Powder Technology, Vol.195, No.3, 190-195, 2009
A novel process for precipitation of ultra-fine particles using sub-critical CO2
Supercritical CO2 has been utilized as solvent. cosolvent or antisolvent in several processes for production of ultra-fine solid particles with narrow size distribution. The key to the precipitation of such particles is to produce a very large, rapid and uniform supersaturation in the solution of a solid substance. This can be achieved either by a rapid and large reduction in the temperature of solution or by drastically increasing the CO2 solubility for imparting the antisolvent effect. Most of these CO2 processes require high-pressure pumps, specially designed nozzles and accurate control of process parameters. In order to obviate these requirements, a simple technique of precipitation by pressure reduction over the gas-expanded liquids (PPRGEL), such as CO2-expanded organic solutions has been utilized to impart a large. uniform and rapid reduction of temperature in the solution for instantaneous precipitation of ultra-fine particles. This process utilizes sub-critical CO2 at relatively low pressures of 40-70 bar and near ambient temperature of 303 K for creating a temperature drop of 30-70 K in the solution within seconds, without using any specially designed nozzle or high-pressure pumps. The present paper validates the process principle for precipitation of Zinc acetate (ZnAc) nanoparticles from its organic solution in a mixed solvent of acetone and dimethyl sulfoxide (DMSO). Nanoparticles are produced with the average size of 20-250 nm (from 100 ml of solution in a high-pressure vessel of 1.09 L working volume), and vary in shapes such as long needles, rods and near spherical depending on pressure (40-70 bar at 303 K), solid concentration (0.01-0.05 g/ml) and addition of stabilizer. (c) 2009 Elsevier B.V. All rights reserved.
Keywords:Zinc acetate;Nanoparticles;Depressurization;Temperature reduction;Sub-critical CO2;Gas-expanded liquids