A chloromethylated polystyrene-divinylbenzene-grafted phosphorustungsten heteropolyacid quaternary ammonium salt catalyst was prepared, and the catalyst was characterized by infrared spectroscopy and inductively coupled plasma atomic emission spectroscopy. The synthesis of 2,2-epoxycyclohexylcarboxylic acid-2’,2’-epoxycyclohexylcarboxylic acid (AOO) was catalyzed without solvent, using H34O5 (w(H3O3)=3.4%) and 3’-cyclohexene methyl ester (abbreviated as A) as raw materials, and the effects of catalyst dosage, n(A):n(H4O2), reaction time, reaction temperature and other factors on the reaction were discussed. The suitable synthesis conditions were obtained (calculated as 2mmol A): reaction temperature 60 °C, reaction time 65 min, catalyst dosage 100.5 g, n(A): n(H0