A method for synthesizing block copolymers using microreactor coupling enzyme catalysis and organocatalysis
A technology of block copolymers and microreactors, which can be used in biochemical equipment and methods, bioreactor/fermenter combinations, bioreactors/fermenters for specific purposes, etc. Advanced problems, to achieve the effect of optimizing the process flow, controllable molecular weight, and retaining the catalytic efficiency
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Embodiment 1
[0035]Fill 1.17 g of immobilized enzyme Novozyme 435 with a particle size of 0.3 to 0.9 mm into an immobilized enzyme microreactor with an inner diameter of 3.8 mm and a length of 300 mm (retention volume is 1.81 mL), using an inner diameter of 1 mm and a length of 9218.2 mm microchannel reactor (reserved volume is 7.24mL), connect the device, and flush the pipeline with toluene solvent after redistillation to remove water. Add ε-caprolactone (6.8484g, 6.65mL, 60mmol), benzyl alcohol (0.21mL, 2mmol), toluene (8.14mL) and δ-valerolactone to two flat-bottomed dry ampoules after removing water at high temperature (1.82mL, 20mmol), TBD (0.1mmol), toluene (13.18mL), after shaking and mixing, move them into the first material sampling device A and the second material sampling device B, and adjust the flow rate of A and B to be 0.362ml / min, the reaction temperatures in the two reactors were 60°C and 25°C respectively, and the reaction was started. After 25min, the reaction was stabl...
Embodiment 2
[0037] Fill 1.17 g of immobilized enzyme Novozyme 435 with a particle size of 0.3 to 0.9 mm into an immobilized enzyme microreactor with an inner diameter of 3.8 mm and a length of 300 mm (retention volume is 1.81 mL), using an inner diameter of 1 mm and a length of 18436.4 mm microchannel (retention volume is 14.48mL), connect the device, and flush the pipeline with toluene solvent after re-distillation to remove water. Add ε-caprolactone (6.65mL, 60mmol), benzyl alcohol (0.21mL, 2mmol), 8.14mL toluene and δ-valerolactone (5.44mL, 60mmol ), 0.3mmol TBD, 9.56mL toluene, oscillated and mixed evenly, and moved into the first material sampling device A and the second material sampling device B, the flow rate of A and B was adjusted to 0.362ml / min, and the reaction temperature was 60°C and 25°C, start the reaction, wait for 25 minutes to stabilize the reaction, collect for 6 minutes, add 80mL of methanol and quencher solid benzoic acid (0.13mmol), stir and precipitate at low tempe...
Embodiment 3
[0039] Fill 0.585 g of immobilized enzyme Novozyme 435 with a particle size of 0.3 to 0.9 mm into an immobilized enzyme microreactor with an inner diameter of 3.8 mm and a length of 150 mm (retention volume is 0.905 mL), using an inner diameter of 1 mm and a length of 3687 mm The microchannel reactor (retention volume is 2.90mL), connect the device, and flush the pipeline with the toluene solvent after distilling off the water. Add ε-caprolactone (6.65mL, 60mmol), benzyl alcohol (0.21mL, 2mmol), 8.14mL toluene and lactide (20mmol), DBU (0.02 mL, 0.1mmol), 14.98mL toluene, after shaking and mixing, move into the first material sampling device A and the second material sampling device B, control the flow rate of A and B to be 0.181ml / min, the reaction in the two reactors The temperature was 60°C and 25°C respectively, and the reaction was started. After 44 minutes, the reaction was stable and collected for 11 minutes. Then, 80 mL of methanol and 0.04 mmol of solid benzoic acid (...
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