FILM MADE FROM C2C3C4 TERPOLYMER - C3C4 COPOLYMER BLEND AND C2C3C4 TERPOLYMER - C3C4 COPOLYMER BLEND

Abstract

Film made from ethylene-propylene-1-butene terpolymer and propene-butene copolymer blend and ethylene-propylene-1-butene terpolymer and propene-butene copolymer blend.

Claims

1. A film made from a blend obtainable by compounding an ethylene-propylene-1-butene terpolymer base resin and a propylene butene random copolymer upgrading resin, wherein the ethylene-propylene-1-butene terpolymer base resin includes a) units derived from ethylene in an amount of 0.1 to 2.0 wt.-% with respect the total ethylene-propylene-1-butene terpolymer base resin; and b) units derived from propylene in an amount of 88.0 to 95.9 wt.-% with respect the total ethylene-propylene-1-butene terpolymer base resin; and c) units derived from butene in an amount of 4.0 to 10.0 wt.-% with respect the total ethylene-propylene-1-butene terpolymer base resin, d) wherein the units derived from ethylene, propylene and butene add up to 100 wt.-%, and e) preferably a total amount of units derived from ethylene and butene of 6.0 to 9.0 wt.-% with respect the total ethylene-propylene-1-butene terpolymer base resin, and f) preferably a ratio of the units derived from butene in weight percent versus the units derived from ethylene in weight percent of 3.0 to 16.0, more preferably 3.0 to 8.0; wherein the ethylene-propylene-1-butene terpolymer base resin has g) 2.1 regioinversions in an amount of 0.10 to 0.80 mol % as determined by .sup.13C-NMR analysis (as described in the experimental part); and h) a melt flow rate MFR.sub.2 (230? C./2.16 kg) measured according to ISO 1133 in the range from 1.0 to 18.0 g/10 min, preferably 1.5 to 7.0 g/10 min, and i) a melting temperature Tm measured by differential scanning calorimetry (DSC) in the range from 123 to 142? C., preferably 125 to 135? C.; and j) preferably a xylene soluble content of 5.0 to 25.0 wt.-% more preferably 15.0 to 19.0 wt. % determined at 25? C.according ISO 16152; 2005; and wherein the propylene butene random copolymer upgrading resin has k) a melting temperature Tm measured by differential scanning calorimetry (DSC) in the range from 70 to 90? C., and l) units derived from butene in an amount of 20.0 to 35.0 wt.-% with respect the total propylene butene random copolymer upgrading resin, m) wherein the units derived from propylene and butene add up to 100 wt.-%, and n) a melt flow rate MFR.sub.2 (230? C./2.16 kg) measured according to ISO 1133 of 1.0 to 18.0 g/10 min and preferably higher than the melt flow rate MFR.sub.2 (230? C./2.16 kg) of the base resin; and o) optionally an elongation at break (ASTM D638) of 100 to 900%, wherein the film has a sealing initiation temperature (SIT) (as determined by a method described in the experimental part) below 106? C.

2. The film according to claim 1, made from a blend obtainable by compounding an ethylene-propylene-1-butene terpolymer base resin and a propylene butene random copolymer upgrading resin, wherein the ethylene-propylene-1-butene terpolymer base resin includes a) units derived from ethylene in an amount 0.5 to 1.9 wt.-% with respect the total ethylene-propylene-1-butene terpolymer base resin; and b) units derived from propylene in an amount of 90.1 to 95.0 wt.-% with respect the total ethylene-propylene-1-butene terpolymer base resin; and c) units derived from butene in an amount of 4.5 to 8.0 wt.-% with respect the total ethylene-propylene-1-butene terpolymer base resin, d) wherein the units derived from ethylene, propylene and butene add up to 100 wt.-%, and e) a total amount of units derived from ethylene and butene of 6.0 to 9.0 wt.-% with respect the total ethylene-propene-butene terpolymer base resin, and f) a ratio of the units derived from butene in weight percent versus the units derived from ethylene in weight percent of 3.0 to 16.0; wherein the ethylene-propylene-1-butene terpolymer base resin has g) 2.1 regioinversions in an amount of 0.20 to 0.50 mol % as determined by .sup.13C-NMR analysis (as described in the experimental part); and h) a melt flow rate MFR.sub.2 (230? C./2.16 kg) measured according to ISO 1133 in the range from 1.5 to 7.0 g/10 min, and i) a melting temperature Tm measured by differential scanning calorimetry (DSC) in the range from 125 to 135? C.; and j) preferably a xylene soluble content of 5.0 to 25.0 wt.-% more preferably 15.0 to 19.0 wt.-% determined at 25? ? C.according ISO 16152; 2005 and wherein the propylene butene random copolymer upgrading resin has k) a melting temperature Tm measured by differential scanning calorimetry (DSC) in the range from 70 to 90? C., and l) units derived from butene in an amount of 20.0 to 35.0 wt-% with respect the total propylene butene random copolymer upgrading resin, and m) wherein the units derived from propylene and butene add up to 100 wt.-%, and n) a melt flow rate MFR.sub.2 (230? C./2.16 kg) measured according to ISO 1133 in the range of 1.0 to 18.0 g/10 min and preferably higher than the melt flow rate MFR.sub.2 (230? C./2.16 kg) of the base resin; and o) optionally an elongation at break (ASTM D638) of 100 to 900%.

3. The film according to claim 1, wherein the propylene butene random copolymer upgrading resin has one or more, preferably all of the following properties: p) a tensile strength at break (ASTM D638) of at least 15 MPa, q) a tensile modulus (according to ASTM D638) of least 200 MPa; r) a shore D hardness (ASTM D2240) of at least 55; s) a melting temperature Tm measured by differential scanning calorimetry (DSC) in the range from 81 to 90? C.

4. The film according to claim 1, wherein the ethylene-propylene-1-butene terpolymer base resin has 2.1 regioinversions in an amount of 0.20 to 0.35 mol %, as determined by .sup.13C-NMR analysis (as described in the experimental part).

5. The film according to claim 1, wherein the ethylene-propylene-1-butene terpolymer base resin is present in an amount of 70 to 95 wt.-% with respect to the total blend and wherein the propylene butene random copolymer upgrading resin is present in an amount of 5 to 30 wt.-% with respect to the total blend, wherein ethylene-propylene-1-butene terpolymer base resin and propylene butene random copolymer upgrading resin add up to at least 98 wt.-% up to 100 wt.-% of the film.

6. The film according to claim 1, wherein haze determined according to ASTM D1003-00 on a test film having a thickness of 50 micrometre is below 3.5%.

7. The film according to claim 1, wherein the ethylene-propylene-1-butene terpolymer base resin is bimodal as to the C4 content and/or is bimodal as to the molecular weight.

8. The film according to claim 1, wherein the ethylene-propylene-1-butene terpolymer base resin has a xylene soluble content of 15.0 to 19.0 wt.-% determined at 25? C. according ISO 16152; 2005.

9. A blend obtainable by compounding an ethylene-propylene-1-butene terpolymer base resin and a propylene butene random copolymer upgrading resin, wherein the ethylene-propylene-1-butene terpolymer base resin includes a) units derived from ethylene in an amount of 0.1 to 2.0 wt.-% with respect the total ethylene-propene-butene terpolymer base resin; and b) units derived from propylene in an amount of 88.0 to 95.9 wt.-% with respect the total ethylene-propene-butene terpolymer base resin; and c) units derived from butene in an amount of 4.0 to 10.0 wt.-% with respect the total ethylene-propene-butene terpolymer base resin, d) wherein the units derived from ethylene, propylene and butene add up to 100 wt.-%, and e) preferably a total amount of units derived from ethylene and butene of 6.0 to 9.0 wt.-% with respect the total ethylene-propene-butene terpolymer base resin, and f) preferably a ratio of the units derived from butene in weight percent versus the units derived from ethylene in weight percent of 3.0 to 16.0; wherein the ethylene-propene-butene terpolymer base resin has g) 2.1 regioinversions in an amount of 0.10 to 0.80 mol-% as determined by .sup.13C-NMR analysis (as described in the experimental part); and h) a melt flow rate MFR.sub.2 (230? C./2.16 kg) measured according to ISO 1133 in the range from 1.0 to 18.0 g/10 min, and i) a melting temperature Tm measured by differential scanning calorimetry (DSC) in the range from 123 to 142? C., and j) preferably a xylene soluble content of 5.0 to 25.0 wt.-% determined at 25? ? C.according ISO 16152; 2005 and wherein the propylene butene random copolymer upgrading resin has k) a melting temperature Tm measured by differential scanning calorimetry (DSC) in the range from 70 to 90? C., and l) units derived from butene in an amount of 20.0 to 35.0 wt.-% with respect the total propylene butene random copolymer upgrading resin, m) wherein the units derived from propylene and butene add up to 100 wt.-%, and n) a melt flow rate MFR.sub.2 (230? C./2.16 kg) measured according to ISO 1133 in the range of 1.0 to 18.0 g/10 min and optionally higher than the melt flow rate MFR.sub.2 (230? C./2.16 kg) of the base resin; and o) optionally an elongation at break (ASTM D638) of 100 to 900%.

10. The blend according to claim 9, obtainable by compounding an ethylene-propylene-1-butene terpolymer base resin and a propylene butene random copolymer upgrading resin, wherein the ethylene-propylene-1-butene terpolymer base resin includes a) units derived from ethylene in an amount 0.5 to 1.9 wt.-% with respect the total ethylene-propene-butene terpolymer base resin; and b) units derived from propylene in an amount of 90.1 to 95.0 wt.-% with respect the total ethylene-propene-butene terpolymer base resin; and c) units derived from butene in an amount of 4.5 to 8.0 wt.-% with respect the total ethylene-propene-butene terpolymer base resin, d) wherein the units derived from ethylene, propylene and butene add up to 100 wt.-%, and e) a total amount of units derived from ethylene and butene of 6.0 to 9.0 wt.-% with respect the total ethylene-propene-butene terpolymer base resin, and f) a ratio of the units derived from butene in weight percent versus the units derived from ethylene in weight percent of 3.0 to 16.0, more preferably 3.0 to 8.0; wherein the ethylene-propene-butene terpolymer base resin has g) 2.1 regioinversions in an amount of 0.20 to 0.50 mol % as determined by .sup.13C-NMR analysis (as described in the experimental part); and h) a melt flow rate MFR.sub.2 (230? C./2.16 kg) measured according to ISO 1133 in the range from 1.5 to 7.0 g/10 min, and i) a melting temperature Tm measured by differential scanning calorimetry (DSC) in the range from 125 to 135? C.; and preferably j) a xylene soluble content of 5.0 to 25.0 wt.-% more preferably 15.0 to 19.0 wt. % determined at 25? C. according ISO 16152; 2005; and wherein the propylene butene random copolymer upgrading resin has k) a melting temperature Tm measured by differential scanning calorimetry (DSC) in the range from 70 to 90? C., and l) units derived from butene in an amount of 22.0 to 29.0 wt.-% with respect the total propylene butene random copolymer upgrading resin, m) wherein the units derived from propylene and butene add up to 100 wt.-%, and n) a melt flow rate MFR.sub.2 (230? C./2.16 kg) measured according to ISO 1133 in the range of 1.0 to 18.0 g/10 min and preferably higher than the melt flow rate MFR.sub.2 (230? C./2.16 kg) of the base resin; and o) optionally an elongation at break (ASTM D638) of 100 to 900%, usually of 200 to 500%.

11. The blend according to claim 9, wherein the propylene butene random copolymer upgrading resin has one or more, preferably all of the following: p) a tensile strength at break (ASTM D638) of at least 15 MPa, q) a tensile modulus of least 250 MPa, measured according to ASTM D638; r) a shore D hardness (ASTM D2240) of at least 55; s) a melting temperature Tm measured by differential scanning calorimetry (DSC) in the range from 81 to 90? C.

12. The blend according to claims 9, wherein the ethylene-propylene-1-butene terpolymer base resin has 2.1 regioinversion in an amount of 0.20 to 0.35 mol % as determined by .sup.13C-NMR analysis (as described in the experimental part).

13. The blend according to claim 9, wherein the ethylene-propylene-1-butene terpolymer base resin is present in an amount of 70 to 95 wt.-% with respect to the total blend and wherein the propylene butene random copolymer upgrading resin is present in an amount of 5 to 30 wt.-% with respect to the total blend, wherein ethylene-propylene-1-butene terpolymer base resin and propylene butene random copolymer upgrading resin add up to at least 98 wt.-%, particularly 100 wt.-% of the total blend.

14. The blend according to claim 9, wherein the ethylene-propylene-1-butene terpolymer base resin is present in an amount of 70 to less than 85 wt.-% with respect to the total blend and wherein the propylene butene random copolymer upgrading resin is present in an amount of more than 15 to 30 wt.-% with respect to the total blend.

15. The blend according to claim 9, wherein the ethylene-propylene-1-butene terpolymer base resin is bimodal as to the units derived from butene and/or bimodal as to the molecular weight.

Description

EXPERIMENTAL PART

A. Measuring Methods

[0262] 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.

a) MFR.sub.2 (230? C.) was measured according to ISO 1133 (230? C., 2.16 kg load).
b) Quantification of microstructure by NMR spectroscopy

[0263] Quantitative nuclear-magnetic resonance (NMR) spectroscopy was used to quantify the comonomer content of the polymers.

[0264] Quantitative .sup.13C{.sup.1H} NMR spectra recorded in the molten-state using a Bruker Avance III 500 NMR spectrometer operating at 500.13 and 125.76 MHz for 1H and .sup.13C respectively. All spectra were recorded using a .sup.13C optimised 7 mm magic-angle spinning (MAS) probehead at 180? C. using nitrogen gas for all pneumatics. Approximately 200 mg of material was packed into a 7 mm outer diameter zirconia MAS rotor and spun at 4 kHz. This setup was chosen primarily for the high sensitivity needed for rapid identification and accurate quantification {klimke06, parkinson07, castignolles09}. Standard single-pulse excitation was employed utilising the NOE at short recycle delays of 3 s {pollard04, klimke06} and the RS-HEPT decoupling scheme {fillip05, griffin07}. A total of 1024 (1k) transients were acquired per spectra.

[0265] Quantitative .sup.13C{.sup.1H} NMR spectra were processed, integrated and relevant quantitative properties determined from the integrals. All chemical shifts are internally referenced to the methyl isotactic pentad (mmmm) at 21.85 ppm. Characteristic signals corresponding to the incorporation of 1-butene were observed {brandolini01} and the comonomer content quantified.

[0266] The amount of isolated 1-butene incorporated in PBP sequences was quantified using the integral of the ?B2 sites at 43.6 ppm accounting for the number of reporting sites per comonomer:

B=I.sub.?B2/2

[0267] The amount of consecutively incorporated 1-butene in PBBP sequences was quantified using the integral of the ??B2B2 site at 40.5 ppm accounting for the number of reporting sites per comonomer:

BB=2*I.sub.??B2B2

[0268] In presence of BB the value of B must be corrected for the influence of the ?B2 sites resulting from BB:

B=(I.sub.?B2/2)?BB/2

[0269] The total 1-butene content was calculated based on the sum of isolated and consecutively incorporated 1-butene:

B.sub.total=B+BB

[0270] Characteristic signals corresponding to the incorporation of ethylene were observed {brandolini01} and the comonomer content quantified.

[0271] The amount of isolated ethylene incorporated in PEP sequences was quantified using the integral of the SBB sites at 24.3 ppm accounting for the number of reporting sites per comonomer:

E=I.sub.S??

[0272] If characteristic signals corresponding to consecutive incorporation of ethylene in PEE sequence was observed the S?? site at 27.0 ppm was used for quantification:

EE=I.sub.S??

[0273] Characteristic signals corresponding to regio defects were observed {resconi00}. The presence of isolated 2,1-erythro regio defects was indicated by the presence of the two methyl sites at 17.7 and 17.2 ppm, by the methylene site at 42.4 ppm and confirmed by other characteristic sites. The presence of 2,1 regio defect adjacent an ethylene unit was indicated by the two inequivalent S?? signals at 34.8 ppm and 34.4 ppm respectively and the T?? at 33.7 ppm.

[0274] The amount of isolated 2,1-erythro regio defects (P.sub.21e isolated) was quantified using the integral of the methylene site at 42.4 ppm (I.sub.e9):

P.sub.21e isolated=I.sub.e9

[0275] If present the amount of 2,1 regio defect adjacent to ethylene (P.sub.E21) was quantified using the methine site at 33.7 ppm (I.sub.T??):

P.sub.E21=I.sub.T??

[0276] The total ethylene content was then calculated based on the sum of ethylene from isolated, consecutively incorporated and adjacent to 2,1 regio defects:

E.sub.total=E+E +P.sub.E21

[0277] The amount of propene was quantified based on the S?? methylene sites at 46.7 ppm including all additional propene units not covered by S?? e.g. the factor 3*P.sub.21e isolated accounts for the three missing propene units from isolated 2,1-erythro regio defects:

P.sub.total=I.sub.S??+3*P.sub.21e isolated+B+0.5*BB+E+0.5*EE+2*P.sub.E21

[0278] The total mole fraction of 1-butene and ethylene in the polymer was then calculated as:

fB=B.sub.total/(E.sub.total+P.sub.total+B.sub.total)

fE=E.sub.total/(E.sub.total+P.sub.total+B.sub.total)

[0279] The mole percent comonomer incorporation was calculated from the mole fractions:

B[mol %]=100*fB

E[mol %]=100*fE

[0280] The weight percent comonomer incorporation was calculated from the mole fractions:

B[wt.-%]=100*(fB*56.11)/((fE*28.05)+(fB*56.11)+((1?(fE+fB))*42.08))

E[wt.-%]=100*(fE*28.05)/((fE*28.05)+(fB*56.11)+((1?(fE+fB))*42.08))

[0281] The mole percent of isolated 2,1-erythro regio defects was quantified with respect to all propene:

[21e] mol %=100*P.sub.21e isolated/P.sub.total

[0282] The mole percent of 2, 1 regio defects adjacent to ethylene was quantified with respect to all propene:

[E21] mol %=100*P.sub.E21/P.sub.total

[0283] The total amount of 2,1 defects was quantified as following:

[21] mol %=[21e]+[E21]

[0284] Characteristic signals corresponding to other types of regio defects (2, 1-threo, 3,1 insertion) were not observed {resconi00}.

[0285] Literature (as referred to above):

TABLE-US-00002 klimke06 Klimke, K., Parkinson, M., Piel, C., Kaminsky, W., Spiess, H. W., Wilhelm, M., Macromol. Chem. Phys. 2006; 207: 382. parkinson07 Parkinson, M., Klimke, K., Spiess, H. W., Wilhelm, M., Macromol. Chem. Phys. 2007; 208: 2128. pollard04 Pollard, M., Klimke, K., Graf, R., Spiess, H. W., Wilhelm, M., Sperber, O., Piel, C., Kaminsky, W., Macromolecules 2004; 37: 813. filip05 Filip, X., Tripon, C., Filip, C., J. Mag. Resn. 2005, 176, 239 griffin07 Griffin, J. M., Tripon, C., Samoson, A., Filip, C., and Brown, S. P., Mag. Res. in Chem. 2007 45, S1, S198. castignolles09 Castignolles, P., Graf, R., Parkinson, M., Wilhelm, M., Gaborieau, M., Polymer 50 (2009) 2373. resconi00 Resconi, L., Cavallo, L., Fait, A., Piemontesi, F., Chem. Rev. 2000, 100, 1253. brandolini01 A. J. Brandolini, D.D. Hills, NMR spectra of polymers and polymer additives, Marcel Deker Inc., 2000

c) DSC Analysis, Melting Temperature (Tm) and Crystallization Temperature (Tc)

[0286] was measured with a TA Instrument Q2000 differential scanning calorimetry (DSC) on 5 to 7 mg samples. DSC is run according to ISO 11357/part 3/method C2 in a heat/cool/heat cycle with a scan rate of 10? C./min in the temperature range of ?30? C. to +225? C. Crystallization temperature (Tc) and crystallization enthalpy (Hc) were determined from the cooling step, while melting temperature (Tm) and melting enthalpy (Hm) were determined from the second heating step.

d) Haze

[0287] was determined according to ASTM D1003-00 on the blown test films of 50 micrometer thickness.

e) Sealing Initiation Temperature (SIT); Sealing End Temperature (SET), Sealing initiation temperature (SIT); sealing end temperature (SET), sealing range: The method determines the sealing temperature range (sealing range) of polypropylene films, in particular blown films or cast films according to ASTM F1921-12. Seal pressure, cool time and peel speed were modified as stated below. The sealing temperature range is the temperature range, in which the films can be sealed according to conditions given below.

[0288] The lower limit (heat sealing initiation temperature (SIT)) is the sealing temperature at which a sealing strength of >5 N is achieved. The upper limit (sealing end temperature (SET)) is reached, when the films stick to the sealing device.

[0289] The sealing range was determined on a J&B Universal Sealing Machine Type 3000 with a blown film of 50 ?m thickness with the following further parameters: [0290] Specimen width: 25.4 mm [0291] Seal Pressure: 0.1 N/mm.sup.2 [0292] Seal Time: 0.1 sec [0293] Cool time: 99 sec [0294] Peel Speed: 10 mm/sec [0295] Start temperature: 80? C. [0296] End temperature: 150? C. [0297] Increments: 10? C.

[0298] Specimen was sealed A to A at each sealbar temperature and seal strength (force) was determined at each step.

[0299] The temperature was determined at which the seal strength reaches 5 N.

f) Tensile Modulus

[0300] Tensile Modulus of film in machine and transverse direction were determined according to ISO 527-3 at 23? C. on blown films of 50 ?m thickness.

[0301] The modulus of the modifier was determined according to ASTM D638. The speed used for modulus detection was 0.6 mm/min, and 5 mm/min for elongation at break.

g) Dart Drop Strength (DDI) Also Called Dart Drop Impact

[0302] Dart-drop was measured using ASTM D1709, method A (Alternative Testing Technique) from the film samples. A dart with a 38 mm diameter hemispherical head was dropped from a height of 0.66 m onto a film clamped over a hole. Successive sets of twenty specimens were tested. One weight was used for each set and the weight was increased (or decreased) from set to set by uniform increments. The weight resulting in failure of 50% of the specimens was calculated and reported.

h) Xylene cold solubles (XCS, wt.-%):

[0303] Content of xylene cold solubles (XCS) was determined at 25? C. according ISO 16152; 2005.

i) Tear Resistance (Determined as Elmendorf Tear (N) in Machine (MD) and Transverse (TD) Direction

[0304] The tear strength was measured using the ISO 6383/2 method. The force required to propagate tearing across a film sample was measured using a pendulum device. The pendulum swings under gravity through an arc, tearing the specimen from pre-cut slit. The specimen was fixed on one side by the pendulum and on the other side by a stationary clamp. The tear resistance is the force required to tear the specimen. The relative tear resistance (N/mm) is then calculated by dividing the tear resistance by the thickness of the film.

B. Examples

[0305] Preparation of the first catalyst system for the ethylene-propene-butene terpolymer base resin.

[0306] The metallocene (MC1) (rac-anti-dimethylsilandiyl(2-methyl-4-phenyl-5-methoxy-6-tert-butyl-indenyl)(2-methyl-4-(4-tert-butylphenyl)indenyl)zirconium dichloride)

##STR00018##

[0307] has been synthesized as described in WO 2013/007650.

Preparation of MAO-Silica Support

[0308] A steel reactor equipped with a mechanical stirrer and a filter net was flushed with nitrogen and the reactor temperature was set to 20? C. Next silica grade DM-L-303 from AGC Si-Tech Co, pre-calcined at 600? C. (7.4 kg) was added from a feeding drum followed by careful pressuring and depressurising with nitrogen using manual valves. Then toluene (32 kg) was added. The mixture was stirred for 15 min. Next 30 wt % solution of MAO in toluene (17.5 kg) from Lanxess was added via feed line on the top of the reactor within 70 min. The reaction mixture was then heated up to 90? C. and stirred at 90? C. for additional two hours. The slurry was allowed to settle and the mother liquor was filtered off. The MAO treated support was washed twice with toluene (32 kg) at 90? C., following by settling and filtration. The reactor was cooled off to 60? C. and the solid was washed with heptane (32.2 kg). Finally MAO treated SiO.sub.2 was dried at 60? under nitrogen flow for 2 hours and then for 5 hours under vacuum (?0.5 barg) with stirring. MAO treated support was collected as a free-flowing white powder found to contain 12.6% Al by weight.

Catalyst System Preparation

[0309] 30 wt % MAO in toluene (2.2 kg) was added into a steel nitrogen blanked reactor via a burette at 20? C. Toluene (7 kg) was then added under stirring. Metallocene MC1 (286 g) was added from a metal cylinder followed by flushing with 1 kg toluene. The mixture was stirred for 60 minutes at 20? C. Trityl tetrakis(pentafluorophenyl) borate (336 g) was then added from a metal cylinder followed by a flush with 1 kg of toluene. The mixture was stirred for 1 h at room temperature. The resulting solution was added to a stirred cake of MAO-silica support prepared as described above over 1 hour. The cake was allowed to stay for 12 hours, followed by drying under N2 flow at 60? C. for 2h and additionally for 5 h under vacuum (?0.5 barg) under stirring. Dried catalyst was sampled in the form of pink free flowing powder containing 13.9 wt % Al and 0.26wt % Zr

Polymerization and Pelletization

[0310] Terpolymer IE1 and Copolymer CE2 were produced in a Borstar pilot plant comprising a prepolymerization reactor, one loop reactor and a gas phase reactor coupled in series using above described catalyst system. The polymerization 10 conditions are indicated in Table 1

TABLE-US-00003 TABLE 1 Polymerization process conditions for IE1 (terpolymer base resin) and CE2 ethylene-propene- butene terpolymer ethylene-propene- base resin copolymer base resin C2C3C4 terpo (IE1) C2C3 copo (CE2) Prepolymerization reactor Temp. (? C.) 20 25 Press. (kPa) 4973 5157 Residence time (h) 0.8 0.40 loop reactor Temp. (? C.) 70 68 Press. (kPa) 4864 5397 Feed H2/C3 ratio 0.1 0.3 (mol/kmol) Feed C2/C3 ratio 16.1 48.3 (mol/kmol) Feed C4/C3 ratio 25.4 0 (mol/kmol) Polymer Split (wt.-%) 41 74 [amount produced in loop reactor] MFR2 (g/10 min) 2 1.5 Total C2 (wt.-%) 1.0 4.8 Total C4 (wt.-%) 5.5 0 nature of polymer C3C2C4 terpolymer C3C2 copolymer produced in loop Gas phase reactor Temp. (? C.) 75 75 Press. (kPa) 2441 2500 H2/C3 ratio 1.5 3.0 (mol/kmol) C2/C3 ratio 120.8 215 (mol/kmol) C4/C3 ratio 61 0 (mol/kmol) Polymer Split [gas 59 26 phase reactor] (wt.-%) nature of polymer C3C2C4 terpolymer C3C2 copolymer produced in gas phase reactor nature of resulting C3C2C4 C3C2 copolymer + polymer in-situ blend terpolymer + C3C2 copolymer C3C2C4 terpolymer mixture mixture Pellet MFR.sub.2 (g/10 min) 2.1 1.2 Tm (? C.) 129 118 Tc (? C.) 91 79 C2 (wt.-%) 1.5 4.6 C4 (wt.-%) 6.6 0 C2 + C4 (wt.-%) 8.1 4.6 Ratio C4/C2 4.4 0 (wt.-%/wt.-%) 2.1 (mol %) 0.26 0.28 XCS (wt.-%) 17.1 7.9

[0311] Both polymer powders were compounded in a co-rotating twin-screw extruder Coperion ZSK 57 at 220? C. with 0.1 wt.-% antiblock agent (synthetic silica; CAS-no. 7631-86-9); 0.05 wt.-% antioxidant (Irgafos 168FF); 0.1 wt.-% of a sterical hindered phenol (Irganox 1010FF); 0.04 wt.-% of DHT-4A (CAS-no. 11097-59-9, Kisuma Chemicals).

[0312] Tafmer XM7080 was used as the propylene butene random copolymer upgrading resin. Tafmer XM7080 has a content of units derived from butene of 26.2 wt.-%, an MFR.sub.2 of 6 g/10 min, a melting temperature Tm of 87?C, a tensile modulus (ASTM D638) of 249 MPa, tensile strength at break (ASTM D638) of 20.2 MPa, and an elongation at break of 393%. Shore D hardness (ASTM D2240) is 55.

Blown Film Production

[0313] Films were produced on a Collin 30 lab scale blown film line. Film thickness was 50 microns and BUR was 1: 2.5. The melt temperature was 215? C., uptake speed is 6.2m/min.

[0314] The characteristics of the polypropylene compositions and the results of the films are provided below in table 2.

TABLE-US-00004 TABLE 2 Characteristics of the polypropylene compositions and the results of the films IE1 IE2 CE1 CE2 CE3 C2C3C4 terpo wt.-% 90 75 100 C2C3 copo wt.-% 100 90 Tafmer XM7080 wt.-% 10 25 10 TM/MD MPa 639 542 807 629 561 TM/TD MPa 646 559 807 654 561 Tear/MD N/mm 8.3 11.3 7.96 8.5 n.m. Tear/TD N/mm 18.39 23.39 16 20.25 n.m. Haze % 3.0 1.8 1.8 4.9 4.3 SIT ? C. 105 96 110 104 101 DDI g 64 110 54 56 68

[0315] As can be seen, blending the upgrading resin, i.e. the propylene butene copolymer with the terpolymer resulted in improved tear, SIT(below 106? C.) and DDI at only a moderate stiffness deterioration and still acceptable haze (below 3.5%). When comparative base resin CE2 (cf. above) was used, haze was not good and the balance of DDI and tensile modulus also turned out to be not favorable, i.e. the DDI was too low for the obtained stiffness.

[0316] It was surprisingly found that the combination of the terpolymer and the upgrading resin results in excellent low sealing initiation temperature (SIT) at a favorable DDI for the resulting (i.e. given) stiffness at simultaneously low haze, i.e. below the frequently accepted 3.5%.