Method of preparing hydrophobic silica
A silica, hydrophobic technology for thin material handling, instrumentation, fibrous fillers, etc.
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Embodiment 1
[0062] To 40 kg of an acidic aqueous dispersion of silica having a pH of about 3 (OMP-1040 from Nissan Chemical) in the reactor was added 27.8 kg of 2-propanol followed by 1.84 kg of octyltriethoxysilane. While heating to 70°C, the resulting mixture was stirred rapidly with an overhead paddle stirrer while circulating through a homogenizer and held for 6 hours. To the reaction mixture was added 3.8 kg of a 3.43% by weight aqueous solution of ammonium hydroxide, and the mixture was stirred at 70° C. for a further 2.5 hours. The reaction mixture was then spray dried at a temperature of 135°C to provide hydrophobic silica particles as a dry powder. The carbon content of the silica particles was 4.28% by weight. The T2 / T3 ratio was 0.48.
Embodiment 2
[0064] To 41 kg of an acidic aqueous dispersion of silica having a pH of about 3 (OYL from Nissan Chemical) in the reactor was added 28.7 kg of 2-propanol followed by 1.87 kg of octyltriethoxysilane. While heating to 68° C., the resulting mixture was stirred rapidly with an overhead paddle stirrer and simultaneously circulated through the homogenizer and maintained this way for 7.5 hours. The reaction mixture was then spray dried at a temperature of 130°C to provide hydrophobic silica particles as a dry powder. The carbon content of the silica particles was 4.8% by weight. The T2 / T3 ratio was 1.45.
Embodiment 3
[0066] To 39 kg of an acidic aqueous dispersion of silica having a pH of about 3 (OYL from Nissan Chemical) in the reactor was added 20.7 kg of deionized water followed by 2.51 kg of hexamethyldisilazane. While heating to 50° C., the resulting mixture was stirred rapidly with an overhead paddle stirrer and simultaneously circulated through the homogenizer and maintained this way for 6 hours. For another purpose, approximately 28 L of the reaction mixture was removed and saved. To the remaining reaction mixture was added 24.6 kg of 2-propanol followed by 0.61 kg of octyltriethoxysilane. The reaction was continued at 70°C for 5.8 hours. The reaction mixture was then spray dried at 125°C to provide hydrophobic silica particles as a dry powder. The carbon content of the silica particles was 2.32% by weight. The T2 / T3 ratio was 0.51. The particle size distribution is shown in the attached figure.
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