研究目的
To apply microreactor technology for the continuous synthesis of polymethylmethacrylate (PMMA) and compare the performance between laboratory and medium scale microreactor systems.
研究成果
The synthesis of PMMA was successfully performed using both laboratory and medium scale microreactor systems, with comparable results. The medium scale plant enabled continuous operation for 8 hours with low variation in product properties. This demonstrates the feasibility of using microreactors for polymerization and ensures performance comparability between scales, supporting future applications in mass production.
研究不足
The study used specific microreactor systems and materials (e.g., stainless steel and PTFE tubes), which may limit generalizability. Heat transfer issues were noted, requiring longer reaction times. The production scales (2-3 t/year and 100 t/year) are not fully mass production levels. Polymerization inhibitors in MMA were not removed, potentially affecting results.
1:Experimental Design and Method Selection:
The study used microreactor systems for polymerization reactions, with designs enabling continuous or pseudo-continuous feeding. The synthesis of PMMA was chosen as a model reaction, involving heating methyl methacrylate (MMA) with an initiator (AIBN) in toluene.
2:Sample Selection and Data Sources:
Reagents included commercially obtained MMA, AIBN, and toluene. Samples were prepared with a 1:1 volume ratio of MMA to AIBN solution (1 mol% in toluene).
3:List of Experimental Equipment and Materials:
Equipment included laboratory and medium scale microreactor systems from Hitachi, Ltd., syringe pumps, triple cam driven pumps, tubes made of stainless steel or PTFE, temperature-controlled baths, back pressure regulators, and a gel permeation chromatography (GPC) system from Hitachi High Technologies, Ltd. for analysis.
4:Experimental Procedures and Operational Workflow:
Reagents were fed into the microreactor and downstream tube immersed in a bath at
5:15 K. Reaction time was controlled by tube length and flow rate. Product solutions were cooled and analyzed by GPC. Continuous operation for 8 hours was performed with the medium scale plant. Data Analysis Methods:
3 Yield, number average molecular weight (Mn), and polydispersity index (PDI) were calculated from GPC data using standard formulas. Statistical variations were assessed over time.
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