CN103804775A - 一种无卤阻燃聚烯烃复合泡沫材料及其制备方法 - Google Patents

一种无卤阻燃聚烯烃复合泡沫材料及其制备方法 Download PDF

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CN103804775A
CN103804775A CN201410078359.0A CN201410078359A CN103804775A CN 103804775 A CN103804775 A CN 103804775A CN 201410078359 A CN201410078359 A CN 201410078359A CN 103804775 A CN103804775 A CN 103804775A
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parts
agent
foam material
halogen
composite foam
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CN103804775B (zh
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郑玉婴
陈志杰
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Fuzhou Futong high tech Material Co.,Ltd.
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Fuzhou University
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Priority to PCT/CN2014/094868 priority patent/WO2015131631A1/zh
Priority to US15/100,944 priority patent/US9856356B2/en
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Abstract

本发明公开了一种无卤阻燃聚烯烃复合泡沫材料及其制备方法，所述的复合泡沫材料包括以下组分（按重量份计）：乙烯-醋酸乙烯酯共聚物80~125份、高密度聚乙烯或低密度聚乙烯8~13份、聚烯烃弹性体15~25份、复合阻燃剂85~110份、阻燃增效剂1~8份、复合发泡剂5.5~8份、交联剂0.7~1.0份、增塑剂4.0~5.5份、表面处理剂0.5~1.6份、增容剂20~35份、无机填料6~14份、其他助剂1.6~4.6份。本发明制得的无卤阻燃聚烯烃复合泡沫材料具有良好的柔软性、弹性、耐冲击性等特性，还有密度小、不易压缩变形、减震性好等优点。由于采用了酸源、炭源、气源原料复合的阻燃剂，使得复合泡沫材料具有良好的阻燃性能，同时也大大改善了复合泡沫材料的机械加工性能和物理力学性能，提高复合泡沫材料的应用性能。

Description

一种无卤阻燃聚烯烃复合泡沫材料及其制备方法
技术领域
本发明属于高分子复合材料技术领域，涉及聚烯烃复合泡沫材料的制备，具体涉及一种无卤阻燃聚烯烃复合泡沫材料及其制备方法。
背景技术
聚烯烃复合泡沫材料，尤其是乙烯-醋酸乙烯酯共聚物(EVA) 复合泡沫材料具有密度低、弹性好、耐冲击等优点。但是同大多数聚合物一样，容易燃烧且放热量大、发烟量大，并释放有毒气体并且其来源于石油化工，在自然环境中难以降解，对环境造成了巨大的压力。
目前，随着社会进步以及人们对生命财产安全的重视、环境保护意识的不断增强，聚烯烃复合泡沫材料需要具有无卤阻燃的功能，采用无卤、低烟、低毒的环保型阻燃剂来制备复合泡沫材料已经成为阻燃研究中的一大重点。
按照阻燃剂的使用方法不同可分为反应型和添加型。其中反应型阻燃剂虽然阻燃性持久、毒性较低，但工艺过程复杂，成本高；而添加型阻燃剂阻燃聚合物的工艺简单，使用范围广泛，可选择的阻燃剂种类多。添加型阻燃剂中的膨胀型阻燃体系(IFR)是近年来研究热门的无卤阻燃剂，与氢氧化铝、氢氧化镁等阻燃剂相比，其特点是阻燃效率高、稳定性好、分散均匀、密度小、价格适中，燃烧时低烟、无熔融滴落。
发明内容
本发明的目的在于提供一种无卤阻燃聚烯烃复合泡沫材料及其制备方法，本发明制得的无卤阻燃聚烯烃复合泡沫材料具有良好的柔软性、弹性、耐冲击性等特性，还有密度小、不易压缩变形、减震性好等优点。
为实现上述目的，本发明采用如下技术方案：
一种无卤阻燃聚烯烃复合泡沫材料包括以下组分，按重量份计：
乙烯-醋酸乙烯酯共聚物80~125份；
高密度聚乙烯或低密度聚乙烯8~13份；
聚烯烃弹性体15~25份；
复合阻燃剂85~110份；
阻燃增效剂1~8份；
复合发泡剂5.5~8份；
交联剂0.7~1.0份；
增塑剂4.0~5.5份；
表面处理剂0.5~1.6份；
增容剂20~35份；
无机填料6~14份；
其他助剂1.6~4.6份；
所述的复合阻燃剂是由以下原料复合而成，按重量份计：酸源原料 60~77份，炭源原料 17~22份，气源原料 8~11份。
所述的聚烯烃弹性体为乙烯-辛烯共聚物、乙烯-苯乙烯共聚物、苯乙烯-乙烯-丙烯嵌段共聚物、苯乙烯-乙烯/丁烯-苯乙烯共聚物、苯乙烯-异戊二烯-苯乙烯共聚物中的一种或多种。
所述的酸源原料为聚磷酸铵、多聚磷酸铵、磷酸、硼酸、硼酸盐中的一种或多种；所述的炭源原料为玉米淀粉、木薯淀粉、马铃薯淀粉、绿豆淀粉中的一种；所述的气源原料为三聚氰胺、成炭发泡剂、尿素中的一种或多种；所述的阻燃增效剂为氢氧化铝、六羟基锡酸锌、有机蒙脱土、硼酸锌中的一种或多种。
所述的复合发泡剂为偶氮二甲酰胺、偶氮二异丁腈、碳酸氢钠、1,3-苯二磺酰肼、对甲苯磺酰肼中的一种或多种；所述的交联剂为过氧化二异丙苯；所述的增塑剂为甘油、柠檬酸、乙醇、聚乙烯醇中的两种或两种以上的复配物。
所述的表面处理剂为硅烷类偶联剂、钛酸酯偶联剂、磷酸酯偶联剂、铝钛复合偶联剂中的一种或多种；所述的增容剂为乙烯-丙烯酸、马来酸酐接枝高密度聚乙烯、甲基丙烯酸甲酯、丙烯酸丁酯共聚物中的一种或多种；所述的无机填料为滑石粉、膨润土、高岭土中的一种或两种。
所述的其他助剂，按重量份计为硬脂酸 0.1~0.6份、硬脂酸锌 0.5~1.0份、氧化锌 1~3份。
制备方法包括以下步骤：
（1）将酸源原料和表面处理剂高速搅拌3~5 min后，40~60℃干燥8~10 h；
（2）将炭源原料和增塑剂高速搅拌5~15 min后，装于密封袋中24~48 h；
（3）先将酸源原料和炭源原料充分混合后，加入气源原料，搅拌均匀后置于密封袋中，即为所述的复合阻燃剂；
（4）先将乙烯-醋酸乙烯酯共聚物、高密度聚乙烯或低密度聚乙烯和聚烯烃弹性体加入密炼机中预热5~8 min，然后加入复合阻燃剂、阻燃增效剂、复合发泡剂、交联剂、增容剂、无机填料和其他助剂，在90~120℃下熔融共混10~15 min后出料；
（5）将步骤（4）混炼后的物料快速移到温度控制在78-85℃的开炼机中进行塑炼3~5遍，然后进行破碎；
（6）称量破碎后的物料加入到预热后的模具中，在平板硫化仪160~175℃、10~13 MPa条件下保压8~10 min进行硫化发泡，即得所述的无卤阻燃聚烯烃复合泡沫材料。
本发明的显著优点在于：本发明无卤阻燃聚烯烃复合泡沫材料采用的基体原料为具有良好相容性的乙烯-醋酸乙烯酯共聚物(EVA)，并加入了高密度聚乙烯/低密度聚乙烯、聚烯烃弹性体、增容剂等，提高了有机体和无机体(粉料)的相容性和结合力，可避免了发泡过程中易破孔的现象、因加入的粉料过多而造成的熔体强度降低等不足。复合阻燃剂采用了具有阻燃效率高、燃烧时低烟、无熔融滴落等优点的膨胀型阻燃体系(IFR)，其中炭源原料淀粉具有完全降解的特点，使得本发明具有环保的优点。而无机填料为常用的填料，其作用是对聚烯烃的性能起到改善了尺寸稳定性、增加强度的作用，也一定程度上降低了生产成本。故本发明无卤阻燃聚烯烃复合泡沫材料具有良好的阻燃性能、力学性能、耐冲击、环境友好等优点，有着广泛的市场前景和显著的社会经济效益。
具体实施方式
为了进一步阐述本发明的具体内容，下面将列出具体实施例，但未限于所列出的实施例。
实施例1~3如下表：
 表1 无卤阻燃聚烯烃复合泡沫材料实施例1~3配方(按重量份计)
Figure 2014100783590100002DEST_PATH_IMAGE002
表1中，聚烯烃弹性体为乙烯-辛烯共聚物(POE)；酸源、炭源、气源原料分别为聚磷酸铵、木薯淀粉、三聚氰胺；阻燃增效剂为有机蒙脱土和硼酸锌(比例为1:1)；复合发泡剂为偶氮二甲酰胺；交联剂为过氧化二异丙苯；增塑剂为甘油和柠檬酸(比例为3:4)；表面处理剂为硅烷类偶联剂(KH570)；增容剂为乙烯-丙烯酸共聚物(EAA)；无机填料为滑石粉；其他助剂分别为硬脂酸、硬脂酸锌、氧化锌。
无卤阻燃聚烯烃复合泡沫材料制备工艺如下：
步骤一，酸源原料的表面处理：将聚磷酸铵和KH570置于高速捏合机中，高速搅拌5 min后置于60 ℃烘箱中干燥8 h，备用。
步骤二，炭源原料的增塑处理：将木薯淀粉和增塑剂置于高速捏合机中，高速搅拌10 min后装于密封袋中36 h，备用。
步骤三，混合阻燃剂的混合处理：先将酸源原料和炭源原料充分混合后，加入气源原料，搅拌均匀后置于密封袋中，备用。
步骤四，先将EVA、HDPE/LDPE、POE加入密炼机中预热5 min，然后加入复合阻燃剂、阻燃增效剂、无机填料等余下原料，在100 ℃下熔融共混12 min后出料。
步骤五，将步骤四混炼后的物料快速移到温度控制在80 ℃左后的开炼机中进行薄塑炼3~5遍，然后在快速破粹机里进行破粹。
步骤六，称量适量的经步骤五破粹后的物料加入到预热后的模具中，在平板硫化仪170 ℃、12 MPa条件下保压9 min进行硫化发泡，即得无卤阻燃聚烯烃复合泡沫材料。
以上实施例(1、2、3)所制备得的无卤阻燃聚烯烃复合泡沫材料的部分性能与adidas PO-EVA00049标准比较结果如下表所示：
表2 部分性能比较结果
Figure 2014100783590100002DEST_PATH_IMAGE004
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。

Claims (7)

1.一种无卤阻燃聚烯烃复合泡沫材料，其特征在于：包括以下组分，按重量份计：
乙烯-醋酸乙烯酯共聚物80~125份；
高密度聚乙烯或低密度聚乙烯8~13份；
聚烯烃弹性体15~25份；
复合阻燃剂85~110份；
阻燃增效剂1~8份；
复合发泡剂5.5~8份；
交联剂0.7~1.0份；
增塑剂4.0~5.5份；
表面处理剂0.5~1.6份；
增容剂20~35份；
无机填料6~14份；
其他助剂1.6~4.6份；
所述的复合阻燃剂是由以下原料复合而成，按重量份计：酸源原料 60~77份，炭源原料 17~22份，气源原料 8~11份。
2.根据权利要求1所述的无卤阻燃聚烯烃复合泡沫材料，其特征在于：所述的聚烯烃弹性体为乙烯-辛烯共聚物、乙烯-苯乙烯共聚物、苯乙烯-乙烯-丙烯嵌段共聚物、苯乙烯-乙烯/丁烯-苯乙烯共聚物、苯乙烯-异戊二烯-苯乙烯共聚物中的一种或多种。
3.根据权利要求1所述的无卤阻燃聚烯烃复合泡沫材料，其特征在于：所述的酸源原料为聚磷酸铵、多聚磷酸铵、磷酸、硼酸、硼酸盐中的一种或多种；所述的炭源原料为玉米淀粉、木薯淀粉、马铃薯淀粉、绿豆淀粉中的一种；所述的气源原料为三聚氰胺、成炭发泡剂、尿素中的一种或多种；所述的阻燃增效剂为氢氧化铝、六羟基锡酸锌、有机蒙脱土、硼酸锌中的一种或多种。
4.根据权利要求1所述的无卤阻燃聚烯烃复合泡沫材料，其特征在于：所述的复合发泡剂为偶氮二甲酰胺、偶氮二异丁腈、碳酸氢钠、1,3-苯二磺酰肼、对甲苯磺酰肼中的一种或多种；所述的交联剂为过氧化二异丙苯；所述的增塑剂为甘油、柠檬酸、乙醇、聚乙烯醇中的两种或两种以上的复配物。
5.根据权利要求1所述的无卤阻燃聚烯烃复合泡沫材料，其特征在于：所述的表面处理剂为硅烷类偶联剂、钛酸酯偶联剂、磷酸酯偶联剂、铝钛复合偶联剂中的一种或多种；所述的增容剂为乙烯-丙烯酸、马来酸酐接枝高密度聚乙烯、甲基丙烯酸甲酯、丙烯酸丁酯共聚物中的一种或多种；所述的无机填料为滑石粉、膨润土、高岭土中的一种或两种。
6.根据权利要求1所述的无卤阻燃聚烯烃复合泡沫材料，其特征在于：所述的其他助剂，按重量份计为硬脂酸 0.1~0.6份、硬脂酸锌 0.5~1.0份、氧化锌 1~3份。
7.一种制备如权利要求1所述的无卤阻燃聚烯烃复合泡沫材料的方法，其特征在于：包括以下步骤：
（1）将酸源原料和表面处理剂高速搅拌3~5 min后，40~60℃干燥8~10 h；
（2）将炭源原料和增塑剂高速搅拌5~15 min后，装于密封袋中24~48 h；
（3）先将酸源原料和炭源原料充分混合后，加入气源原料，搅拌均匀后置于密封袋中，即为所述的复合阻燃剂；
（4）先将乙烯-醋酸乙烯酯共聚物、高密度聚乙烯或低密度聚乙烯和聚烯烃弹性体加入密炼机中预热5~8 min，然后加入复合阻燃剂、阻燃增效剂、复合发泡剂、交联剂、增容剂、无机填料和其他助剂，在90~120℃下熔融共混10~15 min后出料；
（5）将步骤（4）混炼后的物料快速移到温度控制在78-85℃的开炼机中进行塑炼3~5遍，然后进行破碎；
（6）称量破碎后的物料加入到预热后的模具中，在平板硫化仪160~175℃、10~13 MPa条件下保压8~10 min进行硫化发泡，即得所述的无卤阻燃聚烯烃复合泡沫材料。
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