CN111372991A - 阻燃聚(氯乙烯)复合物 - Google Patents
阻燃聚(氯乙烯)复合物 Download PDFInfo
- Publication number
- CN111372991A CN111372991A CN201880067605.9A CN201880067605A CN111372991A CN 111372991 A CN111372991 A CN 111372991A CN 201880067605 A CN201880067605 A CN 201880067605A CN 111372991 A CN111372991 A CN 111372991A
- Authority
- CN
- China
- Prior art keywords
- plasticizer
- vinyl chloride
- composite
- poly
- flame retardant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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Images
Classifications
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F114/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F114/02—Monomers containing chlorine
- C08F114/04—Monomers containing two carbon atoms
- C08F114/06—Vinyl chloride
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明涉及增塑聚(氯乙烯)复合物,其被配制成提供足够的柔性和阻燃性以适用于建筑和施工聚合物制品。本发明的一个方面为阻燃聚(氯乙烯)复合物,其包含以下组分的混合物:聚(氯乙烯);选自聚合物增塑剂、烷基芳基阻燃增塑剂及其组合的增塑剂;以及任选的功能性添加剂,其中所述混合物具有:i)大于50%的根据ASTM D2863的极限氧指数;ii)至少10%的根据ASTM D638(IV型)的断裂延伸率;和iii)小于约15000psi的根据ASTM 638(IV型)的弹性模量。
Description
优先权要求
本申请要求于2017年9月15日提交的代理人案号为12017016的美国临时专利申请序列号62/559,252的权益,其在此通过引用整体并入本文。
技术领域
本发明涉及增塑聚(氯乙烯)复合物用于诸如柔性阻燃聚合物建筑和施工产品的目的的用途。
背景技术
人们受益于塑料制品。从其20世纪中期至今的发明,热塑性聚合物已成为许多消费产品的组成。这样的产品相对轻质、结实且耐腐蚀。
由B.F.Goodrich的Waldo Semon发明的增塑聚(氯乙烯)是数十年来顶级性能的塑料树脂。每年数十亿公斤的聚(氯乙烯)(也被称为“PVC”)树脂被成型并挤出为不计其数的产品。利用常规添加剂,聚(氯乙烯)提供例如无与伦比的耐久性、阻燃性、耐化学品性、耐候性、电特性和透明度。
电线和线缆制造商经常使用增塑PVC用于建筑和施工环境中的绝缘和包覆。基于加速烘箱老化测试,预测增塑PVC复合物在各种温度下的性能。将Underwriters'Laboratories(UL)的额定为60℃的线缆在100℃下测试7天,而将额定为75℃的线缆在100℃下测试10天。一些常规使用的增塑剂为邻苯二甲酸酯、柠檬酸酯、豆油酸酯(soyate)和偏苯三酸酯。
对于在建筑和施工环境中使用的其他类型的材料,ASTM International(www.astm.org)制定了用于测试建筑材料表面燃烧特性的严格标准:“建筑材料表面燃烧特性的ASTM E84-15a标准测试方法。”该E84测试涉及适用于暴露表面(例如墙体和顶棚)的建筑材料的比较表面燃烧行为的燃烧-测试-响应标准。E84测试在这样的情况下进行:样本位于顶棚的位置,待评估的表面面朝下暴露于点火源。为了满足E84测试的要求,材料、产品或组合件应能够在测试期间安装在测试位置。因此,样本应通过自身结构特性而自支撑,通过沿着测试表面的添加支撑物保持在适当位置,或者从背面固定。
发明内容
本领域中需要的是柔性的并且可以通过上述E84测试的增塑PVC复合物。聚(氯乙烯)复合物越硬,就越容易通过E84测试。但是如果在这种情况下为了期望的柔性重新配制聚(氯乙烯)复合物,那么更难通过E84测试。
因此,增塑PVC复合物需要仔细地平衡成分,以呈阻燃的且柔性的。
本发明的一个方面为阻燃聚(氯乙烯)复合物,其包含以下组分的混合物:(a)聚(氯乙烯);(b)选自(1)聚合物增塑剂、(2)烷基芳基阻燃增塑剂及其组合的增塑剂;以及任选的(c)功能性添加剂,其中所述混合物具有大于50%的根据ASTM D2863的极限氧指数;至少10%的根据ASTM D638(IV型)的断裂延伸率;和小于约15000psi的根据ASTM 638(IV型)的弹性模量。
本发明的另一个方面为由上述聚(氯乙烯)复合物制成的建筑和施工制品。
附图说明
图1是实施例4的测试板(plaque)的照片。
具体实施方式
聚(氯乙烯)树脂
聚氯乙烯聚合物可在全世界广泛获得。如本说明书中涉及的聚氯乙烯树脂包括:在任何其他聚合物(例如HDT变形温度提高聚合物)、冲击增韧剂、阻隔聚合物、链转移剂、稳定剂、增塑剂或流动改性剂的存在下聚合的聚氯乙烯均聚物、氯乙烯共聚物、接枝共聚物和氯乙烯聚合物。
例如,可以通过在链转移剂的存在下使低粘度、高玻璃化转变温度(Tg)提高剂(例如SAN树脂或酰亚胺化的聚甲基丙烯酸酯)过度聚合来对PVC聚合物进行组合改性。
在另一个替代方案中,氯乙烯可以在所述Tg提高剂的存在下聚合,所述试剂在氯乙烯聚合之前或在此期间形成。然而,仅那些具有特定平均颗粒尺寸和脆性程度的树脂才表现出适用于本发明的实践的优点。
在本发明的实践中,可以使用聚氯乙烯均聚物或者包含一种或更多种可与其共聚的共聚单体的聚氯乙烯的共聚物。用于氯乙烯的合适共聚单体包括:丙烯酸和甲基丙烯酸;丙烯酸和甲基丙烯酸的酯,其中酯部分具有1至12个碳原子,例如丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯和丙烯酸乙基己酯等;甲基丙烯酸甲酯、甲基丙烯酸乙酯和甲基丙烯酸丁酯等;丙烯酸和甲基丙烯酸的羟烷基酯,例如丙烯酸羟甲基酯、丙烯酸羟乙基酯、甲基丙烯酸羟乙基酯等;丙烯酸和甲基丙烯酸的缩水甘油酯,例如丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯等;α、β不饱和二羧酸及其酸酐,例如马来酸、富马酸、衣康酸和它们的酸酐等;丙烯酰胺和甲基丙烯酰胺;丙烯腈和甲基丙烯腈;马来酰亚胺,例如N-环己基马来酰亚胺;烯烃,例如乙烯、丙烯、异丁烯、己烯等;偏二氯乙烯,例如偏二氯乙烯;乙烯基酯,例如乙酸乙烯酯;乙烯基醚,例如甲基乙烯基醚、烯丙基缩水甘油醚、正丁基乙烯基醚等;交联单体,例如邻苯二甲酸二烯丙基酯、乙二醇二甲基丙烯酸酯、亚甲基双丙烯酰胺、三丙烯酰基三嗪、二乙烯基醚、烯丙基硅烷等;以及包括任何上述共聚单体的混合物。
本发明也可以使用氯化聚氯乙烯(CPVC),其中包含约57%氯的PVC与氯自由基进一步反应产生具有较高的玻璃化转变温度(Tg)和热变形温度的聚合物CPVC,所述氯自由基由分散在水中并被照射而产生溶解在水中的氯自由基的氯气产生。商品化的CPVC通常按重量计包含约58%至约70%,并且优选约63%至约68%氯。CPVC共聚物可以通过使用常规方法(例如通过引用并入本文的美国专利第2,996,489号中描述的方法)使这样的PVC共聚物氯化来获得。CPVC的商业来源包括Lubrizol Corporation。
优选组成为聚氯乙烯均聚物。
聚氯乙烯聚合物的可商购来源包括Dallas,TX的Oxy Vinyls LP;和Freeport,TX的Shintech USA。
PVC复合物
柔性PVC树脂复合物通常包含根据由其制造的制品的性能要求而选择的各种添加剂,这完全在本领域技术人员理解的范围内而无需过多的实验。
增塑剂
通常与聚(氯乙烯)一起使用的增塑剂的非限制性实例为邻苯二甲酸酯、柠檬酸酯、豆油酸酯和偏苯三酸酯。在这种情况下当前优选两种特定的增塑剂。
一种当前优选的增塑剂为PalamollTM 654中等粘度聚合物增塑剂,其为由BASF出售的如下混合物:己二酸跟以下的聚合物:1,4-丁二醇和2,2-二甲基-1,3-丙二醇、异壬酯。该增塑剂为无邻苯二甲酸酯的(考虑到当前的市场条件)并注册为CAS号208945-12-4。
另一种当前优选的增塑剂为SanticizerTM 2148增塑剂,其由Valtris销售并注册为CAS号27460-02-2。
可以使用聚合物增塑剂或烷基芳基增塑剂作为用于阻燃PVC复合物的唯一增塑剂。或者,这两种增塑剂可以以上述之间的任何比例组合。
无论单独还是组合,当前优选的增塑剂的重量份的范围为每100份PVC聚合物约115份至130份。
其他功能性添加剂
根据实施例中所述的实验结果,本文中使用的PVC复合物可以包含有效量的添加剂。
在此公开的适用于需要通过E84测试的建筑和施工环境的聚(氯乙烯)复合物包含:
钙-锌热稳定剂(如果存在)的量为每100份PVC约1份至约4份;
三水合氧化铝阻燃剂(如果存在)的量为每100份PVC约320份至380份;
硼酸锌阻燃剂(如果存在)的量为每100份PVC约20份至30份;
包括在Mg(OH)2上的碱式钼酸锌配合物的抑烟剂(如果存在)的量为每100份PVC 3份至8份;
碳酸钙功能性填料(如果存在)的量为每100份PVC约150份至约300份;
硬脂酸润滑剂(如果存在)的量为每100份PVC约0.25份至约0.75份;和
炭黑颜料(如果存在)的量为每100份PVC约2份至约5份。
在此公开的复合物可以以足以获得该复合物的期望加工特性或性能特性的量包含其他常规的塑料添加剂。该量不应浪费添加剂,也不应有害于复合物的加工或性能。无需过多的实验并且在参考例如Plastics Design Library(www.elsevier.com)的Plastics Additives Database(2004)的论文的情况下,热塑性塑料复合领域的技术人员可以从许多不同类型的添加剂中选择以用于包含在本发明的复合物中。
其他任选添加剂的非限制性实例包括:粘合增进剂;抗微生物剂(抗菌剂、杀菌剂和防霉剂);防雾剂;抗静电剂;粘结剂、起泡剂和发泡剂;分散剂;填料和增量剂;防火剂和阻燃剂以及抑烟剂;冲击改性剂;引发剂;润滑剂;云母;颜料、着色剂和染料;增塑剂;加工助剂;脱模剂;硅烷;钛酸酯和锆酸酯;增滑剂和防堵剂;稳定剂;硬脂酸酯;紫外线吸收剂;粘度调节剂;蜡;以及它们的组合。
加工
本发明的复合物的制备如下。本发明的复合物可以以分批或连续操作由通常以分批操作的方式制备的粉末共混物制得。
这种以分批过程的粉末共混通常在粉末混合器例如Henschel或Littleford混合器、或者带式共混机中进行,所述粉末混合器将包括液体增塑剂在内的所有添加剂与PVC树脂在不使聚合物基体达到熔融温度的情况下物理混合。混合速度的范围为60rpm至3000rpm,混合温度可以为环境至最高250°F(121℃)。混合器的输出为共混良好的粉末产物,其可以流入可以提高共混温度以引起一些成分(包括PVC树脂)熔融的机器中。
以分批过程的混合通常在班伯里密炼机中进行,该密炼机还被升高至足以使聚合物基体熔融的温度以允许添加任何任选添加剂的固体成分添加剂。混合速度的范围为60rpm至3000rpm,混合温度的范围为250°F至430°F(120℃至220℃),通常为325°F(163℃)。然后,将熔融的混合物置于320°F/345°F(160℃至174℃)的双辊混炼机上。将材料混炼约四分钟,然后将经混炼复合的带切成立方体,以用于随后挤出或成型为聚合物制品。或者,为了实验评估,可以通过模压成型使经复合的带成形为板以用于物理测试的目的。
可以使复合物成形为粉末、立方体或丸粒,以用于进一步挤出为型材或片状形式,随后进行或者不进行成型为聚合物部件和零件。
挤出和成型技术是热塑性塑料聚合物工程领域的技术人员公知的。无需过多的实验,并且利用参考文献例如由Plastics Design Library(www.elesevier.com)出版的"Extrusion,The Definitive Processing Guide and Handbook"、"Specialized MoldingTechniques"和"Handbook of Mold,Tool and Die Repair Welding",可以使用本发明的复合物制造任何可预期的形状和外观的制品。非限制性实例为以熔体形式再成形为挤出、成型、热成型、压延或3D打印的聚合物制品。
对于E84测试,可以制造压延、热成型或其他高纵横比的聚合物制品。
发明的实用性
建筑和施工市场可以受益于本文公开的PVC复合物。在兼具足以通过E84测试的阻燃性并且还具有足以用作建筑或施工材料的柔性的情况下,占用空间可以以各种形状利用这些复合物。例如,异型材挤出零件可以与高纵横比零件互补,二者均来自本文公开的相同或相似的复合物。另外,膜、片、板等的后成型可以用于顶棚和墙体施工二者。
如前所述,刚性聚(氯乙烯)可以通过E84测试。但是刚性在建筑和施工中是不优选的。增加聚(氯乙烯)的柔性增加了PVC复合物在建筑和施工中的有用性,但降低了其通过E84测试的可能性。如实施例和比较例所证明的,发现成分的非常好的平衡可以得到用于柔性、阻燃的建筑和施工产品的成功候选者。
实施例
表2示出了实施例和所有比较例的成分来源。表3示出了用于制造所有实验样品的加工条件。
表3--加工说明 |
#1辊式混炼机 |
将所有成分一起称量到一个容器中 |
充分混合,然后在320°F至335°F(160℃至168℃)下混炼4分钟 |
在345°F(174℃)下压缩压制以形成用于物理测试的板 |
表4确定了所进行的物理测试。
*0.63cm厚样品
**5.08cm×508cm×0.63cm样品
***15.2cm×15.2cm×1.9cm样品
****15.2cm×15.2cm×0.32cm样品
表5示出了实施例和比较例的配方和物理特性。
在十个配方中,六个能够满足柔性和阻燃性条件。
所有的十个配方具有相同量的PVC聚合物、热稳定剂、硼酸锌阻燃剂、抑烟剂和炭黑。因此,增塑剂含量、三水合氧化铝阻燃剂、硬脂酸和碳酸钙填料不同。
对于比较例A至B和实施例1、2和5,没有使用Santicizer 2148磷酸芳基酯阻燃增塑剂。实施例1和2与比较例A和B之间的一个区别是Palamoll 654聚合物增塑剂的份数更高,这导致极限氧指数略有降低但延伸率百分比更高(且可接受)。比较例A与实施例5之间的区别为润滑剂的量,这导致延伸率结果的显著差异,虽然弹性模量均在小于15000psi的可接受范围内。
比较例A和B以及实施例5和6的总增塑剂含量为115份,而实施例1至4和比较例均存在总计127份的增塑剂。弹性模量、延伸率和极限氧指数的三个标准的满足使得实施例1至6与比较例A至D区分开来。
使用Palamoll 654增塑剂或Santicizer 2148增塑剂(也具有阻燃特性)或二者也提供了实施例1至6的区别。实施例1、2和5仅使用前者,而实施例6仅使用后者。
比较例C至D以及实施例3和4以67:33(2:1)和50:50(1:1)的比例测试了ParamollTM254增塑剂与Santicizer 2148增塑剂的比例。比较例C与实施例3的比较以及比较例D与实施例4的比较在由实施例3和4测试的两个比例下是一致的,提供了不仅略高的弹性模量结果而且显著更高的延伸率百分比。这两对之间的区别为实施例3和4中存在的三水合氧化铝阻燃剂的量分别相对于比较例C和D大20%。
如在实施例3与比较例D之间,二者的两种类型增塑剂的比例为1:1,极限氧指数(LOI)测试(用于预测E84测试的通过)提供了区分两组物理特性的基础。实施例3的LOI结果优于比较例D的LOI结果20%。
虽然比较例A和B二者确实具有比任何实施例都高的LOI,但是对于本公开内容中预期的成功的建筑和施工聚合物制品而言必须建立的是物理特性的平衡。
仅实施例1至6的配方满足以下标准(以及在实施例1至6中对于所述标准而言的当前优选):
根据ASTM D2863的极限氧指数大于50%(并且当前优选大于55%);
根据ASTM D638(IV型)的断裂延伸率为至少10%(并且当前优选至少20%);和
根据ASTM 638的弹性模量为小于约15000(IV型)(并且当前优选小于约10000。)
在所有三个标准内以它们的当前优选进行操作,实施例4目前是优选的。图1示出了实施例4的柔性的照片,其中相对边缘由于金属长尾夹的约束而接触。
可以根据商业或制造偏好来调节其他物理特性。例如,使用另外的碳酸钙填料或使用另外的不同填料(例如铜或钨金属颗粒或二者)可以增加比重。
无需过多的实验并且利用实验结果,本领域普通技术人员将能够制成适用于分别在可接受和优选的标准内实现阻燃、柔性PVC复合物的物理特性的配方。
本发明不限于上述实施方案。附上权利要求。
Claims (12)
1.一种阻燃聚(氯乙烯)复合物,包含:
以下组分的混合物:
(a)聚(氯乙烯);
(b)选自以下的增塑剂:
(1)聚合物增塑剂,
(2)烷基芳基阻燃增塑剂,和
(3)其组合;以及任选的
(c)功能性添加剂,
其中所述混合物具有大于50%的根据ASTM D2863的极限氧指数;至少10%的根据ASTMD638(IV型)的断裂延伸率;和小于约15000psi的根据ASTM 638(IV型)的弹性模量。
2.根据权利要求1所述的复合物,其中所述极限氧指数大于55%。
3.根据权利要求1或权利要求2所述的复合物,其中所述断裂延伸率为至少20%。
4.根据权利要求1或权利要求2或权利要求3所述的复合物,其中所述弹性模量小于10000psi。
5.根据权利要求1至4中任一项所述的复合物,其中所述聚(氯乙烯)包括聚(氯乙烯)均聚物。
6.根据权利要求1至5中任一项所述的复合物,其中所述增塑剂包含如下作为混合物的聚合物增塑剂:己二酸跟以下物质的聚合物:1,4-丁二醇和2,2-二甲基-1,3-丙二醇、异壬酯。
7.根据权利要求1至6中任一项所述的复合物,其中所述增塑剂包含注册为CAS号208945-12-4的中等粘度聚合物增塑剂。
8.根据权利要求1至7中任一项所述的复合物,其中所述增塑剂包含无卤素、低烟、烷基芳基阻燃增塑剂。
9.根据权利要求1至8中任一项所述的复合物,其中所述增塑剂包含注册为CAS号27460-02-2的磷酸芳基酯。
10.根据权利要求1至9中任一项所述的复合物,其中所述增塑剂包含注册为CAS号208945-12-4的增塑剂和注册为CAS号27460-02-2的增塑剂二者,其中这两种增塑剂以99:1;90:10;75:25;67:33;60:40;50:50;40:60;33:67;25:75;10:90;1:99的比例;以及在如此列出的任意两个比例之间的每个比例组合。
11.根据权利要求1至10中任一项所述的复合物,其中任选的功能性添加剂选自:钙-锌热稳定剂、三水合氧化铝阻燃剂、硼酸锌阻燃剂、在氢氧化镁上的碱式钼酸锌配合物抑烟剂、碳酸钙密度调节填料、金属颗粒密度调节填料、硬脂酸润滑剂、炭黑颜料和如此列出的添加剂的任何组合。
12.一种聚合物制品,包含根据权利要求1至11中任一项所述的复合物。
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US20200216586A1 (en) | 2020-07-09 |
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