Synthesis of spirosilicates directly from silica and ethylene glycol/ethylene glycol derivatives
作者:Varangkana Jitchum、Sun Chivin、Sujitra Wongkasemjit、Hatsuo Ishida
DOI:10.1016/s0040-4020(01)00275-7
日期:2001.4
Tetracoordinated spirosilicates have been synthesized directly from the reaction of a very inexpensive and plentiful material, SiO2, and ethylene glycol in the presence of triethylenetetramine (TETA), as catalyst with and without potassium hydroxide as co-catalyst. The reactions are run under nitrogen gas with constant stirring at 200 degreesC, and complete in a reaction time of 10-18 h depending on the catalysts. The reactions using only TETA are complete in 18 h, while with potassium hydroxide the reactions occur much more quickly. When 3-amino-1,2-propanediol, or 2-amino-2-methyl-1,3-propanediol is employed, the reaction must run under vacuum at 0.1mmHg, 160 degreesC, and is complete in 14 and 24 h, respectively. The structures of spirosilicates are fully characterized using FTIR, H-1, C-13, Si-29 NMR, FAB(+)-MS, and TGA. (C) 2001 Elsevier Science Ltd. All rights reserved.