Graduation Year

2011

Document Type

Dissertation

Degree

Ph.D.

Degree Granting Department

Chemical Engineering

Major Professor

Aydin K. Sunol

Keywords

biopolymer, Chitosan, coating, DMSO, micropthesis

Abstract

Coating of fine pthesiss to produce tailored surface properties is currently a key development for supercritical fluids applications, in different areas such as: pharmaceutical, nutraceutical, cosmetic, agrochemical, electronic and specialty chemistry industries. During the encapsulation process the pthesis surface can be designed with specific properties by spreading a thin film coating material over the surface of the pthesiss.

Chitosan, a natural polymer, was used in this work as the encapsulant material. Chitosan is biocompatible, biodegradable to normal body constituents, safe, non-toxic, bacteriostatic, anticancerogen, and versatile polymer. These attributes are among the properties that make Chitosan an attractive component of pharmaceutical products.

The main objective of this research was to encapsulate solid pthesiss under 5fÝm with a biopolymer, Chitosan, using supercritical CO2 as one of the solvents. In order to reach this goal, some the following initial tasks were completed: the cloud point for the system DMSO-CO2 was determined and compared with published data to validate the experimental system. Subsequently the cloud point experiments were extended to include the ternary system Chitosan-DMSO-CO2, and a dynamic solubility experimental set-up was constructed and used to obtain solubility data for the same ternary system.

A novel SCF fluidized bed was used to micro encapsulate porous (TiO2) and non-porous pthesiss (CaO) through a temperature swing with a Chitosan thin layer. DMSO was used as an entrainer to enable solubilization of Chitosan and removed within the supercritical carbon dioxide.

Several analytical methods were used to characterize these pthesiss; SEM-EDS analysis was used to evaluate a group of pthesiss, determining composition and pthesis diameter on samples up to 900 pthesiss. TEM and AFM confirmed pthesiss of one micron or less were encapsulated with a thickness of less than 5 nm. AFM shows pthesis roughness on the nanometer range, 46 nm or more for uncoated pthesiss and 2-4 nm for the encapsulated ones.

FTIR, NMR and DSC-TGA analysis confirmed that the chemical structure of Chitosan remained constant before and after processing, and the changes observed were attributed to some DMSO and moisture adsorbed during the encapsulation process.

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