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A series of polynaphthalsoimides and polynaphthalimides from 1,4,5,8-naphthalene dianhydride and 4,4'-methylene-bis(2,6-diisopropylaniline) or its hydrochloride in HMPA were synthesized in one-step high temperature polycondensation process. The different temperatures of the reaction from 125°C to 180°C were applied. The products were investigated using PL techniques in both solutions and thin layers. The observed changes in all investigated spectra and photochemical properties were presented. The remarkable changes in emission wavelength in photoluminescence was observed together with the increase of the reaction temperature. This work presents novel approach to the class of polymers well known to literature worldwide trying to explain of some surprising aspects of photoluminescence of these compounds. When investigated in solution, the polymer synthesized at 125°C exhibit almost no photoluminescence. The increase of the temperature to 150°C causes the strong increase in the photoluminescence intensity at 545 nm. When the reaction temperature increase to 180°C the intensity of photoluminescence exhibits moderate increase at 546.5 nm, however, remarkable increase was observed for 476.5 nm and 440 nm. The photoluminescence analysis of the polymers synthesized shows that depending on reaction temperature products emitting at different wavelengths may be obtained. Investigations were repeated for thin layers of the polymers. The obtained results and their comparison with the results in solution were also presented and discussed.