Adsorbing and recycling alcohols and acids from industrial wastewater is of great significance in wastewater treatment; establishing the possible quantitative relationship of alcohol–acid adsorption capacity with the struct0ures of adsorbents and exploring the key factors determining their adsorption performance is very important and challenging in environment science. To solve this difficult problem, the adsorption of C1-5 alcohols, C2-4 acids, and Fischer–Tropsch synthesis (FTS) wastewater on zeolites with similar hydrophobicity and pore structures (β and MFI), similar hydrophilicity but different pore structures (Y and MOR), and similar pore structures but significant differences in hydrophobicity (MOR vs. β and MFI) was systematically investigated. It was found that: (1) For materials with similar pore structures, increased hydrophobicity correlates with enhanced adsorption capacities for alcohols and acids. (2) For materials with similar hydrophobicity, a higher content of ultramicropores leads to increased adsorption of alcohols and acids. (3) Between pore structure and hydrophobicity, it is hydrophobicity that ultimately plays a decisive role in adsorption capacities. The adsorption behavior of zeolites in FTS wastewater exhibits a consistent trend, with β-zeolite demonstrating the highest hydrophobicity (contact angle of 105°) and the greatest adsorption capacity in FTS wastewater, achieving 103 mg/g. Following five adsorption–desorption cycles, the zeolites retained their adsorption capacity without significant degradation, indicating their excellent stability and reusability. The findings identify the critical factors determining adsorption performance and provide a solid foundation for the design and development of high-performance adsorbents for alcohol–acid adsorption.