Resorbable polymer purification process
The present invention is directed to an improved purification process using additive and activated carbon for purifying resorbable polymers suitable for industrial manufacturing. The metal catalyst concentration in the purified resorbable polymers of this invention is preferably less than 1 ppm. The method can be used to obtain high molecular weight polymers that are substantially metal free.
1. A method of reducing the residual tin content in a tin containing resorbable polymer to less than 1 ppm, comprising:
(a) dissolving a polymer in an organic solvent to produce a polymer solution;
(b) combining the polymer solution with activated carbon and an additive; wherein said method results in the formation of a purified polymer; and
(c) recovering the purified polymer by anti-solvent precipitation; and wherein the additive is lactic acid.
2. The method of claim 1 , wherein the polymer is linear.
3. The method of claim 2 , wherein the additive is up to 20 wt % of the solvent, and activated carbon is up to 9 wt % of the linear polymer.
4. The method of claim 1 , wherein the polymer is branched.
5. The method of claim 4 , wherein the additive is up to 20 wt % of the solvent, and activated carbon is between 50-100 wt % of the branched polymer.
6. The method of claim 1 , wherein the additive and activated carbon is exposed to the polymer solution for 2 to 4 hours.
7. A purified polyester which is a branched or a linear polylactide-glycolide having a weight averaged molecular weight of 5 to 315 kDa, a polydispersity M w /M n of 1.5 to 2.5, prepared by the process of ring-opening polymerization of lactide and glycolide in the presence of tin (II)-(2-ethylhexanoate) or tin chloride followed by treatment with activated carbon and an additive; and wherein the additive is lactic acid.
8. The purified polyester of claim 7 having a D,L-lactide/glycolide molar ratio of 100-50/0-50.
9. The purified polyester of claim 7 having a D,L-lactide/caprolactone molar ratio of 100-90/0-10.
10. The purified polyester of claim 7 having a terpolymer of lactide, glycolide, and caprolactone.
11. The purified polyester of claim 7 , wherein the purified polyester is
poly(D,L-lactide),
poly(D,L-lactide-co-glycolide) with more than 50 mole % D,L-lactide content,
poly(D,L-lactide-co-caprolactone) with more than 10 mole % D,L-lactide content,
poly(L-lactide-co-caprolactone) with more than 50 mole % L-lactide content,
poly(D,L-lactide-co-trimethylene carbonate) with more than 50 mole % D,L-lactide content,
poly(D,L-lactide-co-dioxanone) with more than 50 mole % D,L-lactide content, or
poly(D,L-lactide-co-glycolide-co-caprolactone) with less than 50 mole % glycolide content.
12. The purified polyester of claim 7 having an acid number comparable to standard polylactide.
13. The purified polyester of claim 7 having improved thermal stability compared to standard polylactide.