CN110352129B - 屋面膜、制造其的组合物和方法 - Google Patents
屋面膜、制造其的组合物和方法 Download PDFInfo
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- CN110352129B CN110352129B CN201780085960.4A CN201780085960A CN110352129B CN 110352129 B CN110352129 B CN 110352129B CN 201780085960 A CN201780085960 A CN 201780085960A CN 110352129 B CN110352129 B CN 110352129B
- Authority
- CN
- China
- Prior art keywords
- silane
- roofing membrane
- polyolefin
- polyolefin elastomer
- aspects
- Prior art date
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- 239000012528 membrane Substances 0.000 title claims abstract description 159
- 238000000034 method Methods 0.000 title claims description 70
- 239000000203 mixture Substances 0.000 title description 123
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 152
- 229910000077 silane Inorganic materials 0.000 claims abstract description 151
- 229920006124 polyolefin elastomer Polymers 0.000 claims abstract description 133
- 239000003063 flame retardant Substances 0.000 claims abstract description 25
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000007906 compression Methods 0.000 claims abstract description 18
- 230000006835 compression Effects 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 229920000098 polyolefin Polymers 0.000 claims description 133
- 239000003054 catalyst Substances 0.000 claims description 47
- 229920001112 grafted polyolefin Polymers 0.000 claims description 44
- 238000009833 condensation Methods 0.000 claims description 39
- 230000005494 condensation Effects 0.000 claims description 39
- 238000004132 cross linking Methods 0.000 claims description 28
- 239000003999 initiator Substances 0.000 claims description 27
- 229920001971 elastomer Polymers 0.000 claims description 26
- 239000000806 elastomer Substances 0.000 claims description 25
- 230000008569 process Effects 0.000 claims description 24
- 239000003431 cross linking reagent Substances 0.000 claims description 22
- 229920002397 thermoplastic olefin Polymers 0.000 claims description 22
- 238000003490 calendering Methods 0.000 claims description 21
- 238000012360 testing method Methods 0.000 claims description 6
- 230000009477 glass transition Effects 0.000 claims description 3
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- -1 styrene-ethylene-butylene-styrene Chemical class 0.000 description 45
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- 239000000126 substance Substances 0.000 description 13
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- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 12
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 12
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- 125000004432 carbon atom Chemical group C* 0.000 description 10
- 230000035882 stress Effects 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 239000004971 Cross linker Substances 0.000 description 8
- 125000000217 alkyl group Chemical group 0.000 description 8
- 238000001125 extrusion Methods 0.000 description 8
- 229920001519 homopolymer Polymers 0.000 description 8
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 8
- 239000001993 wax Substances 0.000 description 8
- 239000004743 Polypropylene Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 7
- 239000000155 melt Substances 0.000 description 7
- 239000000178 monomer Substances 0.000 description 7
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- 239000004416 thermosoftening plastic Substances 0.000 description 7
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 6
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- 239000000654 additive Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 6
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- 239000000347 magnesium hydroxide Substances 0.000 description 5
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- 238000012545 processing Methods 0.000 description 5
- 150000003254 radicals Chemical class 0.000 description 5
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- 125000005372 silanol group Chemical group 0.000 description 5
- 229920006342 thermoplastic vulcanizate Polymers 0.000 description 5
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- XQBCVRSTVUHIGH-UHFFFAOYSA-L [dodecanoyloxy(dioctyl)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCCCCCC)(CCCCCCCC)OC(=O)CCCCCCCCCCC XQBCVRSTVUHIGH-UHFFFAOYSA-L 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 4
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 4
- 229920002554 vinyl polymer Polymers 0.000 description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 101000666896 Homo sapiens V-type immunoglobulin domain-containing suppressor of T-cell activation Proteins 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 102100038282 V-type immunoglobulin domain-containing suppressor of T-cell activation Human genes 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 3
- 150000001343 alkyl silanes Chemical class 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000000113 differential scanning calorimetry Methods 0.000 description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 3
- IJJVMEJXYNJXOJ-UHFFFAOYSA-N fluquinconazole Chemical compound C=1C=C(Cl)C=C(Cl)C=1N1C(=O)C2=CC(F)=CC=C2N=C1N1C=NC=N1 IJJVMEJXYNJXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 3
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- 239000011572 manganese Substances 0.000 description 3
- 239000012968 metallocene catalyst Substances 0.000 description 3
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- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 3
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- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 description 3
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- ODBCKCWTWALFKM-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhex-3-yne Chemical compound CC(C)(C)OOC(C)(C)C#CC(C)(C)OOC(C)(C)C ODBCKCWTWALFKM-UHFFFAOYSA-N 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
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Images
Classifications
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Abstract
提供一种屋面膜及其制造方法。该屋面膜包括具有阻燃剂和密度小于0.90g/cm3的第一硅烷交联聚烯烃弹性体的顶层;稀松布层;和具有阻燃剂和密度小于0.90g/cm3的第二硅烷交联聚烯烃弹性体的底层。该屋面膜的顶层和底层都表现出根据ASTM D 395(22hrs@70℃)测得的大约5.0%至大约35.0%的压缩变定。
Description
公开领域
本公开总体上涉及可用于形成热塑性屋面膜(roofing membranes)的组合物,更特别涉及用于形成热塑性屋面膜的硅烷接枝聚烯烃弹性体组合物和制造这些组合物和屋面膜的方法。
公开背景
热塑性屋面膜可以是单层或可由多层构成并可在屋面膜的任何两层之间的中心含有加强织物或稀松布加强材料。屋面膜中的各个层需要表现出各种不同的材料性质以适合用在屋面,在此该材料会暴露于阳光和各要素。聚合物层的材料性质应该表现出良好的附着力、抗紫外线性、耐候性(耐久性)、阻燃性、挠性、耐化学性和长寿命。此外,屋面膜应该优选能够形成热风焊缝。
许多不同的聚合物体系可供用于屋面膜。最常用的聚合物体系包括热塑性聚烯烃(TPO)、乙烯丙烯二烯单体(EPDM)和聚氯乙烯(PVC)。根据所选材料,通常观察到不同的优点和缺点。TPO膜广泛可得、价格实惠并通常白,但在暴露于高热和/或太阳紫外线辐射时容易变质。EPDM膜由易得的EPDM合成橡胶制成,但制成的所有EPDM屋面膜的大约95%是黑色的,而联邦和州建筑监管机构正开始推广白色屋面膜。最后,PVC膜广泛可得并提供优异的穿刺性、热焊接性、可着色性和耐热性,但这些膜在制造上昂贵并受困于由不同制造商生产时的性质变异性。
考虑到用于制造屋面膜的各种TPO、EPDM和PVC材料的优点和缺点,制造商需要开发制造更简单、具有更低生产变异性、重量更轻和颜色更浅并经更长时间具有优异耐久性的屋面膜的新聚合物组合物和方法。公开概述
根据本公开的一个方面,公开了一种屋面膜。该单合叠屋面膜(single plyroofing membrane)包括包含阻燃剂和具有小于0.90g/cm3的密度的第一硅烷交联聚烯烃弹性体的顶层;稀松布(scrim)层;和包含阻燃剂和具有小于0.90g/cm3的密度的第二硅烷交联聚烯烃弹性体的底层。该单合叠屋面膜的顶层和底层都表现出根据ASTM D 395(22hrs@70℃)测得的大约5.0%至大约35.0%的压缩变定。
根据本公开的另一方面,提供了一种制造单合叠屋面膜的方法。所述方法包括:挤出第一硅烷可交联聚烯烃弹性体以形成顶层;挤出第二硅烷可交联聚烯烃弹性体以形成底层;将稀松布层压延在顶层和底层之间以形成未固化屋面膜元件;和使所述未固化屋面膜元件中的顶层和底层的硅烷可交联聚烯烃弹性体在固化温度和固化湿度下交联以形成单合叠屋面膜。所述单合叠屋面膜的顶层和底层都表现出根据ASTM D 395(22hrs@70℃)测得的大约5.0%至大约35.0%的压缩变定。
根据本公开的再一方面,提供了一种制造高负荷阻燃热塑性聚烯烃(TPO)屋面膜的方法。所述方法包括:将硅烷接枝聚烯烃弹性体、阻燃剂和缩合催化剂添加到反应性单螺杆挤出机中以产生硅烷可交联聚烯烃弹性体;压延所述硅烷可交联聚烯烃弹性体以形成顶层和底层;将稀松布层压延在顶层和底层之间以形成未固化屋面膜元件;和使所述未固化屋面膜元件中的顶层和底层的硅烷可交联聚烯烃弹性体在环境温度和环境湿度下交联以形成热塑性聚烯烃(TPO)屋面膜。所述热塑性聚烯烃(TPO)屋面膜的顶层和底层都表现出根据ASTM D 395(22hrs@70℃)测得的大约5.0%至大约35.0%的压缩变定。
本领域技术人员在研究下列说明书、权利要求书和附图后会理解和认识到本公开的这些和其它方面、目的和特征。
附图简述
在附图中:
图1是根据本公开的一些方面的屋面膜的横截面视图;
图2是用于制造根据本公开的一些方面的硅烷交联聚烯烃弹性体的示意性反应路径;
图3是使用根据本公开的一些方面的两步Sioplas法用硅烷交联聚烯烃弹性体制造单合叠屋面膜的方法的流程图;
图4A是根据本公开的一些方面的反应性双螺杆挤出机的示意性横截面视图;
图4B是根据本公开的一些方面的单螺杆挤出机的示意性横截面视图;
图5是使用根据本公开的一些方面的单步Monosil法用硅烷交联聚烯烃弹性体制造单合叠屋面膜的方法的流程图;
图6是根据本公开的一些方面的反应性单螺杆挤出机的示意性横截面视图;
图7是图解与常规EPDM化合物比较的根据本公开的各方面的硅烷交联聚烯烃弹性体的应力/应变行为的曲线图;
图8是适用于根据本公开的各方面的屋面膜的示例性硅烷交联聚烯烃弹性体和对比EPDM交联材料的弛豫图(relaxation plot);且
图9是适用于屋面膜的示例性硅烷交联聚烯烃弹性体和对比EPDM交联材料的压缩变定图。
实施方案的详述
对本文中的描述而言,术语“上”、“下”、“右”、“左”、“后”、“前”、“垂直”、“水平”及其派生词应该是涉及图1中所示的本公开的屋面膜。但是,要理解的是,除非明确地作出相反的规定,该装置可呈现各种替代性的朝向和步骤顺序。还要理解的是,附图中所示和下列说明书中描述的具体装置和方法仅是所附权利要求书中规定的本发明的概念的示例性实施方案。因此,除非权利要求书明确地另行规定,与本文中公开的实施方案相关的具体尺寸和其它物理特征不应被视为限制。
本文中公开的所有范围包括列举的端点并可独立地组合(例如,“2至10”的范围包括端点2和10和所有中间值)。本文中公开的范围的端点和任何值不限于精确范围或值;它们足够不精确以包括接近这些范围和/或值的值。
被“大约”和“基本”之类的术语修饰的值不限于指定的精确值。近似语可对应于用于测量该值的仪器的精度。修饰词“大约”也应被认为公开了由两个端点的绝对值规定的范围。例如,短语“大约2至大约4”也公开了范围“2至4”。
本文所用的术语“和/或”当用于两个或更多个项目的名单时是指所列项目的任一个可独自使用,或可使用两个或更多个所列项目的任何组合。例如,如果组合物被描述为含有组分A、B和/或C,则该组合物可含有仅A;仅B;仅C;A和B的组合;A和C的组合;B和C的组合;或A、B和C的组合。
参考图1,公开了单合叠屋面膜10。单合叠屋面膜10包括具有阻燃剂和密度小于0.90g/cm3的第一硅烷交联聚烯烃弹性体的顶层14;稀松布层26;和具有阻燃剂和密度小于0.90g/cm3的第二硅烷交联聚烯烃弹性体的底层38。该单合叠屋面膜的顶层和底层都表现出根据ASTM D 395(22hrs@70℃)测得的大约5.0%至大约35.0%的压缩变定。
TPO屋面膜必须表现出根据TPO屋面膜的ASTM规范概述的至少下列机械性质:1)拉伸强度(CD和MD)大于10MPa;2)致断伸长(CD和MD)大于500%;3)弹性模量(CD和MD)小于100MPa;和4)根据EN ISO 11925-2表面暴露试验测得的分类D的阻燃等级。
再参考图1,提供了单合叠屋面膜10的横截面视图。单合叠屋面膜10包括具有第一和第二表面18、22的顶层14。稀松布层26(也称为稀松布26)具有第三和第四表面30、34,其中稀松布26的第三表面30结合到顶层14的第二表面22上。单合叠屋面膜10另外包括具有第五和第六表面42、46的底层38,其中底层38的第五表面42结合到稀松布26的第四表面34上。
安置在顶层和底层14、38之间的稀松布层26可充当屋面膜中的加强材料,因此增加其结构完整性。可用于稀松布层26的材料可包括例如机织织物和/或非织造物、玻璃纤维和/或聚酯。在一些方面中,可用于稀松布层26的附加材料可包括合成材料,如芳族聚酰胺、KEVLARTM、TWARONTM、聚酰胺、聚酯、RAYONTM、NOMEXTM、TECHNORATM或其组合。在一些方面中,稀松布层26可包括芳族聚酰胺、聚酰胺和/或聚酯。在一些方面中,稀松布层26的韧度可为大约100至大约3000旦。在另一些方面中,稀松布层26可具有大约500至大约1500旦的韧度。在再一些方面中,稀松布层26可具有大约1000旦的韧度。在一些方面中,稀松布层26可具有大于大约14kN/米(80磅力/英寸)的拉伸强度。在另一些方面中,稀松布层26可具有大于大约10kN/米、大于大约15kN/米、大于大约20kN/米或大于大约25kN/米的拉伸强度。根据最终单合叠屋面膜10的所需性质,稀松布层26可视需要改变以适应特定的屋面膜设计。本领域普通技术人员会认识到可以改变这些特征而不背离本公开。
本文中公开的单合叠屋面膜10可具有各种不同尺寸。在一些方面中,单合叠屋面膜10可具有大约30英尺至大约200英尺的长度和大约4英尺至大约12英尺的宽度。在一些方面中,屋面膜10可具有大约10英尺的宽度。宽度的变化可提供各种优点。例如,在一些方面中,具有较小宽度的屋面膜10可有利地使得屋面结构的组装更容易。较小宽度也可有利地使得制成的膜的卷绕或包装更容易。较大宽度可有利地实现更大的结构完整性、快速安装和/或改进包含这些膜的屋面结构的稳定性。
许多不同的阻燃剂可与屋面膜10的顶层和底层14、38中所用的第一和第二硅烷可交联聚烯烃弹性体结合使用。例如,氢氧化镁可在层14、38中提供阻燃性质。氢氧化镁可与硅烷接枝聚烯烃弹性体一起挤出或共混以确保完全分散在组合物共混物中。在一些方面中,氢氧化镁以最多70重量%氢氧化镁的量与硅烷接枝聚烯烃弹性体共混。在另一示例性实施方案中,硅烷接枝聚烯烃弹性体中的氢氧化镁可构成屋面膜组合物的大约20重量%至75重量%。
本公开集中于用于制造单合叠屋面膜10(如图1中描绘)的硅烷交联聚烯烃弹性体的组合物、制造该组合物的方法、用这些组合物制造屋面膜的方法和相应的材料性质,以及与本公开的原理相符的其他屋面膜10。屋面膜10由硅烷接枝聚烯烃形成,其中该硅烷接枝聚烯烃可具有添加的催化剂以形成硅烷可交联聚烯烃弹性体。这种硅烷可交联聚烯烃可随后在暴露于湿和/或热时交联以形成最终硅烷交联聚烯烃弹性体或共混物。在各方面中,该硅烷交联聚烯烃弹性体或共混物包括具有小于0.90g/cm3的密度的第一聚烯烃、具有小于40%的结晶度的第二聚烯烃、硅烷交联剂、接枝引发剂和缩合催化剂。
第一聚烯烃
第一聚烯烃可以是包括烯烃嵌段共聚物、乙烯/α-烯烃共聚物、丙烯/α-烯烃共聚物、EPDM、EPM或这些材料的任何两种或更多种的混合物的聚烯烃弹性体。示例性的嵌段共聚物包括以商品名INFUSETM(一种烯烃嵌段共聚物)(the Dow Chemical Company)和SEPTONTM V-SERIES(一种苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物)(Kuraray Co.,LTD.)出售的那些。示例性的乙烯/α-烯烃共聚物包括以商品名TAFMERTM(例如TAFMER DF710)(MitsuiChemicals,Inc.)和ENGAGETM(例如ENGAGE8150)(the Dow Chemical Company)出售的那些。示例性的丙烯/α-烯烃共聚物包括以商品名VISTAMAXXTM 6102等级(Exxon Mobil ChemicalCompany)、TAFMERTM XM(Mitsui Chemical Company)和VERSIFYTM(Dow Chemical Company)出售的那些。EPDM可具有大约0.5至大约10重量%的二烯含量。EPM可具有45重量%至75重量%的乙烯含量。
术语“共聚单体”是指适合与烯烃单体(如乙烯或丙烯单体)聚合的烯烃共聚单体。共聚单体可包含但不限于脂族C2-C20α-烯烃。合适的脂族C2-C20α-烯烃的实例包括乙烯、丙烯、1-丁烯、4-甲基-1-戊烯、1-己烯、1-辛烯、1-癸烯、1-十二烯、1-十四烯、1-十六烯、1-十八烯和1-二十烯。在一个实施方案中,该共聚单体是乙酸乙烯酯。术语“共聚物”是指通过将多于一种类型的单体连接在同一聚合物链中制成的聚合物。术语“均聚物”是指通过在不存在共聚单体的情况下连接烯烃单体而制成的聚合物。共聚单体的量在一些实施方案中可为基于聚烯烃的重量计大于0重量%至大约12重量%,包括大于0重量%至大约9重量%和大于0重量%至大约7重量%。在一些实施方案中,共聚单体含量为最终聚合物的大于大约2摩尔%,包括大于大约3摩尔%和大于大约6摩尔%。共聚单体含量可小于或等于大约30摩尔%。共聚物可以是无规或嵌段(多相)共聚物。在一些实施方案中,该聚烯烃是丙烯和乙烯的无规共聚物。
在一些方面中,第一聚烯烃选自:烯烃均聚物、均聚物的共混物、使用两种或更多种烯烃制成的共聚物、各自使用两种或更多种烯烃制成的共聚物的共混物、和与使用两种或更多种烯烃制成的共聚物共混的烯烃均聚物的组合。烯烃可选自乙烯、丙烯、1-丁烯、1-丙烯、1-己烯、1-辛烯和其它更高级1-烯烃。第一聚烯烃可使用许多不同的方法(例如使用气相和溶液基茂金属催化和齐格勒纳塔催化)合成,并任选使用适用于聚合乙烯和/或α-烯烃的催化剂。在一些方面中,茂金属催化剂可用于制造低密度乙烯/α-烯烃聚合物。
在一些方面中,用于第一聚烯烃的聚乙烯可分类为几种类型,包括但不限于LDPE(低密度聚乙烯)、LLDPE(线性低密度聚乙烯)和HDPE(高密度聚乙烯)。在另一些方面中,聚乙烯可分类为超高分子量(UHMW)、高分子量(HMW)、中分子量(MMW)和低分子量(LMW)。在再一些方面中,聚乙烯可以是超低密度乙烯弹性体。
在一些方面中,第一聚烯烃可包括LDPE/硅烷共聚物或共混物。在另一些方面中,第一聚烯烃可以是可使用本领域中已知的任何催化剂(包括但不限于铬催化剂、齐格勒纳塔催化剂、茂金属催化剂或后茂金属催化剂)制成的聚乙烯。
在一些方面中,第一聚烯烃可具有小于或等于大约5、小于或等于大约4、大约1至大约3.5、或大约1至大约3的分子量分布Mw/Mn。
第一聚烯烃可以该组合物的大于0至大约100重量%的量存在。在一些实施方案中,聚烯烃弹性体的量为大约30重量%至大约70重量%。在一些方面中,供入挤出机的第一聚烯烃可包含大约50重量%至大约80重量%的乙烯/α-烯烃共聚物,包括大约60重量%至大约75重量%和大约62重量%至大约72重量%。
第一聚烯烃可具有使用布氏粘度计在大约177℃的温度下测得的大约2,000cP至大约50,000cP的熔体粘度。在一些实施方案中,熔体粘度为大约4,000cP至大约40,000cP,包括大约5,000cP至大约30,000cP和大约6,000cP至大约18,000cP。
第一聚烯烃可具有大约20.0g/10min至大约3,500g/10min,包括大约250g/10min至大约1,900g/10min和大约300g/10min至大约1,500g/10min的在190℃下在2.16kg载荷下测得的熔体指数(T2)。在一些方面中,第一聚烯烃具有0.5g/10min至大约3,500g/10min的分熔体指数(fractional melt index)。
在一些方面中,第一聚烯烃的密度小于0.90g/cm3、小于大约0.89g/cm3、小于大约0.88g/cm3、小于大约0.87g/cm3、小于大约0.86g/cm3、小于大约0.85g/cm3、小于大约0.84g/cm3、小于大约0.83g/cm3、小于大约0.82g/cm3、小于大约0.81g/cm3或小于大约0.80g/cm3。在另一些方面中,第一聚烯烃的密度可为大约0.85g/cm3至大约0.89g/cm3、大约0.85g/cm3至大约0.88g/cm3、大约0.84g/cm3至大约0.88g/cm3、或大约0.83g/cm3至大约0.87g/cm3。在再一些方面中,密度为大约0.84g/cm3、大约0.85g/cm3、大约0.86g/cm3、大约0.87g/cm3、大约0.88g/cm3或大约0.89g/cm3。
第一聚烯烃的结晶度百分比可以小于大约60%、小于大约50%、小于大约40%、小于大约35%、小于大约30%、小于大约25%或小于大约20%。结晶度百分比可为至少大约10%。在一些方面中,结晶度为大约2%至大约60%。
第二聚烯烃
第二聚烯烃可以是包括烯烃嵌段共聚物、乙烯/α-烯烃共聚物、丙烯/α-烯烃共聚物、EPDM、EPM或这些材料的任何两种或更多种的混合物的聚烯烃弹性体。示例性的嵌段共聚物包括以商品名INFUSETM(the Dow Chemical Company)和SEPTONTM V-SERIES(KurarayCo.,LTD.)出售的那些。示例性的乙烯/α-烯烃共聚物包括以商品名TAFMERTM(例如TAFMERDF710)(Mitsui Chemicals,Inc.)和ENGAGETM(例如ENGAGE8150)(the Dow ChemicalCompany)出售的那些。示例性的丙烯/α-烯烃共聚物包括以商品名TAFMERTM XM等级(MitsuiChemical Company)和VISTAMAXXTM(例如VISTAMAXX 6102)(Exxon Mobil ChemicalCompany)出售的那些。EPDM可具有大约0.5至大约10重量%的二烯含量。EPM可具有45重量%至75重量%的乙烯含量。
在一些方面中,第二聚烯烃选自:烯烃均聚物、均聚物的共混物、使用两种或更多种烯烃制成的共聚物、各自使用两种或更多种烯烃制成的共聚物的共混物、和烯烃均聚物与使用两种或更多种烯烃制成的共聚物的共混物。烯烃可选自乙烯、丙烯、1-丁烯、1-丙烯、1-己烯、1-辛烯和其它更高级1-烯烃。第一聚烯烃可使用许多不同的方法(例如使用气相和溶液基茂金属催化和齐格勒纳塔催化)合成,并任选使用适用于聚合乙烯和/或α-烯烃的催化剂。在一些方面中,茂金属催化剂可用于制造低密度乙烯/α-烯烃聚合物。
在一些方面中,第二聚烯烃可包括聚丙烯均聚物、聚丙烯共聚物、聚乙烯-共-丙烯共聚物或其混合物。合适的聚丙烯包括但不限于通过丙烯的均聚或丙烯和α-烯烃共聚单体的共聚获得的聚丙烯。在一些方面中,第二聚烯烃可具有比第一聚烯烃更高的分子量和/或更高的密度。
在一些实施方案中,第二聚烯烃可具有小于或等于大约5、小于或等于大约4、大约1至大约3.5、或大约1至大约3的分子量分布Mw/Mn。
第二聚烯烃可以该组合物的大于0重量%至大约100重量%的量存在。在一些实施方案中,聚烯烃弹性体的量为大约30重量%至大约70重量%。在一些实施方案中,供入挤出机的第二聚烯烃可包含大约10重量%至大约50重量%聚丙烯、大约20重量%至大约40重量%聚丙烯或大约25重量%至大约35重量%聚丙烯。该聚丙烯可以是均聚物或共聚物。
第二聚烯烃可具有使用布氏粘度计在大约177℃的温度下测得的大约2,000cP至大约50,000cP的熔体粘度。在一些实施方案中,熔体粘度为大约4,000cP至大约40,000cP,包括大约5,000cP至大约30,000cP和大约6,000cP至大约18,000cP。
第二聚烯烃可具有大约20.0g/10min至大约3,500g/10min,包括大约250g/10min至大约1,900g/10min和大约300g/10min至大约1,500g/10min的在190℃下在2.16kg载荷下测得的熔体指数(T2)。在一些实施方案中,该聚烯烃具有0.5g/10min至大约3,500g/10min的分熔体指数(fractional melt index)。
在一些方面中,第二聚烯烃的密度小于0.90g/cm3、小于大约0.89g/cm3、小于大约0.88g/cm3、小于大约0.87g/cm3、小于大约0.86g/cm3、小于大约0.85g/cm3、小于大约0.84g/cm3、小于大约0.83g/cm3、小于大约0.82g/cm3、小于大约0.81g/cm3或小于大约0.80g/cm3。在另一些方面中,第一聚烯烃的密度可为大约0.85g/cm3至大约0.89g/cm3、大约0.85g/cm3至大约0.88g/cm3、大约0.84g/cm3至大约0.88g/cm3、或大约0.83g/cm3至大约0.87g/cm3。在再一些方面中,密度为大约0.84g/cm3、大约0.85g/cm3、大约0.86g/cm3、大约0.87g/cm3、大约0.88g/cm3或大约0.89g/cm3。
第二聚烯烃的结晶度百分比可以小于大约60%、小于大约50%、小于大约40%、小于大约35%、小于大约30%、小于大约25%或小于大约20%。结晶度百分比可为至少大约10%。在一些方面中,结晶度为大约2%至大约60%。
如所述,例如屋面膜10中(例如在图1中所示的顶层和底层14、38内)所用的硅烷交联聚烯烃弹性体或共混物包括第一聚烯烃和第二聚烯烃。第二聚烯烃通常用于改变具有小于0.90g/cm3的密度的第一聚烯烃的硬度和/或可加工性。在一些方面中,可以不只使用第一和第二聚烯烃形成硅烷交联聚烯烃弹性体或共混物。例如,在一些方面中,一种、两种、三种、四种或更多种具有小于0.90g/cm3、小于0.89g/cm3、小于0.88g/cm3、小于0.87g/cm3、小于0.86g/cm3或小于0.85g/cm3的密度的不同的聚烯烃可取代和/或用于第一聚烯烃。在一些方面中,一种、两种、三种、四种或更多种不同的聚烯烃、聚乙烯-共-丙烯共聚物可取代和/或用于第二聚烯烃。
使用具有小于0.90g/cm3的密度的第一聚烯烃和具有小于40%的结晶度的第二聚烯烃的共混物,因为这些第一和第二聚烯烃材料一起的随后硅烷接枝和交联形成最终硅烷交联聚烯烃弹性体中的核心树脂结构。尽管可将附加聚烯烃作为填料添加到硅烷接枝、硅烷可交联和/或硅烷交联的聚烯烃弹性体的共混物中以根据最终产物所需改进和/或改变杨氏模量,添加到共混物中的任何具有等于或大于40%的结晶度的聚烯烃没有化学或共价并入最终硅烷交联聚烯烃弹性体的交联结构中。
在一些方面中,第一和第二聚烯烃可进一步包括一种或多种具有或没有硅烷接枝结构部分的TPVs和/或EPDM,其中TPV和/或EPDM聚合物以硅烷交联聚烯烃弹性体/共混物的最多20重量%的量存在。
接枝引发剂
接枝引发剂(在本公开中也称为“自由基引发剂”)可通过与各自的聚烯烃反应而用于至少第一和第二聚烯烃的接枝过程以形成可与硅烷交联剂分子反应和/或偶联的反应性物类。接枝引发剂可包括卤素分子、偶氮化合物(例如偶氮双异丁基)、羧酸过氧酸、过氧酯、过氧缩酮和过氧化物(例如烷基氢过氧化物、二烷基过氧化物和二酰基过氧化物)。在一些实施方案中,接枝引发剂是选自二叔丁基过氧化物、叔丁基过氧化异丙苯、过氧化二异丙苯、2,5-二甲基-2,5-二(叔丁基-过氧基)己炔-3、1,3-双(叔丁基-过氧基-异丙基)苯、正丁基-4,4-双(叔丁基-过氧基)戊酸酯、过氧化苯甲酰、过氧苯甲酸叔丁酯、叔丁基过氧基异丙基碳酸酯和过苯甲酸叔丁酯,以及双(2-甲基苯甲酰基)过氧化物、双(4-甲基苯甲酰基)过氧化物、过辛酸叔丁酯、氢过氧化枯烯、甲乙酮过氧化物、十二烷基过氧化物、过乙酸叔丁酯、过氧化二叔戊基、过氧苯甲酸叔戊酯、1,1-双(叔丁基过氧基)-3,3,5-三甲基环己烷、α,α'-双(叔丁基过氧基)-1,3-二异丙基苯、α,α'-双(叔丁基过氧基)-1,4-二异丙基苯、2,5-双(叔丁基过氧基)-2,5-二甲基己烷和2,5-双(叔丁基过氧基)-2,5-二甲基-3-己炔和过氧化2,4-二氯苯甲酰的有机过氧化物。示例性的过氧化物包括以商品名LUPEROXTM出售的那些(可获自Arkema,Inc.)。
在一些方面中,接枝引发剂以该组合物的大于0重量%至大约2重量%的量存在,包括该组合物的大约0.15重量%至大约1.2重量%。所用引发剂和硅烷的量可能影响硅烷接枝聚合物的最终结构(例如接枝聚合物中的接枝度和固化聚合物中的交联度)。在一些方面中,该反应性组合物含有至少100ppm的引发剂或至少300ppm的引发剂。引发剂可以300ppm至1500ppm或300ppm至2000ppm的量存在。硅烷:引发剂重量比可为大约20:1至400:1,包括大约30:1至大约400:1、大约48:1至大约350:1、和大约55:1至大约333:1。
接枝反应可在使副反应(例如接枝剂的均聚)最小化的同时优化互聚物骨架上的接枝的条件下进行。接枝反应可在熔体中、在溶液中、在固态中和/或在溶胀态中进行。可在多种多样的设备(例如双螺杆挤出机、单螺杆挤出机、Brabenders、密闭式混合机如Banbury混合机和分批反应器)中进行硅烷化。在一些实施方案中,聚烯烃、硅烷和引发剂在挤出机的第一阶段中混合。熔融温度(即聚合物开始熔融并开始流动的温度)可为大约120℃至大约260℃,包括大约130℃至大约250℃。
硅烷交联剂
硅烷交联剂可用于将硅烷结构部分共价接枝到第一和第二聚烯烃上且硅烷交联剂可包括烷氧基硅烷、硅氮烷、硅氧烷或其组合。通过由接枝引发剂与各自的硅烷交联剂反应形成的反应性物类促进各种可能的硅烷交联剂或硅烷交联剂分子的接枝和/或偶联。
在一些方面中,硅烷交联剂是硅氮烷,其中该硅氮烷可包括例如六甲基二硅氮烷(HMDS)或双(三甲基甲硅烷基)胺。在一些方面中,硅烷交联剂是硅氧烷,其中该硅氧烷可包括例如聚二甲基硅氧烷(PDMS)和八甲基环四硅氧烷。
在一些方面中,硅烷交联剂是烷氧基硅烷。本文所用的术语“烷氧基硅烷”是指包含硅原子、至少一个烷氧基和至少一个其它有机基团的化合物,其中硅原子通过共价键与有机基团键合。该烷氧基硅烷优选选自烷基硅烷;基于丙烯酰基的硅烷;基于乙烯基的硅烷;芳族硅烷;基于环氧基的硅烷;基于氨基的硅烷和具有-NH2、-NHCH3或-N(CH3)2的胺;基于酰脲的硅烷;基于巯基的硅烷;和具有羟基(即-OH)的烷氧基硅烷。基于丙烯酰基的硅烷可选自β-丙烯酰氧基乙基三甲氧基硅烷;β-丙烯酰氧基丙基三甲氧基硅烷;γ-丙烯酰氧基乙基三甲氧基硅烷;γ-丙烯酰氧基丙基三甲氧基硅烷;β-丙烯酰氧基乙基三乙氧基硅烷;β-丙烯酰氧基丙基三乙氧基硅烷;γ-丙烯酰氧基乙基三乙氧基硅烷;γ-丙烯酰氧基丙基三乙氧基硅烷;β-甲基丙烯酰氧基乙基三甲氧基硅烷;β-甲基丙烯酰氧基丙基三甲氧基硅烷;γ-甲基丙烯酰氧基乙基三甲氧基硅烷;γ-甲基丙烯酰氧基丙基三甲氧基硅烷;β-甲基丙烯酰氧基乙基三乙氧基硅烷;β-甲基丙烯酰氧基丙基三乙氧基硅烷;γ-甲基丙烯酰氧基乙基三乙氧基硅烷;γ-甲基丙烯酰氧基丙基三乙氧基硅烷;3-甲基丙烯酰氧基丙基甲基二乙氧基硅烷。基于乙烯基的硅烷可选自乙烯基三甲氧基硅烷;乙烯基三乙氧基硅烷;对苯乙烯基三甲氧基硅烷、甲基乙烯基二甲氧基硅烷、乙烯基二甲基甲氧基硅烷、二乙烯基二甲氧基硅烷、乙烯基三(2-甲氧基乙氧基)硅烷和乙烯基苄基亚乙基二氨基丙基三甲氧基硅烷。芳族硅烷可选自苯基三甲氧基硅烷和苯基三乙氧基硅烷。基于环氧基的硅烷可选自3-环氧丙氧丙基三甲氧基硅烷;3-环氧丙氧丙基甲基二乙氧基硅烷;3-环氧丙氧丙基三乙氧基硅烷;2-(3,4-环氧环己基)乙基三甲氧基硅烷和环氧丙氧丙基甲基二甲氧基硅烷。基于氨基的硅烷可选自3-氨基丙基三乙氧基硅烷;3-氨基丙基三甲氧基硅烷;3-氨基丙基二甲基乙氧基硅烷;3-氨基丙基甲基二乙氧基硅烷;4-氨基丁基三乙氧基硅烷;3-氨基丙基二异丙基乙氧基硅烷;1-氨基-2-(二甲基乙氧基甲硅烷基)丙烷;(氨基乙基氨基)-3-异丁基二甲基甲氧基硅烷;N-(2-氨基乙基)-3-氨基异丁基甲基二甲氧基硅烷;(氨基乙基氨基甲基)苯乙基三甲氧基硅烷;N-(2-氨基乙基)-3-氨基丙基甲基二甲氧基硅烷;N-(2-氨基乙基)-3-氨基丙基三甲氧基硅烷;N-(2-氨基乙基)-3-氨基丙基三乙氧基硅烷;N-(6-氨基己基)氨基甲基三甲氧基硅烷;N-(6-氨基己基)氨基甲基三甲氧基硅烷;N-(6-氨基己基)氨基丙基三甲氧基硅烷;N-(2-氨基乙基)-1,1-氨基十一烷基三甲氧基硅烷;1,1-氨基十一烷基三乙氧基硅烷;3-(间氨基苯氧基)丙基三甲氧基硅烷;间氨基苯基三甲氧基硅烷;对氨基苯基三甲氧基硅烷;(3-三甲氧基甲硅烷基丙基)二亚乙基三胺;N-甲基氨基丙基甲基二甲氧基硅烷;N-甲基氨基丙基三甲氧基硅烷;二甲基氨基甲基乙氧基硅烷;(N,N-二甲基氨基丙基)三甲氧基硅烷;(N-乙酰基甘氨酰基)-3-氨基丙基三甲氧基硅烷((N-acetylglycysil)-3-aminopropyl trimethoxysilane)、N-苯基-3-氨基丙基三甲氧基硅烷、N-苯基-3-氨基丙基三乙氧基硅烷、苯基氨基丙基三甲氧基硅烷、氨基乙基氨基丙基三甲氧基硅烷和氨基乙基氨基丙基甲基二甲氧基硅烷。基于酰脲的硅烷可以是3-酰脲丙基三乙氧基硅烷。基于巯基的硅烷可选自3-巯丙基甲基二甲氧基硅烷、3-巯丙基三甲氧基硅烷和3-巯丙基三乙氧基硅烷。具有羟基的烷氧基硅烷可选自羟甲基三乙氧基硅烷;N-(羟乙基)-N-甲基氨基丙基三甲氧基硅烷;双(2-羟乙基)-3-氨基丙基三乙氧基硅烷;N-(3-三乙氧基甲硅烷基丙基)-4-羟丁基酰胺;1,1-(三乙氧基甲硅烷基)十一烷醇;三乙氧基甲硅烷基十一烷醇;乙二醇缩醛;和N-(3-乙氧基甲硅烷基丙基)葡糖酰胺(gluconamide)。
在一些方面中,烷基硅烷可由通式:RnSi(OR')4-n表示,其中:n是1、2或3;R是C1-20烷基或C2-20烯基;且R'是C1-20烷基。术语“烷基”独自或作为另一取代基的一部分,是指通过碳-碳单键连接的具有1至20个碳原子,例如1至10个碳原子,例如1至8个碳原子,或例如1至6个碳原子的直链、支化或环状饱和烃基。当在本文中在碳原子后使用下标时,该下标是指指定的基团可含有的碳原子数。因此,例如C1-6烷基是指1至6个碳原子的烷基。烷基的实例是甲基、乙基、丙基、异丙基、丁基、异丁基、仲丁基、叔丁基、2-甲基丁基、戊基、异戊基及其异构体、己基及其异构体、庚基及其异构体、辛基及其异构体、癸基及其异构体、十二烷基及其异构体。术语“C2-20烯基”独自或作为另一取代基的一部分,是指可以是线性或支化的、包含一个或多个碳-碳双键的具有2至20个碳原子的不饱和烃基。C2-6烯基的实例是乙烯基、2-丙烯基、2-丁烯基、3-丁烯基、2-戊烯基及其异构体、2-己烯基及其异构体、2,4-戊二烯基等。
在一些方面中,烷基硅烷可选自甲基三甲氧基硅烷;甲基三乙氧基硅烷;乙基三甲氧基硅烷;乙基三乙氧基硅烷;丙基三甲氧基硅烷;丙基三乙氧基硅烷;己基三甲氧基硅烷;己基三乙氧基硅烷;辛基三甲氧基硅烷;辛基三乙氧基硅烷;癸基三甲氧基硅烷;癸基三乙氧基硅烷;十二烷基三甲氧基硅烷:十二烷基三乙氧基硅烷;十三烷基三甲氧基硅烷;十二烷基三乙氧基硅烷;十六烷基三甲氧基硅烷;十六烷基三乙氧基硅烷;十八烷基三甲氧基硅烷;十八烷基三乙氧基硅烷、三甲基甲氧基硅烷、甲基氢二甲氧基硅烷、二甲基二甲氧基硅烷、二异丙基二甲氧基硅烷、二异丁基二甲氧基硅烷、异丁基三甲氧基硅烷、正丁基三甲氧基硅烷、正丁基甲基二甲氧基硅烷、苯基三甲氧基硅烷、苯基三甲氧基硅烷、苯基甲基二甲氧基硅烷、三苯基硅烷醇、正己基三甲氧基硅烷、正辛基三甲氧基硅烷、异辛基三甲氧基硅烷、癸基三甲氧基硅烷、十六烷基三甲氧基硅烷、环己基甲基二甲氧基硅烷、环己基乙基二甲氧基硅烷、二环戊基二甲氧基硅烷、叔丁基乙基二甲氧基硅烷、叔丁基丙基二甲氧基硅烷、二环己基二甲氧基硅烷及其组合。
在一些方面中,烷基硅烷化合物可选自三乙氧基辛基硅烷、三甲氧基辛基硅烷及其组合。
可用作硅烷交联剂的硅烷的另外的实例包括但不限于通式CH2=CR-(COO)x(CnH2n)ySiR'3的那些,其中R是氢原子或甲基;x是0或1;y是0或1;n是1至12的整数;各R'可以是有机基团并可独立地选自具有1至12个碳原子的烷氧基(例如甲氧基、乙氧基、丁氧基)、芳氧基(例如苯氧基)、芳烷族氧基(araloxy group)(例如苄氧基)、具有1至12个碳原子的脂族酰氧基(例如甲酰氧基、乙酰氧基、丙酰氧基)、氨基或取代氨基(例如烷基氨基、芳基氨基)或具有1至6个碳原子的低碳烷基。x和y可以都等于1。在一些方面中,三个R'基团的不多于一个是烷基。在另一些方面中,三个R'基团的不多于两个是烷基。
在本公开的实践中可使用本领域中已知的可有效接枝到烯烃聚合物上并交联烯烃聚合物的任何硅烷或硅烷混合物。在一些方面中,硅烷交联剂可包括但不限于包含烯属不饱和烃基(例如乙烯基、烯丙基、异丙烯基、丁烯基、环己烯基或γ-(甲基)丙烯酰氧基烯丙基)和可水解基团(例如烃氧基、烃基氧基(hydrocarbonyloxy)或烃基氨基)的不饱和硅烷。可水解基团的非限制性实例包括但不限于甲氧基、乙氧基、甲酰氧基、乙酰氧基、丙酰氧基和烷基,或芳基氨基。在另一些方面中,硅烷交联剂是可接枝到该聚合物上的不饱和烷氧基硅烷。在再一些方面中,附加的示例性硅烷交联剂包括乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、甲基丙烯酸3-(三甲氧基甲硅烷基)丙基酯、γ-(甲基)丙烯酰氧基丙基三甲氧基硅烷及其混合物。
硅烷交联剂可以大于0重量%至大约10重量%,包括大约0.5重量%至大约5重量%的量存在于硅烷接枝聚烯烃弹性体中。硅烷交联剂的量可基于烯烃聚合物的性质、硅烷本身、加工条件、接枝效率、用途和其它因素而变。硅烷交联剂的量可为基于反应性组合物的重量计的至少2重量%,包括至少4重量%或至少5重量%。在另一些方面中,硅烷交联剂的量可为基于反应性组合物的重量计的至少10重量%。在再一些方面中,硅烷交联剂含量为基于反应性组合物的重量计的至少1%。在一些实施方案中,供入挤出机的硅烷交联剂可包含大约0.5重量%至大约10重量%的硅烷单体、大约1重量%至大约5重量%的硅烷单体或大约2重量%至大约4重量%的硅烷单体。
缩合催化剂
缩合催化剂可促进硅烷接枝聚烯烃弹性体上的硅烷接枝的水解和随后缩合以形成交联。在一些方面中,可使用电子束辐射辅助交联。在一些方面中,缩合催化剂可包括例如有机碱、羧酸和有机金属化合物(例如铅、钴、铁、镍、锌和锡的有机钛酸盐和络合物或羧酸盐)。在另一些方面中,缩合催化剂可包括脂肪酸和金属络合物化合物,如金属羧酸盐;三乙酰丙酮铝、三乙酰丙酮铁、四乙酰丙酮锰、四乙酰丙酮镍、六乙酰丙酮铬、四乙酰丙酮钛和四乙酰丙酮钴;金属醇盐,如乙醇铝、丙醇铝、丁醇铝、乙醇钛、丙醇钛和丁醇钛;金属盐化合物,如乙酸钠、辛酸锡、辛酸铅、辛酸钴、辛酸锌、辛酸钙、环烷酸铅、环烷酸钴、二辛酸二丁基锡、二月桂酸二丁基锡、马来酸二丁基锡和二(2-乙基己酸)二丁基锡;酸性化合物,如甲酸、乙酸、丙酸、对甲苯磺酸、三氯乙酸、磷酸、单烷基磷酸、二烷基磷酸、(甲基)丙烯酸对羟乙酯的磷酸酯、单烷基亚磷酸和二烷基亚磷酸;酸,如对甲苯磺酸、邻苯二甲酸酐、苯甲酸、苯磺酸、十二烷基苯磺酸、甲酸、乙酸、衣康酸、草酸和马来酸、这些酸的铵盐、低级胺盐或多价金属盐、氢氧化钠、氯化锂;有机金属化合物,如二乙基锌和四(正丁氧基)钛;和胺,如二环己基胺、三乙基胺、N,N-二甲基苄基胺、N,N,N',N'-四甲基-1,3-丁二胺、二乙醇胺、三乙醇胺和环己基乙基胺。在再一些方面中,缩合催化剂可包括二月桂酸二丁基锡、马来酸二辛基锡、二乙酸二丁基锡、二辛酸二丁基锡、乙酸亚锡、辛酸亚锡、环烷酸铅、辛酸锌和环烷酸钴。根据硅烷交联聚烯烃弹性体或共混物的所需最终材料性质,可以使用单一缩合催化剂或缩合催化剂的混合物。缩合催化剂可以硅烷接枝聚烯烃弹性体/共混物组合物的总重量的大约0.01重量%至大约1.0重量%,包括大约0.25重量%至大约8重量%的量存在。
在一些方面中,交联体系可包括和使用辐射、热、湿和另外缩合催化剂的一种或所有组合。在一些方面中,缩合催化剂可以0.25重量%至8重量%的量存在。在另一些方面中,可包括大约1重量%至大约10重量%或大约2重量%至大约5重量%的量的缩合催化剂。
任选附加组分
硅烷交联聚烯烃弹性体可任选包括一种或多种填料。填料可与硅烷接枝聚烯烃一起挤出并在一些方面中可包括具有大于20%、大于30%、大于40%或大于50%的结晶度的附加聚烯烃。在一些方面中,填料可包括金属氧化物、金属氢氧化物、金属碳酸盐、金属硫酸盐、金属硅酸盐、粘土、滑石、炭黑和二氧化硅。根据用途和/或所需性质,这些材料可以是热解法的(fumed)或煅烧的。
进一步就填料而言,金属氧化物、金属氢氧化物、金属碳酸盐、金属硫酸盐或金属硅酸盐的金属可选自碱金属(例如锂、钠、钾、铷、铯和钫);碱土金属(例如铍、镁、钙、锶、钡和镭);过渡金属(例如锌、钼、镉、钪、钛、钒、铬、锰、铁、钴、镍、铜、钇、锆、铌、锝、钌(ruthernium)、铑、钯、银、铪、钽(taltalum)、钨、铼、锇、铟、铂、金、汞、 和鎶);后过渡金属(例如铝、镓、铟、锡、铊、铅、铋和钋);镧系元素(例如镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱和镥);锕系元素(例如锕、钍、镤、铀、镎、钚、镅、锔、锫、锎、锿、镄、钔、锘和铹);锗;砷;锑;和砹。
硅烷交联聚烯烃弹性体或共混物的填料可以大于0重量%至大约50重量%,包括大约1重量%至大约20重量%和大约3重量%至大约10重量%的量存在。
硅烷交联聚烯烃弹性体和/或形成的各制品(例如图1中描绘的单合叠屋面膜10)还可包括蜡(例如石蜡、微晶蜡、HDPE蜡、LDPE蜡、热降解蜡、副产物聚乙烯蜡、任选氧化的费托蜡和功能化蜡)。在一些实施方案中,蜡以大约0重量%至大约10重量%的量存在。
增粘树脂(例如脂族烃、芳烃、改性烃、萜烯、改性萜烯、氢化萜烯、松香、松香衍生物、氢化松香及其混合物)也可包括在该硅烷交联聚烯烃弹性体/共混物中。增粘树脂可具有70℃至大约150℃的环球法软化点和在177℃下小于大约3,000cP的粘度。在一些方面中,增粘树脂以大约0重量%至大约10重量%的量存在。
在一些方面中,硅烷交联聚烯烃弹性体可包括一种或多种油。油的非限制性类型包括白矿物油和环烷油。在一些实施方案中,油以大约0重量%至大约10重量%的量存在。
在一些方面中,硅烷交联聚烯烃弹性体可包括一种或多种具有大于20%、大于30%、大于40%或大于50%的结晶度的填料聚烯烃。该填料聚烯烃可包括聚丙烯、聚(乙烯-共-丙烯)和/或其它乙烯/α-烯烃共聚物。在一些方面中,填料聚烯烃的使用可以大约5重量%至大约60重量%、大约10重量%至大约50重量%、大约20重量%至大约40重量%、或大约5重量%至大约20重量%的量存在。填料聚烯烃的加入可将最终硅烷交联聚烯烃弹性体的杨氏模量提高至少10%、至少25%或至少50%。
在一些方面中,本公开的硅烷交联聚烯烃弹性体可包括一种或多种稳定剂(例如抗氧化剂)。硅烷交联聚烯烃弹性体可在接枝前、在接枝后、在交联前和/或在交联后处理。也可包括其它添加剂。添加剂的非限制性实例包括抗静电剂、染料、颜料、紫外线吸收剂、成核剂、填料、滑爽剂、增塑剂、阻燃剂、润滑剂、加工助剂、抑烟剂、防粘连剂和粘度控制剂。抗氧化剂可以该组合物的小于0.5重量%,包括小于0.2重量%的量存在。
在一些方面中,可将二氧化钛(一种白色颜料)添加到配方中以提供不透明性和颜色。此外,二氧化钛也可提供紫外线防护。在一些方面中,二氧化钛可与第一和/或第二聚烯烃(上述类型)预混以确保二氧化钛完全分散在该组合物各处。在一些方面中,为了确保在挤出或其它成型技术之前二氧化钛完全分散到该组合物中,二氧化钛可以最多30重量%、最多20重量%或最多10重量%的量与第一和/或第二聚烯烃预混。
制造硅烷接枝聚烯烃弹性体的方法
硅烷交联聚烯烃弹性体的合成/生产可通过使用单步Monosil法在一个挤出机中或使用消除对挤出前混合和运输橡胶化合物的附加步骤的需要的两步Sioplas法在两个挤出机中合并各组分进行。
现在参考图2,提供在用于合成硅烷交联聚烯烃弹性体的单步Monosil法和两步Sioplas法的过程中使用的一般化学工艺。该工艺以接枝步骤开始,其包括由接枝引发剂引发,接着用第一和第二聚烯烃增长和链转移。接枝引发剂,在一些方面中过氧化物或偶氮化合物,均裂以形成两个自由基引发剂片段,它们通过增长步骤转移到第一和第二聚烯烃链之一上。现在位于第一或第二聚烯烃链上的自由基可随后转移至硅烷分子和/或另一聚烯烃链。一旦引发剂和自由基耗尽,第一和第二聚烯烃的硅烷接枝反应完成。
仍参考图2,一旦硅烷接枝反应完成,产生稳定的第一和第二硅烷接枝聚烯烃的混合物。然后可将交联催化剂添加到第一和第二硅烷接枝聚烯烃以形成硅烷接枝聚烯烃弹性体。交联催化剂可首先促进接枝到聚烯烃骨架上的甲硅烷基的水解以形成反应性硅烷醇基团。硅烷醇基团可随后与其它聚烯烃分子上的其它硅烷醇基团反应以形成经由硅氧烷键连接在一起的弹性体聚烯烃聚合物链的交联网络。硅烷接枝聚烯烃弹性体各处的硅烷交联的密度可影响该弹性体表现出的材料性质。
现在参考图3和4A,显示使用两步Sioplas法制造屋面膜10的方法200。方法200可以步骤204开始,其包括一起挤出(例如用双螺杆挤出机252)具有小于0.86g/cm3的密度的第一聚烯烃240、第二聚烯烃244和包含硅烷交联剂(例如乙烯基三甲氧基硅烷,VTMO)和接枝引发剂(例如过氧化二异丙苯)的硅烷配混物(silan cocktail)248以形成硅烷接枝聚烯烃共混物。第一聚烯烃240和第二聚烯烃244可使用加料斗256添加到反应性双螺杆挤出机252中。可在挤出生产线的进一步下游将硅烷配混物(silan cocktail)248添加到双螺杆260中以助于促进与第一和第二聚烯烃240、244共混物的更好混合。在反应性双螺杆挤出机252上可使用强制挥发性有机化合物(VOC)真空264以助于保持所需反应压力。双螺杆挤出机252被认为是反应性的,因为自由基引发剂和硅烷交联剂与第一和第二聚烯烃240、244反应并与第一和第二聚烯烃240、244形成新的共价键。熔融的硅烷接枝聚烯烃共混物可使用齿轮泵268离开反应性双螺杆挤出机252,其将熔融的硅烷接枝聚烯烃共混物注射到水造粒机272中,其可形成丸粒状的硅烷接枝聚烯烃共混物276。在一些方面中,可在并入缩合催化剂280(见图4B)和形成最终制品(例如图1中描绘的屋面膜10)之前将熔融的硅烷接枝聚烯烃共混物276挤出成丸粒、枕块或任何其它配置。
反应性双螺杆挤出机252可配置为具有延伸双螺杆挤出机252的各种长度的多个不同的温度区(例如图4A中所示的Z0-Z12)。在一些方面中,各温度区可具有大约室温至大约180℃、大约120℃至大约170℃、大约120℃至大约160℃、大约120℃至大约150℃、大约120℃至大约140℃、大约120℃至大约130℃、大约130℃至大约170℃、大约130℃至大约160℃、大约130℃至大约150℃、大约130℃至大约140℃、大约140℃至大约170℃、大约140℃至大约160℃、大约140℃至大约150℃、大约150℃至大约170℃、和大约150℃至大约160℃的温度。在一些方面中,Z0可具有大约60℃至大约110℃的温度或无冷却;Z1可具有大约120℃至大约130℃的温度;Z2可具有大约140℃至大约150℃的温度;Z3可具有大约150℃至大约160℃的温度;Z4可具有大约150℃至大约160℃的温度;Z5可具有大约150℃至大约160℃的温度;Z6可具有大约150℃至大约160℃的温度;Z7可具有大约150℃至大约160℃的温度;和Z8-Z12可具有大约150℃至大约160℃的温度。
在一些方面中,硅烷接枝聚烯烃弹性体的数均分子量可为大约4,000g/mol至大约30,000g/mol,包括大约5,000g/mol至大约25,000g/mol和大约6,000g/mol至大约14,000g/mol。接枝聚合物的重均分子量可为大约8,000g/mol至大约60,000g/mol,包括大约10,000g/mol至大约30,000g/mol。
现在参考图3和4B,方法200接着包括一起挤出硅烷接枝聚烯烃共混物276和缩合催化剂280以形成硅烷可交联聚烯烃共混物298的步骤208。在一些方面中,一种或多种任选添加剂284可与硅烷接枝聚烯烃共混物276和缩合催化剂280一起加入以调节硅烷可交联聚烯烃共混物298的最终材料性质。在步骤208中,将硅烷接枝聚烯烃共混物276与形成硅烷醇的缩合催化剂280混合以形成硅烷接枝上的反应性硅烷醇基团,其可随后在暴露于湿和/或热时交联。在一些方面中,缩合催化剂280可包括磺酸、抗氧化剂、加工助剂和用于着色的炭黑的混合物,其中环境湿度足以使这种缩合催化剂280经更长时期(例如大约48小时)交联该硅烷可交联聚烯烃共混物298。硅烷接枝聚烯烃共混物276和缩合催化剂280可使用加料斗(类似于图4A中所示的加料斗256)和加料齿轮泵296添加到反应性单螺杆挤出机288中。可将硅烷接枝聚烯烃共混物276和缩合催化剂280和在一些方面中一种或多种任选添加剂284的组合添加到反应性单螺杆挤出机288的单螺杆292中。单螺杆挤出机288被认为是反应性的,因为将硅烷接枝聚烯烃共混物276和缩合催化剂280熔融并合并在一起以将缩合催化剂280充分和均匀混合在熔融的硅烷接枝聚烯烃共混物276中。在步骤208中形成的熔融的硅烷可交联聚烯烃共混物298可经模头离开反应性单螺杆挤出机288,其可将熔融的硅烷可交联聚烯烃共混物298注射成未固化屋面膜元件的形式。
在步骤208的过程中,在硅烷接枝聚烯烃共混物276与缩合催化剂280一起挤出以形成硅烷可交联聚烯烃共混物298时,可发生一定量的交联。在一些方面中,硅烷可交联聚烯烃共混物298可大约25%固化、大约30%固化、大约35%固化、大约40%固化、大约45%固化、大约50%固化、大约55%固化、大约60%固化、大约65%固化或大约70%固化,其中可使用凝胶试验(ASTM D2765)测定最终硅烷交联聚烯烃弹性体中的交联量。
参考图3和4B,方法200进一步包括挤出和/或压延硅烷可交联聚烯烃弹性体或共混物298以形成包含未固化的硅烷可交联聚烯烃弹性体的顶层和底层14、38的步骤212。硅烷可交联聚烯烃弹性体或共混物298为熔化或熔融状态,此时其可流动并在其离开反应性单螺杆挤出机288时成型。压延系统302是用于将熔融硅烷可交联聚烯烃弹性体共混物298加工成片材或膜的具有两个或更多个辊(辊之间的区域被称为辊隙)的装置。随着熔融硅烷可交联聚烯烃弹性体共混物298离开反应性单螺杆挤出机288,其在压延系统302的第一辊隙点形成硅烷可交联聚烯烃弹性体的池306。然后将硅烷可交联聚烯烃弹性体的池306分别压制或辊轧成顶层或底层14、38。可在压延过程中的任何点使用稀松布卷318将稀松布层26分别添加到顶层或底层14、38。稀松布层26在结合到顶层或底层14、38时形成部分稀松布膜(partial scrim membrane)322。部分稀松布膜322可进一步在分别缺失顶层或底层14、38时压延和压制以形成未固化屋面膜元件。
再参考图3,方法200可进一步包括在环境温度和/或环境湿度下交联该硅烷可交联聚烯烃共混物298或未固化形式的屋面膜元件以形成具有大约0.85g/cm3至大约0.89g/cm3的密度的屋面膜10(见图1)的步骤216。更特别地,在这一交联过程中,水将硅烷可交联聚烯烃弹性体的硅烷水解以产生硅烷醇。各种硅烷接枝上的硅烷醇基团可随后缩合形成分子间的不可逆Si-O-Si交联位点。可通过控制生产方法,包括所用催化剂的量,调节交联硅烷基团的量和因此最终聚合物性质。
方法200的步骤216(见图3)的交联/固化可进行大于0至大约20小时的时期。在一些方面中,固化进行大约1小时至大约20小时、10小时至大约20小时、大约15小时至大约20小时、大约5小时至大约15小时、大约1小时至大约8小时、或大约3小时至大约6小时的时期。交联/固化过程中的温度可为大约室温、大约20℃至大约25℃、大约20℃至大约150℃、大约25℃至大约100℃、或大约20℃至大约75℃。固化过程中的湿度可为大约30%至大约100%、大约40%至大约100%、或大约50%至大约100%。
在一些方面中,使用能在接近TPV加工条件的挤出机热设置下以30比1的长L/D挤出热塑性材料的挤出机设置,其中挤出物在环境条件下交联以变成热固性。在另一些方面中,可通过蒸汽暴露加速这一过程。在刚挤出后,凝胶含量(也称为交联密度)可为大约60%,但在环境条件下96小时后,凝胶含量可达到大于大约95%。
在一些方面中,可以使用一个或多个反应性单螺杆挤出机288以形成具有一种或多种类型的硅烷交联聚烯烃弹性体的未固化屋面膜元件(和相应的单合叠屋面膜10)。例如,在一些方面中,可以使用一个反应性单螺杆挤出机288以生产和挤出用于屋面膜10的顶层14(见图1)的相关的第一硅烷交联聚烯烃弹性体,同时可以使用第二反应性单螺杆挤出机288以生产和挤出用于屋面膜10的底层38的第二硅烷交联聚烯烃弹性体。屋面膜10的复杂性、构造和性质要求决定其制造所必需的反应性单螺杆挤出机288的数量和类型。
要理解的是,概述和教导各种屋面膜10和它们各自的组分和组成的在先描述可以任何组合使用并同样好地适用于使用图3、4A和4B中所示的两步Sioplas法制造屋面膜10的方法200。
现在参考图5和6,显示使用单步Monosil法制造屋面膜10的方法400。方法400可以步骤404开始,其包括一起挤出(例如用单螺杆挤出机444)具有小于0.86g/cm3的密度的第一聚烯烃240、第二聚烯烃244、包含硅烷交联剂(例如乙烯基三甲氧基硅烷,VTMO)和接枝引发剂(例如过氧化二异丙苯)的硅烷配混物(silan cocktail)248和缩合催化剂280以形成可交联的硅烷接枝聚烯烃共混物298。第一聚烯烃240、第二聚烯烃244和硅烷配混物(silancocktail)248可使用加料斗440添加到反应性单螺杆挤出机444中。在一些方面中,可在挤出生产线的进一步下游将硅烷配混物(silan cocktail)248添加到单螺杆448中以助于促进与第一和第二聚烯烃240、244共混物的更好混合。在一些方面中,一种或多种任选添加剂284可与第一聚烯烃240、第二聚烯烃244、缩合催化剂280和硅烷配混物(silan cocktail)248一起加入以调节硅烷可交联聚烯烃共混物298的最终材料性质。单螺杆挤出机444被认为是反应性的,因为硅烷配混物(silan cocktail)248的接枝引发剂和硅烷交联剂与第一和第二聚烯烃240、244反应并与第一和第二聚烯烃240、244形成新的共价键。此外,反应性单螺杆挤出机444将缩合催化剂280与包含第一和第二聚烯烃240、244、硅烷配混物(silancocktail)248和任何任选添加剂284的熔融的硅烷接枝聚烯烃共混物混合在一起。所得熔融的硅烷可交联聚烯烃共混物298可使用齿轮泵(未显示)和/或模头离开反应性单螺杆挤出机444,其可将熔融的硅烷可交联聚烯烃共混物298推出为未固化屋面膜元件的形式。
在步骤404的过程中,在第一聚烯烃240、第二聚烯烃244、硅烷配混物(silancocktail)248和缩合催化剂280一起挤出时,在反应性单螺杆挤出机444中硅烷可交联共混物298可发生一定量的交联。在一些方面中,硅烷可交联聚烯烃共混物298在其离开反应性单螺杆挤出机444时可大约25%固化、大约30%固化、大约35%固化、大约40%固化、大约45%固化、大约50%固化、大约55%固化、大约60%固化、大约65%固化或大约70%。可使用凝胶试验(ASTM D2765)测定最终硅烷交联聚烯烃弹性体中的交联量。
反应性单螺杆挤出机444可配置为具有沿挤出机延伸各种长度的多个不同的温度区(例如图6中所示的Z0-Z7)。在一些方面中,各温度区可具有大约室温至大约180℃、大约120℃至大约170℃、大约120℃至大约160℃、大约120℃至大约150℃、大约120℃至大约140℃、大约120℃至大约130℃、大约130℃至大约170℃、大约130℃至大约160℃、大约130℃至大约150℃、大约130℃至大约140℃、大约140℃至大约170℃、大约140℃至大约160℃、大约140℃至大约150℃、大约150℃至大约170℃、和大约150℃至大约160℃的温度。在一些方面中,Z0可具有大约60℃至大约110℃的温度或无冷却;Z1可具有大约120℃至大约130℃的温度;Z2可具有大约140℃至大约150℃的温度;Z3可具有大约150℃至大约160℃的温度;Z4可具有大约150℃至大约160℃的温度;Z5可具有大约150℃至大约160℃的温度;Z6可具有大约150℃至大约160℃的温度;和Z7可具有大约150℃至大约160℃的温度。
在一些方面中,硅烷接枝聚烯烃弹性体的数均分子量可为大约4,000g/mol至大约30,000g/mol,包括大约5,000g/mol至大约25,000g/mol和大约6,000g/mol至大约14,000g/mol。接枝聚合物的重均分子量可为大约8,000g/mol至大约60,000g/mol,包括大约10,000g/mol至大约30,000g/mol。
参考图5和6,方法400进一步包括挤出和/或压延硅烷可交联聚烯烃弹性体或共混物298以形成包含未固化的硅烷可交联聚烯烃弹性体的顶层和底层14、38的步骤408。硅烷可交联聚烯烃弹性体或共混物298为熔化或熔融状态,此时其可流动并在离开反应性单螺杆挤出机444时成型。如上文提到,压延系统302是用于将熔融硅烷可交联聚烯烃弹性体共混物298加工成片材或膜的具有两个或更多个辊(辊之间的区域被称为辊隙)的装置。随着熔融硅烷可交联聚烯烃弹性体共混物298离开反应性单螺杆挤出机444,其在压延系统302的第一辊隙点形成硅烷可交联聚烯烃弹性体的池306。然后将硅烷可交联聚烯烃弹性体的池306分别压制或辊轧成顶层或底层14、38。可在压延过程中的任何点使用稀松布卷318将稀松布层26添加到顶层或底层14、38上。稀松布层26在结合到顶层或底层14、38上时形成部分稀松布膜322。部分稀松布膜322可进一步在分别缺失的顶层或底层14、38时压延和压制以形成未固化屋面膜元件。
仍参考图5,方法400可进一步包括在环境温度和环境湿度下交联未固化屋面膜元件的硅烷可交联聚烯烃共混物298以使该元件成型为具有大约0.85g/cm3至大约0.89g/cm3的密度的屋面膜10(见图1)的步骤412。可通过控制生产方法,包括所用催化剂的量调节交联硅烷基团的量和因此屋面膜10的最终聚合物性质。
硅烷可交联聚烯烃共混物298的交联步骤412可进行大于0至大约20小时的时期。在一些方面中,固化进行大约1小时至大约20小时、10小时至大约20小时、大约15小时至大约20小时、大约5小时至大约15小时、大约1小时至大约8小时、或大约3小时至大约6小时的时期。交联和固化过程中的温度可为大约室温、大约20℃至大约25℃、大约20℃至大约150℃、大约25℃至大约100℃、或大约20℃至大约75℃。固化过程中的湿度可为大约30%至大约100%、大约40%至大约100%、或大约50%至大约100%。
在一些方面中,使用能在接近TPV加工条件的挤出机热设置下以30比1的长L/D挤出热塑性材料的挤出机设置,其中挤出物在环境条件下交联以变成热固性。在另一些方面中,可通过蒸汽暴露加速这一过程。在刚挤出后,凝胶含量(也称为交联密度)可为大约60%,但在环境条件下96小时后,凝胶含量可达到大于大约95%。
在一些方面中,可以使用一个或多个反应性单螺杆挤出机444形成具有一种或多种类型的硅烷交联聚烯烃弹性体的屋面膜10。例如,在一些方面中,可以使用一个反应性单螺杆挤出机444以生产和挤出与屋面膜10的顶层14(见图1)相关的第一硅烷交联聚烯烃弹性体,同时可以使用第二反应性单螺杆挤出机444以生产和挤出与屋面膜10的底层38相关的第二硅烷交联聚烯烃弹性体。最终屋面膜10的复杂性、构造和所需性质决定根据图5中描绘的方法400使用的反应性单螺杆挤出机444的数量和类型。
要理解的是,概述和教导各种屋面膜10和它们各自的组分和组成的在先描述可以任何组合使用并同样好地适用于使用图5和6中所示的单步Monosil法制造屋面膜10的方法400。
硅烷交联聚烯烃弹性体物理性质
本文所用的“热塑性材料”被定义为是指在暴露于热时变软并在冷却到室温时回到其原始状态的聚合物。本文所用的“热固性材料”被定义为是指在固化时凝固并不可逆地“定形”或“交联”的聚合物。在上述Monosil或Sioplas法中,重要的是理解用于生产最终热固性硅烷交联聚烯烃弹性体或屋面膜10的各种不同材料的热塑性和热固性性质的小心平衡。使用反应性双螺杆挤出机和/或反应性单螺杆挤出机混合和反应的各中间聚合物材料是热固性材料。相应地,硅烷接枝聚烯烃共混物276和硅烷可交联聚烯烃共混物298是热塑性塑料并可通过加热软化以使各自的材料可流动。一旦将硅烷可交联聚烯烃共混物298挤出、模制、压制和/或成型为未固化屋面膜元件或各自的其它制品,硅烷可交联聚烯烃共混物298可在环境温度和环境湿度下开始交联或固化以形成包含一种或多种硅烷交联聚烯烃共混物的屋面膜10(或其它最终产品形式)。
由于使用这些材料提供的潜在节能,硅烷可交联聚烯烃共混物298和相应的硅烷交联聚烯烃共混物的热塑性/热固性行为对本文中公开的各种组合物和制品(例如图1中所示的屋面膜10)是重要的。例如,由于能在环境温度和环境湿度下固化该硅烷可交联聚烯烃共混物298,制造商可节省相当大量的能量。在工业中通常通过施加显著量的能量以热或蒸汽处理可交联聚烯烃298来进行这一固化过程。用环境温度和/或环境湿度固化本发明的硅烷可交联聚烯烃共混物298的能力不是可交联聚烯烃必定固有的能力。相反,这一能力或性质取决于该硅烷可交联聚烯烃共混物298的相对较低密度。在一些方面中,不使用除在挤出机中提供的那些外的附加固化炉、加热炉、蒸汽炉或其它形式的产热机械形成硅烷交联聚烯烃弹性体。
本公开的硅烷交联聚烯烃弹性体的比重可低于本领域中所用的现有TPV和EPDM配制剂的比重。这些材料的降低的比重可产生较低重量的部件,因此有利于屋顶工人和负责安装本公开的屋面膜10的其他人的额外易组装性。例如,与可具有大于2.00g/cm3的比重的常规TPV材料和可具有2.0g/cm3至3.0g/cm3的比重的常规EPDM材料相比,本公开的硅烷交联聚烯烃弹性体的比重可为大约0.80g/cm3至大约1.50g/cm3、大约1.25g/cm3至大约1.45g/cm3、大约1.30g/cm3至大约1.40g/cm3、大约1.25g/cm3、大约1.30g/cm3、大约1.35g/cm3、大约1.40g/cm3、大约1.45g/cm3、大约1.50g/cm3、小于1.75g/cm3、小于1.60g/cm3、小于1.50g/cm3或小于1.45g/cm3。
提供相对于两种现有EPDM材料,本公开的示例性硅烷交联聚烯烃弹性体(即“硅烷交联聚烯烃弹性体”)的应力/应变行为。特别地,图7显示与EPDM化合物A和EPDM化合物B的应力/应变曲线之间的面积相比,本公开的硅烷交联聚烯烃(在图7中标作“硅烷交联聚烯烃弹性体”)的应力/应变曲线之间的较小面积。该硅烷交联聚烯烃弹性体的应力/应变曲线之间的这种较小面积对屋面膜10是理想的。弹性体材料通常在反复受到应力时具有存在显著能量损失的非线性应力/应变曲线。本公开的硅烷交联聚烯烃弹性体可表现出更大弹性和更小的粘弹性(例如具有线性曲线并表现出极低的能量损失)。本文所述的硅烷交联聚烯烃弹性体的实施方案没有将任何填料或增塑剂并入这些材料中,因此它们的相应应力/应变曲线没有或没有表现出任何Mullins效应和/或Payne效应。这些硅烷交联聚烯烃弹性体的Mullins效应的缺乏归因于缺乏添加到硅烷交联聚烯烃共混物中的任何填料或增塑剂,因此应力/应变曲线不依赖于之前遇到的最大荷载,其中没有瞬时和不可逆软化。这些硅烷交联聚烯烃弹性体的Payne效应的缺乏归因于缺乏添加到硅烷交联聚烯烃共混物中的任何填料或增塑剂,因此应力/应变曲线不依赖于之前遇到的小应变幅,其中不存在基于应变幅的粘弹性储能模量变化。
该硅烷交联聚烯烃弹性体或屋面膜10可表现出根据ASTM D 395(22hrs@23℃、70℃、80℃、90℃、125℃和/或175℃)测得的大约5.0%至大约30.0%、大约5.0%至大约25.0%、大约5.0%至大约20.0%、大约5.0%至大约15.0%、大约5.0%至大约10.0%、大约10.0%至大约25.0%、大约10.0%至大约20.0%、大约10.0%至大约15.0%、大约15.0%至大约30.0%、大约15.0%至大约25.0%、大约15.0%至大约20.0%、大约20.0%至大约30.0%、或大约20.0%至大约25.0%的压缩变定。
在另一些实施方案中,该硅烷交联聚烯烃弹性体或屋面膜10可表现出根据ASTM D395(22hrs@23℃、70℃、80℃、90℃、125℃和/或175℃)测得的大约5.0%至大约20.0%、大约5.0%至大约15.0%、大约5.0%至大约10.0%、大约7.0%至大约20.0%、大约7.0%至大约15.0%、大约7.0%至大约10.0%、大约9.0%至大约20.0%、大约9.0%至大约15.0%、大约9.0%至大约10.0%、大约10.0%至大约20.0%、大约10.0%至大约15.0%、大约12.0%至大约20.0%、或大约12.0%至大约15.0%的压缩变定。
该硅烷交联聚烯烃弹性体或屋面膜10可表现出使用密度测量、差示扫描量热法(DSC)、X-射线衍射、红外光谱学和/或固态核磁谱学测定的大约5%至大约40%、大约5%至大约25%、大约5%至大约15%、大约10%至大约20%、大约10%至大约15%、或大约11%至大约14%的结晶度。如本文中公开,DSC用于测量熔化焓以计算各自样品的结晶度。
该硅烷交联聚烯烃弹性体或屋面膜10可表现出根据差示扫描量热法(DSC)使用在5℃/min或10℃/min的速率下的第二加热流程测得的大约-75℃至大约-25℃、大约-65℃至大约-40℃、大约-60℃至大约-50℃、大约-50℃至大约-25℃、大约-50℃至大约-30℃或大约-45℃至大约-25℃的玻璃化转变温度。
该硅烷交联聚烯烃弹性体或屋面膜10可表现出根据ASTM D2244测得的大约0.25ΔE至大约2.0ΔE、大约0.25ΔE至大约1.5ΔE、大约0.25ΔE至大约1.0ΔE、或大约0.25ΔE至大约0.5ΔE的天候色差(a weathering color difference)。
实施例
提供下列非限制性实施例作为示例性实施方案以进一步概述本公开的方面。
材料
所有化学品、成分和前体获自商业供应商并按来样使用而不进一步提纯。
实施例1–硅烷接枝聚烯烃弹性体的制备
通过根据本公开中概述的上述方法之一与3.0重量%SILAN RHS 14/032或SILFIN29一起挤出82.55重量%ENGAGETM 8842和14.45重量%MOSTENTMTB 003以形成硅烷接枝聚烯烃弹性体,制造实施例1(Ex.1)或ED76-4A。实施例1硅烷接枝聚烯烃弹性体然后使用各种缩合催化剂和填料挤出以形成适用于屋面膜的顶层和底层14、38(如下文在实施例2中所述)的硅烷可交联聚烯烃弹性体。实施例1硅烷接枝聚烯烃弹性体的组成提供在下表1中。
表1
成分 | 实施例1 |
ENGAGE 8842 | 82.55 |
MOSTEN TB 003 | 14.45 |
SILFIN 29 | 3.00 |
总计 | 100 |
实施例2–屋面膜的制备
在这一实施例中,使用相同的顶层和底层14、38制造单合叠屋面膜10的一个实施方案。特别地,通过与1.0重量%二月桂酸二辛基锡(DOTL)缩合催化剂一起挤出29.0重量%硅烷接枝聚烯烃弹性体(来自实施例1)和70.0重量%乙烯基硅烷涂布的二氢氧化镁Mg(OH)2(MDH)以形成硅烷可交联聚烯烃弹性体共混物,制造顶层和底层14、38。该共混物然后挤出和压延以提供未固化屋面膜元件的各自顶层和底层14、38。未固化屋面膜元件的层14、38的硅烷可交联聚烯烃弹性体然后在环境温度和湿度下固化以形成屋面膜10。在这一实施例中形成的屋面膜10的组成提供在下表2中。
实施例3–屋面膜的制备
在这一实施例中,使用相同的顶层和底层14、38制造单合叠屋面膜10的另一实施方案。特别地,通过与1.0重量%二月桂酸二辛基锡(DOTL)缩合催化剂一起挤出29.0重量%硅烷接枝聚烯烃弹性体(来自实施例1)和70.0重量%硬脂酸涂布的二氢氧化镁Mg(OH)2(MDH)以形成硅烷可交联聚烯烃弹性体共混物,制造顶层和底层14、38。该共混物然后挤出和压延以提供未固化屋面膜元件的各自顶层和底层14、38。未固化屋面膜元件的层14、38的硅烷可交联聚烯烃弹性体然后在环境温度和湿度下固化以形成屋面膜10。在这一实施例中形成的屋面膜10的组成提供在下表2中。
表2–屋面膜的比较
现在参考图8,相对于对比EPDM过氧化物交联树脂和对比EPDM硫交联树脂提供实施例1的热稳定性。如所示,实施例1可在150℃下保持其弹性性质的接近90%大于500小时。实施例1中提供的弹性性质的保持代表本文中公开的各个本发明的硅烷交联聚烯烃弹性体。根据使用在150℃下大于100hrs、大于200hrs、大于300hrs、大于400hrs和大于500hrs的应力松弛测量测定,由这些硅烷交联聚烯烃弹性体制成的屋面元件可保持其弹性性质的一直到60%、70%、80%或90%。
现在参考图9,Ex.1经过4,000小时的时期提供的压缩变定值证实优异地长期保持用于制造屋面膜10的硅烷交联聚烯烃弹性体材料的弹性性质。如所提供的,Ex.1硅烷交联聚烯烃弹性体材料保持根据ASTM D 395(30%@110℃)测得的35%或更低的压缩变定。这些屋面膜10材料的代表性实施例提供屋面膜10中所用的这些硅烷交联聚烯烃弹性体材料在暴露于模拟室外天候或老化的热时长时间保持其弹性(压缩变定%)的能力。
对本公开而言,术语“耦合”(以其所有形式,couple、coupling、coupled等)通常是指两个组件直接或间接地互相连接。这样的连接可以在性质上是静态的或在性质上可活动。这样的连接可用两个组件和任何附加的中间构件(其与彼此或与这两个组件一体成型为单件整体)实现。除非另行指明,这样的连接可以在性质上是永久的或在性质上可移除或可松开。
也重要的是指出,示例性实施方案中所示的装置的元件的构造和布置仅是示例性的。尽管在本公开中仅详细描述本创新的若干实施方案,但考察本公开的技术人员容易认识到,许多修改是有可能的(例如各种元件的尺寸、维度、结构、形状和比例、参数值、安装布置、材料使用、颜色、取向等的变化)而不实质背离所列举的主题的新颖的教导和优点。例如,显示为一体成型的元件可由多个部件构成或显示为多个部件的元件可一体成型,可以反转或以其它方式改变界面的操作,可以改变该系统的结构和/或构件或连接器或其它元件的长度或宽度,可以改变在元件之间提供的调节位置的性质或数量。应该指出,该系统的元件和/或组装件可由提供足够强度或耐久性的多种多样的材料以多种多样的颜色、质地和组合构成。相应地,所有这样的修改意在包括在本创新的范围内。可对所需和其它示例性实施方案的设计、操作条件和布置作出其它取代、修改、变化和省略而不背离本创新的精神。
要理解的是,任何所述方法或在所述方法内的步骤可与其它公开的方法或步骤组合以形成本装置的范围内的结构。本文中公开的示例性结构和方法用于举例说明并且不应被解释为限制。
上文的描述被认为仅是例举的实施方案的描述。本领域技术人员和制造或使用该装置的人员会想到该装置的修改。因此,要理解的是,附图中显示和上文描述的实施方案仅用于举例说明并且无意限制制品、方法和组合物的范围,它们由根据专利法的原则,包括等同原则解释的下列权利要求书界定。
非限制性实施方案的列表
实施方案A是一种屋面膜,其包含:包含阻燃剂和具有小于0.90g/cm3的密度的第一硅烷交联聚烯烃弹性体的顶层;稀松布层;和包含阻燃剂和具有小于0.90g/cm3的密度第二硅烷交联聚烯烃弹性体的底层,其中该单合叠屋面膜的顶层和底层都表现出根据ASTM D395(22hrs@70℃)测得的大约5.0%至大约35.0%的压缩变定。
实施方案A的屋面膜,其中所述压缩变定为大约10%至大约30%。
实施方案A或具有任何插入特征的实施方案A的屋面膜,其中第一和第二硅烷交联聚烯烃弹性体都表现出大约5%至大约25%的结晶度。
实施方案A或具有任何插入特征的实施方案A的屋面膜,其中第一和第二硅烷交联聚烯烃弹性体具有大约-75℃至大约-25℃的玻璃化转变温度。
实施方案A或具有任何插入特征的实施方案A的屋面膜,其中第一和第二硅烷交联聚烯烃弹性体各自包含具有小于0.86g/cm3的密度的第一聚烯烃、第二聚烯烃、硅烷交联剂、接枝引发剂和缩合催化剂。
实施方案A或具有任何插入特征的实施方案A的屋面膜,其中所述密度为大约0.85g/cm3至大约0.89g/cm3。
实施方案A或具有任何插入特征的实施方案A的屋面膜,其中该单合叠屋面膜表现出根据ASTM D2244测得的大约0.25ΔE至大约2.0ΔE的天候色差(a weathering colordifference)。
实施方案A或具有任何插入特征的实施方案A的屋面膜,其中第一硅烷交联聚烯烃弹性体和第二硅烷交联聚烯烃弹性体在化学上彼此不同。
实施方案B是一种制造屋面膜的方法,所述方法包括:挤出第一硅烷可交联聚烯烃弹性体以形成顶层;挤出第二硅烷可交联聚烯烃弹性体以形成底层;将稀松布层压延在顶层和底层之间以形成未固化屋面膜元件;和使所述未固化屋面膜元件中的顶层和底层的硅烷可交联聚烯烃弹性体在固化温度和固化湿度下交联以形成单合叠屋面膜,其中所述单合叠屋面膜的顶层和底层都表现出根据ASTM D 395(22hrs@70℃)测得的大约5.0%至大约35.0%的压缩变定。
实施方案B的方法,其中第一硅烷可交联聚烯烃弹性体和第二硅烷可交联聚烯烃弹性体在化学上彼此不同。
实施方案B或具有任何插入特征的实施方案B的方法,其中所述固化温度是环境温度。
实施方案B或具有任何插入特征的实施方案B的方法,其中所述固化湿度是环境湿度。
实施方案B或具有任何插入特征的实施方案B的方法,其中第一和第二硅烷可交联聚烯烃弹性体各自包含具有小于0.86g/cm3的密度的第一聚烯烃、第二聚烯烃、硅烷交联剂、接枝引发剂和缩合催化剂。
实施方案B或具有任何插入特征的实施方案B的方法,其中所述单合叠屋面膜表现出根据ASTM D2244测得的大约0.25ΔE至大约2.0ΔE的天候色差(a weathering colordifference)。
实施方案B或具有任何插入特征的实施方案B的方法,其中所述单合叠屋面膜表现出根据EN ISO 11925-2表面暴露试验测得的分类D的阻燃等级。
实施方案C是一种制造高负荷阻燃热塑性聚烯烃(TPO)屋面膜的方法,所述方法包含:将硅烷接枝聚烯烃弹性体、阻燃剂和缩合催化剂添加到反应性单螺杆挤出机中以产生硅烷可交联聚烯烃弹性体;压延所述硅烷可交联聚烯烃弹性体以形成顶层和底层;将稀松布层压延在顶层和底层之间以形成未固化屋面膜元件;和使所述未固化屋面膜元件中的顶层和底层的硅烷可交联聚烯烃弹性体在环境温度和环境湿度下交联以形成热塑性聚烯烃(TPO)屋面膜,其中所述热塑性聚烯烃(TPO)屋面膜的顶层和底层都表现出根据ASTM D 395(22hrs@70℃)测得的大约5.0%至大约35.0%的压缩变定。
实施方案C的方法,其中所述顶层和底层在化学上彼此相同。
实施方案C或具有任何插入特征的实施方案C的方法,其中所述单合叠屋面膜表现出根据EN ISO 11925-2表面暴露试验测得的分类D的阻燃等级。
实施方案C或具有任何插入特征的实施方案C的方法,其中所述硅烷接枝聚烯烃弹性体包含具有小于0.86g/cm3的密度的第一聚烯烃、第二聚烯烃、硅烷交联剂、接枝引发剂。
实施方案C或具有任何插入特征的实施方案C的方法,其中所述高负荷阻燃热塑性聚烯烃(TPO)屋面膜表现出根据ASTM D2244测得的大约0.25ΔE至大约2.0ΔE的天候色差(a weathering color difference)。
Claims (15)
1.一种屋面膜,其包含:
包含阻燃剂和具有小于0.90g/cm3的密度的第一硅烷交联聚烯烃弹性体的顶层;
稀松布层;和
包含阻燃剂和具有小于0.90g/cm3的密度第二硅烷交联聚烯烃弹性体的底层,
其中根据ASTM D 2765测量,所述屋面膜的凝胶含量在60%至95%之间;
其中所述屋面膜的顶层和底层都表现出根据ASTM D 395(22hrs@70℃)测得的5.0%至35.0%的压缩变定。
2.权利要求1的屋面膜,其中所述压缩变定为10%至30%。
3.权利要求1或权利要求2的屋面膜,其中第一和第二硅烷交联聚烯烃弹性体都表现出5%至25%的结晶度。
4.权利要求1或权利要求2的屋面膜,其中第一和第二硅烷交联聚烯烃弹性体具有-75℃至-25℃的玻璃化转变温度。
5.权利要求1或权利要求2的屋面膜,其中第一和第二硅烷交联聚烯烃弹性体各自包含具有小于0.86g/cm3的密度的第一聚烯烃、第二聚烯烃、硅烷交联剂、接枝引发剂和缩合催化剂。
6.权利要求1或权利要求2的屋面膜,其中第一硅烷交联聚烯烃弹性体的所述密度为0.85g/cm3至0.89g/cm3;第二硅烷交联聚烯烃弹性体的所述密度为0.85g/cm3至0.89g/cm3。
7.权利要求1或权利要求2的屋面膜,其中所述单合叠屋面膜表现出根据ASTM D2244测得的0.25ΔE至2.0ΔE的天候色差。
8.权利要求1或权利要求2的屋面膜,其中第一硅烷交联聚烯烃弹性体和第二硅烷交联聚烯烃弹性体在化学上彼此不同。
9.一种制造屋面膜的方法,所述方法包含:
将第一硅烷接枝聚烯烃弹性体、阻燃剂和缩合催化剂添加到反应性单螺杆挤出机中以产生第一硅烷可交联聚烯烃弹性体;
将第二硅烷接枝聚烯烃弹性体、阻燃剂和缩合催化剂添加到反应性单螺杆挤出机中以产生第二硅烷可交联聚烯烃弹性体;
挤出并压延第一硅烷可交联聚烯烃弹性体以形成顶层;
挤出并压延第二硅烷可交联聚烯烃弹性体以形成底层;
将稀松布层压延在顶层和底层之间以形成未固化屋面膜元件;和
使所述未固化屋面膜元件中的顶层和底层的硅烷可交联聚烯烃弹性体在环境温度和环境湿度下交联以形成单合叠屋面膜,
其中根据ASTM D 2765测量,所述屋面膜的凝胶含量在60%至95%之间;
其中所述屋面膜的顶层和底层都表现出根据ASTM D 395(22hrs@70℃)测得的5.0%至35.0%的压缩变定。
10.权利要求9的方法,其中第一硅烷可交联聚烯烃弹性体和第二硅烷可交联聚烯烃弹性体在化学上彼此不同。
11.权利要求9或权利要求10的方法,其中第一和第二硅烷可交联聚烯烃弹性体各自包含具有小于0.86g/cm3的密度的第一聚烯烃、第二聚烯烃、硅烷交联剂、接枝引发剂和缩合催化剂。
12.权利要求9或权利要求10的方法,其中所述屋面膜表现出根据ASTM D2244测得的0.25ΔE至2.0ΔE的天候色差。
13.权利要求9或权利要求10的方法,其中所述屋面膜表现出根据ENISO 11925-2表面暴露试验测得的分类D的阻燃等级。
14.权利要求10的方法,其中第一硅烷可交联聚烯烃弹性体和第二硅烷可交联聚烯烃弹性体在化学上不是彼此不同。
15.权利要求9的方法,其中所述屋面膜是高负荷阻燃热塑性聚烯烃(TPO)屋面膜。
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