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Sommaire du brevet 2583386 

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Disponibilité de l'Abrégé et des Revendications

L'apparition de différences dans le texte et l'image des Revendications et de l'Abrégé dépend du moment auquel le document est publié. Les textes des Revendications et de l'Abrégé sont affichés :

  • lorsque la demande peut être examinée par le public;
  • lorsque le brevet est émis (délivrance).
(12) Demande de brevet: (11) CA 2583386
(54) Titre français: COMPOSITION DE MOULAGE A BASE DE POLYETHYLENE POUR L'ENGAINEMENT EXTERIEUR DE CABLES ELECTRIQUES
(54) Titre anglais: POLYETHYLENE MOLDING COMPOSITION FOR EXTERNAL SHEATHING OF ELECTRIC CABLES
Statut: Réputée abandonnée et au-delà du délai pour le rétablissement - en attente de la réponse à l’avis de communication rejetée
Données bibliographiques
(51) Classification internationale des brevets (CIB):
  • C08L 23/06 (2006.01)
(72) Inventeurs :
  • VOGT, HEINZ (Allemagne)
  • BERTHOLD, JOACHIM (Allemagne)
(73) Titulaires :
  • BASELL POLYOLEFINE GMBH
(71) Demandeurs :
  • BASELL POLYOLEFINE GMBH (Allemagne)
(74) Agent: ROBIC AGENCE PI S.E.C./ROBIC IP AGENCY LP
(74) Co-agent:
(45) Délivré:
(86) Date de dépôt PCT: 2005-11-17
(87) Mise à la disponibilité du public: 2006-05-26
Licence disponible: S.O.
Cédé au domaine public: S.O.
(25) Langue des documents déposés: Anglais

Traité de coopération en matière de brevets (PCT): Oui
(86) Numéro de la demande PCT: PCT/EP2005/012305
(87) Numéro de publication internationale PCT: WO 2006053740
(85) Entrée nationale: 2007-04-05

(30) Données de priorité de la demande:
Numéro de la demande Pays / territoire Date
10 2004 055 587.7 (Allemagne) 2004-11-18

Abrégés

Abrégé français

L'invention concerne une composition de moulage à base de polyéthylène qui présente une distribution plurimodale de masse molaire et qui est particulièrement appropriée pour produire un engainement extérieur de câbles électriques ou de transmission d'informations. Cette composition de moulage présente une densité, à une température de 23 °C, allant de 0,94 à 0,95 g/cm3 et un MFI19015 allant de 1,2 à 2,1 dg/min. De plus, cette composition comprend de 45 à 55 % en poids d'un homopolymère A d'éthylène à faible masse moléculaire, de 30 à 40 % en poids d'un copolymère B à masse moléculaire élevée d'éthylène et une autre oléfine comprenant de 4 à 8 atomes de carbone et de 10 à 20 % en poids d'un copolymère C d'éthylène à masse moléculaire très élevée. L'invention concerne également un câble électrique ou de transmission d'informations qui comprend une gaine extérieure constituée de ladite composition de moulage à base de polyéthylène et dont l'épaisseur est comprise entre 0,2 et 3 cm.


Abrégé anglais


The invention relates to a polyethylene molding composition which has a
multimodal molar mass distribution and is particularly suitable for producing
external sheathing of electric or information transmission cables. The molding
composition has a density at a temperature of 23~C in the range from 0.94 to
0.95 g/cm3 and an MFI19015 in the range from 1.2 to 2.1 dg/min. It comprises
from 45 to 55% by weight of a low molecular weight ethylene homopolymer A,
from 30 to 40% by weight of a high molecular weight copolymer B of ethylene
and another olefin having from 4 to 8 carbon atoms and from 10 to 20% by
weight of an ultra high molecular weight ethylene copolymer C. The invention
also relates to an electric or information transmission cable having an
external sheath of the polyethylene molding composition which has'a thickness
in the range from-0.2 to 3 cm.

Revendications

Note : Les revendications sont présentées dans la langue officielle dans laquelle elles ont été soumises.


Claims
1. A polyethylene molding composition which has a multimodal
molar mass distribution and has a density at a temperature
of 23°C in the range from 0.94 to 0.950 g/cm3 and an
MF1190/5 in the range from 0.5 to 2.1 dg/min and comprises
from 45 to 55% by weight of a low molecular weight
ethylene homopolymer A, from 30 to 40% by weight of a high
molecular weight copolymer B of ethylene and another
olefin having from 4 to 8 carbon atoms and from 10 to 20%
by weight of an ultra high molecular weight ethylene
copolymer C, where all percentages are based on the total
weight of the molding composition.
2. The polyethylene molding composition according to claim 1,
wherein the high molecular weight copolymer B contains
from 1 to 8% by weight, based on the weight of copolymer
B, of comonomers having from 4 to 8 carbon atoms and the
ultra high molecular weight ethylene copolymer C contains
from 1 to 8% by weight, based on the weight of copolymer
C, of comonomers.
3. The polyethylene molding composition according to claim 1
or 2 in which 1-butene, 1-pentene, 1-hexene, 1-octene,
4-methyl-1-pentene or mixtures thereof are present as
comonomers.
4. The polyethylene molding composition according to one or
more of claims 1 to 3 which has a viscosity number VN overall,
measured in accordance with ISO/R 1191 in decalin at a
temperature of 135°C in the range from 260 to 340 cm3/g,
preferably from 280 to 320 cm3/g.
5. The polyethylene molding composition according to one or
more of claims 1 to 4 which has a notched impact toughness

11
AFM (-30°C) in the range from 3.5 to 4.5 kJ/m2 and a
notched impact toughness ACN (+23°C) in the range from 12
to 16 kJ/m2 and has an environmental stress cracking
resistance (FNCT) in the range from 150 to 250 h.
6. A process for preparing a polyethylene molding composition
according to one or more of claims 1 to 5, in which the
polymerization of the monomer is carried out in suspension
at temperatures in the range from 70 to 90°C, a pressure in
the range from 2 to 10 bar and in the presence of a highly
active Ziegler catalyst composed of a transition metal
compound and an organoaluminum compound, wherein the
polymerization is a three-stage polymerization, with the
molar mass of the polyethylene formed in each stage being
regulated in each case by means of hydrogen.
7. The process according to claim 6, wherein the hydrogen
concentration in the first polymerization stage is set so
that the viscosity number VN1 of the low molecular weight
polyethylene A is in the range from 50 to 90 cm3/g.
8. The process according to claim 6 or 7, wherein the
hydrogen concentration in the second polymerization stage
is set so that the viscosity number VN2 of the mixture of
polymer A plus polymer B is in the range from 260 to
320 cm3/g.
9. The process according to any of claims 6 to 8, wherein the
hydrogen concentration in the third polymerization stage
is set so that the viscosity number VN3 of the mixture of
polymer A, polymer B plus polymer C is in the range from
260 to 340 cm3/g, in particular from 280 to 320 cm3/g.
10. The use of a polyethylene molding composition according to
one or more of claims 1 to 5 for the external sheathing of

12
electric cables, wherein the polyethylene molding
composition is firstly plasticized in an extruder at
temperatures in the range from 200 to 250°C and is then
extruded through a nozzle onto the surface of the cable
and is cooled there.
11. An electric or information transmission cable having an
internal, electrically conductive core of metal and an
external, electrically nonconductive sheath comprising a
polyethylene molding composition according to any of
claims 1 to 5, wherein the external sheath has a thickness
in the range from 0.2 to 3 cm.

Description

Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.


CA 02583386 2007-04-05
WO 2006/053740 PCT/EP2005/012305
Title: Polyethylene molding composition for external
sheathing of electric cables
The present invention relates to a polyethylene (PE) molding
composition which has a multimodal molar mass distribution and
is particularly suitable for producing cable sheathing, and a
process for preparing this molding composition in the presence
of a catalytic system comprising a Ziegler catalyst and a
cocatalyst via a multistage reaction sequence comprising
successive polymerization steps.
Polyethylene is widely used for industrial applications in
which a material having a high mechanical strength and a high
resistance to thermooxidative degradation is required in order
to ensure a long life even at elevated use temperatures. In
addition, polyethylene has the particular advantages that it
has good chemical resistance, it has a low intrinsic weight
and it is a material which can easily be processed in the
melt.
PE-molding compositions for cable sheathing should accordingly
possess the following important properties:
- Easy processability.
- Good resistance to weathering influences.
- Good thermal aging resistance.
- Ability to withstand high mechanical stresses and good
abrasion resistance.
- Low permeability to water vapor and oxygen so as to avoid
corrosion of the metallic conductor or conductors.
WO 97/03124 describes a coating composition based on
polyethylene which has a bimodal molar mass distribution. This
coating composition is very suitable for producing external
sheathing for energy and information transmission cables,
CONFIRMATION COPY

CA 02583386 2007-04-05
WO 2006/053740 PCT/EP2005/012305
2
which give the cables sheathed therewith improved durability
in respect of corrosion, in respect of oxidative aging, in
respect of weathering influences of all types and in respect
of mechanical stresses.
Known polyethylene molding compositions having a unimodal
molar mass distribution have disadvantages in terms of their
processability, their environmental stress cracking resistance
and their mechanical toughness. Compared to these, molding
compositions having a bimodal molar mass distribution
represent a technical improvement. They are easier to process
and at the same density have an improved environmental stress
cracking resistance and a higher mechanical strength.
It was thus an object of the present invention to develop a
polyethylene molding composition which retains good
processability but when used as cable sheathing displays
significant advantages in respect of environmental stress
cracking resistance, resistance to mechanical stresses and
improved abrasion behavior for simpler laying and relatively
low water vapor permeation and oxygen permeation.
This object is achieved by a molding composition of the
generic type mentioned at the outset whose distinguishing
features are that it comprises from 45 to 55% by weight of a
low molecular weight ethylene homopolymer A, from 30 to 40% by
weight of a high molecular weight copolymer B of ethylene and
another olefin having from 4 to 8 carbon atoms and from 10 to
20% by weight of an ultra high molecular weight ethylene
copolymer C, where all percentages are based on the total
weight of the molding composition.
The invention further provides a process for preparing this
molding composition in a cascaded suspension polymerization
and a defect-free external sheathing of energy and information

CA 02583386 2007-04-05
WO 2006/053740 PCT/EP2005/012305
3
transmission cables comprising this molding composition and
having excellent mechanical strength properties combined with
high stiffness.
The polyethylene molding composition of the invention has a
density at a temperature of 23 C in the range from 0.94 to
0.950 g/cm3 and a trimodal molar mass distribution. The high
molecular weight copolymer B contains a proportion of further
olefin monomer units having from 4 to 8 carbon atoms, namely
from 1 to 8% by weight. Examples of such comonomers are
1-butene, 1-pentene, 1-hexene, 1-octene and 4-methyl-l-
pentene. The ultra high molecular weight ethylene copolymer C
likewise contains one or more of the abovementioned comonomers
in an amount in the range from 1 to 8% by weight.
Furthermore, the molding composition of the invention has a
melt flow index in accordance.with ISO 1133, expressed as
MFI190/5r in the range from 0.5 to 2.1 dg/min and a viscosity
number VNoverallr measured in accordance with ISO/R 1191 in
decalin at a temperature of 135 C, in the range from 260 to
340 cm3/g, in particular from 280 to 320 cm3/g.
The trimodality as a measure of the position of the centers of
gravity of the three individual molar mass distributions_can
be described with the aid of the viscosity numbers VN in
accordance with ISO/R 1191 of the polymers formed in the
successive polymerization stages. Here, the band widths of the
polymers formed in the individual reaction stages are as
follows:
The viscosity number VN1 measured on the polymer after the
first polymerization stage is identical to the viscosity
number VNA of the low molecular weight polyethylene A and is,
according to the invention, in the range from 50 to 90 cm3/g,
in particular in the range from 60 to 80 cm3/g.

CA 02583386 2007-04-05
WO 2006/053740 PCT/EP2005/012305
4
The viscosity number VN2 measured on the polymer after the
second polymerization stage does not correspond to VNB of the
relatively high molecular weight polyethylene B formed in the
second polymerization stage, but is instead the viscosity
number of the mixture of polymer A plus polymer B. According
to the invention, VN2 is in the range from 260 to 320 cm3/g.
The viscosity number VN3 measured on the polymer after the
third polymerization stage does not correspond to VNc of the
ultra high molecular weight copolymer C formed in the third
polymerization sta.ge, which can likewise be determined only
mathematically, but is instead the viscosity number of the
mixture of the polymer A, polymer B plus polymer C. According
to the invention, VN3 is in the range from 260 to 340 cm3/g, in
particular from 280 to 320 cm3/g.
The polyethylene is obtained by polymerization of the monomers
in suspension at temperatures in the range from 70 to 90 C,
preferably from 75 to 90 C, a pressure in the range from 2 to
10 bar and in the presence of a highly active Ziegler catalyst
composed of a transition metal compound and an organoaluminum
compound. The polymerization is a three-stage polymerization,
i.e. it is carried out in three successive stages, with the
molar mass being regulated in each stage by means of added
hydrogen.
Apart from the polyethylene, the polyethylene molding
composition of the invention can further comprise additional
additives. Such additives are, for example, heat stabilizers,
antioxidants, UV absorbers, light stabilizers, metal
deactivators, peroxide-decomposing compounds, basic
costabilizers, in amounts of from 0 to 10o by weight,
preferably from 0 to 5% by weight, and also carbon black,
fillers, pigments, flame retardants, or combinations of these

CA 02583386 2007-04-05
WO 2006/053740 PCT/EP2005/012305
in total amounts of from 0 to 50% by weight, based on the
total weight of the mixture.
The molding composition of the invention is particularly
5 useful for producing external sheathing of electric cables of
all types, e.g. cables for the transmission of information or
energy. Such cables usually comprise one or more metallic or
nonmetallic conductors which can each be coated with an
insulating layer. The cable sheath has the task of protecting
the cable against damage by external influences, e.g. during
laying, and is preferably applied by extrusion by firstly
plasticizing the polyethylene molding composition in an
extruder at temperatures in the range from 200 to 250 C and
then extruding it through a suitable nozzle onto the cable
surface and cooling it there.
The molding composition of the invention can be processed
particularly well by the extrusion process to produce coatings
and has a notched impact toughness (ISO) in the range from 8
to 14 kJ/m2 and an environmental stress cracking resistance
(ESCR) in the range > 200 h.
The notched impact toughnesslSO is measured at -30 C in
accordance with ISO 179-1/leA / DIN 53453. The dimensions of
the specimen are 10 x 4 x 80 mm, and it is provided with a V-
notch having an angle of 45 , a depth of 2 mm and a radius at
the bottom of the notch of 0.25 mm.
The environmental stress cracking resistance (ESCR) of the
molding composition of the invention is determined by an
internal measurement method and is reported in h. This
laboratory method is described by M. Flei3ner in Kunststoffe
77 (1987), p. 45 ff, and corresponds to ISO/CD 16770 which is
now valid. The publication shows that there is a relationship
between the determination of slow crack growth in a creep test

CA 02583386 2007-04-05
WO 2006/053740 PCT/EP2005/012305
6
on test rods having a circumferential notch and the brittle
branch of the internal pressure test in accordance with
ISO 1167. A shortening of the time to failure is achieved by
shortening the crack initiation time by means of the notch
(1.6 mm/razor blade) in ethylene glycol as medium inducing
environmental stress cracking at a temperature of 80 C and a
tensile stress of 3.5 MPa. The production of the specimens is
carried out by sawing three test specimens having dimensions
of 10 x 10 x 90 mm from a 10 mm thick pressed plate. The test
specimens are in turn notched in the middle by means of a
razor blade in a notching apparatus made in-house for this
purpose (cf. figure 5 in the publication). The notch depth is
1.6 mm.
Example 1
The polymerization of ethylene was carried out in a continuous
process in three reactors connected in series. A Ziegler
catalyst which had been prepared by the method of WO 91/18934,
example 2, and has the operations number 2.2 in the WO in an
amount of 0.08 mmol/h and also sufficient suspension medium
(hexane), triethylaluminum as cocatalyst in an amount of
0.08 mmol/h, ethylene and hydrogen were fed into the first
reactor. The amount of ethylene (= 65 kg/h) and the amount of
hydrogen (= 68 g/h) were set so that a proportion of from 25
to 26% by volume ethylene and a proportion of 65% by volume of
hydrogen were measured in the gas space of the first reactor;
the remainder was a mixture of nitrogen and vaporized
suspension medium.
The polymerization in the first reactor was carried out at a
temperature of 84 C.
The suspension from the first reactor was then passed to a
second reactor in which the proportion of hydrogen in the gas

CA 02583386 2007-04-05
WO 2006/053740 PCT/EP2005/012305
7
space had been reduced to 7 - 9% by volume and into which an
amount of 48.1 kg/h of ethylene plus an amount of 2940 g/h of
1-butene were introduced. The reduction in the amount of
hydrogen was achieved by means of H2 intermediate
depressurization. 73% by volume of ethylene, 8% by volume of
hydrogen and 0.82% by volume of 1-butene were measured in the
gas space of the second reactor; the remainder was a mixture
of nitrogen and vaporized suspension medium.
The polymerization in the second reactor was carried out at a
temperature of 80 C.
The suspension from the second reactor was passed via a
further H2 intermediate depressurization, by means of which the
amount of hydrogen in the gas space in the third reactor was
set to 2.5% by volume, into the third reactor.
An amount of 16.9 kg/h of ethylene plus an amount of 1500 g/h
of 1-butene were introduced into the third reactor. A
proportion of ethylene of 87% by volume, a proportion of
hydrogen of 2.5% by volume and a proportion of 1-butene of
1.2% by volume were measured in the gas space of the third
reactor; the remainder was a mixture of nitrogen and vaporized
suspension medium.
The polymerization in-the third reactor was carried out at a
temperature of 80 C.
The long-term activity of the polymerization catalyst
necessary for the above-described cascaded mode of operation
was ensured by a specially developed Ziegler catalyst having
the composition reported in the abovementioned WO document. A
measure of the usability of this catalyst is its extremely
high response to hydrogen and its high activity which remains
constant over a long period of from 1 to 8 hours.

CA 02583386 2007-04-05
WO 2006/053740 PCT/EP2005/012305
8
The suspension medium is separated off from the polymer
suspension leaving the third reactor, the powder is dried and
the powder is passed to pelletization.
The viscosity numbers and the proportions WA, WB and WC of
polymers A, B and C for the PE molding composition prepared as
described in example 1 are shown in table 1 below:
Table 1
Example 1
WA [% by weight] 50
WB [% by weight] 37
WC [% by weight] 13
VN1 [cm3/g] 80
VN2 [cm3/g] 280
VNoveral.i [cm3/g] 304
FNCT [h] 220
AFM (-30 C) 3.8 kJ/m2
ACN (+23 C) 13 kJ/m2
The abbreviations for the physical properties in table 1 have
the following meaning:
- FNCT = environmental stress cracking resistance (Full
Notch Creep Test) measured by the internal measurement
method described by M. Fleil3ner in [h], conditions: 95 C,
3.5 MPa, water / 2% of Arkopal.

CA 02583386 2007-04-05
WO 2006/053740 PCT/EP2005/012305
9
- AFM (-300C) = notched impact toughness, measured in
accordance with ISO 179-1/leA / DIN 53453 in [kJ/m2] at
-30 C.
- ACN (+23 C) = notched impact toughness, measured in
accordance with ISO 179-1/leA / DIN 53453 in [kJ/m2] at
+23 C.
An energy cable having a diameter of 5 cm was sheathed
externally with the polyethylene molding composition prepared
in this way by plasticizing the molding composition at a
temperature of 220 C in an extruder and then extruding it
through an annular nozzle onto the electric cable and cooling
it there. The sheath produced in this way had a thickness of
0.5 cm.
The resulting surface on the electric cable was smooth and
displayed no visible damage.
The electric cable produced in this way was, for test
= purposes, packed in a steel mesh basket and stored in the
River Main in Frankfurt at a depth of 2 m below the water
surface. The duration of the storage was 1 year, and the water
temperature varied, depending on the time of year, from + 3 to
+ 27 C.
After a storage time of one year, the cable was taken out
again and examined visually. After mechanical removal of
adhering mud and algae, the appearance of the external
sheathing of the cable was no different from the state
immediately after it had been produced.
* ~ * * ~

Dessin représentatif

Désolé, le dessin représentatif concernant le document de brevet no 2583386 est introuvable.

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Historique d'événement

Description Date
Demande non rétablie avant l'échéance 2010-11-17
Le délai pour l'annulation est expiré 2010-11-17
Réputée abandonnée - omission de répondre à un avis sur les taxes pour le maintien en état 2009-11-17
Lettre envoyée 2007-08-28
Inactive : Transfert individuel 2007-07-13
Inactive : Déclaration des droits - Formalités 2007-06-28
Inactive : Lettre pour demande PCT incomplète 2007-06-12
Inactive : Page couverture publiée 2007-06-08
Inactive : Notice - Entrée phase nat. - Pas de RE 2007-06-06
Inactive : CIB en 1re position 2007-05-02
Demande reçue - PCT 2007-05-01
Exigences pour l'entrée dans la phase nationale - jugée conforme 2007-04-05
Demande publiée (accessible au public) 2006-05-26

Historique d'abandonnement

Date d'abandonnement Raison Date de rétablissement
2009-11-17

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Historique des taxes

Type de taxes Anniversaire Échéance Date payée
Taxe nationale de base - générale 2007-04-05
Enregistrement d'un document 2007-07-13
TM (demande, 2e anniv.) - générale 02 2007-11-19 2007-11-02
TM (demande, 3e anniv.) - générale 03 2008-11-17 2008-11-04
Titulaires au dossier

Les titulaires actuels et antérieures au dossier sont affichés en ordre alphabétique.

Titulaires actuels au dossier
BASELL POLYOLEFINE GMBH
Titulaires antérieures au dossier
HEINZ VOGT
JOACHIM BERTHOLD
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Description du
Document 
Date
(aaaa-mm-jj) 
Nombre de pages   Taille de l'image (Ko) 
Description 2007-04-05 9 391
Revendications 2007-04-05 3 104
Abrégé 2007-04-05 1 63
Page couverture 2007-06-08 1 37
Avis d'entree dans la phase nationale 2007-06-06 1 195
Rappel de taxe de maintien due 2007-07-18 1 113
Courtoisie - Certificat d'enregistrement (document(s) connexe(s)) 2007-08-28 1 129
Courtoisie - Lettre d'abandon (taxe de maintien en état) 2010-01-12 1 174
Rappel - requête d'examen 2010-07-20 1 120
PCT 2007-04-05 3 106
Correspondance 2007-06-06 1 17
Correspondance 2007-06-28 3 58