CN107383545A - 一种改性白石墨烯复合聚乙烯管材及其制备方法 - Google Patents
一种改性白石墨烯复合聚乙烯管材及其制备方法 Download PDFInfo
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Abstract
本发明涉及塑料管道技术领域,具体涉及一种改性白石墨烯复合聚乙烯管材,该管材按重量份数组成为100份管材级聚乙烯树脂、5~30份偶联剂、0.1~20份改性白石墨烯、5~40份填料、0.05~10份抗氧剂、0.5‑15份分散剂。还公开了该管材的制备方法,包括白石墨烯改性、共混、母粒制备挤出成型得到改性白石墨烯复合聚乙烯管材成品。本发明充分利用塑料改性、成型加工产业化现有设备,改性白石墨烯少量添加即可提高复合聚乙烯管材的力学性能、抗老化性能、导热性,同时柔韧性好,阻氧性和耐化学腐蚀性也得到明显提升,且易于加工、成本较低,特别适用于建筑地面辐射采暖管道等管材领域,具有很大的应用价值。
Description
技术领域
本发明涉及塑料管道技术领域,具体涉及一种改性白石墨烯复合聚乙烯管材及其制备方法。
背景技术
塑料管道与金属管道相比因具有独特的性能,被广泛应用于冷热给水、排水、燃气管道、能源采暖***等工程领域。随着社会不断发展和人们生活水平的提高,对塑料管道的某些特定性能和综合性能的要求日益苛刻。
聚乙烯是塑料中结构最简单、应用最为广泛的一类高分子材料,聚乙烯因无臭、无毒、化学稳定性好、常温下不溶于一般溶剂、吸湿性小、且耐大多数酸碱腐蚀(但不耐具有氧化性酸)等特性被广泛应用于各种功能性管道***。但聚乙烯对化学和机械等环境应力非常敏感、对氧气等活性气体阻隔性不强以及耐热抗老化性能差等缺陷也限制了在某些特定功能管材领域的进一步应用。
目前市场上采用改性石墨粉、锌氧粉等复合聚乙烯管材来提高聚乙烯管材对氧阻隔性、耐腐蚀性、导热性、耐热抗老化性能,使其在能源采暖管道等这一特定领域得到广泛应用。但这些经过改性复合的聚乙烯管材中改性石墨粉、锌氧粉的添加量很大,性能才复合要求,不利于挤出工艺和管材成型工艺、且成本较大。
发明内容
有鉴于此,有必要针对上述问题,提供一种改性白石墨烯复合聚乙烯管材及其制备方法。
为实现上述目的,本发明采取以下技术方案:
本发明的改性白石墨烯复合聚乙烯管材,按重量份数组成为100份管材级聚乙烯树脂、5~30份偶联剂、0.1~20份改性白石墨烯、5~40份填料、0.05~10份抗氧剂、0.5-15份分散剂。
作为优选的,所述改性白石墨烯复合聚乙烯管材,按重量份数组成为100份管材级聚乙烯树脂、5~15份偶联剂、0.1~10份改性白石墨烯、10~30份填料、0.1~5份抗氧剂、1-10份分散剂。
进一步的,所述偶联剂为硅烷偶联剂KH-570、硅烷偶联剂KH-590、钛酸正丁酯中的一种;
所述填料为气相二氧化硅、轻质纳米碳酸钙、钛白粉中的一种或多种;
所述抗氧剂为酚类抗氧剂1010(CAS号:6683-19-8)、酚类抗氧剂1076(CAS号:2082-79-3)、酚类抗氧剂168(31570-04-4)、胺类抗氧剂1098(23128-74-7)中的一种或多种;
所述分散剂包含硬脂酸钙、石蜡、聚乙烯蜡中的一种或多种。
进一步的,所述改性白石墨烯为选用5-10层的白石墨烯用0.1-0.5%表面活性剂溶液浸泡22-26小时,经离心、真空干燥后得到。
作为优选的,所述改性白石墨烯为选用10层的白石墨烯,用0.4%表面活性剂溶液浸泡24小时,经离心、真空干燥后得到。
作为优选的,所述表面活性剂溶液包括长链路易斯碱、长链路易斯酸、磺酸化物、季胺化物、非离子型表面活性剂溶液中的一种或多种。
作为更优选的,所述长链路易斯碱溶液为油胺水溶液;所述长链路易斯酸溶液为长链硼烷乙醇溶液;所述磺酸化物为十二烷基苯磺酸钠乙醇溶液;所述季胺化物为溴化十六烷基吡啶乙醇溶液;非离子型表面活性剂为聚环氧乙烷烷基醇酰胺乙醇溶液。
一种改性白石墨烯复合聚乙烯管材的制备方法,包括以下步骤:
1)白石墨烯改性:选用5-10层的白石墨烯制备改性白石墨烯;
2)共混:按重量份数分别称取一定量的管材级聚乙烯树脂、偶联剂、改性白石墨烯、填料、抗氧剂以及分散剂,经高速混合机均匀混合;
3)母粒的制备:将步骤2)混合后的原料经双螺杆挤出机熔融挤出,水冷拉条切粒后得到改性白石墨烯聚乙烯母粒;
4)挤出成型:将步骤3)得到的改性白石墨烯聚乙烯母粒再经管材挤出机挤出成型,得到改性白石墨烯复合聚乙烯管材成品。
进一步的,步骤3)所述母粒的制备,双螺杆挤出机各区温度为140-220℃,机头温度为150-230℃。
作为优选的,双螺杆挤出机各区温度为170-210℃,机头温度为220℃。
进一步的,步骤4)所述管材挤出机挤出成型温度为140-230℃。
作为优选的,步骤4)所述管材挤出机挤出成型温度为160-210℃。
进一步的,步骤2)所述高速混合机混合时间为1-20min,优选3-15min。
与现有技术相比,本发明的有益效果为:
5~10层的改性白石墨烯,因其为单层或少层六方氮化硼,具有类似石墨烯原子级厚度的二维特性,耐高温达2000℃,并有良好的隔离气体性能。且强度、导热系数非常高,同时具有柔性、化学惰性等特性。本发明的改性白石墨烯与复合的聚乙烯管材采用恰当的配比组合,在管材级聚乙烯中添加少量改性白石墨烯,当原子层少于十层时,片层排列紧凑、均匀,且阻挡片层数目较多,气体在聚乙烯基体中绕行,路径变长,少量添加就能很好的阻挡氧气等气体通过;同时经改性的白石墨烯与聚乙烯基体有更好的亲和性,致密分散于基体中,而且同样重量下的改性白石墨烯片层数更多,层与层之间会结合得更紧密隔离氧气的能力更强,因此添加改性白石墨烯的复合聚乙烯管材的阻氧性、力学强度、耐化学腐蚀性更强。
本发明的改性白石墨烯复合聚乙烯管材在阻氧性、力学性能、抗老化性能、导热性、柔韧性、耐化学腐蚀性等得到明显提升的同时,又充分利用塑料改性、成型加工产业化现有设备,易于加工、成本较低,可广泛应用于建筑给水、排水、散热器管道,特别适用于建筑地面辐射采暖管道等管材领域,具有很大的应用价值。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面将结合本发明实施例,对本发明的技术方案作进一步清楚、完整地描述。需要说明的是,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
步骤1)白石墨烯改性:选用5-10层的白石墨烯用0.4%油胺水溶液浸泡24小时,经离心、真空干燥后得改性白石墨烯;
步骤2)共混:按重量份数分别称取100份管材级聚乙烯树脂、6份硅烷偶联剂KH-570、0.1份改性白石墨烯、20份气相二氧化硅、0.3份酚类抗氧剂1010以及4份聚乙烯蜡经高速混合机均匀混合8min后出料;
步骤3)母粒的制备:将步骤2)均匀混合后的原料经双螺杆挤出机熔融挤出,挤出机各区温度180℃、机头温度220℃,再经水冷拉条切粒后得到改性白石墨烯聚乙烯母粒;
步骤4)挤出成型:将步骤3)得到的改性白石墨烯聚乙烯母粒再经管材挤出机挤出成型,挤出温度为175℃,得到改性白石墨烯复合聚乙烯管材成品。
实施例2
步骤1)白石墨烯改性:选用5-10层的白石墨烯用0.4%油胺水溶液浸泡24小时,经离心、真空干燥后得改性白石墨烯;
步骤2)共混:按重量份数分别称取100份管材级聚乙烯树脂、8份硅烷偶联剂KH-570、5份改性白石墨烯、25份气相二氧化硅、0.5份酚类抗氧剂1010以及6份聚乙烯蜡经高速混合机均匀混合10min后出料;
步骤3)母粒的制备:将步骤2)均匀混合后的原料经双螺杆挤出机熔融挤出,挤出机各区温度190℃、机头温度220℃,再经水冷拉条切粒后得到改性白石墨烯聚乙烯母粒;
步骤4)挤出成型:将步骤3)得到的改性白石墨烯聚乙烯母粒再经管材挤出机挤出成型,挤出温度为190℃,得到改性白石墨烯复合聚乙烯管材成品。
实施例3
步骤1)白石墨烯改性:选用5-10层的白石墨烯用0.4%长链硼烷乙醇溶液浸泡24小时,经离心、真空干燥后得改性白石墨烯;
步骤2)共混:按重量份数分别称取100份管材级耐热聚乙烯树脂、10份硅烷偶联剂KH-570、10份改性白石墨烯、30份气相二氧化硅、1份酚类抗氧剂168以及8份聚乙烯蜡经高速混合机均匀混合15min后出料;
步骤3)母粒的制备:将步骤2)均匀混合后的原料经双螺杆挤出机熔融挤出,挤出机各区温度200℃、机头温度220℃,再经水冷拉条切粒后得到改性白石墨烯聚乙烯母粒;
步骤4)挤出成型:将步骤3)得到的改性白石墨烯聚乙烯母粒再经管材挤出机挤出成型,挤出温度为200℃,得到改性白石墨烯复合聚乙烯管材成品。
实施例4
步骤1)白石墨烯改性:选用5-10层的白石墨烯用0.5%聚环氧乙烷烷基醇酰胺乙醇溶液浸泡24小时,经离心、真空干燥后得改性白石墨烯;
步骤2)共混:按重量份数分别称取100份管材级耐热聚乙烯树脂、6份钛酸正丁酯、20份改性白石墨烯、20份轻质纳米碳酸钙、0.3份酚类抗氧剂1076以及4份硬脂酸钙经高速混合机均匀混合8min后出料;
步骤3)母粒的制备:将步骤2)均匀混合后的原料经双螺杆挤出机熔融挤出,挤出机各区温度180℃、机头温度220℃,再经水冷拉条切粒后得到改性白石墨烯聚乙烯母粒;
步骤4)挤出成型:将步骤3)得到的改性白石墨烯聚乙烯母粒再经管材挤出机挤出成型,挤出温度为200℃,得到改性白石墨烯复合聚乙烯管材成品。
对比实施例1
步骤1)共混:按重量份数分别称取100份管材级耐热聚乙烯树脂、6份钛酸正丁酯、20份轻质纳米碳酸钙、0.3份酚类抗氧剂1076以及4份硬脂酸钙经高速混合机均匀混合8min后出料;
步骤2)改性白石墨烯聚乙烯母粒的制备:将步骤2)均匀混合后的原料经双螺杆挤出机熔融挤出,挤出机各区温度180℃、机头温度220℃,再经水冷拉条切粒后得到改性白石墨烯聚乙烯母粒;
步骤3)挤出成型:将步骤2)得到的改性白石墨烯聚乙烯母粒再经管材挤出机挤出成型,挤出温度为180℃,得到改性白石墨烯复合聚乙烯管材成品。
表一各实施例对应的性能检测数据
与未添加改性白石墨烯的普通聚乙烯管材性能相比,本发明制备的改性白石墨烯复合聚乙烯管材,拉伸性能最大提高了59%,抗老化性能提高了36%,导热性最高提高了169%,透氧率低至0.02mg/(L.day),同时柔韧性、耐化学腐蚀性和抗老化性能也得到相应的增强,易于加工、成本较低,具有很大的应用空间。
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (9)
1.一种改性白石墨烯复合聚乙烯管材,其特征在于,按重量份数组成为100份管材级聚乙烯树脂、5~30份偶联剂、0.1~20份改性白石墨烯、5~40份填料、0.05~10份抗氧剂、0.5-15份分散剂。
2.根据权利要求1所述的改性白石墨烯复合聚乙烯管材,其特征在于,
所述偶联剂为硅烷偶联剂KH-570、硅烷偶联剂KH-590、钛酸正丁酯中的一种;
所述填料为气相二氧化硅、轻质纳米碳酸钙、钛白粉中的一种或多种;
所述抗氧剂为酚类抗氧剂1010、酚类抗氧剂1076、酚类抗氧剂168、胺类抗氧剂1098中的一种或多种;
所述分散剂包含硬脂酸钙、石蜡、聚乙烯蜡中的一种或多种。
3.根据权利要求1或2所述的改性白石墨烯复合聚乙烯管材,其特征在于,所述改性白石墨烯为选用5-10层的白石墨烯,用0.1-0.5%表面活性剂溶液浸泡22-26小时,经离心、真空干燥后得到。
4.根据权利要求3所述的改性白石墨烯复合聚乙烯管材,其特征在于,所述表面活性剂溶液包括长链路易斯碱、长链路易斯酸、磺酸化物、季胺化物、非离子型表面活性剂溶液中的一种或多种。
5.根据权利要求4所述的改性白石墨烯复合聚乙烯管材,其特征在于,所述长链路易斯碱溶液为油胺水溶液;所述长链路易斯酸溶液为长链硼烷乙醇溶液;所述磺酸化物为十二烷基苯磺酸钠乙醇溶液;所述季胺化物为溴化十六烷基吡啶乙醇溶液;非离子型表面活性剂为聚环氧乙烷烷基醇酰胺乙醇溶液。
6.一种改性白石墨烯复合聚乙烯管材的制备方法,其特征在于,包括以下步骤:
1)白石墨烯改性:选用5-10层的白石墨烯制备改性白石墨烯;
2)共混:按重量份数分别称取一定量的管材级聚乙烯树脂、偶联剂、改性白石墨烯、填料、抗氧剂以及分散剂,经高速混合机均匀混合;
3)母粒的制备:将步骤2)混合后的原料经双螺杆挤出机熔融挤出,水冷拉条切粒后得到改性白石墨烯聚乙烯母粒;
4)挤出成型:将步骤3)得到的改性白石墨烯聚乙烯母粒再经管材挤出机挤出成型,得到改性白石墨烯复合聚乙烯管材成品。
7.根据权利要求6所述的改性白石墨烯复合聚乙烯管材的制备方法,其特征在于,步骤3)所述母粒的制备,双螺杆挤出机各区温度为140-220℃,机头温度为150-230℃。
8.根据权利要求6所述的改性白石墨烯复合聚乙烯管材的制备方法,其特征在于,步骤4)所述管材挤出机挤出成型温度为140-230℃。
9.根据权利要求6所述的改性白石墨烯复合聚乙烯管材的制备方法,其特征在于,步骤2)所述高速混合机混合时间为1-20min。
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