Poly(p-xylylene tetrasulfide) was synthesized from 1,4-bis(chloromethyl)-benzene and sodium tetrasulfide using interfacial polycondensation technique to examine the effect of methyl tributyl ammonium chloride, tetrabutyl ammonium bromide, and benzyl triethyl ammonium chloride as phase transfer catalysts. The structure of the synthesized polysulfide was confirmed via elemental analysis, attenuated total reflectance Fourier transform infrared spectroscopy, Raman spectroscopy, and X-ray diffraction techniques. Moreover, the thermal behavior of this polymer was characterized using differential scanning calorimetry and thermo gravimetric analysis methods. Beyond, Friedman method was applied to analyze the degradation kinetics of the prepared polymer. The synthesized polymer had a molecular weight of about 2584 g/mol.