1：Experimental Design and Method Selection:

The study used a hydrothermal synthesis method to prepare kaolinite/ZnO nanocomposites with 50 wt.% ZnO. The process involved mixing ZnCl2 and NaOH solutions with kaolin suspension, stirring at 100°C for 5 hours, followed by decantation, washing, drying at 105°C, and calcination at 600°C. Reproducibility was assessed by preparing multiple samples and characterizing them using various analytical techniques.

2：Sample Selection and Data Sources:

Samples were prepared in several doses, with five representative samples collected from different loads for each type (KAZN15 dried at 105°C and KAZN65 calcined at 600°C). Kaolin KKAF from LB MINERALS was used as the matrix.

3：List of Experimental Equipment and Materials:

Equipment included SEM (Hitachi SU6600), XRFS (SPECTRO XEPOS), atomic emission spectrometry (SPECTRO CIROS VISION), XRPD (Bruker D8 Advance with V?NTEC 1 detector), FTIR (Nicolet 6700 FT-IR), and UV-vis spectrometer (CINTRA 303). Materials included ZnCl2 (Lach-Ner), NaOH (Lach-Ner), kaolin KKAF (LB MINERALS), and Acid Orange 7 dye.

4：3). Materials included ZnCl2 (Lach-Ner), NaOH (Lach-Ner), kaolin KKAF (LB MINERALS), and Acid Orange 7 dye. Experimental Procedures and Operational Workflow:

4. Experimental Procedures and Operational Workflow: The synthesis involved specific steps: mixing precursors, stirring, decantation, washing until filtrate conductivity <100 μS cm?1, drying, and calcination. Characterization involved SEM for morphology, XRFS for chemical composition, XRPD and Rietveld analysis for phase composition, FTIR for structural analysis, and photodegradation tests using AO7 under UV irradiation.

5：Data Analysis Methods:

Data were analyzed using Scherrer formula for crystallite size calculation, Rietveld refinement with DIFFRACplus TOPAS software for quantitative phase analysis, and standard spectroscopic methods for composition and activity evaluation.