CN114222784A - 热膨胀性耐火树脂组合物及热膨胀性耐火片材 - Google Patents
热膨胀性耐火树脂组合物及热膨胀性耐火片材 Download PDFInfo
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- CN114222784A CN114222784A CN202080057271.4A CN202080057271A CN114222784A CN 114222784 A CN114222784 A CN 114222784A CN 202080057271 A CN202080057271 A CN 202080057271A CN 114222784 A CN114222784 A CN 114222784A
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Abstract
一种热膨胀性耐火树脂组合物,所述组合物包含乙烯基树脂、含氮发泡剂、磷系阻燃剂、多元醇、二氧化钛和直链丙烯酸系聚合物。所述直链丙烯酸系聚合物的重均分子量在大于或等于4,000,000且小于或等于20,000,000的范围内。
Description
技术领域
本公开一般而言涉及热膨胀性耐火树脂组合物和热膨胀性耐火片材,并且更具体地涉及包含发泡剂的热膨胀性耐火树脂组合物和热膨胀性耐火片材。
背景技术
专利文献1公开了一种覆盖材料。所述覆盖材料包括粘合剂、阻燃剂、发泡剂、碳化剂和填料。该覆盖材料还包括醋酸乙烯酯-乙烯共聚物树脂作为粘合剂,所述醋酸乙烯酯-乙烯共聚物树脂在190℃下的熔体质量流动速率为0.1至300g/10min且醋酸乙烯酯含量为15质量%至50质量%。覆盖材料用于保护建筑物等中的各种基材(建筑框架)免受高温影响。
专利文献1的覆盖材料在受到高温例如火时发泡,从而形成碳化隔热层。专利文献1的覆盖材料发泡但可能难以保持碳化隔热层的形状并且可能容易塌陷。这可能导致不令人满意的耐火性。
引文列表
专利文献
专利文献1:WO 2013/008819
发明内容
本公开的目的是提供一种具有改进的耐火发泡性能和改进的泡沫致密度(foamdenseness)的热膨胀性耐火树脂组合物和热膨胀性耐火片材。
根据本公开的一方面,所述热膨胀性耐火树脂组合物包含乙烯基树脂、含氮发泡剂、磷系阻燃剂、多元醇、二氧化钛和直链丙烯酸系聚合物。所述直链丙烯酸系聚合物的重均分子量在大于或等于4,000,000且小于或等于20,000,000的范围内。
根据本公开的一个方面,热膨胀性耐火片材包括由所述热膨胀性耐火树脂组合物形成的树脂层。
附图说明
图1A是在加热前根据本公开的一个实施方案的热膨胀性耐火片材的截面示意图,图1B是加热后所述热膨胀性耐火片材的截面示意图;
图2是加热后的常规的热膨胀性耐火片材的截面示意图;和
图3A是加热后实施例1的热膨胀性耐火片材的截面照片,和图3B是加热后比较例1的热膨胀性耐火片材的截面照片。
具体实施方式
(1)概述
在图1A中,示出根据本实施方案的热膨胀性耐火片材1。热膨胀性耐火片材1包括树脂层11。树脂层11由热膨胀性耐火树脂组合物形成。该热膨胀性耐火树脂组合物包含乙烯基树脂、含氮发泡剂、磷系阻燃剂、多元醇、二氧化钛和直链丙烯酸系聚合物。下面将描述热膨胀性耐火片材1的耐火机理。
当热膨胀性耐火片材1受到加热例如火加热时,树脂层11开始发泡,从而形成如图1B所示的发泡隔热层13。发泡隔热层13包括大量的微细气泡14。这使得热膨胀性耐火片材1能够展现耐火性能。火加热的温度为例如高于或等于600℃。
在图2中,示出了常规的热膨胀性耐火片材10。常规的热膨胀性耐火片材10在受到加热例如火加热时,也形成发泡隔热层130。但是,在此情况下形成的发泡隔热层130中的气泡140往往很大。此外,气泡140可能变得过大并可能因此消失(所谓的气泡消泡或爆破)。这使得发泡隔热层130难以保持它的形状,且因此发泡隔热层130更可能塌陷。因此,常规的热膨胀性耐火片材10难以表现出满意的耐火性能。
这里,图2中所示的每一个大气泡140可能是逐渐扩大的单个气泡或者可能是具有各种尺寸的多个气泡聚结而成的气泡。原因之一可能是每个气泡周围存在的树脂极其有弹性且容易破裂。
因此,在本实施方案中,将直链丙烯酸系聚合物的重均分子量设置在大于或等于4,000,000且小于或等于20,000,000的范围内,从而抑制如图2所示的大气泡140的形成。此外,气泡一旦形成也被抑制免于消失。
因此,本实施方案能够提高耐火发泡性质和泡沫致密度。需要注意的是,耐火发泡性质是根据例如树脂层11的膨胀率进行评价。发泡致密度是根据发泡隔热层13中的气泡的平均直径、直径分布、密度等进行评价。耐火发泡性能和泡沫致密度的具体测试方法会在条目“实施例”中描述。
(2)详情
<热膨胀性耐火树脂组合物>
根据本实施方案的热膨胀性耐火树脂组合物包含乙烯基树脂、含氮发泡剂、磷系阻燃剂、多元醇、二氧化钛和直链丙烯酸系聚合物。在本说明书中,除去直链丙烯酸系聚合物的热膨胀性耐火树脂组合物的剩余部分可被称为“基材”。下面将对热膨胀性耐火树脂组合物中包含的各成分进行描述。
<<乙烯基树脂>>
乙烯基树脂是聚乙烯基化合物。聚乙烯基化合物是通过聚合具有乙烯基团的单体获得的树脂。乙烯基树脂没有特别限制,但优选包括EVA树脂和/或聚烯烃树脂。
[EVA树脂]
EVA树脂是乙烯-醋酸乙烯酯共聚物。EVA树脂是通过高压聚合法制备的。EVA树脂是一种具有橡胶弹性和优良的低温特性和耐候性的树脂。EVA树脂中醋酸乙烯酯的含量百分比没有特别限制,但是例如在大于或等于5%且小于或等于30%的范围内。改变醋酸乙烯酯的含量百分比能够在宽范围内控制柔韧性、粘合性、热密封性质等。注意,醋酸乙烯酯的含量百分比可以通过符合JISK6924-1的方法进行测定。
当热膨胀性耐火片材1的树脂层11被加热时,EVA树脂可以使树脂层11成为优良的发泡隔热层13。此外,当将热膨胀性耐火片材1固定到例如底层构件的建筑结构部分时,EVA树脂赋予热膨胀性耐火片材1以顺应性。
如上所述,EVA树脂是具有橡胶弹性和优良的低温特性和耐候性的树脂。因此,EVA树脂可以将这些性质赋予热膨胀性耐火片材1的树脂层11。
EVA树脂的具体产品的实例包括由TOSOH CORPORATION制造的Ultrasen(Nipoflex)(注册商标)。
EVA树脂的熔体质量流动速率(MFR)优选在大于或等于0.4g/10min且小于或等于75g/10min的范围内。当熔体质量流动速率大于或等于0.4g/10min时,当热膨胀性耐火片材1设置在建筑结构部分例如底层构件时可以令人满意地保持顺应性。此外,在冻融时,热膨胀性耐火片材1的树脂层11不易变脆,因此,可以令人满意地确保长期的抗冻融耐久性。当熔体质量流动速率小于或等于75g/10min时,可以令人满意地维持通过暴露于火焰等而形成的发泡隔热层13的形状保持性。注意,熔体质量流动速率可通过符合JIS K6924-1的方法进行测量。
基于100质量份的基材,EVA树脂的含量优选在大于或等于15质量份且小于或等于40质量份的范围内。当EVA树脂的含量大于或等于15质量份时,当树脂层11由热膨胀性耐火树脂组合物形成时,可以提高热膨胀性耐火片材1的韧性。当EVA树脂的含量小于或等于40质量份时,在热膨胀性耐火片材1暴露于火加热时,可以保持发泡隔热层13的形状。基于100质量份的基材,EVA树脂的含量更优选在大于18质量份且小于35质量份的范围内,更优选在大于18质量份且小于28质量份的范围内。
[聚烯烃树脂]
聚烯烃树脂是烯烃的聚合物。聚烯烃树脂没有特别限制,并且聚烯烃树脂的实例包括聚乙烯、聚丙烯、聚异丁烯、聚异戊二烯和聚丁二烯。优选地,聚烯烃树脂包含茂金属塑性体。
在热膨胀性耐火片材1的树脂层11被加热时,所述茂金属塑性体可以使树脂层11成为优良的发泡隔热层13。此外,茂金属塑性体可以赋予热膨胀性耐火片材1气体阻隔性能。此外,当将热膨胀性阻燃片材1固定到建筑结构部分例如底层构件时,茂金属塑性体可以赋予与热膨胀性耐火片材1顺应性。注意,“塑性体”是指具有易流动性、受热可变形为一种形状并且在该形状下可固化的性质的聚合物。塑性体是与弹性体(其具有这样的性质,即当对弹性体施加外力时,所述弹性体根据所述外力而变形,且当外力去除时,弹性体又在短时间内恢复到其原来的形状)意思相反的术语,并且塑性体不像弹性体那样表现出弹性形变,但容易塑性形变。在本实施方案中,茂金属塑性体是通过乙烯与烯烃例如α-烯烃在催化剂即茂金属作为催化剂的存在下聚合得到的聚合物。
茂金属塑性体具有高柔韧性和高耐热性,以及优良的抗冲击性。因此,茂金属塑性体可以赋予热膨胀性耐火片材1的树脂层11抗冲击性和柔韧性。
茂金属塑性体的制备方法没有特别限制,但如上所述,茂金属塑性体是通过相应地在茂金属催化剂的存在下使乙烯和烯烃如α-烯烃聚合而获得的。茂金属塑性体的具体产品的实例包括由Sumitomo Chemical Company,Limited制造的EXCELLEN(注册商标)FX系列的C6 EXCELLEN FX(FX201、FX301、FX307和FX402)和C4 EXCELLEN FX(FX352、FX555、FX551和FX558)以及由Japan polyethylene Corporation制造的Kernel(KF260T)。当然,茂金属塑性体不限于上述具体实例,但是至少是如上所述通过在茂金属催化剂的存在下聚合烯烃而获得的共聚物。
茂金属塑性体的熔体质量流动速率优选在大于或等于2g/10min且小于或等于40g/10min的范围内。当熔体质量流动速率大于或等于2g/10min时,当热膨胀性耐火片材1设置在建筑结构部分例如底层构件中时,可以令人满意地保持顺应性。此外,在冻融时,热膨胀性耐火片材1的树脂层11不易变脆,因此可以令人满意地确保长期的抗冻融耐久性。当熔体质量流动速率小于或等于40g/10min时,可以令人满意地维持通过暴露于火焰等形成的发泡隔热层的形状保持性。此外,在此情况下,可以使热膨胀性耐火片材1的气体阻隔性能更不可能降低,并且可以令人满意地确保在高温和潮湿气氛下的长期耐久性。熔体质量流动速率更优选在大于或等于4g/10min且小于或等于30g/10min的范围内。
基于100质量份的基材,茂金属塑性体的含量优选在大于或等于15质量份且小于或等于40质量份的范围内。当茂金属塑性体的含量大于或等于15质量份时,当树脂层11由热膨胀性耐火树脂组合物形成时,可以提高热膨胀性耐火片材1的韧性。此外,在此情况下,可以确保热膨胀性耐火片材1的令人满意的气体阻隔性能并且令人满意地保持在热和潮湿条件下的长期耐久性。当茂金属塑性体的含量小于或等于40质量份时,可以在热膨胀性耐火片材1暴露于火加热时保持发泡隔热层13的形状。基于100质量份的基材,茂金属塑性体的含量更优选在大于18质量份且小于35质量份的范围内,更进一步优选在大于18质量份且小于28质量份的范围内。
<<含氮发泡剂>>
含氮发泡剂为含有氮原子的发泡剂。含氮发泡剂在暴露于火加热时分解,并产生不燃性气体如氮气和/或氨气。含氮发泡剂还具有使因火加热和多元醇而碳化的乙烯基树脂膨胀和发泡以形成发泡隔热层13的作用。此外,含氮发泡剂可赋予热膨胀性耐火片材1韧性。这使得热膨胀性耐火片材1对建筑结构部分表现出令人满意的顺应性。
含氮发泡剂没有特别限制,但含氮发泡剂的实例包括三聚氰胺、三聚氰胺衍生物、双氰胺、偶氮二甲酰胺、尿素和胍。即,含氮发泡剂含有选自上述实例中的至少一种。考虑到不燃性气体的产生效率、对建筑结构部分的顺应性和耐火性,含氮发泡剂优选包含三聚氰胺或双氰胺中的至少一种,且更优选包含至少三聚氰胺。
基于100质量份的基材,含氮发泡剂的含量优选在大于或等于5质量份且小于或等于25质量份的范围内。当含氮发泡剂的含量大于或等于5质量份时,可以在暴露于火加热时令人满意地形成发泡隔热层13。另外,可以确保热膨胀性耐火片材1的韧性。当含氮发泡剂的含量小于或等于25质量份时,可以确保由火加热形成的发泡隔热层13的形状保持性。另外,即使反复冻融,热膨胀性耐火片材1也不太可能硬化,且可以抑制耐火性的降低。基于100质量份的基材,含氮发泡剂的含量更优选大于或等于8质量份且小于或等于23质量份。
<<磷系阻燃剂>>
磷系阻燃剂是含有仅有磷或磷化合物中的至少一种的阻燃剂。磷系阻燃剂具有当暴露于火加热时将多元醇脱水的作用,以在发泡隔热层13的表面形成称为“炭”(char)的薄膜。此外,当在高于或等于600℃的高温下加热时磷系阻燃剂与二氧化钛发生反应产生焦磷酸钛。所述焦磷酸钛作为灰分残留在发泡隔热层13中,从而提高发泡隔热层13的形状保持性。
磷系阻燃剂没有特别限制,其实例包括红磷、磷酸酯、磷酸金属盐、磷酸铵、磷酸三聚氰胺、磷酸酰胺和多磷酸铵。磷酸酯的实例包括磷酸三苯酯和磷酸三甲苯酯。金属磷酸盐的实例包括磷酸钠和磷酸镁。多磷酸铵的实例包括多磷酸铵和三聚氰胺改性的多磷酸铵。这些物质中,特别地,考虑到发泡隔热层13令人满意的形成、发泡隔热层13的形状保持性和长期耐久性,磷系阻燃剂中优选含有多磷酸铵。磷系阻燃剂可以是上述实例中的仅一种或两种或更多种。当聚磷酸铵遇火加热,且聚磷酸铵的温度达到分解温度时,聚磷酸铵使氨解除吸附以生成磷酸和缩合磷酸。所述磷酸和缩合磷酸使多元醇脱水和碳化,从而形成炭。此外,由聚磷酸铵分解产生的氨气、由含氮发泡剂分解产生的氨气和氮气等导致整个树脂层11膨胀和发泡。氨气、氮气等不燃性气体的产生降低了氧的浓度,并因此能够进一步抑制燃烧。此外,聚磷酸铵在高于或等于600℃的高温下加热时也分解,且所述聚磷酸铵与二氧化钛反应,从而生成焦磷酸钛。焦磷酸钛作为灰分残留在发泡隔热层13中,从而提高发泡隔热层13的形状保持性。
基于100质量份的基材,磷系阻燃剂的含量优选在大于或等于20质量份且小于或等于50质量份的范围内。当磷系阻燃剂的含量大于或等于20质量份时,可以使热膨胀性耐火片材1的树脂层11有效地碳化和发泡。此外,可以确保这样形成的发泡隔热层13的形状保持性。磷系阻燃剂的含量小于或等于50质量份时,在热和潮湿环境的情况下可确保耐火性。基于100质量份的基材,磷阻燃剂的含量更优选大于或等于30质量份且小于或等于50质量份。
<<多元醇>>
多元醇在暴露于火加热时被磷系阻燃剂脱水和碳化,且有助于由树脂层11形成可发泡隔热层13。多元醇的分解温度优选高于或等于180℃,更优选高于或等于220℃。多元醇的实例包括单季戊四醇、二季戊四醇和三季戊四醇,多糖例如淀粉和纤维素,以及寡糖例如葡萄糖和果糖。多元醇可以是上述组分中的一种或两种或更多种的组合。特别地,多元醇优选含有选自单季戊四醇、二季戊四醇和三季戊四醇中的至少一种。在这种情况下,可以特别地提高热膨胀性耐火片材1的树脂层11的发泡性。
基于100质量份的基材,多元醇的含量优选在大于或等于5质量份且小于或等于25质量份的范围内。当多元醇的含量大于或等于5质量份时,可以令人满意地由树脂层11形成发泡隔热层13。还可以确保发泡隔热层13的形状保持性。当多元醇的含量小于或等于25质量份时,即使在热和潮湿条件下也可以保持热膨胀性耐火片材1的树脂层11的气体阻隔性能,并保持令人满意的耐火性。还可以确保热膨胀性耐火片材1对建筑结构部分的顺应性。
这里,含氮发泡剂与多元醇的质量比优选在大于或等于0.2且小于4.0的范围内。因此,可以确保在热和潮湿条件下以及在冻融条件下的气体阻隔性能,并且在发生火灾时,可以确保耐火性和与建筑结构部分的顺应性。即,在这种情况下,热膨胀性耐火片材1能够在确保耐火性和顺应性的同时形成形状保持性优良的发泡隔热层13。因此,由树脂层11通过火焰形成的发泡隔热层13难以与建筑结构部脱离,并因此可以抑制火灾向建筑物蔓延和建筑物因火焰而倒塌。注意,冻融条件是指重复冻融的条件。
<<二氧化钛>>
当二氧化钛在高于或等于600℃的高温下加热时,二氧化钛与磷系阻燃剂发生反应,因此生成焦磷酸钛。焦磷酸钛作为灰分残留在发泡隔热层13中,从而提高发泡隔热层13的形状保持性。
二氧化钛的晶体结构可以是锐钛矿型或金红石型,但不限于这些实例。二氧化钛的平均粒径优选在大于或等于0.01μm且小于或等于200μm的范围内,更优选在大于或等于0.1μm且小于或等于100μm的范围内。注意,平均粒径是指以体积为基础得到的粒度分布的累积体积分布曲线中对应于50%的点处的粒径,其中总体积为100%,即指直径(D50)对应于在基于体积的累积中的50%。平均粒径通过使用例如激光衍射粒度分布测量装置测量而获得。
基于100质量份的基材,二氧化钛的含量优选在大于或等于5质量份且小于或等于30质量份的范围内。当二氧化钛的含量大于或等于5质量份时,可以通过在大于或等于600℃的高温下加热产生足够的焦磷酸钛。因此,作为灰分组分的焦磷酸钛充分残留在发泡隔热层13中,从而进一步提高发泡隔热层13的形状保持性。当二氧化钛的含量小于或等于30质量份时,可以抑制发泡率的降低和进一步提高耐火性和冻融时对建筑结构部分的顺应性。注意,膨胀率例如是以发泡后的发泡隔热层13的表观密度与发泡前的树脂层11的密度(固体)的比值而获得的。此外,膨胀率可以以发泡后的发泡隔热层13的厚度与发泡前的树脂层11的厚度的比值而获得。
<<直链丙烯酸系聚合物>>
直链丙烯酸系聚合物包括丙烯酸酯的聚合物(聚丙烯酸酯)、甲基丙烯酸酯的聚合物(聚甲基丙烯酸酯),和丙烯酸酯与甲基丙烯酸酯的共聚物。
直链丙烯酸系聚合物的重均分子量在大于或等于4,000,000且小于或等于20,000,000的范围内。如上所述,当热膨胀性耐火树脂组合物中含有高分子量直链丙烯酸系聚合物时,可以提高熔体弹性。即直链丙烯酸系聚合物中分子的长链与基质树脂(通常为乙烯基树脂)的分子缠结,从而达到假交联状态,这赋予热膨胀性耐火树脂组合物以熔体弹性。熔体弹性还改善了产品的外观。直链丙烯酸系聚合物的分子链越长,即重均分子量越大,直链丙烯酸系聚合物的熔体弹性赋予效果越高。直链丙烯酸系聚合物的具体产品的实例包括由Mitsubishi Chemical Corporation制造的METABLEN(注册商标)P型。
然而,当直链丙烯酸系聚合物的重均分子量小于4,000,000时,具有如此低分子量的直链丙烯酸系聚合物的分子链几乎不缠结在基质树脂分子中,因此不易达到假交联状态。然后,类似于图2所示的常规热膨胀性耐火片材10的情况,发泡隔热层130中的气泡140在受到加热例如火加热时变大或过度变大,导致气泡140消失。相反,当直链状丙烯酸系聚合物的重均分子量大于20,000,000时,具有这种超高分子量的直链丙烯酸系聚合物可能降低热膨胀性耐火树脂组合物的流动性。此外,包含在热膨胀性耐火树脂组合物中的组分可能彼此不均匀混合。
基于100质量份的基材,直链丙烯酸系聚合物的含量优选在大于或等于0.1质量份且小于或等于8质量份的范围内,更优选在大于或等于0.1且小于或等于7质量份的范围内。因此,降低直链丙烯酸类聚合物的含量的上限值,能够抑制热膨胀性耐火树脂组合物的流动性降低。
<<其他>>
在不损害本实施方案的效果的范围内,如果需要,热膨胀性耐火树脂组合物可以含有任意添加剂,例如增塑剂、增粘剂、无机填料、抗氧化剂、润滑剂、加工助剂。
增塑剂的实例包括但不限于烃、邻苯二甲酸、磷酸酯、己二酸酯、癸二酸酯、蓖麻油酸酯、聚酯、环氧树脂和氯化石蜡。在本实施方案中,热膨胀性耐火树脂组合物优选不含增塑剂。当热膨胀性耐火树脂组合物不含增塑剂时,可以进一步提高热膨胀性耐火片材1的气体阻隔性能。
粘合剂的实例包括但不限于松香树脂、松香衍生物、硬树胶(damar)、多萜树脂、改性萜烯、脂肪烃树脂、环戊二烯树脂、芳香石油树脂、酚醛树脂、烷基酚-乙炔树脂、苯乙烯树脂、二甲苯树脂、香豆酮-茚树脂和乙烯基甲苯-α甲基苯乙烯共聚物。
无机填料的实例包括但不特别限于无机盐、无机氧化物、无机纤维和无机细粒。无机盐的实例包括碳酸钙、氢氧化铝、氢氧化镁、高岭土、粘土、膨润土和滑石。无机氧化物的实例包括玻璃鳞片和硅灰石。无机纤维的实例包括岩棉、玻璃纤维、碳纤维、陶瓷纤维、氧化铝纤维和二氧化硅纤维。无机细粒的实例包括碳颗粒和热解法二氧化硅颗粒。
抗氧化剂的实例包括但不限于含有酚化合物的抗氧化剂、含有硫原子的抗氧化剂和含有亚磷酸盐化合物的抗氧化剂。
润滑剂的实例包括但不限于矿物或石油基蜡、植物或动物蜡、酯蜡、有机酸、有机醇和酰胺基化合物。矿物或石油基蜡的实例包括聚乙烯、石蜡和褐煤酸。植物或动物蜡的实例包括妥尔油、油胶油、蜂蜡、巴西棕榈蜡和羊毛脂。有机酸的实例包括硬脂酸、棕榈酸和蓖麻油酸。有机醇的实例包括硬脂醇。酰胺基化合物的实例包括二甲基双酰胺。
加工助剂的实例包括但不限于氯化聚乙烯、甲基丙烯酸甲酯-丙烯酸乙酯共聚物和高分子量聚甲基丙烯酸甲酯。
注意,额外组分如以上所解释的添加剂仅仅是实例,不应视为限制性的,且根据热膨胀性耐火树脂组合物和热膨胀性耐火片材1所需的特性可以混入合适的组分。
<<树脂层的形成方法>>
树脂层11例如可以通过以下方法形成。
首先,上述的乙烯基树脂、含氮发泡剂、磷系阻燃剂、多元醇、二氧化钛和直链丙烯酸系聚合物以及任选存在的其他组分用合适的捏合装置捏合,悬浮在有机溶剂或增塑剂中,或被加热和熔化,从而制备混合物。捏合装置的实例包括但不特别限于加热辊、加压捏合机、挤出机、班伯里密炼机、捏合混合机和两件式辊。捏合温度是热膨胀性耐火树脂组合物适当熔融的温度,至少是多元醇不分解的温度,并且是例如在大于或等于80℃且小于或等于200℃的范围内。通过例如捏合制备的混合物通过成型方法例如热压成型、挤出成型或压延而被成型为片材,从而形成树脂层11。如此制备的具有片材形状的树脂层11可用作热膨胀性耐火片材1。
<热膨胀性耐火片材>
根据本实施方案的热膨胀性耐火片材1包括由热膨胀性耐火树脂组合物形成的树脂层11。即,热膨胀性耐火片材1包含以上所述的包括在热膨胀性耐火树脂组合物中的组分。
因此,热膨胀性耐火片材1的耐火发泡性质优良。具体地,可将热膨胀性耐火片材1的树脂层11的膨胀率提高10倍或以上。如上所述,由于膨胀率高,热膨胀性耐火片材1能够具有令人满意的耐火性。
此外,热膨胀性耐火片材1的泡沫致密度优良。即,发泡后的发泡隔热层13的平均气泡直径可以是小的。具体地,平均气泡直径优选小于1000μm,更优选小于100μm。注意,平均气泡直径可通过例如处理通过观察发泡隔热层13获得的截面图像来获得。
另外,热膨胀性耐火片材1具有耐火性和长时间耐久性,以及优良的形状保持性和片材顺应性。
热膨胀性耐火片材1的树脂层11的厚度没有特别限制,但当热膨胀性耐火片材1安装在建筑结构部分例如底层构件中时,在对建筑结构部分的顺应性方面,优选在大于或等于0.1mm且小于或等于5mm的范围内。热膨胀性耐火片材1的树脂层11的厚度更优选在大于或等于0.3mm且小于或等于3mm的范围内。
热膨胀性耐火片材1可以由成型为片材形状的树脂层11构成,或者可以包括树脂层11和层叠在树脂层11的一个表面上的层例如无机层、有机层和金属层。所述无机层、有机层和金属层中的每一个的厚度,以及这些层堆叠的数量、类型、顺序等没有特别限制并且根据使用地方、对象等进行选择。这些层例如无机层、有机层、金属层的厚度(当两层或更多层层叠时为总厚度)为例如大于或等于0.2mm且小于或等于1mm的范围内。
根据本实施方案的热膨胀性耐火片材1包括树脂层11和无机层12。无机层12与树脂层11重叠。无机层12的实例包括无机纤维,例如岩棉、玻璃棉、玻璃布和陶瓷棉。其中,优选无机层12中含有玻璃纤维。当无机层12含有玻璃纤维时,即便具有比较大的面积的热膨胀性耐火片材1用工具例如敲钉机(tacker)固定在建筑结构部分例如底层构件上,通过由火使树脂层11膨胀和发泡而形成的发泡隔热层13也可变得较不可能脱落。玻璃纤维优选为玻璃纸,且优选具有大于或等于10g/m2且小于或等于100g/m2,更优选大于或等于30g/m2且小于或等于60g/m2的基重(单位面积重量)。
有机层的实例包括:基于醚的树脂,例如聚烯烃树脂(例如,聚乙烯树脂和聚丙烯树脂)、聚苯乙烯树脂、聚酯树脂、聚氨酯树脂和聚酰胺树脂;不饱和酯树脂;共聚物树脂例如乙烯-醋酸乙烯酯共聚物、乙烯乙烯醇共聚物、苯乙烯丁二烯共聚物。有机层的形式的实例包括膜和无纺布。
用于金属层的材料的实例包括铁、钢、不锈钢、镀锌钢、镀铝锌合金的钢、和铝。特别地,就操作性质而言,优选铝箔等。
图1A所示的热膨胀性耐火片材1可以通过例如以下方法制备。即,将具有膜形状的树脂层11和无机层12以适当的方法层叠并一体化,由此制备热膨胀性耐火片材1。在这种情况下,热膨胀性耐火片材1具有由树脂层11和无机层12构成的2层结构。注意,热膨胀性耐火片材1可以包括通过在无机层12的与树脂层11相反的表面上进一步堆叠无机层等而堆叠的三层或更多层。此外,成型方法和成型过程中的温度和压力可以类似于树脂层的形成方法。
(3)总结
从上述实施方案可以看出,本公开包括以下几个方面。注意,添加括号中的参考标记只是为了阐明与以下描述中的实施方案的对应关系。
第一方面的热膨胀性耐火树脂组合物包含乙烯基树脂、含氮发泡剂、磷系阻燃剂、多元醇、二氧化钛和直链丙烯酸系聚合物。直链丙烯酸系聚合物的重均分子量在大于或等于4,000,000且小于或等于20,000,000的范围内。
该方面能够提高耐火发泡性能和泡沫致密度。
在参照第一方面的第二方面的热膨胀性耐火树脂组合物中,乙烯基树脂包括EVA树脂或聚烯烃树脂中的至少一种。
该方面能够进一步提高耐火发泡性能和泡沫致密度。
在参照第二方面的第三方面的热膨胀性耐火树脂组合物中,聚烯烃树脂包含茂金属塑性体。
该方面能够进一步提高耐火发泡性能和泡沫致密度。
在参照第一至第三方面中任一项的第四方面的热膨胀性耐火树脂组合物中,直链丙烯酸系聚合物的含量优选在大于或等于0.1质量份且小于或等于8质量份的范围内,基于不包括直链丙烯酸系聚合物的热膨胀性耐火树脂组合物的100质量份的剩余部分。
该方面能够进一步提高耐火发泡性能和泡沫致密度。
第五方面的热膨胀性耐火片材(1)包括由第一至第四方面中任一项的热膨胀性耐火树脂组合物形成的树脂层(11)。
该方面能够提高耐火发泡性能和泡沫致密度。
参照第五方面的第六方面的热膨胀耐火片材还包括与树脂层(11)重叠的无机层(12)。无机层(12)包括玻璃纤维。
该方面能够进一步提高耐火发泡性能和泡沫致密度。
实施例
参照下面实施例对本发明进行具体地描述。然而,本公开不限于这些实施例。只要能够实现本公开的目的,可以根据设计进行各种修改。
(1)热膨胀性耐火树脂组合物的制备
基于表1至表3所示的含量,将乙烯基树脂、含氮发泡剂、磷系阻燃剂、多元醇、二氧化钛、加工助剂和树脂添加剂用加热辊在130℃下捏合,从而制备热膨胀性耐火树脂组合物。将所述热膨胀性耐火树脂组合物形成为片材,从而获得树脂层(厚度0.6mm)。在树脂层上,用设定为100℃的热压机堆叠作为无机层的耐热片材(Oribest Co.,Ltd.制造的玻璃纤维纸,克重:30g/m2),从而获得热膨胀性耐火片材。
表1和表2中所示的每个组分的细节如下:
·茂金属塑性体:C6系列,MFR:8.0g/10min(Sumitomo Chemical Company,Limited,产品名:EXCELLEN FX402)
·EVA树脂:乙烯-醋酸乙烯酯共聚物,MFR:18g/10min,密度:949kg/m3,醋酸乙烯酯的含量百分比:28%,(TOSOH CORPORATION,产品名:Ultrasen(Nipoflex)710)
·含氮发泡剂:三聚氰胺(Nissan Chemical Corporation)
·磷系阻燃剂:聚磷酸铵(Clariant Japan K.K.,产品名:AP422)
·多元醇:季戊四醇(KOEI CHEMICAL COMPANY,LIMITED,产品名:Dipentalite)
·二氧化钛:平均粒径0.24μm(Huntsman Corporation,产品名称:TR92)
·加工助剂:Mitsubishi Chemical Corporation,产品名:METABLEN A3000。
表3中所示的树脂添加剂的细节如下:
·丙烯酸系聚合物:Mitsubishi Chemical Corporation产品名:METABLEN P-501A(重均分子量:500,000)
·丙烯酸系聚合物:Mitsubishi Chemical Corporation商品名:METABLEN P-530A(重均分子量:3,000,000)
·直链丙烯酸系聚合物:Mitsubishi Chemical Corporation产品名:METABLENP-531A(重均分子量:4,500,000)
·直链丙烯酸系聚合物:Mitsubishi Chemical Corporation产品名:METABLENP-1050(重均分子量:10,000,000)
·PTFE体系:Mitsubishi Chemical Corporation产品名:METABLEN A3000(*与表1和表2中的加工助剂相同)。
(2)评价测试
(2.1)耐火发泡性能
根据基于JIS A1304的标准加热曲线,在炉中将用敲钉机(tacker)固定在硅酸钙板上的热膨胀性耐火片材加热,并测量热膨胀性耐火的膨胀率。膨胀率是以发泡后的发泡隔热层的厚度与发泡前的树脂层的厚度的比值获得的。
A:膨胀率大于或等于10(高膨胀率且耐火)
C:膨胀率大于或等于1且小于10(低膨胀率且不耐火)。
(2.2)泡沫致密度
在耐火发泡性能测试后观察热膨胀性耐火片材的发泡隔热层的横截面,并测量平均气泡直径。
S:平均气泡直径小于100μm(大面积密集部分和最佳隔热性能)
A:平均气泡直径大于或等于100μm且小于1000μm(令人满意的隔热性能,尽管同时形成密集部分和稀疏部分)
C:平均气泡直径大于或等于1000μm(大面积稀疏部分和差的隔热性能)。
(2.3)流动性
热膨胀性耐火树脂组合物的捏合扭矩使用LABO PLASTOMILL(Toyo SeikiSeisaku-sho,Ltd.制造)测定并用作流动性的指标。即,将热膨胀性耐火树脂组合物放入100℃的LABO PLASTOMILL中,然后以10rpm的转速捏合5分钟,读取最终扭矩,并基于以下三个阶段评价流动性。
A:小于40N·m(最佳流动性,易成型性)
B:大于或等于40N·m且小于50N·m(令人满意的流动性,取决于成型条件的成型性)
C:大于或等于50N·m(流动性差,对成型装置施加的负荷大,且无法成型为片材形状)。
[表1]
[表2]
[表3]
在比较例1中,耐火发泡性能至少是令人满意的,但如图3B所示,泡沫致密度低,形成大气泡,且发泡隔热层无法保持其形状并塌陷。
此外,比较例2和3各自含有基于PTFE的树脂添加剂。耐火发泡性能与比较例1一样令人满意,但泡沫致密度与比较例1一样低。即,在比较例2和3中也形成了大气泡,并且然后,发泡隔热层塌陷。当比较例2和3之间比较流动性的结果时,确定的是随着基于PTFE的树脂添加剂的含量增加,捏合时的流动性降低。由此推测,热膨胀性耐火片材的增大的尺寸使热膨胀性耐火片材的制备变得困难。这可能是因为流动所需的粘度受到基于PTFE的树脂添加剂的抑制。
此外,比较例4和5各自代表丙烯酸系聚合物的重均分子量小于4,000,000的情况,且在此情况下,耐火发泡性能略有下降,但没有观察泡沫致密度。这可能是因为重均分子量太低导致在发泡时去除缠结。
此外,如比较例1的情况,比较例6不含有树脂添加剂。在比较例6中,耐火发泡性能和泡沫致密度差。其原因之一可能是比较例6和比较例1之间的基材不同。
相比之下,在实施例1至12中,耐火发泡性和泡沫密度均令人满意(参见例如,显示第一实施例的截面照片的图3A)。这可能是因为直链丙烯酸系聚合物的分子链缠结在基质树脂的分子中,抑制了发泡时气泡的扩大和消泡(爆破)。
作为基材1的基质树脂的茂金属塑性体是没有极性的树脂。相反,作为基材2的基质树脂的EVA树脂是具有极性的树脂。从实施例1至12的结果可以推测,无论基质树脂是否具有极性,直链丙烯酸类聚合物均能够缠结在基质树脂中。直链丙烯酸系聚合物具有极性,因此认为直链丙烯酸系聚合物更可能与EVA树脂缠结。
特别地,实施例1至3、9和11中的每一个含有高分子量直链丙烯酸系聚合物。由实施例2、3和9的结果确认,当直链丙烯酸系聚合物的含量在大于或等于2质量份且小于或等于5质量份的范围内时,泡沫致密度更令人满意。
此外,实施例10至12的结果表明,随着直链丙烯酸系聚合物含量的增加,流动性略有下降,但与比较例3相比,此下降可以忽略。
目前,没有重均分子量大于20,000,000的直链丙烯酸系聚合物。即使有重均分子量大于20,000,000的直链丙烯酸系聚合物,也认为流动性差,因此,直链丙烯酸系聚合物的含量是有限的,且泡沫致密度不能如期增长。
参考标志列表
1 热膨胀性耐火片材
11 树脂层
Claims (6)
1.一种热膨胀性耐火树脂组合物,其包含:
乙烯基树脂;
含氮发泡剂;
磷系阻燃剂;
多元醇;
二氧化钛;和
直链丙烯酸系聚合物,
所述直链丙烯酸系聚合物具有的重均分子量在大于或等于4,000,000且小于或等于20,000,000的范围内。
2.权利要求1所述的热膨胀性耐火树脂组合物,其中所述乙烯基树脂包括EVA树脂或聚烯烃树脂中的至少一种。
3.权利要求2所述的热膨胀性耐火树脂组合物,其中所述聚烯烃树脂包含茂金属塑性体。
4.权利要求1至3中任一项所述的热膨胀性耐火树脂组合物,其中基于所述热膨胀性耐火树脂组合物中不包括所述直链丙烯酸系聚合物的剩余部分100质量份,所述直链丙烯酸系聚合物的含量在大于或等于0.1质量份且小于或等于8质量份的范围内。
5.热膨胀性耐火片材,其包括由权利要求1至4中任一项所述的热膨胀性耐火树脂组合物形成的树脂层。
6.权利要求5所述的热膨胀性耐火片材,其进一步包括与所述树脂层重叠的无机层,其中所述无机层包括玻璃纤维。
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