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Figure 100 ‘a’ shows that for a reaction time of 30 minutes although some smooth surfaces remain, vast regions of the surface are covered with pores. Blistering is visible on the remaining smooth sections, indicating that the polymer swelling within the bulk material is advanced. This is further indicated by Figure 100 ‘b’ where it is apparent that some fragmentation of the polymer surface has taken place. After 45 minutes under the reaction conditions the polymer swelling is extensive, with advanced blistering covering almost the entire surface of the sample, Figure 100 ‘c’. Several blisters have ruptured forming fragments and exposing the voids beneath as seen in Figure 100 ‘d’. The shutdown sequence of the reactor was the same in all experiments and is not thought to contribute to the results obtained. By evaluation of Figure 99 and Figure 100 it may be inferred that the decomposition process, when scEtOH is used as a solvent in the presence of Cs2CO3, begins with the swelling of the polymer. Upon reaching the reaction conditions the polymer swelling is confined to the bulk sample and is manifested only in the cracking of the polymer surface, with porosity only observed along leading edges of the polymer post cutting. Within the first 10 minutes under the reaction conditions the polymer swelling process becomes extensive and the cracked sections are able to separate to accommodate the increased bulk volume. As this process takes place it is likely that some of the polymer surface swell and move relative to the bulk material, leading to the loss of the polymer surface and consequently the sub surface pores become visible as can be seen in Figure 100 ‘c’. The degradation products, of which phenol is one [321], are likely to diffuse from the bulk polymer into the bulk solvent and may be involved in the swelling process. As localised swelling takes place 247PDF Image | Supercritical Fluids and Their Application to the Recycling of High-Performance Carbon Fibre Reinforced Composite Materials
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