The polycondensation of Ti(O‐i‐C3H7)4 (1) and Ti(O‐n‐C4H9)4 (2), precursors widely employed in sol‐gel processes, has been investigated by electrospray ionization mass spectrometry. By analysis of 10−6 M methanol solutions of compounds 1 and 2, the same ionic species are detected, proving that the first step in the polycondensation reaction is the i‐propyl (or n‐butyl) alcohol‐methanol complete exchange. This reaction leads to the Ti(OCH3)4 (3) species, representing the synthon of the polycondensation. Various oligomers of 3 have been detected and characterized by MS/MS experiments, and the related mechanisms have been discussed. A minor oligomeric series due to hydroxyl‐containing polycondensation products has also been characterized. Copyright © 2000 John Wiley & Sons, Ltd.
Electrospray ionization in the study of the polycondensation of Ti(O-i-C3H7)4 and Ti(O-n-C4H9)4
Armelao L;GROSS, SILVIA;
2000
Abstract
The polycondensation of Ti(O‐i‐C3H7)4 (1) and Ti(O‐n‐C4H9)4 (2), precursors widely employed in sol‐gel processes, has been investigated by electrospray ionization mass spectrometry. By analysis of 10−6 M methanol solutions of compounds 1 and 2, the same ionic species are detected, proving that the first step in the polycondensation reaction is the i‐propyl (or n‐butyl) alcohol‐methanol complete exchange. This reaction leads to the Ti(OCH3)4 (3) species, representing the synthon of the polycondensation. Various oligomers of 3 have been detected and characterized by MS/MS experiments, and the related mechanisms have been discussed. A minor oligomeric series due to hydroxyl‐containing polycondensation products has also been characterized. Copyright © 2000 John Wiley & Sons, Ltd.
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