Penelitian ini bertujuan menganalisis pengaruh variasi rasio penambahan kalium hidroksida (KOH) dan asam asetat terhadap sifat mekanis busa polyisocyanurate (PIR) berpenguat fly ash 31,15%. Metode eksperimental dilakukan dengan desain faktorial 2 x 5 x 5, meliputi 2 level konsentrasi KOH (55% dan 60%), 5 level rasio dominan KOH (1:1, 2:1, 3:1, 4:1, dan 5:1), dan 5 level rasio dominan asam asetat (1:1, 2:1, 3:1, 4:1, dan 5:1). Parameter pengujian meliputi kuat tekan, modulus elastisitas, kuat lentur (sumbu kuat dan sumbu lemah), kuat tarik, impact strength, densitas, rasio mengembang, waktu setting, elongation, dan specific strength. Hasil penelitian menunjukkan bahwa konsentrasi KOH 55% secara konsisten menghasilkan performa mekanis yang lebih unggul dibandingkan KOH 60%. Variasi terbaik secara keseluruhan diperoleh pada KOH 55% dominan KOH dengan rasio 2:1, yang menghasilkan kuat tekan 23,32 MPa, specific strength 27.830,68 N.m/kg, modulus elastisitas 477,30 MPa, dan densitas 838,08 kg/m³. Kuat lentur sumbu kuat tertinggi (12,14 MPa) diperoleh pada KOH 60% dominan KOH rasio 2:1, sementara impact strength tertinggi (59,206 kJ/mm²) dicapai pada KOH 60% dominan asam asetat rasio 3:1. Rasio optimum per kelompok bervariasi, yaitu 3:1 untuk KOH 60% dominan KOH, 2:1 untuk KOH 60% dominan asam asetat, 2:1 untuk KOH 55% dominan KOH, dan 3:1 untuk KOH 55% dominan asam asetat. Penelitian ini membuktikan bahwa keseimbangan rasio KOH–asam asetat merupakan faktor determinan dalam mengontrol kinetika reaksi dan meningkatkan sifat mekanis busa PIR berpenguat fly ash.
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