Method for removing terminal thiocarbonyl of RAFT (reversible addition-fragmentation chain transfer) polymer at room temperature
A technology of thiocarbonyl and polymer, which is applied in the field of polymer synthesis, can solve the problems of weak ability to extract hydrogen atoms and weak ability to leave macromolecular free radicals, and achieve the effects of improving performance, easy operation, and cost saving
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Embodiment 1
[0046] Embodiment one: CPDB is a chain transfer agent, AIBN is an initiator, and carries out conventional RAFT polymerization
[0047] According to the ratio [St] 0 / [CPDB] 0 / [AIBN] 0 =500 / 5 / 1, add St, CPDB, AIBN and toluene in turn to a 25mL Schlenk tube, after 6 standard cycles of freezing-pumping-thawing, place in a constant temperature (60°C) The reaction is carried out in a magnetic stirring oil bath according to a predetermined time. After the reaction, take out the Schlenk tube, open it, dissolve it with 5 mL of THF, pour it into 200 mL of cold methanol, leave it overnight, filter it with suction, and dry it to obtain polystyrene (PS).
Embodiment 2
[0048] Embodiment two: when TEMPO charges less, carry out the removal of polystyrene terminal thiocarbonyl group
[0049] Proportioned [PS] 0 / [Cu(0)powder] 0 / [PMDETA] 0 / [TEMPO] 0 =1 / 5 / 5 / 10, sequentially add Cu(0)powder, PMDETA, TEMPO and PS dissolved in solvent into a 5mL ampoule, add a stirrer, and go through 6 standard freezing-pumping-thawing inflation cycles Afterwards, the tube was sealed under an oxygen-free atmosphere. Place the sealed ampoule in a magnetic water bath at a constant temperature (25°C) for a predetermined time to react. After the reaction, take out the ampoule, open the ampoule, dissolve with 5mL of THF, and pass the solution through neutral Al 2 o 3 Chromatographic column, remove residual metal or metal ions, pour into 200mL of cold methanol, leave overnight, suction filter and dry to obtain the product.
[0050] Polymerization conditions: St=15.0mL; [St] 0 / [CPDB] 0 / [AIBN] 0 =500 / 5 / 1; solvent is toluene; T=60℃, no oxygen; reaction conditio...
Embodiment 3
[0051] Embodiment three: increase the charging capacity of TEMPO, carry out the removal of polystyrene terminal thiocarbonyl
[0052] Proportioned [PS] 0 / [Cu(0)powder] 0 / [PMDETA] 0 / [TEMPO] 0 =1 / 5 / 5 / 20, sequentially add Cu(0)powder, PMDETA, TEMPO and PS dissolved in solvent into a 5mL ampoule, add a stirrer, and go through 6 standard freezing-pumping-thawing inflation cycles Afterwards, the tube was sealed under an oxygen-free atmosphere. Place the sealed ampoule in a magnetic water bath at a constant temperature (25°C) for a predetermined time to react. After the reaction, take out the ampoule, open the ampoule, dissolve with 5mL of THF, and pass the solution through neutral Al 2 o 3 Chromatographic column, remove residual metal or metal ions, pour into 200mL of cold methanol, leave overnight, suction filter and dry to obtain the product.
[0053] Polymerization conditions: St=15.0mL; [St] 0 / [CPDB] 0 / [AIBN] 0 =500 / 5 / 1; solvent is toluene; T=60℃, no oxygen; react...
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