Sludge from municipal wastewater treatment systems can be used as a source of mixed microbial cultures for the production of polyhydroxyalkanoates (PHA). Stored intracellularly, the PHA is accumulated by some species of bacteria as energy stockpile and can be extracted from the cells by reflux extraction. Dimethyl carbonate was tested as a solvent for the PHA extraction at different extraction times and biomass to solvent ratios, and 1-butanol was tested for purifying the obtained PHA at different purification times and PHA to solvent ratios. Overall, only a very small difference was observed in the different extraction scenarios. An average extraction amount of 30.7 ± 1.6 g of PHA per 100 g of biomass was achieved. After purification with 1-butanol, a visual difference was observed in the PHA between the tested scenarios, although the actual purity of the resulting samples did not present a significant difference. The overall purity increased from 91.2 ± 0.1% to 98.0 ± 0.1%.