US 7,488,783 B2
Method for the production of polyactide from a solution of lactic acid or one of the derivatives thereof
Philippe Coszach, Courcelles (Belgium); Jean-Christophe Bogaert, Ligne (Belgium); and Frederic Van Gansberghe, Linkebeek (Belgium)
Assigned to Brussels Biotech, Brussels (Belgium)
Appl. No. 10/523,061
PCT Filed Aug. 04, 2003, PCT No. PCT/EP03/50360
§ 371(c)(1), (2), (4) Date Aug. 24, 2005,
PCT Pub. No. WO2004/014889, PCT Pub. Date Feb. 19, 2004.
Claims priority of application No. 2002/0469 (BE), filed on Aug. 06, 2002.
Prior Publication US 2006/0014975 A1, Jan. 19, 2006
Int. Cl. C08G 63/08 (2006.01)
U.S. Cl. 525—450  [525/415; 549/274; 549/231; 528/480] 34 Claims
OG exemplary drawing
 
1. A process for the production and purification of lactide, wherein, staffing from an aqueous solution of lactic acid or lactic acid derivatives, the stages comprise:
a) evaporation of free water and a portion of the water of constitution until oligomers having a molecular mass of between 400 and 2000 amu, a total acidity as lactic acid equivalent of between 119 and 124.5% and an optical purity, expressed as L-lactic acid, of between 90 and 100% are obtained;
b) feeding a mixture comprising a depolymerization catalyst and the oligomers obtained in step a) to a depolymerization reactor to produce:
b1) a lactide-rich vapor phase, and
b2) an oligomer-rich liquid residue;
c) selective condensation of the lactide-rich vapor with recovery, in the liquid form, of a crude lactide product freed from the volatile compounds;
d) melt crystallization of the crude lactide product to produce:
d1) a purified lactide fraction having a residual acidity of less than 10 meq/kg, a water content of less than 200 ppm, a total lactide content of 99-99.9% and a meso-lactide content of less than 1%; and
d2) at least a first residual fraction having a lactide content comprise between 35 and 80%; and
e) separating the purified lactide from the step d1) and the at least first residual fraction from the step d2); and
f) aqueous treatment of said at least first residual fraction from the step d2) of melt crystallization, consisting of:
f1) extractive and controlled crystallization of the residue fractions in an aqueous medium, with control of the geometry of crystals formed and with segregation of a lactide suspension towards a solid phase and of impurities towards a liquid phase to carry out aqueous extraction of the impurities;
f2) separation of the suspension of crystals formed in step e1) from the liquid phase and then draining to separate a wet cake rich in lactide crystals from a liquid phase depleted in lactide and laden with impurities; and
f3) drying the wet cake to provide prepurified lactide obtained from said at least first residual fraction of said step d2).