A process for the prepn. of silicon and aluminum N,N-dialkylcarbamates, Si(O2CNR2)4 (R = Et, CHMe2) and Al[O2CN(CHMe2)2]3 resp., comprises treatment of SiCl4 or AlBr3 with secondary amine and CO2 in anhyd. toluene. Hydrolyzing the N,N-dialkylcarbamate was achieved by adding H2O at temp. of from 15 to 40 in an org. solvent, i.e., THF. For example, stirring SiCl4 and HN(CHMe2)2 in PhMe under CO2 at atm. pressure for 12 h, filtration of insol. HN(CHMe2)2.HCl, and evapn. gave Si[O2CN(CHMe2)2]4. Hydrolysis of this in aq. THF gave a solid with Si content 8.8% (81% yield vs. SiCl4), which upon thermogravimetric anal. showed most wt. loss substantially below 100, being complete at 600 in air. The resulting SiO2-contg. product had surface area 700 m2/g.

Silicon and aluminum N,N-dialkylcarbamates and their hydrolysis products and process for their preparation

BELLI, DANIELA;CALDERAZZO, FAUSTO;
1993

Abstract

A process for the prepn. of silicon and aluminum N,N-dialkylcarbamates, Si(O2CNR2)4 (R = Et, CHMe2) and Al[O2CN(CHMe2)2]3 resp., comprises treatment of SiCl4 or AlBr3 with secondary amine and CO2 in anhyd. toluene. Hydrolyzing the N,N-dialkylcarbamate was achieved by adding H2O at temp. of from 15 to 40 in an org. solvent, i.e., THF. For example, stirring SiCl4 and HN(CHMe2)2 in PhMe under CO2 at atm. pressure for 12 h, filtration of insol. HN(CHMe2)2.HCl, and evapn. gave Si[O2CN(CHMe2)2]4. Hydrolysis of this in aq. THF gave a solid with Si content 8.8% (81% yield vs. SiCl4), which upon thermogravimetric anal. showed most wt. loss substantially below 100, being complete at 600 in air. The resulting SiO2-contg. product had surface area 700 m2/g.
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Utilizza questo identificativo per citare o creare un link a questo documento: http://hdl.handle.net/11568/22940
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