A novel process for precipitation of ultra-fine particles using sub-critical CO 2

Abstract

Supercritical CO 2 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 CO 2 solubility for imparting the antisolvent effect. Most of these CO 2 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 CO 2-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 CO 2 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.