US 11,859,046 B2
High-viscosity polyester with improved impact properties
Nicolas Jacquel, Lambersart (FR); René Saint-Loup, Lomme (FR); Jean-Pierre Pascault, Villeurbanne (FR); Françoise Fenouillot, L'Isle d'abeau (FR); and Alain Rousseau, Saint-Priest (FR)
Assigned to ROQUETTE FRERES, Lestrem (FR)
Appl. No. 15/576,205
Filed by Roquette Freres, Lestrem (FR)
PCT Filed May 20, 2016, PCT No. PCT/FR2016/051208
§ 371(c)(1), (2) Date Nov. 21, 2017,
PCT Pub. No. WO2016/189239, PCT Pub. Date Dec. 1, 2016.
Claims priority of application No. 1554597 (FR), filed on May 22, 2015.
Prior Publication US 2018/0155493 A1, Jun. 7, 2018
Int. Cl. C08G 63/80 (2006.01); C08G 63/672 (2006.01); C08G 63/78 (2006.01); C08G 63/183 (2006.01); C08G 63/91 (2006.01)
CPC C08G 63/80 (2013.01) [C08G 63/183 (2013.01); C08G 63/672 (2013.01); C08G 63/78 (2013.01); C08G 63/916 (2013.01)] 13 Claims
 
1. A process for producing a polyester comprising:
1,4:3,6-dianhydrohexitol units (A);
alicyclic diol units (B) other than the 1,4:3,6-dianhydrohexitol units (A); and
terephthalic acid units (C),
the polyester not containing any aliphatic non-cyclic diol units or comprising less than 5 molar % of aliphatic non-cyclic diol units, relative to all the monomer units of the polyester, and the polyester having a reduced viscosity in solution (25° C.; phenol (50% m): ortho-dichlorobenzene (50% m); 5 g polyester/1) of greater than 50 ml/g, the process comprising:
introducing, into a reactor, monomers comprising the 1,4: 3,6-dianhydrohexitol (A), the alicyclic diol (B) other than the 1,4:3,6-dianhydrohexitols (A) and the terephthalic acid (C), a molar ratio ((A)+(B))/(C) ranging from 1.05 to 1.5, the monomers not containing any aliphatic non-cyclic diols or comprising, relative to all of the monomers introduced, a molar amount of aliphatic non-cyclic diol units of less than 5%;
introducing a catalyst system into the reactor, the catalyst system comprising tin;
after introducing the catalyst system, polymerizing the monomers in the presence of the catalyst system to form a polyester, the polymerizing comprising:
a first stage of oligomerization carried out at a pressure of between 5 to 7.5 bar, during which a reaction medium is stirred under an inert atmosphere at a temperature in a range of 265 to 280° C.;
a second stage of condensation of the oligomers, during which the oligomers formed are stirred under vacuum, at a temperature in a range of 278 to 300° C. so as to form the polyester; and
recovering the polyester.