Combining phase change materials with hygroscopic materials in building construction is considered a promising solution for improving the indoor environment of building envelopes. In this study, a diatomite-based Phase Change Humidity Control Material (PCHCM) sourced from the Sig mine in northwest Algeria was used as a finishing layer in buildings and experimentally analyzed in a thermal chamber. The experiment involved exposing three brick walls with different insulation layers (mortar, Algerian diatomite, and PCHCM) to controlled temperatures and humidities using a ZL-7918A controller. Temperature fluctuations were measured every 30 minutes for 38 hours using an infrared camera (TESTO890) based on the experimental conditions. Two sets of results were obtained depending on the conditions. PCHCM demonstrated better output conditions when the charging temperatures were equal to or greater than the PCM fusion temperature. However, diatomite alone provided more interesting results when the charging temperatures were below the PCM fusion temperature. The numerical study, compared to a previous benchmark, showed good agreement with a relative error of less than 4.8%. A second analysis focused on two types of PCHCM: the first type had one PCM with a melting point of 28 °C, while the second type combined two PCMs with different melting points (28 °C and 22 °C). Comparative analysis revealed a better desired temperature and humidity when using the second type of PCHCM on the inner side of the wall.