Method for preparing stereoblock polylactide
View Patent ↗The present invention relates to a method for preparing a stereoblock polylactide, comprising: a step of obtaining a first reaction mixture with a monomer conversion rate of 80 to 95% by adding a catalyst to a D-lactide and growing a PDLA chain; a step of obtaining a second reaction mixture with a monomer conversion rate of 80 to 95% by adding an L-lactide to the first reaction mixture and growing a racemic PDLLA chain at the end of the PDLA chain; and a step of further adding an L-lactide to the second reaction mixture and growing a PLLA chain at the end of the PDLLA chain through a polymerization reaction. The preparation method is capable of providing a more convenient synthesis by skipping a process of removing residual monomers in the middle of the reaction, and also of preventing multi-blocking and oligomerization of polymer chains due to a mixture of chains by gradually adding polymerizable monomers while controlling the monomer conversion rate in a one-port synthesis, thereby reducing chain transfer during the polymerization.
1. A method for preparing a stereoblock polylactide (sb-PLA), which consists essentially of:
(1) adding a catalyst to D-lactide, performing a polymerization reaction to grow a poly(D-lactide) (PDLA) chain and obtaining a first reaction mixture having a monomer conversion of 80% to 95%;
(2) adding L-lactide to the first reaction mixture, performing a polymerization reaction to grow a racemic poly(D,L-lactide) (PDLLA) chain at a terminal of the PDLA chain and obtaining a second reaction mixture having a total monomer conversion of D-lactide and L-lactide of 80% to 95%; and
(3) adding L-lactide to the second reaction mixture and performing a polymerization reaction to grow a poly(L-lactide) (PLLA) chain at a terminal of the PDLLA chain,
wherein the reactions in steps (1) to (3) are a one-pot reaction where the reactions are continuously performed in one reactor,
wherein the polymerization reaction in step (3) is performed by additionally adding stannous octoate (Sn(Oct) 2 ) to the second reaction mixture as the catalyst.
2. The method of claim 1 , wherein the L-lactide in step (2) is added in an amount of 10 to 30 mol % based on a total mole number of L-lactide added in steps (2) and (3).
3. The method of claim 1 , wherein the catalyst in step (1) is added in an amount of 0.0001 to 0.001 parts by mole based on 1 part by mole of the D-lactide.
4. The method of claim 1 , wherein the catalyst in step (1) is stannous octoate (Sn(Oct) 2 ).
5. The method of claim 1 , wherein the D-lactide and the L-lactide are dried in vacuum for 1 to 10 hours.
6. The method of claim 1 , wherein the catalyst in step (1) is added hi a dissolved state in a solvent, and the solvent is primarily removed prior to the polymerization reaction.