Ph. Bolt et al., A SMALL-ANGLE X-RAY-SCATTERING STUDY ON HIGH PH SILICA PRECIPITATIONS, Colloids and surfaces. A, Physicochemical and engineering aspects, 122(1-3), 1997, pp. 183-187
Silica precipitations were carried out at high pH (7-10) and elevated
temperatures (60-90 degrees C) by means of simultaneous dosing of dilu
ted water glass and sulphuric acid into a stirred thermostatted reacti
on vessel. In order to investigate the development of the vulnerable s
ilica structures during the processes, every 5-10 min small samples we
re taken from the reaction mixture and analysed using small angle X-ra
y scattering. It was found that a narrow particle size distribution wa
s maintained throughout the entire preparation procedure (or at least
from about 1 h until the end of the process), despite the fact that th
e primary silica particles were growing continuously. In addition, a c
ontinuous decrease in the total number of primary particles was observ
ed, indicating that the primary particles were involved in clustering
and aging processes, and that (except for the initial reaction stages)
newly dosed silica does not form new particles but is deposited onto
the already existing particles. Ostwald ripening, which is regarded as
the most important aging mechanism, probably proceeds relatively rapi
dly under the applied process conditions, leading to a persistent high
degree of monodispersity.