IP Library Granted Patent US 12,116,450
Granted Patent B2
US 12,116,450 · App. 17/050,138 · Granted Oct 15, 2024

Urethane exchange catalysts and methods for reprocessing cross-linked polyurethanes

Inventors: David J. Fortman (Pittsburgh, PA); William R. Dichtel (Wilmette, IL); Daylan T. Sheppard (Evanston, IL)
Assignees: Northwestern University; Cornell University
C08G18/7671C08G18/222C08G18/227C08G18/4247C08G18/4833C08G18/73C08G18/82
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Quick Facts
Patent No.
US 12,116,450
App. No.
17/050,138
Granted
Oct 15, 2024
Kind
B2
Abstract

Disclosed herein are polyurethane compositions and methods for reprocessing cross-linked polyurethane compositions. The polyurethane composition comprises a network polymer and a polyurethane exchange catalyst permeated within the network polymer. The network polymer comprises a dynamic network formed from an isocyanate constitutional unit and a second constitution unit having a hydroxyl group capable of reacting with an isocyanate group of the isocyanate constitutional unit to form a urethane bond. The catalyst comprises a metal atom and a ligand coordinated to the metal atom.

Claims (29)

1. A method for reprocessing a polyurethane composition, the method comprising providing a polyurethane composition, heating the polyurethane composition to an effective bond-exchange temperature, and applying mechanical force to the polyurethane composition for an effective bond-exchange time,

wherein the polyurethane composition comprises a network polymer and a polyurethane exchange catalyst post-synthetically impregnated into the network polymer;

wherein the network polymer comprises a dynamic network formed from an isocyanate constitutional unit and a second constitution unit having a hydroxyl group capable of reacting with an isocyanate group of the isocyanate constitutional unit to form a urethane bond;

wherein the polyurethane exchange catalyst comprises a metal selected from Bi, Fe, Zr, Ti, Hf, Al, Zn, Cu, Ni, Co, Mn, V, Sc, Y, Ce, or Mo and a ligand coordinated with the metal atom;

and

wherein a mol % of the polyurethane exchange catalyst to total isocyanate functionality is less or equal to 5 mol %.

2. The method of claim 1 , wherein the effective bond-exchange temperature is less than or equal to 200° C.

3. The method of claim 2 , wherein the effective bond-exchange temperature is less than or equal to 160° C.

4. The method of claim 1 , wherein the effective bond-exchange time is less than or equal to 30 minutes.

5. The method of claim 1 further comprising the mechanically processing the provided polyurethane composition prior to heating or mechanically processing the network polymer prior to impregnation.

6. The method of claim 5 , wherein mechanically processing the provided polyurethane composition comprises grinding the provided polyurethane composition.

7. The method of claim 1 , wherein the polyurethane exchange catalyst does not comprise Sn.

8. A method for reprocessing a polyurethane composition, the method comprising impregnating a polyurethane exchange catalyst into a network polymer, heating the polyurethane composition to an effective bond-exchange temperature, and applying mechanical force to the polyurethane composition for an effective bond-exchange time, wherein the network polymer comprises a dynamic network formed from an isocyanate constitutional unit and a second constitution unit having a hydroxyl group capable of reacting with an isocyanate group of the isocyanate constitutional unit to form a urethane bond;

wherein the polyurethane exchange catalyst comprises a metal selected from Bi, Fe, Zr, Ti, Hf, Al, Zn, Cu, Ni, Co, Mn, V, Sc, Y, Ce, or Mo and a ligand coordinated with the metal atom;

and

wherein a mol % of the polyurethane exchange catalyst to total isocyanate functionality is less or equal to 5 mol %.

9. The method of claim 8 , wherein the catalyst comprises Bi(neo) 3 , Fe(acac) 3 , Ti(OiPr) 2 (acac) 2 , Hf(acac) 4 , Zr(acac) 4 , Mn(acac) 2 , Bi(oct) 3 , Zn(tmhd) 2 , Zr(tmhd) 4 , or any combination thereof.

10. The method of claim 8 , wherein the catalyst is Bi(neo) 3 .

11. The method of claim 8 , wherein the catalyst is Fe(acac) 3 .

12. The method of claim 8 , wherein the second constitutional unit is a prepolymer molecule comprising a polyether, a polyester, a polycarbonate, a polyacrylate, a polyolefin, a polybutadiene, a polysulfide, or a polysiloxane.

13. The method of claim 12 , wherein the second constitutional unit comprises a polyether.

14. The method of claim 12 , wherein the second constitutional unit comprises a polyester.

15. The method of claim 8 , wherein the second constitutional unit is a branch unit having at least three hydroxyl groups each capable of reacting with the isocyanate group of the first constitutional unit to form the urethane bond.

16. The method of claim 15 , wherein the second constitutional unit further comprises one or more molecules selected from a polyether, a polyester, a polycarbonate, a polyacrylate, a polyolefin, a polybutadiene, a polysulfide, a polysiloxane, a plant-based oil, an alcohol, or an amine.

17. The method of claim 8 , wherein the isocyanate constitutional unit is an aromatic isocyanate constitutional unit.

18. The method of claim 8 , wherein the effective bond-exchange temperature is less than or equal to 200° C.

19. The method of claim 8 , wherein the effective bond-exchange time is less than or equal to 30 minutes.

20. The method of claim 8 further comprising the mechanically processing the provided polyurethane composition prior to heating or mechanically processing the network polymer prior to impregnation.

21. The method of claim 8 , wherein the polyurethane exchange catalyst does not comprise Sn.

Assignments (3)
CONFIRMATORY LICENSE Recorded Feb 13, 2025
From: NORTHWESTERN UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 070206/0461 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 10, 2020
From: DICHTEL, WILLIAM; SHEPPARD, DAYLAN
To: NORTHWESTERN UNIVERSITY
Reel/Frame 054328/0106 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 10, 2020
From: FORTMAN, DAVID J.
To: NORTHWESTERN UNIVERSITY; CORNELL UNIVERSITY
Reel/Frame 054375/0017 →
Continuity (2)
Provisional Application 62662593 · Apr 25, 2018
Related Publication 20210095067A1 · Apr 1, 2021