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(11) EP 2 877 534 B1


(12) EUROPEAN PATENT SPECIFICATION

(45) Date of publication and mention (51) Int Cl.:


of the grant of the patent: C08L 23/10 (2006.01) C08L 23/12 (2006.01)
10.05.2017 Bulletin 2017/19 C08F 255/02 (2006.01) C08L 23/14 (2006.01)

(21) Application number: 13739222.1 (86) International application number:


PCT/EP2013/065262
(22) Date of filing: 19.07.2013
(87) International publication number:
WO 2014/016205 (30.01.2014 Gazette 2014/05)

(54) FOAM PRODUCED FROM POLYPROPYLENE WITH LOW GEL CONTENT


AUS POLYPROPYLEN MIT GERINGEM GELANTEIL HERGESTELLTER SCHAUM
MOUSSE PRODUITE À PARTIR DE POLYPROPYLÈNE AYANT UNE FAIBLE TENEUR EN GEL

(84) Designated Contracting States: • BRAUN, Hermann


AL AT BE BG CH CY CZ DE DK EE ES FI FR GB A-4020 Linz (AT)
GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO
PL PT RO RS SE SI SK SM TR (74) Representative: Maiwald Patentanwalts GmbH
Elisenhof
(30) Priority: 25.07.2012 EP 12177879 Elisenstrasse 3
80335 München (DE)
(43) Date of publication of application:
03.06.2015 Bulletin 2015/23 (56) References cited:
EP-A1- 2 000 504 EP-A1- 2 492 293
(73) Proprietor: Borealis AG WO-A1-2011/141070 US-A- 6 077 907
1220 Vienna (AT) US-A1- 2007 004 861 US-A1- 2010 047 544
US-A1- 2010 063 212
(72) Inventors:
• PROKSCHI, Hermann
A-4231 Wartberg ob der Aist (AT)
EP 2 877 534 B1

Note: Within nine months of the publication of the mention of the grant of the European patent in the European Patent
Bulletin, any person may give notice to the European Patent Office of opposition to that patent, in accordance with the
Implementing Regulations. Notice of opposition shall not be deemed to have been filed until the opposition fee has been
paid. (Art. 99(1) European Patent Convention).

Printed by Jouve, 75001 PARIS (FR)


EP 2 877 534 B1

Description

[0001] The present invention relates to a method of providing a polypropylene composition having high melt strength
and a low gel content. Furthermore, the present invention also relates to a corresponding high melt strength (HMS)
5 polypropylene composition with low gel content as well as to the manufacture of a foam based on the polypropylene
composition with high melt strength and low gel content.
[0002] High melt strength polypropylene (HMS-PP) compositions are generally known in the art. However, one chal-
lenge within existing HMS-PP is their varying foam quality. The foam quality is increased in case the gel content of the
used high melt strength polypropylene is low.
10 [0003] Further, as known in the art, additives are normally added to plastic materials in order to improve the performance
thereof. Examples of typical additives are e.g. antioxidants or pigments. These additives are often added to the plastic
base material in the form of an additive mixture having incorporated the additives into a small amount of polymer powder.
The additive mixture is sometimes also referred to as masterbatch. The small quantity of polymer powder used for the
additive mixture is normally dosed at the end of the HMS process. However, the contribution to the final gel content of
15 this additive mixture is often overlooked. Further up to now it has been not recognized that also the molecular weight of
the base polymer powder in the manufacture of the high melt strength polypropylene (HMS-PP) has significant impact
on the final foam properties.
[0004] EP 0 879 830, filed by Borealis in 1997, describes the basics of the Borealis high melt strength (HMS) post-
reactor process where peroxide and butadiene are used to make long chain branched polypropylene (LCB-PP) materials.
20 This patent covers a wide range of powder melt flow rates (MFRs) and particle sizes. However, it does not specify the
impact of the type of base polymer as well as the polypropylene powder used for the preparation of the additive mixture
on the HMS quality in particular on the foam quality based on the gel content in the high melt strength polypropylene.
[0005] There remains a need in the art for a method to produce high melt strength polypropylene (HMS-PP) of reliable
and/or improved quality.
25 [0006] Accordingly the object of the present invention is to provide a process which enables a skilled person to produce
a polypropylene composition and a foam made of said polypropylene composition with low gel content.
[0007] The present inventors now surprisingly found that the final gel content can be significantly reduced by increasing
the MFR of the base polymer.
[0008] Thus, the present invention relates to a process for providing a polypropylene composition comprising a
30 branched polypropylene (b-PP), the process comprises at least a step (a) in which a polypropylene (PP) is reacted with
a thermally decomposing free radical-forming agent and optionally with bifunctionally unsaturated monomer(s) and/or
with multifunctionally unsaturated low molecular weight polymer(s) obtaining thereby the branched polypropylene (b-PP),
wherein

35 (a) the polypropylene (PP) has a melt flow rate MFR2 (230°C) of more than 0.5 g/10 min;

(b) the polypropylene composition and/or the branched polypropylene (b-PP) has/have a F30 melt strength of more
than 20.0 cN and a v30 melt extensibility of more than 200 mm/s, wherein the F30 melt strength and the v30 melt
extensibility are measured according to ISO 16790:2005 and the polypropylene is used in the form of particles
40
having a particle size distribution d90 of below 1,500 mm, d50 of below 1,000 mm and a d90/d50 ratio of below 1.80.
[0009] The present invention further provides a polypropylene composition comprising

(a) 95 to 99 parts by weight of a branched polypropylene (b-PP); and


45
(b) optionally 1 to 5 parts by weight of a polypropylene (PP’) having a melt flow rate MFR2 (230°C) measured
according to ISO 1133 of more than 0.5 to 18.0 g/10 min,

wherein the polypropylene composition has


50
- a melt flow rate MFR 2(230 °C) measured according to ISO 1133 of 1.0 to below 7.0 g/10min, and
- a gel content of less than 1.00 wt.-%, preferably below 0.80 wt.-%;

and wherein the polypropylene composition and/or the branched polypropylene (b-PP) has/have a F30 melt strength of
55 25.0 cN to 50.0 cN and a v30 melt extensibility of 210 to 300 mm/s, wherein the F30 melt strength and the v30 melt
extensibility are measured according to ISO 16790:2005.
[0010] The present invention further relates to a process for the manufacture of a foam comprising

2
EP 2 877 534 B1

(A) the process for providing of a polypropylene composition comprising a branched polypropylene (b-PP), the
process comprises at least a step (a) in which a polypropylene (PP) is reacted with a thermally decomposing free
radical-forming agent and optionally with bifunctionally unsaturated monomer(s) and/or with multifunctionally un-
saturated low molecular weight polymer(s) obtaining thereby the branched polypropylene (b-PP),
5 wherein

(i) the polypropylene (PP) has a melt flow rate MFR2 (230°C) of more than 0.5 g/10min;
(ii) the polypropylene composition and/or the branched polypropylene (b-PP) has/have a F30 melt strength of
more than 20.0 cN and a v30 melt extensibility of more than 200 mm/s, wherein the F30 melt strength and the
10 v30 melt extensibility are measured according to ISO 16790:2005,

(B) subjecting the polypropylene composition of step (A) to a foaming process obtaining thereby a foam.

[0011] Additionally the present invention is directed to a process for the manufacture of a foam comprising the step
15 of subjecting a polypropylene composition to a foaming process obtaining thereby a foam, wherein the polypropylene
composition comprises

(a) 95 to 99 parts by weight of a branched polypropylene (b-PP); and


(b) optionally 1 to 5 parts by weight of a polypropylene (PP’) having a melt flow rate MFR 2 (230 °C) measured
20 according to ISO 1133 of more than 0.5 to 18.0 g/10min,

wherein the polypropylene composition has

- a melt flow rate MFR2 (230 °C) measured according to ISO 1133 of 1.0 to below 7.0 g/10min, and
25 - a gel content of less than 1.00 wt.-%, preferably below 0.80 wt.-%;

and wherein the polypropylene composition and/or the branched polypropylene (b-PP) has/have a F30 melt strength of
25.0 cN to 50.0 cN and a v30 melt extensibility of 210 to 300 mm/s, wherein the F30 melt strength and the v30 melt
extensibility are measured according to ISO 16790:2005.
30 [0012] Additionally the invention is directed to the use of a polypropylene (PP) having a melt flow rate MFR2 (230°C)
of more than 0.5 g/10min in the manufacture of a branched polypropylene (b-PP) and thus in the manufacture of a
polypropylene composition comprising the branched polypropylene (b-PP) to reduce the gel content of the branched
polypropylene (b-PP) and/or of the polypropylene composition comprising the branched polypropylene (b-PP). Preferably
the gel content is reduced in case the branched polypropylene (b-PP) and/or the polypropylene composition comprising
35 the branched polypropylene (b-PP) has/have a gel content of less than 1.00 wt.-%, preferably of less than 0.80 wt.-%.
[0013] In the following the invention is described in more detail.
[0014] First the individual components, i.e. the polypropylene (PP), like the linear polypropylene (1-PP’), the polypro-
pylene (PP’), like the linear polypropylene (1-PP’), the branched polypropylene (b-PP), and the additives (A), used in
the instant invention as well as the polypropylene composition are described. Subsequently the claimed processes are
40 described in more detail as well as the foam and the use of the polypropylene (PP). However any information or any
preferred embodiment provided for the individual components or the polypropylene composition is also applicable for
the inventive processes and for the inventive use, if reference is made to the individual components and the polypropylene
composition, respectively.

45 The branched polypropylene (b-PP)

[0015] The major component for the polypropylene composition to be provided according to the invention is a branched
polypropylene (b-PP). A branched polypropylene differs from a linear polypropylene that the polypropylene backbone
covers side chains whereas a non-branched polypropylene, i.e. a linear polypropylene, does not cover side chains. The
50 side chains have significant impact on the rheology of the polypropylene. Accordingly linear polypropylenes and branched
polypropylenes can be clearly distinguished by its flow behavior under stress.
[0016] Branching can be achieved by using specific catalysts, i.e. specific single-site catalysts, or by chemical modi-
fication. Concerning the preparation of a branched polypropylene obtained by the use of a specific catalyst reference is
made to EP 1 892 264. With regard to a branched polypropylene obtained by chemical modification it is referred to EP
55 0 879 830 A1. In such a case the branched polypropylene is also called high melt strength polypropylene. The branched
polypropylene (b-PP) according to the instant invention is obtained by chemical modification as described in more detail
below and thus is a high melt strength polypropylene (HMS-PP). Therefore the terms "branched polypropylene (b-PP)"
and "high melt strength polypropylene (HMS-PP)" can be regarded in the instant invention as synonyms.

3
EP 2 877 534 B1

[0017] Therefore the branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-PP), as the major
component of the polypropylene composition has a F30 melt strength of more than 20.0 cN and a v30 melt extensibility
of more than 200 mm/s, preferably has a F30 melt strength of more than 20.0 to 50.0 cN and a v30 melt extensibility of
more than 200 to 300 mm/s, in order to provide a resulting polypropylene composition with good shear thinning properties.
5 The F30 melt strength and the v30 melt extensibility are measured according to ISO 16790:2005.
[0018] Typically the instant polypropylene composition also has a F30 melt strength of more than 20.0 cN and a v30
melt extensibility of more than 200 mm/s, preferably has a F30 melt strength of more than 20.0 to 50.0 cN and a v30 melt
extensibility of more than 200 to 300 mm/s.
[0019] In a preferred embodiment, the branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-
10 PP), has

(a) a F30 melt strength of more than 20.0 cN, like of more than 20.0 to 50.0 cN, more preferably of more than 21.0
cN, still more preferably of 21.0 to 50.0 cN, yet more preferably of 25.0 to 50.0 cN, still yet more preferably of 25.0
to 45.0 cN, most preferably of 30.0 to 45.0 cN, like of 32.0 to 42.0 cN;
15 and
(b) a v30 melt extensibility of more than 210 to 300 mm/s, like of more than 220 to 300 mm/s, more preferably of
more than 225 mm/s, still more preferably of 225 to 300 mm/s, yet more preferably of 230 to 290 mm/s.

[0020] In especially preferred embodiment the branched polypropylene (b-PP), i.e. the high melt strength polypropylene
20 (HMS-PP), has a F30 melt strength of more than 20.0 cN and a v30 melt extensibility of more than 210 to 300 mm/s, like
a F30 melt strength of more than 20.0 to 50.0 cN and v30 melt extensibility of more than 220 to 300 mm/s, more preferably
a F30 melt strength of more than 21.0 cN and v30 melt extensibility of more than 225 mm/s, still more preferably a F30
melt strength of 21.0 to 50.0 cN and v30 melt extensibility of 225 to 300 mm/s, yet more preferably a F30 melt strength
of 25.0 to 50.0 cN and v30 melt extensibility of 230 to 290 mm/s, still yet more preferably a F30 melt strength of 25.0 to
25 45.0 cN and v30 melt extensibility of 230 to 290 mm/s, most preferably a F30 melt strength of 30.0 to 45.0 cN and v30
melt extensibility of 230 to 290 mm/s, like a F30 melt strength of 32.0 to 42.0 cN and v30 melt extensibility of 230 to 290 mm/s.
[0021] Further it is preferred that said branched polypropylene (b-PP), preferably the high melt strength polypropylene
(HMS-PP), has a melt flow rate MFR 2 (230 °C) measured according to ISO 1133 of not more than 7.0 g/10min, more
preferably in a range of 0.5 to 7.0 g/10 min, still more preferably in a range of 0.5 to 6.0 g/10 min, yet more preferably
30 in a range of 1.0 to 6.0 g/10 min, like in the range of 1.5 to 5.0 g/10min or like in the range of 1.0 to 5.0 g/10min.
[0022] Hence in one specific embodiment, the branched polypropylene (b-PP), i.e. the high melt strength polypropylene
(HMS-PP), has

(a) a melt flow rate MFR2 (230 °C) not more than 7.0 g/10min, preferably in a range of 0.5 to 7.0 g/10 min, more
35 preferably in a range of 0.5 to 6.5 g/10 min, still more preferably in a range of 0.5 to 6.0 g/10 min, yet more preferably
in a range of 1.0 to 6.0 g/10 min, like in the range of 1.5 to 5.0 g/10min or like in the range of 1.0 to 5.0 g/10min;
(b) a F30 melt strength of more than 20.0 cN, like of more than 20.0 to 50.0 cN, more preferably of more than 21.0
cN, still more preferably of 21.0 to 50.0 cN, yet more preferably of 25.0 to 50.0 cN, still yet more preferably of 25.0
to 45.0 cN, most preferably of 30.0 to 45.0 cN, like of 32.0 to 42.0 cN; and
40 (c) a v30 melt extensibility of more than 210 to 300 mm/s, like of more than 220 to 300 mm/s, more preferably of
more than 225 mm/s, still more preferably of 225 to 300 mm/s, yet more preferably of 230 to 290 mm/s.

[0023] Accordingly in specific embodiment the branched polypropylene (b-PP), i.e. the high melt strength polypropylene
(HMS-PP), has a melt flow rate MFR2 (230 °C) of not more than 7.0 g/10min, a F30 melt strength of more than 20.0 cN
45 and a v30 melt extensibility of more than 210 to 300 mm/s, like a melt flow rate MFR2 (230 °C) in a range of 0.5 to 7.0
g/10 min, a F30 melt strength of more than 20.0 to 50.0 cN and v30 melt extensibility of more than 220 to 300 mm/s,
more preferably a melt flow rate MFR2 (230 °C) in a range of 0.5 to 6.0 g/10 min, a F30 melt strength of more than 21.0
cN and v30 melt extensibility of more than 225 mm/s, still more preferably a melt flow rate MFR2 (230 °C) in a range of
1.0 to 6.0 g/10 min, a F30 melt strength of 21.0 to 50.0 cN and v30 melt extensibility of 225 to 300 mm/s, yet more
50 preferably a melt flow rate MFR2 (230 °C) in a range of 1.0 to 6.0 g/10min, a F30 melt strength of 25.0 to 50.0 cN and
v30 melt extensibility of 230 to 290 mm/s, still yet more preferably a melt flow rate MFR2 (230 °C) in a range of 1.0 to
5.0 g/10min, a F30 melt strength of 25.0 to 45.0 cN and v30 melt extensibility of 230 to 290 mm/s, most preferably a melt
flow rate MFR2 (230 °C) in a range of 1.0 to 5.0 g/10min, a F30 melt strength of 30.0 to 45.0 cN and v30 melt extensibility
of 230 to 290 mm/s, like a melt flow rate MFR2 (230 °C) in a range of 1.0 to 5.0 g/10min, a F30 melt strength of 32.0 to
55 42.0 cN and v30 melt extensibility of 230 to 290 mm/s.
[0024] Preferably, the branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-PP), has a
melting point of at least 130°C, more preferably of at least 135°C and most preferably of at least 140°C. The crystallization
temperature is preferably at least 110 °C, more preferably at least 120 °C.

4
EP 2 877 534 B1

[0025] Further, the branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-PP), can be a
branched random propylene copolymer (b-R-PP), i.e. a high melt strength random propylene copolymer (R-HMS-PP),
or a branched propylene homopolymer (b-H-PP), i.e. a high melt strength propylene homopolymer (H-HMS-PP), the
latter being preferred.
5 [0026] For the purpose of the present invention, the expression "propylene homopolymer" refers to a polypropylene
that consists substantially, i.e. of at least 97 mol.-%, preferably of at least 98 mol.-%, more preferably of at least 99 mol.-
%, most preferably of at least 99.8 mol.-% of propylene units. In a preferred embodiment only propylene units in the
propylene homopolymer are detectable.
[0027] In case the branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-PP), is a branched
10 random propylene copolymer (b-R-PP), i.e. a high melt strength random propylene copolymer (R-HMS-PP), it comprises
monomers copolymerizable with propylene, for example comonomers such as ethylene and/or C4 to C12 α-olefins, in
particular ethylene and/or C4 to C10 α-olefins, e.g. 1-butene and/or 1-hexene. Preferably the branched random propylene
copolymer (b-R-PP), i.e. the high melt strength random propylene copolymer (R-HMS-PP), comprises, especially consists
of, monomers copolymerizable with propylene from the group consisting of ethylene, 1-butene and 1-hexene. More
15 specifically the branched random propylene copolymer (b-R-PP), i.e. the high melt strength random propylene copolymer
(R-HMS-PP), comprises - apart from propylene - units derivable from ethylene and/or 1-butene. In a preferred embodiment
the branched random propylene copolymer (b-R-PP), i.e. the high melt strength random propylene copolymer (R-HMS-
PP), comprises units derivable from ethylene and propylene only. The comonomer content in the branched random
propylene copolymer (b-R-PP), i.e. in the high melt strength random propylene copolymer (R-HMS-PP), is preferably in
20 the range of more than 0.2 to 10.0 mol.-%, still more preferably in the range of more than 0.5 to 7.0 mol.-%.
[0028] In this regard it is to mention that the high melt strength polypropylene (HMS-PP) being either a high melt
strength propylene homopolymer (H-HMS-PP) or a high melt strength random propylene copolymer (R-HMS-PP) may
comprise additionally unsaturated monomers different to the comonomers defined for the high melt strength random
propylene copolymer (R-HMS-PP). In other words the high melt strength propylene homopolymer (H-HMS-PP) or the
25 high melt strength random propylene copolymer (R-HMS-PP) may comprise unsaturated units, like bifunctionally un-
saturated monomer(s) and/or multifunctionally unsaturated low molecular weight polymer(s) as defined in detail below,
being different to propylene, ethylene and other C 4 to C12 α-olefins. Accordingly the definition of homopolymer and
copolymer in view of the high melt strength polypropylene (HMS-PP) refers actually to the unmodified polypropylene,
i.e. to the polypropylene (PP), preferably to the linear polypropylene (1-PP), used to obtain the melt strength polypropylene
30 (HMS-PP) by chemical modification as defined in detail below.
[0029] Accordingly in one preferred embodiment the branched polypropylene (b-PP), i.e. the high melt strength poly-
propylene (HMS-PP), comprises

(a) if it is a high melt strength propylene homopolymer (H-HMS-PP) units derived from
35
(i) propylene and
(ii) bifunctionally unsaturated monomer(s) and/or multifunctionally unsaturated low molecular weight polymer(s),

or
40 (b) if it is a high melt strength random propylene copolymer (R-HMS-PP) units derived from

(i) propylene
(ii) ethylene and/or C4 to C10 α-olefins, e.g. 1-butene and/or 1-hexene, preferably erthylene, and
(iii) bifunctionally unsaturated monomer(s) and/or multifunctionally unsaturated low molecular weight polymer(s),
45
[0030] "Bifunctionally unsaturated" or "multifunctionally unsaturated" as used above means preferably the presence
of two or more non-aromatic double bonds, as in e.g. divinylbenzene or cyclopentadiene or polybutadiene. Only such
bi- or multifunctionally unsaturated compounds are used which can be polymerized preferably with the aid of free radicals
(see below). The unsaturated sites in the bi- or multifunctionally unsaturated compounds are in their chemically bound
50 state not actually "unsaturated", because the double bonds are each used for a covalent bond to the polymer chains of
the unmodified polypropylene, i.e. of the polypropylene (PP), preferably of the linear polypropylene (1-PP).
[0031] Reaction of the bifunctionally unsaturated monomer(s) and/or multifunctionally unsaturated low molecular
weight polymer(s), preferably having a number average molecular weight (Mn) ≤ 10000 g/mol, synthesized from one
and/or more unsaturated monomers with the unmodified polypropylene, i.e. with the polypropylene (PP), preferably with
55 the linear polypropylene (1-PP), are performed in the presence of a thermally free radical forming agent, e. g. decomposing
free radical-forming agent, like a thermally decomposable peroxide.
[0032] The bifunctionally unsaturated monomers may be

5
EP 2 877 534 B1

- divinyl compounds, such as divinylaniline, m-divinylbenzene, p-divinylbenzene, divinylpentane and divinylpropane;


- allyl compounds, such as allyl acrylate, allyl methacrylate, allyl methyl maleate and allyl vinyl ether;
- dienes, such as 1,3-butadiene, chloroprene, cyclohexadiene, cyclopentadiene, 2,3-dimethylbutadiene, heptadiene,
hexadiene, isoprene and 1,4-pentadiene;
5 - aromatic and/or aliphatic bis (maleimide) bis (citraconimide) and mixtures of these unsaturated monomers.

[0033] Especially preferred bifunctionally unsaturated monomers are 1,3-butadiene, isoprene, dimethyl butadiene and
divinylbenzene.
[0034] The multifunctionally unsaturated low molecular weight polymer, preferably having a number average molecular
10 weight (Mn) ≤ 10000 g/mol may be synthesized from one or more unsaturated monomers.
[0035] Examples of such low molecular weight polymers are

- polybutadienes, especially where the different microstructures in the polymer chain, i.e. 1,4-cis, 1,4-trans and 1,2-(vi-
nyl) are predominantly in the 1,2-(vinyl) configuration
15 - copolymers of butadiene and styrene having 1,2- (vinyl) in the polymer chain.

[0036] A preferred low molecular weight polymer is polybutadiene, in particular a polybutadiene having more than
50.0 wt.-% of the butadiene in the 1,2-(vinyl) configuration.
[0037] The branched polypropylene, i.e. the high melt strength polypropylene (HMS-PP), may contain more than one
20 bifunctionally unsaturated monomer and/or multifunctionally unsaturated low molecular weight polymer. Even more
preferred the amount of bifunctionally unsaturated monomer(s) and multifunctionally unsaturated low molecular weight
polymer(s) together in the branched polypropylene, i.e. in the high melt strength polypropylene (HMS-PP), is 0.01 to
10.0 wt.-% based on said branched polypropylene, i.e. based on said high melt strength polypropylene (HMS-PP).
[0038] In a preferred embodiment the branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-
25 PP), is free of additives (A). Accordingly in case the instant polypropylene composition comprises additives (A), these
additives (A) are not brought in the polypropylene composition during the manufacture of the branched polypropylene
(b-PP), i.e. of the high melt strength polypropylene (HMS-PP).

The polypropylene (PP)


30
[0039] As mentioned above, the branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-PP),
is a modified polypropylene, which is obtained by reacting the polypropylene (PP) with a thermally decomposing free
radical-forming agent and optionally with bifunctionally unsaturated monomer(s) and/or with multifunctionally unsaturated
low molecular weight polymer(s).
35 [0040] Essential aspect of the invention is that a specific unmodified polypropylene must be used in the present
invention for the manufacture of the branched polypropylene (b-PP), i.e. of the high melt strength polypropylene (HMS-
PP), and thus for the manufacture of the polypropylene composition comprising the branched polypropylene (b-PP), i.e.
comprising the high melt strength polypropylene (HMS-PP). A particular finding is that the polypropylene (PP), preferably
the linear polypropylene (1-PP), must have a rather low molecular weight and thus a rather high melt flow rate. Accordingly
40 it is preferred that the polypropylene (PP), preferably the linear polypropylene (1-PP), has a melt flow rate MFR2 (230°C)
measured according to ISO 1133 of more than 0.5 g/10min, preferably in the range of more than 0.5 to 18.0 g/10min,
like of more than 0.5 to 15.0 g/10min or of more than 0.6 to 15.0 g/10min, more preferably of more than 0.5 to below
10.0 g/10min, still more preferably of more than 0.6 to 9.0 g/10min, yet more preferably of 0.8 to 8.0 g/10min.
[0041] In one specific example the polypropylene (PP), preferably the linear polypropylene (1-PP), has a melt flow
45 rate MFR2 (230°C) measured according to ISO 1133 of more than 0.5 g/10min, preferably in the range of more than 0.5
to 18.0 g/10min, like of more than 0.5 to 15.0 g/10min or of more than 0.6 to 15.0 g/10min, more preferably of more than
0.5 to below 10.0 g/10min, still more preferably of more than 0.6 to 9.0 g/10min, yet more preferably of 0.8 to 8.0 g/10min,
with the proviso that the values of 1.0 g/10min, 10.0 g/10min and 45.0 g/10min are excluded.
[0042] The branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-PP), differs from the poly-
50 propylene (PP) which is used for its manufacture that the backbone of the branched polypropylene (b-PP), i.e. of the
high melt strength polypropylene (HMS-PP), covers side chains whereas the staring product, i.e. the polypropylene (PP),
does not cover or nearby does not cover side chains. The side chains have significant impact on the rheology of the
polypropylene. Accordingly staring product, i.e. the polypropylene (PP), and the obtained branched polypropylene (b-
PP), i.e. the high melt strength polypropylene (HMS-PP), can be clearly distinguished by its flow behavior under stress.
55 [0043] Further, as mentioned above the polypropylene (PP) is preferably a linear polypropylene (1-PP). The same
considerations apply to the polypropylene (PP’) as discussed in detail below which is also in a preferred embodiment a
linear polypropylene (1-PP’). Accordingly, throughout the instant invention, the term "linear polypropylene" indicates that
the linear polypropylene, shows no or nearby no-branching structure. Due to the absence of branches, the linear poly-

6
EP 2 877 534 B1

propylenes, i.e. the linear polypropylene (1-PP) and the linear polypropylene (1-PP’), are preferably featured by a low
v30 melt extensibility and/or a low F30 melt strength.
[0044] Thus it is preferred that the linear polypropylene (1-PP) has

5 (a) a F30 melt strength of more than 1.0 cN, preferably of more than 2.0 cN, more preferably in the range of 1.0 to
below 68.0 cN, still more preferably in the range of 1.5 to 65.0 cN, yet more preferably in the range of 2.0 to 60.0
cN, still yet more preferably in the range of 2.5 to 50.0 cN like in the range of 2.5 to 45.0 cN;
and
(b) a v30 melt extensibility of below 200 mm/s, preferably of below 190 mm/s, more preferably in the range of 100
10 to below 200 mm/s, still more preferably in the range of 120 to 190 mm/s, yet more preferably in the range of 120
to 175 mm/s, like in the range of 125 to 170 mm/s.

[0045] In other words it is preferred that the linear polypropylene (1-PP) has a F30 melt strength of more than 1.0 cN
and a v30 melt extensibility of below 200 mm/s, preferably a F30 melt strength of more than 2.0 cN and a v30 melt
15 extensibility of below 190 mm/s, more preferably a F30 melt strength in the range of 1.0 to below 68.0 cN and a v30 melt
extensibility in the range of 100 to below 200 mm/s, yet more preferably a F30 melt strength in the range of 1.5 to 65.0
cN and in the range of 120 to 190 mm/s, still yet more preferably a F30 melt strength in the range of 2.0 to 60.0 cN and
in the range of 120 to 190 mm/s, like a F30 melt strength in the range of 2.5 to 50.0 cN and a v30 melt extensibility in the
range of 120 to 175 mm/s.
20 [0046] Accordingly in one specific embodiment the linear polypropylene (1-PP) has

(a) a melt flow rate MFR2 (230 °C) measured according to ISO of more than 0.5 g/10min, preferably in the range of
more than 0.5 to 18.0 g/10min, like of more than 0.5 to 15.0 g/10min or of more than 0.6 to 15.0 g/10min, more
preferably of more than 0.5 to below 10.0 g/10min, still more preferably of more than 0.6 to 9.0 g/10min, yet more
25 preferably of 0.8 to 8.0 g/10min;
(b) a F30 melt strength of more than 1.0 cN, preferably of more than 2.0 cN, more preferably in the range of 1.0 to
below 68.0 cN, still more preferably in the range of 1.5 to 65.0 cN, yet more preferably in the range of 2.0 to 60.0
cN, still yet more preferably in the range of 2.5 to 50.0 cN like in the range of 2.5 to 45.0 cN; and
(c) a v30 melt extensibility of below 200 mm/s, preferably of below 190 mm/s, more preferably in the range of 100
30 to below 200 mm/s, still more preferably in the range of 120 to 190 mm/s, yet more preferably in the range of 120
to 175 mm/s, like in the range of 125 to 170 mm/s.

[0047] Therefore, in one specific embodiment the polypropylene (PP) is a linear polypropylene (1-PP) having a melt
flow rate MFR2 (230 °C) of more than 0.5 g/10min, a F30 melt strength of more than 1.0 cN and a v30 melt extensibility
35 of below 200 mm/s, preferably a melt flow rate MFR2 (230 °C) in the range of more than 0.5 to 18.0 g/10min, a F30 melt
strength of more than 2.0 cN and a v30 melt extensibility of below 190 mm/s, more preferably a melt flow rate MFR2 (230
°C) in the range of more 0.6 to 15.0 g/10min, a F30 melt strength in the range of 1.0 to 68.0 cN and a v30 melt extensibility
in the range of 100 to below 200 mm/s, yet more preferably a melt flow rate MFR2 (230 °C) in the range of more 0.5 to
10.0 g/10min a F30 melt strength in the range of 2.0 to 60.0 cN and in the range of 120 to 190 mm/s, still yet more
40 preferably a melt flow rate MFR2 (230 °C) in the range of more 0.6 to 9.0 g/10min, a F30 melt strength in the range of
2.5 to 50.0 cN and in the range of 120 to 190 mm/s, like a melt flow rate MFR2 (230 °C) in the range of more 0.8 to 8.0
g/10min a F30 melt strength in the range of 2.5 to 45.0 cN and a v30 melt extensibility in the range of 120 to 175 mm/s.
[0048] Preferably, the polypropylene (PP), preferably the linear polypropylene (1-PP), has a melting point of at least
140°C, more preferably of at least 150°C and still more preferably of at least 158°C.
45 [0049] Additionally it is preferred that the polypropylene (PP), preferably the linear polypropylene (1-PP), is used in
form of particles of specific size. Accordingly it is preferred that the polypropylene (PP), preferably the linear polypropylene
(1-PP), has

(a) a particle size distribution d90 of below 1,500 mm; more preferably below 1,200 mm, still more preferably in the
50 range of 50 to below 1,200 mm, yet more preferably in the range of 100 to below1,100 mm, like in the range of 150
to below 1,100 mm;
and/or
(b) a particle size distribution d50 of below 1,000 mm; more preferably below 800 mm, still more preferably in the
range of 30 to below 1,000 mm, yet more preferably in the range of 50 to 850 mm, like in the range of 100 to 750 mm;
55 and/or
(c) a d90/d50 ratio of below 1.80, more preferably below 1.75, still more preferably below 1.60, yet more preferably
in the range of 1.00 to 1.75, still yet more preferably in the range of 1.10 to 1.60.

7
EP 2 877 534 B1

[0050] The polypropylene (PP), preferably the linear polypropylene (1-PP), can be produced in a known manner for
instance by employing a single-site or a Ziegler Natta catalyst. The polypropylene (PP), preferably the linear polypropylene
(1-PP), can be a propylene homopolymer (H-PP), preferably a linear propylene homopolymer (1-H-PP), or a propylene
copolymer (R-PP), preferably a linear propylene copolymer (1-R-PP). Concerning the comonomer content and type of
5 comonomer it is referred to the information provided above for the branched polypropylene (b-PP), especially it is referred
to the high melt strength random propylene copolymer (R-HMS-PP). Preferably the polypropylene (PP) is a linear
polypropylene (1-PP). Still more preferably the polypropylene (PP) is a linear propylene homopolymer (1-H-PP). Ac-
cordingly all information provided with regard to melt flow rate MFR2 (230°C), melting point, F30 melt strength, v30 melt
extensibility, and particle size and particle size distribution, respectively, applies especially for the linear propylene
10 homopolymer (1-H-PP).
[0051] In a preferred embodiment the polypropylene (PP), preferably the linear polypropylene (1-PP), is free of additives
(A). Accordingly in case the instant polypropylene composition comprises additives (A), these additives (A) are not
brought in the polypropylene composition during the manufacture of the branched polypropylene (b-PP), i.e. of the high
melt strength polypropylene (HMS-PP).
15
The polypropylene (PP’)

[0052] During the preparation of the instant polypropylene composition a further polypropylene (PP’) may be added.
This polypropylene (PP’) is preferably used to bring additives (A) in the instant polypropylene composition. Accordingly
20 in a preferred embodiment the additives (A) are introduced in the instant polypropylene composition in the form of an
additive mixture (AM), wherein said additive mixture comprises, preferably consists of, the polypropylene (PP’) and the
additives (A).
[0053] Preferably the polypropylene (PP’) is a linear polypropylene (1-PP’).
[0054] More preferably the polypropylene (PP’), i.e. the linear polypropylene (PP’), must have a rather low molecular
25 weight and thus a rather high melt flow rate. Accordingly it is preferred that the polypropylene (PP’), preferably the linear
polypropylene (1-PP’), has a melt flow rate MFR2 (230°C) measured according to ISO 1133 of more than 0.5 g/10min,
preferably in the range of more than 0.5 to 18.0 g/10min, like of more than 0.5 to 15.0 g/10min or of more than 0.6 to
15.0 g/10min, more preferably of more than 0.5 to below 10.0 g/10min, still more preferably of more than 0.6 to 9.0
g/10min, yet more preferably of 0.8 to 8.0 g/10min.
30 [0055] Preferably, the polypropylene (PP’), preferably the linear polypropylene (1-PP’), has a melting point of at least
140°C, more preferably of at least 150°C and still more preferably of at least 158°C.
[0056] Further, as mentioned above the polypropylene (PP’) is preferably a linear polypropylene (1-PP’) and thus
shows no or nearby no-branching structure. Due to the absence of branches the linear polypropylene (1-PP’) is preferably
featured by a low v30 melt extensibility and/or a low F30 melt strength.
35 [0057] Thus it is preferred that the linear polypropylene (1-PP’) has

(b) a F30 melt strength of more than 1.0 cN, preferably of more than 2.0 cN, more preferably in the range of 1.0 to
below 68.0 cN, still more preferably in the range of 1.5 to 65.0 cN, yet more preferably in the range of 2.0 to 60.0
cN, still yet more preferably in the range of 2.5 to 50.0 cN, like in the range of 2.5 to 45.0 cN; and
40 and
(b) a v30 melt extensibility of below 200 mm/s, preferably of below 190 mm/s, more preferably in the range of 100
to below 200 mm/s, still more preferably in the range of 120 to 190 mm/s, yet more preferably in the range of 120
to 175 mm/s, like in the range of 125 to 170 mm/s.

45 [0058] In other words it is preferred that the linear polypropylene (1-PP’) has a F30 melt strength of more than 1.0 cN
and a v30 melt extensibility of below 200 mm/s, preferably a F30 melt strength of more than 2.0 cN and a v30 melt
extensibility of below 190 mm/s, more preferably a F30 melt strength in the range of 1.0 to below 68.0 cN and a v30 melt
extensibility in the range of 100 to below 200 mm/s, yet more preferably a F30 melt strength in the range of 1.5 to 65.0
cN and in the range of 120 to 190 mm/s, still yet more preferably a F30 melt strength in the range of 2.0 to 60.0 cN and
50 in the range of 120 to 190 mm/s, like a F30 melt strength in the range of 2.5 to 50.0 cN and a v30 melt extensibility in the
range of 120 to 175 mm/s.
[0059] Accordingly in one specific embodiment the linear polypropylene (1-PP’) has

(a) a melt flow rate MFR2 (230 °C) measured according to ISO 1133 of more than 0.5 g/10min, preferably in the
55 range of more than 0.5 to 18.0 g/10min, like of more than 0.5 to 15.0 g/10min or of more than 0.6 to 15.0 g/10min,
more preferably of more than 0.5 to below 10.0 g/10min, still more preferably of more than 0.6 to 9.0 g/10min, yet
more preferably of 0.8 to 8.0 g/10min;
(b) a F30 melt strength of more than 1.0 cN, preferably of more than 2.0 cN, more preferably in the range of 1.0 to

8
EP 2 877 534 B1

below 68.0 cN, still more preferably in the range of 1.5 to 65.0 cN, yet more preferably in the range of 2.0 to 60.0
cN, still yet more preferably in the range of 2.5 to 50.0 cN like in the range of 2.5 to 45.0 cN; and
(c) a v30 melt extensibility of below 200 mm/s, preferably of below 190 mm/s, more preferably in the range of 100
to below 200 mm/s, still more preferably in the range of 120 to 190 mm/s, yet more preferably in the range of 120
5 to 175 mm/s, like in the range of 125 to 170 mm/s.

[0060] Therefore, in one specific embodiment the polypropylene (PP’) is a linear polypropylene (1-PP’) having a melt
flow rate MFR2 (230 °C) of more than 0.5 g/10min, a F30 melt strength of more than 1.0 cN and a v30 melt extensibility
of below 200 mm/s, preferably a melt flow rate MFR2 (230 °C) in the range of more than 0.5 to 18.0 g/10min, a F30 melt
10 strength of more than 2.0 cN and a v30 melt extensibility of below 190 mm/s, more preferably a melt flow rate MFR2 (230
°C) in the range of more 0.6 to 15.0 g/10min, a F30 melt strength in the range of 1.0 to 68.0 cN and a v30 melt extensibility
in the range of 100 to below 200 mm/s, yet more preferably a melt flow rate MFR2 (230 °C) in the range of more 0.5 to
10.0 g/10min a F30 melt strength in the range of 2.0 to 60.0 cN and in the range of 120 to 190 mm/s, still yet more
preferably a melt flow rate MFR2 (230 °C) in the range of more 0.6 to 9.0 g/10min, a F30 melt strength in the range of
15 2.5 to 50.0 cN and in the range of 120 to 190 mm/s, like a melt flow rate MFR2 (230 °C) in the range of more 0.8 to 8.0
g/10min a F30 melt strength in the range of 2.5 to 45.0 cN and a v30 melt extensibility in the range of 120 to 175 mm/s.
[0061] Additionally it is preferred that the polypropylene (PP’), preferably the linear polypropylene (1-PP’), is used in
form of particles of specific size. Accordingly it is preferred that the polypropylene (PP’), preferably the linear polypropylene
(1-PP’), has
20
(a) a particle size distribution d90 of below 1,500 mm; more preferably below 1,200 mm, still more preferably in the
range of 50 to below 1,200 mm, yet more preferably in the range of 100 to below1,100 mm, like in the range of 150
to below 1,100 mm;
and/or
25 (b) a particle size distribution d50 of below 1,000 mm; more preferably below 800 mm, still more preferably in the
range of 30 to below 1,000 mm, yet more preferably in the range of 50 to 850 mm, like in the range of 100 to 750 mm;
and/or
(c) a d90/d50 ratio of below 1.80, more preferably below 1.75, still more preferably below 1.60, yet more preferably
in the range of 1.00 to 1.75, still yet more preferably in the range of 1.10 to 1.60
30
[0062] The polypropylene (PP’), preferably the linear polypropylene (1-PP’), can be produced in a known manner for
instance by employing a single-site or a Ziegler Natta catalyst. The polypropylene (PP’), preferably the linear polypro-
pylene (1-PP’), can be a propylene homopolymer (H-PP’), preferably a linear propylene homopolymer (1-H-PP’), or a
propylene copolymer (R-PP’), preferably a linear propylene copolymer (1-R-PP’). Concerning the comonomer content
35 and type of comonomer it is referred to the information provided above for the branched polypropylene (b-PP) especially
it is referred to the high melt strength random propylene copolymer (R-HMS-PP). Preferably the polypropylene (PP’) is
a linear polypropylene (1-PP’). Still more preferably the polypropylene (PP’) is a linear propylene homopolymer (1-H-
PP’). Accordingly all information provided with regard to melt flow rate MFR2 (230°C), melting point, F30 melt strength,
v30 melt extensibility, and particle size and particle size distribution, respectively, applies especially for the linear propylene
40 homopolymer (1-H-PP’).
[0063] In a specific embodiment the polypropylene (PP) and the polypropylene (PP’) are the same. Accordingly in one
preferred embodiment the polypropylene (PP) and the polypropylene (PP’) are linear propylene homopolymers, i.e. a
linear propylene homopolymer (1-H-PP) and a linear propylene homopolymer (1-H-PP’), with the same properties, in
particular in view of melt flow rate MFR2 (230 °C), F30 melt strength and v30 melt extensibility as discussed above.
45 [0064] As mentioned above the polypropylene (PP’) is used as a carrier to introduce the additives (A) in the polypro-
pylene composition. In other words an additive mixture (AM) comprising, preferably consisting of, the polypropylene
(PP’) and the additives (A) is used in the instant process for the manufacture of the polypropylene composition.
[0065] The additives (A) can be any additives useful in the technical area of the high melt strength polypropylene
(HMS-PP) and its applications. Accordingly the additives (A) to be used in the polypropylene composition of the invention
50 and thus in form of the additive mixture (AM) include, but are not limited to, stabilizers such as antioxidants (e.g. sterically
hindered phenols, phosphites/phosphonites, sulphur containing antioxidants, alkyl radikal scavangers, aromatic amines,
hindered amine stabilizers, or blends thereof), metal deactivators (e.g. Irganox MD 1024), or UV stabilizers (e.g. hindered
amine light stabilizers). Other typical additives are modifiers such as antistatic or antifogging agents (e.g. ethoxylated
amines and amides, or glycerol esters), acid scavengers (e.g. Ca-stearate), blowing agents, cling agents (e.g.
55 polyisobutene), lubriciants and resins (ionomer waxes, PE- and ethylene copolymer waxes, Fischer-Tropsch waxes,
Montan-based waxes, Fluoro-based compounds, or paraffin waxes), nucleating agents (e.g. talc, benzoates, phospho-
rous-based compounds, sorbitoles, nonitol-based compounds, or amide-based compounds), as well as slip and anti-
blocking agents (e.g. erucamide, oleamide, talc natural silica and synthetic silica, or zeolites). Preferably the additives

9
EP 2 877 534 B1

(A) are selected from the group consisting of antioxidants (e.g. sterically hindered phenols, phosphites/phosphonites,
sulphur containing antioxidants, alkyl radikyl scavangers, aromatic amines, hindered amine stabilizers, or blends thereof),
metal deactivators (e.g. Irganox MD 1024), or UV stabilizers (e.g. hindered amine light stabilizers), antistatic or antifogging
agents (e.g. ethoxylated amines and amides, or glycerol esters), acid scavengers (e.g. Ca-stearate), blowing agents,
5 cling agents (e.g. polyisobutene), lubriciants and resins (ionomer waxes, PE- and ethylene copolymer waxes, Fischer-
Tropsch waxes, Montan-based waxes, Fluoro-based compounds, or paraffin waxes), nucleating agents (e.g. talc, ben-
zoates, phosphorous-based compounds, sorbitoles, nonitol-based compounds, or amide-based compounds), slip
agents, antiblocking agents (e.g. erucamide, oleamide, talc natural silica and synthetic silica, or zeolites) and mixtures
thereof.
10 [0066] Typically the total amount of additives (A) in the additive mixture (AM) is not more than 25 wt.-%, more preferably
not more than 20 wt.-%, like in the range of 5 to 20 wt.-% based on the total weight of the additive mixture (AM).

The polypropylene composition

15 [0067] As mentioned above due to the instant process a polypropylene composition is obtained which comprises a
branched polypropylene (b-PP), i.e. a high melt strength polypropylene (HMS-PP). In one embodiment the instant
polypropylene composition comprises a branched polypropylene (b-PP), i.e. a high melt strength polypropylene (HMS-
PP), a polypropylene (PP’), preferably a linear polypropylene (1-PP’), and optionally at least one additive (A).
[0068] The major component in the instant polypropylene composition is the branched polypropylene (b-PP), i.e. the
20 high melt strength polypropylene (HMS-PP). Accordingly the polypropylene composition comprises at least 70 wt.-%,
more preferably at least 75 wt.-%, yet more preferably at least 80 wt.-%, still more preferably at least 85 wt.-%, still yet
more preferably at least 90 wt.-%, like at least 95 wt.-%, of the branched polypropylene (b-PP), i.e. the high melt strength
polypropylene (HMS-PP).
[0069] More preferably the instant polypropylene composition comprises
25
(a) 80 to 99 parts by weight, preferably 90 to 99 parts by weight, more preferably 95 to 99 parts by weight, of the
branched polypropylene (b-PP), preferably of the high melt strength polypropylene (HMS-PP); and
(b) optionally 1 to 20 parts by weight, preferably 1 to 10 parts by weight, more preferably 1 to 5 parts by weight, of
polypropylene (PP’), preferably of the linear polypropylene (1-PP).
30
[0070] In a preferred embodiment the branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-
PP), and the polypropylene (PP’), preferably the linear polypropylene (1-PP’), are the only polymer components in the
polypropylene composition. In other words the polypropylene composition may comprise further at least one additive
(A) as defined in more detail above but no other polymers in an amount exceeding 5 wt.-%, more preferably exceeding
35 2 wt.-%, still more preferably exceeding 1 wt.-%, based on the total weight of the polypropylene composition. In a specific
embodiment polypropylene composition consists of the branched polypropylene (b-PP), i.e. the high melt strength poly-
propylene (HMS-PP), the polypropylene (PP’), preferably the linear polypropylene (1-PP’), and at least one additive (A).
[0071] Preferably the total amount of additives (A) in the polypropylene composition is not more than 5.0 wt.-%, more
preferably not more than 1.0 wt.-%, like in the range of 0.005 to 0.5 wt.-%, based on the total weight of the polypropylene
40 composition.
[0072] Therefore the present process is directed to the manufacture of a polypropylene composition comprising

(a) 80 to 99 parts by weight, preferably 90 to 99 parts by weight, more preferably 95 to 99 parts by weight, of the
branched polypropylene (b-PP), i.e. of the high melt strength polypropylene (HMS-PP);
45 (b) optionally 1 to 20 parts by weight, preferably 1 to 10 parts by weight, more preferably 1 to 5 parts by weight, of
polypropylene (PP’), preferably of the linear polypropylene (1-PP’), having a melt flow rate MFR2 (230 °C) measured
according to ISO 1133 of more than 0.5 g/10min, preferably in the range of more than 0.5 to 18.0 g/10min, like of
more than 0.5 to 15.0 g/10min or of more than 0.6 to 15.0 g/10min, more preferably of more than 0.5 to below 10.0
g/10min, still more preferably of more than 0.6 to 9.0 g/10min, yet more preferably of 0.8 to 8.0 g/10min; and
50 (c) optionally 0.005 to 5.0, preferably 0.005 to 2.0, more preferably 0.05 to 1.0, like 0.05 to 0.5, parts by weight of
additives (A), wherein said additives(A) are preferably selected from the group consisting of antioxidants, metal
deactivators, UV-stabilizers, antistatic agents, antifogging agents, acid scavengers, blowing agents, cling agents,
lubricants, nucleating agents, slip agents, antiblocking agents and mixtures thereof.

55 [0073] As mentioned above the branched polypropylene (b-PP), i.e the high melt strength polypropylene (HMS-PP),
is the dominant part in the instant polypropylene composition. Accordingly it is preferred that the final polypropylene
composition shows a similar rheology behavior as the branched polypropylene (b-PP), i.e. the high melt strength poly-
propylene (HMS-PP).

10
EP 2 877 534 B1

[0074] Thus the instant polypropylene composition has

(a) a F30 melt strength of more than 20.0 cN, like of more than 20.0 to 50.0 cN, more preferably of more than 21.0
cN, still more preferably of 21.0 to 50.0 cN, yet more preferably of 25.0 to 50.0 cN, still yet more preferably of 25.0
5 to 45.0 cN, most preferably of 30.0 to 45.0 cN, like of 32.0 to 42.0 cN;
and
(b) a v30 melt extensibility of more than 210 to 300 mm/s, like of more than 220 to 300 mm/s, more preferably of
more than 225 mm/s, still more preferably of 225 to 300 mm/s, yet more preferably of 230 to 290 mm/s.

10 [0075] In especially preferred embodiment the instant polypropylene composition has a F30 melt strength of more than
20.0 cN and a v30 melt extensibility of more than 210 to 300 mm/s, like a F30 melt strength of more than 20.0 to 50.0 cN
and v30 melt extensibility of more than 220 to 300 mm/s, more preferably a F30 melt strength of more than 21.0 cN and
v30 melt extensibility of more than 225 mm/s, still more preferably a F30 melt strength of 21.0 to 50.0 cN and v30 melt
extensibility of 225 to 300 mm/s, yet more preferably a F30 melt strength of 25.0 to 50.0 cN and v30 melt extensibility of
15 230 to 290 mm/s, still yet more preferably a F30 melt strength of 25.0 to 45.0 cN and v30 melt extensibility of 230 to 290
mm/s, most preferably a F30 melt strength of 30.0 to 45.0 cN and v30 melt extensibility of 230 to 290 mm/s, like a F30
melt strength of 32.0 to 42.0 cN and v30 melt extensibility of 230 to 290 mm/s.
[0076] Further it is preferred that the instant polypropylene composition has a melt flow rate MFR2 (230 °C) measured
according to ISO 1133 of not more than 7.0 g/10min, preferably in a range of 0.5 to 7.0 g/10 min, more preferably in a
20 range of 0.5 to 6.5 g/10 min, still more preferably in a range of 0.5 to 6.0 g/10 min, yet more preferably in a range of 1.0
to 6.0 g/10 min, like in the range of 1.5 to 5.0 g/10min or like in the range of 1.0 to 5.0 g/10min.
[0077] Hence in one specific embodiment, the instant polypropylene composition has

(a) a melt flow rate MFR2 (230 °C) measured according to ISO 1133 of not more than 7.0 g/10min, preferably in a
25 range of 0.5 to 7.0 g/10 min, more preferably in a range of 0.5 to 7.0 g/10 min, still more preferably in a range of 0.5
to 6.0 g/10 min, yet more preferably in a range of 1.0 to 6.0 g/10 min, like in the range of 1.5 to 5.0 g/10min or like
in the range of 1.0 to 5.0 g/10min;
(b) a F30 melt strength of more than 20.0 cN, like of more than 20.0 to 50.0 cN, more preferably of more than 21.0
cN, still more preferably of 21.0 to 50.0 cN, yet more preferably of 25.0 to 50.0 cN, still yet more preferably of 25.0
30 to 45.0 cN, most preferably of 30.0 to 45.0 cN, like of 32.0 to 42.0 cN; and
(c) a v30 melt extensibility of more than 210 to 300 mm/s, like of more than 220 to 300 mm/s, more preferably of
more than 225 mm/s, still more preferably of 225 to 300 mm/s, yet more preferably of 230 to 290 mm/s.

[0078] Accordingly in a more specific embodiment the instant polypropylene composition has a melt flow rate MFR2
35 (230 °C) has a melt flow rate MFR2 (230 °C) of not more than 7.0 g/10min, a F30 melt strength of more than 20.0 cN
and a v30 melt extensibility of more than 210 to 300 mm/s, like a melt flow rate MFR2 (230 °C) in a range of 0.5 to 7.0
g/10 min, a F30 melt strength of more than 20.0 to 50.0 cN and v30 melt extensibility of more than 220 to 300 mm/s,
more preferably a melt flow rate MFR2 (230 °C) in a range of 0.5 to 6.0 g/10 min, a F30 melt strength of more than 21.0
cN and v30 melt extensibility of more than 225 mm/s, still more preferably a melt flow rate MFR2 (230 °C) in a range of
40 1.0 to 6.0 g/10 min, a F30 melt strength of 21.0 to 50.0 cN and v30 melt extensibility of 225 to 300 mm/s, yet more
preferably a melt flow rate MFR2 (230 °C) in a range of 1.0 to 6.0 g/10min, a F30 melt strength of 25.0 to 50.0 cN and
v30 melt extensibility of 230 to 290 mm/s, still yet more preferably a melt flow rate MFR2 (230 °C) in a range of 1.0 to
5.0 g/10min, a F30 melt strength of 25.0 to 45.0 cN and v30 melt extensibility of 230 to 290 mm/s, most preferably a melt
flow rate MFR2 (230 °C) in a range of 1.0 to 5.0 g/10min, a F30 melt strength of 30.0 to 45.0 cN and v30 melt extensibility
45 of 230 to 290 mm/s, like a melt flow rate MFR2 (230 °C) in a range of 1.0 to 5.0 g/10min, a F30 melt strength of 32.0 to
42.0 cN and v30 melt extensibility of 230 to 290 mm/s.
[0079] Essential finding of the present invention is that the branched polypropylene (b-PP), i.e. the high melt strength
polypropylene (HMS-PP), and/or the instant polypropylene composition show(s) a reduced gel content. Accordingly it
is preferred that the branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-PP), and/or the
50 instant polypropylene composition has/have a gel content of less than 1.00 wt.-%, preferably of less than 0.80 wt.-%,
more preferably less than 0.50 wt.-%, still more preferably in the range of 0.01 to less than 1.00 wt.-%, yet more preferably
in the range of 0.01 to less than 0.80 wt.-%, still yet more preferably in the range of 0.02 to less than 0.50 wt.-%.
[0080] Keeping the information provide above in mind the present invention for instance covers a polypropylene
composition comprising
55
(a) 80 to 99 parts by weight, preferably 90 to 99 parts by weight, more preferably 95 to 99 parts by weight, of the
branched polypropylene (b-PP), i.e. of the high melt strength polypropylene (HMS-PP);
(b) optionally 1 to 20 parts by weight, preferably 1 to 10 parts by weight, more preferably 1 to 5 parts by weight, of

11
EP 2 877 534 B1

polypropylene (PP’), preferably of the linear polypropylene (1-PP), having a melt flow rate MFR2 (230 °C) measured
according to ISO 1133 of more than 0.5 g/10min, preferably in the range of more than 0.5 to 18.0 g/10min, like of
more than 0.5 to 15.0 g/10min or of more than 0.6 to 15.0 g/10min, more preferably of more than 0.5 to below 10.0
g/10min, still more preferably of more than 0.6 to 9.0 g/10min, yet more preferably of 0.8 to 8.0 g/10min; and
5 (c) optionally 0.005 to 5.0, preferably 0.005 to 2.0, more preferably 0.05 to 1.0, like 0.05 to 0.5, parts by weight of
additives (A), wherein said additives(A) are preferably selected from the group consisting of antioxidants, metal
deactivators, UV-stabilizers, antistatic agents, antifogging agents, acid scavengers, blowing agents, cling agents,
lubricants, nucleating agents, slip agents, antiblocking agents and mixtures thereof;

10 wherein the polypropylene composition has

- a melt flow rate MFR2 (230 °C) of not more than 7.0 g/10min, preferably in a range of 0.5 to 7.0 g/10 min, more
preferably in a range of 0.5 to 6.5 g/10 min, still more preferably in a range of 0.5 to 6.0 g/10 min, yet more preferably
in a range of 1.0 to 6.0 g/10 min, like in the range of 1.5 to 5.0 g/10min or like in the range of 1.0 to 5.0 g/10min; and
15 - a gel content of less than 1.00 wt.-%, preferably of less than 0.80 wt.-%, more preferably less than 0.50 wt.-%, still
more preferably in the range of 0.01 to less than 1.00 wt.-%, yet more preferably in the range of 0.01 to less than
0.80 wt.-%, still yet more preferably in the range of 0.02 to less than 0.50 wt.-%;

and wherein the polypropylene composition and/or the branched polypropylene (b-PP), i.e. the high melt strength poly-
20 propylene (HMS-PP), has/have

- a F30 melt strength of more than 20.0 cN, like of more than 20.0 to 50.0 cN, more preferably of more than 21.0 cN,
still more preferably of 21.0 to 50.0 cN, yet more preferably of 25.0 to 50.0 cN, still yet more preferably of 25.0 to
45.0 cN, most preferably of 30.0 to 45.0 cN, like of 32.0 to 42.0 cN; and
25 - a v30 melt extensibility of more than 210 to 300 mm/s, like of more than 220 to 300 mm/s, more preferably of more
than 225 mm/s, still more preferably of 225 to 300 mm/s, yet more preferably of 230 to 290 mm/s.

The foam

30 [0081] As mentioned above, the present invention also features a foam comprising the instant polypropylene compo-
sition described herein. Preferably the foam comprises at least 70 wt.-%, more preferably at least 80 wt.-%, more
preferably at least 90 wt.-%, yet more preferably at least 95 wt.-%, of the polypropylene composition according to the
instant invention. In a preferred embodiment the foam consists of the instant polypropylene composition (apart from the
foaming agents if still present in the foam after the foaming process).
35
The Process

[0082] One essential aspect of the present invention is that the manufacture of the polypropylene composition com-
prising the branched polypropylene (b-PP), i.e. comprising the high melt strength polypropylene (HMS-PP), by using
40 the polypropylene (PP), preferably the linear polypropylene (1-PP). In other words, the present invention relates to a
process for providing a polypropylene composition comprising the branched polypropylene (b-PP), wherein the process
comprises at least a step (a) in which a polypropylene (PP) is reacted with a thermally decomposing free radical-forming
agent and optionally with bifunctionally unsaturated monomer(s) and/or with multifunctionally unsaturated low molecular
weight polymer(s) obtaining thereby the branched polypropylene (b-PP). Preferably the instant process comprises sub-
45 sequent to step (a) a further step (b), in which to the branched polypropylene (b-PP), i.e. to the high melt strength
polypropylene (HMS-PP), the polypropylene (PP’) is added. Even more preferred the instant process comprises sub-
sequent to step (a) a further step (b), in which to the branched polypropylene (b-PP), i.e. to the high melt strength
polypropylene (HMS-PP), the additive mixture (AM) comprising the polypropylene (PP’) and the additives (A) is added.
[0083] Subsequently the so produced polypropylene composition is subjected to a foaming process obtaining thereby
50 a foam comprising the instant polypropylene composition.
[0084] Concerning the definitions and preferred embodiments of the foam, the polypropylene composition, the
branched polypropylene (b-PP), the polypropylene (PP), the polypropylene (PP’), the additives (A) and the additive
mixture (AM) reference is made to the information provide above.
[0085] As mentioned above, in step (a) of the process for the manufacture of polypropylene composition the branched
55 polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-PP), is obtained by treating the polypropylene
(PP), preferably the linear polypropylene (1-PP), with thermally decomposing radical-forming agents. However in such
a case a high risk exists that the polypropylene (PP), preferably the linear polypropylene (PP), is degraded, which is
detrimental. Thus it is preferred that the chemical modification is accomplished by the additional use of bifunctionally

12
EP 2 877 534 B1

unsaturated monomer(s) and/or multifunctionally unsaturated low molecular weight polymer(s) as chemically bound
bridging unit(s). A suitable method to obtain the branched polypropylene (b-PP), i.e. the high melt strength polypropylene
(HMS-PP), is for instance disclosed in EP 0 787 750, EP 0 879 830 A1 and EP 0 890 612 A2. Thereby, the amount of
thermally decomposing radical-forming agents, preferably of peroxide, is preferably in the range of 0.05 to 3.00 wt.-%
5 based on the amount of the polypropylene (PP). Typically the thermally decomposing radical-forming agents are added
together with the bifunctionally unsaturated monomer(s) and/or with multifunctionally unsaturated low molecular weight
polymer(s) to the polypropylene (PP), preferably to the linear polypropylene (1-PP). However it is also possible, but less
preferred, that first the bifunctionally unsaturated monomer(s) and/or multifunctionally unsaturated low molecular weight
polymer(s) is/are added to the polypropylene (PP), preferably to the linear polypropylene (1-PP), and subsequent the
10 thermally decomposing radical-forming agents, or the other way round,
first the thermally decomposing radical-forming agents are added to the polypropylene (PP), preferably to the linear
polypropylene (1-PP), and subsequent the bifunctionally unsaturated monomer(s) and/or multifunctionally unsaturated
low molecular weight polymer(s).
[0086] Concerning the bifunctionally unsaturated monomer(s) and/or multifunctionally unsaturated low molecular
15 weight polymer(s) used for the manufacture of the branched polypropylene (b-PP), i.e. the high melt strength polypro-
pylene (HMS-PP), reference is made to the section "the branched polypropylene".
[0087] As stated above it is preferred that the bifunctionally unsaturated monomer(s) and/or multifunctionally unsatu-
rated low molecular weight polymer(s) are used in the presence of a thermally decomposing free radical-forming agent.
[0088] Peroxides are preferred thermally decomposing free radical-forming agents. More preferably the thermally
20 decomposing free radical-forming agents are selected from the group consisting of acyl peroxide, alkyl peroxide, hy-
droperoxide, perester and peroxycarbonate.
[0089] The following listed peroxides are in particular preferred:

Acyl peroxides: benzoyl peroxide, 4-chlorobenzoyl peroxide, 3-methoxybenzoyl peroxide and/or methyl benzoyl
25 peroxide.

[0090] Alkyl peroxides: allyl t-butyl peroxide, 2,2-bis(t-butylperoxybutane), 1,1-bis(t-butylperoxy)-3,3,5-trimethylcy-


clohexane, n-butyl-4,4-bis(t-butylperoxy) valerate, diisopropylaminomethyl-t-amyl peroxide, dimethylaminomethyl-t-
amyl peroxide, diethylaminomethyl-t-butyl peroxide, dimethylaminomethyl-t-butyl peroxide, 1,1-di-(t-amylperoxy)cy-
30 clohexane, t-amyl peroxide, t-butylcumyl peroxide, t-butyl peroxide and/or 1-hydroxybutyl n-butyl peroxide.
[0091] Peresters and peroxy carbonates: butyl peracetate, cumyl peracetate, cumyl perpropionate, cyclohexyl pera-
cetate, di-t-butyl peradipate, di-t-butyl perazelate, di-t-butyl perglutarate, di-t-butyl perthalate, di-t-butyl persebacate, 4-
nitrocumyl perpropionate, 1-phenylethyl perbenzoate, phenylethyl nitro-perbenzoate, t-butylbicyclo-(2,2,1)heptane per-
carboxylate, t-butyl-4-carbomethoxy perbutyrate, t-butylcyclobutane percarboxylate, t-butylcyclohexyl peroxycarboxy-
35 late, t-butylcyclopentyl percarboxylate, t-butylcyclopropane percarboxylate, t-butyldimethyl percinnamate, t-butyl-2-(2,2-
diphenylvinyl) perbenzoate, t-butyl-4-methoxy perbenzoate, t-butylperbenzoate, t-butylcarboxycyclohexane, t-butyl per-
naphthoate, t-butyl peroxyisopropylcarbonate, t-butyl pertoluate, t-butyl-1-phenylcyclopropyl percarboxylate, t-butyl-2-
propylperpentene-2-oate, t-butyl-1-methylcyclopropyl percarboxylate, t-butyl-4-nitrophenyl peracetate, t-butylnitrophe-
nyl peroxycarbamate, t-butyl-N-succiimido percarboxylate, t-butyl percrotonate, t-butyl permaleic acid, t-butyl permeth-
40 acrylate, t-butyl peroctoate, t-butyl peroxyisopropylcarbonate, t-butyl perisobutyrate, t-butyl peracrylate and/or t-butyl
perpropionate.
[0092] Also contemplated are mixtures of these above listed free radical-forming agents.
[0093] Preferably step (b) is initiated when at least 70 %, preferably at least 80 %, yet more preferably at least 90 %,
like at least 95 or 99 %, of the reaction between the polypropylene (PP) and the thermally decomposing free radical-
45 forming agent and optionally the bifunctionally unsaturated monomer has taken place to obtain the branched polypro-
pylene (b-PP), i.e. the high melt strength polypropylene (HMS-PP).
[0094] In a preferred embodiment, an extruder, such as a twin screw extruder, is used for step (a) and for the optional
step (b).
[0095] The use of an extruder is particularly advantageous in that it can simultaneously be used for the preparation
50 of the branched propylene (b-PP), i.e. the high melt strength polypropylene (HMS-PP), and subsequent for adding the
polypropylene (PP’) or for adding the additive mixture (AM) to said branched propylene (b-PP). In a preferred embodiment,
the polypropylene (PP) is added to an extruder together with - as described in detail above - the thermally decomposing
free radical-forming agent, preferably a peroxide, and optionally with the bifunctionally unsaturated monomer(s) and/or
with the multifunctionally unsaturated low molecular weight polymer(s), preferably with the bifunctionally unsaturated
55 monomer(s) selected from divinyl compounds, allyl compounds or dienes, to provide the branched polypropylene (b-
PP), i.e. the high melt strength polypropylene (HMS-PP), in step (a). It is also possible to use a combination of an extruder
downstream a pre-mixing device, wherein the bifunctionally unsaturated monomer(s) and/or the multifunctionally un-
saturated low molecular weight polymer(s) and the thermally decomposing free radical-forming agent are add to the

13
EP 2 877 534 B1

polypropylene in the pre-mixing device.


[0096] Subsequently, in a step (b) the polypropylene (PP’), preferably the linear polypropylene (1-PP), or the additive
mixture (AM) based on said polypropylene (PP’), preferably based on said linear polypropylene (1-PP’), comprising the
at least one additive (A) is preferably added at the downstream end of the extruder screw in order not to interfere with
5 the modification reaction for providing branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-
PP), as described above. In this respect, the term "downstream end of the extruder screw" is understood as within the
last 60 % of the length of the extruder screw, preferably within the last 65 % of the length of the extruder screw, more
preferably at least 70 % of the length of the extruder screw, like at least 75 % of the extruder screw.
[0097] Accordingly, the extruder (E) used for the instant process preferably comprises in operation direction a feed-
10 throat (FT), a first mixing zone (MZ1), a second mixing zone (MZ2) and a die (D), wherein between the first mixing zone
(MZ1) and the second mixing zone (MZ2) a side feed-throat (SFT) is located. Preferably the extruder is a screw extruder,
like a twin screw extruder. Accordingly the polypropylene (PP), the thermally decomposing free radical-forming agent,
preferably a peroxide, and optionally the bifunctionally unsaturated monomer and/or the multifunctionally unsaturated
low molecular weight polymer monomer, preferably selected from divinyl compounds, allyl compounds or dienes, but
15 not the polypropylene (PP’), i.e. not the linear polypropylene (1-PP’), and not the additives (A), are fed via the feed-throat
(FT), thereby preferably using a feeder, into the extruder and is/are subsequently passed downstream through the first
mixing zone (MZ1). Preferably the shear stress in said first mixing zone (MZ1) is of such extent that the polypropylene
(PP) is molten and the chemical reaction with the radical-forming agent and with the optional bifunctionally unsaturated
monomer and/or multifunctionally unsaturated low molecular weight polymer is initiated. After the first mixing zone (MZ1),
20 i.e. between the first mixing zone (MZ1) and the second mixing zone (MZ2), the polypropylene (PP’), preferably the
linear polypropylene (1-PP’), or the additive mixture (AM) is added, i.e. fed into the extruder. Preferably the polypropylene
(PP’), preferably the linear polypropylene (1-PP’), or the additive mixture (AM) is added via the side feed-throat (SFT),
thereby preferably using a side feeder. Subsequently all components of the polypropylene composition, including the
polypropylene (PP’), preferably the linear polypropylene (1-PP’), or the additive mixture (AM) are passed downstream
25 through the second mixing zone (MZ2). Finally the polypropylene composition is discharged via the die (D).
[0098] Preferably, the first mixing zone (MZ1) is longer than the second mixing zone (MZ2). Preferably the length ratio
between the first mixing zone (MZ1) to the second mixing zone (MZ2) [mm (MZ1) / mm (MZ2)] is at least 2/1, more
preferably 3/1, yet more preferably in the range of 2/1 to 15/1, still more preferably 3/1 to 10/1.
[0099] The foaming process is in the skilled knowledge. In such a process, a melt of the instant polypropylene com-
30 position comprising a gaseous foaming agent such as butane, HFC or CO2 is suddenly expanded through pressure
drop. Continuous foaming processes as well as discontinuous process may be applied. In a continuous foaming process,
the polypropylene composition is melted and laden with gas in an extruder under pressures typically above 20 bar before
extruded through a die where the pressure drop causes the formation of a foam. The mechanism of foaming polypropylene
in foam extrusion is explained, for example, in H. E. Naguib, C. B. Park, N. Reichelt, Fundamental foaming mechanisms
35 governing the volume expansion of extruded polypropylene foams, Journal of Applied Polymer Science, 91, 2661-2668
(2004). Processes for foaming are outlined in S. T. Lee, Foam Extrusion, Technomic Publishing (2000). In a discontinuous
foaming process, the polypropylene composition (micro-)pellets are laden with foaming agent under pressure and heated
below melting temperature before the pressure in the autoclave is suddenly relaxed. The dissolved foaming agent forms
bubbles and creates a foam structure. Such preparation of discontinuously foamed beads is described for example in
40 DE 3 539 352.

The use

[0100] Additionally the invention is directed to the use of a polypropylene (PP) having a melt flow rate MFR2 (230°C)
45 of more than 0.5 g/10min in the manufacture of a branched polypropylene (b-PP) and thus in the manufacture of a
polypropylene composition comprising the branched polypropylene (b-PP) to reduce the gel content of the branched
polypropylene (b-PP) and/or of the polypropylene composition comprising the branched polypropylene (b-PP). Preferably
the gel content is reduced in case the branched polypropylene (b-PP) and/or the polypropylene composition comprising
the branched polypropylene (b-PP) has/have a gel content of less than 1.00 wt.-%, preferably of less than 0.80 wt.-%,
50 more preferably less than 0.50 wt.-%, still more preferably in the range of 0.01 to less than 1.00 wt.-%, yet more preferably
in the range of 0.01 to less than 0.80 wt.-%, still yet more preferably in the range of 0.02 to less than 0.50 wt.-%.
[0101] Preferred embodiments of polypropylene (PP) are those as defined in the section "the polypropylene (PP)".
Concerning the preferred branched polypropylene (b-PP) and the preferred polypropylene composition reference is
made to the section the "branched polypropylene (b-PP)" and to the section "the polypropylene composition", respectively.
55 Preferably the polypropylene (PP) is used in a process as described in the section "the process". Accordingly all preferred
embodiments discussed above for the branched polypropylene (b-PP), the polypropylene composition, the polypropylene
(PP), the polypropylene (PP’), the additives (A) and the additive mixture (AM) are also preferred for the instant use. Thus
for instance the present invention is directed to the use of a polypropylene (PP) in the process for the manufacture of a

14
EP 2 877 534 B1

branched polypropylene (b-PP) and thus for the manufacture of a polypropylene composition comprising the branched
polypropylene (b-PP) to reduce the gel content of the branched polypropylene (b-PP) and/or of the polypropylene
composition comprising the branched polypropylene (b-PP), wherein the process comprises at least a step (a) in which
the polypropylene (PP) is reacted with a thermally decomposing free radical-forming agent and optionally with bifunc-
5 tionally unsaturated monomer(s) and/or with multifunctionally unsaturated low molecular weight polymer(s) obtaining
thereby the branched polypropylene (b-PP),
wherein

(a) the polypropylene (PP) has


10
(a1) a melt flow rate MFR2 (230 °C) measured according to ISO 1133 of more than 0.5 g/10min, preferably in
the range of more than 0.5 to 18.0 g/10min, like of more than 0.5 to 15.0 g/10min or of more than 0.6 to 15.0
g/10min, more preferably of more than 0.5 to below 10.0 g/10min, still more preferably of more than 0.6 to 9.0
g/10min, yet more preferably of 0.8 to 8.0 g/10min;
15 (a2) preferably a F30 melt strength of more than 1.0 cN, more preferably of more than 2.0 cN, still more preferably
in the range of 1.0 to below 68.0 cN, yet more preferably in the range of 1.5 to 65.0 cN, still yet more preferably
in the range of 2.0 to 60.0 cN, like preferably in the range of 2.5 to 50.0 cN, most in the range of 2.5 to 45.0 cN; and
(a3) preferably a v30 melt extensibility of below 200 mm/s, more preferably of below 190 mm/s, still more
preferably in the range of 100 to below 200 mm/s, yet more preferably in the range of 120 to 190 mm/s, still yet
20 more preferably in the range of 120 to 175 mm/s, like in the range of 125 to 170 mm/s;

and
(b) the polypropylene composition and/or the branched polypropylene (b-PP) has/have

25 (b1) a melt flow rate MFR2 (230 °C) not more than 7.0 g/10min, preferably in a range of 0.5 to 7.0 g/10 min,
more preferably in a range of 0.5 to 6.5 g/10 min, still more preferably in a range of 0.5 to 6.0 g/10 min, yet more
preferably in a range of 1.0 to 6.0 g/10 min, like in the range of 1.5 to 5.0 g/10min or like in the range of 1.0 to
5.0 g/10min;
(b2) a F30 melt strength of more than 20.0 cN, like of more than 20.0 to 50.0 cN, more preferably of more than
30 21.0 cN, still more preferably of 21.0 to 50.0 cN, yet more preferably of 25.0 to 50.0 cN, still yet more preferably
of 25.0 to 45.0 cN, most preferably of 30.0 to 45.0 cN, like of 32.0 to 42.0 cN; and
(b3) a v30 melt extensibility of more than 210 to 300 mm/s, like of more than 220 to 300 mm/s, more preferably
of more than 225 mm/s, still more preferably of 225 to 300 mm/s, yet more preferably of 230 to 290 mm/s;

35 wherein further
the gel content is reduced in case the branched polypropylene (b-PP) and/or the polypropylene composition comprising
the branched polypropylene (b-PP) has/have a gel content of less than 1.00 wt.-%, preferably of less than 0.80 wt.-%,
more preferably less than 0.50 wt.-%, still more preferably in the range of 0.01 to less than 1.00 wt.-%, yet more preferably
in the range of 0.01 to less than 0.80 wt.-%, still yet more preferably in the range of 0.02 to less than 0.50 wt.-%.
40 [0102] In one embodiment the branched polypropylene (b-PP), i.e. the high melt strength polypropylene (HMS-PP),
has been mixed with a polypropylene (PP’) or with an additive mixture (AM) after step (A). Accordingly the polypropylene
composition preferably comprises

(a) 80 to 99 parts by weight, preferably 90 to 99 parts by weight, more preferably 95 to 99 parts by weight, of the
45 branched polypropylene (b-PP), i.e. of the high melt strength polypropylene (HMS-PP);
(b) optionally 1 to 20 parts by weight, preferably 1 to 10 parts by weight, more preferably 1 to 5 parts by weight, of
polypropylene (PP’), preferably of the linear polypropylene (1-PP), having a melt flow rate MFR2 (230 °C) measured
according to ISO 1133 of more than 0.5 g/10min, preferably in the range of more than 0.5 to 18.0 g/10min, like of
more than 0.5 to 15.0 g/10min or of more than 0.6 to 15.0 g/10min, more preferably of more than 0.5 to below 10.0
50 g/10min, still more preferably of more than 0.6 to 9.0 g/10min, yet more preferably of 0.8 to 8.0 g/10min; and
(c) optionally 0.005 to 5.0, preferably 0.005 to 2.0, more preferably 0.05 to 1.0, like 0.05 to 0.5, parts by weight of
additives (A), wherein said additives(A) are preferably selected from the group consisting of antioxidants, metal
deactivators, UV-stabilizers, antistatic agents, antifogging agents, acid scavengers, blowing agents, cling agents,
lubricants, nucleating agents, slip agents, antiblocking agents and mixtures thereof.
55
[0103] In the following, the present invention is described in more detail by way of examples.

15
EP 2 877 534 B1

EXAMPLES

A. Measuring methods

5 [0104] The following definitions of terms and determination methods apply for the above general description of the
invention as well as to the below examples unless otherwise defined.

Comonomer content in polypropylene

10 [0105] The comonomer content is determined by quantitative Fourier transform infrared spectroscopy (FTIR) after
basic assignment calibrated via quantitative 13C nuclear magnetic resonance (NMR) spectroscopy in a manner well
known in the art. Thin films are pressed to a thickness of 250 mm and spectra recorded in transmission mode.
[0106] Specifically, the ethylene content of a polypropylene-co-ethylene copolymer is determined using the baseline
corrected peak area of the quantitative bands found at 720-722 and 730-733 cm-1. Propylene-1-butene-copolymers
15 were evaluated at 767 cm-1.Quantitative results are obtained based upon reference to the film thickness.
[0107] Melting temperature (Tm) and heat of fusion (Hf), crystallization temperature (Tc) and heat of crystalli-
zation (Hc): measured with Mettler TA820 differential scanning calorimetry (DSC) on 5 to 10 mg samples. DSC is run
according to ISO 3146 / part 3 /method C2 in a heat / cool / heat cycle with a scan rate of 10 °C/min in the temperature
range of +23 to +210°C. Crystallization temperature and heat of crystallization (Hc) are determined from the cooling
20 step, while melting temperature and heat of fusion (Hf) are determined from the second heating step
MFR2 (230 °C) is measured according to ISO 1133 (230 °C, 2.16 kg load).
[0108] F30 melt strength and v30 melt extensibility
[0109] The test described herein follows ISO 16790:2005.
[0110] The strain hardening behaviour is determined by the method as described in the article "Rheotens-Mastercurves
25 and Drawability of Polymer Melts", M. H. Wagner, Polymer Engineering and Sience, Vol. 36, pages 925 to 935. The
strain hardening behaviour of polymers is analysed by Rheotens apparatus (product of Göttfert, Siemensstr.2, 74711
Buchen, Germany) in which a melt strand is elongated by drawing down with a defined acceleration.
[0111] The Rheotens experiment simulates industrial spinning and extrusion processes. In principle a melt is pressed
or extruded through a round die and the resulting strand is hauled off. The stress on the extrudate is recorded, as a
30 function of melt properties and measuring parameters (especially the ratio between output and haul-off speed, practically
a measure for the extension rate). For the results presented below, the materials were extruded with a lab extruder
HAAKE Polylab system and a gear pump with cylindrical die (L/D = 6.0/2.0 mm). The gear pump was pre-adjusted to a
strand extrusion rate of 5 mm/s, and the melt temperature was set to 200°C. The spinline length between die and
Rheotens wheels was 80 mm. At the beginning of the experiment, the take-up speed of the Rheotens wheels was
35 adjusted to the velocity of the extruded polymer strand (tensile force zero): Then the experiment was started by slowly
increasing the take-up speed of the Rheotens wheels until the polymer filament breaks. The acceleration of the wheels
was small enough so that the tensile force was measured under quasi-steady conditions. The acceleration of the melt
strand drawn down is 120 mm/sec2. The Rheotens was operated in combination with the PC program EXTENS. This
is a real-time data-acquisition program, which displays and stores the measured data of tensile force and drawdown
40 speed. The end points of the Rheotens curve (force versus pulley rotary speed) is taken as the F30 melt strength and
drawability values.

Gel content

45 [0112] About 2 g of the polymer (mp) are weighted and put in a mesh of metal which is weighted (mp+m). The polymer
in the mesh is extracted in a soxhlet apparatus with boiling xylene for 5 hours. The eluent is then replaced by fresh
xylene and the boiling is continued for another hour. Subsequently, the mesh is dried and weighted again (mXHU+m).
The mass of the xylene hot unsolubles (mXHU) obtained by the formula m XHU+m - mm = mXHU is put in relation to the
weight of the polymer (mp) to obtain the fraction of xylene insolubles mXHU/mp.
50
Particle size/Particle size distribution

[0113] A gradation test was performed on the polymer samples. The sieve analysis involved a nested column of sieves
with wire mesh screen with the following sizes: >20 mm, >32 mm, >63 mm, >100 mm, >125 mm, >160 mm, > 200 mm,
55 >250 mm, > 315 mm, > 400 mm, >500 mm, >710 mm, >1 mm, >1.4 mm, > 2 mm, >2.8 mm. The samples were poured
into the top sieve which has the largest screen openings. Each lower sieve in the column has smaller openings than the
one above (see sizes indicated above). At the base is the receiver. The column was placed in a mechanical shaker. The
shaker shook the column. After the shaking was completed the material on each sieve was weighed. The weight of the

16
EP 2 877 534 B1

sample of each sieve was then divided by the total weight to give a percentage retained on each sieve.

B. Examples

5 Linear polypropylene (1-PP)

[0114]

1-PP1 is a linear propylene homopolymer having a MFR2 (230°C) of 0.37 g/10min, a d50 of 1,100 mm, a d90 of 1,650
10 mm, a melting temperature Tm of 164 °C, a F30 melt strength of 68 cN and v30 melt extensibility 146 mm/s.
1-PP2 is a linear propylene homopolymer having a MFR2 (230°C) of 0.90 g/10min, a d50 of 625 mm, a d90 of 970
mm, a melting temperature Tm of 162°C, a F30 melt strength of 39 cN and v30 melt extensibility 155 mm/s.

Additive mixture
15
[0115] The linear polypropylenes 1-PP2 was used to provide additive mixture (AM) containing further additives as a
masterbatch for incorporating into a base polymer of branched polypropylene. The additive mixture contains 85wt.-%
of the linear polypropylenes 1-PP1, 10.00 wt.-% Irganox B 225 FF (antioxidant), and 2.50 wt.-% Hydrotalcit and 2,50
wt% of Ca Stearate.
20
Inventive Examples IE1 and IE2 and comparative examples CE1 to CE3:

[0116] 1-PP1 for the comparative examples CE1 to CE3 and 1-PP2 for the inventive examples IE1 and IE2 were
subjected to a reactive extrusion in the presence of butadiene and peroxide as described in the following. Both the
25 butadiene and the peroxide (75 % solution of tert-butylperoxy isopropyl carbonate "Trigonox BPIC-C75" of Akzo Nobel)
(amounts are indicated in table 3) were pre-mixed with the 1-PP1 powder prior or 1-PP2 powder to the melt-mixing step
in a horizontal mixer with paddle stirrer at a temperature of 65°C, maintaining an average residence time of 15 to 20
minutes. The pre-mixture was transferred under inert atmosphere to a co-rotating twin screw extruder of the type Theyson
TSK60 having a barrel diameter of 60 mm and an L/D-ratio of 48 equipped with a high intensity mixing screw having 3
30 kneading zones and a two-step degassing setup. The melt temperature profile is given in table 1. The screw speed and
throughput is indicated in table 2. In the first 3/4 of the extruder length the branched polypropylene is produced (b-PP).
Subsequently, via a side feeder, i.e. at the last 1/4 of the extruder length, the additive mixture is fed into the extruder to
the produced branched polypropylene (b-PP) The extruded polypropylene composition was discharged and pelletized.
From the pellets the gel content has been measured. The final properties are indicated in table 3.
35
Table 1: Set temperature profile in the extruder
Zone 1 to 6 7 8 9 10 11 12 13 14
Temperature [°C] 280 270 260 220 250 270 240 240 230
40

Table 2: Process conditions


IE 1 IE 2 CE 1 CE 2 CE 3
45 Peroxide* [wit-%] 0.675 0.750 0.675 0.825 0.860
butadiene* [wit-%] 1.6 1.8 1.6 1.5 1.9
screw speed [rpm] 400 400 400 400 400
throughput [kg/h] 225 225 225 225 225
50
additive mixture* [wt.-%] 2 2 2 2 2
* based on the total amount of the polypropylene composition

55

17
EP 2 877 534 B1

Table 3: Properties of polypropylene composition


MFR2 F30 V30 Gel content
[g/10min] [cN] [mm/s] [wt.-%]
5
IE1 2.3 35.6 249 0.04
IE2 2.6 36.9 249 0.10
CE1 2.2 31.0 253 0.76

10 CE2 1.9 32.3 249 1.31


CE3 1.5 36.6 241 2.03

Claims
15

1. Process for providing a polypropylene composition comprising a branched polypropylene (b-PP), the process com-
prises at least a step (a) in which a polypropylene (PP) is reacted with a thermally decomposing free radical-forming
agent and optionally with bifunctionally unsaturated monomer(s) and/or with multifunctionally unsaturated low mo-
lecular weight polymer(s) obtaining thereby the branched polypropylene (b-PP),
20
wherein

(a) the polypropylene (PP) has a melt flow rate MFR 2 (230°C) of more than 0.5 g/10min;
(b) the polypropylene composition and/or the branched polypropylene (b-PP) has/have a F30 melt strength of
more than 20.0 cN and a v30 melt extensibility of more than 200 mm/s, wherein the F30 melt strength and the
25
v30 melt extensibility are measured according to ISO 16790:2005, and
(c) the polypropylene (PP) is used in the form of particles having a particle size distribution d90 of below 1,500
mm, d50 of below 1,000 mm, and a d90/d50 ratio of below 1.80.

2. Process according to claim 1, wherein the polypropylene (PP)


30

(a) is a propylene homopolymer;


and/or
(b) is a linear polypropylene (1-PP) having preferably a F30 melt strength of more than 1.0 cN and a v30 melt
extensibility of below 200 mm/s, wherein the F30 melt strength and the v30 melt extensibility are measured
35 according to ISO 16790:2005.

3. Process according to anyone of the preceding claims, wherein

(a) the thermally decomposing free radical-forming agent is a peroxide;


40
and/or
(b) the bifunctionally unsaturated monomer is selected from the group consisting of divinyl compounds, allyl
compounds and dienes.

4. Process according to anyone of the preceding claims, wherein the process comprises subsequent to step (a) a
45
further step (b), in which to the branched polypropylene (b-PP) a polypropylene (PP’) having a melt flow rate MFR2
(230°C) of 0.5 to 18.0 g/10min is added.

5. Process according to claim 4, wherein

50
(a) step (b) is initiated when at least 80 % of the reaction between the polypropylene (PP) and the thermally
decomposing free radical-forming agent and optionally the bifunctionally unsaturated monomer has taken place;
and/or
(b) the polypropylene (PP’) is a linear polypropylene (1-PP’), said linear polypropylene (1-PP’) preferably has
a F30 melt strength of more than 1.0 cN and a v30 melt extensibility of below 200 mm/s, more preferably has a
55
F30 melt strength of more than 1.0 to below 68.0 cN and a v30 melt extensibility of below 200 mm/s, wherein
the F30 melt strength and the v30 melt extensibility are measured according to ISO 16790:2005.

18
EP 2 877 534 B1

6. The process according to anyone of the preceding claims, wherein the step (a) and the optional step (b) are accom-
plished in an extruder, said extruder preferably comprises in operation direction a first mixing zone (MZ1) and a
second mixing zone (MZ2), wherein further the step (a) takes place in the first mixing zone (MZ1) whereas step (b)
takes place in the second mixing zone (MZ2), preferably the extruder comprises in operation direction a feed-throat
5 (FT), the first mixing zone (MZ1), the second mixing zone (MZ2) and a die (D), wherein between the first mixing
zone (MZ1) and the second mixing zone (MZ2) a side feed-throat (SFT) is located, wherein further the polypropylene
(PP), the thermally decomposing free radical-forming agent, and optionally the bifunctionally unsaturated monomer
are fed via the feed-throat (FT) and the polypropylene (PP’) is fed via the side feed-throat (SFT).

10 7. The process according to claim 6, wherein

(a) the reaction between the polypropylene (PP) and the thermally decomposing free radical-forming agent and
optionally the bifunctionally unsaturated monomer takes place in the first mixing zone (MZ1);
and/or
15 (b) not more than 10 wt.-% of the total amount of the branched polypropylene (b-PP) of the polypropylene
composition is produced in the second mixing zone (MZ2).

8. The process according to anyone of the preceding claims 4 to 7, wherein 1 to 5 parts by weight of the polypropylene
(PP’) are added to 95 to 99 parts by weight of branched polypropylene (b-PP), preferably wherein 1 to 3 parts by
20 weight of the polypropylene (PP’) are added to 97 to 99 parts by weight of branched polypropylene (b-PP), more
preferably wherein 2 parts by weight of the polypropylene (PP’) are added to 98 parts by weight of branched
polypropylene (b-PP).

9. The process according to anyone of the preceding claims, wherein


25
(a) the polypropylene (PP’) comprises at least one additive (A) selected from the group consisting of antioxidants,
metal deactivators, UV-stabilizers, antistatic agents, antifogging agents, acid scavengers, blowing agents, cling
agents, lubricants, nucleating agents, slip agents, antiblocking agents and mixtures thereof;
and/or
30 (b) the branched polypropylene (b-PP) is free of additives (A).

10. The process according to anyone of the preceding claims, wherein the resulting polypropylene composition has

(a) a F30 melt strength of 25.0 cN to 50.0 cN and a v30 melt extensibility of 210 to 300 mm/s;
35 and/or
(b) a gel content of less than 1.00 wt.-%, preferably of less than 0.80 wt.-%.

11. Polypropylene composition obtainable by the process according to any one of claims 1 to 10 comprising

40 (a) 95 to 99 parts by weight of a branched polypropylene (b-PP);


(b) optionally 1 to 5 parts by weight of a polypropylene (PP’) having a melt flow rate MFR2 (230 °C) measured
according to ISO 1133 of more than 0.5 to 18.0 g/10min; and
(c) optionally 0.005 to 5.0 parts by weight of additives (A), wherein said additives(A) are preferably selected
from the group consisting of antioxidants, metal deactivators, UV-stabilizers, antistatic agents, antifogging
45 agents, acid scavengers, blowing agents, cling agents, lubricants, nucleating agents, slip agents, antiblocking
agents and mixtures thereof;

wherein the polypropylene composition has

50 - a melt flow rate MFR2 (230 °C) measured according to ISO 1133 of 1.0 to below 7.0 g/10min, and
- a gel content of less than 1.00 wt.-%, preferably of less than 0.80 wt.-%;

and wherein the polypropylene composition and/or the branched polypropylene (b-PP) has/have a F 30 melt strength
of 25.0 cN to 50.0 cN and a v30 melt extensibility of 210 to 300 mm/s, wherein the F30 melt strength and the v30 melt
55 extensibility are measured according to ISO 16790:2005.

12. Process for the manufacture of a foam comprising

19
EP 2 877 534 B1

(A) the process for providing of a polypropylene composition comprising a branched polypropylene (b-PP), the
process comprises at least a step (a) in which a polypropylene (PP) is reacted with a thermally decomposing
free radical-forming agent and optionally with bifunctionally unsaturated monomer(s) and/or with multifunctionally
unsaturated low molecular weight polymer(s) obtaining thereby the branched polypropylene (b-PP),
5 wherein

(i) the polypropylene (PP) has a melt flow rate MFR2 (230°C) of more than 0.5 g/10min;
(ii) the polypropylene composition and/or the branched polypropylene (b-PP) has/have a F30 melt strength
of more than 20.0 cN and a v30 melt extensibility of more than 200 mm/s, wherein the F30 melt strength
10 and the v30 melt extensibility are measured according to ISO 16790:2005, and
(iii) the polypropylene (PP) is used in the form of particles having a particle size distribution d90 of below
1,500 mm, d50 of below 1,000 mm, and a d90/d50 ratio of below 1.80,

(B) subjecting the polypropylene composition of step (A) to a foaming process obtaining thereby a foam.
15
13. Process according to claim 12, wherein the polypropylene composition comprises

(a) 95 to 99 parts by weight of a branched polypropylene (b-PP); and


(b) optionally 1 to 5 parts by weight of a polypropylene (PP’) having a melt flow rate MFR2 (230 °C) measured
20 according to ISO 1133 of more than 0.5 to 18.0 g/10min,
(c) optionally 0.005 to 5.0 parts by weight of additives (A), wherein said additives(A) are preferably selected
from the group consisting of antioxidants, metal deactivators, UV-stabilizers, antistatic agents, antifogging
agents, acid scavengers, blowing agents, cling agents, lubricants, nucleating agents, slip agents, antiblocking
agents and mixtures thereof;
25
wherein the polypropylene composition has

- a melt flow rate MFR2 (230 °C) measured according to ISO 1133 of 1.0 to below 7.0 g/10min, and
- a gel content of less than 1.00 wt.-%, preferably of less than 0.80 wt.-%;
30
and wherein the polypropylene composition and/or the branched polypropylene (b-PP) has/have a F 30 melt strength
of 25.0 cN to 50.0 cN and a v30 melt extensibility of 210 to 300 mm/s, wherein the F30 melt strength and the v30 melt
extensibility are measured according to ISO 16790:2005.

35 14. Process for the manufacture of a foam comprising the step of subjecting a polypropylene composition to a foaming
process obtaining thereby a foam, wherein the polypropylene composition comprises

(a) 95 to 99 parts by weight of a branched polypropylene (b-PP); and


(b) optionally 1 to 5 parts by weight of a polypropylene (PP’) having a melt flow rate MFR2 (230 °C) measured
40 according to ISO 1133 of more than 0.5 to 18.0 g/10min,
(c) optionally 0.005 to 5.0 parts by weight of additives (A), wherein said additives(A) are preferably selected
from the group consisting of antioxidants, metal deactivators, UV-stabilizers, antistatic agents, antifogging
agents, acid scavengers, blowing agents, cling agents, lubricants, nucleating agents, slip agents, antiblocking
agents and mixtures thereof;
45
wherein the polypropylene composition has

- a melt flow rate MFR2 (230 °C) measured according to ISO 1133 of 1.0 to below 7.0 g/10min, and
- a gel content of less than 1.00 wt.-%, preferably of less than 0.80 wt.-%;
50
and wherein the polypropylene composition and/or the branched polypropylene (b-PP) has/have a F 30 melt strength
of 25.0 cN to 50.0 cN and a v30 melt extensibility of 210 to 300 mm/s, wherein the F30 melt strength and the v30 melt
extensibility are measured according to ISO 16790:2005, wherein the polypropylene composition is obtained by a
process comprising at least a step (a) in which a polypropylene (PP) is reacted with a thermally decomposing free
55 radical-forming agent and optionally with bifunctionally unsaturated monomer(s) and/or with multifunctionally un-
saturated low molecular weight polymer(s) obtaining thereby the branched polypropylene (b-PP),
wherein

20
EP 2 877 534 B1

(i) the polypropylene (PP) has a melt flow rate MFR2 (230°C) of more than 0.5 g/10min;
(iii) the polypropylene (PP) is used in the form of particles having a particle size distribution d90 of below 1,500
mm, d50 of below 1,000 mm, and a d90/d50 ratio of below 1.80.

5 15. Foam comprising a polypropylene composition according to claim 11.

16. Use of a polypropylene (PP) having a melt flow rate MFR2 (230°C) of more than 0.5 g/10min and a particle size
distribution of d90 of below 1,500 mm, d50 of below 1,000 mm, and a d90/d50 ratio of below 1.80, in the process for
the manufacture of a branched polypropylene (b-PP) and thus in the process for the manufacture of a polypropylene
10 composition comprising the branched polypropylene (b-PP) to reduce the gel content of the branched polypropylene
(b-PP) and/or of the polypropylene composition comprising the branched polypropylene (b-PP).

17. Use according to claim 16, wherein the process is further defined according to anyone of the preceding claims 1 to 11.

15 18. Use according to claim 16 or 17, wherein the gel content is reduced in case the branched polypropylene (b-PP)
and/or the polypropylene composition comprising the branched polypropylene (b-PP) has/have a gel content of less
than 1.00 wt.-%, preferably of less than 0.80 wt.-%.

20 Patentansprüche

1. Verfahren zum Bereitstellen einer Polypropylen-Zusammensetzung, umfassend ein verzweigtes Polypropylen (b-
PP), wobei das Verfahren mindestens einen Schritt (a) umfasst, in welchem ein Polypropylen (PP) mit einem ther-
misch sich zersetzenden, freie Radikale bildenden Mittel und gegebenenfalls mit bifunktionell ungesättigtem/n Mo-
25 nomer(en) und/oder mit multifunktionell ungesättigtem/n Polymer(en) mit niederem Molekular-Gewicht umgesetzt
wird, wobei das verzweigte Polypropylen (b-PP) erhalten wird,
wobei

(a) das Polypropylen (PP) eine Schmelze-Fließ-Rate MFR2 (230°C) von mehr als 0,5 g/10 min aufweist;
30 (b) die Polypropylen-Zusammensetzung und/oder das verzweigte Polypropylen (b-PP) eine F30 Schmelze-
Festigkeit von mehr als 20,0 cN und eine v30 Schmelze-Dehnung von mehr als 200 mm/s aufweist/aufweisen,
wobei die F30 Schmelze-Festigkeit und die v30 Schmelze-Dehnung gemäß ISO 16790:2005 gemessen werden,
und
(c) das Polypropylen (PP) in Form von Teilchen mit einer Teilchen-Größen-Verteilung d90 von unter 1 500 mm,
35 d50 von unter 1 000 mm und einem d90/d50-Verhältnis von unter 1,80 verwendet wird.

2. Verfahren nach Anspruch 1, wobei das Polypropylen (PP)

(a) ein Propylen-Homopolymer ist;


40 und/oder
(b) ein lineares Polypropylen (1-PP) mit vorzugsweise einer F30 Schmelze-Festigkeit von mehr als 1,0 cN und
einer v30 Schmelze-Dehnung von unter 200 mm/s ist, wobei die F30 Schmelze-Festigkeit und die v30 Schmelze-
Dehnung gemäß ISO 16790:2005 gemessen werden.

45 3. Verfahren nach einem der vorangehenden Ansprüche, wobei

(a) das thermisch sich zersetzende, freie Radikale bildende Mittel ein Peroxid ist;
und/oder
(b) das bifunktionell ungesättigte Monomer ausgewählt ist aus der Gruppe, bestehend aus Divinyl-Verbindungen,
50 Allyl-Verbindungen und Dienen.

4. Verfahren nach einem der vorangehenden Ansprüche, wobei das Verfahren anschließend an Schritt (a) einen
weiteren Schritt (b) umfasst, in welchem zu dem verzweigten Polypropylen (b-PP) ein Polypropylen (PP’) mit einer
Schmelze-Fließ-Rate MFR2 (230°C) von 0,5 bis 18,0 g/10 min gegeben wird.
55
5. Verfahren nach Anspruch 4, wobei

(a) Schritt (b) gestartet wird, wenn mindestens 80 % der Reaktion zwischen dem Polypropylen (PP) und dem

21
EP 2 877 534 B1

thermisch sich zersetzenden, freie Radikale bildenden Mittel und gegebenenfalls dem bifunktionell ungesättigten
Monomer stattgefunden haben;
und/oder
(b) das Polypropylen (PP’) ein lineares Polypropylen (1-PP’) ist, wobei das lineare Polypropylen (1-PP’) vor-
5 zugsweise eine F30 Schmelze-Festigkeit von mehr als 1,0 cN und eine v30 Schmelze-Dehnung von unter 200
mm/s aufweist, bevorzugter eine F30 Schmelze-Festigkeit von mehr als 1,0 bis unter 68,0 cN und eine v30
Schmelze-Dehnung von unter 200 mm/s aufweist, wobei die F30 Schmelze-Festigkeit und die v30 Schmelze-
Dehnung gemäß ISO 16790:2005 gemessen werden.

10 6. Verfahren nach einem der vorangehenden Ansprüche, wobei der Schritt (a) und der wahlweise Schritt (b) in einem
Extruder ausgeführt werden, wobei der Extruder in Betriebs-Richtung vorzugsweise eine erste Misch-Zone (MZ1)
und eine zweite Misch-Zone (MZ2) umfasst, wobei weiterhin der Schritt (a) in der ersten Misch-Zone (MZ1) stattfindet,
während Schritt (b) in der zweiten Misch-Zone (MZ2) stattfindet, wobei der Extruder in Betriebs-Richtung vorzugs-
weise eine Material-Einfüll-Öffnung (FT), die erste Misch-Zone (MZ1), die zweite Misch-Zone (MZ2) und eine Düse
15 (D) umfasst, wobei zwischen der ersten Misch-Zone (MZ1) und der zweiten Misch-Zone (MZ2) eine Seiten-Material-
Einfüll-Öffnung (SFT) angeordnet ist, wobei weiterhin das Polypropylen (PP), das thermisch sich zersetzende, freie
Radikale bildende Mittel und gegebenenfalls das bifunktionell ungesättigte Monomer über die Material-Einfüll-Öff-
nung (FT) zugeführt werden und das Polypropylen (PP’) über die Seiten-Material-Einfüll-Öffnung (SFT) zugeführt
wird.
20
7. Verfahren nach Anspruch 6, wobei

(a) die Reaktion zwischen dem Polypropylen (PP) und dem thermisch sich zersetzenden, freie Radikale bilden-
den Mittel und gegebenenfalls dem bifunktionell ungesättigten Monomer in der ersten Misch-Zone (MZ1) statt-
25 findet;
und/oder
(b) nicht mehr als 10 Gew.-% von der Gesamt-Menge von dem verzweigten Polypropylen (b-PP) der Polypro-
pylen-Zusammensetzung in der zweiten Misch-Zone (MZ2) hergestellt wird.

30 8. Verfahren nach einem der vorangehenden Ansprüche 4 bis 7, wobei 1 bis 5 Gewichts-Teile von dem Polypropylen
(PP’) zu 95 bis 99 Gewichts-Teilen von verzweigtem Polypropylen (b-PP) gegeben werden, vorzugsweise wobei 1
bis 3 Gewichts-Teile von dem Polypropylen (PP’) zu 97 bis 99 Gewichts-Teilen von verzweigtem Polypropylen (b-
PP) gegeben werden, bevorzugter wobei 2 Gewichts-Teile von dem Polypropylen (PP’) zu 98 Gewichts-Teilen von
verzweigtem Polypropylen (b-PP) gegeben werden.
35
9. Verfahren nach einem der vorangehenden Ansprüche, wobei

(a) das Polypropylen (PP’) mindestens ein Additiv (A) umfasst, ausgewählt aus der Gruppe, bestehend aus
Antioxidantien, Metall-Desaktivatoren, UV-Stabilisatoren, antistatischen Mitteln, Antischleier-Mitteln, Säure-
40 Fängern, Treib-Mitteln, Haft-Mitteln, Schmier-Mitteln, Nukleierungs-Mitteln, Gleit-Mitteln, Antiblockierungs-Mit-
teln und Gemischen davon;
und/oder
(b) das verzweigte Polypropylen (b-PP) frei von Additiven (A) ist.

45 10. Verfahren nach einem der vorangehenden Ansprüche, wobei die erhaltene Polypropylen-Zusammensetzung auf-
weist

(a) eine F30 Schmelze-Festigkeit von 25,0 cN bis 50,0 cN und eine v30 Schmelze-Dehnung von 210 bis 300 mm/s;
und/oder
50 (b) einen Gel-Gehalt von weniger als 1,00 Gew.-%, vorzugsweise von weniger als 0,80 Gew.-%.

11. Polypropylen-Zusammensetzung, erhältlich durch das Verfahren nach einem der Ansprüche 1 bis 10, umfassend

(a) 95 bis 99 Gewichts-Teile von einem verzweigten Polypropylen (b-PP);


55 (b) gegebenenfalls 1 bis 5 Gewichts-Teile von einem Polypropylen (PP’) mit einer Schmelze-Fließ-Rate MFR2
(230°C), gemessen gemäß ISO 1133, von mehr als 0,5 bis 18,0 g/10 min; und
(c) gegebenenfalls 0,005 bis 5,0 Gewichts-Teile von Additiven (A), wobei die Additive (A) vorzugsweise aus-
gewählt sind aus der Gruppe, bestehend aus Antioxidantien, Metall-Desaktivatoren, UV-Stabilisatoren, antista-

22
EP 2 877 534 B1

tischen Mitteln, Antischleier-Mitteln, Säure-Fängern, Treib-Mitteln, Haft-Mitteln, Schmier-Mitteln, Nukleierungs-


Mitteln, Gleit-Mitteln, Antiblockierungs-Mitteln und Gemischen davon;

wobei die Polypropylen-Zusammensetzung aufweist


5
- eine Schmelze-Fließ-Rate MFR2 (230°C), gemessen gemäß ISO 1133, von 1,0 bis unter 7,0 g/10 min, und
- einen Gel-Gehalt von weniger als 1,00 Gew.-%, vorzugsweise von weniger als 0,80 Gew.-%;

und wobei die Polypropylen-Zusammensetzung und/oder das verzweigte Polypropylen (b-PP) eine F30 Schmelze-
10 Festigkeit von 25,0 cN bis 50,0 cN und eine v30 Schmelze-Dehnung von 210 bis 300 mm/s aufweist/aufweisen,
wobei die F30 Schmelze-Festigkeit und die v30 Schmelze-Dehnung gemäß ISO 16790:2005 gemessen werden.

12. Verfahren zur Herstellung von einem Schaum, umfassend

15 (A) das Verfahren zum Bereitstellen einer Polypropylen-Zusammensetzung, umfassend ein verzweigtes Poly-
propylen (b-PP), wobei das Verfahren mindestens einen Schritt (a) umfasst, in welchem ein Polypropylen (PP)
mit einem thermisch sich zersetzenden, freie Radikale bildenden Mittel und gegebenenfalls mit bifunktionell
ungesättigtem/n Monomer(en) und/oder mit multifunktionell ungesättigtem/n Polymer(en) mit niederem Mole-
kular-Gewicht umgesetzt wird, wobei das verzweigte Polypropylen (b-PP) erhalten wird,
20 wobei

(i) das Polypropylen (PP) eine Schmelze-Fließ-Rate MFR2 (230°C) von mehr als 0,5 g/10 min aufweist;
(ii) die Polypropylen-Zusammensetzung und/oder das verzweigte Polypropylen (b-PP) eine F30 Schmelze-
Festigkeit von mehr als 20,0 cN und eine v30 Schmelze-Dehnung von mehr als 200 mm/s aufweist/aufwei-
25 sen, wobei die F30 Schmelze-Festigkeit und die v30 Schmelze-Dehnung gemäß ISO 16790:2005 gemessen
werden, und
(iii) das Polypropylen (PP) in Form von Teilchen mit einer Teilchen-Größen-Verteilung d90 von unter 1 500
mm, d50 von unter 1 000 mm, und einem d90/d50-Verhältnis von unter 1,80 verwendet wird,

30 (B) Unterziehen der Polypropylen-Zusammensetzung von Schritt (A) einem Schäumungs-Verfahren, wobei ein
Schaum erhalten wird.

13. Verfahren nach Anspruch 12, wobei die Polypropylen-Zusammensetzung umfasst

35 (a) 95 bis 99 Gewichts-Teile von einem verzweigten Polypropylen (b-PP) ; und


(b) gegebenenfalls 1 bis 5 Gewichts-Teile von einem Polypropylen (PP’) mit einer Schmelze-Fließ-Rate MFR2
(230°C), gemessen gemäß ISO 1133, von mehr als 0,5 bis 18,0 g/10 min,
(c) gegebenenfalls 0,005 bis 5,0 Gewichts-Teile von Additiven (A), wobei die Additive (A) vorzugsweise aus-
gewählt sind aus der Gruppe, bestehend aus Antioxidantien, Metall-Desaktivatoren, UV-Stabilisatoren, antista-
40 tischen Mitteln, Antischleier-Mitteln, Säure-Fängern, Treib-Mitteln, Haft-Mitteln, Schmier-Mitteln, Nukleierungs-
Mitteln, Gleit-Mitteln, Antiblockierungs-Mitteln und Gemischen davon;

wobei die Polypropylen-Zusammensetzung aufweist

45 - eine Schmelze-Fließ-Rate MFR2 (230°C), gemessen gemäß ISO 1133, von 1,0 bis unter 7,0 g/10 min, und
- einen Gel-Gehalt von weniger als 1,00 Gew.-%, vorzugsweise von weniger als 0,80 Gew.-%;

und wobei die Polypropylen-Zusammensetzung und/oder das verzweigte Polypropylen (b-PP) eine F30 Schmelze-
Festigkeit von 25,0 cN bis 50,0 cN und eine v30 Schmelze-Dehnung von 210 bis 300 mm/s aufweist/aufweisen,
50 wobei die F30 Schmelze-Festigkeit und die v30 Schmelze-Dehnung gemäß ISO 16790:2005 gemessen werden.

14. Verfahren zur Herstellung von einem Schaum, umfassend den Schritt des Unterziehens einer Polypropylen-Zusam-
mensetzung einem Schäumungs-Verfahren, wobei ein Schaum erhalten wird, wobei die Polypropylen-Zusammen-
setzung umfasst
55
(a) 95 bis 99 Gewichts-Teile von einem verzweigten Polypropylen (b-PP) ; und
(b) gegebenenfalls 1 bis 5 Gewichts-Teile von einem Polypropylen (PP’) mit einer Schmelze-Fließ-Rate MFR2
(230°C), gemessen gemäß ISO 1133, von mehr als 0,5 bis 18,0 g/10 min,

23
EP 2 877 534 B1

(c) gegebenenfalls 0,005 bis 5,0 Gewichts-Teile von Additiven (A), wobei die Additive (A) vorzugsweise aus-
gewählt sind aus der Gruppe, bestehend aus Antioxidantien, Metall-Desaktivatoren, UV-Stabilisatoren, antista-
tischen Mitteln, Antischleier-Mitteln, Säure-Fängern, Treib-Mitteln, Haft-Mitteln, Schmier-Mitteln, Nukleierungs-
Mitteln, Gleit-Mitteln, Antiblockierungs-Mitteln und Gemischen davon;
5
wobei die Polypropylen-Zusammensetzung aufweist

- eine Schmelze-Fließ-Rate MFR2 (230°C), gemessen gemäß ISO 1133, von 1,0 bis unter 7,0 g/10 min, und
- einen Gel-Gehalt von weniger als 1,00 Gew.-%, vorzugsweise von weniger als 0,80 Gew.-%;
10
und wobei die Polypropylen-Zusammensetzung und/oder das verzweigte Polypropylen (b-PP) eine F30 Schmelze-
Festigkeit von 25, 0 cN bis 50, 0 cN und eine v30 Schmelze-Dehnung von 210 bis 300 mm/s aufweist/aufweisen,
wobei die F30 Schmelze-Festigkeit und die v30 Schmelze-Dehnung gemäß ISO 16790:2005 gemessen werden,
wobei die Polypropylen-Zusammensetzung durch ein Verfahren erhalten wird, umfassend mindestens einen Schritt
15 (a), in welchem ein Polypropylen (PP) mit einem thermisch sich zersetzenden, freie Radikale bildenden Mittel und
gegebenenfalls mit bifunktionell ungesättigtem/n Monomer/n und/oder mit multifunktionell ungesättigtem/n Poly-
mer/n mit niederem Molekular-Gewicht umgesetzt wird, wobei das verzweigte Polypropylen (b-PP) erhalten wird,
wobei

20 (i) das Polypropylen (PP) eine Schmelze-Fließ-Rate MFR2 (230°C) von mehr als 0,5 g/10 min aufweist;
(ii) das Polypropylen (PP) in Form von Teilchen mit einer Teilchen-Größen-Verteilung d90 von unter 1 500 mm,
d50 von unter 1 000 mm und einem d90/d50-Verhältnis von unter 1,80 verwendet wird.

15. Schaum, umfassend eine Polypropylen-Zusammensetzung nach Anspruch 11.


25
16. Verwendung von einem Polypropylen (PP) mit einer Schmelze-Fließ-Rate MFR2 (230°C) von mehr als 0,5 g/10 min
und einer Teilchen-Größen-Verteilung d90 von unter 1 500 mm, d50 von unter 1 000 mm und einem d90/d50-Verhältnis
von unter 1,80, in dem Verfahren zur Herstellung von einem verzweigten Polypropylen (b-PP) und somit in dem
Verfahren zur Herstellung von einer Polypropylen-Zusammensetzung, umfassend das verzweigte Polypropylen (b-
30 PP) zum Vermindern des Gel-Gehalts von dem verzweigten Polypropylen (b-PP) und/oder von der Polypropylen-
Zusammensetzung, umfassend das verzweigte Polypropylen (b-PP).

17. Verwendung nach Anspruch 16, wobei das Verfahren weiterhin nach einem der vorangehenden Ansprüche 1 bis
11 definiert ist.
35
18. Verwendung nach Anspruch 16 oder 17, wobei der Gel-Gehalt vermindert ist, falls das verzweigte Polypropylen (b-
PP) und/oder die Polypropylen-Zusammensetzung, umfassend das verzweigte Polypropylen (b-PP), einen Gel-
Gehalt von weniger als 1,00 Gew.-%, vorzugsweise von weniger als 0,80 Gew.-%, aufweist/aufweisen.

40
Revendications

1. Procédé pour former une composition de polypropylène comprenant un polypropylène ramifié (b-PP), lequel procédé
comprend au moins une étape (a) dans laquelle un polypropylène (PP) est mis à réagir avec un agent formant des
45 radicaux libres se décomposant thermiquement et éventuellement avec un ou plusieurs monomère(s) à insaturation
bifonctionnelle et/ou avec un ou plusieurs polymère(s) de faible masse moléculaire à insaturation multifonctionnelle,
ce qui donne ainsi le polypropylène ramifié (b-PP), dans lequel

(a) le polypropylène (PP) présente un indice de fluage MFR2 (230°C) supérieur à 0,5 g/10 min ;
50 (b) la composition de polypropylène et/ou le polypropylène ramifié (b-PP) présente(nt) une résistance à l’état
fondu F30 supérieure à 20,0 cN et une extensibilité à l’état fondu v30 supérieure à 200 mm/s, la résistance à
l’état fondu F30 et l’extensibilité à l’état fondu v30 étant mesurées conformément à la norme ISO 16790:2005, et
(c) le polypropylène (PP) est utilisé sous la forme de particules présentant une distribution de granulométrie
d90 inférieure à 1500 mm, une valeur d50 inférieure à 1000 mm, et un rapport d90/d50 inférieur à 1, 80.
55
2. Procédé selon la revendication 1, dans lequel le polypropylène (PP)

(a) est un homopolymère de propylène ;

24
EP 2 877 534 B1

et/ou
(b) est un polypropylène linéaire (l-PP) présentant de préférence une résistance à l’état fondu F30 supérieure
à 1,0 cN et une extensibilité à l’état fondu v30 inférieure à 200 mm/s, la résistance à l’état fondu F30 et l’extensibilité
à l’état fondu v30 étant mesurées conformément à la norme ISO 16790:2005.
5
3. Procédé selon l’une quelconque des revendications précédentes, dans lequel

(a) l’agent formant des radicaux libres se décomposant thermiquement est un peroxyde ;
et/ou
10 (b) le monomère à insaturation bifonctionnelle est choisi dans l’ensemble constitué par les composés divinyli-
ques, les composés allyliques et les diènes.

4. Procédé selon l’une quelconque des revendications précédentes, lequel procédé comprend, suite à l’étape (a), une
autre étape (b) dans laquelle un polypropylène (PP’) présentant un indice de fluage MFR2 (230°C) de 0,5 à 18,0
15 g/10 min est ajouté au polypropylène ramifié (b-PP).

5. Procédé selon la revendication 4, dans lequel

(a) l’étape (b) est initiée quand au moins 80 % de la réaction entre le polypropylène (PP) et l’agent formant des
20 radicaux libres se décomposant thermiquement et éventuellement le monomère à insaturation bifonctionnelle
ont eu lieu ;
et/ou
(b) le polypropylène (PP’) est un polypropylène linéaire (l-PP’), lequel polypropylène linéaire (l-PP’) présente
de préférence une résistance à l’état fondu F30 supérieure à 1,0 cN et une extensibilité à l’état fondu v30 inférieure
25 à 200 mm/s, plus préférablement présente une résistance à l’état fondu F30 de plus de 1,0 à moins de 68,0 cN
et une extensibilité à l’état fondu v30 inférieure à 200 mm/s, la résistance à l’état fondu F30 et l’extensibilité à
l’état fondu v30 étant mesurées conformément à la norme ISO 16790:2005.

6. Procédé selon l’une quelconque des revendications précédentes, dans lequel l’étape (a) et l’étape optionnelle (b)
30 sont effectuées dans une extrudeuse, laquelle extrudeuse comprend de préférence, dans la direction de son fonc-
tionnement, une première zone de mélange (MZ1) et une deuxième zone de mélange (MZ2), dans lequel en outre
l’étape (a) a lieu dans la première zone de mélange (MZ1) tandis que l’étape (b) a lieu dans la deuxième zone de
mélange (MZ2), de préférence l’extrudeuse comprend, dans la direction de son fonctionnement, une goulotte d’ali-
mentation (FT), la première zone de mélange (MZ1), la deuxième zone de mélange (MZ2) et une filière (D), une
35 goulotte d’alimentation latérale (SFT) étant placée entre la première zone de mélange (MZ1) et la deuxième zone
de mélange (MZ2), dans lequel en outre le polypropylène (PP), l’agent formant des radicaux libres se décomposant
thermiquement et éventuellement le monomère à insaturation bifonctionnelle sont introduits via la goulotte d’ali-
mentation (FT) et le polypropylène (PP’) est introduit via la goulotte d’alimentation latérale (SFT).

40 7. Procédé selon la revendication 6, dans lequel

(a) la réaction entre le polypropylène (PP) et l’agent formant des radicaux libres se décomposant thermiquement
et éventuellement le monomère à insaturation bifonctionnelle a lieu dans la première zone de mélange (MZ1) ;
et/ou
45 (b) au plus 10 % en poids de la quantité totale du polypropylène ramifié (b-PP) de la composition de polypropylène
sont produits dans la deuxième zone de mélange (MZ2).

8. Procédé selon l’une quelconque des revendications 4 à 7, dans lequel 1 à 5 parties en poids du polypropylène (PP’)
sont ajoutées à 95 à 99 parties en poids du polypropylène ramifié (b-PP), de préférence dans lequel 1 à 3 parties
50 en poids du polypropylène (PP’) sont ajoutées à 97 à 99 parties en poids du polypropylène ramifié (b-PP), plus
préférablement dans lequel 2 parties en poids du polypropylène (PP’) sont ajoutées à 98 parties en poids du
polypropylène ramifié (b-PP).

9. Procédé selon l’une quelconque des revendications précédentes, dans lequel


55
(a) le polypropylène (PP’) comprend au moins un additif (A) choisi dans l’ensemble constitué par les antioxydants,
les désactivateurs métalliques, les stabilisants UV, les agents antistatiques, les agents anti-voile, les piégeurs
d’acide, les agents d’expansion, les agents d’adhésion, les lubrifiants, les agents de nucléation, les agents de

25
EP 2 877 534 B1

glissement, les agents antiblocage et leurs mélanges ;


et/ou
(b) le polypropylène ramifié (b-PP) est exempt d’additifs (A) .

5 10. Procédé selon l’une quelconque des revendications précédentes, dans lequel la composition de polypropylène
résultante présente

(a) une résistance à l’état fondu F30 de 25,0 cN à 50,0 cN et une extensibilité à l’état fondu v30 de 210 à 300 mm/s ;
et/ou
10 (b) une teneur en gel inférieure à 1,00 % en poids, de préférence inférieure à 0,80 % en poids.

11. Composition de polypropylène pouvant être obtenue par le procédé de l’une quelconque des revendications 1 à
10, comprenant

15 (a) 95 à 99 parties en poids d’un polypropylène ramifié (b-PP) ;


(b) éventuellement 1 à 5 parties en poids d’un polypropylène (PP’) présentant un indice de fluage MFR2 (230°C),
mesuré conformément à la norme ISO 1133, de plus de 0,5 à 18,0 g/10 min ; et
(c) éventuellement 0,005 à 5,0 parties en poids d’additifs (A), lesdits additifs (A) étant de préférence choisis
dans l’ensemble constitué par les antioxydants, les désactivateurs métalliques, les stabilisants UV, les agents
20 antistatiques, les agents anti-voile, les piégeurs d’acide, les agents d’expansion, les agents d’adhésion, les
lubrifiants, les agents de nucléation, les agents de glissement, les agents antiblocage et leurs mélanges ;

laquelle composition de polypropylène présente

25 - un indice de fluage MFR2 (230°C), mesuré conformément à la norme ISO 1133, de 1,0 à moins de 7,0 g/10
min, et
- une teneur en gel inférieure à 1,00 % en poids, de préférence inférieure à 0,80 % en poids ;

laquelle composition de polypropylène et/ou dans laquelle le polypropylène ramifié (b-PP) présente(nt) une résis-
30 tance à l’état fondu F30 de 25, 0 cN à 50, 0 cN et une extensibilité à l’état fondu v30 de 210 à 300 mm/s, la résistance
à l’état fondu F30 et l’extensibilité à l’état fondu v30 étant mesurées conformément à la norme ISO 16790:2005.

12. Procédé pour la fabrication d’une mousse comprenant

35 (A) un procédé pour se procurer une composition de polypropylène comprenant un polypropylène ramifié (b-
PP), lequel procédé comprend au moins une étape (a) dans laquelle un polypropylène (PP) est mis à réagir
avec un agent formant des radicaux libres se décomposant thermiquement et éventuellement avec un ou
plusieurs monomère(s) à insaturation bifonctionnelle et/ou avec un ou plusieurs polymère(s) de faible masse
moléculaire à insaturation multifonctionnelle, ce qui donne ainsi le polypropylène (ramifié (b-PP),
40 dans lequel

(i) le polypropylène (PP) présente un indice de fluage MFR2 (230°C) supérieur à 0,5 g/10 min ;
(ii) la composition de polypropylène et/ou le polypropylène ramifié (b-PP) présente(nt) une résistance à
l’état fondu F30 supérieure à 20,0 cN et une extensibilité à l’état fondu v30 supérieure à 200 mm/s, la
45 résistance à l’état fondu F30 et l’extensibilité à l’état fondu v30 étant mesurées conformément à la norme
ISO 16790:2005, et
(iii) le polypropylène (PP) est utilisé sous la forme de particules présentant une distribution de granulométrie
d90 inférieure à 1500 mm, une valeur d50 inférieure à 1000 mm, et un rapport d90/d50 inférieur à 1,80,

50 (B) la soumission de la composition de polypropylène de l’étape (A) à un traitement d’expansion, ce qui donne
ainsi une mousse.

13. Procédé selon la revendication 12, dans lequel la composition de polypropylène comprend

55 (a) 95 à 99 parties en poids d’un polypropylène ramifié (b-PP) ; et


(b) éventuellement 1 à 5 parties en poids d’un polypropylène (PP’) présentant un indice de fluage MFR2 (230°C),
mesuré conformément à la norme ISO 1133, de plus de 0,5 à 18,0 g/10 min ;
(c) éventuellement 0,005 à 5,0 parties en poids d’additifs (A), lesdits additifs (A) étant de préférence choisis

26
EP 2 877 534 B1

dans l’ensemble constitué par les antioxydants, les désactivateurs métalliques, les stabilisants UV, les agents
antistatiques, les agents anti-voile, les piégeurs d’acide, les agents d’expansion, les agents d’adhésion, les
lubrifiants, les agents de nucléation, les agents de glissement, les agents antiblocage et leurs mélanges ;

5 dans lequel la composition de polypropylène présente

- un indice de fluage MFR2 (230°C), mesuré conformément à la norme ISO 1133, de 1,0 à moins de 7,0 g/10
min, et
- une teneur en gel inférieure à 1,00 % en poids, de préférence inférieure à 0,80 % en poids ;
10
et dans lequel la composition de polypropylène et/ou le polypropylène ramifié (b-PP) présente(nt) une résistance
à l’état fondu F30 de 25,0 cN à 50,0 cN et une extensibilité à l’état fondu v30 de 210 à 300 mm/s, la résistance à
l’état fondu F30 et l’extensibilité à l’état fondu v30 étant mesurées conformément à la norme ISO 16790:2005.

15 14. Procédé pour la fabrication d’une mousse, comprenant l’étape de soumission d’une composition de polypropylène
à un traitement d’expansion, ce qui donne ainsi une mousse, dans lequel la composition de polypropylène comprend

(a) 95 à 99 parties en poids d’un polypropylène ramifié (b-PP) ; et


(b) éventuellement 1 à 5 parties en poids d’un polypropylène (PP’) présentant un indice de fluage MFR2 (230°C),
20 mesuré conformément à la norme ISO 1133, de plus de 0,5 à 18,0 g/10 min ; et
(c) éventuellement 0,005 à 5,0 parties en poids d’additifs (A), lesdits additifs (A) étant de préférence choisis
dans l’ensemble constitué par les antioxydants, les désactivateurs métalliques, les stabilisants UV, les agents
antistatiques, les agents anti-voile, les piégeurs d’acide, les agents d’expansion, les agents d’adhésion, les
lubrifiants, les agents de nucléation, les agents de glissement, les agents antiblocage et leurs mélanges ;
25
dans lequel la composition de polypropylène présente

- un indice de fluage MFR2 (230°C), mesuré conformément à la norme ISO 1133, de 1,0 à moins de 7,0 g/10
min, et
30 - une teneur en gel inférieure à 1,00 % en poids, de préférence inférieure à 0,80 % en poids ;

et dans lequel la composition de polypropylène et/ou le polypropylène ramifié (b-PP) présente(nt) une résistance
à l’état fondu F30 de 25,0 cN à 50,0 cN et une extensibilité à l’état fondu v30 de 210 à 300 mm/s, la résistance à
l’état fondu F30 et l’extensibilité à l’état fondu v30 étant mesurées conformément à la norme ISO 16790:2005, et
35 dans lequel la composition de polypropylène est obtenue par un procédé comprenant au moins une étape (a) dans
laquelle un polypropylène (PP) est mis à réagir avec un agent formant des radicaux libres se décomposant thermi-
quement et éventuellement avec un ou plusieurs monomère(s) à insaturation bifonctionnelle et/ou avec un ou
plusieurs polymère(s) de faible masse moléculaire à insaturation multifonctionnelle, ce qui donne ainsi le polypro-
pylène (ramifié (b-PP),
40 dans lequel

(i) le polypropylène (PP) présente un indice de fluage MFR2 (230°C) supérieur à 0,5 g/10 min ;
(ii) le polypropylène (PP) est utilisé sous la forme de particules présentant une distribution de granulométrie
d90 inférieure à 1500 mm, une valeur d50 inférieure à 1000 mm, et un rapport d90/d50 inférieur à 1, 80.
45
15. Mousse comprenant une composition de polypropylène selon la revendication 11.

16. Utilisation d’un polypropylène (PP) présentant un indice de fluage MFR2 (230°C) supérieur à 0,5/10 min et une
distribution de granulométrie d90 inférieure à 1500 mm, une valeur d50 inférieure à 1000 mm, et un rapport d90/d50
50 inférieur à 1,80, dans le procédé de fabrication d’un polypropylène ramifié (b-PP) et donc dans le procédé de
fabrication d’une composition de polypropylène comprenant le polypropylène ramifié (b-PP), pour réduire la teneur
en gel du polypropylène ramifié (b-PP) et/ou de la composition de polypropylène comprenant le polypropylène
ramifié (b-PP).

55 17. Utilisation selon la revendication 16, dans laquelle le procédé est en outre défini selon l’une quelconque des reven-
dications 1 à 11.

18. Utilisation selon la revendication 16 ou 17, dans lequel la teneur en gel est réduite dans le cas où le polypropylène

27
EP 2 877 534 B1

ramifié (b-PP) et/ou la composition de polypropylène comprenant le polypropylène ramifié (b-PP) présente (nt) une
teneur en gel inférieure à 1,00 % en poids, de préférence inférieure à 0,80 % en poids.

10

15

20

25

30

35

40

45

50

55

28
EP 2 877 534 B1

REFERENCES CITED IN THE DESCRIPTION

This list of references cited by the applicant is for the reader’s convenience only. It does not form part of the European
patent document. Even though great care has been taken in compiling the references, errors or omissions cannot be
excluded and the EPO disclaims all liability in this regard.

Patent documents cited in the description

• EP 0879830 A [0004] • EP 0787750 A [0085]


• EP 1892264 A [0016] • EP 0890612 A2 [0085]
• EP 0879830 A1 [0016] [0085] • DE 3539352 [0099]

Non-patent literature cited in the description

• H. E. NAGUIB ; C. B. PARK ; N. REICHELT. Fun- • S. T. LEE. Foam Extrusion. Technomic Publishing,


damental foaming mechanisms governing the vol- 2000 [0099]
ume expansion of extruded polypropylene foams. • M. H. WAGNER. Rheotens-Mastercurves and Draw-
Journal of Applied Polymer Science, 2004, vol. 91, ability of Polymer Melts. Polymer Engineering and
2661-2668 [0099] Sience, vol. 36, 925-935 [0110]

29

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