主权项 |
1. A method for preparing silica modified by a silane coupling agent, comprising:
(a) adding water to an organic solvent; (b) adjusting pH value of the mixture of step (a) to either below 6 by adding an acid or over 8 by an alkali; (c) adding the coupling agent to the mixture of step (b), wherein the molar ratio of the coupling agent to water is in the range of 1:0.1-1:10000; (d) letting the mixture of step (c) stand for 0.5-48 h, whereby a stabilized sol solution of the coupling agent is formed; (e) adding silica to the sol solution to produce precipitated silica in an amount less than 10 g/ml and fumed silica in an amount less than 1 g/ml, g/ml being a mass to volume ratio of the silica to the so solution; (f) dispersing the silica fully into the sol solution to make a uniformly-dispersed turbid solution by one of the following dispersing methods:
(1) performing 1-100 ultrasonic dispersion processes on the mixture of step (e) for a total of over 1 h under an ultrasonic frequency of over 20 kHz to produce a turbid solution, wherein each ultrasonic dispersion process lasts 10 min-1 h, and wherein the temperature of the turbid solution is lowered to room temperature by stirring the turbid solution between two ultrasonic dispersion processes,(2) performing 1-100 shearing dispersion processes on the mixture of step (e) at a shearing rate of over 1000 r/min using a shear blender to produce a turbid solution, wherein each shearing dispersion process lasts 10 min-10 h, and wherein the temperature of the turbid solution is lowered to room temperature by stirring the turbid solution between two shearing dispersion processes, or(3) stirring the mixture of step (e) at a stirring rate of greater than 300 r/min for 0.5-168 h to produce a turbid solution; (g) stirring and evaporating the uniformly-dispersed turbid solution at room temperature to produce a mixture having a weight that is 0.1%-50% of the weight of the turbid solution of step (f); (h) heating a stirring the mixture of step (g) at 50-80° C. for 0.5-120 h and then at 81-260° C. for 0.5-48 h; and (i) drying and crushing the mixture of step (h), wherein each of steps (a)-(g) and (l) is carried out, at a temperature less than 50° C., whereby, silica modified by the coupling agent is obtained. |