To assess the performance and future possibilities of catalytic microwave pyrolysis, laboratory-scale experiments were conducted on a widely available biomass feedstock, Eucalyptus grandis. Non-catalysed microwave pyrolysis was conducted under varying conditions to determine important factors of the microwave pyrolysis process and to conduct a basic performance evaluation. Future possibilities of microwave pyrolysis were determined by comparison to available technologies. Calcined Mg-Al LDH clay (layered double oxide or LDO) was used as catalyst to improve the quality of the pyrolysis process and its products. The heating and reaction mechanisms for microwave pyrolysis show that it offers distinct advantages over conventional pyrolysis. The main advantages are rapid and efficient volumetric heating, as well as acceptable yields at lower temperatures (much lower than those required by conventional pyrolysis), which can possibly lead to significant energy savings. Comparing the performance of a modified domestic microwave to an off-the-shelf microwave unit (Roto Synth) proved that cheap and comparative microwave research is possible. The yields from the domestic microwave products compared very closely to those of the Roto Synth unit, each having yields for char, oil and gas of 47.9%, 33.2%, 18.9% and of 46.8%, 32.7%, 20.55% respectively. The cost of the modified domestic setup was ~1% of that of the off-the-shelf unit. The use of a quartz reactor and slight adjustments to the stepper motor driver and thermocouple are recommended for future use. The pyrolysis process was found to be very dependent on power and power density. Higher powers increase the liquid and gas yields and a critical power density was identified between 800W and 1000W. The effects of power density were interesting and led to conclusions regarding the penetration depth of microwaves which could possibly play a significant role in the scale-up of microwave pyrolysis technology. Microwave pyrolysis undeniably has several advantages over conventional pyrolysis. However, for it to become competitive, microwave fast pyrolysis technologies need to be developed through the use of mixed bed reactors that can achieve fast heating rates. Possible candidates include rotating cone and fluidised bed reactors. Hybrid technology also provides unique advantages and has huge potential. Comparison of pyrolysis technologies is difficult without good data on continuous microwave pyrolysis reactors, and therefore the development of such reactors is recommended for future research. Catalysis of microwave pyrolysis with LDO proved effective. The catalyst promoted the formation of volatiles (gas and liquid), even when present in small ratios. It also promoted the formation of esters and even anhydrides and small fractions of hydrocarbons at high catalyst ratios. The catalyst activity led to increased water yields. This indicated that it removes oxygen from the pyrolysis products, thereby improving their quality. The catalyst was believed to be limited by the low temperatures used in this investigation and higher temperatures might increase the release of CO2 and should be investigated. Significant reduction in the total acid number (TAN) and an improved dry-basis heating value were also achieved by the addition of the catalyst. The water content increased from 50% to 70%, the TAN reduced from 174 mg KOH/(g oil) to 72 mg KOH/(g oil), and the calorific value increased from 19.1 MJ/kg to 21.5 MJ/kg. / Dissertation (MEng)--University of Pretoria, 2017. / Chemical Engineering / MEng / Unrestricted