atom and production of alcohol
Summary
Voluminous precipitates of triethylamine or pyridine hydrochlorides, produced in this reaction, badly thicken the reaction mixtures and demand great amounts of solvents, which need to be carefully dewatered, as the initial compounds and the products are hydrolytically unstable In this context finding a more convenient method of obtaining alkoxysilyl derivatives of amidophosphates seems an urgent problem. APTES was analyzed on the gas chromatograph "Tsvet-530" in the stainless steel column 0.3 200 cm, filled by solid support Chromaton-N-AW-DMCS with 5 % liquid phase XC–2–1; thermal conductivity detector; helium as the carrier gas; temperature of the column thermostat 160 °С, temperature of the detector and vaporizer thermostat 220 °С. APTES and TPP in molar ratio 1:1, 2:1 or 3:1 (Table 1) were placed at room temperature into a round-bottom flask with a stirrer and a reflux condenser
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