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Publication numberCN1890276 A
Publication typeApplication
Application numberCN 200480035710
PCT numberPCT/US2004/037833
Publication date3 Jan 2007
Filing date12 Nov 2004
Priority date14 Nov 2003
Also published asCA2545203A1, CA2545203C, CA2546075A1, CA2546075C, CN1878799A, CN1878799B, CN1890276B, EP1687345A1, EP1687345B1, EP1687346A1, EP1687346B1, US7390866, US7605217, US7928165, US8013093, US20050107529, US20050107530, US20050107534, US20050131142, WO2005049670A1, WO2005049671A1, WO2005049672A1
Publication number200480035710.2, CN 1890276 A, CN 1890276A, CN 200480035710, CN-A-1890276, CN1890276 A, CN1890276A, CN200480035710, CN200480035710.2, PCT/2004/37833, PCT/US/2004/037833, PCT/US/2004/37833, PCT/US/4/037833, PCT/US/4/37833, PCT/US2004/037833, PCT/US2004/37833, PCT/US2004037833, PCT/US200437833, PCT/US4/037833, PCT/US4/37833, PCT/US4037833, PCT/US437833
InventorsS达塔, 赵锐, S斯里尼瓦斯, M阿明, 程佳永, A萨努内, PS拉维尚卡尔
Applicant埃克森美孚化学专利公司
Export CitationBiBTeX, EndNote, RefMan
External Links: SIPO, Espacenet
Propylene-based elastomers and uses thereof
CN 1890276 A
Abstract
The present invention provides curable and cured propylene-based elastomers, optionally including a diene, and having isotactic polypropylene crystallinity, a melting point by DSC equal to or less than 110 DEG C, and a heat of fusion of from 5 J/g to 50 J/g. The present invention also provides blend compositions comprising any of the propylene-based elastomers described herein. The present invention also provides compositions comprising any of the propylene-based elastomers described herein and 1 to 100 parts by weight of inorganic filler per 100 parts of polymer. The present invention also provides films, fibers, non-wovens, molded objects, and extruded forms which include any of the inventive compositions described herein.
Claims(43)  translated from Chinese
1.弹性体,其包含:(a)丙烯衍生的单元,其量为至少60wt%,优选在80-90wt%的范围内,基于组分(a)、(b)和(c)的总重量计;(b)二烯衍生的单元,其量在0.3-10wt%的范围内,优选在0.3-3wt%的范围内,基于组分(a)、(b)和(c)的总重量计;和(c)乙烯衍生的单元,其量为至少6wt%,优选在8-20wt%的范围内,更优选在10-20wt%的范围内,基于组分(a)、(b)和(c)的总重量计;其中所述弹性体具有等规聚丙烯结晶性,等于或低于110℃的DSC熔点,和5J/g至50J/g的熔化热。 1. elastomer, comprising: (a) propylene-derived units in an amount of at least 60wt%, preferably in the range of 80-90wt%, based on component (a), (b) and (c) of the total weight of count; (b) a diene-derived units in an amount in the range 0.3-10wt%, preferably in the range of 0.3-3wt%, based on component (a), (b) and (c) the total weight of ; and (c) ethylene-derived units in an amount of at least 6wt%, preferably in the range of 8-20wt%, more preferably in the range of 10-20wt%, based on component (a), (b) and ( c) the total weight; wherein the elastomer has a crystalline isotactic polypropylene, is equal to or lower than the DSC melting point of 110 ℃, and 5J / g to 50J / g heat of fusion.
2.权利要求1的弹性体,其中所述二烯为5-乙叉-2-降冰片烯,并且其优选以基于组分(a)、(b)和(c)的总重量计1-3wt%范围内的量存在。 The total weight of elastomer of claim 1, wherein said diene is 5-ethylidene-2-norbornene, and it is preferably based on the component (a), (b) and (c) count 1- an amount within the range of 3wt% exists.
3.权利要求1的弹性体,其中所述二烯为5-乙烯基-2-降冰片烯,并且其优选以基于组分(a)、(b)和(c)的总重量计0.5-1.5wt%范围内的量存在。 Elastomer of claim 1, wherein said diene is 5-vinyl-2-norbornene, and it is preferably based on the total weight of components (a), (b) and (c) 0.5 to count an amount within the range of the presence of 1.5wt%.
4.前述权利要求中任一项的弹性体,其中所述弹性体具有0.5至100,优选5-40的门尼粘度ML(1+4)@125℃。 Elastomer according to any one of the preceding claims, wherein said elastomer has from 0.5 to 100, preferably 5 to 40 Mooney viscosity ML (1 + 4) @ 125 ℃.
5.前述权利要求中任一项的弹性体,其中所述弹性体是部分不溶性的,并且通过本发明中所描述的萃取方法测定,在23℃和31℃下可溶级分的乙烯含量差5wt%或更小。 Elastomer according to any one of the preceding claims, wherein said elastomer is partially insoluble and method of the present invention by extraction as described in the determination, ethylene content 23 ℃ and 31 ℃ lower soluble fraction in the difference 5wt% or less.
6.前述权利要求中任一项的弹性体,其中所述弹性体具有65-95%的等规丙烯三单元组立构规整度,和/或所述弹性体具有6-8的m/r比,和/或所述弹性体具有40-55的全同立构规整度指数。 Elastomer according to any one of the preceding claims, wherein said elastomer has 65-95% of an isotactic propylene triad tacticity, and / or the elastomer has 6-8 m / r ratio, and / or the elastomer has an isotactic tacticity index of 40-55.
7.可硫化的组合物,其包含前述权利要求1-6中任一项的弹性体,和作为硫化包的化学交联配制物,不考虑这里所使用的聚合物或填料部分。 7. A curable composition comprising any of the preceding claims 1-6 one of the elastomer, and chemical crosslinking formulation as a curing package, not considered part of the polymer or filler material used herein.
8.权利要求7的可硫化组合物,其还包含分散在所述弹性体形成的基质中的分散相,该分散相包含DSC熔点为115℃或更高的结晶聚合物组分,优选熔化热为至少50J/g、优选至少75J/g的等规聚丙烯,该结晶聚合物组分选自下组:丙烯均聚物、丙烯接枝共聚物、丙烯嵌段共聚物、丙烯无规共聚物,和它们的混合物。 7 vulcanizable composition is preferably heat of fusion of claim 1, further comprising the elastomer dispersed in a matrix formed of a dispersed phase comprising a DSC melting point of 115 ℃ or higher crystallinity polymer component, of at least 50J / g, preferably at least 75J / g of isotactic polypropylene, the crystalline polymer component is selected from the group: propylene homopolymer, propylene graft copolymers, propylene block copolymers, propylene random copolymer , and mixtures thereof.
9.权利要求7或8的可硫化组合物,其还包含具有或不具有乙烯类型结晶性的聚合物,该聚合物优选包含至少50摩尔%的乙烯衍生的单元。 7 or vulcanizable composition of claim 8, further comprising a polymer having or not having an ethylene type crystallinity, the polymer preferably comprises at least 50 mole% of ethylene-derived units.
10.权利要求7-9中任一项的可硫化组合物,其还包含任选含有二烯的乙丙橡胶。 A curable composition according to any of claim 7-9, further comprising, optionally containing ethylene-propylene diene rubber.
11.权利要求7-10中任一项的可硫化组合物,其还包含1-100重量份无机填料/100份聚合物,其中所述无机填料选自下组:炭黑、粘土、氧化钛和氧化镁、硅石、玻璃纤维、云母和它们的混合物。 A curable composition according to any of claim 7-10, further comprising 1-100 parts by weight of an inorganic filler / 100 parts of polymer, wherein the inorganic filler is selected from the group: carbon black, clay, titanium oxide and magnesium oxide, silica, glass fiber, mica and mixtures thereof.
12.权利要求7-11中任一项的可硫化组合物,其还包含基于所述组合物总重量计少于30wt%、任选少于10wt%的增量油。 A curable composition according to any of claim 7-11, further comprising count less than 30wt% based on the total weight of the composition, optionally less than 10wt% of extender oil.
13.权利要求7-11中任一项的可硫化组合物,其不含增量油,或含有以所述组合物总重量计少于1wt%的增量油。 A curable composition according to any of claim 7-11, which does not contain extender oil, or containing the total weight of the composition is less than 1wt% of extender oil.
14.硫化的组合物,其中权利要求7-13中任一项所述的组合物被硫化至使得所述弹性体的粘度比为1-10,优选1.2-10的程度。 14. A cured composition, wherein any of claims 7-13, wherein the composition of claim one is vulcanized to the elastomeric body such that the viscosity ratio is 1 to 10, preferably from 1.2 to 10 of the degree.
15.硫化的组合物,其中权利要求7-14中任一项所述的组合物被硫化至如下程度:按照本文所描述的萃取方法测定,至少2wt%、优选至少10wt%、尤其是至少20wt%的弹性体被硫化,并且任选地少于95wt%的弹性体被硫化。 The composition of any one of claims 7-14 15. A cured composition, wherein the claim is vulcanized to the following extent: the extraction methods described herein in accordance with the determination of at least 2wt%, preferably at least 10wt%, especially at least 20wt % of the elastomer is cured and optionally less than 95wt% of the elastomer is vulcanized.
16.权利要求14或15的硫化的组合物,其中所述组合物在200%的伸长后的永久变形小于50%,和/或极限拉伸强度为至少1000psi(6.89MPa)。 14 or vulcanized composition of claim 15, wherein said composition is in permanent deformation after 200% elongation of less than 50%, and / or an ultimate tensile strength of at least 1000psi (6.89MPa).
17.权利要求14-16中任一项的硫化的组合物,该组合物具有符合以下关系式的以MPa度量的拉伸强度(TS):TS=30*(肖氏A硬度/MI(@190℃)-300+B1,其中B1为至少2。 14-16 The composition of any one of claim vulcanization, the composition has to meet the following relationship measure MPa tensile strength (TS): TS = 30 * (Shore A hardness / MI (@ 190 ℃) -300 + B1, wherein B1 is at least 2.
18.权利要求14-17中任一项的硫化的组合物,该组合物具有符合以下关系式的以MPa度量的拉伸强度(TS):TS=30*(肖氏A硬度/MI@190℃)-300+B1,其中B1为至少4,优选至少6,尤其至少12。 The composition according to any one of 14-17 vulcanization of claim, the composition has to meet the following relationship measure tensile strength MPa (TS): TS = 30 * (Shore A hardness / MI @ 190 ℃) -300 + B1, wherein B1 is at least 4, preferably at least 6, especially at least 12.
19.权利要求14-18中任一项的硫化的组合物,该组合物具有符合以下关系式的以Kn/m度量的口模C撕裂强度(口模C):口模C=40*(肖氏A硬度/MI@190℃)-400+B2,其中B2为至少5、优选至少10、尤其至少15、最优选至少20。 The composition of any one of 14-18 vulcanization of Claim, the composition has to meet the following relationship Kn / m measured die C tear strength (Die C): Die C = 40 * (Shore A hardness / MI @ 190 ℃) -400 + B2, wherein B2 is at least 5, preferably at least 10, especially at least 15, most preferably at least 20.
20.制造挤出制品的方法,所述方法包括:(a)挤出权利要求7-13中任一项所述的组合物,以产生挤出的制品,和(b)使所述挤出的制品暴露在硫化处理下,以提供具有权利要求14-19中任一项所述的组合物的挤出制品。 20. The extruded article, said method of manufacturing comprising: (a) the composition according to any one of 7-13 claims extrusion, to produce extruded products, and (b) such that the extrusion The article is exposed to the vulcanization treatment, in order to provide a composition of any of claims 14-19, wherein one of the extruded product.
21.按照权利要求20的方法生产的纤维或薄膜。 21. A method according to claim 20 of producing a fiber or film.
22.按照权利要求20的方法生产的无纺布。 22. A method according to claim 20 of producing a nonwoven fabric.
23.由权利要求14-19中任一项所述的组合物制备的模制物件。 Claim 23. The molded article by composition according to any one of prepared 14-19.
24.制备挤出制品的方法,该方法包括:(a)挤出包含弹性体的组合物以产生挤出的制品,所述弹性体具有等规聚丙烯结晶性,110℃或更低的DSC熔点,和5至50J/g的熔化热,并且包含:(i)丙烯衍生的单元,其量为至少60wt%,优选在80-97wt%的范围内,更优选在80-90wt%的范围内,基于组分(i)、(ii)和(iii)的总重量计;(ii)乙烯衍生的单元,其量为至少6wt%,优选在10-20wt%的范围内,基于组分(i)、(ii)和(iii)的总重量计;和(iii)任选的二烯衍生的单元,其量在0.1-10wt%的范围内,优选在0.3-10wt%的范围内,更优选在0.3-3wt%的范围内,基于组分(i)、(ii)和(iii)的总重量计;和(b)将所述挤出的制品暴露在辐射下,以至少部分硫化所述挤出的制品。 24. A method for preparing extruded article, the method comprising: (a) extruding a composition comprising an elastomer to produce extruded article, said elastomer having isotactic polypropylene crystallinity, 110 ℃ or lower DSC melting point, and from 5 to 50J / g heat of fusion, and comprising: (i) propylene-derived units in an amount of at least 60wt%, preferably in the range of 80-97wt%, more preferably in the range of 80-90wt% of , based on component (i), (ii) and (iii) the total weight; (ii) ethylene-derived units in an amount of at least 6wt%, preferably in the range of 10-20wt%, based on component (i ), (ii) and (iii) the total weight; diene derived units and (iii) optionally, an amount in the range 0.1-10wt%, preferably in the range 0.3-10wt%, more preferably in the range of 0.3-3wt%, based on component (i), (ii) and (iii) the total weight; and (b) exposing the extruded article to radiation to at least partially cure said extruded article.
25.权利要求24的方法,其中所述弹性体具有0.5至100,优选5-40的门尼粘度ML(1+4)@125℃。 25. The method of claim 24, wherein said elastomer has from 0.5 to 100, preferably 5 to 40 Mooney viscosity ML (1 + 4) @ 125 ℃.
26.权利要求24或25的方法,其中所述弹性体是部分不溶性的,并且通过本文中所描述的萃取方法测定,在23℃和31℃下可溶级分的乙烯含量差别小于5wt%,优选小于2wt%。 26. The method of claim 24 or claim 25, wherein said elastomer is partially insoluble and extraction by the methods described herein determined, the ethylene content difference at 23 ℃ and 31 ℃ in the soluble fraction of less than 5wt%, preferably less than 2wt%.
27.前述权利要求24-26中任一项的方法,其中所述弹性体具有65-95%的等规丙烯三单元组立构规整度,和/或所述弹性体具有6-8的m/r比,和/或所述弹性体具有40-55的全同立构规整度指数。 The method according to any one of the preceding claims 24-26 27., wherein said elastomer has 65-95% of an isotactic propylene triad tacticity, and / or the elastomer has 6-8 m / r ratio, and / or the elastomer has an isotactic tacticity index of 40-55.
28.前述权利要求24-27中任一项的方法,其中所述组合物还包含分散在所述弹性体形成的基质中的分散相,该分散相包含DSC熔点为115℃或更高的结晶聚合物组分,优选熔化热为至少50J/g、优选至少75J/g的等规聚丙烯,该结晶聚合物组分选自下组:丙烯均聚物、丙烯接枝共聚物、丙烯嵌段共聚物、丙烯无规共聚物,和它们的混合物。 The method according to any one of the preceding claims 24-27 28., wherein the composition further comprises an elastomer dispersed in a matrix formed in the dispersed phase, the dispersed phase comprising a DSC melting point or a higher crystallinity 115 ℃ polymer component, preferably a heat of fusion of at least 50J / g, preferably at least 75J / g of isotactic polypropylene, the crystalline polymer component is selected from the group consisting of: propylene homopolymer, propylene graft copolymers, propylene block copolymers, propylene random copolymers, and mixtures thereof.
29.前述权利要求24-28中任一项的方法,其中所述组合物还包含具有或不具有乙烯类型结晶性的聚合物,该聚合物优选包含至少50摩尔%的乙烯衍生的单元。 The method according to any one of the preceding claims 24-28 29., wherein the composition further comprises a unit that may have a crystallinity of ethylene type polymer, the polymer preferably comprises at least 50 mole% of ethylene-derived.
30.前述权利要求24-29中任一项的方法,其中所述组合物还包含任选含有二烯的乙丙橡胶。 The method according to any one of the preceding claims 24-29 30., wherein the composition further comprises optionally containing ethylene-propylene diene rubber.
31.前述权利要求24-30中任一项的方法,其中所述组合物还包含1-100重量份的无机填料/100份聚合物,其中所述无机填料可以是炭黑、粘土、氧化钛和氧化镁、硅石、玻璃纤维、云母或它们的混合物。 The method according to any one of the preceding claims 24-30 31., wherein the composition further comprises 1-100 parts by weight of an inorganic filler / 100 parts of polymer, wherein the inorganic filler may be carbon black, clay, titanium oxide and magnesium oxide, silica, glass fiber, mica or mixtures thereof.
32.权利要求24-31中任一项的方法,其中所述组合物还包含基于所述组合物总重量计少于30wt%、任选少于10wt%的增量油。 The method of any one of claims 24-31 32., wherein the composition further comprises less than 30wt% based on the count of the total composition weight, optionally less than 10wt% of extender oil.
33.权利要求24-31中任一项的方法,其中所述组合物不含增量油,或包含基于所述组合物总重量计少于1wt%的增量油。 The method of any one of claims 24-31 33., wherein the composition is free of extender oil, or comprising, based on the total weight of the composition is less than 1wt% of extender oil.
34.权利要求24-33中任一项的方法,其中所述组合物还包含作为硫化包的化学交联配制物,不考虑这里所使用的聚合物或填料部分。 The method of any one of claims 24-33 34., wherein the composition further comprises a chemical crosslinking formulation as a curing package, not considered part of the polymer or filler material used herein.
35.权利要求24-34中任一项的方法,其中所述组合物被硫化至所述弹性体的粘度比为1-10,优选1.2-10的程度。 The method of any one of claims 24-34 35., wherein the composition is cured to a viscosity ratio of the elastomer is 1-10, preferably 1.2-10 degree of.
36.权利要求24-35中任一项的方法,其中所述组合物被硫化至如下程度:按照本文所描述的萃取方法测定,至少2wt%、优选至少10wt%、尤其是至少20wt%的弹性体被硫化,并且任选地少于95wt%的弹性体被硫化。 Especially at least 20wt% of the elastic determined according to the extraction method described herein, at least 2wt%, preferably at least 10wt%,: one of 36. The method of any of claim 24-35, wherein said composition is cured to an extent body is cured and optionally less than 95wt% of the elastomer is vulcanized.
37.权利要求24-36中任一项的方法,其中所述挤出制品在200%的伸长后的永久变形小于50%,和/或极限拉伸强度为至少1000psi(6.89MPa)。 The method of any one of claims 24-36 37., wherein said permanent deformation in the extruded article after 200% elongation of less than 50%, and / or an ultimate tensile strength of at least 1000psi (6.89MPa).
38.权利要求24-37中任一项的方法,其中所述挤出制品具有符合以下关系式的以MPa度量的拉伸强度(TS):TS=30*(肖氏A硬度/MI@190℃)-300+B1,其中B1为至少2。 The method of any one of claims 24-37 38., wherein the extruded article has to meet the following relationship measure tensile strength MPa (TS): TS = 30 * (Shore A hardness / MI @ 190 ℃) -300 + B1, wherein B1 is at least 2.
39.权利要求24-37中任一项的方法,其中所述挤出制品具有符合以下关系式的以MPa度量的拉伸强度(TS):TS=30*(肖氏A硬度/MI@190℃)-300+B1,其中B1为至少4,优选至少6,尤其是至少12。 The method of any one of claims 24-37 39., wherein the extruded article has to meet the following relationship measure tensile strength MPa (TS): TS = 30 * (Shore A hardness / MI @ 190 ℃) -300 + B1, wherein B1 is at least 4, preferably at least 6, especially at least 12.
40.权利要求24-39中任一项的方法,其中所述挤出制品具有符合以下关系式的以Kn/m度量的口模C撕裂强度(口模C):口模C=40*(肖氏A硬度/MI@190℃)-400+B2,其中B2为至少5、优选至少10、尤其是至少15、最优选至少20。 The method of any one of claims 24-39 40., wherein the extruded article has to meet the following relationship Kn / m measured die C tear strength (Die C): Die C = 40 * (Shore A hardness / MI @ 190 ℃) -400 + B2, wherein B2 is at least 5, preferably at least 10, especially at least 15, most preferably at least 20.
41.按照前述权利要求24-40中任一项所述的方法制备的纤维。 41. The method according to any preceding claim fiber according to any one of claims 24-40 prepared.
42.按照前述权利要求24-40中任一项所述的方法制备的无纺布。 42. The method according to any preceding claim nonwoven fabric according to any one of claims 24-40 prepared.
43.按照前述权利要求24-40中任一项所述的方法制备的薄膜。 43. The method according to the preceding claims film according to any one of claims 24-40 prepared.
Description  translated from Chinese
基于丙烯的弹性体及其用途 Propylene-based elastomer and use thereof

技术领域 FIELD

[0001]本发明总体上涉及弹性体组合物,该组合物具有等规聚丙烯结晶性,等于或低于110℃的通过DSC测定的熔点,5J/g至50J/g的熔化热,并且包含至少60wt%的丙烯衍生的单元,至少6wt%的乙烯衍生的单元和任选的二烯衍生的单元。 Relates to elastomeric compositions [0001] The present invention generally, the composition has a crystalline isotactic polypropylene, is equal to or lower than 110 ℃ melting point measured by DSC, 5J / g to 50J / g heat of fusion, and comprises at least 60wt% of propylene-derived units, units and diene derived units of at least 6wt% ethylene-derived optional. 本发明的实施方案包括可硫化的和硫化的弹性体组合物,以及这种组合物在诸如纤维、薄膜、非织造片材和模制物件之类的应用中的用途。 Embodiments of the present invention comprises a vulcanizable and vulcanized elastomer compositions, and such compositions in applications such as the class of fibers, films, nonwoven sheet and the molded article in use.

背景技术 BACKGROUND

[0002]无定型的和部分结晶的(通常称为半结晶的)聚合物可以提供例如ASTM D1566中所定义的弹性体性质。 [0002] (commonly referred to as semi-crystalline) polymer may provide, for example elastomeric properties as defined in ASTM D1566 amorphous and partially crystalline. 一类重要的弹性体衍生自聚烯烃,通常使用采用齐格勒-纳塔型催化剂体系的加成聚合。 An important class of elastomers derived from polyolefins, generally used Ziegler - Natta addition polymerization catalyst system. 通常,聚烯烃弹性体是乙烯、提供短支链的破坏结晶性的α-烯烃如丙烯及任选地小量的多烯如二烯的共聚体,所述多烯用于提供可用于提供不同链之间的交联的不饱和短支链。 Typically, the polyolefin elastomer is ethylene, to provide short chain branches destruction crystalline α- olefins such as propylene and, optionally, a small amount of polyene such as diene interpolymer, the polyene may be used to provide different for providing crosslinked unsaturated short-branched chains. 这些共聚体可以是不含二烯衍生的单元的乙烯-丙烯共聚物(EP),或乙烯-丙烯-二烯三元共聚物(EPDM)。 These interpolymers can be free of diene-derived units of ethylene - propylene copolymer (EP), or ethylene - propylene - diene terpolymers (EPDM).

[0003]存在不同的技术用于硫化EP和EPDM共聚体。 [0003] There are different techniques for vulcanization EP and EPDM copolymers. 硫化可以逐渐地进行,从最初的产生长链分枝(其中大分子单体或聚合物链本身插入到已经形成的聚合物链中),到中间形式(其中硫化的聚合物部分是可溶的和部分是不可溶的),再到全硫化的形式(其中聚合物的整体是不可溶的,并且全部聚合物链都连接到网络中,没有孤立的聚合物链残留下来可供单独萃取)。 Curing can be carried out gradually, from the initial generation of long chain branching (wherein macromer or polymer chain itself is inserted into the polymer chain has formed), the intermediate form (which is part of the polymer soluble sulfurized and is insoluble portion), and then to form a full-vulcanized (wherein the polymer as a whole is insoluble, and all of the polymer chains are connected to the network, there is no isolation of the polymer chains are left behind for a separate extraction).

[0004]本领域的技术人员选择所述共聚体、硫化/交联体系及其它配制成分,以平衡最终产品的可加工性和物理性能,例如老化、硬度、延展性(extensibility)、压缩永久变形、拉伸强度及冷的时候的性能。 [0004] Those skilled in the art to select the interpolymer, vulcanization / cross-linking system and other formulation ingredients, in order to balance the processability and physical properties of the final product, such as aging, hardness, ductility (extensibility), compression set tensile strength and performance when cold.

[0005]EP 964641、EP 946640、EP 1003814、USP 6,245,856及USP 6,525,157及其它专利公开了聚烯烃共聚体,它们是弹性体,并且具有由聚合物链中等规排列的丙烯衍生序列形成的结晶性。 [0005] EP 964641, EP 946640, EP 1003814, USP 6,245,856 and USP 6,525,157 and other patents disclose a polyolefin copolymer which is an elastomer, a polymer chain and having a propylene-derived medium-gauge arranged sequence is formed of crystallinity. 这与目前商业应用中的结晶性源自乙烯衍生的序列的EP和EPDM共聚体相反。 This is the current commercial applications crystalline ethylene-derived opposite from EP and EPDM interpolymers sequence. 这类基于丙烯的弹性体的性质在很多方面不同于已知的EP和EPDM共聚体弹性体。 Such propylene based elastomeric properties different from the known EP and EPDM elastomeric copolymers in many aspects. 二烯在这些新的基于丙烯的弹性体中的应用已经被想到。 Diene in these new propylene-based elastomer application has been thought of. 参见例如WO 00/69964,包括第15页18至25行。 See, for example WO 00/69964, including page 15 lines 18-25.

发明概述 Summary of the Invention

[0006]在一个方面,本发明提供了基于丙烯的弹性体,其被硫化至不同程度以进一步扩大所述弹性体的弹性体性能范围并允许进行方便的加工。 [0006] In one aspect, the present invention provides a propylene-based elastomer which is cured to different degrees in order to further expand the range of elastomeric properties of the elastic body and allow for easy processing.

[0007]在另一个方面,所述改进的基于丙烯的弹性体包括二烯,以有利于硫化和在复配及加工的各种选择中的最佳的最终应用性能。 [0007] In another aspect, the modified propylene-based elastomer comprises a diene, to facilitate the compounding and vulcanization and processing of various options in the best performance of the final application.

[0008]在另一个方面,本发明提供了改进的复配物,其含有这种基于丙烯的弹性体,以提供使用EP和EPDM共聚体弹性体所不能够实现的外观及最终应用性能特性。 [0008] In another aspect, the present invention provides an improved compound thereof, comprising such propylene-based elastomer to provide the appearance and performance characteristics of the final application using the EP and EPDM interpolymers resilient body can not be achieved.

[0009]在一个实施方案中,本发明提供了一种弹性体,其包括丙烯衍生的单元、乙烯衍生的单元和二烯衍生的单元,并且具有等规聚丙烯的结晶性,等于或低于110℃的通过DSC测定的熔点,和5J/g至50J/g的熔化热。 [0009] In one embodiment, the present invention provides an elastomer comprising a propylene-derived units, units and diene derived units derived from ethylene, and having a crystalline isotactic polypropylene, etc., is equal to or lower than melting point measured by DSC of 110 ℃, and 5J / g to 50J / g heat of fusion. 所述丙烯衍生的单元以至少60wt%的量存在,基于衍生自丙烯、二烯和乙烯的单元的总重量计。 In the propylene-derived units present in an amount of at least 60wt%, based on units derived from propylene, ethylene and diene units on the total weight. 所述乙烯衍生的单元以至少6wt%的量存在,基于衍生自丙烯、二烯和乙烯的单元的总重量计。 The ethylene-derived units in an amount of at least 6wt%, based on units derived from propylene, ethylene and diene units on the total weight. 所述二烯衍生的单元以0.3-10wt%的量存在,基于衍生自丙烯、二烯和乙烯的单元的总重量计。 The diene-derived units present in an amount in 0.3-10wt%, based on units derived from propylene, and ethylene diene units on the total weight.

[0010]在另一个实施方案中,本发明提供了一种包含这里所描述的基于丙烯的弹性体和硫化包(curing package)的可硫化组合物。 [0010] In another embodiment, the present invention provides a pharmaceutical composition comprising described herein propylene-based elastomer and a vulcanizing package (curing package) of the vulcanizable composition.

[0011]在另一个实施方案中,本发明提供了一种硫化的组合物,其中这里所描述的可硫化组合物被硫化至使弹性体的粘度比为1至10的程度。 [0011] In another embodiment, the present invention provides a cured composition, wherein the vulcanizable composition described herein is vulcanized to the viscosity of the elastomer ratio of 1 to 10 degrees.

[0012]在另一个实施方案中,本发明提供了一种硫化的组合物,其中这里所描述的可硫化组合物被硫化至使至少2wt%的弹性体被硫化的程度,所述硫化程度通过这里所描述的萃取方法确定。 [0012] In another embodiment, the present invention provides a cured composition, wherein the vulcanizable composition described herein is vulcanized to the extent so that at least 2wt% of the elastomer is vulcanized, the degree of cure by extraction methods described herein determined.

[0013]在另一个实施方案中,本发明提供了一种制造挤出制品的方法,该方法包括挤出这里所描述的可硫化组合物以生产挤出的制品,和使所述挤出的制品暴露于硫化处理如化学交联或辐射,以提供具有如这里所描述的硫化组合物组成的挤出制品。 [0013] In another embodiment, the present invention provides a method of manufacturing an extruded article, the method comprising extruding the vulcanizable composition described herein in the production of extruded articles, and so that the extruded article is exposed to the vulcanization treatment such as chemical or radiation cross-linking, such as to provide a cured extruded article having a composition described herein thereof.

[0014]在另一个实施方案中,本发明提供了包含这里所描述的任何本发明组合物的薄膜、纤维、非织造片材、模制物件或挤出成型物。 [0014] In another embodiment, the present invention provides a film comprising any of the herein described compositions of the present invention, the fibers, nonwoven sheet, molded article or extrusion molded.

详细描述基于丙烯的弹性体 Detailed description of the propylene-based elastomer

[0015]本发明的基于丙烯的弹性体是无规的丙烯均聚物,或具有被非结晶区干扰的结晶区的共聚物。 Propylene-based elastomer is a random propylene [0015] The present invention is a homopolymer or copolymer of a non-crystalline regions is disturbed crystalline region having. 所述非结晶区可以源自不可结晶的聚丙烯链段的区域和/或包含共聚单体单元。 Region of the amorphous region may be derived from non-crystalline polypropylene segments and / or containing comonomer units. 通过引入丙烯插入错误和/或通过存在共聚单体,所述基于丙烯的弹性体的结晶度和熔点与高等规的聚丙烯相比被降低。 Compared propylene insertions is reduced by the introduction of errors and / by the presence of comonomer, the propylene-based elastomer of crystallinity and melting point and highly isotactic polypropylene or.

[0016]所述基于丙烯的弹性体的结晶度可以以熔化热表示。 [0016] Based on the degree of crystallinity of the propylene elastomer can be expressed as the heat of fusion. 在特别的实施方案中,所述基于丙烯的弹性体具有在下限为1.0J/g、或1.5J/g、或3.0J/g、或4.0J/g、或6.0J/g、或7.0J/g,上限为30J/g、或40J/g、或50J/g、或60J/g、或75J/g的范围内的由DSC测定的熔化热。 In a particular embodiment, the propylene-based elastomer having a lower limit of 1.0J / g, or 1.5J / g, or 3.0J / g, or 4.0J / g, or 6.0J / g, or 7.0J / g, an upper limit of 30J / g, or 40J / g, or 50J / g, or 60J / g, or 75J / heat of fusion measured by DSC within the range g.

[0017]所述基于丙烯的弹性体的结晶度也可以用结晶度百分数表示。 [0017] The crystallinity of the propylene elastomer can be expressed in percentage of crystallinity. 最高等级的聚丙烯的热能据估计为189J/g,即100%结晶度等于189J/g。 It is estimated that the highest level of thermal energy of polypropylene is 189J / g, i.e., 100% crystallinity is equal to 189J / g. 因此,在特别的实施方案中,所述基于丙烯的弹性体具有在上限为65%、或40%、或30%、或25%、或20%,下限为1%、或3%、或5%、或7%、或8%的范围内的丙烯结晶度。 Thus, in particular embodiments, the propylene-based elastomer has an upper limit of 65%, or 40%, or 30%, or 25%, or 20%, the lower limit is 1%, or 3%, or 5 %, or 7%, or propylene crystallinity in the range of 8%.

[0018]结晶度的水平还反映在熔点上。 [0018] The level of crystallinity is also reflected in the melting point. 这里所用的术语“熔点”是通过DSC测定的、主熔融峰和次熔融峰中的最高峰。 As used herein, the term "melting point" is measured by DSC, the main melting peak and a secondary peak of the melting peak. 在特别的实施方案中,所述基于丙烯的弹性体的由DSC测定的熔点在上限为110℃、或105℃、或90℃、或80℃、或70℃,下限为0℃、或20℃、或25℃、或30℃、或35℃、或40℃、或45℃的范围内。 In a particular embodiment, the melting point measured by DSC of the propylene-based elastomer in the upper limit is 110 ℃, or 105 ℃, or 90 ℃, or 80 ℃, or 70 ℃, the lower limit is 0 ℃, or 20 ℃ within the range or 25 ℃, or 30 ℃, or 35 ℃, or 40 ℃, or 45 ℃ for.

[0019]所述基于丙烯的弹性体通常包含至少60wt%的丙烯衍生的单元,并且在特别的实施方案中,所述基于丙烯的弹性体包含至少75wt%、或至少80wt%、或至少90wt%的丙烯衍生的单元。 [0019] The propylene-based elastomers typically contain at least 60wt% of propylene-derived units, and in particular embodiments, the propylene-based elastomer comprises at least 75wt%, or at least 80wt%, or at least 90wt% of propylene-derived units.

[0020]适合于本发明的基于丙烯的弹性体的等规丙烯三单元组立构规整度在下限为65%、或70%、或75%,上限为95%、或97%、或98%、或99%的范围内。 [0020] Suitable propylene-based elastomer isotactic propylene triad tacticity of the present invention is configured in a lower limit of 65%, or 70%, or 75% and up to 95%, or 97%, or 98% , or in the range of 99%. 聚合物的等规丙烯三单元组立构规整度是由头-尾键组成、表示为m和r序列的二元组合的三个相邻丙烯单元序列即链的相对立构规整度。 Isotactic propylene triad tacticity of the polymer is from head - tail bonds, expressed in three binary combination of m and r sequences adjacent relative tacticity of the propylene unit sequences i.e. chain. 这里所公开的聚合物的等规丙烯三单元组立构规整度使用C13NMR和在USP 5,504,172中阐述的计算方法测定。 Isotactic propylene triad tacticity of the polymer disclosed herein, and measured using C13NMR calculation method set forth in USP 5,504,172.

[0021]本发明的基于丙烯的弹性体的全同立构规整度指数大于0%,或者在上限为50%或25%,下限为3%或10%的范围内。 [0021] The present invention is based on isotactic tacticity index of the elastomer is greater than 0% of propylene, or in the upper limit is 50% or 25%, the lower limit is 3% or 10% of the range.

[0022]本发明的基于丙烯的弹性体的立构规整度指数(m/r)在上限为8、或10、或12,下限为4或6的范围内。 [0022] The present invention is based on tacticity index of the propylene elastomer (m / r) at the upper limit of 8, or 10, or 12, a lower limit of a range of 4 or 6.

[0023]在某些实施方案中,通过使丙烯与有限量的一种或多种选自乙烯、C4-C20α-烯烃及多烯的共聚单体共聚合来降低所述基于丙烯的弹性体的结晶度。 [0023] In certain embodiments, by reacting propylene with limited amounts of one or more selected from ethylene, C4-C20α- -olefin and polyene comonomer copolymerization to reduce the propylene-based elastomer crystallinity. 在这些共聚物中,以所述基于丙烯的弹性体的总重量计,在所述基于丙烯的弹性体中存在的丙烯衍生单元的量上限为99.9wt%、或97wt%、或95wt%、或94wt%、或92wt%、或90wt%、或85wt%,下限为60wt%、68wt%、或70wt%、或71wt%、或75wt%、或76wt%或80wt%。 In these copolymers, based on the total weight of the propylene-based elastomer, the upper limit on the amount of the propylene-based elastomer in the presence of propylene-derived units is 99.9wt%, or 97wt%, or 95wt%, or 94wt%, or 92wt%, or 90wt%, or 85wt%, the lower limit is 60wt%, 68wt%, or 70wt%, or 71wt%, or 75wt%, or 76wt% or 80wt%. 以所述基于丙烯的弹性体的总重量计,所述基于丙烯的弹性体中存在的衍生自乙烯和/或C4-C20α-烯烃的任选单元的量上限为40wt%、或35wt%、或30wt%、或28wt%、或25wt%、或20wt%、或15wt%,下限为0wt%、或0.5wt%、或1wt%、或2wt%、或3wt%、或5wt%、或6wt%、或8wt%或10wt%。 In the elastomer based on the total weight of the propylene, the propylene-based elastomer is present in an amount derived from the upper limit of ethylene and / or C4-C20α- optionally olefin units is 40wt%, or 35wt%, or 30wt%, or 28wt%, or 25wt%, or 20wt%, or 15wt%, the lower limit is 0wt%, or 0.5wt%, or 1wt%, or 2wt%, or 3wt%, or 5wt%, or 6wt%, or 8wt% or 10wt%. 以所述基于丙烯的弹性体的总重量计,所述基于丙烯的弹性体中存在的任选的多烯衍生单元的量上限为25wt%、或20wt%、或15wt%、或10wt%、或7wt%、或5wt%、或4.5wt%、或3wt%、或2.5wt%,下限为0wt%、或0.1wt%、或0.2wt%、或0.3wt%、或0.5wt%、或1wt%、或1.5wt%。 In the elastomer based on the total weight of propylene, based on the upper limit of the amount of elastomeric propylene optionally in the presence of the polyene derived units is 25wt%, or 20wt%, or 15wt%, or 10wt%, or 7wt%, or 5wt%, or 4.5wt%, or 3wt%, or 2.5wt%, the lower limit is 0wt%, or 0.1wt%, or 0.2wt%, or 0.3wt%, or 0.5wt%, or 1wt%, or 1.5wt%.

[0024]任选存在于所述基于丙烯的弹性体中的优选α-烯烃的非限制性实例包括丙烯、1-丁烯、1-戊烯、1-己烯、1-辛烯和1-癸烯。 [0024] optionally present in the non-limiting examples based on the propylene elastomer is preferably α- olefins include propylene, 1-butene, 1-pentene, 1-hexene, 1-octene and 1- decene. 任选存在于所述基于丙烯的弹性体中的多烯衍生单元可以衍生自具有至少两个不饱和键的任何烃结构,其中至少一个不饱和键可以被引入聚合物中。 Optionally present in the propylene-based elastomer of polyene derived units may be derived from having at least two unsaturated bonds any hydrocarbon structure, wherein the at least one unsaturated bond may be introduced into the polymer. 优选的多烯的非限制性实例包括5-乙叉-2-降冰片烯(″ENB″)、5-乙烯基-2-降冰片烯(″VNB ″)、二乙烯基苯(″DVB ″)以及双环戊二烯(″DCPD ″)。 Preferred polyene Non-limiting examples include 5-ethylidene-2-norbornene ("ENB"), 5- vinyl-2-norbornene ("VNB"), divinyl benzene ("DVB" ) and dicyclopentadiene ("DCPD").

[0025]在一个特别的实施方案中,所述基于丙烯的弹性体的在125℃的门尼粘度ML(1+4)为0.5至100、或5至40、或10至40。 [0025] In a particular embodiment, the propylene-based elastomer at 125 ℃ Mooney viscosity ML (1 + 4) of from 0.5 to 100, or 5-40, or 10-40.

[0026]本发明的基于丙烯的弹性体的重均分子量(Mw)在上限为5,000,000g/mol、或1,000,000g/mol、或500,000g/mol,下限为10,000g/mol、或15,000g/mol、或20,000g/mol、或80,000g/mol的范围内,并且有时被称为“多分散指数”(PDI)的分子量分布Mw/Mn(MWD)在上限为40、或20、或10、或5、或4.5、或4.0、或3.2、或3.0,下限为1.5、或1.8、或2.0的范围内。 [0026] The present invention is based on the weight of the propylene elastomer-average molecular weight (Mw) upper limit of 5,000,000g / mol, or 1,000,000g / mol, or 500,000g / mol, a lower limit of 10,000g / mol, or 15,000g / mol , or in the range of 20,000g / mol, or 80,000g / mol, and is sometimes referred to as "polydispersity index" (PDI) of a molecular weight distribution Mw / Mn (MWD) at the upper limit of 40, or 20, or 10, or 5, or 4.5, or 4.0, or 3.2, or 3.0, the lower limit of 1.5, or 1.8, or in the range of 2.0.

[0027]合适的基于丙烯的弹性体以及用于制备它们的方法的示例性非限制实例包括:在未决的美国临时专利申请号60/519,975中所公开的″FPC″;在美国专利申请公布号2003/0204017中所公开的″等规的丙烯共聚物″;在USP 6,525,157中所公开的″丙烯乙烯共聚物″;以及在PCT公布号WO 02/083754中所公开的″丙烯乙烯共聚物″,其公开内容通过引用全部结合在此。 [0027] Suitable elastomeric propylene and an exemplary method for their preparation is based on non-limiting examples include: U.S. Provisional Patent Application No. 60 pending / 519,975 disclosed "FPC"; published in U.S. Patent Application No. 2003/0204017 disclosed "isotactic propylene copolymer"; in USP 6,525,157 disclosed "propylene ethylene copolymer"; and in PCT Publication No. WO 02/083754 disclosed "propylene ethylene copolymer" , the disclosure of which is incorporated herein by reference in its entirety.

[0028]与前述分开地或相组合地,所述基于丙烯的弹性体的结晶度也可以通过立体不规则地引入丙烯衍生的单元来降低,这可能被例如催化剂和聚合温度的选择所影响。 [0028] The aforementioned separately or in combination, the crystallinity of the propylene elastomer can also be introduced irregularly propylene-derived units to reduce by three-dimensional, which may be for example the choice of catalyst and the polymerization temperature affected.

[0029]本发明的基于丙烯的弹性体不受任何具体的制备聚合方法限制,并且这里所描述的聚合方法不受任何具体的反应容器类型限制。 [0029] The present invention is a propylene-based elastomer is not any particular polymerization method for preparing limit, and the polymerization methods described herein without any specific type of reaction vessel limits.

[0030]在一个特别的实施方案中,用于生产基于丙烯的弹性体的催化剂体系包括一种或多种过渡金属化合物及一种或多种活化剂。 [0030] In a particular embodiment, the catalyst system for the production of elastomers based on propylene comprising one or more transition metal compounds and one or more activators. 当使用铝氧烷或烷基铝活化剂时,结合的前催化剂-活化剂摩尔比通常为1∶5000至10∶1。 When alumoxane or aluminum alkyl activators, bound catalyst precursor - activator molar ratio is usually 1:5000 to 10:1. 当使用离子化活化剂时,结合的前催化剂-活化剂摩尔比通常为10∶1至1∶10。 When using ionizing activators, bound catalyst precursor - activator molar ratio is usually 10:1 to 1:10. 可以使用多重活化剂,包括使用铝氧烷或烷基铝与离子化活化剂的混合物。 Multiple activators may be used, including the use of alkyl alumoxane or a mixture of aluminum and ionizing activators.

[0031]在另一个特别的实施方案中,所述催化剂体系包括双(环戊二烯基)金属化合物,和(1)非配位的相容的阴离子活化剂,或(2)铝氧烷活化剂。 [0031] In another particular embodiment, the catalyst system comprises a bis (cyclopentadienyl) metal compound, and (1) a non-coordinating compatible anion activator, or (2) an aluminoxane activator. 可以使用的催化剂体系的非限制性实例描述在USP5,198,401和5,391,629中,通过引用将其结合在此。 Non-limiting examples of catalyst system can be used are described in USP5,198,401 and 5,391,629, and which is incorporated by reference herein.

[0032]在另一个实施方案中,所述基于丙烯的弹性体是在活化助催化剂存在下制得的,该助催化剂是包含卤化的四芳基取代的第13族阴离子的母体离子化合物,其中每个芳基取代基含至少两个环芳环。 [0032] In another embodiment, the propylene-based elastomer in the presence of activating co-catalyst, the cocatalyst is a precursor ionic compound comprising a halogenated tetraaryl-substituted Group 13 anion wherein each aryl substituent contains at least two aromatic rings. 在该实施方案的一个具体方面,所述基于丙烯的弹性体含有大于0.2ppm、或大于0.5ppm、或大于1ppm、或大于5ppm的所述活化助催化剂的残余物。 In a particular aspect of this embodiment, the propylene-based elastomer comprises greater than 0.2ppm, or greater than 0.5ppm, or greater than 1ppm, or greater than the activating cocatalyst residue of 5ppm.

[0033]在另一个特别的实施方案中,用于生产基于丙烯的弹性体的催化剂体系包括含Hf的茂金属催化剂,例如但不限于二甲基二甲基甲硅烷基双(茚基)合铪,和非配位阴离子活化剂,例如但不限于二甲基苯铵四(七氟萘基)硼酸盐。 [0033] In another particular embodiment, the catalyst system for the production of elastomers based on propylene containing Hf metallocene catalysts include, for example, but not limited to, di methyl dimethylsilyl bis (indenyl) hafnium, and non-coordinating anion activator, such as, but not limited to, dimethylanilinium tetrakis (heptafluoronaphthyl) borate.

[0034]在又一个特别的实施方案中,使用在美国专利申请公布2004/0024146中所公开的任何催化剂体系及聚合方法制备所述基于丙烯的弹性体,该文件公开的内容通过引用结合在此。 [0034] In yet another particular embodiment, using any in U.S. Patent Application Publication 2004/0024146 catalyst system and polymerization process as disclosed for preparing the propylene-based elastomer, the disclosure of which document is incorporated herein by reference .

[0035]在另一个特别的实施方案中,使用催化剂体系,例如在美国专利申请公布2003/0204017中描述的非茂金属的、金属中心的、杂芳基配体的催化剂体系之一来制备所述基于丙烯的弹性体,该文件公开的内容通过引用结合在此。 [0035] In another particular embodiment, the catalyst system used, e.g., be prepared as reported by the non-metallocene catalyst systems, metal-centered 2003/0204017 described, heteroaryl ligand in U.S. Patent Application said propylene-based elastomer, the disclosure of which document is incorporated herein by reference.

[0036]适合用于制备所述基于丙烯的弹性体的其它一般工艺条件信息可以在包括但不限于USP 5,001,205及PCT公布WO 96/33227和WO 97/22639的公开内容中找到。 [0036] Suitable for the preparation of the general process conditions based on other information propylene elastomers may include, but are not limited to, USP 5,001,205 and PCT Publication WO 96/33227 and WO 97/22639 the disclosures found in. 关于气相聚合工艺的进一步的信息可以在包括但不限于以下的公开内容中找到:USP 4,543,399;4,588,790;5,028,670;5,317,036;5,352,749;5,405,922;5,436,304;5,453,471;5,462,999;5,616,661;5,627,242;5,665,818;5,668,228和5,677,375,以及欧洲公布EP-A-0 794 200;EP-A-0 802 202;及EP-B-634 421。 Further information about the gas-phase polymerization process may include, but are not limited to, the following disclosures found: USP 4,543,399; 4,588,790; 5,028,670; 5,317,036; 5,352,749; 5,405,922; 5,436,304; 5,453,471; 5,462,999; 5,616,661; 5,627,242; 5,665,818; 5,668,228 and 5,677,375, and European publications EP-A-0 794 200; EP-A-0 802 202; and EP-B-634 421. 涉及将液体催化剂引入到流化床聚合中贫粒子区(particle lean zone)中的方法的信息可在包括但不限于USP 5,693,727的公开内容中找到。 Relates to a liquid catalyst is introduced into the particle lean zone in a fluidized bed polymerization (particle lean zone) of the method of information may include, but are not limited to, USP 5,693,727 the disclosure of which is found in. 关于淤浆聚合工艺的进一步的信息可以在包括但不限于USP 3,248,179和4,613,484的公开内容中找到。 Further information about the slurry polymerization process may include, but are not limited to the disclosure of USP 3,248,179 and 4,613,484 are found in. PCT公布WO 96/08520及USP 5,712,352是描述在不存在或基本不存在任何清除剂下操作的聚合方法的公开内容的非限制性实例。 PCT Publication WO 96/08520 and USP 5,712,352 is described in the absence or substantial absence of a polymerization method of the disclosure in any scavenger operation of non-limiting examples.

结晶聚合物组分 Crystalline polymer component

[0037]本发明的一些实施方案包括结晶的丙烯聚合物组分。 Some embodiments of the [0037] present invention comprises a crystalline propylene polymer component. 所述结晶聚合物组分可以选自:丙烯均聚物、丙烯共聚物及通常被称为反应器共聚物或抗冲共聚物的其混合物。 The crystalline polymer component may be selected from: propylene homopolymers, propylene copolymers, and commonly referred to a reactor copolymer or an impact copolymer of a mixture thereof. 在其中结晶聚合物组分包括丙烯共聚物的实施方案中,所述丙烯共聚物可以是接枝共聚物、嵌段共聚物或无规共聚物。 In which the crystalline polymer component comprises a propylene copolymer embodiments, the propylene copolymer may be a graft copolymer, block copolymer or random copolymer.

[0038]存在于结晶聚合物组分中的丙烯衍生单元的量为90wt%或更高,或92wt%或更高,或95wt%或更高,或97wt%或更高,或100wt%,基于所述结晶聚合物组分的总重量。 [0038] crystalline polymer component present in the amount of propylene-derived units is 90wt% or more, or 92wt% or more, or 95wt% or more, or 97wt% or more, or 100wt%, based on The total weight of the crystalline polymer component.

[0039]在一个实施方案中,所述结晶聚合物组分包括丙烯和至少一种共聚单体的无规共聚物,所述至少一种共聚单体选自乙烯和C4-C12α-烯烃中的一种或多种。 [0039] In one embodiment, the crystalline polymer component comprises propylene and at least one comonomer of the random copolymer, said at least one comonomer selected from ethylene and C4-C12α- olefins one or more. 在该实施方案的一个具体方面,共聚单体的量的上限为9wt%、或8wt%、或6wt%,下限为2wt%,以所述结晶聚合物组分的总重量计。 In a particular aspect of this embodiment, the upper limit of the amount of comonomer is 9wt%, or 8wt%, or 6wt%, the lower limit of 2wt%, of the crystalline polymer component to the total weight.

[0040]本发明的结晶聚合物组分具有至少110℃、或至少115℃、或至少130℃的DSC熔点,和至少60J/g、或至少70J/g、或至少80J/g的由DSC测定的熔化热。 [0040] The crystalline polymer component of the present invention has at least 110 ℃, or at least 115 ℃, or a DSC melting point of at least 130 ℃ and at least 60J / g, or at least 70J / g, or at least 80J / g measured by DSC heat of fusion.

[0041]本发明的结晶聚合物组分的重均分子量(Mw)在上限为5,000,000g/mol或500,000g/mol,下限为10,000g/mol或50,000g/mol的范围内,并且有时被称为“多分散指数”(PDI)的分子量分布Mw/Mn(MWD)在上限为40,下限为1.5的范围内。 [0041] The weight of the crystalline polymer component of the present invention average molecular weight (Mw) within a maximum of 5,000,000g / mol or 500,000g / mol, a lower limit of 10,000g / mol or 50,000g / mol range, and are sometimes referred to distribution Mw / Mn (MWD) as "polydispersity index" (PDI) of a molecular weight in the upper limit is 40, the lower limit is in the range of 1.5.

[0042]本发明不受任何制备所述结晶聚合物组分的具体方法的限制。 [0042] The present invention is not limited by the specific method of preparation of the crystalline polymer component. 在一个实施方案中,所述结晶聚合物组分可以是通过众所周知的在单段或多段反应器中的丙烯均聚方法得到的丙烯均聚物。 In one embodiment, the crystalline polymer component may be known by one or more pieces of propylene in single stage reactor is homopolymerization of propylene homopolymer obtained. 在另一个实施方案中,所述结晶聚物组分可以是通过众所周知的在单段或多段反应器中共聚合丙烯与一种或多种共聚单体的方法得到的丙烯共聚物。 In another embodiment, the prepolymer component may be crystallized by a known segment in a single section of the reactor or copolymerizing propylene with one or more comonomers of the propylene copolymer obtained by the method.

[0043]制备所述结晶聚合物组分的聚合方法包括高压法、淤浆法、气相法、本体法、溶液相法及它们的组合。 [0043] Preparation of the crystalline polymer component include polymerization process high pressure, slurry, gas phase, bulk, solution phase method and a combination thereof. 可以使用的催化剂体系包括传统的齐格勒-纳塔催化剂及单中心茂金属催化剂体系。 The catalyst system can be used include conventional Ziegler - Natta catalysts and single-site metallocene catalyst system. 在一个实施方案中,所使用的催化剂具有高的立体专一性(isospecificity)。 In one embodiment, the catalyst used has a high stereospecificity (isospecificity).

[0044]结晶聚合物组分的聚合可以通过连续或间歇法进行,并可以包括链转移剂、清除剂或本领域技术人员所熟知的其它的这样的添加剂的使用。 Polymerization [0044] of the crystalline polymer component can be produced by a continuous or batch process and may include use of chain transfer agents, scavengers, or the skilled artisan of other such additives. 所述结晶聚合物组分可以还含有诸如流动改进剂、成核剂及抗氧剂的添加剂,所述添加剂通常被添加到等规聚丙烯中以改进或保持性能。 The crystalline polymer component may further contain as flow improvers, nucleating agents and antioxidant additives which are usually added to isotactic polypropylene to improve or maintain performance.

基于乙烯的聚合物 Ethylene-based polymer

[0045]本发明的某些实施方案包括具有没有结晶性或没有乙烯型结晶性的基于乙烯的聚合物。 [0045] Certain embodiments of the invention include those having no crystallinity or no crystallinity of the ethylene-vinyl-based polymer. 所述基于乙烯的聚合物是乙烯、α-烯烃和任选的二烯的共聚物。 The ethylene-based polymer is an ethylene, α- olefins and optionally diene. 在所述基于乙烯的聚合物中,乙烯衍生单元的量为50摩尔%或更高。 In the ethylene-based polymer, the amount of ethylene-derived units is 50 mol% or more. 在一个实施方案,所述基于乙烯的聚合物为乙烯-己烯共聚物。 In one embodiment, the ethylene-based polymer is an ethylene - hexene copolymer. 在另一个实施方案中,所述基于乙烯的聚合物是通常称为EPDM的乙烯、丙烯和二烯的聚合物。 In another embodiment, the ethylene-based polymer is generally known as ethylene, propylene and a diene polymer of EPDM. 在该实施方案的一个具体方面,在所述基于乙烯的聚合物中的丙烯衍生单元的量为40摩尔%或更高。 In a particular aspect of this embodiment, the amount of the ethylene-based polymer of propylene derived units in 40 mol% or more.

共混 Blends

[0046]在一个实施方案中,本发明提供了包含至少一种基于丙烯的弹性体和至少一种另外的组分的共混组合物,所述另外的组分选自结晶的基于丙烯的聚合物和基于乙烯的聚合物。 [0046] In one embodiment, the present invention provides a composition comprising at least one propylene-based elastomer blend composition and at least one additional component, said additional component selected from a crystalline propylene-based polymerization and ethylene-based polymer composition.

[0047]包括至少一种基于丙烯的弹性体、至少一种结晶的基于丙烯的聚合物和任选的基于乙烯的聚合物的本发明组合物具有由不同结晶性的区域所组成的多相形态。 [0047] comprising at least one propylene-based elastomer, at least one crystalline propylene-based polymer and optionally ethylene-based polymer composition of the present invention having a multi-phase morphology different crystalline regions composed of . 这些不同结晶性的区域将本发明组合物与通常可以获得的具有单一结晶相的丙烯反应器共聚物(即,等规聚丙烯与丙烯和乙烯共聚物的共混物)区分开。 These different crystalline region and the compositions of the invention can generally be obtained as reactor copolymers of propylene having a single crystalline phase (i.e., a blend of isotactic polypropylene and copolymers of propylene and ethylene) on the other.

[0048]这里所描述的多相共混组合物的连续相具有无定型或可结晶的形态,并含有基于丙烯的弹性体和任选的基于乙烯的聚合物。 [0048] the continuous phase of the heterophasic blend compositions described herein may have amorphous or crystalline form, and contains the propylene-based elastomer and optionally ethylene-based polymer. 分散相具有结晶形态,并含有结晶的基于丙烯的聚合物、任选的填料,并且可以还包含相对于所述连续相来说较少量的基于丙烯的弹性体和基于乙烯的聚合物。 A dispersed phase having a crystal form, and containing the propylene-based polymer, optionally a filler crystals, and may also contain relative to the continuous phase is a propylene-based elastomers and ethylene-based polymer of a relatively small amount. 所述基于丙烯的弹性体相对于结晶的基于丙烯的聚合物组分具有低的结晶度;因此,相对于分散相,本发明组合物的连续相具有较低的结晶度。 The propylene-based elastomer having a relative crystallinity of low crystallinity propylene-based polymer component; therefore, with respect to the dispersed phase, the continuous phase composition of the present invention has a lower degree of crystallinity. 所述低结晶度的连续相使得本发明的组合物区别于通常可获得的具有高度结晶连续相的耐冲击丙烯共聚物、热塑性弹性体、热塑性硫化胶和热塑性聚烯烃。 Impact propylene copolymers, thermoplastic elastomers, thermoplastic vulcanizates, and thermoplastic polyolefin continuous phase such that the low crystallinity of the compositions of the invention is highly different from the commonly available crystalline continuous phase resistance.

[0049]所述共混组合物的组分应相容至可以不需要加入预形成的或原位形成的增容剂来得到和保持优良的共混形态的程度。 [0049] The components of the blend compositions should be compatible to the compatibilizer may not be required to join a pre-formed or formed in situ to obtain and maintain an excellent degree of blend morphology.

[0050]这里所描述的多相共混组合物的分散相的区域较小,平均最小轴小于5微米。 Region [0050] heterogeneous blend compositions described herein dispersed phase is small, the average minor axis of less than 5 microns. 分散相的较大的轴可以大至100微米。 The larger axis of the dispersed phase can be as large as 100 microns.

添加剂 Additive

[0051]本领域技术人员将明白,除聚合物组分以外,本发明的组合物可以包含其它添加剂。 [0051] Those skilled in the art will appreciate, in addition to the polymer component, the compositions of the present invention may contain other additives. 可以存在各种添加剂以提高具体的性能,或者各种添加剂可以由于对各组分的加工而存在。 Various additives may be present to improve specific properties, or various additives may be due to processing of the components exists. 可以加入的添加剂包括但不限于加工油、防火剂、抗氧剂、增塑剂、颜料、硫化剂或固化剂、硫化或固化促进剂、硫化延迟剂、加工助剂、阻燃剂、增粘剂、流动改进剂等。 The additives may be added include, but are not limited to, processing oils, fire retardants, antioxidants, plasticizers, pigments, vulcanizing or curing agents, vulcanizing or curative accelerators, cure retarders, processing aids, flame retardants, tackifying agents, flow improvers, and the like. 还可以使用防粘连剂、着色剂、润滑剂、脱模剂、成核剂、增强剂及填料(包括粒状的、纤维状的或粉状的)。 You can also use anti-blocking agents, colorants, lubricants, mold release agents, nucleating agents, reinforcing agents and fillers (including granular, fibrous or powdered). 成核剂和填料可以改进制品的刚性。 Nucleating agents and fillers may improve the rigidity of the article. 这里所述的名单并不是意图包括可用于本发明中的所有类型的添加剂。 The list described herein is not intended to be included in the present invention can be used in all types of additives. 本领域的技术人员将明白,可以采用其它添加剂来提高所述组合物的性能。 Those skilled in the art will appreciate that other additives may be employed to improve the performance of the composition. 如本领域技术人员所理解的,本发明的组合物可以被改性,以按照需要调节共混物的特性。 As the skilled artisan will appreciate, the compositions of the present invention may be modified, as necessary to adjust the characteristics of the blends.

[0052]这里描述的组合物可以还含有无机颗粒填料,所述填料可以改进所述组合物的机械及耐磨损性能,尤其是在包括硫化的组分的组合物中。 [0052] The composition described herein may further contain an inorganic particulate filler, the filler can improve the mechanical and wear properties of the composition, especially in a composition comprising components vulcanization. 使用的无机填料的量通常为1至100重量份无机填料/100份聚合物材料。 Amount of the inorganic filler used is generally 1 to 100 parts by weight of an inorganic filler / 100 parts of polymer material. 所述无机填料包括直径小于1mm的颗粒,长度小于1cm的棒状物及表面积小于0.2cm2的片状物。 The inorganic filler comprises particles smaller than 1mm in diameter, the length of the rods is less than 1cm and a surface area of less than 0.2cm2 sheet. 示例性的颗粒填料包括炭黑、粘土、钛和镁的氧化物,以及硅石。 Exemplary particulate fillers include carbon black, clays, titanium and magnesium oxide, and silica. 此外,也可以使用其它颗粒填料如碳酸钙、氧化锌、白粉及氧化镁。 In addition, other particulate fillers may also be used such as calcium carbonate, zinc oxide, whiting, and magnesium oxide. 棒状填料的一个实例是玻璃纤维。 One example of a rod-like filler is glass fiber. 片状填料的一个实例是云母。 An example of the sheet-like filler is mica. 添加通常称为纳米复合材料的非常小的颗粒填料也是可以想到的。 Add commonly referred to as very small particulate filler nanocomposites also conceivable. 所述填料的添加可以改变这里所描述的组合物的性质。 The filler may be added to change the nature of the composition described herein. 例如,包括无机填料的组合物可以具有改进的热稳定性和耐磨性。 For example, a composition comprising an inorganic filler may have improved thermal stability and wear resistance. 添加白色填料可以改善烃聚合物在暴露于日光下时温度的变化。 Adding a white filler may improve hydrocarbon polymers on exposure to sunlight when the temperature changes. 添加填料超过某一水平可能导致粘度急剧增加和可加工性相应降低。 Filler is added above a certain level may lead to a sharp increase in viscosity and a corresponding decrease in workability. 该临界水平被称为突破阈值(percolation threshold)。 The critical level is called the breakthrough threshold (percolation threshold). 除了粘度增加外,所述突破阈值还伴随着弹性性质的改进,而在稍高于突破阈值的水平下,共混物的弹性回复下降。 In addition to increasing viscosity, the threshold value of the break is accompanied by improved elastic properties, and in the breakthrough level slightly higher than the threshold value, the elastic response blend drop. 突破阈值在不同的填料添加水平下得到,取决于所使用的填料类型。 Breakthrough threshold at different levels have been added fillers, depending on the type of filler used. 通常,具有较小尺寸的填料在比具有较大尺寸的填料更低的水平下获得所述突破阈值。 Typically, filler having a smaller size at a lower filler having a larger size than the level obtained the breakthrough threshold.

[0053]这里所描述的组合物可以含有0至500重量份、或2至200重量份、或5至150重量份、或10至100重量份的加工油,相对于每100份聚合物。 [0053] The compositions described herein can contain from 0 to 500 parts by weight, or from 2 to 200 parts by weight, or from 5 to 150 parts by weight, or 10 to 100 parts by weight of processing oil, per 100 parts of polymer. 适宜量加工油的加入可以降低共混物的粘度和挠曲性,同时改进所述共混物在接近和低于0℃的温度下的性能。 Adding suitable amounts of processing oil may reduce blend viscosity and flexibility, while improving the properties of the blend at temperatures near and below 0 ℃ temperature. 据信这些潜在的好处源自所述共混物的玻璃化转变温度(Tg)的降低。 It is believed these potential benefits derived from the blend has a glass transition temperature (Tg) is reduced. 向共混物中加入加工油也可以改进可加工性,并提供更好的弹性与拉伸强度的平衡。 Blend was added to the processing oil can also improve processability and provide a better balance of elastic and tensile strength. 所述加工油在橡胶应用中通常被称为增量油。 The processing oil in rubber applications commonly referred extender oil. 加工油包括具有(a)痕量杂原子如氧或(b)至少一个杂原子的烃,例如邻苯二甲酸二辛酯、醚及聚醚。 Processing oils include those having (a) trace amounts of hetero atoms such as oxygen or (b) at least one hetero atom of a hydrocarbon, such as dioctyl phthalate, ethers and polyethers. 加工油的沸点使得其在200℃基本上是不挥发的。 Process oil having a boiling point such that it is substantially at 200 ℃ non-volatile. 这些加工油通常可以以净的固体、液体的形式,或以这些材料吸附在惰性载体(例如粘土、硅石)上以形成自由流动粉末的物理吸收混合物的形式获得。 These processing oils may generally be net form of solid, liquid, or any of these materials adsorbed on an inert support (e.g. clays, silica) to form a physical absorbent in the form of a free flowing powder mixture is obtained. 加工油通常包括很多化合物的混合物,所述化合物可以由线性的、无环但支化的、环状的及芳族的含碳结构组成。 Process oils usually include a mixture of many compounds, the compound may be formed of linear, acyclic but branched, cyclic and aromatic carbonaceous structures family composition. 另一类加工油是分子量(Mn)低于10,000的某些有机酯及烷基醚酯。 Another class of processing oil having a molecular weight (Mn) is less than certain organic esters and alkyl ether esters 10,000. 加工油的组合也可以用于本发明的实践中。 Combination of processing oil can also be used in the practice of the present invention. 所述加工油应该与呈熔体的聚合物共混组合物相容或混溶,并且在室温下可以基本上混溶在所述基于丙烯的弹性体中。 The process oil should be compatible or miscible with the polymer showed a melt blend composition, and at room temperature can be substantially miscible in the propylene-based elastomer in. 加工油可以用本领域中已知的任何常规方法加入共混组合物中,包括在回收聚合物之前添加全部或部分的加工油,和添加全部或部分加工油至聚合物中作为用于掺混基于丙烯的弹性体的配混操作的一部分。 Processing oil may be any conventional method known in the art by the addition of the blend composition, comprising, prior to recovering the polymer add all or part of process oil, and add all or part of process oil to the polymer as a blend for part of the action-based mixed with propylene elastomer. 配混步骤可以在间歇混合机中进行,例如在开炼机中或在密闭式混合机如班伯里密炼机中进行。 Compounding step may be carried out in a batch mixer, e.g., carried out in an open roll mill or in a mixer such as a Banbury mixer. 配混操作也可以在连续工艺中进行,例如在双螺杆挤出机中进行。 Compounding operation may be carried out in a continuous process, for example in a twin-screw extruder. 加入加工油以降低等规聚丙烯和乙烯-丙烯-二烯橡胶的共混物的玻璃化转变温度描述在USP 5,290,886和5,397,832中,其公开内容通过引用结合在此。 Added process oil to reduce isotactic polypropylene and ethylene - propylene - diene rubber blends glass transition temperature are described in USP 5,290,886 and 5,397,832, the disclosure of which is incorporated by reference herein.

[0054]将加工助剂,例如脂肪酸酯混合物或结合在矿物填料上的脂肪酸皂钙加入这里所描述的组合物中,可有助于所述组合物的混合和将所述组合物注射到模具中。 [0054] The processing aids, such as fatty acid ester mixture or bound to the mineral filler added to the composition of fatty acid soaps of calcium described herein, can help to the mixed composition and the composition is injected into mold. 加工助剂的其它实例是低分子量聚乙烯共聚物蜡和石蜡。 Other examples of processing aids are low molecular weight polyethylene copolymer wax and paraffin. 使用的加工助剂的量可以在0.5至5phr的范围内。 Amounts of processing aids may be used in the range of 0.5 to 5phr.

[0055]向这里所描述的组合物中加入抗氧剂可以改进长期老化性。 [0055] to the composition described herein is added antioxidants may improve long-term aging. 抗氧剂的实例包括但不限于喹啉(quinolein),例如三甲基羟基喹啉(TMQ);咪唑,例如巯基甲苯甲酰基咪唑锌(ZMTI);和常规的抗氧剂,例如受阻酚、内酯及亚磷酸酯。 Examples of antioxidants include, but are not limited to quinoline (quinolein), e.g. trimethyl-hydroxy quinoline (TMQ); imidazole, e.g., mercapto zinc toluyl imidazole (ZMTI); and conventional antioxidants, such as hindered phenols, lactone and phosphite. 使用的抗氧剂的量可以在0.001至5phr的范围内。 Amount of the antioxidant used can range from 0.001 to 5phr in.

硫化的产物 Vulcanized product

[0056]在一个实施方案中,所述基于丙烯的弹性体的弹性体性能通过硫化所述弹性体至不同程度而被改进。 [0056] In one embodiment, the elastomeric properties based on the propylene elastomer is improved to different degrees by vulcanization of the elastomer. 在另一个实施方案中,所述基于丙烯的弹性体被硫化至不同程度,以允许进行方便的加工。 In another embodiment, the propylene-based elastomer is vulcanized to a different extent, to permit convenient processing. 在某些实施方案中,所述基于丙烯的弹性体包括二烯,以有利于硫化和在配制和加工的各种选项中最佳的最终用途性能。 In certain embodiments, the propylene-based elastomer comprises a diene, to facilitate curing and the best performance in end-use formulation and processing of the various options. 在其它的实施方案中,例如当使用辐射诱导硫化时,二烯在所述基于丙烯的弹性体中的存在是任选的。 In other embodiments, such as when using radiation-induced curing, the diene present in the propylene-based elastomer in is optional.

[0057]在某些实施方案中,所述硫化程度通过测量在任何溶解硫化前的所述组合物的溶剂中的不溶物wt%来确定。 [0057] In certain embodiments, measuring the degree of the cure of the composition in a solvent to dissolve before vulcanization in any insolubles wt% determined by. 这里所描述的组合物可以被硫化至一定程度,以提供至少2wt%、或至少5wt%、或至少10wt%、或至少20wt%、或至少35wt%、或至少45wt%、或至少65wt%、或至少75wt%、或至少85wt%、或少于95wt%的不溶物。 The composition described herein can be cured to a certain extent, to provide at least 2wt%, or at least 5wt%, or at least 10wt%, or at least 20wt%, or at least 35wt%, or at least 45wt%, or at least 65wt%, or at least 75wt%, or at least 85wt%, or less than 95wt% of insolubles.

[0058]在某些实施方案中,硫化的程度通过粘度比来测量。 [0058] In certain embodiments, the extent of cure measured by the ratio of the viscosity. 这里所描述的组合物可以被硫化至一定程度,以提供1至10或1.2至10的粘度比。 The composition described herein can be cured to a certain extent, in order to provide a viscosity ratio of from 1 to 10 or 1.2 to 10.

[0059]这里所描述的硫化的组合物可以具有改进的从拉伸形变弹性回复性能,如测量永久变形所显示的。 [0059] The composition described herein vulcanization may have improved elastic recovery from tensile deformation, such as measuring the permanent deformation displayed. 永久变形是在单轴形变后样品尺寸的回复。 Permanent deformation in the sample size after uniaxial deformation response. 永久变形表示的是机械延伸一段短时间后的物理效果。 Permanent deformation represents the physical effects of mechanical extension after a short time. 在某一具体伸长率下的永久变形简称为TSx%,其中X为伸长率。 Permanent deformation at a particular elongation is abbreviated as TSx%, where X is the elongation. 这样,TS100%、TS200%、TS300%、TS400%和TS500%分别表示在100%、200%、300%、400%和500%伸长率下的永久变形。 Thus, TS100%, TS200%, TS300%, TS400% and TS500% respectively permanent deformation at 100%, 200%, 300%, 400% and 500% elongation. 在一个实施方案中,这里所描述的包括硫化的基于丙烯的弹性体的组合物可以具有低于硫化前相同组合物永久变形的95%、或低于硫化前相同组合物永久变形的90%、或低于硫化前相同组合物永久变形的80%、或低于硫化前相同组合物永久变形的70%、或低于60%硫化前相同组合物永久变形的的TS100%、TS200%、TS300%、TS400%或TS500%。 In one embodiment, described herein include vulcanized compositions based on propylene elastomer may have the same composition before curing is lower than 95% permanent deformation, or less than the same composition before vulcanization permanent deformation of 90%, or less than 80% identical composition before vulcanization permanent deformation, or less than 70% identical composition before vulcanization permanent deformation, or less than 60% before vulcanization TS100% identical composition of permanent deformation, TS200%, TS300% , TS400% or TS500%.

[0060]这里所描述的硫化的组合物在拉伸形变期间可以具有显著的应力松弛。 [0060] The composition described herein vulcanized during the stretching deformation can have a significant stress relaxation. 所述应力松弛是在单轴形变后,在延长的时间内维持样品尺寸的一定延伸所需要力的减小。 The stress relaxation is the uniaxial deformation, maintaining a certain extend reduced sample size required force over an extended period of time. 应力松弛表示的是机械延伸一段的物理效果。 Stress relaxation represents the physical effects of mechanical stretching paragraph. 在某一具体伸长率下的应力松弛简称为SRx%,其中X为伸长率。 Stress at a particular elongation is abbreviated as relaxation SRx%, where X is the elongation. 这样,SR100%、SR200%和SR300%分别表示在100%、200%和300%伸长率下的应力松弛。 Thus, SR100%, SR200% and SR300% respectively at 100%, 200% stress relaxation and 300% elongation of. 在一个实施方案中,这里所描述的包括硫化的基于丙烯的弹性体的组合物可以具有小于硫化前相同组合物应力松弛的95%、或小于硫化前相同组合物应力松弛的90%、或小于硫化前相同组合物应力松弛的80%、或小于硫化前相同组合物应力松弛的70%、或小于硫化前相同组合物应力松弛的60%的SR100%、SR200%或SR300%。 In one embodiment, described herein include vulcanized compositions based on propylene elastomer may have the same composition before vulcanization less than the stress relaxation of 95%, or less than the same composition before vulcanization stress relaxation of 90%, or less than Before vulcanization of the same composition Stress Relaxation 80% or less than the same composition before vulcanization stress relaxation of 70%, or less than 60% of the same composition before vulcanization stress relaxation SR100%, SR200% or SR300%.

[0061]这里所描述的硫化组合物可以具有比硫化所述基于丙烯的弹性体之前的相应组合物大至少20%、或大至少40%、或大至少100%的口型C撕裂强度。 [0061] The sulfurized composition described herein may have a ratio based on the corresponding composition of the vulcanized elastomeric propylene before at least 20%, or at least 40% greater, or at least 100% of the Die C tear strength.

[0062]这里所描述的硫化组合物可以具有比硫化所述基于丙烯的弹性体之前的相应组合物小20%、或小40%、或小60%、或小80%、或小90%、或小95%的应力松弛。 [0062] The sulfurized composition described herein may have a ratio based on the corresponding composition of the vulcanized elastomeric propylene little before 20%, or 40% less, or 60% less, or 80% less or 90% less, or 95% of small stress relaxation.

[0063]本发明的一个实施方案包括一种共混组合物,该组合物包括(a)包含基于丙烯的弹性体和任选的基于乙烯的聚合物的连续相,和(b)包含结晶的基于丙烯的聚合物组分的分散相,其中至少2wt%、或至少5wt%、或至少10wt%、或至少20wt%、或至少35wt%、或至少45wt%、或至少65wt%、或至少75wt%、或至少85wt%、或至少95wt%的连续相被硫化,通过在溶解硫化前的所述组合物的任何溶剂中的不溶物wt%测定。 [0063] An embodiment of the present invention comprises a blend composition, the composition comprising (a) a propylene-based elastomer and optionally a continuous phase based on ethylene polymer, and (b) comprises crystallized propylene-based polymer component of the dispersed phase, wherein at least 2wt%, or at least 5wt%, or at least 10wt%, or at least 20wt%, or at least 35wt%, or at least 45wt%, or at least 65wt%, or at least 75wt% , or at least 85wt%, or at least 95wt% of the continuous phase is cured, by any solvent in the composition are dissolved before vulcanization insolubles wt% was measured.

[0064]本发明的另一个实施方案包括一种共混组合物,该组合物包括(a)包含基于丙烯的弹性体和任选的基于乙烯的聚合物的连续相,和(b)包含结晶的基于丙烯的聚合物组分的分散相,其中所述连续相被硫化至使得所述硫化组合物的粘度高于硫化前所述组合物的粘度的程度,如由粘度比所显示的。 [0064] Another embodiment of the present invention comprises a blend composition, the composition comprising (a) a propylene-based elastomer-based continuous phase and optionally the ethylene polymer, and (b) comprises a crystalline The propylene-based polymer component of the dispersed phase, wherein the continuous phase is vulcanized to such that the viscosity of the curing composition is higher than the degree of cure before the viscosity of the composition, as shown by the viscosity ratio. 例如,所述共混组合物可以被硫化至使得所述粘度比为1至10,或1.2至10的程度。 For example, the blend composition can be cured to such that the viscosity ratio of 1 to 10, or the extent of 1.2 to 10.

[0065]本发明的一个实施方案包括一种组合物,该组合物包含至少一种硫化的基于丙烯的弹性体、任选的结晶的基于丙烯的聚合物组分、任选的基于乙烯的聚合物和炭黑。 [0065] An embodiment of the present invention comprises a composition, said composition comprising at least one sulfurized propylene-based elastomer, optionally a crystalline propylene-based polymer component, based on the polymerization of ethylene optionally matter and carbon black. 炭黑可以以在上限为500、或250、或200、或100、或50phr,下限为1、或2、或5、或25phr的范围内的量存在。 Carbon black may be at the upper limit of 500, or 250, or 200, or 100, or 50phr, a lower limit of 1, or 2, or 5, or an amount within the range of the presence of 25phr. 在该实施方案的一个具体方面,所述组合物可以具有等于40*(肖氏A硬度/MI@190℃)-600+B的以MPa度量的拉伸强度,其中B为至少0、或至少2、或至少4、或至少10。 In a particular aspect of this embodiment, said composition may have equal to 40 * (Shore A hardness / MI @ 190 ℃) -600 + B of the tensile strength measured in MPa, wherein B is at least 0, or at least 2, or at least 4, or at least 10. 在该实施方案的另一个具体方面,所述组合物可以具有等于15*(肖氏A硬度/MI@190℃)-600+B的以Kn/m度量的口型C撕裂强度,其中B为至少2、或至少5、或至少10、或至少15。 In another particular aspect of this embodiment, the composition may have equal to 15 * (Shore A hardness / MI @ 190 ℃) -600 + B to Kn / m measured Die C tear strength, wherein B is at least 2, or at least 5, or at least 10, or at least 15.

[0066]本发明的一个实施方案包括一种组合物,该组合物包含至少一种硫化的基于丙烯的弹性体、任选的结晶的基于丙烯的聚合物组分、任选的基于乙烯的聚合物,并且不含填料。 [0066] An embodiment of the present invention comprises a composition, said composition comprising at least one sulfurized propylene-based elastomer, optionally a crystalline propylene-based polymer component, based on the polymerization of ethylene optionally and does not contain fillers. 在该实施方案的一个具体方面,所述组合物可以具有等于30*(肖氏A硬度/MI@190℃)-300+B的以MPa度量的拉伸强度,其中B为至少2、或至少4、或至少6、或至少12。 In a particular aspect of this embodiment, said composition may have equal to 30 * (Shore A hardness / MI @ 190 ℃) -300 + B of the tensile strength measured in MPa, wherein B is at least 2, or at least 4, or at least 6, or at least 12. 在该实施方案的另一个具体方面,所述组合物可以具有等于40*(肖氏A硬度/MI@190℃)-400+B的以Kn/m度量的口型C撕裂强度,其中B为至少5、或至少10、或至少15、或至少20。 In another particular aspect of this embodiment, the composition may have equal to 40 * (Shore A hardness / MI @ 190 ℃) -400 + B to Kn / m measured Die C tear strength, wherein B at least 5, or at least 10, or at least 15, or at least 20.

[0067]本发明的一个实施方案包括一种组合物,该组合物包含至少一种硫化的基于丙烯的弹性体、任选的结晶的基于丙烯的聚合物组分、任选的基于乙烯的聚合物和非黑色填料。 [0067] An embodiment of the present invention comprises a composition, said composition comprising at least one sulfurized propylene-based elastomer, optionally a crystalline propylene-based polymer component, based on the polymerization of ethylene optionally and non-black filler material. 所述填料可以是白色、红色、绿色、蓝色、黄色或任何非黑颜色。 The filler may be white, red, green, blue, yellow, or any non-black color. 所述填料可以以在上限为500、或250、或200、或100、或50phr,下限为1、或2、或5、或25phr的范围内的量存在。 The filler may be at the upper limit of 500, or 250, or 200, or 100, or 50phr, a lower limit of 1, or 2, or 5, or an amount within the range of the presence of 25phr. 在该实施方案的一个具体方面,所述组合物可以具有等于30*(肖氏A硬度/MI@190℃)-300+B的以MPa度量的拉伸强度,其中B为至少2、或至少4、或至少6、或至少12。 In a particular aspect of this embodiment, said composition may have equal to 30 * (Shore A hardness / MI @ 190 ℃) -300 + B of the tensile strength measured in MPa, wherein B is at least 2, or at least 4, or at least 6, or at least 12. 在该实施方案的另一个具体方面,所述组合物可以具有等于40*(肖氏A硬度/MI@190℃)-400+B的以Kn/m度量的口型C撕裂强度,其中B为至少5、或至少10、或至少15、或至少20。 In another particular aspect of this embodiment, the composition may have equal to 40 * (Shore A hardness / MI @ 190 ℃) -400 + B to Kn / m measured Die C tear strength, wherein B at least 5, or at least 10, or at least 15, or at least 20.

[0068]在一个实施方案中,本发明提供了一种硫化的组合物,该硫化的组合物包含基于丙烯的弹性体、结晶的基于丙烯的聚合物组分和基于乙烯的聚合物,其中所述硫化的组合物的机械性能与单独的硫化的基于乙烯的聚合物的机械性能相比有改进。 [0068] In one embodiment, the present invention provides a composition cured, the cured composition comprising the propylene-based elastomer, a crystalline polymer component and a propylene-based polymers based on ethylene, wherein Mechanical properties of said cured composition and separate ethylene-based polymers compared to the mechanical properties of the cured improvement. 例如,基于丙烯的弹性体、结晶的基于丙烯的聚合物组分和基于乙烯的聚合物的硫化共混物的拉伸强度(TS)和/或口型C撕裂强度(TEAR)可以比单独的基于乙烯的聚合物的TS和TEAR高至少10%,并满足以下关系:TS>TS(TPC)+0.9*R*TS(FPC+SPC)TEAR>TEAR(TPC)+0.9*TS(FPC+SPC)其中TS(FPC+SPC)是基于丙烯的弹性体和任选量的结晶的基于丙烯的聚合物的拉伸强度,TEAR(FPC+SPC)是基于丙烯的弹性体和任选量的结晶的基于丙烯的聚合物的口型C撕裂强度,TS(TPC)是基于乙烯的聚合物的拉伸强度,TEAR(TPC)是基于乙烯的聚合物的口型C撕裂强度,条件是在所有这些对比中,基于丙烯的弹性体与结晶的基于丙烯的聚合物的比是恒定的。 For example, propylene-based elastomer, a crystalline propylene-based polymer component and the ethylene-based polymer blend of sulfurized tensile strength (TS) and / or a Die C tear strength (TEAR) alone can be compared TS-based polymers and ethylene-TEAR is at least 10%, and satisfies the following relationship: TS> TS (TPC) + 0.9 * R * TS (FPC + SPC) TEAR> TEAR (TPC) + 0.9 * TS (FPC + SPC) where TS (FPC + SPC) is a propylene-based elastomer and an optional amount of a crystalline propylene-based polymer of the tensile strength, TEAR (FPC + SPC) is a propylene-based elastomer and an optional amount of crystalline The propylene-based polymer Die C tear strength, TS (TPC) is based on the tensile strength of the ethylene polymer, TEAR (TPC) is an ethylene-based polymer Die C tear strength, provided that in All of these comparison, the propylene-based elastomer and a crystalline propylene-based polymer ratio is constant.

[0069]这里所描述的组合物可以通过保证聚合物组分形成紧密混合物的任何方法制备。 [0069] The composition described herein is prepared by any method can be formed by an intimate mixture of the polymer components guaranteed. 通常,所述方法的第一步骤为混合聚合物组分与任选的添加剂,例如加工油、填料、着色剂、抗氧剂、成核剂以及流动改进剂,使用设备例如但不限于用于熔融压制所述组分在一起的Carver压机,用于各组分的溶液或熔体共混的密闭式混合机如班伯里密炼机或Brabender混炼机,以及用于连续混合方法的设备,包括单和双螺杆挤出机、静态混合器、撞击式混合器以及设计成使各组分分散以紧密接触的其它机器和工艺。 Typically, the first step of the method for mixing the polymer components and optional additives, such as process oils, fillers, colorants, antioxidants, nucleating agents and flow improvers using equipment such as, but not limited to, for melt pressing the components together in a Carver press, the components of the solution or melt blending mixer such as a Banbury mixer or a Brabender mixer, and a continuous mixing method used for equipment, including single and twin screw extruders, static mixers, impact mixers, and other machines and processes designed to disperse the components are in intimate contact. 聚合物组分的完全混合由组合物形态的均匀性来指示。 Complete mixing of the polymer components from a homogeneous composition morphology indicated. 这样的方法对本领域技术人员来说是众所周知的。 Such methods of the skilled artisan is well known. 在一个实施方案中,下一步是将化学硫化剂如过氧化物或硫化合物与所述紧密混合物混合,和然后将包括所述化学硫化剂的所述紧密混合物制造成最终形状的制品,并升高温度一段时间,以允许所述基于丙烯的弹性体硫化。 In one embodiment, the next step is a chemical curing agent such as a peroxide or a sulfur compound is mixed with the intimate mixture, and then the chemical vulcanizing agents include the intimate mixture into the final shape of the manufactured article, and L High temperature period of time to allow the propylene-based elastomer vulcanization. 在另一个实施方案中,下一步是将所述紧密混合物制成最终形状的制品,和然后使所述成形的混合物暴露于外硫化剂如高能辐射,以允许所述基于丙烯的弹性体硫化。 In another embodiment, the next step is the intimate mixture into the final shape of the article, and the shaped mixture is then exposed to high energy radiation such as curatives, to allow the propylene-based elastomer vulcanization.

[0070]可用于本发明实践中的硫化体系包括硫基硫化剂、过氧化物硫化剂、树脂硫化、氢化硅烷化(hydrosilation)、不稳定的或迁移的硫化体系和高能辐射中的一种或多种。 [0070] can be used in the practice of the present invention the vulcanization system comprises sulfur-based vulcanizing agent, a peroxide curing agent, a resin cure, hydrosilylation (hydrosilation), curing system unstable and high-energy radiation or migration of one or variety. 这些硫化体系是本领域中所熟知的。 These cure systems are well known in the art.

[0071]当使用化学硫化剂如硫、硫给体、过氧化物及树脂以诱导反应时,所述硫化剂通常在制造最终形状的待制备制品之前混合到所述基于丙烯的弹性体中或包含所述弹性体的共混物中。 [0071] When using a chemical vulcanizing agents such as sulfur, sulfur donors, peroxides, and the resin to induce the reaction, the curing agent is generally manufactured prior to the final shape of the article to be produced is mixed into the propylene-based elastomer, or comprising the blend elastomer. 当使用外交联剂如活性化学试剂和高能辐射诱导反应时,将所述基于丙烯的弹性体或包含所述弹性体的共混物制造成最终形状的待制备制品,然后与外交联剂接触。 When using an external crosslinker-induced reactions such as active chemical agents and high-energy radiation, the propylene-based elastomer or a blend of the elastomer comprising producing a final shape of articles to be prepared, and then contacted with an external crosslinker.

纤维 Fiber

[0072]在一个实施方案中,本发明提供了一种包含这里所描述的组合物的纤维。 [0072] In one embodiment, the present invention provides a composition comprising a fiber as described herein. 制造本发明纤维的方法包括本领域技术人员众所周知的那些方法。 The method of producing fibers of the present invention include those methods well known to the skilled person. 本发明的纤维可以具有期望的软度和弹性性质,并可以用于各种应用中,例如连续长丝纱、膨体连续长丝纱、常产纤维、熔融吹制的纤维和纺粘纤维(spunbound fiber)。 Softness and elastic properties of the fiber of the present invention may have a desired, and can be used in various applications, such as continuous filament yarns, bulked continuous filament yarns, staple fibers, meltblown fibers and spunbond fibers ( spunbound fiber). 在该实施方案的一个具体方面,包含这里所描述的组合物的纤维可以具有以下优点之一或两者:1)可以通过经喷丝头的挤出,接着拉丝至要求的但尼尔而容易地纺成纤维,和2)在宽的共混物组成范围内由纺丝速率度量的纺纤维的能力可以不受影响,即使是在通过向基于丙烯的弹性体中加入结晶的基于丙烯的聚合物而使所述共混物的熔体流动速率(MFR)缓慢下降时。 In a particular aspect of this embodiment, the fiber comprising the composition described herein may have one or both of the following advantages: 1) can be extruded through a spinneret, and then drawing to the desired denier easily spun into fibers, and 2) over a wide range of compositions blend spinning rate measured by the ability to spin fibers may not be affected, even by the addition of a crystalline propylene-based elastomer based on the polymerization of propylene was leaving the blend has a melt flow rate (MFR) slowly drops. 在宽的共混物组成范围内纺丝速率的恒定不变是特别出人意外的,因为纺丝速率对聚合物(或聚合物共混物)的MFR敏感,低MFR的聚合物具有差的纺丝性能。 Over a wide composition range of blends constant spinning rate is particularly surprising, since the spinning rate of the polymer (or polymer blend) MFR of sensitive, low MFR polymer have poor spinning performance.

[0073]在一个实施方案中,本发明纤维的弹性回复、应力松弛和拉伸回复性能可以通过退火和/或机械取向来提高。 [0073] In one embodiment, the elastic fibers of the present invention to reply, stress relaxation and tensile recovery properties can be improved by annealing and / or mechanical orientation. 退火部分地释放在伸长的纤维中的内应力,并恢复纤维中的共混物的弹性回复性能。 Annealing partially release the internal stress in the stretched fiber and restores the elastic fiber blend recovery properties. 退火已显示出导致结晶结构的内部组织化方面以及无定型和半结晶相的相对有序化方面的显著变化,这导致弹性性能的回复。 Annealing has been shown to lead to significant changes in the internal organization of the crystalline structure and the relative areas of ordering aspects amorphous and semi-crystalline phase, which results in the elastic properties of the reply. 所述纤维可以在高于室温至少40,或高于室温至少20,但稍低于所述共混组合物的结晶熔点的温度下退火。 The fibers may be at least above room temperature 40, or above room temperature at least 20, but slightly lower than the crystalline melting point of the blend composition of the annealing temperature. 加温退火通过将聚合物纤维在室温至160℃或130℃的温度下维持5分钟至7天的时间来进行。 Thermal annealing by maintaining the polymer fibers 5-7 minutes of time to be at a temperature of room temperature to 160 ℃ or 130 ℃ of. 典型的退火时间为50℃下3天,或100℃下5分钟。 The typical annealing time at 50 ℃ 3 days, or at 100 ℃ 5 minutes. 退火时间和温度可以针对任何具体的聚合物纤维进行调整,通过试验确定。 The annealing time and temperature can be adjusted for any particular polymer fibers, determined by tests. 可以相信,在该退火工艺过程中,存在聚合物链的分子间重排,导致具有比未退火材料更大的从拉伸形变回复性能的材料。 It is believed that during this annealing process, the presence of inter-molecular rearrangement of the polymer chains, resulting in a greater response from tensile deformation than the unannealed material properties of the material. 所述纤维的退火是在没有机械取向的情况下完成的,但是机械取向可以是退火过程的一部分,例如在挤出操作后。 Annealing the fibers in the absence of mechanical orientation of the case is completed, but can be part of the mechanical alignment of the annealing process, for example after the extrusion operation.

[0074]机械取向可以通过使聚合物纤维在被允许在无延伸力下松弛之前临时强制延伸一段短的时间来进行。 [0074] Mechanical orientation can be obtained by the polymer fibers are allowed without mandatory temporary extension force extends a short period of time prior to relaxation. 据信,所述纤维的机械取向导致纤维的可结晶部分重新取向。 It is believed that the mechanical orientation of the fiber can cause fiber reorientation in the crystalline portion. 取向的聚合物纤维可以通过将聚合物纤维在100%至700%的延伸下维持0.1秒至24小时的时间来进行。 Oriented polymer fibers may be polymer fibers by maintaining 0.1 to 24 seconds of time to be carried out under 100 to 700% extension. 典型的取向是在室温下维持200%的延伸短暂的时间。 A typical orientation is an extension of 200% to maintain a short time at room temperature.

[0075]为了获得纤维的取向,在升高的温度(但低于聚合物的结晶熔点)下的聚合物纤维从一个纤维供料辊出来,绕过两个被以不同表面速度驱动的辊,并最终到达卷取辊。 [0075] In order to obtain the orientation of the fibers, at an elevated temperature (but below the crystalline melting point of the polymer) of polymer fibers from a fiber under the supply roll out, bypassing both are driven at different surface speeds of the rollers, and finally reaches the take-up roll. 与卷取辊最接近的被驱动辊比与供料辊最接近的被驱动辊被更快地驱动,使得所述纤维在所述被驱动辊之间被伸长。 And take-up roller than the driven roller closest to the feed roller and the driven roller is closest driven faster, so that the fibers are to be stretched between the driving roller in the. 所述组件可以包括在第二辊与卷取辊之间的用于冷却纤维的辊。 The assembly may include a roll for cooling the fiber in the second roller and take-up roll. 第二辊和卷取辊可以被以相同的圆周速度驱动,以维持纤维在延伸状态。 The second roller and take-up roller may be driven at the same circumferential speed, to maintain the fibers in an extended state. 如果没有使用辅助冷却,所述纤维将在卷取辊上冷却至环境温度。 If no auxiliary cooling, the fiber will cool to ambient temperature on the take-up roll.

[0076]在一个实施方案中,本发明提供了用本发明纤维制造的织物。 [0076] In one embodiment, the present invention provides a fiber produced by the present invention is a fabric. 所述织物可以通过任何已知的用于制造非织造或织造织物的方法制成。 The fabric may be made by any method known for the manufacture of a nonwoven or woven fabric.

薄膜 Film

[0077]在一个实施方案中,本发明提供了包含这里所描述的组合物的薄膜。 [0077] In one embodiment, the present invention provides a film comprising the composition described herein. 用于制造本发明的薄膜的方法包括本领域技术人员众所周知的那些方法,包括但不限于常规的管形挤出法或吹泡法,及流延挤出。 The method for manufacturing a thin film of the present invention include those methods well known to persons skilled in the art, including but not limited to, a conventional tubular extrusion or blown bubble method, cast and extruded. 挤出温度、模头温度及冷却辊温度取决于采用的组合物,但对于这里所描述的组合物通常在以下范围内:熔体温度350-450;模头温度350-450;冷却辊温度70-130。 Extrusion temperature, the composition of the die and the cooling roll temperature depends on the temperature employed, but for the compositions described herein is generally within the following ranges: melt temperature 350-450; die temperature 350-450; chill roll temperature 70-130. 所述薄膜制造工艺可以还包括压花辊,以冷却并形成薄膜。 The film manufacturing process may also include an embossing roll, to cool and form a film.

[0078]本发明的薄膜可以有粘合到所述本发明薄膜的一面或两面上的层。 [0078] The film of the present invention may have an adhesive layer to one or both sides of the film of the invention. 所述各层可以通过共挤出本发明的薄膜与任选的另外的一层或多层来粘合在一起。 Said layers can be coextruded film of the invention and optional additional layer or layers to be bonded together. 在共挤出的薄膜中,各层在组成上是不同的,并且除了界面层以外所述各层保持其组成。 In the coextruded films, the layers are different in composition, and in addition to the layers to maintain its interface layer composition. 所述任选的另外的层可以是例如软的材料,例如乙烯-丙烯共聚物弹性体,其可以降低本发明薄膜的粘性(即发粘的)感觉。 The optional additional layer may be for example a soft material, such as ethylene - propylene copolymer elastomer, which can reduce the viscosity of the present invention, a thin film (i.e., sticky) feel. 所述任选的另外的层也可以是例如热塑性的。 The optional additional layer may be, for example thermoplastic. 热塑性层例如可以被用作弹性薄膜的机械支撑物以防止下垂,和被用作防止聚合物薄膜粘合到其它表面上的阻隔物。 The thermoplastic layer may be used as an elastic film such as a mechanical support to prevent sagging, and is used as a polymeric film adhered to the other to prevent the barrier on the surface. 热塑性层可以成为整体使用弹性薄膜的一部分,因为所述复合薄膜可以被拉伸超出所述热塑性层的屈服点,例如大于50%的伸长率,并且可以因所述弹性薄膜的弹力而缩回。 The thermoplastic layer may be part of an elastic film as a whole, because the composite film may be stretched beyond the yield point of the thermoplastic layer, e.g., greater than 50% elongation, and can be retracted by the elastic force of the elastic film . 在这种应用中,使所述热塑性薄膜变皱,以产生所述复合弹性薄膜的希望的表面处理(surface finish)。 In this application, so that the thermoplastic film creased to produce the composite elastic film of the desired surface treatment (surface finish). 可用于该目的的热塑性材料包括但不限于聚丙烯和聚乙烯。 The thermoplastic material can be used for this purpose include but are not limited to, polypropylene and polyethylene.

[0079]在一个实施方案中,本发明薄膜的机械性能如弹性回复和应力松弛可以通过加温退火和/或机械取向而提高。 [0079] In one embodiment, the mechanical properties of the films of this invention, such as elastic recovery and stress relaxation by thermal annealing and / or mechanical orientation increases.

[0080]加温退火通过将聚合物共混物或由该共混物制成的制品在室温至160℃的温度下维持5分钟至7天的时间来进行。 [0080] By the thermal annealing of the polymer blend or article made from the blend is maintained at a temperature of room temperature to 160 ℃ of 5-7 minutes time to carry out. 典型的退火时间为50℃下3天,或100℃下5分钟。 The typical annealing time at 50 ℃ 3 days, or at 100 ℃ 5 minutes. 退火时间和温度可以针对任何具体的共混组合物进行调整,通过试验确定。 The annealing time and temperature can be adjusted for any particular blend composition, determined by tests. 据信,在这种退火工艺过程中,存在聚合物链的分子间重排,导致比未退火材料具有更大的从拉伸形变回复的性能的材料。 It is believed that, in this annealing process, there is intermolecular rearrangement of the polymer chains, resulting in a greater than the unannealed material from tensile deformation recovery properties of the material.

[0081]机械取向可以通过使共混物沿一个或多个轴短暂地强制延伸一段短的时间,然后允许其在无延伸力的情况下松弛来进行。 [0081] Mechanical orientation can be obtained by the blend along one or more axes extending briefly forced a short period of time, and then allow its relaxed extending force in the absence of a case to carry out. 据信,所述聚合物的机械取向导致共混物的可结晶部分的重新取向。 It is believed that the mechanical orientation of the polymer leads to reorientation of the crystallizable portions of the blend. 取向通过将聚合物共混物或由该共混物制成的制品在10%至400%的延伸下维持0.1秒至24小时的时间来进行。 Orientation by polymer blend or article made from the blend is maintained from 0.1 to 24 seconds at a time to 10 to 400% of the elongation. 典型的取向是在室温下维持200%的延伸短暂的时间(通常少于1分钟)。 A typical orientation is an extension of 200% to maintain a short time at room temperature (typically less than 1 minute).

[0082]薄膜取向可以使用常规的设备和方法,在纵向(MD)或横向(TC)或两个方向(双轴)上进行。 [0082] orientation of the film using conventional equipment and methods, carried out in the machine direction (MD) or transverse (TC) or both directions (biaxially) on. 为了获得MD取向,在升高的温度(但低于聚合物的结晶熔点)下的聚合物薄膜从一个薄膜供料辊出来,绕过两个被以不同表面速度驱动的辊,并最终到达卷取辊。 In order to obtain MD orientation, at elevated temperature (but below the crystalline melting point of the polymer) from a polymer film under the film supply roll out, bypassing both are driven at different surface speeds of the rolls, and finally to the volume Take rolls. 与卷取辊最接近的被驱动辊比与供料辊最接近的被驱动辊被更快地驱动,使得所述薄膜在所述被驱动辊之间被伸长。 And take-up roller than the driven roller closest to the feed roller and the driven roller is closest driven faster, so that the film is stretched between the driving roller is at the. 所述组件可以包括在第二辊与卷取辊之间的用于冷却薄膜的辊。 The assembly may comprise between the second roller and take-up roll for cooling the film roll. 第二辊和卷取辊可以被以相同的圆周速度驱动,以维持薄膜在延伸状态。 The second roller and take-up roller may be driven at the same circumferential speed, to maintain the film in the extended state. 如果没有使用辅助冷却,所述薄膜将在卷取辊上冷却至环境温度。 If no auxiliary cooling, the film will cool to ambient temperature on the take-up roll. 延展度将取决于所述被驱动辊的相对圆周速度和所述辊之间的距离。 Elongation will depend on the relative distance between the peripheral velocity of the driven roller and the roll. 对于大多数的MD取向应用,50-500%/分钟的延展速率将是令人满意的。 For most MD orientation applications, extension rate of 50-500% / minute will be satisfactory.

[0083]为了获得TD取向,薄膜取向在伸幅装置中进行。 [0083] In order to obtain the TD orientation, the orientation film is carried out in the tentering apparatus. 所述薄膜被流延或从薄膜卷松开,然后被边缘抓住以通过取向步骤进行加工。 The film was cast from the film roll or release, and then caught by the edge to be processed by the orientation step. 所述薄膜连续地通过预热步骤、在升高的温度(例如从100至稍低于乙烯可结晶共聚物的结晶熔点的温度)下的延展步骤、退火步骤和最终的冷却步骤。 The film is passed successively through the preheating step, at elevated temperature (e.g. from 100 to slightly below the crystalline melting point of the ethylene crystallizable copolymer of temperature) under the expanding step, a final annealing step and cooling step. 在预热和延展步骤和退火步骤的一部分中,温度被控制在升高的温度但低于聚合物的结晶熔点。 In the preheating part and the expanding step and the annealing step, the temperature is controlled at an elevated temperature but below the crystalline melting point of the polymer. 在退火和冷却步骤期间可以维持在薄膜上的张力,以使回缩最小化。 In the cooling step during annealing can be maintained and the tension on the film, so that retraction is minimized. 在冷却至环境温度即室温或接近环境温度后,可以释放所述保持力。 After cooling to ambient temperature, i.e., at or near ambient temperature, the holding force may be released. 所述薄膜在TD可能有一定收缩(急速返回),但将保持其延展长度的相当部分。 The film may have a contraction (snapback) in the TD, but will maintain a considerable part of its extended length. 伸幅机操作条件可以在相当宽的范围内变化,并且将取决于几个变量,包括例如薄膜组成、薄膜厚度、希望的取向度和退火条件。 Tenter operating conditions can take place over a fairly wide range, and will depend on several variables, including for example, film composition, film thickness, a desired degree of orientation and annealing conditions.

[0084]如前所述,所述取向工艺可以包括退火步骤。 [0084] As described above, the orientation process may include an annealing step. 退火部分释放在延展的薄膜中的内应力,并使薄膜尺寸稳定以进行储存。 Annealing partial release of internal stress in the stretched film, and the film is dimensionally stable for storage. 退火可以在一定的时间和温度下进行,二者有依存关系。 Annealing may be at a certain time and temperature, there are two dependencies.

[0085]在用于薄膜取向的一个具体方法中,使用相互交叉开槽的辊组件来同时产生希望的起皱的表面处理(surface finish)和使薄膜取向。 [0085] In one specific method for the oriented film using interdigitated grooved roller assembly to produce the desired surface treatment while wrinkling (surface finish) and the film orientation. 这种方法描述在USP 4,368,565中,其公开内容通过引用结合在此。 This method is described in USP 4,368,565, the disclosure of which is incorporated by reference herein. 在该方法中,所述薄膜在两个相互交叉开槽的辊之间延展,所述辊可以双轴延展所述薄膜并使其取向。 In this method, the thin film between the two mutually intersecting grooved rollers extend, the roller of the film may be biaxially stretched and allowed orientation.

[0086]本发明的纤维、薄膜和模制物件以及最终的织物、成型物(forms)和成形物(shapes)可以通过其中最终温度低于250℃的蒸汽或其它高温方法进行灭菌处理,没有形状的显著扭曲和机械性能的显著损失。 [0086] The fibers of the present invention, films and molded articles and final fabrics, molded articles (forms) and molded product (shapes) can be sterilized by steam or other high temperature processes wherein the final temperature is below 250 ℃ no shape significantly distorted and significant loss of mechanical properties. 本发明的纤维、薄膜和模制物件以及最终的织物、成型物和成形物也可以用低于100℃的热水和洗涤剂洗涤,没有形状的显著扭曲和机械性能的显著损失。 Fibers of the present invention, films and molded articles and the final fabric, molded product and the molded product can also be washed with detergent and hot water with less than 100 ℃, no significant loss of significant shape distortion and mechanical properties.

定义和测试方法 Definitions and test methods

[0087]共聚单体含量:聚合物的共聚单体含量和序列分布可以通过本领域技术人员所熟知的方法,使用13C核磁共振(NMR)测定。 [0087] The comonomer content: comonomer content and sequence distribution of the polymer by the skilled artisan, a method using 13C nuclear magnetic resonance (NMR) measurement. 离散的分子量范围的共聚单体含量可以使用本领域技术人员熟知的方法测定,包括对样品进行GPC分析结合傅立叶变换红外光谱法(FTIR),如Wheeler和Willis,Applied Spectroscopy,1993,第47卷第1128-1130页中所描述的。 Comonomer content of discrete molecular weight ranges can be performed using methods well known to those skilled measured, comprising combining the sample was analyzed by GPC Fourier transform infrared spectroscopy (FTIR), as Wheeler and Willis, Applied Spectroscopy, 1993, vol. 47 1128-1130 page described.

[0088]在含有大于75wt%丙烯的丙烯-乙烯共聚物的特定情况中,共聚单体含量可以如下测定:在约150℃或更高的温度下压制薄的均匀的薄膜,并固定在Perkin Elmer PE 1760红外光谱仪上。 [0088] In the propylene containing more than 75wt% of a propylene - ethylene copolymer in specific cases, the comonomer content can be determined as follows: at a temperature of about or higher 150 ℃ pressing a thin uniform film, and fixed Perkin Elmer PE 1760 infrared spectrometer. 记录从600cm-1至4000cm-1的样品的全光谱,乙烯的单体重量百分数可以按照以下方程式计算:乙烯wt%=82.585-111.987X+30.045X2,其中X是1155cm-1的峰高与722cm-1或732cm-1中较高峰的峰高之比。 Recording the full spectrum of the sample from the 600cm-1 to 4000cm-1, and the monomer weight percent of ethylene can be calculated according to the following equation: Ethylene wt% = 82.585-111.987X + 30.045X2, wherein X is the peak height of 1155cm-1 and 722cm -1 or the peak height of the more than 732cm-1 peak.

[0089]多烯含量:聚合物中存在的多烯的量可以通过定量测量聚合后聚合物中存在的侧挂的游离烯烃的量来推断。 [0089] polyene content: the amount of polyene present in the polymer can measure the amount present in the polymer after the polymerization of the pendant free-olefins by quantitative inferred. 已经建立了几种方法,例如碘值及通过H1或13C核磁共振(NMR)测定烯烃含量。 Several methods have been established, such as iodine number and olefin content determined by H1 or 13C nuclear magnetic resonance (NMR). 在这里所描述的其中所述多烯是ENB的实施方案中,聚合物中存在的多烯的量可以使用ASTM D3900测定。 Described herein in which the polyene is ENB embodiment, the amount of polyene present in the polymer can be determined using ASTM D3900.

[0090]全同立构:术语“全同立构”在这里定义为这样的聚合物序列,其中在位于以区域规则的1,2方式插入到所述链中的相邻丙烯单元上并且不是骨架结构部分的侧挂甲基对中的50%以上位于主链中的原子以上或以下,当主链中的这种原子全部在一个平面中时。 [0090] isotactic: The term "isotactic" is defined herein as a sequence of such a polymer, wherein the rule is located in the region of 1,2 inserted into the chain and is not adjacent propylene units above skeletal structure portion side hanging methyl 50% in the main-chain atoms or more or less, when the main chain atoms of this all in one plane. 在共混物中的聚合物或在单一聚合物内的聚合物序列的某些组合被描述为具有“基本上相同的立构规整度”,这里它意味着两种聚合物都是按照以上定义的全同立构的。 Some combination of polymers in the blend of the polymer or polymers in a single sequence is described as having "substantially the same tacticity", it means that the two polymers herein are defined in accordance with the above The isotactic's.

[0091]立构规整度:术语“立构规整度”是指聚合物中源自丙烯的甲基残基的取向的立体规整性。 [0091] The tacticity: The term "tacticity" refers to a polymer derived from propylene methyl residues orientation stereoregularity. 相对于聚合物骨架具有相同取向的、来自相邻的等同地插入的丙烯单元的甲基残基对被称为“内消旋的”(m)。 With respect to the polymer backbone having the same orientation, from the adjacent equally-methyl residues inserted propylene units to be referred to as "meso" (m). 相反构型的那些甲基残基对被称为“外消旋的”(r)。 Opposite configuration to those of methyl residues is called "racemic" (r). 当三个相邻的丙烯基团具有采取相同取向的甲基时,所述三单元组的立构规整性为“mm”。 When the group of three adjacent propylene having to take the same orientation methyl, the triad of stereoregularity is "mm". 如果在一个三单体序列中的两个相邻单体具有相同的取向,且该取向与第三单元的相对构型不同,所述三单元组的立构规整性为“mr”。 If a three-monomer sequence two adjacent monomers having the same orientation, and the relative configuration of the different orientation of the third unit, the triad of stereoregularity as "mr". 当中间的单体单元具有与任一相邻单体单元相反的构型时,所述三单元组具有“rr”立构规整性。 When the middle monomer unit having monomer units with any adjacent opposite configuration, said triads having "rr" stereoregularity. 聚合物中各类型的三单元组的分数可以被确定,并且当乘以100时表示在聚合物中发现的该类型的百分数。 Polymer triad fraction of each type can be determined, and indicates the percentage of that type found in the polymer, when multiplied by 100.

[0092]这里所描述的聚合物的三单元组立构规整度可以从所述聚合物的13C核磁共振(NMR)谱测定,如以下所描述的和在USP 5,504,172中所描述的,其公开内容通过引用结合在此。 The triad tacticity [0092] The polymers described herein can be determined from the spectrum of the polymer is 13C nuclear magnetic resonance (NMR), as described below and as described in the USP 5,504,172, the disclosure of which is incorporated by reference herein.

[0093]立构规整度指数:这里表示为“m/r”的立构规整度指数通过13C核磁共振(NMR)测定。 [0093] The tacticity index: here represented 13C nuclear magnetic resonance (NMR) was determined to be "m / r" stereoregularity index through. 立构规整度指数m/r按照HNCheng,Macromolecules,17,1950(1984)中所描述的进行计算。 The tacticity index m / r in accordance HNCheng, Macromolecules, 17,1950 (1984) as described in the calculation. 1.0的m/r比通常描述间规聚合物,2.0的m/r比通常描述无规的材料。 1.0 m / r ratio between generally described syndiotactic polymer, 2.0 m / r ratio described generally random material. 等规材料理论上可以具有接近无穷大的比,并且很多副产物无规聚合物具有足够大的全同立构含量,从而导致大于50的比。 Isotactic material theoretically may have a ratio approaching infinity, and many by-product atactic polymers have sufficient isotactic content, resulting in greater than 50 ratio.

[0094]熔点及熔化热:这里所描述的聚合物的熔点(Tm)及熔化热可以通过差示扫描量热法(DSC),采用ASTM E-794-95的程序确定。 [0094] Melting point and heat of fusion: polymer melting point (Tm) as described herein and a heat of fusion by Differential scanning calorimetry (DSC), using ASTM E-794-95 procedure determined. 用冲压模头取下在约200℃至230℃下压制的约6至10mg的聚合物片,并在室温下退火48小时。 Remove the stamping die at about 200 ℃ to 230 ℃ pressed for about 6 to 10mg of the polymer sheet, and annealed at room temperature for 48 hours. 在该时间结束时,将样品置于差示扫描量热仪(Perkin Elmer Pyris Analysis System)上,并冷却至约-50℃至-70℃。 At the end of that time, the samples were placed in a differential scanning calorimeter (Perkin Elmer Pyris Analysis System) on, and cooled to about -50 ℃ to -70 ℃. 以约20℃/min的速率加热样品达到约180℃至200℃的最终温度。 To about 20 ℃ / min heating rate of the sample to a final temperature of about 180 ℃ to 200 ℃ of. 这里所使用的术语“熔点”是通过以上所讨论的DSC测定的主熔融峰和次熔融峰中的最高峰。 As used herein, the term "melting point" is measured by DSC as discussed above the main melting peak measured melting peak and a secondary peak. 热输出记录为样品的熔融峰下的面积,其通常在约30℃至约175℃出现最大峰,并发生在约0℃至约200℃的温度之间。 Thermal output is recorded as the area under the melting peak of the sample, which typically occurs at about 30 ℃ maximum peak to about 175 ℃, and occurs at a temperature between about 0 ℃ to about 200 ℃ of. 热输出以焦耳测量,作为熔化热的量度。 Joule heat output to measure, as a measure of the heat of fusion. 熔点记录为样品熔化范围内最大吸热的温度。 Melting point of the sample is recorded as the maximum endothermic melting temperature range.

[0095]分子量和分子量分布:这里所描述的聚合物的分子量和分子量分布可如下测量。 [0095] Molecular weight and molecular weight distribution: polymers described herein the molecular weight and molecular weight distribution can be measured as follows. 分子量分布(MWD)是在给定的聚合物样品内分子量范围的量度。 The molecular weight distribution (MWD) is a measure of a given polymer sample in the molecular weight range. 众所周知,MWD的宽度可以通过各种分子量平均值的比,例如重均分子量与数均分子量之比Mw/Mn,或Z均分子量与重均分子量之比Mz/Mw表征。 Known, MWD width by various molecular weight averages than, for example, the weight average molecular weight to number average molecular weight ratio Mw / Mn, or Z-average molecular weight and weight-average molecular weight ratio Mz / Mw characterization.

[0096]Mz、Mw和Mn可以使用还称为尺寸排阻色谱法(SEC)的凝胶渗透色谱法(GPC)测定。 [0096] Mz, Mw and Mn can be determined using size exclusion chromatography, also known as (SEC) by gel permeation chromatography (GPC). 该技术利用包括装填有多孔珠粒的柱、洗提溶剂及检测器的仪器,以分离不同大小的聚合物分子。 The technique includes the use of porous beads filled with a column elution solvent, and detector devices to separate polymer molecules of different sizes. 在典型的测量中,所使用的GPC仪器是装有在145℃下运行的ultrastyro凝胶柱的Waters色谱仪。 In a typical measurement, GPC instrument used is a Waters chromatograph equipped at 145 ℃ running ultrastyro gel columns. 使用的洗提溶剂是三氯苯。 Elution solvent used is trichlorobenzene. 所述柱子用16个具有准确已知分子量的聚苯乙烯标准样品进行校准。 The column was calibrated using 16 polystyrene standard samples with accurately known molecular weight. 从标准样品得到的聚苯乙烯保留体积与测试聚合物的保留体积之间的相互关系给出所述聚合物的分子量。 Reserved Reserved volume as the relationship between a given test the polymer molecular weight of the polymer obtained from a standard sample of polystyrene.

[0097]平均分子量M可以从以下表达式计算:M=ΣiNiMin+1ΣiNiMin]]>其中Ni是具有分子量Mi的分子的数目。 [0097] The average molecular weight M is calculated from the following expression: M = & Sigma; iNiMin + 1 & Sigma; iNiMin]]> where Ni is the number of molecules having a molecular weight Mi. 当n=0时,M是数均分子量Mn。 When n = 0,, M is the number average molecular weight Mn. 当n=1时,M是重均分子量Mw。 When when n = 1, M is the weight average molecular weight Mw. 当n=2时,M是Z均分子量Mz。 When n = 2 时, M is the Z average molecular weight Mz. 希望的MWD函数(例如Mw/Mn或Mz/Mw)是相应的M值的比值。 Desired MWD function (e.g., Mw / Mn or Mz / Mw) is the ratio of the corresponding M values. M及MWD的测量是本领域中熟知的,并更详细地描述在例如Slade,PEEd.,Polymer Molecular Weights第II部分,Marcel Dekker,Inc.,NY,(1975)287-368;Rodriguez,F.,Principles of Polymer Systems第3版,Hemisphere Pub.Corp.,NY,(1989)155-160;USP 4,540,753;Verstrate等,Macromolecules,第21卷,(1988)3360;以及其中所引用的参考文件中。 Measurement of M and MWD is well known in the art, and described in more detail in e.g. Slade, PEEd, Polymer Molecular Weights Part II, Marcel Dekker, Inc., NY, (1975) 287-368;. Rodriguez, F. , Principles of Polymer Systems 3rd Edition, Hemisphere Pub.Corp, NY, (1989) 155-160;. USP 4,540,753; Verstrate etc., Macromolecules, vol. 21 (1988) 3360; and references cited therein.

[0098]永久变形:永久变形可以按照通用的ASTM D790程序,通过单轴向地使样品变形至不同的伸长率来测量。 [0098] permanent deformation: permanent deformation can follow the general procedure ASTM D790, Gravitropism by uniaxial deformation of the sample to be measured in different elongation.

[0099]应力松弛:应力松弛可以使用以下程序测量:将样品固定在Instron 4465试验机上,并伸长至200%的伸长率。 [0099] Stress relaxation: Stress relaxation may be measured using the following procedure: The sample was fixed on a Instron 4465 testing machine and elongated to 200% elongation. 在此伸长率下的负荷测定为L1。 Load measured at this elongation for L1. 将样品保持在该伸长下30秒钟,并在该30秒钟结束时测量新的负荷,为L130。 The sample was held at that elongation for 30 seconds, and measure the new load at the end of 30 seconds, for L130. 薄膜的松弛率(R1)测定为100(L1-L130)/L1,并以百分数表示。 Film at a relaxation rate (R1) was determined to be 100 (L1-L130) / L1, and expressed as a percentage. 使样品回复到0%的初始伸长率。 The samples were returned to 0% of the initial elongation. 然后将样品伸长至200%的伸长率。 The sample was then elongated to 200% elongation. 在此伸长率下的负荷测定为L2。 Load measured at this elongation for L2. 将样品保持在该伸长率下30秒钟,并在该30秒钟结束时测量新的负荷,为L230。 The sample was held at that elongation for 30 seconds, and measure the new load at the end of 30 seconds, for L230. 薄膜的松弛率(R2)测定为100(L2-L230)/L2,并以百分数表示。 Film at a relaxation rate (R2) was determined to be 100 (L2-L230) / L2, and expressed as a percentage. 使样品回复到0%的初始伸长率。 The samples were returned to 0% of the initial elongation. 在第二循环中样品上负荷为0时的伸长率称为变定%。 In the second cycle the sample load elongation becomes 0 is called a fixed%. 样品中的滞后现象指定为100(L1-L2)/L1,并以百分数表示。 Samples hysteresis designated 100 (L1-L2) / L1, and expressed as a percentage.

[00100]应力应变测量:这里所描述的硫化的混合物的应力应变伸长性能可以按照下面描述的ASTM D790方法测量。 [00100] Stress Strain Measurement: a mixture of sulfide stress described herein strain elongation properties can be measured according to ASTM D790 method described below. 将哑铃型样品制成模制成6英寸6英寸尺寸的硫化片(pad),并用冲模取出。 The dumbbell-shaped sample made of molded 6 inches 6-inch form vulcanized sheet (pad), and remove with a die. 样品的应力应变评价在Instron Corporation,Canton,MA制造的Instron 4465型试验机上对共混物以20英寸/分钟进行。 Stress strain evaluation of the samples in the Instron Corporation, Canton, MA manufactured by Instron 4465 testing machine type blend of 20 inches / min. 数位式数据收集在通过可从Instron Corporation得到的Series IX Material Testing System收集的文件中,并用得自WA Redmond的微软公司的Excel(一种电子数据表程序)进行分析。 Bit digital data is collected in a file collected Series IX Material Testing System available from Instron Corporation by obtained and used from WA Redmond of Microsoft Excel (a spreadsheet program) were analyzed.

[00101]PHR:这里所使用的术语“phr”是指份数/百份橡胶或份数/百份弹性体聚合物。 [00101] PHR: As used herein, the term "phr" refers to parts / hundred parts of rubber or parts / hundred parts of elastomeric polymer.

[00102]回流二甲苯中的溶解度:在回流二甲苯中的溶解度是在含有硫化的基于丙烯的弹性体及硫化的基于乙烯的聚合物(如果存在)的组合物中,不可溶解的和不可萃取的基于丙烯的弹性体及任选的基于乙烯的聚合物的量的量度。 [00102] The solubility in xylene at reflux: The solubility in xylene under reflux in a solution containing sulfide-based ethylene-based polymer (if present) in the composition, insoluble and non-extractable propylene elastomers and vulcanizable The propylene-based elastomer, and optionally the amount of ethylene-based polymer of the measure. 测定二甲苯中的溶解度的方法如下:称量具有薄的截面即小于0.5英寸和重约2g的样品,重量记录为W1。 Method for determining the solubility in xylene as follows: weighing the sample with a thin cross section that is less than 0.5 inches and weighing about 2g, and the weight recorded as W1. 使样品在萃取装置中暴露于50ml回流的二甲苯中。 Exposing the sample to 50ml refluxing xylene in the extraction apparatus. 通过回流的溶剂使样品的温度维持在140℃或接近140℃。 Refluxing the solvent through the sample temperature is maintained at 140 ℃ or near 140 ℃. 萃取24小时后,倾析掉溶剂并加入50ml新的溶剂,并在相同条件下再进行24小时萃取。 Extraction After 24 hours, the solvent was decanted off and added to 50ml of fresh solvent, and under the same conditions for 24 hours and then extracted. 在该段时间结束后,取出样品并在真空烘箱中在100℃下干燥24小时。 At the end of that period, a sample was taken in a vacuum oven at 100 ℃ dried for 24 hours. 然后冷却样品并称量最终的重量,记录为W2。 The sample was then cooled and weighed a final weight is recorded as W2. 在回流二甲苯中不溶的聚合物的分数通过下式确定:FIPX=100[W2(1-FFi)]/[W1(1-Fs-Fp-FFi)],其中Fs是组合物中存在的结晶聚合物组分的重量分数,Fp是组合物中存在的在回流二甲苯中可被萃取的增塑剂、加工油及其它低分子量材料的重量分数,FFi是组合物中存在的在回流二甲苯中通常不可萃取的填料和其它无机材料的重量分数。 In refluxing xylene insoluble fraction of the polymer is determined by the following equation: FIPX = 100 [W2 (1-FFi)] / [W1 (1-Fs-Fp-FFi)], where Fs is present in the composition of the weight fraction of the crystalline polymer component, Fp is a plasticizer in refluxing xylene extract composition may be present in, processing oil and other low molecular weight material weight fraction, FFi is present in the composition in the two reflux toluene is usually non-extractable filler and other inorganic materials weight fraction.

[00103]室温下的溶剂溶胀:室温下的溶剂溶胀度量含硫化的基于丙烯的弹性体的组合物在室温下的溶剂吸收量。 [00103] The solvent swell at room temperature: room temperature solvent swell measurements of the sulfur absorption amount of the solvent at room temperature based on the composition of a propylene elastomer. 用于测定室温下的溶剂溶胀的方法如下:称重具有薄的截面即小于0.5英寸和重约2g的样品,并且该重量记录为W3。 A method for solvent swell of the suspension was as follows: weighing the sample having a thin cross-section that is less than 0.5 inches and weighing about 2g, and the weight recorded as W3. 使样品暴露于在浸没装置中的50ml IRM 903油中。 The samples were exposed to the immersion apparatus 50ml IRM 903 oil. 样品的温度维持在接近室温。 Sample temperature was maintained at close to room temperature. 浸没70小时后,倾析出油并用己烷即刻洗涤样品。 After 70 hours immersion, the oil was decanted and washed with hexane instantly sample. 然后样品在80℃的真空烘箱中干燥24小时。 The samples were then in a vacuum oven at 80 ℃ dried for 24 hours. 随后冷却样品,并称取最终重量,该重量记录为W4。 Subsequently cooling the sample, the final weight were weighed, the weight is recorded as W4. 室温下的溶剂溶胀(SSA)通过下式确定:SSA=100(W4-W3)/W3。 Solvent swell at room temperature (SSA) is determined by the following equation: SSA = 100 (W4-W3) / W3.

[00104]在升高的温度下的溶剂溶胀:室温下的溶剂溶胀度量含硫化的基于丙烯的弹性体的组合物在升高的温度下的溶剂吸收量。 [00104] at an elevated temperature of the solvent swell: solvent swell measurements at room temperature sulfur absorption amount of the solvent at elevated temperature under elastomer-based composition of propylene. 测定在升高的温度下的溶剂溶胀的方法如下:称重具有薄的截面即小于0.5英寸和重约2g的样品,并且该重量记录为W5。 Determination of swelling in a solvent of an elevated temperature as follows: weighing the sample having a thin cross-section that is less than 0.5 inches and weighing about 2g, and the weight recorded as W5. 使样品暴露于在浸没装置中的50ml IRM 903油中。 The samples were exposed to the immersion apparatus 50ml IRM 903 oil. 样品的温度维持在70℃。 Sample temperature was maintained at 70 ℃. 浸没70小时后,倾析出油并用己烷即刻洗涤样品。 After 70 hours immersion, the oil was decanted and washed with hexane instantly sample. 然后样品在80℃的真空烘箱中干燥24小时。 The samples were then in a vacuum oven at 80 ℃ dried for 24 hours. 随后冷却样品,并称取最终重量,该重量记录为W6。 Subsequently cooling the sample, the final weight were weighed, the weight is recorded as W6. 在升高的温度下的溶剂溶胀(SSS)通过下式确定:SSS=100(W6-W5)/W5。 At elevated temperature solvent swell (SSS) is determined by the following equation: SSS = 100 (W6-W5) / W5.

[00105]口型C撕裂:口型C撕裂性能按照ASTM D624的00版程序以磅力/英寸报告。 [00105] Die C Tear: Die C tear properties in accordance with ASTM D624 version 00 program to lbf / in the report. 这里的数据是峰值力,并且三个样品的平均值报告为平均数据。 The data here is the peak force, and the average value reported is the average of three samples of data. 原始数据可以被乘以0.175,以将单位从磅力/英寸转换成千牛顿/米2。 Source data may be multiplied by 0.175 to convert the units from pounds-force / inch tens N / m 2.

[00106]裤形(Trouser)撕裂:裤形撕裂性能按照ASTM D624的00版程序以磅力/英寸报告。 [00106] Trouser (Trouser) Tear: Trouser tear resistance in accordance with ASTM D624 version 00 program to lbf / in the report. 这里的数据是峰值力,并且三个样品的平均值报告为平均数据。 The data here is the peak force, and the average value reported is the average of three samples of data. 原始数据可以被乘以0.175,以将单位从磅力/英寸转换成千牛顿/米2。 Source data may be multiplied by 0.175 to convert the units from pounds-force / inch tens N / m 2.

[00107]门尼粘度:这里所使用的门尼粘度按照ASTM D1646测量,为ML(1+4)@125℃。 [00107] The Mooney viscosity: As used herein, Mooney viscosity measured in accordance with ASTM D1646, is ML (1 + 4) @ 125 ℃.

[00108]熔体流动速率和熔融指数:聚合物的熔体流动速率(MFR)和熔融指数的测定按照ASTM D1238,使用2.16kg负荷的改进1进行。 [00108] The melt index and melt flow rate: Determination of the polymer melt flow rate (MFR) and the melt index according to ASTM D1238, using a load of 2.16kg Improvement 1. 在所述方法的该版本中,一部分在试验期间被挤出的样品被收集并称重。 In this version of the method, a portion of the sample extruded during the test was collected and weighed. 样品分析在230℃下进行,采用1分钟的样品预热,以提供测试期间稳定的温度。 Samples were analyzed at 230 ℃, a 1-minute sample was preheated, in order to provide a stable temperature during the test. 表示为每分钟挤出的样品的dg数的该数据被称为MFR。 Expressed as the number of the extruded sample dg per minute This data is referred to MFR. 在备选的方法中,所述测试以相同的方式进行,除了温度为190℃。 In an alternative method, the test in the same manner, except that the temperature was 190 ℃. 该数据被称为MI@190℃。 This data is referred MI @ 190 ℃.

[00109]肖氏A硬度和肖氏D硬度:聚合物的肖氏A硬度和肖氏D硬度的测定按照ASTM D 2240进行。 [00109] The Shore A hardness and Shore D hardness: Shore A hardness of the polymer and the Shore D hardness was measured in accordance with ASTM D 2240 be. 在所述方法的该版本中,在室温下测试一部分样品。 In this version of the method, the test portion of the sample at room temperature. 在样品中产生压痕15秒钟后记录数据。 Indentation in the sample after 15 seconds of recorded data.

[00110]全同立构指数:全同立构指数按照EP 0374695A2中描述的方法进行计算。 [00110] Isotactic index: isotactic index is calculated according to the method described in EP 0374695A2. 记录所述材料的薄膜的IR光谱,并确定在997cm-1的吸光度和在973cm-1的吸光度。 IR spectra were recorded of the material of the film, and determining the absorbance at 997cm-1 and the absorbance at 973cm-1. 将997cm-1的吸光度与973cm-1的吸光度之商乘以100,得到全同立构指数。 The absorbance at 997cm-1 and 973cm-1 absorbance of the quotient multiplied by 100 to obtain isotactic index. 在确定这两个位置的吸光度时,0吸光度的位置是当在样品光束(beam)中没有分析样品存在时的吸光度。 Absorbance was determined at these two positions, the position is 0 when the absorbance did not exist when the absorbance of the sample in the analysis sample beam (beam) in.

[00111]粘度比:在辐射前和辐射后的样品上进行流变试验。 [00111] The viscosity ratio: rheological tests conducted on the samples before and after irradiation of radiation. 试验在Rheometrics ARES流变仪上使用25mm直径的平行板几何形状的板进行。 Test using 25mm diameter parallel plate geometry plate on Rheometrics ARES rheometer. 在190℃和20%的应变下从0.1至100rad/s进行小振幅振荡剪切测量。 At 190 ℃ and 20% strain were measured from small amplitude oscillatory shear 0.1 to 100rad / s. 在辐射后样品在0.1rad/s下的粘度与辐射之前的样品该粘度之比取为所述粘度比。 After radiation than the sample viscosity 0.1rad / s under radiation before the viscosity of the sample is taken as the viscosity ratio.

实施例[00112]Sunpar 150为可以从Sunoco Inc,Philadelphia,PA得到的加工油。 Example [00112] Sunpar 150 that can be obtained from Sunoco Inc, Philadelphia, PA processing oils.

[00113]Translink 37为得自Engelhard Corporation,Iselin,NJ的表面处理的高岭土。 [00113] Translink 37 is available from Engelhard Corporation, Iselin, NJ surface treatment of kaolin.

[00114]V2504、V3666、V404、ESC4292、Achieve 3854和EMPR 103是可得自ExxonMobil Chemical Co.,Houston,TX的聚烯烃。 [00114] V2504, V3666, V404, ESC4292, Achieve 3854 and EMPR 103 are available from ExxonMobil Chemical Co., Houston, TX polyolefins.

[00115]Irganox 1076是可得自Novatris Corporation的抗氧剂。 [00115] Irganox 1076 is available from Novatris Corporation antioxidant.

实施例1-具有等规聚丙烯结晶性并包括二烯(VNB)的弹性体的合成[00116]聚合在3.8升的连续搅拌釜式聚合反应器中进行,反应器装配有一个用于溶于己烷混合物中的乙烯、丙烯和二烯的混合物的进料口,和用于催化剂进料的另一个进料口。 Isotactic polypropylene and crystalline and comprising synthetic diene (VNB) elastomer [00116] Polymerization Example 1- having equal 3.8 liter continuous stirred tank polymerization reactor, a reactor equipped with a dissolved for hexane mixture mixture of ethylene, propylene and a diene feed ports, and the other for the catalyst feed inlet. 本实施例中使用的二烯是5-乙烯基-2-降冰片烯(VNB)。 Diene used in this embodiment is 5-vinyl-2-norbornene (VNB). 用倾斜浆叶双螺旋桨搅拌器以750rpm的速度搅动反应器的内容物。 Inclined blade stirrer at a speed of 750rpm double propeller agitator of the reactor contents. 聚合在聚合环境的不同区域内没有反应物或产物的组成梯度或温度梯度的情况下进行。 Where the composition gradient or temperature gradient of the polymerization in a polymerization environment in different regions of the reactants or products do not have the next. 使用进料冷冻来保持聚合温度。 Frozen using a feed to maintain the polymerization temperature. 聚合使用催化剂外消旋的二甲基二甲基甲硅烷基双(茚基)合铪和活化剂二甲基苯铵四(五氟苯基)硼酸盐的基本等摩尔的混合物引发。 Polymerization catalyst racemic dimethyl dimethylsilyl bis (indenyl) hafnium and a mixture of an activator of dimethylanilinium tetrakis (pentafluorophenyl) borate substantially equimolar initiator. 将溶解在己烷中的三乙基铝(TEA)的溶液加入聚合混合物中,用作外来水分和氧气的清除剂。 Dissolved in hexane triethylaluminum (TEA) was added to the polymerization mixture, is used as external moisture and oxygen scavenger. 清除剂进料在以下表中表示为清除剂与催化剂的摩尔比。 Scavenger feed expressed as scavengers to catalyst molar ratio in the following table. 在任何聚合条件下至少4倍停留时间后,收集并分析所得聚合物的代表性的稳态的样品。 Under any polymerization conditions at least four times after a residence time, the steady state of the sample collection and analysis of the resulting polymer representative. 聚合条件见表1-1中所示,聚合结果见表1-2中所示。 Polymerization conditions shown in Table 1-1, the polymerization results in Table 1-2 below.

表1-1 Table 1-1

表1-2 Table 1-2

实施例2-弹性体的辐射硫化[00117]实施例2中使用的基于丙烯的弹性体(″FPC″)含有15.3wt%的乙烯衍生单元,其余为丙烯衍生单元,其MFR@230℃为5.3,并且是按照以上实施例1中和EP1 223 191(其公开内容通过引用结合在此)中所描述的实验程序制备的。 Example 2 Radiation cured elastomer [00117] Example 2 using the propylene-based elastomer ("FPC") contained 15.3wt% of ethylene-derived units, the balance of propylene derived units, its MFR @ 230 ℃ 5.3 , and in accordance with the above Example 1 and EP1 223 191 are prepared as described in experimental procedure (the disclosure of which is incorporated by reference herein) of.

[00118]实施例2中使用的结晶聚合物组分(″SPC″)是Escorene4292,即一种MFR@230℃为1.5的均聚等规聚丙烯,可得自TX Houston的ExxonMobil Chemical Co.。 [00118] The crystalline polymer component used in Example 2 ("SPC") embodiment is Escorene4292, i.e. a MFR @ 230 ℃ for 1.5 homopolymeric syndiotactic polypropylene, etc., available from TX Houston of ExxonMobil Chemical Co ..

[00119]实施例2中使用的基于乙烯的聚合物(″TPC″)为Exact3024,即一种MI@190℃为4.5,密度为0.905g/cc的乙烯-己烯共聚物,可得自TX Houston的ExxonMobil Chemical Co.。 [00119] Example 2 used the ethylene-based polymer ("TPC") is Exact3024, i.e., an MI @ 190 ℃ of 4.5, a density of 0.905g / cc ethylene - hexene copolymer available from TX Houston, ExxonMobil Chemical Co ..

[00120]实施例2的各个试样中使用的聚合物组分的量在表2-1中给出。 [00120] Example weight polymer component of each sample was used in Example 2 are given in Table 2-1. 样品按以下步骤制备:只含FPC的组合物(实施例2-1至2-5)被压模成要求的几何形状。 Samples were prepared as follows: a composition containing only the FPC (Examples 2-1 to 2-5) are molded into the required geometry. FPC与TPC的共混物(实施例2-6至2-10)通过在Brabender密炼机中在185℃-220℃的控制温度下混合3分钟而制得。 A blend of FPC and TPC (Examples 2-6 to 2-10) by mixing in a Brabender mixer at a temperature of -220 ℃ 185 ℃ control for 3 minutes in the system. 高剪切辊式浆叶被用于所述混合。 High shear roller blades were used for the mixing. FPC和SPC的共混物(实施例2-11至2-15)在Haake双螺杆挤出机中在190℃-220℃范围内的温度下制备。 A blend of FPC and SPC (Examples 2-11 to 2-15) prepared in a Haake twin screw extruder at a temperature within the range -220 ℃ of 190 ℃.

[00121]然后取出共混物,并在200℃下在4英寸4英寸的模具中压制3-5分钟而成为0.004″厚的薄膜。在该阶段结束后,冷却并取出薄膜,并在进一步试验前允许其在室温下退火14天。 [00121] blend then removed, and pressed for 3-5 minutes at 200 ℃ in 4 inches 4 inches mold becomes 0.004 "thick film. After the end of this period, the film was cooled and taken out, and further Before the test, 14 days allowed to anneal at room temperature.

[00122]然后,在环境条件(室温和1个大气压)下,每个样品用来自钴-60源的γ射线辐射不同的剂量,如表2-1中所示。 [00122] Then, at ambient conditions (room temperature and 1 atm), each sample was γ-ray radiation from a cobalt-60 source different doses as shown in Table 2-1. 样品的硫化程度使用以下的萃取方法来评价。 The degree of cure of the sample was extracted using the following methods to evaluate. 将约0.4克的各样品封入400目的不锈钢筛网袋中,并在沸腾的二甲苯中萃取20小时。 Each sample of about 0.4 grams of 400 mesh stainless steel screen sealed bag and extracted in boiling xylene for 20 hours. 然后,将网袋拉出溶剂平面以上,并用回流的二甲苯洗涤数个小时。 Then, the flat bag is pulled out or more solvents, and washed with xylene at reflux for several hours. 洗涤后,在50℃下在真空烘箱中干燥所述袋,直到重量恒定(最少4小时),并冷却至室温,然后称重。 After washing, at 50 ℃ was dried in a vacuum oven the bag, until the weight is constant (minimum of 4 hours), and cool to room temperature, and then weighed. 各样品中不溶材料的wt%使用以下方程式计算:硫化%=100(W3-W1)/(W2-W1)其中,W1为空不锈钢袋的重量,W2为萃取前样品+袋的重量,W3为萃取后样品+袋的重量。 Each sample wt% insoluble material calculated using the following equation: curing% = 100 (W3-W1) / (W2-W1) wherein, W1 is the weight of the empty bag of stainless steel, W2 is the weight of the pre-extracted sample bags +, W3 + sample after extraction bag weight. 萃取后的不溶物%用于指示硫化。 Insolubles% after extraction is used to indicate vulcanization.

[00123]在辐射前和辐射后的样品上进行流变试验。 [00123] rheological tests conducted on the samples before and after irradiation of radiation. 所述流变试验在Rheometrics ARES流变仪上使用25mm直径的平行板几何形状的板进行。 The rheological tests using 25mm diameter parallel plate geometry on board Rheometrics ARES rheometer. 在190℃和20%的应变下从0.1至100rad/s进行小振幅振荡剪切测量。 At 190 ℃ and 20% strain were measured from small amplitude oscillatory shear 0.1 to 100rad / s. 在辐射后样品在0.1rad/s下的粘度与辐射之前的样品该粘度之比显示在下表中。 After the irradiation the sample prior to the sample than the viscosity of radiation 0.1rad / s under the viscosities are shown below. 样品2-3至2-5和2-8至2-10的粘度未测量,因为由于过度硫化所述薄膜样品不能被模制成用于流变试验的样品。 Samples 2-3 to 2-5 and 2-8 to 2-10 viscosity is not measured because the film due to excessive sulfide samples can not be molded samples for rheological testing. 我们预期,对于这些过度硫化的样品而言,辐射后的粘度比辐射前的粘度大得多。 We expect that, for a sample of these excessive curing, the viscosity of the radiation is much greater than the viscosity after radiation ago.

表2-1 Table 2-1

实施例3-具有等规聚丙烯结晶性并包括二烯(ENB)的弹性体的合成[00124]聚合按以下程序进行:在装配有双倾斜桨叶涡轮搅拌器的27升连续流搅拌釜反应器中,每小时加入92kg干燥己烷、34kg丙烯、1.8kg乙烯、1.1kg 5-乙叉-2-降冰片烯(ENB)。 Example 3 having a crystallinity of isotactic polypropylene and comprising synthetic diene (ENB) elastomer [00124] Polymerization according to the following procedure: In a turbine equipped with a dual pitched blade agitator 27 l continuous flow stirred tank reactor vessel, per hour of dry hexane was added 92kg, 34kg propylene, 1.8kg ethylene, 1.1kg 5- ethylidene-2-norbornene (ENB). 反应器在反应过程中被以650rpm的速度搅动,并在1600psi压力(表压)下保持液体是满的,以使聚合区中的所有区域在整个聚合过程中都具有相同的组成。 The reactor was agitated at a speed of 650rpm during the reaction, and the liquid is maintained at 1600psi full pressure (gauge pressure), so that the polymerization zone all areas throughout the polymerization process have the same composition. 将1.5610-3g二甲基二甲基甲硅烷基茚基合铪及2.4210-3g二甲基苯铵四(七氟萘基)硼酸盐的在甲苯中的催化剂溶液以6.35ml/min的速度加入以引发聚合。 The catalyst solution 1.5610-3g dimethyl dimethylsilyl indenyl hafnium and 2.4210-3g dimethylanilinium tetrakis (heptafluoronaphthyl) borate in toluene to 6.35ml / min speed was added to initiate polymerization. 在聚合过程中加入另外的三正辛基铝(TNOA)溶液以除去外来的水分。 An additional tri-n-octyl aluminum (TNOA) solution in the polymerization process to remove extraneous moisture. 聚合在59℃进行,并且在聚合期间通过加入温度为-3℃至2℃的预冷的己烷来维持所述温度。 Polymerization at 59 ℃ performed, and to maintain the temperature during the polymerization by the addition of a temperature of -3 ℃ to 2 ℃ precooled hexane. 所述聚合是有效的,并且导致形成9.5kg聚合物/小时。 The polymerization is effective, and results in the formation of polymer 9.5kg / hr. 聚合物通过两段式溶剂脱除来回收,首先使用如WO 0234795A1中所述的低临界溶液方法除去70%的溶剂,然后在LIST脱挥发分挤出机中除掉剩余溶剂。 Removal of the solvent by a two-stage polymer was recovered, 70% was removed first using a solvent such as a lower critical solution method described in WO 0234795A1, then LIST devolatilizing extruder remove residual solvent. 聚合物以主轴为约1/8至1/4英寸的颗粒形式回收。 Polymer spindle is about 1/8 to 1/4 inch particles recovered in the form. 经分析所述聚合物含12.4wt%乙烯、2.34%结合ENB,并且ML(1+4)@125℃为22。 The analysis of the polymer contains 12.4wt% ethylene, 2.34% combined with ENB, and ML (1 + 4) @ 125 ℃ 22.

[00125]该聚合的其它样品的聚合条件示于表3-1中,聚合结果示于表3-2中。 [00125] The polymerization conditions of the other samples of the polymerization are shown in Table 3-1, the polymerization results are shown in Table 3-2.

[00126]表3-1中的催化剂进料含有在甲苯中的5.7710-4Mol/L的催化剂,而活化剂进料含有在甲苯中的3.7410-4Mol/L的活化剂。 [00126] Table 3-1 catalyst feed containing toluene 5.77 10-4Mol catalyst / L, and the activator feed contained in toluene is 3.74 10-4Mol / L activator. 两种进料在最初的约60秒钟的预混合后按照以下所示的速率引入聚合反应器中。 Two feeds in the first pre-mixed for about 60 seconds after the introduction of the polymerization reactor at the rate shown below.

表3-1 Table 3-1

表3-2 Table 3-2

[00127]然后对聚合物样品3-1至3-9分析如下:在180℃-220℃的控制的温度下,将总共至少72g的聚合物在Brabender密炼机中均化3分钟。 [00127] Then the polymer samples 3-1 to 3-9 as follows: at a temperature of 180 ℃ -220 ℃ control of the polymer in the total of at least 72g Brabender mixer homogenized three minutes. 将高剪切辊式桨叶用于所述混合,并向共混物中加入约0.4gIrganox 1076。 The high shear roller blades for the mixing, and adding about 0.4gIrganox 1076 blend. 混合结束后,将所述混合物取出,并在215℃下在6″6″的模具中压制3-5分钟,制成厚度为0.25″的片。在压制结束后,将所述片冷却2.5分钟并取出,并允许其退火40-48小时。从所述片上取下要求的哑铃几何形状的试验样品,并在Instron试验机上进行评价,得到表3-3中所示的数据。 After the end of the mixing, the mixture was removed and pressed at 6 " 6" mold for 3-5 minutes at 215 ℃, having a thickness of 0.25 "sheet. After the pressing, the sheet was cooled 2.5 minute and removed, and allowed to anneal 40-48 hours. The sheet was removed from the required dumbbell geometry of the test sample, and evaluated on an Instron test machine, to obtain the data shown in Table 3-3.

表3-3 Table 3-3

[00128]聚合物的分子间溶解度分布和分子间组成分布通过本说明书中所描述的程序测量,结果在表3-4中给出。 Intermolecular [00128] The solubility between the polymer composition distribution and molecular distribution as measured by procedures described in this specification, the results are given in Table 3-4.

表3-4 Table 3-4

*未测试 * Not tested

[00129]样品的熔点和熔化热通过本说明书中所描述的DSC方法测量。 [00129] The melting point and heat of fusion of the sample is measured by DSC method described in this specification. 在下表3-5中,熔点数据的第一个数值指示主峰,第二个数值指示最高的次峰的近似位置。 Table 3-5 below, the first value indicating the peak melting point data, the second highest of the sub-peak value indicating the approximate position. mm%、立构规整度指数(m/r)和1,3插入%使用样品的13C NMR光谱确定,并且样品的全同立构指数使用聚合物的IR光谱确定。 mm%, tacticity index (m / r) and 1,3% using a sample of the insert 13C NMR spectrum is determined, and the isotactic index of the polymer sample was determined using the IR spectrum. 结果在表3-5中给出。 The results are given in Table 3-5.

表3-5 Table 3-5

实施例4-弹性体与非黑色填料的配混与硫化[00130]在以约50rpm运行的Brabender混炼机中,在180-200℃的温度下,使表4-1的组分与1000ppm Irganox 1076共混5-7分钟,直到得到匀和的混合物,并且所有的组分都分散良好。 Compounding and vulcanization Example 4 elastomer and the non-black filler [00130] In a run of about 50rpm a Brabender mixer, at a temperature of 180-200 ℃, so that the components of Table 4-1 and 1000ppm Irganox 1076 blend for 5-7 minutes until a smoothing and mixtures thereof, and all components are well dispersed. 取出所述共混的配混物,并将少量样品用于通过测量MFR@230℃分析粘度。 Remove blended with the blend, and a small amount of sample was used for analysis by measuring MFR @ 230 ℃ viscosity. 从剩余部分的样品中取220g,在辊式开炼机上与8g氧化锌、4g硬脂酸、3g硫磺、3g二硫化-2-巯基苯并噻唑(MBTS)和3g单硫化四甲基秋兰姆(TMTMS)进行配混。 Samples taken from the remaining portion of 220g, in the roll open mill and 8g zinc oxide, 4g stearic acid, 3g sulfur, 3g disulfide-2-mercapto-benzothiazole (MBTS) and tetramethylthiuram 3g single Orchids Farm (TMTMS) were compounded. 然后将该配混物轧制成光滑的片材。 The compounded composition is then rolled into a smooth sheet. 然后该配混的材料以适宜于随后进行分析的压缩模制片的形式在170℃下硫化30分钟。 In the form of compression molded sheet of material is then mixed with the formulation suitable for subsequent analysis at 170 ℃ vulcanized 30 minutes. 从所述硫化的片上取下合适几何形状的样品,得到下表4-1中所示的结果。 Remove the appropriate geometry from the sheet of the vulcanized sample, the results shown in 4-1 to give the following table.

表4-1 Table 4-1

实施例5-弹性体与黑色填料的配混和硫化[00131]在以约50rpm运行的Brabender混炼机中,在180-200℃的温度下,使表5-1的组分与1000ppm Irganox 1076共混5-7分钟,直到得到匀和的混合物,并且所有的组分都分散良好。 Example 5- elastomer compounding and vulcanization black filler [00131] In embodiments of about 50rpm in a Brabender mixer operating at a temperature of 180-200 ℃, so that the components in Table 5-1 with a total of 1000ppm Irganox 1076 mixed 5-7 minutes until a smoothing and mixtures thereof, and all components are well dispersed. 取出所述共混的配混物,并将少量样品用于通过测量MFR@230℃分析粘度。 Remove blended with the blend, and a small amount of sample was used for analysis by measuring MFR @ 230 ℃ viscosity. 从剩余部分的样品中取220g,在辊式开炼机上与8g氧化锌、4g硬脂酸、3g硫磺、3g MBTS和3g TMTMS进行配混。 220g samples taken from the remaining portion, on the roll open mill and 8g zinc oxide, 4g stearic acid, 3g sulfur, 3g MBTS and 3g TMTMS be compounded. 然后将该配混物轧制成光滑的片材。 The compounded composition is then rolled into a smooth sheet. 然后该配混的材料以适宜于随后进行分析的压缩模制片的形式在170℃下硫化30分钟。 In the form of compression molded sheet of material is then mixed with the formulation suitable for subsequent analysis at 170 ℃ vulcanized 30 minutes. 从所述硫化的片上取下合适几何形状的样品,得到下表5-1中所示的结果。 Remove the appropriate geometry from the sheet of the vulcanized sample, the results obtained 5-1 shown in the following table.

表5-1 Table 5-1

*未测定实施例6-弹性体与黑色填料、非黑色填料和高Tg增粘剂的配混与硫化[00132]在以约50rpm运行的Brabender混炼机中,在180-200℃的温度下,使表6-1的组分与1000ppm Irganox 1076共混5-7分钟,直到得到匀和的混合物,并且所有的组分都分散良好。 * Not determined Example embodiments 6- elastomer and black filler, non-black fillers and high Tg tackifier is compounded with vulcanizing [00132] In a run of about 50rpm a Brabender mixer at a temperature of 180-200 ℃ , so that the components in Table 6-1 and 1000ppm Irganox 1076 blend for 5-7 minutes, until the mixture obtained smoothing, and all components are well dispersed. 取出所述共混的配混物,并将少量样品用于通过测量MFR@230℃分析粘度。 Remove blended with the blend, and a small amount of sample was used for analysis by measuring MFR @ 230 ℃ viscosity. 从剩余部分的样品中取220g,在辊式开炼机上与8g氧化锌、4g硬脂酸、3g硫磺、3g MBTS和3g TMTMS进行配混。 220g samples taken from the remaining portion, on the roll open mill and 8g zinc oxide, 4g stearic acid, 3g sulfur, 3g MBTS and 3g TMTMS be compounded. 然后将该配混物轧制成光滑的片材。 The compounded composition is then rolled into a smooth sheet. 然后该配混的材料以适宜于随后进行分析的压缩模制片的形式在170℃下硫化30分钟。 In the form of compression molded sheet of material is then mixed with the formulation suitable for subsequent analysis at 170 ℃ vulcanized 30 minutes. 从所述硫化的片上取下合适几何形状的样品,得到下表6-1中所示的结果。 Remove the appropriate geometry from the sheet of the vulcanized sample, the results shown in 6-1 to obtain the following table.

表6-1 Table 6-1

实施例7-弹性体与黑色填料、非黑色填料和EPDM的配混与硫化[00133]在以约50rpm运行的Brabender混炼机中,在180-200℃的温度下,使表7-1的组分与1000ppm Irganox 1076共混5-7分钟,直到得到匀和的混合物,并且所有的组分都分散良好。 Example 7- elastomer and black filler, non-black fillers and compounding and vulcanization of EPDM [00133] In a run of about 50rpm a Brabender mixer, at a temperature of 180-200 ℃, so that the table 7-1 component and 1000ppm Irganox 1076 blended for 5-7 minutes, until a smoothing and mixtures thereof, and all components are well dispersed. 取出所述共混的配混物,并将少量样品用于通过测量MFR@230℃分析粘度。 Remove blended with the blend, and a small amount of sample was used for analysis by measuring MFR @ 230 ℃ viscosity. 从剩余部分的样品中取220g,在辊式开炼机上与8g氧化锌、4g硬脂酸、3g硫磺、3g MBTS和3g TMTMS进行配混。 220g samples taken from the remaining portion, on the roll open mill and 8g zinc oxide, 4g stearic acid, 3g sulfur, 3g MBTS and 3g TMTMS be compounded. 然后将该配混物轧制成光滑的片材。 The compounded composition is then rolled into a smooth sheet. 然后该配混的材料以适宜于随后进行分析的压缩模制片的形式在170℃下硫化30分钟。 In the form of compression molded sheet of material is then mixed with the formulation suitable for subsequent analysis at 170 ℃ vulcanized 30 minutes. 从所述硫化的片上取下合适几何形状的样品,得到下表7-1中所示的结果。 Remove the appropriate geometry from the sheet of the vulcanized sample, the results obtained 7-1 shown in the following table.

表7-1 Table 7-1

实施例8-硫化的纤维、薄膜和模制物件的制造[00134]在以约50rpm运行的Brabender混炼机中,在180-200℃的温度下,使表8-1的组分与1000ppm Irganox 1076共混5-7分钟,直到得到匀和的混合物,并且所有的组分都分散良好。 Example 8 Manufacturing vulcanized fiber, film and molded article [00134] In embodiments of about 50rpm in a Brabender mixer operating at a temperature of 180-200 ℃, so that the components in Table 8-1 and 1000ppm Irganox 1076 blend for 5-7 minutes until a smoothing and mixtures thereof, and all components are well dispersed. 取出所述共混的配混物,并将少量样品用于通过测量MFR@230℃分析粘度。 Remove blended with the blend, and a small amount of sample was used for analysis by measuring MFR @ 230 ℃ viscosity.

表8-1 Table 8-1

[00135]通过在约230℃的温度下经具有圆柱形挤出物横截面的模头挤出熔融的混合物而得到纤维。 [00135] through at a temperature of about 230 ℃ via a cylindrical extrudate having a cross-section of the die of the molten mixture was extruded to obtain fiber. 纤维段(fiber segment)的最小长度为10cm。 Fiber segments (fiber segment) of the minimum length of 10cm. 所述纤维段的样品通过在室温下在不含水分的气氛中暴露于二氯化硫20小时而被硫化。 Samples of the fiber segments through water at room temperature without exposure to the atmosphere for 20 hours sulfur dichloride is vulcanized. 从样品8-1、8-2、8-3、8-4、8-5、8-6和8-7得到的硫化的纤维段分别被标记为样品8-FB1X、8-FB2X、8-FB3X、8-FB4X、8-FB5X、8-FB6X和8-FB7X。 From the sample 8-1,8-2,8-3,8-4,8-5,8-6 and 8-7 obtained vulcanized fiber segments are marked as sample 8-FB1X respectively, 8-FB2X, 8- FB3X, 8-FB4X, 8-FB5X, 8-FB6X and 8-FB7X. 分析所述纤维样品的拉伸伸长率、溶解度和回复性能,得到下表8-2中所示的结果。 Tensile elongation of the fiber sample analysis, solubility and recovery properties, obtained as shown in the following table 8-2 results.

表8-2 Table 8-2

[00136]通过在扁平口模(flat die)中在约230℃的温度下压缩模塑熔融的混合物而得到薄膜。 [00136] by the flat die (flat die) at a temperature of about 230 ℃ compression molding the mixture to obtain a molten film. 薄膜段的最小长度和宽度为10cm。 The minimum length and width of the film section is 10cm. 所述薄膜段的样品通过在室温下在不含水分的气氛中暴露于二氯化硫20小时而被硫化。 Samples of the film segments through water at room temperature without exposure to an atmosphere of sulfur dichloride was cured for 20 hours. 从样品8-1、8-2、8-3、8-4、8-5、8-6和8-7得到的硫化的薄膜段分别被标记为样品8-FL1X、8-FL2X、8-FL3X、8-FL4X、8-FL5X、8-FL6X和8-FL7X。 8-1,8-2,8-3,8-4,8-5,8-6 film segment from the sample vulcanized and 8-7 Samples obtained were labeled as 8-FL1X respectively, 8-FL2X, 8- FL3X, 8-FL4X, 8-FL5X, 8-FL6X and 8-FL7X. 分析所述薄膜样品的拉伸伸长率、溶解度和回复性能,得到下表8-3中所示的结果。 Tensile elongation of the film sample analysis, solubility and recovery properties, as shown in 8-3 to give the results of the following table.

表8-3 Table 8-3

[00137]通过在模头中在约230℃的温度下压缩模塑熔融的混合物而得到模制物件。 [00137] By a die at a temperature of about 230 ℃ compression molding the molten mixture obtained molded articles. 所述模制物件的样品通过在室温下在不含水分的气氛中暴露于二氯化硫20小时而被硫化。 Samples of the molded article by the water at room temperature without exposure to an atmosphere of sulfur dichloride was cured for 20 hours. 从样品8-1、8-2、8-3、8-4、8-5、8-6和8-7得到的硫化的模制物件分别被标记为样品8-M1X、8-M2X、8-M3X、8-M4X、8-M5X、8-M6X和8-M7X。 From the sample 8-1,8-2,8-3,8-4,8-5,8-6 and molded article obtained by vulcanizing 8-7 are labeled Sample 8-M1X respectively, 8-M2X, 8 -M3X, 8-M4X, 8-M5X, 8-M6X and 8-M7X. 从所述硫化的模制物件上取下试样拉伸条。 Remove the strip tensile specimens from the vulcanization of the molded article. 分析所述试样拉伸条的拉伸伸长率、溶解度和回复性能,得到下表8-4中所示的结果。 Analyzing said sample stretched strip tensile elongation, solubility and recovery properties, as shown in 8-4 to give the results of the following table.

表8-4 Table 8-4

实施例9-弹性体与黑色填料、非黑色填料和高分子量EPDM的配混与硫化[00138]在以约50rpm运行的Brabender混炼机中,在180-200℃的温度下,使表9-1的组分与1000ppm Irganox 1076共混5-7分钟,直到得到匀和的混合物,并且所有的组分都分散良好。 9- elastomer compounding example embodiment with black filler, non-black filler and high molecular weight EPDM with the cure [00138] In a run of about 50rpm a Brabender mixer, at a temperature of 180-200 ℃, so that the table 9- component of Irganox 1076 and 1000ppm 1 blended for 5-7 minutes, until a smoothing and mixtures thereof, and all components are well dispersed. 取出所述共混的配混物,并将少量样品用于通过测量MFR@230℃分析粘度。 Remove blended with the blend, and a small amount of sample was used for analysis by measuring MFR @ 230 ℃ viscosity. 从剩余部分的样品中取220g,在辊式开炼机上与8g氧化锌、4g硬脂酸、3g硫磺、3g MBTS和3g TMTMS进行配混。 220g samples taken from the remaining portion, on the roll open mill and 8g zinc oxide, 4g stearic acid, 3g sulfur, 3g MBTS and 3g TMTMS be compounded. 然后将该配混物轧制成光滑的片材。 The compounded composition is then rolled into a smooth sheet. 然后该配混的材料以适宜于随后进行分析的压缩模制片的形式在170℃下硫化30分钟。 In the form of compression molded sheet of material is then mixed with the formulation suitable for subsequent analysis at 170 ℃ vulcanized 30 minutes. 从所述硫化的片上取下合适几何形状的样品,得到下表9-1中所示的结果。 Remove the sample from the appropriate geometry of the on-chip vulcanized to give 9-1 as shown in the following table results.

表9-1 Table 9-1

实施例10[00139]按照以下的通用程序制备4个样品。 Example 10 [00139] The following general procedure 4 sample preparation. 将含有基于丙烯的弹性体(″FPC″)和结晶的聚合物组分(″SPC″)的熔融共混的树脂体系进料到纤维纺丝挤出机中。 Containing the propylene-based elastomer ("FPC") and a crystalline polymer component ("SPC") melt blending the resin system is fed into the fiber spinning extruder. 纤维纺丝在常规的纤维纺丝线中在POY(部分取向纱)模式下进行。 In a conventional fiber spinning line fiber spinning performed under POY (partially oriented yarn) mode. 该纤维纺丝线配备有2英寸直径的单螺杆挤出机。 The fiber spinning line is equipped with a 2 inch diameter single screw extruder. 将来自挤出机的熔融聚合物进料到熔体泵中,该泵将所述熔融聚合物输送到喷丝嘴。 The molten polymer from the extruder is fed into a melt pump, the pump of the molten polymer supplied to the spinneret. 该喷丝嘴含有72个毛细管,每个毛细管的直径为0.6mm。 The spinneret contained 72 capillaries, each capillary having a diameter of 0.6mm. 离开喷丝嘴的熔融聚合物被60的、速度为60ft/min的冷空气骤冷。 The molten polymer leaving the spinneret is 60, the speed of 60ft / min cool air quenched. 已被骤冷的纤维被机械辊(或导丝轮)卷取,该机械辊(或导丝轮)的速度可以在0-5000m/min的范围内变化。 The quenched fiber was mechanically roll (or godet) winding, the machine roll (or godet) velocity may vary within the scope 0-5000m / min of. 为了测量样品的最大纺丝速度,输出量恒定保持在0.6克/孔/分钟。 To measure the maximum spinning speed of the sample, the amount of output constant at 0.6 g / hole / min. 逐渐增加导丝轮的速度,这将会增加纤维的速度并减小纤维的直径。 Gradually increasing the speed of godet, which will increase the speed and reduce the fiber diameter of the fiber. 增加速度直至发生纤维断裂。 Increase the speed until the occurrence of fiber breakage. 发生纤维断裂时的速度是所述样品的最大纺丝速度。 Fiber breakage occurs when the speed is the maximum spinning speed of the sample. 重复同样的过程三次,记录下平均读数。 The same procedure was repeated three times, the average reading recorded.

表10 Table 10

*FPC是含15wt%乙烯的20MFR的丙烯-乙烯共聚物。 * FPC is a propylene containing 15wt% of ethylene 20MFR - ethylene copolymer.

**SPC1是PP 3155,即一种可商购自TX Houston的ExxonMobilChemical Company的36MFR的等规丙烯均聚物。 ** SPC1 is PP 3155, ExxonMobilChemical i.e., a commercially available from the Company TX Houston 36MFR isotactic propylene homopolymer.

***SPC2是PP3505G,即一种可商购自TX Houston的ExxonMobilChemical Company的400MFR的丙烯均聚物。 *** SPC2 is PP3505G, i.e. a propylene commercially available from TX Houston of ExxonMobilChemical Company of 400MFR homopolymer.

实施例11[00140]按照如下方法生产纺粘型织物。 Example 11 [00140] The following method for producing a spunbonded fabric of Example. 所述纺粘系统使用由德国Troisdorf的Reifenhauser GmbH制造的1米宽的单纺粘梁(beam)生产线。 The spunbond system used by the Reifenhauser GmbH Troisdorf, Germany made a one-meter wide spunbond beam (beam) production line. 将熔融共混或干混的树脂体系进料到所述纺粘系统的挤出机中。 The melt blended resin system or dry blending of the spunbond system fed to an extruder. 输出量通常为0.2-0.3克/孔/分钟,取决于要求的纤维尺寸。 Output is typically 0.2-0.3 g / hole / min, depending on the requirements of the fiber size. 加工条件与使用常规聚丙烯的纺粘制造相似。 Processing conditions with the use of conventional polypropylene spunbond manufacturing similar.

[00141]生产了6个样品。 [00141] produced six samples. 样品11-1和11-2的基于丙烯的弹性体(FPC)是VM2210,即一种含有15wt%的乙烯、MFR@230℃为22的基于丙烯的弹性体。 Samples 11-1 and propylene-based elastomer (FPC) 11-2 is VM2210, i.e., containing 15wt% of ethylene, MFR @ 230 ℃ propylene-based elastomer 22. VM2210可商购自TX Houston的ExxonMobilChemicalCo.。 VM2210 commercially available from TX Houston's ExxonMobilChemicalCo .. 在样品11-3至11-12中,在生成纤维和织物之前,通过在单螺杆挤出机中熔融共混聚合物组分并造粒,以产生含有均匀共混物的颗粒,来制备聚合物共混物。 In Sample 11-3 to 11-12, before generating fibers and fabrics, by melt blending the polymer components in a single screw extruder and pelletized to produce a homogeneous blend of particles containing, produced by polymerization of blends thereof. 样品11-3至11-12的基于丙烯的弹性体(FPC)按照上面实施例3中所给出的方法制备,并具有如表11-1中所示的组成。 Samples 11-3 to 11-12 of the propylene-based elastomer (FPC) was prepared according to the above method given in Example 3 embodiment, and having the composition as shown in Table 11-1. 样品11-3至11-12的结晶丙烯聚合物(SPC)是ESC PP3155。 Samples of the crystalline propylene polymer (SPC) 11-3 to 11-12 are ESC PP3155.

[00142]所述纺粘系统的挤出机将均化的熔融聚合物输送至熔体泵,该熔体泵输送熔融聚合物至纺丝梁。 [00142] The spunbond extruder system homogenized molten polymer delivered to the melt pump, the pumping of the molten polymer to the melt spinning beam. 所述纺丝梁具有约1米宽的长方形喷丝板,该喷丝板具有约4000个孔。 The spinning beam has about 1 meter wide rectangular spinnerets, the spinneret having about 4000 holes. 每个孔的直径为0.6mm。 The diameter of each hole is 0.6mm. 离开喷丝板的熔融聚合物线被冷空气骤冷,并被拉成细纤维。 Molten polymer strand leaving the spinneret were quenched with cold air, and drawn into fine fibers. 已被骤冷并高度拉曳的纤维被堆积在一个移动的多孔织物上,形成非织造织物对。 Has been quenched and highly pulling fibers are deposited on a moving porous web, to form a nonwoven fabric pair. 所述未粘合的织物经过被加热至约200的压延机辊。 The unbonded fabric through the calender rolls are heated to about 200 of. 随着所述织物经过压延机的辊隙,纤维在单一步骤中被退火,并且纤维的弹性被提高。 With the fabric through a calender nip, the fiber is annealed in a single step, and the elastic fibers is improved. 熔体温度是450,压延机辊压力为100磅/线性英寸。 The melt temperature is 450, calender roll pressure of 100 lbs / linear inch.

表11-1 Table 11-1

表11-2织物机条件 Table 11-2 fabric machine condition

表11-3无纺布性质 Table 11-3 non-woven nature

实施例12:用二氯化硫交联织物[00143]将得自实施例11的以下织物样品暴露于蒸气形式的二氯化硫60分钟。 Example 12: crosslinked with sulfur dichloride Fabrics [00143] The obtained 60 minutes following fabric samples from Example 11 is exposed to the vapor form of sulfur dichloride. 然后在真空下将样品加热至100℃以完成交联,并除去未反应的反应物和副产物。 The sample is then heated under vacuum to 100 ℃ to complete crosslinking, and removal of reactants and byproducts unreacted. 3小时后,取出样品并称重。 After 3 hours, the sample was removed and weighed. 这些重量在表12的第2栏中给出。 These weights are given in column 2 of Table 12.

[00144]然后用回流的二甲苯萃取样品120分钟。 [00144] Then the sample was extracted with refluxing xylene for 120 minutes. 然后用回流的二甲苯萃取样品120分钟。 Then the sample was extracted with refluxing xylene for 120 minutes. 将残余物从萃取液中取出,并在130℃下在真空烘箱中干燥,得到残余物,其重量示于表12中的第3栏。 The residue was removed from the extract, and dried in a vacuum oven at 130 ℃, to give a residue, which weight is shown in Table 12, column 3. 假设所有样品都是85%的FPC和15%的SPC,并且假设所述SPC未被交联,因此无论FPC的交联程度如何SPC都会被二甲苯萃取出来,这样来确定二甲苯萃取后不溶FPC的量。 Assuming that all the samples are 85% FPC and 15% SPC, and assume that the SPC is not cross-linked, and therefore regardless of the degree of crosslinking of the FPC will be extracted SPC xylene, thus to determine xylene extraction insoluble FPC amount. 交联的程度在表12中第4栏给出。 The extent of crosslinking in column 4 of Table 12 are given.

表12 Table 12

实施例13:用过氧化物交联织物[00145]在室温下将6g Trigonox C溶解在600g己烷中。 Example 13: with a peroxide crosslinking Fabrics [00145] A mixture of 6g Trigonox C was dissolved in 600g hexane. 将得自实施例11的12英寸12英寸的织物样品用该溶液饱和,并移除过量溶液。 Fabric samples 12 inches 12 inches obtained from Example 11, saturated with the solution, and removing excess solution. 该湿的织物被空气干燥,并在真空烘箱中暴露在120℃的温度下2小时。 The wet fabric is air dried, and exposed at a temperature of 120 ℃ for 2 hours in a vacuum oven. 在该操作结束后,称重织物,结果示于表13中第2栏。 At the end of this operation, the fabric weighing results are shown in Table 13, column 2. 我们估计每个织物含有0.3g过氧化物。 We estimate that each fabric contains 0.3g peroxide.

[00146]然后用回流的二甲苯萃取样品120分钟。 [00146] Then the sample was extracted with refluxing xylene for 120 minutes. 将残余物取出,并在130℃下在真空烘箱中干燥,得到残余物,其重量示于表13中的第3栏。 The residue was taken out, and dried in a vacuum oven at 130 ℃, to give a residue, which weight is shown in Table 13, column 3. 假设所有样品都是85%的FPC和15%的SPC,并且假设所述SPC未被交联,因此无论FPC的交联程度如何SPC都会被二甲苯萃取出来,这样来确定交联的程度。 Assuming that all the samples are 85% FPC and 15% SPC, and assume that the SPC is not cross-linked, and therefore regardless of the degree of crosslinking of the FPC will be extracted SPC xylene, and to determine the degree of crosslinking. 交联的程度在表13中第4栏给出。 The extent of crosslinking in column 4 of Table 13 are given.

表13 Table 13

实施例14:交联薄膜[00147]按照上面实施例3中的方法制备含13.5wt%的乙烯、2.1wt%的5-乙叉-2-降冰片烯(ENB)、并且MFR@230℃为25的基于丙烯的弹性体(FPC)。 Crosslinked film [00147] Preparation of ethylene containing 13.5wt% of the above embodiment according to the method of Example 3, 2.1wt% 5-ethylidene-2-norbornene (ENB), and MFR @ 230 ℃ was: Example 14 propylene-based elastomer 25 (FPC). 然后将该基于丙烯的弹性体(FPC)与ESC PP 3155(SPC)在约180-200℃的温度下,在以约50rpm速度运行的Banbury密炼机中共混。 Then with ESC PP 3155 (SPC) at a temperature of about 180-200 ℃ of, Banbury at about 50rpm speed running mixer blending the propylene-based elastomer (FPC). 所述基于丙烯的弹性体与ESC PP 3155的比为90/10。 The propylene-based elastomer with ESC PP 3155 90/10 ratio. 将混合物冷却并造粒,然后按照表14-1中所示的条件在3段式6″宽模头的Killion单螺杆挤出机上将其流延成为片膜。然后将该膜送到冷的辊上,并在辊上卷取,以供进一步测量和分析。得到了4.5和11密耳(1密耳=1/1000英寸)厚度的薄膜。 The mixture was cooled and granulated, and then as shown in Table 14-1 in a condition in 3 sections 6 "wide die Killion single screw extruder which will be cast into a sheet membrane. The film was then sent to the cold of roller, and the take-up roll, for further measurement and analysis. 4.5 and the obtained thin film 11 mils (1 mil = 1/1000 inches) thickness.

[00148]将薄膜在NJ Cranbury的E-Beam Services,Inc.暴露于电子束辐射。 [00148] The film NJ Cranbury the E-Beam Services, Inc. Exposed to electron beam radiation. 辐射剂量设定为三个不同的水平:5、10和20兆拉德。 Radiation dose is set to three different levels: 5, 10 and 20 Mrad. 通过回流的二甲苯萃取得到了11密耳厚薄膜辐射后的交联程度。 By refluxing xylene extraction degree of crosslinking was 11 mil thick film after irradiation. 假设所有样品都是90%的FPC和10%的SPC,并且假设所述SPC未被交联,因此无论FPC的交联程度如何SPC都会被二甲苯萃取出来,这样来确定交联的程度。 Assuming that all the samples are 90% FPC and 10% SPC, and assume that the SPC is not cross-linked, and therefore regardless of the degree of crosslinking of the FPC will be extracted SPC xylene, and to determine the degree of crosslinking. 交联的程度在表14-2中给出。 The extent of crosslinking is given in Table 14-2.

表14-1 Table 14-1

表5-2 Table 5-2

[00149]包括优先权文件的所有专利、测试方法及其它在此所引的文件全部通过引用而结合,至这种公开内容与本发明不矛盾的程度和为了其中这种结合被允许的所有权限。 [00149] All patents, test methods including priority documents and other documents cited herein all incorporated by reference to this disclosure is not inconsistent with the present invention, and all rights to the degree in which such incorporation is permitted in .

[00150]尽管本发明的示例性实施方案已被具体地描述,应该指出,各种其它改变对本领域技术人员来说是明显的,并且可以被本领域技术人员在不背离本发明精神和范围的情况下容易地做出。 [00150] Although the exemplary embodiments of the invention have been specifically described, it should be noted that various other changes to the skilled artisan is apparent, and may be skilled in the art without departing from the spirit and scope of the invention readily made case. 因此,所附权利要求书的范围不打算局限于实施例及这里所做的说明,相反,所述权利要求书应被理解为包括了本发明中存在的可取得专利权新颖性的全部特征,包括那些被本发明所属领域技术人员视为其等同物的全部特征。 Accordingly, the scope of the appended claims are not intended to Examples and limited to the embodiment described herein made, on the contrary, the book of the claims should be understood to include the present invention may be present in all the patentable novelty characteristics, including all features that are considered the present invention to those skilled in the equivalents thereof.

[00151]当在此列出数字的低限和数字的高限时,从任何低限至任何高限的范围都被想到。 [00151] When the numbers listed in this low limit and high limit numbers from any lower limit to any upper limit of the range have been thought of.

Referenced by
Citing PatentFiling datePublication dateApplicantTitle
CN102264804B10 Dec 20093 Jul 2013埃克森美孚化学专利公司Process for forming polymer blends
CN104883916A *17 Dec 20132 Sep 2015埃克森美孚化学专利公司Footwear sole comprising a propylene-based elastomer, footwear comprising said sole, and methods of making them
Classifications
International ClassificationC08F210/18, C08F8/00, C08L23/16, C08F4/659, C08F210/06
Cooperative ClassificationY10T442/678, A43B13/04, C08F210/18, C08F4/65908, C08F210/06
European ClassificationC08F210/18, C08F210/06
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