CN106867080B - 一种滚塑专用阻燃抗静电聚乙烯组合物及其制备方法 - Google Patents
一种滚塑专用阻燃抗静电聚乙烯组合物及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分按质量百分比为LLDPE 5%~25%,LDPE 25%~45%,阻燃抗静电母料30%~50%;其中所述无卤阻燃抗静电母料的组分包含LLDPE 20%~35%,导电碳黑5%~12%,可膨胀石墨8%~16%,磷氮系膨胀型阻燃剂30%~38%,抗静电剂1%~2%,偶联剂0.6%~1.5%,增韧剂4%~8%,PE蜡0.6%~2%,抗氧剂0.4%~1.0%。本发明同时也公开了一种滚塑专用无卤阻燃抗静电聚乙烯组合物的制备方法。所制备的组合物其熔融指数为≥5g/10min,拉伸强度为10~12MPa,简支梁缺口冲击强度为5~10kJ/m2,表面电阻为106~107Ω,阻燃级别为UL94 V‑0级。
Description
技术领域
本发明涉及阻燃抗静电聚乙烯组合物领域,具体涉及滚塑专用的阻燃抗静电聚乙烯组合物及其制备方法。
背景技术
聚乙烯(PE)作为产量最大的通用塑料之一,由于质轻、易成型、低毒性、良好的电气绝缘性和机械性能,已应用于日常生活的方方面面。然而它的极限氧指数很低,极易燃烧,严重影响了它的广泛应用。
此外,PE也具有优良的电绝缘性能,但在某些特殊应用领域,正是由于PE的高电阻率(1016Ω·cm)往往使其在使用过程中容易产生静电积累,从而造成静电吸尘乃至静电放电等不良现象,严重的甚至会引起火灾。因此,对于特定的场所(如矿山内),必须对PE进行阻燃和抗静电改性。
滚塑成型工艺通常用于制备中、大型中空制品,如大型水箱、风机外壳、儿童滑梯、洗地机等。由于滚塑过程为了保证物料快速熔融,因此原料必须磨粉至40目左右才能使用;而且滚塑过程通常需要在250℃左右加热10min以上,一般的工程塑料很难承受这么长时间的加热而发生降解,因此目前滚塑成型所使用的原料大部分是PE粉。
由于滚塑成型过程中没有剪切力的作用,物料熔融后主要依靠重力作用而在模具内部成型,因此物料的流变学性能十分重要。通常用于制备滚塑制品的PE原料,其熔融指数要大于3g/10min才能满足成型,而对于结构复杂的模具,熔融指数的要求更高。
目前涉及阻燃抗静电PE的专利,其填充量通常达到30%~40%,如此高的填充量导致共混物的流动性极差,就算加入流动改性剂,其熔指也一般<0.5g/10min,无法用于滚塑成型工艺。专利CN201210557511涉及阻燃抗静电双功能改性聚乙烯复合材料及其制备方法,专利中得到的阻燃抗静电聚乙烯组合物的熔指<0.5g/10min,远远无法满足滚塑成型的需求。
发明内容
本发明的范围只由权利要求书所规定,在任何程度上都不受这一节发明内容的陈述所限。
本发明旨在提供一种适用于滚塑工艺的阻燃效果佳、抗静电性能高的阻燃抗静电聚乙烯及其制备方法。
为实现上述目的本发明采用的技术方案是:一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分包含LLDPE 5%~25%,LDPE 25%~45%,阻燃抗静电母料30%~50%;其中,所述的无卤阻燃抗静电母料的组分包含LLDPE 20%~35%、导电碳黑5%~12%、可膨胀石墨8%~16%、磷氮系膨胀型阻燃剂30%~38%、抗静电剂1%~2%、偶联剂0.6%~1.5%、增韧剂4%~8%、PE蜡0.6%~2%、抗氧剂0.4%~1.0%。以上比例均为质量百分比。
其中,所述的LLDPE熔融指数≥20g/10min,拉伸屈服强度≥13MPa,简支梁缺口冲击强度≥50kJ/m2;LDPE熔融指数≥50g/10min,拉伸屈服强度≥8MPa,简支梁缺口冲击强度≥60kJ/m2。
其中,所述的磷氮系膨胀型阻燃剂为聚磷酸胺(APP)、三聚氰胺(MEL)、季戊四醇(PER)按重量份数APP:MEL:PER=7:3:4的比例混合而成。
其中,所述的无卤阻燃抗静电母料中,导电碳黑的粒径≥800目
其中,所述的无卤阻燃抗静电母料中,可膨胀石墨(EG)为超细可膨胀石墨,粒度≥200目,膨胀倍率为20~50mL/g,含碳率>99.3%。
其中,所述的无卤阻燃抗静电母料中,抗静电剂为季铵盐类抗静电剂HDC-103、HDC-200、HDC-100K、Irgastat P18中的一种或其组合。
其中,所述的无卤阻燃抗静电母料中,偶联剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂中的一种或其组合。
其中,所述的无卤阻燃抗静电母料中,增韧剂为POE-g-MAH、POE-g-GMA、PE-g-MAH中的一种或其组合。
其中,所述的无卤阻燃抗静电母料中,抗氧剂为1010、168、1098、H10中的一种或其组合。
一种滚塑专用无卤阻燃抗静电聚乙烯组合物的制备方法,包括以下步骤:
(1)母料制备:按重量配比称取导电碳黑、可膨胀石墨、偶联剂、PE蜡加入高速混合机中,共混温度85~110℃,共混时间5~8min;再加入LLDPE、磷氮系膨胀型阻燃剂、抗静电剂、增韧剂、抗氧剂在80℃左右共混3~5min;将上述混合均匀的物料投入双螺杆挤出机中挤出、冷却、切粒、干燥,即得阻燃抗静电母料;
(2)造粒:按照重量配比称取阻燃抗静电母料、LLDPE、LDPE,在高速混合机中共混3min,再次投入双螺杆挤出机中挤出、冷却、切粒、所得粒子干燥备用;
(3)磨粉:在氮气的保护下,使用磨粉机将步骤(2)所得粒子磨成40目左右的粉末,既得滚塑专用无卤阻燃抗静电聚乙烯组合物。
采用本发明提供的技术方案,制备的滚塑专用无卤阻燃抗静电聚乙烯组合物熔指≥5g/10min,其拉伸强度为10~12MPa,简支梁缺口冲击强度为5~10kJ/m2,表面电阻为106~107Ω,阻燃等级达到UL 94V-0级别。
具体实施方式
下面结合具体实施例来进一步说明本发明的技术方案。
实施例1:
一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分按质量百分配比为:LLDPE15%、LDPE 35%、阻燃抗静电母料50%;其中所述的阻燃抗静电母料的组分包含LLDPE34.4%、导电碳黑12%、可膨胀石墨12%、磷氮系膨胀型阻燃剂30%、抗静电剂HDC-100K2.0%、铝酸酯偶联剂1.0%、POE-g-GMA6.0%、PE蜡2.0%,抗氧剂0.6%。
制备方法:
(1)母料制备:按重量配比称取导电碳黑、可膨胀石墨、偶联剂、PE蜡加入高速混合机中,共混温度85~110℃,共混时间5~8min;再加入LLDPE、磷氮系膨胀型阻燃剂、抗静电剂、增韧剂、抗氧剂在80℃左右共混3~5min;将上述混合均匀的物料投入双螺杆挤出机中挤出、冷却、切粒、干燥,即得阻燃抗静电母料;
(2)造粒:按照重量配比称取阻燃抗静电母料、LLDPE、LDPE,在高速混合机中共混3min,再次投入双螺杆挤出机中挤出、冷却、切粒、所得粒子干燥备用;
(3)磨粉:在氮气的保护下,使用磨粉机将步骤(2)所得粒子磨成40目左右的粉末,既得滚塑专用无卤阻燃抗静电聚乙烯组合物。
实施例2:
一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分按质量百分配比为:LLDPE20%、LDPE 30%、阻燃抗静电母料50%;其中所述的阻燃抗静电母料的组分包含LLDPE30%、导电碳黑10%、可膨胀石墨16%、磷氮系膨胀型阻燃剂32%、抗静电剂HDC-100K2.0%、硅烷偶联剂1.0%、POE-g-GMA6.0%、PE蜡2.0%,抗氧剂1.0%。
制备方法:同实施例1。
实施例3:
一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分按质量百分配比为:LLDPE5%、LDPE 45%、阻燃抗静电母料50%;其中所述的阻燃抗静电母料的组分包含LLDPE20%、导电碳黑12%、可膨胀石墨16%、磷氮系膨胀型阻燃剂38%、抗静电剂HDC-2002%、硅烷偶联剂1%、POE-g-GMA8%、PE蜡2%,抗氧剂1%。
制备方法:同实施例1。
实施例4:
一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分按质量百分配比为:LLDPE12%、LDPE 43%、阻燃抗静电母料45%;其中所述的阻燃抗静电母料的组分包含LLDPE20%、导电碳黑10%、可膨胀石墨15%、磷氮系膨胀型阻燃剂36%、抗静电剂HDC-100K2%、钛酸酯偶联剂1%、POE-g-GMA 8%、PE蜡2%,抗氧剂1%。
制备方法:同实施例1。
实施例5:
一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分按质量百分配比为:LLDPE20%、LDPE 40%、阻燃抗静电母料40%;其中所述的阻燃抗静电母料的组分包含LLDPE30%、导电碳黑8%、可膨胀石墨13%、磷氮系膨胀型阻燃剂35%、抗静电剂HDC-2001.5%、硅烷偶联剂1.5%、POE-g-MAH 8%、PE蜡2%,抗氧剂1%。
制备方法:同实施例1。
实施例6:
一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分按质量百分配比为:LLDPE25%、LDPE 45%、阻燃抗静电母料30%;其中所述的阻燃抗静电母料的组分包含LLDPE35%、导电碳黑5%、可膨胀石墨8%、磷氮系膨胀型阻燃剂38%、抗静电剂HDC-100K2%、铝酸酯偶联剂1.5%、PE-g-MAH 7.5%、PE蜡2%,抗氧剂1%。
制备方法:同实施例1。
实施例7:
一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分按质量百分配比为:LLDPE22%、LDPE 43%、阻燃抗静电母料35%;其中所述的阻燃抗静电母料的组分包含LLDPE35%、导电碳黑10%、可膨胀石墨10%、磷氮系膨胀型阻燃剂33%、抗静电剂HDC-100K 1%、硅烷偶联剂0.6%、POE-g-GMA 8%、PE蜡2%,抗氧剂0.4%。
制备方法:同实施例1。
实施例8:
一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分按质量百分配比为:LLDPE25%、LDPE 25%、阻燃抗静电母料50%;其中所述的阻燃抗静电母料的组分包含LLDPE35%、导电碳黑12%、可膨胀石墨12%、磷氮系膨胀型阻燃剂30%、抗静电剂HDC-100K 1%、钛酸酯偶联剂1%、POE-g-MAH 6%、PE蜡2%,抗氧剂1%。
制备方法:同实施例1。
实施例9:
一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分按质量百分配比为:LLDPE15%、LDPE 41%、阻燃抗静电母料44%;其中所述的阻燃抗静电母料的组分包含LLDPE35%、导电碳黑12%、可膨胀石墨15%、磷氮系膨胀型阻燃剂30%、抗静电剂HDC-100K1.3%、硅烷偶联剂1.5%、PE-g-MAH 4%、PE蜡0.6%,抗氧剂0.6%。
制备方法:同实施例1。
实施例10:
一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其组分按质量百分配比为:LLDPE8%、LDPE 45%、阻燃抗静电母料47%;其中所述的阻燃抗静电母料的组分包含LLDPE35%、导电碳黑5.2%、可膨胀石墨9%、磷氮系膨胀型阻燃剂38%、抗静电剂HDC-100K2%、铝酸酯偶联剂0.8%、POE-g-GMA8%、PE蜡1.2%,抗氧剂1%。
制备方法:同实施例1。
表1各实施例物性表
Claims (7)
1.一种滚塑专用无卤阻燃抗静电聚乙烯组合物,其特征在于,组合物包含LLDPE 5%~25%,LDPE 25%~45%,阻燃抗静电母料30%~50%;所述的阻燃抗静电母料的组分包含LLDPE 20%~35%、导电碳黑5%~12%、可膨胀石墨8%~16%、磷氮系膨胀型阻燃剂30%~38%、抗静电剂1%~2%、偶联剂0.6%~1.5%、增韧剂4%~8%、PE蜡0.6%~2%、抗氧剂0.4%~1.0%;以上比例均为质量百分比;
所述的LLDPE的熔融指数≥20g/10min,拉伸屈服强度≥13MPa,简支梁缺口冲击强度≥50kJ/m2;所述的LDPE的熔融指数≥50g/10min,拉伸屈服强度≥8MPa,简支梁缺口冲击强度≥60kJ/m2;所述的阻燃抗静电母料中,导电碳黑的粒径≥800目;所述的阻燃抗静电母料中,可膨胀石墨为超细可膨胀石墨,粒度≥200目,膨胀倍率为20~50mL/g,含碳率>99.3%。
2.根据权利要求 1所述的滚塑专用无卤阻燃抗静电聚乙烯组合物,其特征在于,所述的阻燃抗静电母料中,磷氮系膨胀型阻燃剂为聚磷酸胺APP、三聚氰胺MEL、季戊四醇PER按重量份数APP:MEL:PER=7:3:4的比例混合而成。
3.根据权利要求 1所述的滚塑专用无卤阻燃抗静电聚乙烯组合物,其特征在于,所述的阻燃抗静电母料中,抗静电剂为季铵盐类抗静电剂HDC-103、HDC-200、HDC-100K、Irgastat P18中的一种或其组合。
4.根据权利要求 1所述的滚塑专用无卤阻燃抗静电聚乙烯组合物,其特征在于,所述的阻燃抗静电母料中,偶联剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂中的一种或其组合。
5.根据权利要求 1所述的滚塑专用无卤阻燃抗静电聚乙烯组合物,其特征在于,所述的阻燃抗静电母料中,增韧剂为POE-g-MAH、POE-g-GMA、PE-g-MAH中的一种或其组合。
6.根据权利要求 1所述的滚塑专用无卤阻燃抗静电聚乙烯组合物,其特征在于,所述的阻燃抗静电母料中,抗氧剂为1010、168、1098、H10中的一种或其组合。
7.根据权利要求 1所述的一种滚塑专用无卤阻燃抗静电聚乙烯组合物的制备方法,其特征在于,包括以下步骤:
(1)母料制备:按重量配比称取导电碳黑、可膨胀石墨、偶联剂、PE蜡加入高速混合机中,共混温度85~110℃,共混时间5~8min;再加入LLDPE、磷氮系膨胀型阻燃剂、抗静电剂、增韧剂、抗氧剂在80℃共混3~5min;将上述混合均匀的物料投入双螺杆挤出机中挤出、冷却、切粒、干燥,即得阻燃抗静电母料;
(2)造粒:按照重量配比称取阻燃抗静电母料、LLDPE、LDPE,在高速混合机中共混3min,再次投入双螺杆挤出机中挤出、冷却、切粒、所得粒子干燥备用;
(3)磨粉:在氮气的保护下,使用磨粉机将步骤(2)所得粒子磨成40目的粉末,即得滚塑专用无卤阻燃抗静电聚乙烯组合物。
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