IP Library Granted Patent US 12,435,252
Granted Patent B2
US 12,435,252 · App. 18/005,020 · Granted Oct 7, 2025

Adhesive polyethylene composition

Inventors: Katja Klimke (Linz, AT); John Jamieson (Porvoo, FI); Jari-Jussi Ruskeeniemi (Kulloo, FI); Floran Prades (Linz, AT); Noureddine Ajellal (Kulloo, FI); Tua Sundholm (Porvoo, FI); Jouni Purmonen (Kulloo, FI); Angelica Legras (Linz, AT); Andreas Albrecht (Linz, AT)
Assignee: BOREALIS AG
C09J123/0869B32B1/08B32B7/12B32B15/085B32B27/32C08F210/16C09J123/0815C09J123/26F16L9/147B32B15/18B32B2255/06B32B2255/26B32B2270/00B32B2307/748B32B2597/00
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Quick Facts
Patent No.
US 12,435,252
App. No.
18/005,020
Granted
Oct 7, 2025
Kind
B2
Abstract

The present invention relates to an adhesive polyethylene composition comprising (A) from 60 to 90 wt % of a non-elastomeric polyethylene; (B) from 9.0 to 38 wt % of an ethylene based elastomer being a copolymer of ethylene and alpha-olefin comonomer units having from 4 to 12 carbon atoms; wherein onto component (A) or components (A) and (B) an acid grafting agent (C) has been grafted in an amount of from 0.01 to 3.0 wt %, all based on the total weight of the adhesive polyethylene composition, a multi-layer structure comprising said adhesive polyethylene composition and the use of said adhesive polyethylene composition for the production of a multi-layer structure.

Claims (24)

1. An adhesive polyethylene composition comprising

(A) from 60 to 90 wt % of a non-elastomeric polyethylene;

(B) from 9.0 to 38 wt % of an ethylene based elastomer being a copolymer of ethylene and alpha-olefin comonomer units having from 4 to 12 carbon atoms, which has a density in the range of from 840 to 900 kg/m 3 ;

wherein onto components (A) and (B) an acid grafting agent (C) has been grafted in an amount of from 0.01 to 3.0 wt %, all based on the total weight of the adhesive polyethylene composition.

2. The adhesive polyethylene composition according to claim 1 , wherein the non-elastomeric polyethylene (A) is a copolymer of ethylene and one or more comonomer units selected from alpha-olefins having from 4 to 12 carbon atoms.

3. The adhesive polyethylene composition according to claim 1 , wherein the acid grafting agent (C) is selected from unsaturated carboxylic acids or derivatives thereof.

4. The adhesive polyethylene composition according to claim 1 , having a polydispersity index PDI (LS), being the ratio of Mw/Mn of from 1.5 to 4.5, determined by GPC-VISC-LS analysis.

5. The adhesive polyethylene composition according to claim 1 , having an elasticity index at a loss modulus G″=0.5 kPa EI(0.5 kPa) of from 75 to 320 Pa.

6. The adhesive polyethylene composition according to claim 1 , having only one peak in the GPC curve, which is defined below in the measurement methods as the concentration normalized LS 15 signal along the molecular weight of conventional GPC, obtained from the GPC-VISC-LS analysis.

7. The adhesive polyethylene composition according to claim 2 , wherein the non-elastomeric polyethylene (A) is a copolymer of ethylene and one single comonomer selected from alpha-olefins having from 4 to 12 carbon atoms.

8. The adhesive polyethylene composition according to claim 2 , wherein the non-elastomeric polyethylene (A) is a terpolymer of ethylene and two comonomers selected from alpha-olefins having from 4 to 12 carbon atoms.

9. The adhesive polyethylene composition according to claim 1 , obtained from a process comprising the steps of:

feeding components (A), (B) and (C) into an extruder into the feeding section of an extruder comprising a feeding section, a barrel section and a die plate, wherein the barrel section of the extruder downstream of the feeding section and upstream of the die plate is divided into a plurality of control zones, and the first control zone represents the first control zone within the barrel section downstream of the feeding zone in which the fed component(s) (A) and/or (B) start(s) to melt;

compounding the components (A) and (B) in the extruder in order to form the adhesive polyethylene composition; and

grafting components (A) and (B) with component (C) during the compounding step.

10. The adhesive polyethylene composition according to claim 9 , wherein the temperature of the second to the last control zone in the barrel section is maintained constant over all of these control zones with a total deviation of not more than 20° C.

11. The adhesive polyethylene composition according to claim 9 , wherein the process further comprises the step of:

independently controlling the temperature of each control zone of the plurality of control zones of the barrel section of the extruder as such that

a) the temperature in the first control zone of the barrel section downstream of the feeding section is in the range of from higher than 85° C. to 180° C.,

b) the temperature of the control zones of the barrel section from the first control zone of the barrel section downstream the feeding section to the control zone in the middle of the barrel section is increased over the length of the barrel section in two or more steps so that the temperature of the control zone in the middle of the barrel section is from 105% to 145% of the temperature in the first control zone of the barrel section downstream of the feeding section; and

c) the temperature of the control zones of the barrel section from control zone in the middle of the barrel section to the control zone of the barrel section directly upstream of the die plate in maintained at the same temperature or increased to a temperature of not more than 120% of the temperature of the control zone in the middle of the barrel section.

12. A multi-layer structure comprising one layer comprising the adhesive polyethylene composition according to claim 1 .

13. The multi-layer structure according to claim 12 , being a three-layer coating of a metal pipe.

14. The multi-layer structure according to claim 12 , having a peel strength at 23° C. of at least 350 N/cm and/or a peel strength at 80° C. of at least 60 N/cm.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 12, 2023
From: KLIMKE, KATJA; JAMIESON, JOHN; RUSKEENIEMI, JARI-JUSSI; PRADES, FLORAN; AJELLAL, NOUREDDINE; SUNDHOLM, TUA; PURMONEN, JOUNI; LEGRAS, ANGELICA; ALBRECHT, ANDREAS
To: BOREALIS AG
Reel/Frame 062360/0827 →
Priority Claims (1)
EP 20185451 · Jul 13, 2020 · regional
Continuity (1)
Related Publication 20230250320A1 · Aug 10, 2023
References Cited (80)
US 3236917A · Giulio et al. · 1966 [cited by applicant]
US 4639495A · Waggoner · 1987 [cited by applicant]
US 4950541A · Tabor et al. · 1990 [cited by applicant]
US 4957968A · Adur et al. · 1990 [cited by applicant]
US 5001205A · Hoel · 1991 [cited by applicant]
US 5001244A · Welborn, Jr. · 1991 [cited by applicant]
US 5194509A · Hasenbein et al. · 1993 [cited by applicant]
US 6210765B1 · Tanaka et al. · 2001 [cited by applicant]
US 8207265B2 · Mcgee et al. · 2012 [cited by applicant]
US 20050163996A1 · Lee et al. · 2005 [cited by applicant]
US 20150210902A1 · Botros · 2015 [cited by examiner]
US 20170327677A1 · Neuteboom · 2017 [cited by examiner]
CN 102300921A · 2011 [cited by applicant]
CN 106574156A · 2017 [cited by applicant]
CN 109575855A · 2019 [cited by applicant]
EA 018678B1 · 2011 [cited by applicant]
EP 0678103B1 · 1995 [cited by applicant]
EP 0688794B1 · 1995 [cited by applicant]
EP 0721474A1 · 1996 [cited by applicant]
EP 0769027A1 · 1997 [cited by applicant]
EP 0810235 · 1998 [cited by applicant]
EP 1316598B1 · 2003 [cited by applicant]
EP 1859926B1 · 2007 [cited by applicant]
EP 3409739A1 · 2018 [cited by applicant]
RU 2477299C2 · 2013 [cited by applicant]
RU 2600167C2 · 2016 [cited by applicant]
RU 2697560C2 · 2019 [cited by applicant]
RU 2705584C1 · 2019 [cited by applicant]
WO 8703604A1 · 1987 [cited by applicant]
WO 199212182A1 · 1992 [cited by applicant]
WO 9325590A1 · 1993 [cited by applicant]
WO 9509191A1 · 1995 [cited by applicant]
WO 9512622A1 · 1995 [cited by applicant]
WO 9618662A1 · 1996 [cited by applicant]
WO 9728170A1 · 1997 [cited by applicant]
WO 9856831A1 · 1998 [cited by applicant]
WO 9858001A1 · 1998 [cited by applicant]
WO 9951646A1 · 1999 [cited by applicant]
WO 9965949A1 · 1999 [cited by applicant]
WO 0034341A2 · 2000 [cited by applicant]
WO 00040620A1 · 2000 [cited by applicant]
WO 2001055230A1 · 2001 [cited by applicant]
WO 2001055275A1 · 2001 [cited by applicant]
WO WO0155275A1 · 2001 [cited by examiner]
WO 2005118655A1 · 2005 [cited by applicant]
WO WO2008054637A1 · 2008 [cited by examiner]
WO 2008089978A1 · 2008 [cited by applicant]
WO 2015158790A1 · 2015 [cited by applicant]
WO 2015158791A2 · 2015 [cited by applicant]
WO 2017108951A1 · 2017 [cited by applicant]
WO 2017108969A1 · 2017 [cited by applicant]
WO 2018108917A1 · 2018 [cited by applicant]
WO 2018108918A1 · 2018 [cited by applicant]
WO 2018178151A1 · 2018 [cited by applicant]
WO 2018178152A1 · 2018 [cited by applicant]
WO WO2020115071A1 · 2020 [cited by examiner]
Anita J. Brandolini, NMR Spectra of Polymers and Polymer Additives, Marcel Dekker, Inc. New York, 2000 pp. 1-660. [cited by applicant]
Castignolles, et al., “Detection and quantification of branching in polyacrylates by size-exclusion chromatography (SEC) and melt-state 13C NMR spectroscopy” Polymer 5, 2009, 2373-2383. [cited by applicant]
Christian Jackson, et al. Molecular Weight-Sensitive Detectors for Size Exclusion Chromatography, 2004, pp. 103-144. [cited by applicant]
Definition of terms relating to the Non-Ultimate Mechanical Properties of Polymers Pure & Appl. Chem. vol. 70, pp. 701-754, 1998. [cited by applicant]
E-L. Heino, et al., “Rheological Characterization of Polyethylene Fractions” Theoretical and Applied Rheology, Aug. 17-21, 1992, pp. 360-362. [cited by applicant]
Eeav-Leena Heino, “The Influence of molecular structure on some rheological properties of polyethylene” Annual transactions of the Nordic Rheology Society, vol. 3, 1995. [cited by applicant]
Gerhard Hubner, Application of Melt-State NMR Spectroscopy for Polyolefin Characterization in Industry, Macromolecules, Chapter 24, 401, 2011. [cited by applicant]
J. Randall, Macromol. Chem Phys. 1989, C29, 201_NPL. [cited by applicant]
John M. Griffin, “Low-load rotor-synchronised Hahn-echo pulse train (RS-HEPT) 1H decoupling in solid-state NMR: factors affecting MAS spin-echo dephasing times”, Magnetic Reson. Chem. 2007; 45: S198-S208. [cited by applicant]
Katja Klimke, et al. “Optimisation and Application of Polyolefin Branch Quantification by Melt-State 13C NMR Spectroscopy” Macromol. Chem. Phys. 2006, 207, 382-395. [cited by applicant]
M. Pollard, et al. “Observation of Chain Branching in Polyethylene in the Solid State and Melt via 13C NMR Spectroscopy and Melt NMR Relaxation Time Measurements” Macromolecules 2004, 37, 813-825. [cited by applicant]
Matthew Parkinson, et al. “Effect of Branch Length on 13C NMR Relaxation Properties in Molten Poly[ethyleneco-(a-olefin)] Model Systems” Macromol. Chem Phys. 2007, 208, 2128-2133. [cited by applicant]
Vincent Busico, et al. 1H NMR Analysis of Chain Unsaturations in Ethene/1-Octene Copolymers Prepared with Metallocene Catalysts at High Temperature, Macromolecules 2005, 38, 6988-6996. [cited by applicant]
Vincent Busico, et al., “Alk-1-ene Polymerization in the Presence of a Monocyclopentadienyl Zirconium(IV) Acetamidinate Catalyst: Microstructural and Mechanistic Insights”, Macromol. Rapid Commun. 2007, 28, 1128-1134. [cited by applicant]
Weixia Liu, Poly(ethylene-co-1-octene) Characterization by High-Temperature Multidimensional NMR at 750 MHZ, Macromolecules 2001, 34, 4757-4767. [cited by applicant]
Kenia Filip, et al., “Heteronuclear decoupling under fast MAS by a rotor-synchronized Hahn-echo pulse train” Journal of Magentic Resonance 176, 2005, 239-243. [cited by applicant]
XiaoHua Qiu, et al., Improved Peak Assignments for the 13C NMR Spectra of Poly(ethylene-co-1-octene)s, Macromolecules 2007, 40, 6879-6884. [cited by applicant]
Yiyong He, Unexpected proton spin-lattice relaxation in the solutions of polyolefin and tetrachloroethane, Res. Chem, 2010, 48, 537-542. [cited by applicant]
Zhe Zhou, et al., “A new decoupling method for accurate quantification of polyethylene copolymer composition and triad sequence distribution with 13C NMR” Journal of Magnetic Resonance 187 (2007) 225-233. [cited by applicant]
EP20185451 European Search Report dated Dec. 9, 2020. [cited by applicant]
Russian Application No. 2023102785/04, Office Action dated Jul. 12, 2023. [cited by applicant]
Chinese Application No. 202180049413.7, Office Action dated Apr. 30, 2025. [cited by applicant]
Common Knowledge Evidence Document Building Materials. [cited by applicant]
Korean Application No. 10-2023-7004631, Office Action dated Apr. 27, 2025. [cited by applicant]