Method and apparatus for dispersion of high-surface-area, low-bulk-density fumed silica
View Patent ↗The present invention generally relates to methods of preparing stable colloidal dispersions of nanoparticulate size fumed silica particles. More particularly, the invention relates to a method of rapidly wetting and dispersing fumed silica powder for obtaining a coatable dispersion, particularly in the manufacture of inkjet media.
1. A method for dispersing and wetting fumed silica powder, comprising fumed silica particles, in an aqueous medium comprising the steps of:
(a) providing a vessel equipped with a cover lid and a radial flow mixer, one or more baffles, means for cooling the vessel, an outlet for removing a final dispersion, and an inlet for the fumed silica powder, wherein the inlet is located on the vessel bottom below the radial flow mixer and radially offset from the axis of the radial flow mixer, wherein the inlet for the fumed silica powder is connected to, or formed from, a flush bottom valve;
(b) charging the vessel with an aqueous liquid comprising at least 50 percent by weight water;
(c) subjecting the aqueous liquid in the vessel to vacuum and high-shear radial flow mixing;
(d) drawing the fumed silica powder into the vessel through the inlet, which inlet is below the surface of the aqueous liquid, while maintaining the temperature of the dispersion below 35° C., wherein the fumed silica powder is added until at least 30% solids are present;
(e) maintaining the mixing for a period sufficient to break up non-colloidal aggregates of fumed silica powder;
(f) reducing solids concentration in the vessel by at least 5 percent solids; and
(g) filtering the dispersion to reduce presence of impurities and agglomerates;
wherein the flush bottom valve is a ball valve.
2. The method of claim 1 wherein surface area of the fumed silica particles used to make the dispersion is 90 to 250 m 2 /g.
3. The method of claim 1 wherein bulk density of the fumed silica particles used to make the dispersion is less than 100 g/l.
4. The method of claim 1 wherein the aqueous liquid comprises greater than 95 percent by weight water.
5. The method of claim 1 wherein the weight percent of dispersed particles is greater than 40 weight percent.
6. The method of claim 1 wherein the fumed silica particles are characterized by a mean secondary particle size of less than 250 nm in the filtered dispersion.
7. The method of claim 6 wherein the fumed silica particles are characterized by a mean secondary particle size of less than 150 nm.
8. The method of claim 1 wherein the pH of the dispersion is adjusted to a pH of 8 to 10.
9. The method of claim 1 wherein at least 90 volume percent of the dispersed fumed silica particles have a diameter smaller than 200 nm.
10. The method of claim 1 further comprising withdrawing the dispersion from the vessel to form a first composition and combining the first composition with a second composition comprising a polymeric binder.
11. The method of claim 1 wherein one to four elongated baffles, parallel to a mixer shaft for the radial flow mixer, is attached to a removable cover lid for the vessel such that one or more baffles can be lowered into the vessel adjacent an inside side wall of the vessel without being attached to the vessel.
12. The method of claim 1 wherein the flush bottom valve is a ball valve comprising a moveable control element that partially or slightly extends above the vessels internal bottom-wall surface, thereby providing zero dead space in the vessel.
13. The method of claim 12 wherein the flush bottom valve forms a water-tight seal, so the fumed silica powder on an upstream side of the control element remains dry.
14. The method of claim 1 further comprising process control for simultaneously controlling the speed or power of a mixer driver, the vacuum in the vessel, and the flow of fumed silica powder into the vessel.
15. A method for dispersing and wetting fumed silica powder, comprising fumed silica particles, in an aqueous medium comprising the steps of:
(a) providing a vessel equipped with a cover lid and a radial flow mixer, one or more baffles, means for cooling the vessel, an outlet for removing a final dispersion, and an inlet for the fumed silica powder, wherein the inlet is located on the vessel bottom below the radial flow mixer and radially offset from the axis of the radial flow mixer, wherein the inlet for the fumed silica powder is connected to, or formed from, a flush bottom valve;
(b) charging the vessel with an aqueous liquid comprising at least 50 percent by weight water:
(c) subjecting the aqueous liquid in the vessel to vacuum and high-shear radial flow mixing;
(d) drawing the fumed silica powder into the vessel through the inlet, which inlet is below the surface of the aqueous liquid, while maintaining the temperature of the dispersion below 35° C., wherein the fumed silica powder is added until at least 30% solids are present:
(e) maintaining the mixing for a period sufficient to break up non-colloidal aggregates of fumed silica powder;
(f) reducing solids concentration in the vessel by at least 5 percent solids; and
(g) filtering the dispersion to reduce presence of impurities and agglomerates;
wherein the radial flow mixer comprises a substantially flat, circular blade with a saw tooth arrangement at the periphery.
16. The method of claim 15 wherein the flush bottom valve is a ball valve.
17. The method of claim 15 wherein the tip speed of the blade is at least 3000 ft/min tip speed during the dispersion process, and 0.25 to 1 horsepower per gallon is provided to the radial flow mixer by a motor driver.
18. A method for dispersing and wetting fumed silica powder, comprising fumed silica particles, in an aqueous medium comprising the steps of:
(a) providing a vessel equipped with a cover lid and a radial flow mixer, one or more baffles, means for cooling the vessel, an outlet for removing a final dispersion, and an inlet for the fumed silica powder, wherein the inlet is located on the vessel bottom below the radial flow mixer and radially offset from the axis of the radial flow mixer, wherein the inlet for the fumed silica powder is connected to, or formed from, a flush bottom valve;
(b) charging the vessel with an aqueous liquid comprising at least 50 percent by weight water;
(c) subjecting the aqueous liquid in the vessel to vacuum and high-shear radial flow mixing;
d) drawing the fumed silica powder into the vessel through the inlet, which inlet is below the surface of the aqueous liquid, while maintaining the temperature of the dispersion below 35° C., wherein the fumed silica powder is added until at least 30% solids are present;
e) maintaining the mixing for a period sufficient to break up non-colloidal aggregates of fumed silica powder;
(f) reducing solids concentration in the vessel by at least 5 percent solids; and
(g) filtering the dispersion to reduce presence of impurities and agglomerates;
wherein the flush bottom valve comprises a control element for regulating flow and an upstream and downstream flange at two ends thereof, wherein the downstream flange is mounted flush to the vessel by welding.
19. The method of claim 18 wherein the distance from the control element of the flush bottom valve to the vessel's internal bottom-wall surface is less than one times the diameter of a conduit supplying the fumed silica power to the vessel.