According to the Bureau of National Statistics of the Republic of Kazakhstan, by the end of 2023, approximately 120 million tons of municipal solid waste (MSW) had been generated across over 3200 landfills in the country. About 4.5 million tons are generated annually, of which only about 15% are recycled. The accumulation of both unsorted and sorted waste poses significant environmental risks, primarily through the generation of methane, a greenhouse gas that is 28 times more dangerous than carbon dioxide in contributing to the planet’s greenhouse effect over a century and 84 times more effective over a 20-year timeframe. The objective of this research is to examine the physicochemical composition, as well as the physical and thermal-chemical properties, of municipal solid waste from six cities in Kazakhstan: Astana, Almaty, Shymkent, Aktobe, Karaganda, and Ust-Kamenogorsk. Unlike existing studies, this study has a uniform waste sample, which includes the complete emptying of dozens of containers from different areas of the cities under consideration. Thus, the average composition of solid waste across the cities was maintained. Analysis of the physicochemical composition was conducted for both unsorted and sorted municipal solid waste from all cities, determining the total and analytical moisture content, ash content, and volatile matter, as well as the higher and lower calorific values. The calorific value of unsorted waste by city was as follows, in kJ/kg: Astana,8850.37; Almaty, 9244.57; Atobe, 9596.41; Shymkent, 9425.48; Karaganda, 8902.8; Ust-Kamenogorsk, 9669.07. The calorific value of sorted waste was as follows, in kJ/kg: Astana, 11,922.79; Almaty, 11,692.31; Atobe, 11,913.13; Shymkent, 12,494.38; Karaganda, 11,671.92; Ust-Kamenogorsk, 12,462.52. The efficiency of sorting was estimated as the first stage of MSW processing. The efficiency factor of the manual sorting process in practice was 0.4–0.8. The results obtained enable the evaluation of technologies for the effective management of municipal solid waste and facilitate experimental investigations into semi-industrial pyrolysis, combustion, plasma processing, and composting facilities.