A novel process for precipitation of ultra-fine particles using sub-critical CO2
โ Scribed by Sameer V. Dalvi; Mamata Mukhopadhyay
- Publisher
- Elsevier Science
- Year
- 2009
- Tongue
- English
- Weight
- 779 KB
- Volume
- 195
- Category
- Article
- ISSN
- 0032-5910
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โฆ Synopsis
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.
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