Title of Invention

PIPE MADE OF POLYETHYLENE COMPOSITION AND PROCESS OF MANUFACTURE THEREFOR

Abstract According to the invention there is provided a pipe made of polyethylene composition comprising a polyethylene base resin, which comprises a. a copolymer of ethylene and C4 to C20 alpha-olefin comonomers as fraction (A), and b. an ethylene copolymer and an alpha-olefin comonomer with 4 or more carbon atoms as fraction (B),with fraction (A) having a lower molecular weight than fraction (B), wherein the polyethylene base resin is obtained by a polymerization process in which fraction (A) and fraction (B) are polymerised in the presence of the same single-site catalyst (SSC), the base resin having: (i) a density of below 940 kg/ m3, and (ii) a MFR5 at 190° C/5.00 kg of at least 0.20 g/10 min, wherein the polyethylene composition has a time to failure of at least 250 h at 95°C and 4.3 MPa. in which the polyethylene base resin has an SHI 2.7/210 of below 20; and the comonomer content of fraction (A) is between 0.1 and 3.0 mol % and the comonomer content of fraction (B) is between 0.1 and 2.0 mol %. There is also provided a process for manufacture of the pipe.
Full Text

Pipe having Improved High Temperature Resistance
The present invention relates to a pipe with improved high temperature
resistance made of a polyethylene composition comprising a polyethylene
resin produced by a polymerisation process in the presence of a single-site
catalyst (SSC), and to a process for the production of such a pipe.
Pipes, in particular pressure pipes, are used in various applications like the
transport of drinking water, sewage, different industrial applications, gas
and more.
Based on the polymer strength, polyethylene pipes for pressurised systems
can be classified in different categories, such as PE63, PE80 or PE100. The
higher the number, the longer the service life under high pressure.
However, polyethylene has a limited pressure resistance at elevated
temperature. Especially, it is difficult to combine good pressure resistance
at higher temperatures with a high flexibility of the piping materials.
The classic tool to improve the pressure resistance of a pipe at elevated
temperature is to cross-link the material. However, the inferior purity of
cross-linked resins can be an obstacle for their use in pipes which are in
contact with drinking water and/or food. Furthermore, the recycling of
cross-linked material is difficult. Thus, thermoplastic solutions would be
preferred if the technical performance, such as pressure resistance at
elevated temperatures, can be sufficiently improved. Many attempts to
design such materials have been made.
Presently, the best polyethylene pressure pipes are prepared in a multistage
process with Ziegler-Natta catalysts. The densities of such polyethylene
resins are high in order to reach a high pressure resistance. However, high

density gives a high stiffness, which is a drawback e.g. when installing the
pipes.
There has also been an intensive research on polyolefin resins produced
with metallocene or "single-site" catalysts, but still the introduction of such
resin into the market is low. The main areas where single site resins have
been introduced are film or extrusion coating, as disclosed e.g. in WO
03/066699. The films disclosed in this document have excellent mechanical
properties and outstanding sealability.
However, it is known that the catalytic activity of single-site catalysts is
moderate and the highest activity is reached in the medium to low density
regions.
Furthermore, pressure pipe resins prepared by single-site catalysts of the
state of the art, as described e.g. in WO 02/34829, have traditionally a
density higher than 940 kg/m3. The consequence is that the flexibility of
the pipes is rather low.
Still further, for the production of pressure pipes it is necessary that the
polyethylene compositions used have a suitable melt flow rate and
molecular weight distribution, in order to ensure a good processability of
the composition during the extrusion process.
Hence, the object of the present invention is to provide a pipe having
improved pressure resistance at elevated temperature by simultaneously
improving the flexibility of the pipe.
It has now surprisingly been found that such a pipe can be produced by
using a polyethylene composition comprising a base resin which has been
produced using a single site catalyst, which has a density below 940 kg/m3
and a MFR5 of at least 0.2 g/10min.

Therefore, the present invention provides a pipe made of a polyethylene
composition comprising a polyethylene base resin, which comprises
a. an ethylene copolymer as fraction (A), and
b. an ethylene homo- or copolymer as fraction (B),
with fraction (A) having a lower molecular weight than fraction (B),
wherein the polyethylene base resin is obtainable in a polymerisation
process in which a single-site catalyst (SSC) is used in the polymerisation
of at least one of fractions (A) and (B), the base resin having
(i) a density of below 940 kg/m3,
and
(ii) a MFR5 at 190 °C / 5.00 kg of at least 0.20 g/10 min, and
the polyethylene composition having a time to failure of at least 250 h
measured according to ISO 1167 at 95°C and 4.3 MPa.
As demonstrated below, the invention enables preparation of more flexible
pipes still meeting the requirements for high pressure resistance at elevated
temperatures.
Hence, for example, the enhanced flexibility of the pipes of the invention
allow for an easier bending thereof and thus an easier coiling into a roll.
This offers the advantage that installing the pipes is much simplified.
The term "base resin" denotes the entirety of polymeric components in the
polyethylene composition of the pipe according to the invention, usually
making up at least 90 wt% of the total composition. Preferably, the base
resin is consisting of fractions (A) and (B), optionally further comprising a
prepolymer fraction in an amount of up to 20 wt%, preferably up to 10
wt%, more preferably up to 5 wt% of the total base resin.

The density of the base resin, lies in the medium range, i.e. below 940
kg/m3, preferably below 939 kg/m3, more preferably in the range of 910 to
below 940 kg/m3, even more preferably in the range of 915 to below 940
kg/m3, and most preferably in the range of 920 to below 939 kg/m3,
measured according to ISO 1183.
Despite a 5 to 10 kg/m3 units lower density of the base resin compared to
conventional resins, the pipes of the invention fulfill high temperature
requirements.
The melt flow rate (MFR) and the flow rate ratio (FRR) are important
properties of the polyethylene base resin, because MFR and FRR are
indications of the flowability and thus processability of the polymer. The
higher the melt flow rate, the lower the viscosity of the polymer.
In the present invention the polyethylene base resin should have an MFR5
of at least 0.20 g/10 min, preferably of at least 0.5 g/10 min, and most
preferably of at least 1.3 g/10 min. The MFR5 of the polyethylene base
resin is usually below 7.0 g/10 min, more preferably is 3.5 g/10min or
lower, and most preferably is 1.5 g/10min or lower.
Furthermore, it is preferred that the polyethylene base resin has an MFR2
from 0.06 to 10 g/10 min, more preferred from 0.1 to 5.0 g/10 min, still
more preferred from 0.1 to 1.0 g/10 min, and most preferred from 0.1 to 0.5
g/10 min.
Moreover, for pipe applications a good processability of the polyethylene
composition is important. High molecular weight is needed for meeting the
requirement of good pressure resistance at elevated temperatures and low
creep, however, processing of such high molecular weight resins is more
difficult. Improved processability is reached by the multimodal design of

the base resin. This means at least one lower molecular weight fraction (A)
giving easier processability and one fraction with a higher molecular
weight (B) contributing to mechanical strength, are present in the
composition used for pipes of the invention.
Usually, a polyethylene composition comprising at least two polyethylene
fractions, which have been produced under different polymerisation
conditions resulting in different (weight average) molecular weights for the
fractions, is referred to a "multimodal". The prefix "multi" relates to the
number of different polymer fractions the composition is consisting of.
Thus, for example, a composition consisting of two fractions only is called
"bimodal".
The form of the molecular weight distribution curve, i.e. the appearance of
the graph of the polymer weight fraction as function of its molecular
weight, of such a multimodal polyethylene will show two or more maxima
or will at least be distinctly broadened in comparison with the curves for
the individual fractions.
For example, if a polymer is produced in a sequential multistage process,
utilising reactors coupled in series and using different conditions in each
reactor, the polymer fractions produced in different reactors will each have
their own molecular weight distribution and weight average molecular
weight. When the molecular weight distribution curve of such a polymer is
recorded, the individual curves from these fractions are superimposed into
the molecular weight distribution curve for total resulting polymer product,
usually yielding a curve with two or more distinct maxima.
The polyethylene base resin of the present invention is a multimodal-, or
more preferred a bimodal, polyethylene base resin, comprising fractions

(A) and (B) as defined above, wherein fraction (A) has a lower molecular,
weight than fraction (B).
In the preferred embodiment in which the base resins consists of fractions
(A) and (B), optionally a prepolymer fraction in an amount as defined
above may be present.
The term'molecular weight where used herein denotes the weight average
molecular weight Mw.
The polyethylene base resin of the present invention preferably has a
molecular weight distribution (MWD) of 5 to 25, more preferably of 5 to
20, and most preferably of 5 to 15.
It is preferred that ethylene copolymer (A) has a density of below 945
kg/m3, more preferably below 940 kg/m3. The preferred density range for
ethylene copolymer (A) is from 920 to below 945 kg/m3, more preferred
from 925 to below 940 kg/m3.
Furthermore, in the present invention fraction (A) is an ethylene copolymer
and fraction (B) can be an ethylene homo- or copolymer. However, it is
preferred that fraction (B) is an ethylene copolymer.
The used comonomers of both fractions maybe equal or different.
As comonomers various alpha-olefins with C4 to C2o carbon atoms may be
used, but the comonomers are preferably a C4-C20 alkene selected from the
group of 1-butene, 1-pentene, 4-methyl- 1-pentene, 1-hexene, 1-heptene, 1-
octene, 1-decene and 1-eicosene. In particular preferred embodiment, the
comonomeris 1-butene and/or 1-hexene.

The polyethylene base resin of the present invention may also comprise a
terpolymer, which means that at least on of the fractions (A) and (B)
consists of ethylene and two different comonomer units.
Preferably, fraction (B) is an ethylene copolymer, and the comonomer used
is an alpha-olefin with 4, more preferably 6, or more carbon atoms, more
preferably is 1-hexene or 1-octene.
The amount of the comonomer used in fraction (A) preferably is between
0.1 to 3.0 mol-%, more preferably 0.2 to 2.0 mol-%, even more preferably
0.5 to 1.5mol-%.
The amount of the comonomer used in fraction (B) preferably is between
0.1 to 2.0 mol-%, more preferably 0.1 to 1.5 mol-%, even more preferably
0.2 to 1.0 mol-%.
Moreover, the melt flow rate MFR2 (190°C/2.16 kg) of fraction (A)
preferably is between 10 to 300 g/10 min, more preferably between 10 to
200 g/10 min, and most preferably between 50 to 140 g/10 min.
It is previously known that in order to produce multimodal, in particular
bimodal, olefin polymers, such as the polyethylene base resin of the present
invention, two or more reactors or zones connected in series as described in
EP 517 868, which is hereby incorporated by way of reference in its
entirety, can be used.
According to the present invention, the main polymerisation stages are
preferably carried out as a combination of slurry polymerisation/gas-phase
polymerisation. The slurry polymerisation is preferably performed in a so-
called loop reactor.

Optionally and advantageously, the main polymerisation stages may be
preceded by a pre-polymerisation, in which case a prepolymer in the
amount as described above, most preferably in an amount of 1 to 5% by
weight of the total amount of polymers is produced. The pre-polymer may
be an ethylene homo- or copolymer.
If a pre-polymerisation takes place, in this case all of the catalyst is
preferably charged into the first prepolymerisation reactor and the pre-
polymerisation is performed as slurry polymerisation. Such a polymeri-
sation leads to less fine particles being produced in the following reactors
and to a more homogeneous product being obtained in the end. Generally,
this technique results in a multimodal polymer mixture through
polymerisation with the aid of a catalyst, in the present invention with the
aid of a single site catalyst.
The single-site catalyst used in the examples of the present invention has
been disclosed in EP 1 462 464, example 5, catalyst 3.
In the process of the invention for producing the base resin of the polymer
composition of the invention, at least fraction (A) or fraction (B) are
produced in a polymerisation reaction in the presence of a single-site
catalyst. For example, fraction (A), or alternatively (B), may be produced
in the presence of a single-site catalyst and fraction (B), or alternatively
(A), may be produced in the presence of a Ziegler-Natta catalyst.
It is, however, preferred that both fractions (A) and (B) are prepared in the
presence of a single-site catalyst.
Furthermore, it is preferred that fraction (A) and fraction (B) are
polymerised in the presence of the same single-site catalyst.

In the production of a polyethylene base resin of the present invention it is
preferred that fraction (A) is produced in a loop reactor under certain
conditions with respect to hydrogen, monomer and comonomer
concentration, temperature, pressure, and so forth.
Furthermore, it is preferred that fraction (B) is produced in a gas-phase
reactor.
Still further, preferably, after the polymerisation fraction (A) including the
catalyst is transferred to the reactor, preferably a gas-phase reactor, where
fraction (B) is produced under different conditions.
The resulting end product consists of an intimate mixture of the polymers
from the two main reactors, the different molecular-weight-distribution
curves of these polymers together forming a molecular-weight-distribution
curve having a broad maximum or two maxima, i.e. the end product is a
bimodal polymer mixture.
Owing to the flexibility with respect to reaction conditions thus obtained, it
is most preferred that the polymerization is carried out in a pre-
polymerization reactor/a loop reactor/ a gas-phase reactor. Preferably, the
polymerization conditions in the preferred three-step method are chosen so
that fraction (A) is produced in one step, preferably the second reactor,
whereas fraction (B) is produced in another step, preferably the third
reactor. The order of these steps may, however, be reversed.
In the present invention it is preferred that the pre-polymerisation operates
at a temperature between 40 to 70 °C, more preferred between 50 to 65 °C
and preferably at a pressure of 50 to 70 bar, more preferably of 55 to 65
bar.

In the second reactor the polymerisation temperature is preferably between
60 to 100 °C, more preferably between 70 to 90 °C, and preferably at a
pressure of 40 to 70 bar, more preferably of 50 to 60 bar.
In the third reactor the temperature is preferably between 60 to 105 °C,
more preferably between 70 and 90 °C and preferably at a pressure of
10 to 40 bar, more preferably of 15 to 20 bar.
The weight ratio between both fractions (A) and (B) produced in the second
and third reactor is preferably from 60 : 40 to 40 : 60, more preferably from
55 : 45 to 45 : 55.
The polyethylene composition the pipe of the invention is made of may
also comprise additives like process aids, antioxidants, pigments, UV-
stabilizers and the like. Usually, the amount at those additives is 10 wt% or
lower, based on the total composition.
The pipe of the present invention may be prepared in any conventional
manner, preferably by extrusion of the polyolefin composition in an
extruder. This is a technique well known to the person skilled in the art.
The pipe of the present invention shows good stress resistance as well as a
high flexibility.
The shear thinning index (SHI) is the ratio of the viscosity of the
polyethylene base resin at different shear stresses and may serve as a
measure of the broadness of the molecular weight distribution. In the
present invention, the shear stresses at 2.7 kPa and 210 kPa as well as 5
kPa and 300 kPa are used for the determination of SHI of the polyethylene
base resin. The definition and measurement conditions are described in
detail on page 8, line 29 to page 11, line 25 of WO 00/22040.

The polyethylene base resin has preferably an SHIp^jo) of below 20, more
preferably of below 15, and most preferably of below 10. It is preferred the
range of SHI(2.7/2io) is from 1 to below 20.
It is also preferred that the SHI(5/3oo) is below 35, more preferred below 30
and most preferred below 25. The preferred range of the SHI(5/3oo> is
between 5 to below 35.
Additionally, the viscosity at shear stress of 0.05 kPa (etao.05) of tne
polyethylene base resin is preferably at least 15,000 Pa s , more preferably
at least 18,000 Pa s, and most preferably at least 20,000 Pa s.
Furthermore, the viscosity at shear stress of 0.05 kPa (etao.05) of the
polyethylene base resin is preferably less than 80,000 Pa s.
The Charpy impact test at low temperature assesses impact toughness and
therefore provides a way to evaluate resistance to rapid crack propagation
(RCP).
In the preferred embodiment of the present invention the polyethylene
composition of the pipe has a Charpy impact strength at 0°C of at least 8
kJ/m2, most preferably of at least 10 kJ/m2, measured according to ISO 179.
The rapid crack propagation resistance of the polyethylene composition
according to the present invention is determined by a method called S4
(Small Scale Steady State), which has been developed at Imperial College,
London, and is described in ISO 13477:1977 (E). The pipes of the present
invention preferably reach a critical temperature, i.e. RCP-S4 value, of
+ 2°C or lower, more preferably of+lqC or lower.

The slow crack propagation resistance is determined according to ISO
13479:1997 in terms of the number of hours the notched pipe withstands a
certain pressure at a certain temperature before failure.
Additionally, the time to failure of the polyethylene composition at 95 °C
and 4.3 MPa according to ISO 1167 preferably is at least 250 h, more
preferably at least 300 h, most preferably at least 350 h. .
The fiexural modulus of the polyethylene composition is preferably below
700 MPa, more preferably below 650 MPa, and most preferably below 600
MPa, measured according to ISO 178. It is preferred that the fiexural
modulus of the polyethylene composition is 300 MPa or higher, more
preferably is 400 MPa or higher.
The modulus of elasticity of the pipe of the present invention has been
determined according to ISO 527. The polymer composition according to
the present invention has preferably a modulus of elasticity from 400 to
900 MPa, more preferably from 425 to 850 MPa and most preferably from
450 to 800 MPa.
Methods and Examples
Melt flow rate (MFR)
The MFR is determined according to ISO 1133 and is indicated in g/10min.
For polyethylene resins, a temperature of 190 °C is applied. The MFR is
determined at different loadings such as 2.16 kg (MFR2; ISO 1133), 5 kg
(MFR5; ISO 1133) or 21.6 kg MFR21 (ISO 1133). The flow rate ratio, FRR
is the ratio between MFRweighti and MFRweight2, i.e. FRR21/5 means the ratio
between MFR2] and MFR5.

Molecular weight
The weight average molecular weight Mw and the molecular weight
distribution (MWD = Mw/Mn, wherein MB is the number average molecular
weight and Mw is the weight average molecular weight) is measured by
based on ISO 1014-4:2003. A Waters 150CV plus instrument was used with
column 3 x HT&E styragel from Waters (divinylbenzene) and
trichlorobenzene (TCB) as solvent at 140 °C. The column set was
calibrated using universal calibration with narrow MWD PS standards (the
Mark Rowings constant K: 9.54 *10"s and a: 0.725 for PS, and K: 3.92 *
10"4 and a: 0.725 for PE). The ratio of Mw and Mn is a measure of the
broadness of the distribution, since each is influenced by opposite end of
the "population".
Rapid crack propagation (S4)
The rapid crack propagation (RCP) resistance of a pipe is determined
according to ISO 13477 (E). According to the RCP-S4 method a pipe is
tested which has an axial length not below 7 pipe diameters. The outer
diameter of the pipe is about 110 mm or greater and its wall thickness
about 10 mm or greater. When determining the RCP properties of a pipe in
connection with the present invention the outer diameter and the wall
thickness have been selected to be 110 mm and 10 mm respectively. While
the exterior of the pipe is at ambient pressure (atmospheric pressure), the
pipe is pressurized internally and the internal pressure in the pipe is kept
constant at a pressure of 0.5 MPa positive pressure. The pipe and the
equipment surrounding it are thermostated to a predetermined temperature.
A number of discs have been mounted on a shaft inside the pipe to prevent
decompression during the test. A knife projectile is shot, with well-defined
forms, towards the pipe close to its end in the so-called initiating zone in

order to start a rapidly running axial crack. The initiating zone is provided
with an abutment for avoiding unnecessary deformation to the pipe. The
test equipment is adjusted in such a manner that crack initiation takes place
in the material involved and a number of tests are effected at varying
temperatures. The axial crack length in the measuring zone, having a total
length of 4.5 diameters, is measured for each test and is plotted against the
set test temperature. If the crack length exceeds 4 diameters the crack is
assessed to propagate. If the pipe passes the test at a given temperature, the
temperature is lowered successively until a temperature (TCntjcai) is reached,
at which the pipe no longer passes the test.
Pressure test on un-notched pipes
The pressure test on un-notched 32 mm pipes is carried out according to
ISO 1167 3 at 4.3 MPa and 95 °C. The time to failure is determined in
hours.
Pressure test on notched pipes
The pressure test on notched 110 mm pipes is carried out according to ISO
13479.
Charpy Notch impact test
The impact strength is determined as Charpy Impact Strength according to
ISO 179-1 non-instrumented or IS0179-2 instrumented.
Flexural modulus
The flexural modulus is determined according to ISO 178 at a constant
speed of 2 mm/min.

E-modulus
The modulus of elasticity is determined according to ISO 527-2 (test
speciniel?. IB), at a constant speed of 1 mm/min.
Rheological parameters
Rheological parameters such as Shear Thinning Index SHI and viscosity are
determined by using a rheometer, preferably a Physica MCR 300
Rheometer from Anton Paar. The definition and measurement conditions
are described in detail on page 8, line 29 to page 11, line 25 of WO
00/22040.
Examples
Example I
Into a 50 dm3 loop reactor 32 kg/h propane and 8.3 g/h hydrogen were
added. The operating temperature was 60°C and operating pressure 61 bar.
The slurry was taken out of the reactor and transferred into a 500 dm3 loop
reactor. The reactor was operated at 85 °C and 58 bar. pressure. The single
site catalyst prepared as disclosed in EP 1 462 464, Example 5, catalyst 3
was continuously fed at a rate of 29 g/min into the loop reactor. Additional
ethylene, 1-butene, propane diluent and hydrogen were continuously
introduced into the reactor so that the rate of polymer production was 35
kg/h and the MFR2 of the polymer was 110 g/10min and the density of
polymer was 939 kg/m3.
The slurry was continuously withdrawn from the reactor to a flash stage
where hydrocarbons were removed from the polymer. The polymer was
then transferred into a gas phase reactor where the polymerisation was
continued. The reactor was operated at 80°C temperature and 20 bar

pressure. Ethylene, hydrogen and 1-hexene were fed into the reactor to
obtain such conditions that the rate of polymer production was 34 kg/h,
MFR5 of the polymer was 1.4 g/10min, MFR2 of the polymer was
0.45 g/10min and the density 936 kg/m3. The productivity of the catalyst
was 2.4 kg/g catalyst.
The ratio between polymer amounts produced in the slurry (reactor 2) and
gas phase (reactor 3) reactors was 51:49.
The polymer was then compounded in with 1500 ppm Calcium stearate and
3000 ppm B225. The properties of the compounded resin are given in Table
1, where also the reaction conditions for the production of the base resin
are shown.
The compounded material was extruded into pipes having an external
diameter of about 110 mm and thickness of about 10 mm and 32 mm' and a
thickness of 3 mm respectively. The pressure test result of the pipe is given
in Table 1.
Comparative Example 1
A pipe resin was produced by means of a three-step process in a pre-
polymerisation loop-reactor followed by first a loop-reactor and then a gas
phase-reactor, as described in Example 1. The split was 2:38:60. No
comonomer was used in the prepolymerisation reactor, while 1-butene was
used as comonomer in the production of the low and of the high molecular
weight fraction produced in the loop and gas-phase reactor, respectively, in
the amounts as indicated in Table 1 such that the 1-butene comonomer
content of the total resulting polymer was 2.9 % by weight. A Ziegler-Natta
type catalyst as disclosed in EP 688 794 was used. The properties of the
resin are listed in Table 1.

The base resin produced was compounded in the same ways as in Example
1 and the compounded material was then extruded into pipes having an
external diameter of about 110 mm and thickness of about 10 mm and a
diameter of 32 mm and a thickness of 3 mm respectively. The result of the
pressure testing is also given in Table 1.





WE CLAIM:
1. A pipe made of polyethylene composition comprising a polyethylene base resin,
which comprises:
a. a copolymer of ethylene and C4 to C20 alpha-olefin comonomers as fraction (A),
and
b. an ethylene copolymer and an alpha-olefin comonomer with 4 or more carbon
atoms as fraction (B),
with fraction (A) having a lower molecular weight than fraction (B), wherein the
polyethylene base resin is obtained by a polymerization process in which fraction (A) and
fraction (B) are polymerised in the presence of the same single-site catalyst (SSC), the
base resin having:
(i) a density ofbelow 940 kg/ m3, and
(ii) a MFRs at 190° C/5.00 kg of at least 0.20 g/10 min,
wherein the polyethylene composition has a time to failure of at least 250 h at
95°C and 4.3 MPa,
in which the polyethylene base resin has an SHI 2.7/210 of below 20; and
the comonomer content of fraction (A) is between 0.1 and 3.0 mol % and the
comonomer content of fraction (B) is between 0.1 and 2.0 mol %.
2. The pipe as claimed in claim 1, wherein the ethylene copolymer (A) has a density
below 945 kg/ m3
3. The pipe as claimed in claim 1, wherein fraction (A) has a melt flow rate MFR2 of
10 to 300 g/10 min.

4. The pipe as claimed in claim 1. wherein in the base polyethylene resin the weight
ratio between fraction (A) and fraction (B) is between 60 :40 to 40: 60.
5. The pipe as claimed in claim 1. wherein the molecular weight distribution
(MWD) of the polyethylene base resin is from 5 to 25.
6. The pipe as claimed in claim 1, wherein the SHI(5/300) is below 35.
7. The pipe as claimed in claim 1, wherein the viscosity of the polyethylene base
resin at a shear rate of 0.05 kPa (eta 0.05) is at least 15,000 kPa.
8. The pipe as claimed in claim 1, wherein the polyethylene composition has a
Charpy impact strength at O°C of at least 8 kJ/m5
9. The pipe as claimed in claim 1, wherein the polyethylene composition has an
RCP-S4 value of+2°C or lower.
10. The pipe as claimed in claim 1, wherein the polyethylene composition has a
modulus of elasticity from 400 to 900 Mpa.
11. A process for the manufacturing of a pipe, wherein a polyethylene composition
comprising a polyethylene base resin, which comprises:
a. a copolymer of ethylene and C4 to C20 alpha-olefin comonomers
as fraction (A), and
b. an ethylene copolymer and an alpha-olefin comonomer with 4 or
more carbon atoms as fraction (B),

with fraction (A) having a lower molecular weight than fraction (B), wherein the
polyethylene base resin is obtainable in a polymerisation process in which a single-site
catalyst (SSC) is used in the polymerisation of at least one of fractions (A) and (B), the
base resin having:
(i) a density of below 940 kg/ m3, and
(ii) a MFR5 at 190°C /5.00 kg of at least 0.20 g/10 min, and
the polyethylene composition having a time to failure of at least 250 h at 95°C
and 4.3 MPa,
the SHI (2.7/210) of the polyethylene base resin is below 20; and
the comonomer content of fraction (A) is between 0.1 and 3.0 mol % and the
comonomer content of fraction (B) is between 0.1 and 2.0 mol %:
is formed into a pipe.
12. The process as claimed in claim 11, wherein the fraction (A) and fraction (B) are
polymerised in the presence of the same single site catalyst.



ABSTRACT


PIPE MADE OF POLYETHYLENE COMPOSITION AND
PROCESS OF MANUFACTURE THERE FOR
According to the invention there is provided a pipe made of polyethylene
composition comprising a polyethylene base resin, which comprises a. a copolymer of
ethylene and C4 to C20 alpha-olefin comonomers as fraction (A), and b. an ethylene
copolymer and an alpha-olefin comonomer with 4 or more carbon atoms as fraction
(B),with fraction (A) having a lower molecular weight than fraction (B), wherein the
polyethylene base resin is obtained by a polymerization process in which fraction (A)
and fraction (B) are polymerised in the presence of the same single-site catalyst (SSC),
the base resin having: (i) a density of below 940 kg/ m3, and (ii) a MFR5 at 190° C/5.00
kg of at least 0.20 g/10 min, wherein the polyethylene composition has a time to failure
of at least 250 h at 95°C and 4.3 MPa. in which the polyethylene base resin has an SHI
2.7/210 of below 20; and the comonomer content of fraction (A) is between 0.1 and 3.0
mol % and the comonomer content of fraction (B) is between 0.1 and 2.0 mol %.
There is also provided a process for manufacture of the pipe.

Documents:

1776-KOLNP-2009-(03-01-2014)-ABSTRACT.pdf

1776-KOLNP-2009-(03-01-2014)-ANNEXURE TO FORM 3.pdf

1776-KOLNP-2009-(03-01-2014)-CLAIMS.pdf

1776-KOLNP-2009-(03-01-2014)-CORRESPONDENCE.pdf

1776-KOLNP-2009-(03-01-2014)-FORM-1.pdf

1776-KOLNP-2009-(03-01-2014)-FORM-2.pdf

1776-KOLNP-2009-(03-01-2014)-OTHERS.pdf

1776-KOLNP-2009-(03-01-2014)-PETITION UNDER RULE 137.pdf

1776-KOLNP-2009-(19-04-2013)-CORRESPONDENCE.pdf

1776-kolnp-2009-abstract.pdf

1776-KOLNP-2009-ASSIGNMENT.pdf

1776-KOLNP-2009-CANCELLED PAGES.pdf

1776-kolnp-2009-claims.pdf

1776-kolnp-2009-correspondence.pdf

1776-kolnp-2009-description (complete).pdf

1776-KOLNP-2009-EXAMINATION REPORT.pdf

1776-kolnp-2009-form 1.pdf

1776-KOLNP-2009-FORM 18.pdf

1776-kolnp-2009-form 3.pdf

1776-kolnp-2009-form 5.pdf

1776-kolnp-2009-gpa.pdf

1776-KOLNP-2009-GRANTED-ABSTRACT.pdf

1776-KOLNP-2009-GRANTED-CLAIMS.pdf

1776-KOLNP-2009-GRANTED-DESCRIPTION (COMPLETE).pdf

1776-KOLNP-2009-GRANTED-FORM 1.pdf

1776-KOLNP-2009-GRANTED-FORM 2.pdf

1776-KOLNP-2009-GRANTED-FORM 3.pdf

1776-KOLNP-2009-GRANTED-FORM 5.pdf

1776-KOLNP-2009-GRANTED-SPECIFICATION-COMPLETE.pdf

1776-kolnp-2009-international preliminary examination report.pdf

1776-kolnp-2009-international publication.pdf

1776-KOLNP-2009-INTERNATIONAL SEARCH REPORT & OTHERS.pdf

1776-kolnp-2009-others.pdf

1776-kolnp-2009-pct priority document notification.pdf

1776-kolnp-2009-pct request form.pdf

1776-KOLNP-2009-PETITION UNDER RULE 137.pdf

1776-KOLNP-2009-REPLY TO EXAMINATION REPORT.pdf

1776-kolnp-2009-specification.pdf

1776-KOLNP-2009-TRANSLATED COPY OF PRIORITY DOCUMENT.pdf


Patent Number 262647
Indian Patent Application Number 1776/KOLNP/2009
PG Journal Number 36/2014
Publication Date 05-Sep-2014
Grant Date 02-Sep-2014
Date of Filing 12-May-2009
Name of Patentee BOREALIS TECHNOLOGY OY
Applicant Address P.O. BOX 330, FIN-06101 PORVOO
Inventors:
# Inventor's Name Inventor's Address
1 PALMLÖF, MAGNUS MÅRDGATAN, 23, S-426 71 VÄSTRA FRÖLUNDA
2 VAHTERI, MARKKU TAPANI LÖFVINGINKATU 2-4 B 9, FIN-06100 PORVOO
3 JOHANSSON, SLOVEIG HAGLINGEVÄGEN 1, S-444 47 STENUNGSUND
PCT International Classification Number C08L 23/06,F16L 9/12
PCT International Application Number PCT/EP2007/010093
PCT International Filing date 2007-11-21
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 06024951.3 2006-12-01 EUROPEAN UNION