Materials and Method
For these characterizations, the PolyBLOCK 4 was used in standard laboratory conditions. Large SS316 and glass reactors were used; the SS316 reactors of 300 mL and 500 mL were placed in positions 1 and 3 (Figure 1). The 500 mL and 300 mL glass reactors were placed in positions 2 and 4 of the reactor (Table 1).
Silicone oil (Huber P20-275-50) was the main solvent used for these tests, due its wide operating range. In all cases, stirring was provided via magnetically coupled agitation provided by the PolyBLOCK in-built magnetic stirrer at 400 rpm. Six-blade PTFE Rushton impellers were used in both the glass and metal reactors. In addition, a Huber Unistat 430 was attached to the PolyBLOCK to provide active cooling. The Unistat 430 is larger than the recommended circulator for a PolyBLOCK. However, it has similar cooling and heating capacities to other smaller models, and thus allows for a performance comparison.
To achieve the maximum operating temperature of a PolyBLOCK, a circulator is not required. The circulator provides active cooling that aids in removing the access heat from a reactor, thus assisting in accurate temperature control. labCONSOL® was used to operate the PolyBLOCK 4, this software can control the reactor in several modes such as Constant Reactor Temperature or Heat/Cool Reactor (ramping reactor temperature). Heat/Cool Reactor changes the reactor temperature at a defined rate -see Figure 2 for example.
In contrast, Constant Reactor Temperature Control (Figure 3) heats the reactor contents to a specified temperature as quickly as possible. Both heating modes were investigated.