The purpose of this paper was to investigate the physical and mechanical properties of compressed expanded graphite (CEG) and their porous derivatives after impregnation, polymerization; and carbonization by the use of acoustic emission method (AE). The mechanical and structural characteristics of compressed expanded graphite and their three groups of porous composites after each technological process are presented and discussed. The measurements of acoustic emission parameters in these materials were carried out at wide range of frequency of the waves (0.1÷2.5 MHz). The changes of two of parameters: - AE pulses counts rate and spectrum distribution of AE waves - are presented in this paper. The analysis of the respective parameters AE also gives possibility to determine the micro- and macro structural changes of materials at different levels of technological processes. Applications of these materials as catalysts with high specific surface make them very interesting subject of study. Also compressed expanded graphite composite membranes prepared from furfuryl alcohol polymers are promising for gas separation.