IP Library Granted Patent US 9,650,465
Granted Patent B2
US 9,650,465 · App. 12/811,846 · Granted May 16, 2017

Heterophasic propylene copolymer with improved creep behavior

Inventors: Kristien Roegiers (Wolvertem, BE); Geert Snellings (Sint-Lievens-Houtem, BE); Alain Standaert (Brussels, BE)
Assignee: Total Research & Technology Feluy
C08F297/08C08F10/06C08L23/12C08F110/06C08L23/16C08L2207/02
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Quick Facts
Patent No.
US 9,650,465
App. No.
12/811,846
Granted
May 16, 2017
Kind
B2
Abstract

The present invention concerns heterophasic propylene copolymers, comprising a propylene homopolymer (PPH) and an ethylene-propylene rubber (EPR), having a very broad molecular weight distribution, a well-defined total ethylene content and a specific intrinsic viscosities of the ethylene-propylene rubber (EPR). The invention further concerns the process to produce such heterophasic propylene copolymers. The heterophasic propylene copolymers of the present invention are particularly suited for pails, pallets, IBCs and crates. In particular, the heterophasic propylene copolymers of the present invention are characterized by an improved resistance to creep.

Claims (34)

1. A heterophasic propylene copolymer comprising:

(i) a propylene homopolymer (PPH); and

(ii) from 12.0 wt % to 18.0 wt % of an ethylene propylene rubber (EPR), wherein the heterophasic propylene copolymer exhibits a melt flow index in the range from 2.0 dg/min to 6.0 dg/min (measured according to ISO 1133, condition L, 230° C. 2.16 kg), a molecular weight distribution M w /M n of 11.0 or more (as measured on pellets) and a total ethylene content in the range from 6.0 wt % to 11.0 wt % relative to the total weight of the heterophasic propylene copolymer, wherein the EPR has an intrinsic viscosity (measured in tetralin at 135° C.) in the range from 2.0 dl/g to 4.0 dl/g;

wherein an injection molded VDA RL-KLT crate of the heterophasic propylene copolymer exhibits greater resistance to creep, as determined by a creep test in accordance with VDA 4500 KLT-System, in comparison to an injection molded VDA RL-KLT crate of a comparative heterophasic propylene copolymer having a molecular weight distribution M w /M n of 8.5.

2. The heterophasic propylene copolymer of claim 1 , wherein the EPR, determined as the acetone insoluble fraction of the xylene soluble fraction, is present in an amount from 13.0 wt % to 17.0 wt % of the total weight of the heterophasic propylene copolymer.

3. The heterophasic propylene copolymer of claim 1 , wherein the PPH comprises at least two propylene homopolymer fractions of different melt flow index (measured according to ISO 1133, condition L, 230° C., 2.16 kg) and wherein the fraction with the lowest melt flow index has a melt flow index in the range from 0.50 dg/min to 1.50 dg/min.

4. The heterophasic propylene copolymer of claim 3 , wherein the PPH has a melt flow index in the range from 5.0 dg/min to 8.0 dg/min.

5. The heterophasic propylene copolymer of claim 3 , wherein the fraction with the lowest melt flow index has a melt flow index in the range from 0.75 dg/min to 1.25 dg/min.

6. The heterophasic propylene copolymer of claim 1 , wherein the PPH and the EPR, together, comprise at least 95.0 wt % of the heterophasic propylene copolymer.

7. The heterophasic propylene copolymer of claim 1 , further comprising a nucleating agent.

8. An article comprising the heterophasic propylene copolymer of claim 1 .

9. The article of claim 8 , wherein the article is a crate, a pallet, an IBC or a pail.

10. The article of claim 8 manufactured by injection molding.

11. The heterophasic propylene copolymer of claim 1 , wherein the heterophasic propylene copolymer is polymerized in the presence of a catalyst comprising an internal donor, wherein the internal donor is either:

selected from a group consisting of phthalates, diethers, and combinations thereof; or

selected from a group consisting of succinates, di-ketones, enamino-imines, and combinations thereof.

12. The heterophasic propylene copolymer of claim 1 , wherein the total ethylene content is at most 9.5 wt %.

13. The heterophasic propylene copolymer of claim 1 , wherein the heterophasic propylene copolymer exhibits a molecular weight distribution M w /M n of 11.5 or more (as measured on pellets).

14. The heterophasic propylene copolymer of claim 1 , wherein the heterophasic propylene copolymer exhibits a molecular weight distribution M w /M n of 12.0 or more (as measured on pellets).

15. The heterophasic propylene copolymer of claim 1 , wherein the EPR has an intrinsic viscosity (measured in tetralin at 135° C.) in the range from 2.5 dl/g to 3.5 dl/g.

16. The heterophasic propylene copolymer of claim 1 , wherein the PPH has a melt flow index in the range from 6.0 dg/min to 7.0 dg/min.

17. The heterophasic propylene copolymer of claim 1 , wherein the PPH and the EPR, together, comprise at least 95 wt % of the heterophasic propylene copolymer, and wherein the heterophasic propylene copolymer is adapted for injection molding.

18. The heterophasic propylene copolymer of claim 1 , wherein the PPH has a xylene solubles content of at most 3.0 wt. % relative to a total weight of the PPH.

19. The heterophasic propylene copolymer of claim 1 , wherein the PPH and the EPR, together, comprise at least 97 wt % of the heterophasic propylene copolymer, and wherein the heterophasic propylene copolymer is adapted for injection molding.

20. The heterophasic propylene copolymer of claim 1 , wherein the EPR, determined as the acetone insoluble fraction of the xylene soluble fraction, is present in an amount from 14.0 wt % to 16.0 wt % of the total weight of the heterophasic propylene copolymer.

21. A process for the production of a heterophasic propylene copolymer comprising a propylene homopolymer (PPH), and from 12.0 wt % to 18.0 wt % of an ethylene propylene rubber (EPR) in presence of a Ziegler-Natta polymerization catalyst, an aluminium alkyl, an external electron donor and hydrogen, said process comprising:

(a) polymerizing propylene to produce the PPH;

(b) subsequently transferring the PPH obtained in step (a) to a further polymerization reactor;

(c) copolymerizing propylene and ethylene to produce the EPR in said further polymerization reactor, wherein the heterophasic propylene copolymer has a melt flow index (measured according to ISO 1133, condition L, 230° C., 2.16 kg) in the range from 2.0 dg/min to 6.0 dg/min, a molecular weight distribution M w /M n , of 11.0 or more (measured on pellets) and a total ethylene content in the range from 6.0 wt % to 11.0 wt %, relative to the total weight of the heterophasic propylene copolymer, wherein the EPR has an intrinsic viscosity (measured in tetralin at 135° C.) in the range from 2.0 dl/g to 4.0 dl/g;

wherein an injection molded VDA RL-KLT crate of the heterophasic propylene copolymer exhibits greater resistance to creep, as determined by a creep test in accordance with VDA 4500 KLT-System, in comparison to an injection molded VDA RL-KLT crate of a comparative heterophasic propylene copolymer having a molecular weight distribution M w /M n of 8.5.

22. The process of claim 21 , wherein the Ziegler-Natta polymerization catalyst comprises an internal donor selected from the group consisting of phthalates, diethers and combinations thereof.

23. The process of claim 21 , wherein the PPH comprises at least two propylene homopolymer fractions of different melt flow index (measured according to ISO 1133, condition L, 230° C., 2.16 kg), and wherein the process further comprises regulating the melt flow index of the fraction with the lowest melt flow index to be in the range from 0.50 dg/min to 1.50 dg/min.

24. The process of claim 23 , wherein the fraction with the lowest melt flow index has a melt flow index in the range from 0.75 dg/min to 1.25 dg/min.

25. The process of claim 21 , wherein the EPR has an intrinsic viscosity (measured in tetralin at 135° C.) in the range from 2.5 dl/g to 3.5 dl/g.

Assignments (2)
CHANGE OF NAME Recorded Mar 28, 2014
From: TOTAL PETROCHEMICALS RESEARCH FELUY
To: TOTAL RESEARCH & TECHNOLOGY FELUY
Reel/Frame 032553/0832 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 19, 2011
From: ROEGIERS, KRISTIEN; SNELLINGS, GEERT; STANDAERT, ALAIN
To: TOTAL PETROCHEMICALS RESEARCH FELUY
Reel/Frame 026148/0532 →
Priority Claims (1)
EP 08150072 · Jan 7, 2008 · regional
Continuity (1)
Related Publication 20110124798A1 · May 26, 2011