In classical experimental research work on catalytic olefin polymerization,
kinetics and powder properties are always determined as an average value o
ver a large number of polymer particles. When studying the properties of th
e polymer, the powder has to be evacuated from the reactor system. This eva
cuation step will often change the properties to be measured.
Here, a method for direct observation of growing polymer particles is shown
. To allow individual observation of a number of growing polymer particles
in a catalytic gas phase polymerization, a polymerization cell was built wi
th a transparent lid. The cell was placed in a microscopic video system in
such a way that the particles could be observed during reaction and picture
s of the particles were stored with a preset time interval.
Using a 4(th) generation Ziegler-Natta catalyst at 40 degreesC and a propyl
ene pressure of 8 bar, polymerizations were carried out in the presence of
hydrogen. It was shown that reaction kinetics can be derived from these exp
eriments, not only average values for larger number of particles, but also
kinetics for individual particles. It is shown that kinetic results can be
obtained in a reproducible way, and thus it is well possible to kinetically
characterize a catalyst in gas phase polymerization using this method.
As the current lid is not only transparent to visible light, but also to in
frared light, an infrared camera can be applied to measure surface temperat
ures of the growing polymer particles. This can be of large help in develop
ment of single particle models. One can also think about different applicat
ions and extensions. New analysis method could be applied to the same princ
iple, for example Raman spectroscopy or X-ray tomography. Next to that, cur
rently a stirrer is being implemented to introduce convective cooling of th
e particles and one can also think about application of other media than ga
s phase, like the slurry phase.