IP Library Granted Patent US 8,476,076
Granted Patent B2
US 8,476,076 · App. 13/289,444 · Granted Jul 2, 2013

Chromatography of polyolefin polymers

Inventors: Freddy A. Van Damme (Brugge, BE); John W. Lyons (Midland, MI); William L. Winniford (Lake Jackson, TX); Alexander Willem deGroot (Sugar Land, TX); Matthew D. Miller (Lake Jackson, TX)
Assignee: Dow Global Technologies LLC
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Quick Facts
Patent No.
US 8,476,076
App. No.
13/289,444
Granted
Jul 2, 2013
Kind
B2
Abstract

A method and apparatus for chromatography of a polyolefin polymer by flowing a solution of the polyolefin polymer through liquid flowing through a graphitic carbon liquid chromatography stationary phase. The method can be used to determine the monomer to comonomer ratio of a polyolefin copolymer such as a copolymer of ethylene and 1-octene or a copolymer of propylene and ethylene.

Claims (18)

1. A method for chromatography of a polyolefin polymer, comprising the following step: introducing a solution of the polyolefin polymer into a liquid flowing through a liquid chromatography stationary phase, the liquid chromatography stationary phase comprising graphitic carbon, and wherein the polyolefin polymer emerging from the liquid chromatography stationary phase has a retention factor greater than zero.

2. The method of claim 1 , where the polyolefin polymer is a copolymer consisting essentially of ethylene and an alpha olefin.

3. The method of claim 2 , where the alpha olefin consists essentially of 1-octene.

4. The method of claim 1 , where the polyolefin polymer is a copolymer consisting essentially of propylene and an alpha olefin.

5. The method of claim 4 , where the alpha olefin consists essentially of ethylene.

6. The method of claim 1 , where the concentration of the polyolefin polymer in the solution of polyolefin polymer is greater than 0.1 milligrams per milliliter of solution.

7. The method of claim 1 , where the liquid chromatography stationary phase consists essentially of graphitic carbon.

8. An improved liquid chromatography method comprising the step of introducing a solution of a polyolefin polymer into a liquid flowing through a liquid chromatography stationary phase, the polyolefin polymer emerging from the liquid chromatography stationary phase with a retention factor greater than zero, the improvement comprising the liquid chromatography stationary phase comprising graphitic carbon.

9. The method of claim 8 , where the polyolefin polymer is a copolymer consisting essentially of ethylene and an alpha olefin.

10. The method of claim 9 , where the alpha olefin consists essentially of 1-octene.

11. The method of claim 8 , where the polyolefin polymer is a copolymer consisting essentially of propylene and an alpha olefin.

12. The method of claim 11 , where the alpha olefin consists essentially of ethylene.

13. The method of claim 8 , where the concentration of the polyolefin polymer in the solution of polyolefin polymer is greater than 0.1 milligrams per milliliter of solution.

14. The method of claim 8 , where the liquid chromatography stationary phase consists essentially of graphitic carbon.

15. An apparatus for determining the monomer to comonomer ratio of a copolymer, wherein the apparatus comprises a high temperature liquid chromatography unit comprising a graphitic carbon liquid chromatography column, a pump, a polymer solution, and

a means for an additional fractionation by size exclusion chromatography or asymmetric flow field flow fractionation, added after the fractionation by the graphitic column.

16. The apparatus of claim 15 , wherein the apparatus further comprises a means to increase the temperature of the stationary phase within the column.

17. The apparatus of claim 15 , wherein the apparatus further comprises a gradient composition mobile phase.

Continuity (4)
Continuation 12572313
Provisional Application 61195326 · Oct 6, 2008
Provisional Application 61181015 · May 26, 2009
Related Publication 20120047990A1 · Mar 1, 2012