IP Library › Granted Patent US 11,254,797
Granted Patent B2
US 11,254,797 · App. 16/475,858 · Granted Feb 22, 2022

Pet regranulate having high intrinsic viscosity and method for the production thereof

Inventors: Andreas Weber (Thuringen, AT); Franz Michael Lässer (Lochau, AT); Michael Schranz (Rankweil, AT)
C08J11/26B29B9/06B29B17/0412C08G63/183B29K2067/003B29K2105/0094C08J2367/02
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Quick Facts
Patent No.
US 11,254,797
App. No.
16/475,858
Granted
Feb 22, 2022
Kind
B2
Abstract

The invention relates to a PET regranulate which, after modification of a granulated PET recyclate, has an intrinsic viscosity of at least 0.95 dl/g measured according to ASTM D 4603, preferably greater than 1.0 dl/g and particularly preferably between 1.1 dl/g and 1.7 dl/g and is suitable for the production of extrusion blow-molded containers.

Claims (33)

1. Polyethylene terephthalate (PET) regranulate suitable for forming extrusion blow-molded containers, the PET regranulate at least partially formed from a modified granulated PET recyclate, wherein modification of the granulated PET recyclate is obtainable by condensation of a granulated PET recyclate by crushing post-consumer PET bottles or industrial waste from PET bottle production into flakes, and subsequently melting the flakes by extruding the flakes with an extruder with simultaneous degradation of the intrinsic viscosity and increase of the reactive carboxyl and hydroxyl end groups, using PET recyclate which has carboxyl end groups between 30 mmol/kg and 60 mmol/kg and hydroxyl end groups between 30 mmol/kg and 70 mmol/kg and, prior to modification of the PET recyclate to form the PET regranulate, setting a water content of the PET recyclate to between 100 ppm and 5000 ppm and effecting condensing by a solid phase polycondensation at a temperature between 185° C. and 230° C. and without adding chain extensions or crosslinking additives, such that the PET regranulate has an intrinsic viscosity of at least 1.0 dl/g measured according to ASTM D 4603.

2. The PET regranulate of claim 1 , wherein the PET regranulate has an intrinsic viscosity between 1.1 dl/g and 1.7 dl/g.

3. The PET regranulate of claim 1 , wherein the PET recyclate has an intrinsic viscosity of less than 0.8 dl/g measured according to ASTM D 4603.

4. The PET regranulate of claim 1 , wherein the PET recyclate has carboxyl end groups between 32 mmol/kg and 40 mmol/kg and hydroxyl end groups between 50 mmol/kg and 60 mmol/kg.

5. The PET regranulate of claim 1 , wherein the PET regranulate comprises spherical pellets.

6. The PET regranulate of claim 1 , wherein the condensing is effected by a solid phase polycondensation at a temperature between 200° C. and 210° C.

7. The PET regranulate of claim 1 , wherein the PET regranulate is food-safe.

8. A polyethylene terephthalate PET container formed by an extrusion blow-molded process, the PET container formed from a PET regranulate, wherein the PET regranulate is obtainable by condensation of a granulated PET recyclate by crushing post-consumer PET bottles or industrial waste from PET bottle production into flakes, and subsequently melting the flakes by extruding the flakes with an extruder with simultaneous degradation of the intrinsic viscosity and increase of the reactive carboxyl and hydroxyl end groups, using PET recyclate which has carboxyl end groups between 30 mmol/kg and 60 mmol/kg and hydroxyl end groups between 30 mmol/kg and 70 mmol/kg and, prior to modification of the PET recyclate to form the PET regranulate, setting a water content of the PET recyclate to between 100 ppm and 5000 ppm and effecting condensing by a solid phase polycondensation at a temperature between 185° C. and 230° C. and without adding chain extensions and/or crosslinking additives, wherein:

for the production of containers with a volume of between 100 ml and 300 ml, the PET recyclate is modified in such a way that the intrinsic viscosity of the PET regranulate measured according to ASTM D 4603 is between 1.0 dl/g and 1.2 dl/g;

for the production of containers with a volume between 250 ml and 1000 ml, the PET recyclate is modified such that the intrinsic viscosity of the PET regranulate measured according to ASTM D 4603 is between 1.1 dl/g and 1.5 dl/g; or

for the production of containers with a volume between 750 ml and 5000 ml, the PET recyclate is modified such that the intrinsic viscosity of the PET regranulate measured according to ASTM D 4603 is between 1.2 dl/g and 1.6 dl/g.

9. The PET container of claim 8 , wherein the PET container comprises a bottle.

10. The PET container of claim 8 , wherein the PET container is processed into PET recyclate after use.

11. A method of producing a PET regranulate for forming extrusion blow-molded containers, comprising:

modifying a granulated PET recyclate, wherein modification of the granulated PET recyclate is obtainable by condensation of a granulated PET recyclate by crushing post-consumer PET bottles or industrial waste from PET bottle production into flakes; and

melting the flakes by extruding the flakes with an extruder with simultaneous degradation of the intrinsic viscosity and increase of the reactive carboxyl and hydroxyl end groups;

using PET recyclate which has carboxyl end groups between 30 mmol/kg and 60 mmol/kg and hydroxyl end groups between 30 mmol/kg and 70 mmol/kg and prior to modification of the PET recyclate to form the PET regranulate;

setting a water content of the PET recyclate to between 100 ppm and 5000 ppm; and

effecting condensation by a solid phase polycondensation at a temperature between 185° C. and 230° C. and without adding chain extensions or crosslinking additives, such that the PET regranulate is formed with an intrinsic viscosity of at least 0.95 dl/g measured according to ASTM D 4603.

12. The method of claim 11 , wherein the intrinsic viscosity is between 1.1 dl/g and 1.7 dl/g.

13. The method of claim 11 , further comprising:

washing the flakes as needed;

pressing the melted flakes through a pinhole aperture to form a melt strand;

cooling the melt strand; and

granulating the cooled melt strand into the PET recyclate.

14. The method of claim 11 , wherein the PET recyclate has an intrinsic viscosity of less than 0.8 dl/g.

15. The method of claim 11 , further comprising modifying the PET recyclate in a solid phase polycondensation reactor at an increased temperature between 195° C. and 220° C.

16. The method of claim 11 , further comprising modifying the PET recyclate in a solid phase polycondensation reactor at an increased temperature between 200° C. and 210° C.

17. The method of claim 16 , further comprising subjecting the PET recyclate to the increased temperature for 6 to 40 hours.

18. The method of claim 16 , further comprising subjecting the PET recyclate to the increased temperature for 15 to 30 hours.

19. The method of claim 15 , further comprising subjecting the PET recyclate in the solid phase polycondensation reactor to a negative pressure of less than 50 mbar.

20. The method of claim 15 , further comprising subjecting the PET recyclate in the solid phase polycondensation reactor to a negative pressure of less than 10 mbar.

21. The method of claim 11 , further comprising setting a water content of the PET recyclate to between 300 ppm and 3000 ppm prior to forming the PET regranulate.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 6, 2019
From: WEBER, DI DR. MONT, ANDREAS; LÄSSER, FRANZ MICHAEL; SCHRANZ, MICHAEL
To: ALPLA WERKE ALWIN LEHNER GMBH & CO. KG
Reel/Frame 050297/0933 →
Priority Claims (1)
CH 00002/17 · Jan 3, 2017 · national
Continuity (1)
Related Publication 20200283596A1 · Sep 10, 2020
Cited By (1)
US 12,654,361