Title of Invention

PROPYLENE POLYMER OBTAINED BY SINGLE SITE CATALYST POLYMERIZATION AND PROCESS FOR ITS PRODUCTION

Abstract A polypropylene with a low amount of impurities, in particular a low amount of aluminum and boron residues.
Full Text Propylene polymer composition
The present invention is related to a new propylene polymer having a low
amount of impurities as well as to the process of the same and its use.
Conventional polymers contaminated with impurities - although sometimes
in rather low levels - make the polymer unsuitable for certain end
applications such as capacitor films or for certain food or medical
applications where a high purity is needed. The ash content of the polymer
product is one of the indicators of the undesired impurities. The impurities
include metallic and non-metallic impurities, which are often originating
from the catalyst system used for the polymerization, particularly
aluminum, titanium, silicon, halogen (such as CI and F) and boron residues.
This specific problem may arise especially in cases where supported
metallocene catalysts are employed since due to the low activities of the
same usually considerably high amounts of catalyst are needed. As a
negative side effect, the polymer product is contaminated with high amount
of residual catalyst components. To achieve very low levels of these
residues, the polymer products are often washed after production.
Of course for high demanding applications not only the amount of
impurities should be considered but also the mechanical properties as for
example the stiffness of the product.
WO 02/16455 discloses a propylene homopolymer with a molecular weight
distribution (MWD) of 1.7 to 5. The pentad content of this polymer is
higher than 93 % and the xylene solubles (XS) is lower than 1 wt.-%.
Moreover, the aluminum and chloride levels in this propylene
homopolymer are lower than 25 ppm. The polymer is prepared by a two-
stage process using metallocene catalyst supported on fluorinated silica in
the presence of a highly fluorinated trisarylboron activator compound. The
aluminum and chloride level in this propylene homopolymer is reduced i.a.
due to the use of a boron-based cocatalyst, which in turn can provide boron
residues to the polymer.
The object of the present invention is to provide further propylene
polymers having a low amount of impurities making the product suitable
for high demanding end applications as for example capacitor films, food

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packaging or medical packaging articles. Preferably propylene polymer is
suitable for end applications requiring good mechanical properties as inter
alia a high stiffness.
The finding of the present invention is that a propylene polymer can be
produced which contains significantly reduced amounts of residues in the
final propylene polymer enabling the use of the polymer in demanding end
applications without that any washing step is needed. Also a method using
a very feasible catalyst system for producing such polymer is provided.
Hence, the patent invention provides a propylene polymer which
particularly comprises a low Al-content and advantageously low amounts
of other residues mainly originating from the catalyst. Accordingly, the
propylene polymer of the invention comprises an aluminum residue content
of less than 25 ppm, more preferably less than 10 ppm, still more
preferably less than 9 ppm and boron residue content of less than 25 ppm,
more preferably less than 10 ppm, still more preferably less than 9 ppm.
Such a polymer with very low amounts of metallic or non-metallic residues
arising from the catalyst component makes it suitable for high demanding
applications, wherein the presence of such residues should be avoided, as
for example for capacitor films or for food packaging or medical packaging
articles.
In a very preferable embodiment the propylene polymer comprises the
above low content of Al- and B-residues and additionally a reduced amount
of silicon (Si) residues or chlorine (CI) residues or a reduced amount of
both silicon and chlorine residues. Preferably the silicon residues content in
the propylene polymer is less than 10 ppm, more preferably less than 5
ppm. Depending on the desired end application, the polypropylene polymer
may contain Si-residues even less than 1 ppm. The chlorine content in the
propylene polymer is less than 10 ppm, more preferably less than 5 ppm.
Depending on the desired end application the polymer propylene of the
invention may contain even as low as 1 ppm of Cl-residues.
In a further embodiment the total amount of aluminum, boron and silicon
residues is less than 10 ppm. In another embodiment the total amount of Al,
B, Si and CI is less than 15 ppm, more preferably less than 10 ppm.

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The terms "aluminium (Al), boron (B), chlorine (CI) or silicon (Si)
content" or "A1-, B-, CI- or Si-residue" used above and below mean any
residues of Al, B, CI and Si, in elementary or non-elementary form (e.g.
ionic/non-ionic form, such as in a form of an oxide) that are mainly
originating from the catalyst and can be recovered from the propylene
polymer. These residues may be determined using the methods as defined
later below under "Determination methods and definitions".
In a preferred embodiment the propylene polymer is avoid of any boron
residues that originate from the catalyst system. The catalyst system
includes one or more catalyst components selected from one or more
catalytically active component and optionally one or more activators as the
cocatalyst. The components can be combined, e.g. supported on a carrier
material, before the catalyst system is subjected to a polymerization reactor
or they can be added separately to the polymerization reactor.
The purity of the propylene polymer can be further characterized by the
amount of its volatiles. The volatiles are substances being driven off as
vapor at room or slightly elevated temperatures, from a polymer. Hence, it
is preferred that the volatiles content is lower than 400 ppm, more
preferably lower than 300 ppm, still more preferred lower than 200 ppm.
The volatiles content may be determined by the method described later
below under "Determination methods and definitions".
Not only the amount of volatiles, but preferably also the amount of non-
volatile residues may significantly be reduced in the propylene polymer of
the invention. The ash content is the non-volatile inorganic matter of a
composition which remains after subjecting it to a high decomposition
temperature. The ash content may be determined by the method described
later below under "Determination methods and definitions" It is in
particular preferred that the ash content of the propylene polymer is less
than 50 ppm, more preferably less than 40 ppm and most preferably less
than 30 ppm.
In a preferable embodiment, especially for the above mentioned high
demanding applications, the propylene polymer is a high crystalline
propylene polymer. A high crystalline propylene polymer is characterized
by a high stereoregularity, i.e. high isotacticity. Generally, a high isotactic

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propylene polymer is preferred as it has better mechanical properties, in
particular an improved stiffness. Therefore, it is preferred that the
propylene polymer has an isotacticity expressed in mmmm pentad
concentration of at least 0.940, more preferably of at least 0.945 and still
more preferably of at least 0.950, determined by NMR-spectroscopy (for
the determination method see below under "Determination methods and
definitions").
Xylene solubles a part of the polymer soluble in cold xylene determined by
dissolution in boiling xylene and letting the insoluble part crystallize from
the cooling solution (for the method see below "Determination methods and
definitions"). The xylene solubles fraction contains polymer chains with
low molecular weight and low stereo-regularity. Hence, as a preferable
embodiment of the invention the propylene polymer having a high
crystallinity has xylene solubles below 2.0 wt.-%, more preferably below
1.5 wt.-% and still more preferably below 1.0 wt.-%.
The molecular weight distribution (MWD) (also determined herein as
polydispersity) is the relation between the numbers of molecules in a
polymer and the individual chain length. The molecular weight distribution
can be measured e.g. by gel permeation chromatography (GPC), whereby it
is expressed as the ratio of weight average molecular weight (Mw) and
number average molecular weight (Mn). Number average molecular weight
(Mn) and weight average molecular weight (Mw) as well as the molecular
weight distribution (MWD) are determined according to ISO 16014.
As a broad molecular weight distribution improves the processability of the
propylene polymer, therefore, advantageously the polydispersity (Mw/Mn)
is up to 20, preferably up to 10, more preferably up to 8. In an alternative
embodiment the polydispersity (Mw/Mn) is between 1 to 8.
Moreover, the molecular weight of a polymer can be further expressed by
way of its melt flow rate (MFR). The melt flow rate (MFR) mainly depends
on the average molecular weight. An increase in molecular weight means a
decrease in the MFR-value.
The melt flow rate MFR is measured in g/10 min of the polymer discharged
under specific temperature and pressure conditions and is the measure of a

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viscosity of a polymer. Melt flow rate measured under a load of 2.16 kg
(ISO 1133) is denoted as MFR2.
It is preferred that the propylene polymer has an MFR2 of up to 10 g/10
min, more preferably up to 6 g/10 min, still more preferably up to 4 g/10
min. A preferred range for the MFR2 is 1 to 10 g/10 min.
The propylene polymer includes both homo- and copolymers of propylene.
A homopolymer according to this invention has less than 0.2 wt.-%, more
preferably less than 0.1 wt.-%, still more preferably less than 0.05 wt.-%,
yet more preferably less than 0.005 wt.-%, other alpha-olefins than
propylene in the polymer. Most preferred no other alpha-olefins are
detectable.
In case the propylene polymer is a propylene copolymer, the copolymer is
preferably a random propylene copolymer. The comonomers can be
selected from the list consisting of ethylene, C4-alpha-olefin, C5-alpha-
olefin, C6.alpha-olefin, C7-alpha-olefin, Cg-alpha-olefin, C9-alpha-olefin,
Cio-alpha-olefin, Cn-alpha-olefin and C12-alpha-olefm. The alpha-olefins
can be linear, branched, aliphatic cyclic or aromatic cyclic alpha-olefins.
Preferably, the comonomer is ethylene. The amount of the comonomer is
not limited and e.g. conventionally used amounts can be used deoending on
the desired end application. In one embodiment the content of the
comonomer in the propylene copolymer may be up to 2 wt.-%, preferably
up to 1.5 wt.-%. In another embodiment lower amounts e.g. up to 0.8 wt.-
%, preferably up to 0.5 wt.-% may be desired.
Preferably the propylene polymer is a homopolymer.
The invention further covers both unimodal and multimodal propylene
polymers with respect to the molecular weight distribution (MWD).
A propylene polymer with a broad molecular weight distribution (MWD) may be
unimodal (very broad single maxima) or multimodal, preferably bimodal, with
respect to the weight average molecular weight distribution (MWD).
"Multimodal" or "multimodal distribution" describes a frequency
distribution that has several relative maxima. In particular, the expression
"modality of a polymer" refers to the form of its molecular weight

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distribution (MWD) curve, i.e. the appearance of the graph of the polymer
weight fraction as a function of its molecular weight.
The molecular weight distribution (MWD) of polymer produced in a single
polymerization stage using a single monomer mixture, a single
polymerization catalyst and a single set of process conditions (i.e.
temperature, pressure, etc.) shows a single maximum the breadth of which
depends on catalyst choice, reactor choice, process conditions, etc., i.e.
such a polymer is unimodal.
As an alternative for a unimodal propylene, the invention covers also a
propylene polymer which comprises at least the two components
(i) a propylene homopolymer or copolymer and
(ii) another propylene homopolymer or copolymer
which components (i) and (ii) are different with respect to the weight
average molecular weight (Mw) and/or in the comonomer distribution.
If component (i) or component (ii) or both are copolymers, these are
preferably random copolymers. Furthermore, the components (i) and (ii)
may have the same or different comonomer contents. In case of different
comonomer contents the propylene polymer has multimodality with respect
to the comonomer distribution.
It is preferred that one of the components (i) and (ii) has a lower molecular
weight and thus higher MFR than the other of components (i) and (ii), i.e. than
the higher molecular weight component. Accordingly, as a further embodiment,
at least a bimodal propylene polymer, preferably at least a bimodal
homopropylene, is provided which comprises a lower molecular weight (LMW)
component and a higher molecular weight (HMW) component. The weight ratios
thereof may vary. The amount of component (i) may be 30 to 70 wt-%,
preferably 40 to 60 wt-%, more preferably 45 to 55 wt.-% and the amount of
component (ii) may be 30 to 70 wt-%, preferably 40 to 60 wt.-%, more
preferably 45 to 55 wt.-%, calculated from the total propylene polymer.
In a preferred embodiment, the propylene polymer as described above is a
reactor-made propylene polymer (also called as a reactor powder). The
reactor-made propylene polymer means herein the reaction product as obtained
from the polymerization process, i.e. the reactor-made propylene polymer has not

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been subjected to any washing or treatment step to decrease or remove (1) the
Al- and B-residues, preferably the A1-, B-, CI- and Si-residues, which mainly
originate from the catalyst. Also preferably, the reactor-made propylene polymer
has not been subjected to (2) any deashing step in a manner known in the art to
decrease or remove the ash content of the polymer. If desired, the reactor-made
propylene polymer of this embodiment may then further be treated in a
subsequent treatment step, e.g. washing step, in a known manner for optimizing,
e.g. for further reducing one or more of the following: Al, B, CI, Si and ash
content of the product.
Moreover, it is in particular preferred that the propylene polymer is
obtainable by a single site catalyst (SSC) polymerization. The SSC includes
metallocene and non-metallocene catalysts as known in the art. Preferably,
the propylene polymer is obtainable by a metallocene catalysed
polymerization, more preferably using the process and/or catalyst as
defined below.
In a further advantageous embodiment, the propylene polymer is obtainable
by a solid, non-silica supported catalyst, preferably solid non-silica
supported single site -based catalyst, such as a metallocene-based catalyst.
According to a further preferable embodiment of the invention, the
propylene polymer as defined above is obtainable by a solid catalyst which
(1) comprises at least a metallocene complex as a catalytically active
component, optionally together with an activator as the cocatalyst and (2)
has a productivity of at least 30 kg PP/g catalyst, typically of at least 40 kg
PP/g catalyst, preferably of at least 50 kg/PP/g catalyst, more preferably of
at least 60 kg PP/g catalyst. The productivity as defined above is a known
expression in the field and describes the catalytic activity of the catalyst.
The term "kg PP/g catalyst" means the amount of polypropylene produced
with 1 g of the catalyst.
In addition, the present invention comprises also the use of the propylene
polymer as described above as such or as a component of a polymer blend
in various end use applications with high purity requirements. Accordingly,
the invention further provides an article comprising the propylene polymer
of the invention. Such articles include containers and packaging articles for
medical, food and electrical applications (such as capacitor film applications).

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Accordingly, the propylene polymer can be processed as such or as a blend
with further polymer component(s), optionally in the presence with
additives (such as well known in the art) to produce various end
applications in a known manner. E.g. the propylene polymer can be
moulded or extruded to articles, e.g. for films, mono- and biaxially oriented
films, fibers and molded articles. Such extruded or molded articles include
mono- and multilayered articles as known in the art. Furthermore, films
include cast and blown films. Due to the high purity the inventive
propylene polymer is very feasible in the field of food packaging and
medical packaging, as well as in electrical applications.
Moreover the present invention is directed to a layered structure, preferably
a film, which comprises at least one layer comprising the propylene
polymer as defined above. Preferably the layers of the film consist
essentially of the propylene polymer as defined above. In addition, the film
comprising the inventive propylene polymer may be a bi-oriented film
and/or a capacitor film.
The articles including films can be produced according to or analogously to
methods well known in the art.
Moreover, the present invention provides also a polymerization process for
producing the propylene polymer.
The process for preparing the inventive propylene polymer comprises at
least the step of polymerizing propylene in the presence of a catalyst,
preferably non-silica supported catalyst. "Non-silica supported catalyst"
means herein that part or all of the active catalyst components have not
been supported on a solid, porous silica-based carrier material as is the case
in a silica-supported catalyst, wherein the catalyst component(s) are
conventionally impregnated to the pores of silica carrier particles.
In principal any polymerization method including slurry and gas phase
polymerization can be used for producing the polymer composition. Slurry
polymerization is preferably a bulk polymerization. "Bulk" means a
polymerization in a reaction medium comprising at least 60 wt.-%
monomer.

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The invention also provides a process for producing the propylene polymer
comprising at least a propylene homo- or copolymer component (i) as
defined above, wherein the propylene, optionally together with one or more
comonomers, are polymerized in the presence of a polymerization catalyst.
In case the propylene polymer consists of component (i) only the process is
a single stage process.
In case a multimodal, e.g. at least bimodal, polymer comprising at least two
different components (i) and (ii) with different molecular weight
distribution (MWD) and/or with different comonomer contents, the
propylene polymer may be produced by blending each or part of the
components in-situ during the polymerization process thereof (in-situ
process) or, alternatively, by blending mechanically two or more separately
produced components in a manner known in the art.
It is also possible to produce a multimodal propylene polymer in one
reactor by selecting e.g. one or more of (1) changing polymerization
conditions, (2) using at least two different catalysts, (3) using multi site,
e.g. dual site catalysts and (4) using at least two different comonomer
feeds.
Alternatively, the invention further provides a process for producing a
propylene polymer comprising at least two different propylene homo- or
copolymer components (i) and (ii) as defined above, wherein each
component (i) and (ii) is produced by polymerizing propylene, optionally
together with one or more comonomers, in the presence of a polymerization
catalyst in a multistage polymerization process using one or more
polymerization reactors, which may be the same or different, e.g. at least
loop-loop, gas-gas or any combination of loop and gas reactors. Each stage
may be effected in parallel or sequentially using the same or different
polymerization method(s). In case of a sequential stages each components,
e.g. (i) and (ii), may be produced in any order by carrying out the
polymerization in each step, except the first step, in the presence of the
polymer component formed, in the preceding step. Preferably, the catalyst
used and added in the first step is present in the subsequent step(s).
Alternatively, the same or different catalyst can be added in the subsequent
step(s).

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Multistage processes include also bulk/gas phase reactors known as
multizone gas phase reactors for producing multimodal propylene polymer.
Thus a further embodiment provides a process for producing any of the
above polymer composition, which comprises (i) a propylene homo- or
copolymer component and, optionally, (ii) an propylene homo- or
copolymer component, wherein the process includes a step of:
(a) polymerizing in a slurry reactor, preferably a loop reactor, propylene,
optionally together with one of more comonomers, in the presence of a
polymerization catalyst to produce a first propylene polymer
component (one of components (i) and (ii)), and,
optionally, transferring the reaction product of step (a) to a subsequent
gas phase reactor and
(b) polymerizing in a gas phase reactor propylene, optionally together
with one or more comonomers, in the presence of the reaction product
of step (a) to produce a second polymer component (the other of
components (i) and (ii)) for obtaining the propylene polymer, and
recovering the obtained composition.
A preferred multistage process is a "loop-gas phase"-process, such as
developed by Borealis A/S, Denmark (known as BORSTAR® technology)
described e.g. in patent literature, such as in EP 0887 379 or in
W092/12182.
If the polymer composition has at least a multimodal MWD, then the lower
molecular weight (LMW) fraction and the higher molecular weight (HMW)
fraction can be made in different steps (a) and (b), in any order.
Optionally, and preferably, the process may also comprise a
prepolymerization step in a manner known in the field and which may
precede the polymerisation step (a).
If desired, a further elastomeric comonomer component, so-called rubber
component, may be incorporated into the obtained propylene polymer to
form a heterophasic copolymer of the polymer mentioned above. The
rubber component, preferably elastomeric propylene copolymer, with at

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least ethylene comonomer, may preferably be produced after the gas phase
polymerization step (b) in a subsequent second or further gas phase
polymerizations using one or more gas phase reactors.
The process is preferably a continuous process.
Preferably, in the process for producing the propylene polymer as defined
above the conditions for the slurry reactor of step (a) may be as follows:
the temperature is within the range of 40°C to 110°C, preferably
between 60°C and 100°C, 70-90 °C,
the pressure is within the range of 20 bar to 80 bar, preferably
between 30 bar to 60 bar,
hydrogen can be added for controlling the molar mass in a manner
known per se.
Subsequently, the reaction mixture from the slurry (bulk) reactor (step a) is
transferred to the gas phase reactor, i.e. to step (b), whereby the conditions
in step (b) are preferably as follows:
the temperature is within the range of 50°C to 130°C, preferably
between 60°C and 100°C,
the pressure is within the range of 5 bar to 50 bar, preferably between
15 bar to 35 bar,
hydrogen can be added for controlling the molar mass in a manner
known per se.
The residence time can vary in both reactor zones. In one embodiment of
the process for producing the propylene polymer the residence time in
slurry reactor, e.g. loop is in the range 0.5 to 5 hours, e.g. 0.5 to 2 hours
and the residence time in gas phase reactor will generally be 1 to 8 hours.
If desired, the polymerization may be effected in a known manner under
supercritical conditions in the slurry, preferably loop reactor, and/or as a
condensed mode in the gas phase reactor.

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The process of the invention or any embodiments thereof above or below
enable highly feasible means for producing and further tailoring the
propylene polymer composition within the invention. E.g. the properties of
the polymer composition can be adjusted or controlled in a known manner
e.g. with one or more of the following process parameters: temperature,
hydrogen feed, comonomer feed, propylene feed e.g. in the gas phase
reactor, catalyst, the type and amount of an external donor (if used), split
between components, e.g. components (i) and (ii).
The above process enables very feasible means for obtaining the reactor-
made propylene polymer as defined above.
In principal any catalyst can be used which provides the propylene polymer
of the invention. Preferably the catalyst is a solid non-silica supported
catalyst comprising at least a single site catalyst component, including a
metallocene or a non-metallocene catalyst component, preferably a
metallocene complex, as a catalytically active component. The catalyst may
optionally comprise an activator as a cocatalyst. Preferably, the catalyst
comprises a metallocene component and an activator as the cocatalyst
component. Further preferable, the cocatalyst contains aluminium, i.e. is a Al-
containing cocatalyst, such as aluminoxane.
In a further preferable embodiment the propylene polymer is obtainable by
a solid non-silica supported catalyst polymerization, whereby the catalyst
preferably contains an Al-based cocatalyst. More preferably, said solid
non-silica supported catalyst is free from any boron-containing cocatalyst,
more preferably free from any boron-based catalyst components. "Non-
silica supported catalyst" means a support or carrier material which is other
than silica or a modified silica carrier.
It is in particular preferable that the catalyst is obtainable by the emulsion
solidification technology described in WO03/051934. This document is
herewith included entirely to this application by reference. Hence the
catalyst is preferably a non-silica supported metallocene catalyst
comprising an organo-metallic compound of a transition metal of group 3
to 10 or the periodic table (IUPAC), or of an actinide or lantanide, in the
form of solid catalyst particles, obtainable by a process comprising the
steps of

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a) preparing a solution of one or more catalyst components;
b) dispersing said solution in a solvent immiscible therewith to
form an emulsion in which said one or more catalyst
components are present in the droplets of the dispersed
phase,
c) solidifying said dispersed phase to convert said droplets to
solid particles and optionally recovering said particles to
obtain said catalyst.
Preferably a solvent, more preferably an organic solvent, is used to form
said solution. Still more preferably the organic solvent is selected from the
group consisting of a linear alkane, cyclic alkane, linear alkene, cyclic
alkene, aromatic hydrocarbon and halogen-containing hydrocarbon.
Moreover the immiscible solvent forming the continuous phase is an inert
solvent, more preferably the inmiscible solvent comprises a fluorinated
organic solvent and/or a functionalized derivative thereof, still more
preferably the inmiscible solvent comprises a semi-, highly- or
perfluorinated hydrocarbon and/or a functionalized derivative thereof. It is
in particular preferred, that said immiscible solvent comprises a
perfluorohydrocarbon or a functionalised derivative thereof, preferably C3-C30
perfluoroalkanes, -alkenes or -cycloalkanes, more preferred C4-C10 perfluoro-
alkanes, -alkenes or -cycloalkanes, particularly preferred perfluorohexane,
perfluoroheptane, perfluorooctane or perfluoro (methylcyclohexane) or a mixture
thereof.
Furthermore it is preferred that the emulsion comprising said continuous phase
and said dispersed phase is a bi-or multiphasic system as known in the art. An
emulsifier may be used for forming the emulsion. After the formation of the
emulsion system, said catalyst is formed in situ from catalyst components
in said solution.
In principle, the emulsifying agent may be any suitable agent which
contributes to the formation and/or stabilization of the emulsion and which
does not have any adverse effect on the catalytic activity of the catalyst.
The emulsifying agent may e.g. be a surfactant based on hydrocarbons
optionally interrupted with (a) heteroatom(s), preferably halogenated

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hydrocarbons optionally having a functional group, preferably semi-,
highly- or perfluorinated hydrocarbons as known in the art. Alternatively,
the emulsifying agent may be prepared during the emulsion preparation,
e.g. by reacting a surfactant precursor with a compound of the catalyst
solution. Said surfactant precursor may be a halogenated hydrocarbon with
at least one functional group, e.g. a highly fluorinated C{ to C30 alcohol,
which reacts e.g. with a cocatalyst component, such as aluminoxane.
In principle any solidification method can be used for forming the solid particles
from the dispersed droplets. According to one preferable embodiment the
solidification is effected by a temperature change treatment. Hence the emulsion
subjected to gradual temperature change of up tolO °C per minute, preferably 0.5
to 6 per minute and more preferably 1 to 5 °C per minute. Even more preferred
the emulsion is subjected to a temperature change of more than 40 C, preferably
more than 50 °C within less than 10 seconds, preferably less than 6 seconds.
The recovered particles have preferably an average size range of 5 to 200 pm,
more preferably 10 to lOOum.
Moreover, the form of solidified particles have preferably a spherical shape, a
predetermined particles size distribution and a surface area of less than 50 m /g,
preferably less than 30 m /g and more preferably less than 20 m /g, wherein said
particles are obtained by the process as described above.
For further details, embodiments and examples of the catalyst components,
continuous and dispersed phase system, emulsion formation method, emulsifying
agent and solidification methods reference is made e.g. to the above
WO03/051934.
The catalytically active component is preferably of a transition metal
compound of formula (I)
(L)mRnMXq (I)
wherein
M is a transition metal of group 3 to 10 or the periodic table
(IUPAC), or of an actinide or lantanide,
each X is independently a monovalent anionic ligand, such as c-
ligand,

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each L is independently an organic ligand which coordinates to
M,
R is a bridging group linking two ligands L,
m is 1,2 or 3,
n is 0 or 1,
q is 1,2 or 3 and
m+q is equal to the valency of the metal.
Said catalytically active component is preferably a single site (SS) catalyst
component including metallocenes and non-metallocenes
In a more preferred definition, each L is independently
(a) a substituted or unsubstituted cyclopentadiene or a mono-, bi- or multifused
derivative of a cyclopentadiene which optionally bear further substiruents and/or
one or more hetero ring atoms from a Group 13 to 16 of the Periodic Table
(IUPAC); or
(b) an acyclic, η1- to η4- or -η6-ligand composed of atoms from Groups 13 to 16
of the Periodic Table, and in which the open chain ligand may be fused with one
or two, preferably two, aromatic or non-aromatic rings and/or bear further
substiruents; or (c) a cyclic a-, η1- to η4- or η6-, mono-, bi- or multidentate ligand
composed of unsubstituted or substituted mono-, bi- or multicyclic ring systems
selected from aromatic or non-aromatic or partially saturated ring systems and
containing carbon ring atoms and optionally one or more heteroatoms selected
from Groups 15 and 16 of the Periodic Table.
By "σ-ligand" is meant in a known manner a group bonded to the metal at one or
more places via a sigma bond.
According to a preferred embodiment said organotransition metal compound (I)
is a group of compounds known as metallocenes. Said metallocenes bear at least
one organic ligand, generally 1, 2 or 3, e.g. 1 or 2, which is η-bonded to the
metal, e.g. a η2-6-ligand, such as a η5-ligand. Preferably, a metallocene is a Group
4 to 6 transition metal, which contains at least one η5-ligand..
Preferably the metallocene compound has a formula (II):
(Cp)mRnMXq (II)

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wherein M is Zr, Hf or Ti, m=l or 2, and at least one Cp is independently a
cyclopenadienyl, indenyl, tetrahydroindenyl or fluorenyl, whereby each of
said Cp may be unsubstituted or substituted; the optional one or more
substituent(s) may be independently selected from a group including
halogen, hydrocarbyl (e.g. Cl-C20-alkyl, C2-C20-alkenyl, C2-C20-
alkynyl, C3-C12-cycloalkyl, C6-C20-aryl or C7-C20-arylalkyl), C3-C12-
cycloalkyl which contains 1, 2, 3 or 4 heteroatom(s) in the ring moiety, C6-
C20-heteroaryl, Cl-C20-haloalkyl, -SiR"3, -OSiR"3, -SR", -PR"2 or -NR"2,
each R" is independently a hydrogen or hydrocarbyl, e.g. Cl-C20-alkyl,
C2-C20-alkenyl, C2-C20-alkynyl, C3-C12-cycloalkyl or C6-C20-aryl; or
e.g. in case of -NR"2, the two substituents R" can form a ring, e.g. five- or
six-membered ring, together with the nitrogen atom wherein they are
attached to; preferably, m is 2 and both Cp-rings are indenyl rings which
each independently bear one or two substituents, preferably one substituent,
at the five ring of the indenyl moiety, more preferably at 2-position (such
substituent at 2-position is preferably selected from an alkyl, such as Ci-C6
alkyl, e.g. methyl or ethyl, or trialkyloxysiloxy, wherein each alkyl is
independently selected from CrC6 alkyl, such as methyl or ethyl), and one
or more substituents, preferably one substituent, at the six ring of the
indenyl moiety, more preferably at 4-position (such substituent at the 4-
position is preferably C6-C2o aromatic or heteroaromatic ring moiety, such
as phenyl or naphthyl, preferably phenyl, which is optionally substituted
with one or more substitutents, such as C1-C6 alkyl). The Cp ligands of the
metallocene are preferably linked with a bridge member R, in case of
indenyl, typically at 1-position. The bridge member R may contain one or
more bridge atoms selected from e.g. C, Si and/or Ge, preferably from C
and/or Si. One preferable bridge R is R'2Si=, wherein R' is selected
independently from one or more of e.g. C1-C10 alkyl, CrC2o alkyl, such as
C6-C12 aryl, or C7-C40, such as C7-C12 arylalkyl, wherein alkyl as such or as
part of arylalkyl is preferably CrC6 alkyl, such as ethyl or methyl,
preferably methyl, and aryl is preferably phenyl. The bridge R'2Si= is
preferably e.g. Q-C6 alkyl2Si=, diphenylSi= or Ci-C6 alkylphenylSi=, such
as Me2Si=.
The above described active catalyst components are commercially available
or may be prepared according to the methods described in the literature. As
an example of feasible single site catalysts, preferably metallocenes, and

- 17-
the preparation methods thereof, reference is made to the above
WO03/051934, as well as to EP836608, EP 576 970 and EP722 956,
without limiting to these.
As mentioned above the catalyst system may further comprise an activator
as a cocatalyst, as described in WO 03051934, which is enclosed hereby
with reference.
Preferred as cocatalysts for metallocenes and non-metallocenes, if desired,
are the aluminoxanes, in particular the Cl-ClO-alkylaluminoxanes, most
particularly methylaluminoxane (MAO). Such aluminoxanes can be used as
the sole cocatalyst or together with other cocatalyst(s). Thus besides or in
addition to aluminoxanes, other cation complex forming catalysts activators
can be used. Said activators are commercially available or can be prepared
according to the prior art literature.
Further aluminoxane cocatalysts are described i.a. in WO-A-9428034
which is incorporated herein by reference. These are linear or cyclic
oligomers of having up to 40, preferably 3 to 20, -(A1(R"')0)- repeat units
(wherein R'" is hydrogen, Cl-ClO-alkyl (preferably methyl) or C6-C18-
aryl or mixtures thereof).
The use and amounts of such activators are within the skills of an expert in
the field. As an example, with the boron activators, 5:1 to 1:5, preferably
2:1 to 1:2, such as 1:1, ratio of the transition metal to boron activator may
be used. In case of preferred aluminoxanes, such as methylaluminumoxane
(MAO), the amount of Al, provided by aluminoxane, can be chosen to
provide a molar ratio of Al: transition metal e.g. in the range of 1 to 10 000,
suitably 5 to 8000, preferably 10 to 7000, e.g. 100 to 4000, such as 1000 to
3000. Typically in case of solid (heterogeneous) catalyst the ratio is
preferably below 500.
The quantity of cocatalyst to be employed in the catalyst of the invention is
thus variable, and depends on the conditions and the particular transition
metal compound chosen in a manner well known to a person skilled in the
art.

-18-
Any additional components to be contained in the solution comprising the
organotransition compound may be added to said solution before or,
alternatively, after the dispersing step.
Determination Methods and Definitions
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.
Elementary analysis
The below described elementary analysis was used for determining the content of
the elementary residues which are mainly originating from the catalyst,
especially the A1-, B- and Si-residues in the polymer. Said A1-, B- and Si-
residues can be in any form, e.g. in elementary or ionic form, which can be
recovered and detected from the propylene polymer using e.g. the below
described ICP-method. The method can also be used for determining the Ti
content of the polymer. It is understood that also other known methods can be
used which would result in similar results.
ICP (Inductively coupled plasma emission) -spectrometry
ICP-instrument: The instrument for determination of A1-, Si- and B-content was
ICP Optima 2000 DV, PSN 620785 (supplier PerkinElmer Instruments, Belgium)
with the software of the instrument.
Detection limits are 0,1 ppm (Al), 0,1 ppm (Si) and 0,1 ppm (B).
The polymer sample was first ashed in a known manner, then dissolved in an
appropriate acidic solvent. The dilutions of the standards for the calibration curve
are dissolved in the same solvent as the sample and the concentrations chosen so
that the concentration of the sample would fall within the standard calibration
curve.
ppm: means parts per million by weight.
Ash content: Ash content is measured according to ISO 3451-1 (1997)
standard.

-19-
Calculated ash, Al- and B-content:
The ash and the above listed elements, Al and/or B can also be calculated
from a propylene polymer based on the polymerization activity of the
catalyst as exemplified in the examples. These values would give the upper
limit of the presence of said residues originating from the catalyst.
Thus the estimate catalyst residues is based on catalyst composition and
polymerization productivity, catalyst residues in the polymer can be
estimated according to:
Total catalyst residues [ppm] = 1/ productivity [kgPP/gcatalyst] *1000
Al residues [ppm]= wAl,Catalyst [%] * total catalyst residues [ppm] /TOO
Zr-residues [ppm] = wZr,Calatyst [%] * total catalyst residues [ppm] /100
(Similar calculations apply also e.g. for B, CI and Si residues)
Particle size distribution: is measured via Coulter Counter LS 200 at
room temperature with n-heptane as medium.
NMR
NMR-spectroscopy measurements:
The C13NMR spectra of polypropylenes were recorded on Bruker 400MHz
spectrometer at 130 °C from samples dissolved in 1,2,4-
trichlorobenzene/benzene-d6 (90/10 w/w). For the pentad analysis the
assignment is done according to the methods described in literature.
(T. Hayashi, Y. Inoue, R. Chiijo, and T. Asakura, Polymer 29 138-43
(1988).and Chujo R, et al,Polymer 35 339(1994).
The NMR-measurement was used for determining the mmmm pentad
concentration in a manner well known in the art.
The volatiles content: can be measured by so called static Headspace
Analysis described in the texbiook: Pyrolysis and GC in Polymer Analysis,
Edited by S.A. Liebman and E.J. Levy, Marcel Dekker, Inc., 1985. The gas
chromatography/head-space gas chromatography (GC-HS) analysis is

-20-
widely used in the automotive industry. The company Volkswagen AG has
developed a standard, which is generally accepted and used in the plastic
industry. It is known as "VW standard PV 3341". Test duration was one
hour and the test temperature 160°C according to the requirements used for
capacitor films.
The molecular weights, Mw and Mn, and molecular weight distribution
MWD expressed as polydispersity Mw/M„ of polymers were determined with
A Millipore Waters ALC/GPC operating at 135 °C and equipped with two mixed
bed and one 107 A TSK-Gel columns (TOSOHAAS 16S) and a differential
refractometer detector. The solvent 1,2,4-trichlorobezene was applied at flow rate
of 1 ml/min. The columns were calibrated with narrow molecular weight
distribution polystyrene standards and narrow and broad polypropylenes.
Reference is also made to ISO 16014.
The xylene solubles (XS, wt%): analysis according to the known method: 2.0 g
of polymer was dissolved in 250 ml p-xylene at 135°C under agitation. After
30±2 minutes the solution was allowed to cool for 15 minutes at ambient
temperature and then allowed to settle for 30 minutes at 25±0.5°C. The solution
was filtered and evaporated in nitrogen flow and the residue dried under vacuum
at 90°C until constant weight is reached.
XS%=(100 x mi x v0) / (mo x vO, wherein
mo= initial polymer amount (g)
mi= weight of residue (g)
v0= initial volume (ml)
Vi= volume of analyzed sample (ml)
Melting temperature Tm, crystallization temperature T„ and the degree of
crystallinity: measured with Mettler TA820 differential scanning calorimetry
(DSC) on 5-10 mg samples. Both crystallization and melting curves were
obtained during 10°C/min cooling and heating scans between 30°C and 225°C.
Melting and crystallization temperatures were taken as the peaks of endotherms
and exotherms.
Also the melt- and crystallization enthalpy (Hm and He) were measured by the
DSC method according to ISO 11357-3.

-21-
Chlorine residues content: The content of Cl-residues is measured from
samples in the known manner using X-ray fluorescence (XRF) spectometry. The
instrument was X-ray fluorescention Philips PW2400, PSN 620487, (Supplier:
Philips, Belgium) software X47. Detection limit for CI is 1 ppm.
MFR2: measured according to ISO 1133 (230°C, 2.16 kg load).
Stiffness Film TD (transversal direction), Stiffness Film MD (machine
direction), Elongation at break TD and Elongation at break MD: these were
determined according to IS0527-3
Haze and transparency: were determined: ASTM D1003
Experimental part
The used raw materials and chemicals are commercially available or can be
prepared according to the known methods described in the literature.
Example 1:
Catalyst preparation
The catalyst was prepared as described in example 5 of WO 03/051934, but
adjusting the Al- and Zr-ratio (Al/Zr) to 291 in a manner known in the art
(Zr = 0,42 wt.-% and Al = 36,27 wt%).
Catalyst characteristics:
Al- and Zr- content were analyzed via above mentioned method to 36,27
wt.-% Al and 0,42 %-wt. Zr. The average particle diameter (analyzed via
Coulter counter) is 20 urn and particle size distribution is shown in Fig. 1
Polymerization:
A 5 liter stainless steel reactor was used for propylene polymerizations.
1100 g of liquid propylene (Borealis polymerization grade) was fed to
reactor. 0.1 ml triethylaluminum (100%, purchased from Crompton) was
fed as a scavenger and 15 mmol hydrogen (quality 6.0, supplied by Aga) as

chain transfer agent. Reactor temperature was set to 30 °C. 21,4 mg catalyst
were flushed into to the reactor with nitrogen overpressure. The reactor was
heated up to 70 °C in a period of about 14 minutes. Polymerization was
continued for 50 minutes at 70 °C, then propylene was flushed out, 5 mmol
hydrogen were fed and the reactor pressure was increased to 20 bars by
feeding (gaseous-) propylene. Polymerization continued in gas-phase for
210 minutes, then the reactor was flashed, the polymer was dried and
weighted.
Polymer yield was weighted to 790 g, that equals a productivity of 36,9
kgpp/gcatalyst-
Ash content: Ash content was analyzed to 68 ppm
Estimate residues:
Total catalyst residues estimated to 27 ppm
Al residues estimated to 9,8 ppm
Zr residues estimated to 0,1 ppm
Example 2:
The catalyst was prepared as in Example 1 (Al/Zr = 291)
Polymerization
A 5 liter stainless steel reactor was used for propylene polymerizations.
1100 g of liquid propylene (Borealis polymerization grade) was fed to
reactor. 0.1 ml triethylaluminum (100%, purchased from Crompton) was
fed as a scavenger and 15 mmol hydrogen (quality 6.0, supplied by Aga) as
chain transfer agent. Reactor temperature was set to 30 °C. 30,6 mg catalyst
was flushed into to the reactor with nitrogen overpressure. The reactor was
heated up to 70 °C in a period of about 14 minutes. Polymerization was
continued for 40 minutes at 70 °C, then propylene was flushed out, 5 mmol
hydrogen were fed and the reactor pressure was increased to 20 bars by
feeding (gaseous) propylene. Polymerization continued in gas-phase for
181 minutes, then the reactor was flashed, the polymer was dried and
weighted.

-23-
Polymer yield was weighted to 890 g, equalling a productivity of 29
kgpp/gcatalyst-
Ash content: Ash content was analyzed to 47 ppm
Estimate residues:
Total catalyst residues estimated to 34 ppm
Al residues estimated to 12 ppm
Zr residues estimated to 0,1 ppm
Example 3:
The same catalyst as in Example 1 was used in this example (Al/Zr= 291)
Polymerization
A 5 liter stainless steel reactor was used for propylene polymerizations.
1100 g of liquid propylene (Borealis polymerization grade) was fed to
reactor. 0.1 ml triethylaluminum (100%, purchased from Crompton) was
fed as a scavenger and 20 mmol hydrogen (quality 6.0, supplied by Aga) as
chain transfer agent. Reactor temperature was set to 30 °C. 29,4 mg catalyst
was flushed into to the reactor with nitrogen overpressure. The reactor was
heated up to 70 °C in a period of about 14 minutes. Polymerization was
continued for 55 minutes at 70 °C, then propylene was flushed out, 10
mmol hydrogen were fed and the reactor pressure was increased to 20 bars
by feeding (gaseous) propylene. Polymerization continued in gas-phase for
189 minutes, then the reactor was flashed, the polymer was dried and
weighted.
Polymer yield was weighted to 815 g, equalling a productivity of 27,7
kgpp/gcatalyst-
Estimate residues:
Total catalyst residues estimated to 36 ppm
Al residues estimated to 13 ppm

-24-
Zr residues estimated to 0,2 ppm
Example 4:
Catalyst preparation
The catalyst was prepared as described in example 1, but using the ratio:
Al/Zr = 271 (Al = 34,50 wt.-% and Zr = 0,43 wt-%).
Polymerization:
A 5 liter stainless steel reactor was used for propylene polymerizations.
1100 g of liquid propylene (Borealis polymerization grade) was fed to
reactor. 0.2 ml triethylaluminum (100%, purchased from Crompton) was
fed as a scavenger and 15 mmol hydrogen (quality 6.0, supplied by Aga) as
chain transfer agent. Reactor temperature was set to 30 °C. 29.1 mg catalyst
were flushed into to the reactor with nitrogen overpressure. The reactor was
heated up to 70 °C in a period of about 14 minutes. Polymerization was
continued for 50 minutes at 70 °C, then propylene was flushed out, 5 mmol
hydrogen were fed and the reactor pressure was increased to 20 bars by
feeding (gaseous-) propylene. Polymerization continued in gas-phase for
144 minutes, then the reactor was flashed, the polymer was dried and
weighted.
Polymer yield was weighted to 901 g, that equals a productivity of 31
kgpp/gcatalyst-
Estimate residues:
Total catalyst residues estimated to 32 ppm
Al residues estimated to 11 ppm
Zr residues estimated to 0,1 ppm
Example 5:
The same catalyst as in Example 1 was used (Al/Zr= 291).

-25-
Polymerization:
A 5 liter stainless steel reactor was used for propylene polymerizations.
1100 g of liquid propylene (Borealis polymerization grade) was fed to
reactor. 0.05 ml triethylaluminum (100%, purchased from Crompton) was
fed as a scavenger and 30 mrnol hydrogen (quality 6.0, supplied by Aga) as
chain transfer agent. Reactor temperature was set to 30 °C. 20,1 mg catalyst
was flushed into to the reactor with nitrogen overpressure. The reactor was
heated up to 70 °C in a period of about 15 minutes. Polymerization was
continued for 40 minutes at 70 °C, then propylene was flushed out, the
reactor pressure was increased to 20 bars by feeding (gaseous) propylene.
Polymerization continued in gas-phase for 370 minutes, then the reactor
was flashed, the polymer was dried and weighed.
Polymer yield was weighed to 1096 g, equaling a productivity of 54.4
kgpp/gcatalyst-
Estimate residues:
Total catalyst residues estimated to 18 ppm
Al residues estimated to 6,5 ppm
Zr residues estimated to 0,08 ppm
The experimental data of the propylene polymers of examples 1 to 5 are
listed in table 1 below. The data show the advantageous properties of the
present propylene polymer already when obtained directly from the
polymerization process without any treatment steps for removing any of the
catalysts. Also the advantageous mechanical properties of the polymers of
the invention are apparent from the below table.

Table 1: Experimental data of examples 1-5

Example no. Ex. 1 Ex.2 Ex. 3 Ex.4 Ex.5
Productivity kgpp/gcat 36,9 29 27,7 31 54.4
Catalyst residue
(Calculated) ppm 27 34 36 32 18
B ppm n.d. n.d. n.d. n.d. n.d.
Al ppm 9,8 12 13 11 8.4
Si ppm n.d. n.d. n.d. n.d. n.d.
Zr ppm 0,1 0,1 0,2 0,1 0.08
CI ppm n.d. n.d. n.d. n.d. n.d.
MFR g/10' 1,79 1,78 3,9 2 1,6
Mw g/mol 467000 499000 400000 453000 481000
Mw/Mn - 2,7 2,7 3 2,8 2,8
XS wt% 0,51 0,56 0,4 0,85 n.d.
mmmm - 0,95 0,96 0,96 0,96 n.d.
Stiffness Film
TD MPa 1008 964 1019 1011 638
Stiffness Film
MD MPa 1013 1028 1094 1059 658
Elongation at
Break TD % 718 613 780 700 701
Elongation at
Break MD % 660 608 702 691 641

-27-

Tm °C 149,8 150,2 152 150,6 151
Hm J/g 97,4 95,1 97,7 99,5 99
Tc °C 106,4 106,5 113,3 111,9 105
He J/g 88,6 88,7 94,8 74,6 89
Transparency % 94 n.d.
Haze % 7,8 n.d.
Volatiles ppm 200 n.d.

-28-
Claims
1. A propylene polymer having an aluminum residue content of less
than 25 ppm and a boron residue content less than 25 ppm.
2. A propylene polymer according to claim 1 wherein the propylene
polymer is a high crystalline propylene polymer.
3. A propylene polymer according to claim 1 or 2, wherein the
propylene polymer has an isotacticity of higher than 0.940 mmmm
pentad concentration determined by NMR-spectroscopy.
4. A propylene polymer according to anyone of the preceding claims
wherein the aluminum residue content is less than 10 ppm.
5. A propylene polymer according to anyone of the preceding claims
wherein the boron residue content is less than 10 ppm.
6. A propylene polymer according to anyone of the preceding claims
wherein the ash content is less than 50 ppm.
7. A propylene polymer according to anyone of the preceding claims
wherein the silicon residue content is less than 10 ppm.
8. A propylene polymer according to anyone of the preceding claims
wherein the total amount of aluminum, boron and silicon residues is
less than 10 ppm.
9. A propylene polymer according to anyone of the-preceding claims
wherein the chlorine residue content in the propylene polymer is less
than 10 ppm, more preferably less than 5 ppm.
10. A propylene polymer according to anyone of the preceding claims
wherein the volatiles content determined by GC-HS for one hour at
160°C is less than 400 ppm.
11. A propylene polymer according to anyone of the preceding claims
wherein the propylene polymer is a reactor-made propylene polymer.

-29-
12. A propylene polymer according to anyone of the preceding claims
wherein the propylene polymer is a propylene homopolymer.
13. A propylene polymer according to anyone of the preceding claims
wherein the propylene polymer has xylene solubles (XS) of less than
2.0 wt.-%.
14. A propylene polymer according to anyone of the preceding claims
wherein the propylene polymer has an Mw/Mn of not higher than
20.0.
15. A propylene polymer according to anyone of the preceding claims
wherein the propylene polymer has an MFR2 of up to 10 g/lOmin.
16. A propylene polymer according to anyone of the preceding claims
wherein the propylene polymer is obtainable by a metallocene
catalyzed polymerization, preferably in the absence of a boron-
containing activator as a cocatalyst.
17. A propylene polymer according to anyone of the preceding claims
wherein the propylene polymer is obtainable by a solid, non-silica
supported catalyst, preferably in the presence of Al-containing
activator as a cocatalyst.
18. A propylene polymer according to anyone of the preceding claims
wherein the propylene polymer is obtainable by a solid catalyst
which: (1) comprises at least a metallocene complex as a
catalytically active component, optionally together with an activator
as the cocatalyst, and (2) has a productivity of at least 30 kg PP/g
catalyst, preferably of at least 40 (kg PP)/(g catalyst), more
preferably of at least 50 (kg PP)/(g catalyst).
19. A propylene polymer as defined in any of the preceding claims
comprising at least two propylene homo- or copolymer components
(i) and (ii) wherein one of the components (i) and (ii) is a LMW
component with higher MFR and the other of components (i) and (ii)
is a HMW component with lower MFR.

-30-
20. A process for producing a propylene polymer according to anyone of
the preceding claims comprising the step of polymerising propylene
in the presence of a non-silica supported catalyst, preferably a solid
non-silica supported catalyst.
21. A process according to claim 20, wherein the catalyst is a non-silica
supported metallocene catalyst comprising an organo-metallic
compound of a transition metal of group 3 to 10 of the periodic table
(IUPAC), or of an actinide or lantanide, in the form of solid catalyst
particles, obtainable by a process comprising the steps of

a) preparing a solution of one or more catalyst components;
b) dispersing said solution in a solvent immiscible therewith to
form an emulsion in which one or more catalyst components
are present in the droplets of the dispersed phase,
c) solidifying said dispersed phase to convert said droplets to
solid particles and optionally recovering said particles to
obtain said catalyst.
22. A process according to claim 20 or 21 wherein the catalyst comprises
a catalyst component of a transition metal compound of formula (I)
(L)mRnMXq (I)
wherein
M is a transition metal as defined in claim 18, and
each X is independently a a-ligand,
each L is independently an organic ligand which coordinates to
M,
R is a bridging group linking two ligands L,
m is 1,2 or 3,
n is 0 or 1,
q is 1,2 or 3 and
m+q is equal to the valency of the metal.

-31-
23. A process according to anyone of claims 20 to 22 wherein the
catalyst further comprises an aluminum based cocatalyst, preferably
aluminoxane cocatalyst.
24. A process according to anyone of the preceding claims 20 to 23
wherein the immiscible solvent comprises a perfluorohydrocarbon or
a functionalized derivative thereof, preferably C3 to C30
perfluoralkane, -alkenes or cycloalkanes.
25. A process according to anyone of the preceding claims 20 to 24
wherein (b) the emulsion system is formed optionally by using an
emulsifying agent and (c) said catalyst is formed in situ from catalyst
components in said solution.
26. A process according to anyone of the preceding claims 20 to 25
wherein the solidification is effected by a temperature change
treatment.
27. A process according to claim 20 to 26 wherein the catalyst comprises
a metallocene catalyst component of formula (I)
(L)mRnMXq (I)
wherein
M is a Zr, Hf or Ti, and
each X is independently a a-ligand,
each L is independently an organic ligand containing a substituted
or unsubstituted cyclopentadienyl ligand which is bonded to M
via a 7t-bond, preferably a cyclopentadienyl, indenyl,
tetrahydroindenyl or fluorenyl, whereby each of said L may be
unsubstituted or substituted with one or more substituents;
R is a bridging group linking two ligands L,
m is 1,2 or 3,
n is 0 or 1,
q is 1,2 or 3 and
m+q is equal to the valency of the metal.

-32-
28. A process according to anyone of the preceding claims 20 to 27
wherein the process is a multi-stage process comprising the steps of
a) polymerizing propylene monomers, optionally together with
one or more comonomers, in the presence of the catalyst
obtainable as claimed in anyone of the preceding claims 20
ti 27 to produce a first propylene polymer component,
b) transferring the reaction product of step a) to a subsequent
gas phase reactor,
c) polymerizing propylene monomers optionally in the
presence of one or more comonomers, in the presence of the
reaction product of step a) to produce a second propylene
polymer component for obtaining the propylene polymer as
defined in anyone of the preceding claims 1 to 19 and
recovering the obtained product.

29. A propylene polymer obtainable by the process as defined in any of
the preceding claims 20 to 28.
30. A method for reducing the aluminum and boron content of an a-
olefin polymer obtainable by polymerization of alpha-olefin
monomers, optionally together with one or more comonomers, in the
presence of a metallocene catalyst, wherein said polymer is produced
using a process as defined in anyone of claims 20 to 28.
31. Use of a the propylene polymer according to anyone of the claims 1
to 19 or claim 29 for films, fibers and molded articles.
32. Use of the propylene polymer according to anyone of the preceding
claims 1 to 19 or claim 29 for food packaging or medical packaging
articles.
33. An article comprising the propylene polymer according to anyone of
the preceding claims 1 to 19 or claim 29.
34. An article according to claim 33 wherein the article is a film, fiber or
molded article.

-33-
35. An article according to claim 33 wherein the article is a food
packaging or medical packaging article.
36. Layered structure, preferably a film, comprising one or more layers
of which at least one layer comprises the propylene polymer of
anyone of the preceding claims 1 to 19 or claim 29.
37. A film according to claim 34 or 36, comprising at least one layer
which consists essentially of the propylene polymer as defined in
anyone of claims 1 to 19 or claim 29.
38. A film according to claim 34, 36 or 37, which is a capacitor film.
39. A biaxially oriented polypropylene film comprising a propylene
polymer according to anyone of the preceding claims 1 to 19 or claim
29.


A polypropylene with a low amount of impurities, in particular a low amount of aluminum and boron residues.

Documents:

04801-kolnp-2007-abstract.pdf

04801-kolnp-2007-claims.pdf

04801-kolnp-2007-correspondence others.pdf

04801-kolnp-2007-description complete.pdf

04801-kolnp-2007-drawings.pdf

04801-kolnp-2007-form 1.pdf

04801-kolnp-2007-form 3.pdf

04801-kolnp-2007-form 5.pdf

04801-kolnp-2007-gpa.pdf

04801-kolnp-2007-international exm report.pdf

04801-kolnp-2007-international search report.pdf

04801-kolnp-2007-pct priority document notification.pdf

4801-KOLNP-2007-(12-03-2013)-AMANDED PAGES OF SPECIFICATION.pdf

4801-KOLNP-2007-(12-03-2013)-EXAMINATION REPORT REPLY RECEIVED.pdf

4801-KOLNP-2007-(20-04-2012)-CORRESPONDENCE.pdf

4801-KOLNP-2007-(20-04-2012)-OTHERS.pdf

4801-KOLNP-2007-(21-09-2012)-CORRESPONDENCE.pdf

4801-KOLNP-2007-(21-09-2012)-OTHERS.pdf

4801-KOLNP-2007-(22-10-2013)-CORRESPONDENCE.pdf

4801-KOLNP-2007-(22-10-2013)-OTHERS.pdf

4801-KOLNP-2007-(25-04-2012)-CORRESPONDENCE.pdf

4801-KOLNP-2007-(25-04-2012)-OTHERS.pdf

4801-KOLNP-2007-(26-09-2012)-ABSTRACT.pdf

4801-KOLNP-2007-(26-09-2012)-AMANDED PAGES OF SPECIFICATION.pdf

4801-KOLNP-2007-(26-09-2012)-ANNEXURE TO FORM 3.pdf

4801-KOLNP-2007-(26-09-2012)-CLAIMS.pdf

4801-KOLNP-2007-(26-09-2012)-CORRESPONDENCE.pdf

4801-KOLNP-2007-(26-09-2012)-DESCRIPTION (COMPLETE).pdf

4801-KOLNP-2007-(26-09-2012)-DRAWINGS.pdf

4801-KOLNP-2007-(26-09-2012)-FORM-1.pdf

4801-KOLNP-2007-(26-09-2012)-FORM-13.pdf

4801-KOLNP-2007-(26-09-2012)-FORM-2.pdf

4801-KOLNP-2007-(26-09-2012)-OTHERS.pdf

4801-KOLNP-2007-(26-09-2012)-PETITION UNDER RULE 137.pdf

4801-KOLNP-2007-(26-11-2012)-CORRESPONDENCE.pdf

4801-KOLNP-2007-(26-11-2012)-OTHERS.pdf

4801-KOLNP-2007-(27-10-2014)-CLAIMS.pdf

4801-KOLNP-2007-(27-10-2014)-CORRESPONDENCE.pdf

4801-KOLNP-2007-(27-10-2014)-FORM-13.pdf

4801-KOLNP-2007-(27-10-2014)-OTHERS-1.1.pdf

4801-KOLNP-2007-(27-10-2014)-OTHERS.pdf

4801-KOLNP-2007-ASSIGNMENT.pdf

4801-KOLNP-2007-CORRESPONDENCE OTHERS 1.1.pdf

4801-KOLNP-2007-CORRESPONDENCE OTHERS 1.2.pdf

4801-kolnp-2007-form 18.pdf

4801-KOLNP-2007-FORM 3 1.1.pdf

4801-KOLNP-2007-FORM 3-1.1.pdf

abstract-04801-kolnp-2007.jpg


Patent Number 263453
Indian Patent Application Number 4801/KOLNP/2007
PG Journal Number 44/2014
Publication Date 31-Oct-2014
Grant Date 29-Oct-2014
Date of Filing 10-Dec-2007
Name of Patentee BOREALIS TECHNOLOGY OY
Applicant Address P.O. BOX 330, FIN-06101, PORVOO
Inventors:
# Inventor's Name Inventor's Address
1 LEHMUS PETRI PURJETUULENKUJA 19 D, 00850 HELSINKI
2 ERNST EBERHARD HATTMANNSDORF 6, 4210 UTERWEITERSDORF
3 BARTKE MICHAEL HAMEENTIE 8 B 9, 04400 JARVENPAA
4 HUHTANEN LAURI PEIKKOVUORENTIE 13, 07940 LOVIISA
PCT International Classification Number C08F 4/659
PCT International Application Number PCT/EP06/006736
PCT International Filing date 2006-07-10
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 05014905.3 2005-07-08 EUROPEAN UNION