CN115038762A - 用于制作耐火三元乙丙epdm橡胶的组合物及方法 - Google Patents

用于制作耐火三元乙丙epdm橡胶的组合物及方法 Download PDF

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Publication number
CN115038762A
CN115038762A CN202180010169.3A CN202180010169A CN115038762A CN 115038762 A CN115038762 A CN 115038762A CN 202180010169 A CN202180010169 A CN 202180010169A CN 115038762 A CN115038762 A CN 115038762A
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Prior art keywords
composition
membrane
film
epdm
vulcanized
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O·福金加
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Carlyle Building Materials Co ltd
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Carlyle Building Materials Co ltd
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Publication of CN115038762A publication Critical patent/CN115038762A/zh
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Abstract

本文中的公开内容涉及三元乙丙(EPDM)橡胶。更明确来说，本公开涉及耐火EPDM橡胶。在一个实施例中，所述耐火EPDM是用于使建筑物抗风化的膜。在另一实施例中，所述耐火EPDM膜是屋面材料。在其它实施例中，所述耐火EPDM橡胶可在电场中使用。

Description

用于制作耐火三元乙丙EPDM橡胶的组合物及方法
相关申请案的交叉参考
本申请案主张2020年3月12日申请的相同标题的序列号为62/988,558的美国临时专利申请案的优先权；所述申请案的全部公开内容出于所有目的以其全文引用方式并入本文中。
技术领域
本文中的公开内容涉及三元乙丙(EPDM)橡胶。更明确来说，本公开涉及耐火EPDM橡胶。在一个实施例中，耐火EPDM橡胶用于使建筑物抗风化，特定来说，用作用于立面应用的膜。
背景技术
三元乙丙(EPDM)橡胶具有许多显著的性质，例如(仅举几例)耐热性、耐化学性、低导电性、在从-50℉到350℉的温度范围下的稳定性、低温下的柔韧性及耐候性。EPDM具成本效益且可以各种方式制造，包含定制模制及挤压。EPDM在汽车行业中具有众多应用(例如软管、密封件、O形环、垫片、蓄能器气囊、电线及电缆连接器以及绝缘体、隔膜及挡风雨条)；建筑(例如屋面及防水)；HVAC(例如压缩机垫圈、管道、垫片及密封件)；及许多其它行业。
EPDM橡胶的主要缺点是其易燃性。在建筑行业中，耐火通常通过两种不同方法实现，首先是添加外部阻燃剂且其次是使用压载(ballasted)屋顶系统。因此，需要一种耐火EPDM橡胶。
发明内容
本文中的公开内容涉及耐火EPDM橡胶。在一个实施例中，所述EPDM包含三元乙丙(EPDM)聚合物、氢氧化铝、磷酸三(2-乙基己基)酯、消耗性石墨及聚丁二烯的马来酸酐加合物；其中所述组合物不含矿物油。前述组合物还可包含固化剂，例如硫或硫释放化合物。前述组合物还可包含活化剂及/或促进剂，例如氧化锌、硬脂酸、二硫化四苄基秋兰姆。在一个实施例中，所述组合物不含卤素。在一个实施例中，所述组合物不含三氧化锑。在一个实施例中，所述组合物不含卤素且不含三氧化锑。
耐火EPDM配方的非限制性实例是硫、二硫化四苄基秋兰姆、N-环己基-2-苯并噻唑基次磺酰胺、氧化锌、硬脂酸、聚丁二烯的马来酸酐加合物、可膨胀石墨、碳黑N550、磷酸三(2-乙基己基)酯及氢氧化铝。在一个实施例中，所述组合物不包含矿物油。在一个实施例中，所述组合物可不含卤素。在一个实施例中，所述组合物可不含三氧化锑。在一个实施例中，所述组合物可既不含卤素又不含三氧化锑。
在本发明的另一方面中，提供一种用于制作EPDM屋面膜的方法，其包括以下步骤：使用压延或辊模挤出机加工先前实施例中的任一者的组合物的同质混合物；及在有或没有压力的情况下将所述膜热固化。
具体实施方式
三元乙丙(EPDM)橡胶是一种由可经由硫硫化交联的乙烯、丙烯及二烯单体制成的合成橡胶化合物。因为EPDM是纯碳氢化合物，因此其可能容易着火。本公开涉及耐火的EPDM橡胶。特定来说，本公开涉及符合欧洲建筑材料分类EN 13501-1 B类的EPDM橡胶。
定义
在下文描述中，许多术语被广泛使用。以下非限制性定义提供对说明书及权利要求书的清晰且一致的理解，包含被赋予此类术语的示范性范围。
当在本公开中使用术语“一个”、“一(a或an)”时，除非另有指示，否则它们意味着“至少一个”或“一或多个”。
如本文中使用，术语“发明”或“本发明”希望是非限制性的且不希望指特定发明的任何单个实施例，而是涵盖如说明书及权利要求中所描述的所有可能实施例及其等效物。
当组成成分的比例以百分比表示时，它们应被理解为表示为每百份橡胶的份数(PHR)。
组合物
EPDM橡胶化合物通常包含EPDM聚合物，(提供防水及弹性性质)及以下中的一或多种：(1)油填充剂；(2)交联剂/固化剂；(3)加工助剂；(4)促进剂(其有助于硫化过程)；(5)抗氧剂(用于耐候性)；(6)抗臭氧剂(用于抗臭氧)；(7)柔软剂及增塑剂(其改进柔韧性)；(8)填充剂，增强型(其增加弹性模数及韧性)及/或非增强型；(9)阻燃剂；及(10)其它试剂。
各种二烯单体可用于形成EPDM聚合物。合适的二烯单体的非限制性实例包含亚乙基降冰片烯、二环戊二烯、乙烯基降冰片烯、烷基二环戊二烯、1,4-戊二烯、1,4-己二烯、1,5-己二烯、1,4-庚二烯、2-甲基-1,5-己二烯、环辛二烯、1,4-辛二烯、1,7-辛二烯、5-亚乙基-2-降冰片烯、5-正亚丙基-2-降冰片烯及5-(2-甲基-2-丁烯基)-2-降冰片烯及其混合物。
在某些实施例中，油可被卤化。
合适的交联剂/固化剂的非限制性实例包含过氧化物，例如α-枯基过氧化氢、过氧化甲乙酮、过氧化氢、过氧化乙酰丙酮、叔丁基过氧化氢、过氧化苯甲酸叔丁酯、2,5-双(叔丁基过氧)-2,5-二甲基己烯、十二烷基过氧化物、过氧化苯甲酰基、过氧化2,4-二氯苯甲酰、过氧化二苯甲酰、过氧化双(对单亚甲基-苯甲酰)、过氧化双(对硝基苯甲酰)、过氧化苯乙酰、对醌二肟、过氧化铅、过氧化锌、过氧化钡、过氧化铜、过氧化钾、过氧化银、过氧化钠、过氧化钙、金属过氧硼酸盐、过氧铬酸盐、过氧二碳酸盐、过氧二磷酸盐、过二硫酸盐、过氧锗酸盐、过氧钼酸盐、过氧硝酸盐、过氧化镁、过氧化焦磷酸钠及其混合物。交联剂/固化剂的其它非限制性实例包括硫与促进剂、树脂及辐射。
合适的加工助剂的非限制性实例包括石油树脂、脂肪酸皂、脂肪酸酯、石蜡、聚乙烯蜡、EVA蜡、酚醛树脂、乙烯丙烯酸共聚物及其混合物。
合适的促进剂的非限制性实例包含硫、硫醇、苯并噻唑、秋兰姆、氧化锌、硬脂酸、苯并噻唑次磺酰胺、二硫代氨基甲酸酯、硫脲、N-环己基-2-苯并噻唑次磺酰胺(CBS)、N-叔丁基-2-苯并噻唑次磺酰胺(TBBS)、2,2'-二硫代双(苯并噻唑)(MBTS)、二硫化四甲基秋兰姆(TMTD)、一硫化四甲基秋兰姆(TMTM)、二丁基二硫代氨基甲酸锌(ZDBC)、二甲基二硫代氨基甲酸锌(ZDM)、二硫化四苄基秋兰姆(TBzTD)、二邻甲苯基胍(DOTG)、二苯基胍(DPG)、4,4'-二硫代二吗啉(DTDM)、六亚甲基四胺(HMTA)、巯基苯并噻唑(MBT)、二丁基二硫代氨基甲酸镍(NDBDC)、N-(环己基硫代)邻苯二甲酰亚胺(PVI)、二烷基二硫代磷酸铜(CUT)、二硫代己内酰胺、锌胺-二硫代磷酸(ZAT)、二硫化四丁基秋兰姆(TBTS)、二苄基二硫代氨基甲酸锌(ZBEC)、二烷基二硫代磷酸锌(ZDDP)、二乙基二硫代氨基甲酸锌(ZDEC)、乙基苯基二硫代氨基甲酸锌(ZEPD)、四硫化双五亚甲基秋兰姆(DPTT)、2-巯基苯并噻唑；2,2'-二硫代苯并噻唑、N-环己基苯并噻唑-2-次磺酰胺、N-叔丁基苯并噻唑-2-次磺酰胺、二硫化四甲基秋兰姆、一硫化四甲基秋兰姆、二硫化四丁基秋兰姆、一硫化四乙基秋兰姆、六硫化双五甲撑秋兰姆、N,N-二丁基硫脲、N,N-二乙基硫脲、载硫促进剂、其它有机促进剂及其混合物。
合适的软化剂及增塑剂的非限制性实例包含石蜡油、环烷油、邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)、邻苯二甲酸二辛酯(DOP)、邻苯二甲酸二己酯、磷酸异癸基二苯酯(例如
Figure BDA0003755409920000041
148)、磷酸三(2-乙基己基)酯(TEHP)及其混合物。
合适的填充剂的非限制性实例包括碳黑、粘土、滑石、煤粉、二氧化硅、云母、碳酸钙、其它有机材料及其混合物。
合适的阻燃剂的非限制性实例包括氢氧化铝(也被称为三氢氧化铝)、氢氧化镁、可膨胀石墨、硼酸锌、多磷酸铵、三聚氰胺聚磷酸盐、氧化锑及其混合物。
其它合适试剂的非限制性实例包括聚丁二烯的马来酸酐加合物、抗降解剂(例如蜡及石蜡产品)、聚(1,2-二氢-2,2,4-三甲基喹啉(TMQ)、甲基-2-巯基苯并咪唑(MMBI)、N-异丙基-N'-苯基-1,4-苯二胺(IPPD)、N-(1,3-二甲基丁基)-N'-苯基-对苯二胺(6PPD)、丁基化羟基甲苯(BHT))及其混合物。
在某些实施例中，EPDM橡胶化合物包括阻燃剂。在此类实施例中，阻燃剂的量可为从约2％到约90％。在某些实施例中，阻燃剂是氢氧化铝、可膨胀石墨或两者。在此类实施例中，氢氧化铝的量可为从约10％到约90％，且可膨胀石墨的量可为从约2％到约25％。
在某些实施例中，EPDM橡胶化合物包含交联剂。在此类实施例中，交联剂的量可为从约1％到约10％。在某些实施例中，交联剂可为聚丁二烯的马来酸酐加合物。在此类实施例中，聚丁二烯的马来酸酐加合物的量可为从约1％到约10％。
在某些实施例中，EPDM橡胶化合物包含增塑剂。在此类实施例中，增塑剂的量可为从约1％到约60％。在某些实施例中，增塑剂不是矿物油。在某些实施例中，增塑剂是磷酸三(2-乙基己基)酯。在此类实施例中，磷酸三(2-乙基己基)酯的量可为从约1％到25％。
在某些实施例中，EPDM橡胶化合物包含填充剂。在此类实施例中，填充剂的量可为从约1％到约50％。在某些实施例中，填充剂可为碳黑。在此类实施例中，碳黑的量可为从约1％到约50％。
在某些实施例中，EPDM橡胶化合物包含固化剂。在此类实施例中，固化剂的量可为从约1％到约5％。在某些实施例中，固化剂是硫。在此类实施例中，硫的量可为从约1％到约3％。
在某些实施例中，EPDM橡胶化合物包含促进剂。在此类实施例中，促进剂的量可为从约1％到约10％。在某些实施例中，促进剂是二硫化四苄基秋兰姆、氧化锌、硬脂酸或其组合。在此类实施例中，二硫化四苄基秋兰姆的量可为从约1％到约8％，氧化锌的量可为从约1％到约10％，且硬脂酸的量可为从约1％到约5％。
在某些实施例中，EPDM橡胶化合物包含EPDM、氢氧化铝、消耗性石墨及聚丁二烯的马来酸酐加合物。在一个实施例中，所述化合物不含矿物油。在一个实施例中，所述化合物不含卤素。在一个实施例中，所述化合物不含三氧化锑。在一个实施例中，所述化合物既不含卤素又不含三氧化锑。
在某些实施例中，EPDM橡胶化合物包含EPDM、硫、二硫化四苄基秋兰姆、N-环己基-2-苯并噻唑次磺酰胺、氧化锌、硬脂酸、聚丁二烯的马来酸酐加合物、Carbofoil L-120、碳黑n550、磷酸三(2-乙基己基)酯；及氢氧化铝。在一个实施例中，所述化合物不含矿物油。在一个实施例中，所述化合物不含卤素。在一个实施例中，所述化合物不含三氧化锑。在一个实施例中，所述化合物既不含卤素又不含三氧化锑。
方法
制作EPDM橡胶产品通常涉及两个步骤：将混合物加工成产品，及接着，将所述产品固化。为了形成同质混合物，可使用高剪切混合机，例如密炼机(internal mixer)将成分混合在一起。合适的混合器的非限制性实例包含班伯里(Banbury)混合器，其是密炼机或研磨机或挤出机。在加工步骤期间，可使用模制、压延或挤出(例如，辊模)将同质混合物形成为其最终形状。可使用各种方法进行固化，包含加热(有或没有压力)及辐射(有或没有压力)。
在一个实施例中，本文中描述的EPDM橡胶化合物可被加工成屋顶材料，特别是用于立面应用的EPDM膜。膜通常为约0.5毫米(mm)厚到约3毫米厚。膜通常由一层EPDM橡胶或可被压延或层压在一起的两层或更多层EPDM橡胶制成。在一些实施例中，膜可包含在一侧或两侧中或层压在一侧或两侧上的织物层。在一些实施例中，膜可包含粘附到一侧或两侧的玻璃纤维网格布(glass scrim)层。
实例
实例1-EPDM橡胶配方
在此实例中，使用以下配方制作各种耐火EPDM橡胶膜。
Figure BDA0003755409920000051
Figure BDA0003755409920000061
*PHR＝每百份橡胶的份数
将上述量的材料添加到班伯里混合器中，且混合5分钟从而达到135℃的最终温度。将混合物放到压片机上并形成8毫米厚的板坯。板坯被加工成1.0及1.2毫米厚的片材。任选地，可将两个较薄的片材层压成相同厚度的一个膜。施加聚酰胺衬垫，并将膜放置在辊上。将辊装载到热风烘箱中以进行加热固化。
实例2–明火测试
在此实例中，实例1的EPDM膜通过与单个火焰直接接触进行评估。来自喷枪的火焰在膜上保持30秒，单帧源测试EN 11925-2 B、C或D类。膜在火焰接触它的地方发出红光。然而，一旦火焰被移除，余火便立即熄灭。膜显露大约10毫米x20毫米的燃烧点。
实例3–单个燃烧项目测试
使用单个燃烧项目(SBI)测试(EN 13823)评估实例1的EPDM膜。SBI测试测量横向火焰蔓延、热释放速率、产生焰滴的倾向及烟雾产生速率。将EPDM膜的样品安装到垂直表面并放置在罩中。在收集基线数据之后，30KW火焰冲击膜21分钟。根据上述因素，在20分钟时段内评估膜的性能。
实例4–额外EPDM橡胶配方
额外EPDM橡胶配方在下表中展示。量基于每百份橡胶的份数(PHR)。
Figure BDA0003755409920000062
Figure BDA0003755409920000071
Figure BDA0003755409920000081
Figure BDA0003755409920000091
Figure BDA0003755409920000092
Figure BDA0003755409920000101
Figure BDA0003755409920000111
Figure BDA0003755409920000121
Figure BDA0003755409920000122
Figure BDA0003755409920000131
Figure BDA0003755409920000141
Figure BDA0003755409920000151
Figure BDA0003755409920000152
Figure BDA0003755409920000161
Figure BDA0003755409920000171
Figure BDA0003755409920000181
Figure BDA0003755409920000182
Figure BDA0003755409920000191
Figure BDA0003755409920000201
Figure BDA0003755409920000211
Figure BDA0003755409920000221
Figure BDA0003755409920000231
Figure BDA0003755409920000241
Figure BDA0003755409920000251
Figure BDA0003755409920000261
Figure BDA0003755409920000271
Figure BDA0003755409920000281
Figure BDA0003755409920000291
Figure BDA0003755409920000301
Figure BDA0003755409920000311
Figure BDA0003755409920000321
Figure BDA0003755409920000331
Figure BDA0003755409920000341
Figure BDA0003755409920000342
Figure BDA0003755409920000351
Figure BDA0003755409920000361
Figure BDA0003755409920000371
Figure BDA0003755409920000372
Figure BDA0003755409920000381
Figure BDA0003755409920000391
Figure BDA0003755409920000401
Figure BDA0003755409920000402
Figure BDA0003755409920000411
Figure BDA0003755409920000421
Figure BDA0003755409920000431
Figure BDA0003755409920000432
Figure BDA0003755409920000441
Figure BDA0003755409920000451
Figure BDA0003755409920000461
Figure BDA0003755409920000462
Figure BDA0003755409920000471
实例5—配方的评估
评估来自实例4的选择配方的物理性质及初步阻燃测试。结果总结在下表中(“MR”是最低要求)。
Figure BDA0003755409920000481
Figure BDA0003755409920000491
Figure BDA0003755409920000492
Figure BDA0003755409920000501
Figure BDA0003755409920000502
Figure BDA0003755409920000511
Figure BDA0003755409920000512
Figure BDA0003755409920000521
Figure BDA0003755409920000522
Figure BDA0003755409920000531
Figure BDA0003755409920000532
Figure BDA0003755409920000541
Figure BDA0003755409920000542
Figure BDA0003755409920000551
Figure BDA0003755409920000552
Figure BDA0003755409920000561
Figure BDA0003755409920000562
Figure BDA0003755409920000571
Figure BDA0003755409920000572
Figure BDA0003755409920000581
Figure BDA0003755409920000582
Figure BDA0003755409920000583
Figure BDA0003755409920000591
Figure BDA0003755409920000592
Figure BDA0003755409920000601
Figure BDA0003755409920000602
Figure BDA0003755409920000603
Figure BDA0003755409920000611
Figure BDA0003755409920000612
Figure BDA0003755409920000621
Figure BDA0003755409920000622
Figure BDA0003755409920000623
Figure BDA0003755409920000631
Figure BDA0003755409920000632
Figure BDA0003755409920000641
Figure BDA0003755409920000642
Figure BDA0003755409920000651
Figure BDA0003755409920000652
Figure BDA0003755409920000661
Figure BDA0003755409920000662
Figure BDA0003755409920000663
Figure BDA0003755409920000671
Figure BDA0003755409920000672
Figure BDA0003755409920000681
Figure BDA0003755409920000682
Figure BDA0003755409920000691
Figure BDA0003755409920000692
Figure BDA0003755409920000701
Figure BDA0003755409920000702
Figure BDA0003755409920000711
Figure BDA0003755409920000712
提供上文陈述的实例是以为所属领域的一般技术人员赋予如何制作及使用组合物的各种实施例的完整公开及描述，且不希望限制发明者认为是他们的发明的内容的范围。对所属领域的技术人员显而易见的用于实施本发明的上述模式的修改希望在以下权利要求书的范围内。本说明书中引用的所有公开案、专利及专利申请案通过引用的方式并入本文中，就好像每一此公开案、专利或专利申请案都被明确且个别地指示为通过引用的方式并入本文中一样。

Claims (20)

1.一种组合物，其包括：
三元乙丙(EPDM)聚合物、氢氧化铝、消耗性石墨、磷酸三(2-乙基己基)酯及聚丁二烯的马来酸酐加合物，其中所述组合物不含矿物油。
2.根据权利要求1所述的组合物，其进一步包括固化剂。
3.根据权利要求2所述的组合物，其中所述固化剂包括硫或硫释放化合物。
4.根据权利要求1所述的组合物，其进一步包括促进剂。
5.根据权利要求4所述的组合物，其中所述促进剂包括氧化锌、硬脂酸、二硫化四苄基秋兰姆、N-环己基-2-苯并噻唑次磺酰胺或其组合。
6.根据权利要求1所述的组合物，其进一步包括填充剂。
7.根据权利要求6所述的组合物，其中所述填充剂包括碳黑。
8.根据权利要求1所述的组合物，其中所述组合物不含卤素。
9.根据权利要求1所述的组合物，其中所述组合物不含三氧化锑。
10.一种组合物，其包括：
三元乙丙(EPDM)聚合物、硫、二硫化四苄基秋兰姆、N-环己基-2-苯并噻唑次磺酰胺、氧化锌、硬脂酸、聚丁二烯的马来酸酐加合物、可膨胀石墨、碳黑、磷酸三(2-乙基己基)酯及氢氧化铝，其中所述组合物不含矿物油。
11.一种制作EPDM膜的方法，其包括以下步骤：
使用压延或辊模挤出机将根据权利要求1所述的组合物的同质混合物加工成膜；及
将所述膜热固化。
12.根据权利要求11所述的方法，其进一步包括在所述膜被硫化之前或之后，将织物层层压到所述膜的一侧的步骤。
13.根据权利要求11所述的方法，其进一步包括在所述膜被硫化之前或之后，将织物层层压到所述膜的每一侧的步骤。
14.根据权利要求11所述的方法，其进一步包括在所述膜被硫化之前或之后，将玻璃纤维网格布层层压到所述膜的一侧的步骤。
15.根据权利要求11所述的方法，其进一步包括在所述膜被硫化之前或之后，将玻璃纤维网格布层层压到所述膜的每一侧的步骤。
16.一种制作EPDM膜的方法，其包括以下步骤：
使用压延或辊模挤出机将根据权利要求10所述的组合物的同质混合物加工成膜；及
将所述膜热固化。
17.根据权利要求16所述的方法，其进一步包括在所述膜被硫化之前或之后，将织物层层压到所述膜的一侧的步骤。
18.根据权利要求16所述的方法，其进一步包括在所述膜被硫化之前或之后，将织物层层压到所述膜的每一侧的步骤。
19.根据权利要求16所述的方法，其进一步包括在所述膜被硫化之前或之后，将玻璃纤维网格布层层压到所述膜的一侧的步骤。
20.根据权利要求16所述的方法，其进一步包括在所述膜被硫化之前或之后，将玻璃纤维网格布层层压到所述膜的每一侧的步骤。
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