E. Bilgili et al., Analysis of rubber particles produced by the solid state shear extrusion pulverization process, RUBBER CHEM, 73(2), 2000, pp. 340-355
Vulcanized natural rubber was pulverized using a single screw extruder in a
non-cryogenic Solid State Shear Extrusion (SSSE) process where rubber gran
ulates were subjected to high compressive and shear stresses. The produced
particles had diameters ranging from 40 to 1700 mu m Reprocessing of the pr
oduced powder resulted in a narrower particle size distribution. Considerab
le heat generated in the extruder due to friction caused surface oxidation
of the fine rubber particles and. in turn, initiation of agglomeration of a
portion of the produced particles.
Physical, chemical, and thermal analyses were performed on the produced rub
ber particles and the rubber granulates to determine the effects of the pul
verization process. The produced particles had irregular shapes with rough
surfaces. The external surfaces of the particles were porous, but no microp
orosity was detected by nitrogen BET analysis. Swelling and extraction expe
riments showed that both the crosslink density and gel fraction of the part
icles were lower than those of the rubber granulates. The reprocessing of t
he produced particles caused further reduction in the crosslink density and
the eel fraction A correlation was established between the crosslink densi
ty and the gel fraction. Thermal analysis revealed similar behavior of all
particles and the granulates in a nitrogen environment, but there was consi
derable thermo-oxidative degradation of the fine panicles in air. The chemi
cal analysis indicated that some of the bonds were broken during the pulver
ization process, and partial devulcanization had taken place.