CA2588770A1 - Homogeneous polymer blend and articles therefrom - Google Patents
Homogeneous polymer blend and articles therefrom Download PDFInfo
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- CA2588770A1 CA2588770A1 CA002588770A CA2588770A CA2588770A1 CA 2588770 A1 CA2588770 A1 CA 2588770A1 CA 002588770 A CA002588770 A CA 002588770A CA 2588770 A CA2588770 A CA 2588770A CA 2588770 A1 CA2588770 A1 CA 2588770A1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
- C08L23/142—Copolymers of propene at least partially crystalline copolymers of propene with other olefins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2314/00—Polymer mixtures characterised by way of preparation
- C08L2314/06—Metallocene or single site catalysts
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Nonwoven Fabrics (AREA)
- Artificial Filaments (AREA)
Abstract
This invention relates to homogeneous blends of: 1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight % alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 170° C. and a melt flow rate of 200 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having: a) 10 to 50 percent crystallinity or less; b) a melt flow rate of 200 dg/min or less; c) a DSC melting point (second melt Tm) of 130° C. or less; d) an intermolecular composition distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt % comonomer content with a difference of no greater than 20 wt % relative to the average wt % comonomer content of the copolymer; e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, for use in films, fibers, non-wovens, molded articles and the like.
Claims (100)
1. A film comprising a homogeneous blend of:
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 170°C
and a melt flow rate of 200 dg/min or less preferably the semi-crystalline polymer is a homopolymer, preferably of propylene); and
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 170°C
and a melt flow rate of 200 dg/min or less preferably the semi-crystalline polymer is a homopolymer, preferably of propylene); and
2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 10 to 50 percent crystallinity;
b) a melt flow rate of 200 dg/min or less;
c) a DSC melting point (second melt Tm) of 130°C or less;
d) an intermolecular composition distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer;
e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, where the blend has:
i) a melt flow rate of 0.5 to 100 dg/min; and ii) less than 5 weight % filler, based upon the weight of the polymers and the filler; and iii) a permanent set of greater than 65%; and where the film has:
1) a thickness of 2.5 to 635 microns;
2) a haze of 10% or less, prior to addition of clarifying or nucleating agents;
a) 10 to 50 percent crystallinity;
b) a melt flow rate of 200 dg/min or less;
c) a DSC melting point (second melt Tm) of 130°C or less;
d) an intermolecular composition distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer;
e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, where the blend has:
i) a melt flow rate of 0.5 to 100 dg/min; and ii) less than 5 weight % filler, based upon the weight of the polymers and the filler; and iii) a permanent set of greater than 65%; and where the film has:
1) a thickness of 2.5 to 635 microns;
2) a haze of 10% or less, prior to addition of clarifying or nucleating agents;
3) a 45 degree gloss of 85 or more;
4) a 1° Secant tensile modulus of 860 to 205 MPa;
5) an Elmendorf tear in the machine direction of 1.57 g/micron or more;
6) an Elmendorf tear in the transverse direction of 1.57 g/micron or more;
and
and
7) a total energy impact at 23 °C of 2.7 J or more.
2. The film of claim 1 wherein the difference in comonomer content is no greater than 10 weight%.
3. The film of claim 1 or 2 wherein the composition distribution of the semi-amorphous copolymer is 90 or more.
4. The film of any of claims 1 to 3 wherein the film has a machine direction Elmendorf Tear or 2.16 g/micron or greater.
5. The film of any of claims 1 to 4 wherein the film has a Total energy impact of 4 J or greater.
6. The film of any of claims 1 to 5 wherein the film has a Puncture Energy of 0.12 J/micron or greater.
7. The film of any of claims 1 to 6 wherein the film has a 1% Secant tensile modulus of 518 MPa or lower.
2. The film of claim 1 wherein the difference in comonomer content is no greater than 10 weight%.
3. The film of claim 1 or 2 wherein the composition distribution of the semi-amorphous copolymer is 90 or more.
4. The film of any of claims 1 to 3 wherein the film has a machine direction Elmendorf Tear or 2.16 g/micron or greater.
5. The film of any of claims 1 to 4 wherein the film has a Total energy impact of 4 J or greater.
6. The film of any of claims 1 to 5 wherein the film has a Puncture Energy of 0.12 J/micron or greater.
7. The film of any of claims 1 to 6 wherein the film has a 1% Secant tensile modulus of 518 MPa or lower.
8. The film of any of claims 1 to 7 wherein the film has a haze of 5% or less.
9. The film of any of paragraphs 1 to 8 wherein the film has a 45 degree gloss of 88 units or greater.
10. The film of any of claims 1 to 9 wherein the film has a 1% secant tensile modulus of 690 MPa or less, an MD Elmendorf Tear of 1.77 g/micron or more, a haze of 2% or lower, a 45 degree gloss of 88 units or higher, and a Total energy impact at 23°C of 4 J or greater.
11. The film of any of paragraphs 1 to 10 wherein the film has a 1% secant tensile modulus of 518 MPa or lower, an MD Elmendorf tear of 2.16 g/microns or greater, a haze of 2% or lower, a 45 degree gloss of 88 units or higher, and a Total energy impact at 23 °C of 4.75J or greater.
12. The film of any of paragraphs 1 to 11 wherein the blend has a permanent set of 85% or greater.
13. A molded article comprising a homogeneous blend of 1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 170°C
and a melt flow rate of 200 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight %
of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 10 to 50 percent crystallinity or less;
b) a melt flow rate of 200 dg/min or less;
c) a DSC melting point (second melt Tm) of 130°C or less;
d) an intermolecular composition distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer;
e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, where the blend has:
i) a melt flow rate of 0.5 to 200 dg/min; and ii) less than 5 weight % filler, based upon the weight of the polymers and the filler; and iii) a permanent set of greater than 65%; and iv) a haze of 12% or less measured on a 1 mm thick injection molded chip, where the molded article has:
1) a thickness of 250 µm to 10 mm;
2) a 1% Secant Flexural Modulus at 23 °C of 1035 MPa or less;
3) a Gardner Impact Strength at 23°C of 11.3 J or more; and 4) a Gardner Impact Strength at 0°C of 50 5.6 J or more.
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 170°C
and a melt flow rate of 200 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight %
of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 10 to 50 percent crystallinity or less;
b) a melt flow rate of 200 dg/min or less;
c) a DSC melting point (second melt Tm) of 130°C or less;
d) an intermolecular composition distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer;
e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, where the blend has:
i) a melt flow rate of 0.5 to 200 dg/min; and ii) less than 5 weight % filler, based upon the weight of the polymers and the filler; and iii) a permanent set of greater than 65%; and iv) a haze of 12% or less measured on a 1 mm thick injection molded chip, where the molded article has:
1) a thickness of 250 µm to 10 mm;
2) a 1% Secant Flexural Modulus at 23 °C of 1035 MPa or less;
3) a Gardner Impact Strength at 23°C of 11.3 J or more; and 4) a Gardner Impact Strength at 0°C of 50 5.6 J or more.
14. The molded article of claim 13 wherein the molded article has a Notched Izod Impact Strength at 23°C of 53J/m or more.
15. The molded article of claim 13 or 14 wherein the molded article has a Gardner Impact Strength at 23°C of 22.6 J or more.
16. The molded article of any of claims 13 to 15 wherein the molded article has a Notched Izod Impact Strength at 23°C of 80 J/m or more.
17. The molded article of any of claims 13 to 16 wherein the molded article has a Gardner Impact Strength at 23°C of 22.6 J or more with failure being in ductile mode.
18. The molded article of any of claims 13 to 17 wherein the molded article has an Ultimate Elongation at 23 °C of 1000% or more.
19. The molded article of any of claims 13 to 18 where the difference in comonomer content is no greater than 10 weight%.
20. The molded article of any of claims 13 to 19 wherein the intermolecular composition distribution of the semi-amorphous copolymer is 90% or more.
21. The molded article of any of claims 13 to 20 wherein the intermolecular composition distribution of the semi-amorphous copolymer is 90% or more and the difference in comonomer content is no greater than 10 weight%.
22. The molded article of any of claims 13 to 21 wherein the molded article has a 1% secant flexural modulus at 23 °C of less than 690 MPa.
23. The molded article of any of claims 13 to 22 wherein the blend has a haze of less than 10%.
24. The molded article of any of claims 13 to 23 wherein the molded article has a 1% secant flexural modulus at 23 °C of less than 690 MPa, an ultimate elongation at 23 °C of greater than 1000%, a Gardner at both 23°C and 0°C of greater than 22.6 J, an Instrumented impact at both 23°C and 0°C
of greater than 27.1 J.
of greater than 27.1 J.
25. The molded article of any of claims 13 to 24 wherein the molded article has a 1% secant flexural modulus less than 690 MPa, a notched Izod impact strength at 23°C of greater than 80 J/m, an Instrumented impact at both 23°C and 0°C of greater than 27.1J where failures are all in ductile mode.
26. The molded article of any of claims 13 to 25 wherein the blend has permanent set of 85% or greater.
27. The molded article of any of claims 13 to 26 wherein the blend has permanent set of 150% or greater.
28. The molded article of any of claims 13 to 27 where in the semi-crystalline polymer is a propylene homopolymer.
29. The molded article of any of claims 13 to 28 wherein the semi-amorphous polymer has a heat of fusion of from 10 to 40 J/g.
30. The molded article of any of claims 13 to 29 wherein the semi-crystalline polymer has a melting point of from 125 to 160°C.
31. The molded article of any of claims 13 to 30 wherein the semi-amorphous polymer has a melting point of from 35 to 100°C.
32. A non-woven comprising a homogeneous blend of:
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight % alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 170°C and a melt flow rate of 2000 dg/min or less (preferably the semi-crystalline polymer is a homopolymer, preferably of propylene); and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) less than 50 percent crystallinity;
b) a melt flow rate of 2000 dg/min or less;
c) a DSC melting point (second melt Tm) of 130°C or less;
d) an intermolecular composition distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer and e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, where the blend has:
i) a melt flow rate of 1 to 2000 dg/min; and ii) less than 5 weight % filler, based upon the weight of the polymers and the filler, iii) a permanent set of greater than 65%; and iv) a haze of 12 % or less measured on a 1 mm thick injection molded chip where the non-woven has:
1) a Hand of 40 g or less for 35 g/sm fabrics;
2) an optimum bonding temperature at least 5°C lower than the optimum bonding temperature for the same nonwoven article made from the same composition except that the semi-amorphous copolymer is absent.
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight % alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 170°C and a melt flow rate of 2000 dg/min or less (preferably the semi-crystalline polymer is a homopolymer, preferably of propylene); and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) less than 50 percent crystallinity;
b) a melt flow rate of 2000 dg/min or less;
c) a DSC melting point (second melt Tm) of 130°C or less;
d) an intermolecular composition distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer and e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, where the blend has:
i) a melt flow rate of 1 to 2000 dg/min; and ii) less than 5 weight % filler, based upon the weight of the polymers and the filler, iii) a permanent set of greater than 65%; and iv) a haze of 12 % or less measured on a 1 mm thick injection molded chip where the non-woven has:
1) a Hand of 40 g or less for 35 g/sm fabrics;
2) an optimum bonding temperature at least 5°C lower than the optimum bonding temperature for the same nonwoven article made from the same composition except that the semi-amorphous copolymer is absent.
33. The non-woven of claim 32 wherein the nonwoven has a hand on 35 g/sm fabric of 30 g or less, preferably 20 g or less, preferably 15 g or less.
34. The non-woven of claim 32 or 33 wherein the nonwoven has an optimum bonding temperature at least 7.5°C lower than the optimum bonding temperature for the same nonwoven made from the same composition except that the semi-amorphous copolymer is absent.
35. The non-woven of any of paragraphs 32 to 34 wherein the nonwoven has an optimum bonding temperature at least 10°C lower than the optimum bonding temperature for the same nonwoven made from the same composition except that the semi-amorphous copolymer is absent.
36. The non-woven of any of paragraphs 32 to 35 wherein at 35 g/sm the non-woven has a hand of 30 g or lower and a TD peak tensile load under optimum bonding of 3180 g force or greater.
37. The non-woven of. any of claims 32 to 36 wherein the difference in comonomer content is no greater than 10 weight%.
38. The non-woven of any of claims 32 to 37 wherein the intermolecular composition distribution of the semi-amorphous copolymer is 90% or more.
39. The non-woven of any of claims 32 to 38 wherein the intermolecular composition distribution of the semi-amorphous copolymer is 90% or more and the difference in comonomer content is no greater than 10 weight%.
40. The non-woven of any of claims 32 to 39 wherein the blend has a haze of less than 10%.
41. The non-woven of any of claims 32 to 40 wherein the blend comprises from 1 to 5000 ppm of a slip agent.
42. The non-woven of any of claims 32 to 41 wherein the blend comprises a nucleating agent.
43. The non-woven of any of claims 32 to 42 wherein the blend further comprises nucleating agent selected from the group consisting of adipic acid, benzoic acid, or metal salts of these acids, sorbitols, and 3,4-dimethylbenzylidene sorbitol.
44. A homogeneous polymer blend comprising:
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 160°C
and a melt flow rate of 50 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C 10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 8 to 35 percent crystallinity or less;
b) a melt flow rate of 1 to 50 dg/min;
c) a DSC melting point (second melt Tm) of 90°C or less;
d) an intermolecular composition distribution compositional distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer; and e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, and g) the blend comprises less than 5 weight % filler, based upon the weight of the polymers and the filler,, where the blend has:
a) a permanent set of greater than 65%;
b) a haze of 20% or less;
c) a melt flow rate of 1 to 50 dg/min; and d) optionally, a heat deflection temperature of 45°C or more.
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 160°C
and a melt flow rate of 50 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C 10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 8 to 35 percent crystallinity or less;
b) a melt flow rate of 1 to 50 dg/min;
c) a DSC melting point (second melt Tm) of 90°C or less;
d) an intermolecular composition distribution compositional distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer; and e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, and g) the blend comprises less than 5 weight % filler, based upon the weight of the polymers and the filler,, where the blend has:
a) a permanent set of greater than 65%;
b) a haze of 20% or less;
c) a melt flow rate of 1 to 50 dg/min; and d) optionally, a heat deflection temperature of 45°C or more.
45. The composition of claim 44 the intermolecular composition distribution of the semi-amorphous copolymer is 90% or more and/or the difference in comonomer content is no greater than 10 weight%.
46. The composition of claim 44 or 45 wherein the blend has a permanent set of 85% or greater, preferably 100% or greater, preferably 150% or greater.
47. The composition of any of claims 44 to 46 wherein the blend comprises from 1 to 5000 ppm of a slip agent.
48. The composition of any of claims 44 to 47 wherein the blend comprises a nucleating agent.
49. The composition of any of claims 44 to 48 wherein the semi-crystalline polymer comprises propylene and from 1 to 3 weight % of one or more comonomers selected from the group consisting of ethylene, butene, pentene, hexene, heptene, octene, nonene, and decene.
50. The composition of any of claims 44 to 49 wherein the semi-crystalline polymer is a propylene homopolymer.
51. The composition of any of claims 44 to 50 wherein the semi-amorphous polymer has a heat of fusion of from 10 to 40 J/g.
52. The composition of any of claims 44 to 51 wherein the semi-amorphous polymer has a melting point of from 35 to 100°C.
53. A film comprising a homogeneous polymer blend comprising:
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 160°C
and a melt flow rate of 50 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 8 to 35 percent crystallinity or less;
b) a melt flow rate of 1 to 50 dg/min;
c) a DSC melting point (second melt Tm) of 90°C or less;
d) an intermolecular composition distribution compositional distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer; and e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, and g) the blend comprises less than 5 weight % filler, based upon the weight of the polymers and the filler, where the blend has:
a) a permanent set of greater than 65%;
b) a haze of 20% or less;
c) a melt flow rate of 0.5 to 100 dg/min, and where the film has:
1) a thickness of 0.1 to 25 mils (2.5 to 635 microns);
2) a haze of 20% or less, prior to addition of clarifying or nucleating agents;
3) a 1° Secant flexural modulus of 860 to 205 MPa;
4) an Elmendorf tear in the machine direction 1.57 g/micron or more;
5) an Elmendorf tear in the transverse direction of 1.57 g/micron or more;
and 6) a total energy impact at 23 °C of 2.7 J or more.
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 160°C
and a melt flow rate of 50 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 8 to 35 percent crystallinity or less;
b) a melt flow rate of 1 to 50 dg/min;
c) a DSC melting point (second melt Tm) of 90°C or less;
d) an intermolecular composition distribution compositional distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer; and e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, and g) the blend comprises less than 5 weight % filler, based upon the weight of the polymers and the filler, where the blend has:
a) a permanent set of greater than 65%;
b) a haze of 20% or less;
c) a melt flow rate of 0.5 to 100 dg/min, and where the film has:
1) a thickness of 0.1 to 25 mils (2.5 to 635 microns);
2) a haze of 20% or less, prior to addition of clarifying or nucleating agents;
3) a 1° Secant flexural modulus of 860 to 205 MPa;
4) an Elmendorf tear in the machine direction 1.57 g/micron or more;
5) an Elmendorf tear in the transverse direction of 1.57 g/micron or more;
and 6) a total energy impact at 23 °C of 2.7 J or more.
54. The film of claim 53 wherein the difference in comonomer content is no greater than 10 weight%
55. The film of claim 53 or 54 the intermolecular composition distribution of the semi-amorphous copolymer is 90% or more.
56. The film of any of claims 53 to 55 wherein the film has a machine direction Elmendorf Tear or 2.16 g/micron or greater.
57. The film of any of claims 53 to 56 wherein the film has a Total energy impact of 4 J or greater.
58. The film of any of claims 53 to 57 wherein the film has a Puncture Energy of 0.12 J/micron or greater.
59. The film of any of claims 53 to 58 wherein the film has a 1% Secant tensile modulus of 518 MPa or lower.
60. The film of any of claims 53 to 59 wherein the film has a haze of 5% or less.
61. The film of any of claims 53 to 60 wherein the film has a 45 degree gloss of 88 units or greater.
62. The film of any of claims 53 to 61 wherein the film has a 1% secant tensile modulus of 690 MPa or less, an MD Elmendorf Tear of 1.77 g/micron or more, a haze or 2% or lower, a 45 degree gloss of 88 units or higher, and a Total energy impact at 23°C of 4 J or greater.
63. The film of any of claims 53 to 63 wherein the film has a 1% secant tensile modulus of 518 MPa or lower, an MD Elmendorf tear of 2.16 g/microns or greater, a haze of 2% or lower, a 45 degree gloss of 88 units or higher, and a Total energy impact at 23 °C of 4.75J or greater.
64. The film of any of claims 53 to 63 wherein the blend has a permanent set of 85% or greater.
65. The film of any of claims 53 to 64 wherein the blend comprises from 1 to 5000 ppm of a slip agent.
66. The film of any of claims 53 to 65 wherein the blend comprises a nucleating agent.
67. The film of any of claims 53 to 66 wherein the semi-crystalline polymer comprises propylene and from 1 to 3 weight % of one or more comonomers selected from the group consisting of ethylene, butene, pentene, hexene, heptene, octene, nonene, and decene.
68. The film of any of claims 53 to 67 wherein the semi-crystalline polymer is a propylene homopolymer.
69. The film of any of claims 53 to 68 wherein the semi-amorphous polymer has a heat of fusion of from 10 to 40 J/g.
70. The film of any of claims 53 to 69 wherein the semi-amorphous polymer has a melting point of from 35 to 100°C.
71. A fiber comprising a homogeneous polymer blend comprising:
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 160°C
and a melt flow rate of 50 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 8 to 35 percent crystallinity;
b) a melt flow rate of 1 to 50 dg/min;
c) a DSC melting point (second melt Tm) of 90°C or less;
d) an intermolecular composition distribution compositional distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer;
e) an Mw/Mn of 1.5 to 4; and f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, where the blend:
1) comprises less than 5 weight % filler, based upon the weight of the polymers and the filler;
2) has a permanent set of greater than 65%;
3) has a haze of 20% or less; and 4) has a melt flow rateof from 1 to 50 dg/min, and where the fiber has:
1) a Hand of 40 g or less when converted into spunbond fabric of 35 g/sm fabrics basis weight.
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 160°C
and a melt flow rate of 50 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 8 to 35 percent crystallinity;
b) a melt flow rate of 1 to 50 dg/min;
c) a DSC melting point (second melt Tm) of 90°C or less;
d) an intermolecular composition distribution compositional distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer;
e) an Mw/Mn of 1.5 to 4; and f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, where the blend:
1) comprises less than 5 weight % filler, based upon the weight of the polymers and the filler;
2) has a permanent set of greater than 65%;
3) has a haze of 20% or less; and 4) has a melt flow rateof from 1 to 50 dg/min, and where the fiber has:
1) a Hand of 40 g or less when converted into spunbond fabric of 35 g/sm fabrics basis weight.
72. A non-woven comprising a homogeneous polymer blend comprising:
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 160°C
and a melt flow rate of 50 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 8 to 35 percent crystallinity;
b) a melt flow rate of 1 to 50 dg/min;
c) a DSC melting point (second melt Tm) of 90°C or less;
d) an intermolecular composition distribution compositional distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer; and e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, and g) the blend comprises less than 5 weight % filler, based upon the weight of the polymers and the filler, where the blend has:
a) a permanent set of greater than 65%;
b) a haze of 20% or less; and c) melt flow rate of 1 to 2000 dg/min, and and where the non-woven has:
1) a Hand of 40 g or less for 35 g/sm fabrics;
2) an optimum bonding temperature at least 5°C lower than the optimum bonding temperature for the same nonwoven article made from the same composition except that the semi-amorphous copolymer is absent.
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 160°C
and a melt flow rate of 50 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 8 to 35 percent crystallinity;
b) a melt flow rate of 1 to 50 dg/min;
c) a DSC melting point (second melt Tm) of 90°C or less;
d) an intermolecular composition distribution compositional distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer; and e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, and g) the blend comprises less than 5 weight % filler, based upon the weight of the polymers and the filler, where the blend has:
a) a permanent set of greater than 65%;
b) a haze of 20% or less; and c) melt flow rate of 1 to 2000 dg/min, and and where the non-woven has:
1) a Hand of 40 g or less for 35 g/sm fabrics;
2) an optimum bonding temperature at least 5°C lower than the optimum bonding temperature for the same nonwoven article made from the same composition except that the semi-amorphous copolymer is absent.
73. The non-woven of claim 72 wherein the nonwoven has a hand on 35 g/sm fabric of 30 g or less.
74. The non-woven of claim 72 or 73 wherein the nonwoven has an optimum bonding temperature at least 7.5°C lower than the optimum bonding temperature for the same nonwoven made from the same composition except that the semi-amorphous copolymer is absent.
75. The non-woven of any of claims 72 to 74 wherein the nonwoven has an optimum bonding temperature at least 10°C lower than the optimum bonding temperature for the same nonwoven made from the same composition except that the semi-amorphous copolymer is absent.
76. The non-woven of any of claims 72 to 75 wherein at 35 g/sm the non-woven has a hand of 30 g or lower and a TD peak tensile load under optimum bonding of 3180 g force or greater.
77. The fiber of claim 71 or the non-woven of any of claims 72 to 76 the difference in comonomer'content is no greater than 10 weight%.
78. The fiber of claim 71 or the non-woven of any of claims 72 to 77 wherein the intermolecular composition distribution of the semi-amorphous copolymer is 90% or more.
79. The fiber of claim 71 or the non-woven of any of claims 72 to 78 wherein the intermolecular composition distribution of the semi-amorphous copolymer is 90% or more and the difference in comonomer content is no greater than 10 weight%.
80. The fiber of claim 71 or the non-woven of any of claims 72 to 79 wherein the blend has a haze of less than 10%.
81. The fiber of claim 71 or the non-woven of any of claims 72 to 80 wherein the blend comprises from 1 to 5000 ppm of a slip agent.
82. The fiber of claim 71 or the non-woven of any of claims 72 to 81 wherein the blend comprises a nucleating agent selected from the group consisting of adipic acid, benzoic acid, or metal salts of these acids, sorbitols, and 3,4-dimethylbenzylidene sorbitol.
83. A molded article comprising a homogeneous polymer blend comprising:
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 160°C
and a melt flow rate of 50 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 8 to 35 percent crystallinity;
b) a melt flow rate of 1 to 50 dg/min;
c) a DSC melting point (second melt Tm) of 90°C or less;
d) an intermolecular composition distribution compositional distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer; and e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, and g) the blend comprises less than 5 weight % filler, based upon the weight of the polymers and the filler, where the blend has:
i) a melt flow rate of 0.5 to 200 dg/min; and ii) optionally, less than 5 weight % filler, based upon the weight of the polymers and the filler; and iii) a permanent set of greater than 65%; and iv) a haze of 12% or less measured on a 1 mm thick injection molded chip;
and v) optionally, a heat deflection temperature of 45°C or more, where the molded article has:
1) a thickness of 250 µm to 10 mm;
2) a 1% Secant Flexural Modulus at 23 °C of 1035 MPa or less;
3) a Gardner Impact Strength at 23°C of 11.3 J or more; and 4) a Gardner Impact Strength at 0°C of 5.6 J or more.
1) from 60 to 99 weight percent of one or more semi-crystalline polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-crystalline polymer comprising propylene and from 0 to 5 weight %
alpha-olefin comonomer (based upon the weight of the polymer), said semi-crystalline polymers each having a melting point between 100 and 160°C
and a melt flow rate of 50 dg/min or less; and 2) from 1 to 40 weight % of one or more semi-amorphous polymers (based upon the weight of the semi-crystalline and semi-amorphous polymers), each semi-amorphous polymer comprising propylene and from 5 to 12 weight % of one or more C2 and or C4 to C10 alpha-olefin comonomers, said semi-amorphous polymers each having:
a) 8 to 35 percent crystallinity;
b) a melt flow rate of 1 to 50 dg/min;
c) a DSC melting point (second melt Tm) of 90°C or less;
d) an intermolecular composition distribution compositional distribution as determined by thermal fractionation in hexane such that 85% by weight or more of the polymer is isolated as one or two adjacent, soluble fractions with the balance of the polymer in immediately preceding or succeeding fractions; and wherein each of these fractions has a wt% comonomer content with a difference of no greater than 20 wt% relative to the average wt% comonomer content of the copolymer; and e) an Mw/Mn of 1.5 to 4, f) a triad tacticity of three propylene units, as measured by 13C NMR, of 75% or greater, and g) the blend comprises less than 5 weight % filler, based upon the weight of the polymers and the filler, where the blend has:
i) a melt flow rate of 0.5 to 200 dg/min; and ii) optionally, less than 5 weight % filler, based upon the weight of the polymers and the filler; and iii) a permanent set of greater than 65%; and iv) a haze of 12% or less measured on a 1 mm thick injection molded chip;
and v) optionally, a heat deflection temperature of 45°C or more, where the molded article has:
1) a thickness of 250 µm to 10 mm;
2) a 1% Secant Flexural Modulus at 23 °C of 1035 MPa or less;
3) a Gardner Impact Strength at 23°C of 11.3 J or more; and 4) a Gardner Impact Strength at 0°C of 5.6 J or more.
84. The molded article of claim 83 wherein the molded article has a Notched Izod Impact Strength at 23°C of 53J/m or more.
85. The molded article of claim 83 or 84 wherein the molded article has a Gardner Impact Strength at 23°C of 22.6 J or more.
86. The molded article of any of claims 83 to 85 wherein the molded article has a Notched Izod Impact Strength at 23°C of 80 J/m or more.
87. The molded article of any of claims 83 to 86 wherein the molded article has a Gardner Impact Strength at 23°C of 22.6 J or more with failure being in ductile mode.
88. The molded article of any of claims 83 to 87 wherein the molded article has an Ultimate Elongation at 23 °C of 1000% or more.
89. The molded article of any of claims 83 to 88 wherein the difference in comonomer content is no greater than 10 weight%.
90. The molded article of any of claims 83 to 89 the intermolecular composition distribution of the semi-amorphous copolymer is 90% or more.
91. The molded article of any of claims 83 to 90 wherein the intermolecular composition distribution of the semi-amorphous copolymer is 90% or more and the difference in comonomer content is no greater than 10 weight%.
92. The molded article of any of claims 83 to 91 wherein the molded article has a 1% secant flexural modulus at 23 °C of less than 690 MPa.
93. The molded article of any of claims 83 to 92 wherein the blend has a haze of less than 10%.
94. The molded article of any of claims 83 to 93 wherein the molded article has a 1% secant flexural modulus at 23 °C of less than 690 MPa, an ultimate elongation at 23 °C of greater than 1000%, a Gardner at both 23°C and 0°C of greater than 22.6 J, an Instrumented impact at both 23°C and 0°C
of greater than 27.1 J.
of greater than 27.1 J.
95. The molded article of any of claims 83 to 94 wherein the molded article has a 1% secant flexural modulus less than 690 MPa, a notched Izod impact strength at 23°C of greater than 80 J/m, an Instrumented impact at both 23°C and 0°C of greater than 27.1J where failures are all in ductile mode.
96. The molded article of any of claims 83 to 95 wherein the blend has permanent set of 85% or greater.
97. The molded article of any of claims 83 to 96 where in the semi-crystalline polymer is a propylene homopolymer.
98. The molded article of any of claims 83 to 97 wherein the semi-amorphous polymer has a heat of fusion of from 10 to 40 J/g.
99. The molded article of any of claims 83 to 98 wherein the semi-crystalline polymer has a melting point of from 125 to 160°C.
100. The molded article of any of claims 83 to 99 wherein the semi-amorphous polymer has a melting point of from 35 to 100°C.
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US60/655,310 | 2005-02-22 | ||
PCT/US2005/044615 WO2006065648A1 (en) | 2004-12-17 | 2005-12-09 | Homogeneous polymer blend and articles therefrom |
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CA2588770C CA2588770C (en) | 2010-03-23 |
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EP (1) | EP1831304B1 (en) |
JP (1) | JP4782800B2 (en) |
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2005
- 2005-12-09 DE DE602005021248T patent/DE602005021248D1/en active Active
- 2005-12-09 EP EP05853516A patent/EP1831304B1/en not_active Not-in-force
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- 2005-12-09 CA CA2588770A patent/CA2588770C/en not_active Expired - Fee Related
- 2005-12-09 US US11/299,022 patent/US7619038B2/en not_active Expired - Fee Related
- 2005-12-09 AT AT05853516T patent/ATE467658T1/en not_active IP Right Cessation
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CA2588770C (en) | 2010-03-23 |
JP4782800B2 (en) | 2011-09-28 |
US7619038B2 (en) | 2009-11-17 |
EP1831304A1 (en) | 2007-09-12 |
WO2006065648A1 (en) | 2006-06-22 |
EP1831304B1 (en) | 2010-05-12 |
DE602005021248D1 (en) | 2010-06-24 |
JP2008524387A (en) | 2008-07-10 |
US20060183860A1 (en) | 2006-08-17 |
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