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This research investigates the mechanical activation of kaolin as a supplementary cementitious material at the laboratory scale, aiming to optimize milling parameters using the response surface methodology. The study evaluated the effects of rotation speed and milling time on the amorphous phase content, the reduction in crystalline kaolinite, and impurity incorporation into the activated clay through the Rietveld method. The results demonstrated that adjusting milling parameters effectively enhanced clay activation, which is crucial for its use in low-carbon cements. High rotation speeds (300/350 rpm) and prolonged grinding times (90/120 min) in a planetary ball mill increased the pozzolanic activity by boosting the formation of amorphous phases from kaolinite and illite and reducing the particle size. However, the results evidenced that intermediate milling parameters are sufficient for reaching substantial degrees of amorphization and pozzolanic activity, avoiding the need for intensive grinding. Exceedingly aggressive milling introduced impurities like ZrO2 from the milling equipment wear, underscoring the need for a balanced approach to optimizing reactivity while minimizing impurities, energy consumption, and equipment wear. Achieving this balance is essential for efficient mechanical activation, ensuring the prepared clay’s suitability as supplementary cementitious materials without excessive costs or compromised equipment integrity.

Within the thermal energy storage field, one of the main challenges of this study is the development of new enhanced heat storage materials to be used in the building sector. The purpose of this study is the development of alkali-activated cements (AACs) with mechanical properties to store high amounts of heat. These AACs incorporate wastes from industrial glass process as well as microencapsulated phase change materials (mPCMs) to improve the thermal inertia of building walls, and accordingly respective energy savings. The research presented below consists of the exhaustive characterization of different AACs formulated from some waste generated during the proper management of municipal waste used as precursor. In this case study, AACs were formulated with the waste generated during the recycling of glass cullet, namely ceramic, stone, and porcelain (CSP), which is embedding a mPCM. The addition of mPCM was used as thermal energy storage (TES) material. The mechanical properties were also evaluated in order to test the feasibility of the use of the new formulated materials as a passive TES system. The results showed that the AAC obtained from CSP (precursors) mixed with mPCMs to obtain a thermal regulator material to be implemented in building walls was reached successfully. The material developed was resistant enough to perform as insulating panels. The formulated materials had high storage capacity depending on the PCM content. The durability of the mPCM shell was studied in contact with alkaline medium (NaOH 4 M) and no degradation was confirmed. Moreover, the higher the content of mPCM, the lower the mechanical properties expected, due to the porosity increments with mPCM incorporation in the formulations.