CN108556426A - 一种无机纳米片/塑料叠层阻隔薄膜的制备方法 - Google Patents

一种无机纳米片/塑料叠层阻隔薄膜的制备方法 Download PDF

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CN108556426A
CN108556426A CN201710265526.6A CN201710265526A CN108556426A CN 108556426 A CN108556426 A CN 108556426A CN 201710265526 A CN201710265526 A CN 201710265526A CN 108556426 A CN108556426 A CN 108556426A
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Abstract

本发明提供一种无机纳米片/塑料叠层阻隔薄膜的制备方法。所述的无机纳米片/塑料叠层阻隔薄膜是以无机纳米片和塑料为原料,先将无机纳米片在水表面形成一层均匀透明的超薄膜,再将无机纳米片超薄膜转移到塑料膜表面,然后将多个覆盖有无机纳米片超薄膜的塑料膜堆叠并加热或加压成为一体。本发明的突出特点是利用在水表面形成的无机纳米片超薄膜构筑无机纳米片/塑料叠层阻隔薄膜,其中每个无机纳米片超薄膜有效阻隔气体透过,多个无机纳米片超薄膜共同作用产生高阻隔性能。本发明制备工艺简单,所制备的无机纳米片/塑料叠层阻隔薄膜可用于医疗器具、食品等产品的密封包装。

Description

一种无机纳米片/塑料叠层阻隔薄膜的制备方法
技术领域
本发明涉及纳米材料科学与技术领域,特别涉及无机纳米片/塑料阻隔薄膜的制备。
背景技术
随着包装行业的发展,人们对包装材料的要求也在逐渐的提高。包装材料需要对气体具有高阻隔能力,还需要有较高的力学性能、优良的化学稳定性和热稳定性,以满足内容物的高温消毒和低温储藏要求。由于容易加工成型和价格便宜,塑料被广泛用于各种包装材料;但塑料由于分子间作用力较小,对气体或其他小分子的阻隔性能较差,尤其当包装物为食品、药品等对氧气和水蒸气十分敏感的物质,普通塑料包装材料往往会出现产品变质、产品保质期较短的问题。目前,提高塑料阻隔性能的方法主要有:1)在塑料表面真空蒸镀金属氧化物,2)不同塑料通过多层共挤复合形成多层结构,3)通过熔融共混或者溶液共混的方式在塑料中添加粘土、氧化石墨烯、石墨烯等无机纳米片。其中,真空蒸镀金属氧化物成本高昂;多层共挤复合薄膜的阻隔性能仍然难以满足许多应用要求;通过溶液共混或者熔融共混填充无机纳米颗粒,无机纳米颗粒在薄膜内部往往难以均匀分散,而且取向难以控制,呈无归律分布状态,使得塑料膜阻隔性能提高幅度有限。
随着纳米科技的不断进步,许多二维无机纳米片相继开发出来,这些二维无机纳米片具有大的长径比、完美的晶体结构,能够阻挡氧气、水蒸气等气体透过。因此,二维无机纳米片可以作为塑料阻隔薄膜的填充剂,以提高塑料的气体阻隔能力。当二维无机纳米片均匀分散在塑料基体中时,由于气体分子不能扩散透过二维无机纳米片,只能绕着无机纳米片扩散,延长了气体的扩散路程,降低了聚合物的透气性。为了最大化气体的扩散路径,需要将均匀分布的无机纳米片沿着薄膜平面方面取向,因此,发展新技术控制无机纳米片的分散和取向在提高塑料薄膜阻隔性能方面具有重要意义。
发明内容
针对上述技术问题,本发明的目的在于提出一种无机纳米片/塑料叠层阻隔薄膜的制备方法,步骤包括:
(1)将无机纳米片分散在能与水互溶的有机溶剂中,形成均匀分散液;
(2)将均匀的无机纳米片分散液沿容器壁缓慢注射到盛水容器中,无机纳米片在水表面形成一层均匀透明的超薄膜;
(3)将热塑性塑料膜导入水中并导出,使得水表面的无机纳米片超薄膜转移覆盖到塑料膜表面;
(4)将多个覆盖有无机纳米片超薄膜的塑料膜堆叠并加热或者加压成为一体,形成无机纳米片/塑料叠层阻隔薄膜。
所述的无机纳米片包括石墨烯、二硫化钼(MoS2)、氮化硼(BN)、硫化钨(WS2)、硒化钼(MoSe2)、碲化钼(MoTe2)、硒化钽(TaSe2)、硒化铌(NbSe)、碲化镍(NiTe2)、碲化铋(Bi2Te3)、二硒化钨(WSe2)、二碲化钨(WTe2)、硫化镓(GaS)、硫化铪(HfSe2)、硒化铟(In2Se3)、硫锡铅(PbSnS2)、硒化铂(PtSe2)、硫化铼(ReS2)、硫化锡(SnS2)、硒化锡(SnSe2)、硫化钽(TaS2)、硫化钛(TiS2)、硒化钛(TiSe2)或硒化钒(VSe2)、粘土、云母中的一种或者几种。
所述的无机纳米片分散在能与水互溶的有机溶剂中,所述有机溶剂包括但不限于N-甲基吡咯烷酮、N,N二甲基甲酰胺、N,N-二甲基乙酰胺、N-乙烯基吡咯烷酮、甲醇、乙醇、异丙醇、丙酮、二甲基亚砜中的一种或者几种。
所述的塑料膜的材料为热塑性聚合物,包括但不限于聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、聚偏二氯乙烯、聚酰胺、聚酯、聚乙烯醇、乙烯-乙烯醇共聚物或聚氨酯中的一种或几种。
步骤(3)中所述的亲水处理包括等离子体处理、紫外臭氧清洗处理。
步骤(1)中均匀分散液的浓度为0.001-2mg/ml,优选为0.1-1mg/ml。
所述纳米叠层阻隔薄膜中无机纳米片的重量百分含量不超过10%。
该方法能够将二维纳米片和塑料均匀有序的整合成有机-无机纳米复合薄膜,获得的纳米复合薄膜内部具有叠层结构,无机纳米片超薄膜在水表面形成,叠层结构中每个无机纳米片层的厚度为0.34~10纳米,该方法解决了无机纳米片在聚合物复合材料中分散难的问题,还解决了无机纳米片的取向难的问题,该方法制备工艺简单易行,阻隔性能和力学性能有了较大提高,所制备的纳米杂化叠层复合薄膜适合医疗器具、食品等密封产品的包装。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整的描述。显然,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作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
(1)将石墨烯分散在N-甲基吡咯烷酮中,形成浓度为0.1mg/ml的均匀分散液;
(2)将石墨烯/N-甲基吡咯烷酮分散液用注射泵以10ml/h的速度沿容器壁注射到盛水容器中,在水表面形成一层均匀透明的石墨烯超薄膜;
(3)用传送装置将等离子体处理的聚酰胺薄膜导入步骤2中的盛水容器中并导出,石墨烯超薄膜覆盖在导出的聚酰胺薄膜表面;
(4)将多个覆盖有石墨烯超薄膜的聚酰胺薄膜堆叠,并热压在一起,得到石墨烯/聚酰胺纳米叠层阻隔薄膜。
实施例2
(1)将二硫化钼分散在N-乙烯基吡咯烷酮中,形成浓度为0.2mg/ml的均匀分散液;
(2)将二硫化钼/N-乙烯基吡咯烷酮分散液用注射泵以5ml/h的速度沿容器壁注射到盛水容器中,在水表面形成一层均匀透明的二硫化钼超薄膜;
(3)用传送装置将紫外臭氧清洗处理的聚乙烯薄膜导入步骤2中的盛水容器中并导出,二硫化钼超薄膜覆盖在导出的聚乙烯薄膜表面;
(4)将多个覆盖有二硫化钼超薄膜的聚乙烯薄膜堆叠,并压延在一起,得到二硫化钼/聚乙烯纳米叠层阻隔薄膜。
实施例3
(1)将二硫化钨分散在二甲基亚砜中,形成浓度为0.2mg/ml的均匀分散液;
(2)将二硫化钨/二甲基亚砜分散液用注射泵以5ml/h的速度沿容器壁注射到盛水容器中,在水表面形成一层均匀透明的二硫化钨超薄膜;
(3)用传送装置将等离子体处理的聚氯乙烯薄膜导入步骤2中的盛水容器中并导出,二硫化钨超薄膜覆盖在导出的聚氯乙烯薄膜表面;
(4)将多个覆盖有二硫化钨超薄膜的聚氯乙烯薄膜堆叠,并热压在一起,得到二硫化钨/聚氯乙烯纳米叠层阻隔薄膜。
实施例4
(1)将氮化硼分散在N,N-二甲基乙酰胺中,形成浓度为0.1mg/ml的均匀分散液;
(2)将氮化硼/N,N-二甲基乙酰胺分散液用注射泵以10ml/h的速度沿容器壁注射到盛水容器中,在水表面形成一层均匀透明的氮化硼超薄膜;
(3)用传送装置将等离子体处理的聚酰胺薄膜导入步骤2中的盛水容器中并导出,氮化硼超薄膜覆盖在导出的聚酰胺薄膜表面;
(4)将多个覆盖有氮化硼超薄膜的聚酰胺薄膜堆叠,并热压在一起,得到氮化硼/聚酰胺纳米叠层阻隔薄膜。
实施例5
(1)将氮化硼和二硫化钼分散在N,N-二甲基乙酰胺中,形成浓度为0.2mg/ml的均匀分散液;
(2)将氮化硼和二硫化钼/N,N-二甲基乙酰胺分散液用注射泵以5ml/h的速度沿容器壁注射到盛水容器中,在水表面形成一层均匀透明的氮化硼和二硫化钼超薄膜;
(3)用传送装置将等离子体处理的聚酰胺薄膜导入步骤2中的盛水容器中并导出,氮化硼和二硫化钼超薄膜覆盖在导出的聚酰胺薄膜表面;
(4)将多个覆盖有氮化硼和二硫化钼超薄膜的聚酰胺薄膜堆叠,并热压在一起,得到氮化硼和二硫化钼/聚酰胺纳米叠层阻隔薄膜。
实施例6
(1)将石墨烯分散在异丙醇中,形成浓度为0.1mg/ml的均匀分散液;
(2)将石墨烯/异丙醇分散液用注射泵以10ml/h的速度沿容器壁注射到盛水容器中,在水表面形成一层均匀透明的石墨烯超薄膜;
(3)用传送装置将等离子体处理的聚氨酯薄膜导入步骤2中的盛水容器中并导出,石墨烯超薄膜覆盖在导出的聚氨酯薄膜表面;
(4)将多个覆盖有石墨烯超薄膜的聚氨酯薄膜堆叠,并热压在一起,得到石墨烯/聚氨酯纳米叠层阻隔薄膜。
实施例7
(1)将二硫化钛分散在N-甲基吡咯烷酮中,形成浓度为0.3mg/ml的均匀分散液;
(2)将二硫化钛/N-甲基吡咯烷酮分散液用注射泵以10ml/h的速度沿容器壁注射到盛水容器中,在水表面形成一层均匀透明的二硫化钛超薄膜;
(3)用传送装置将等离子体处理的聚酰胺薄膜导入步骤2中的盛水容器中并导出,二硫化钛超薄膜覆盖在导出的聚酰胺薄膜表面;
(4)将多个覆盖有二硫化钛超薄膜的聚酰胺薄膜堆叠,并热压在一起,得到二硫化钛/聚酰胺纳米叠层阻隔薄膜。
实施例8
(1)将二硫锡铅分散在N-甲基吡咯烷酮中,形成浓度为0.5mg/ml的均匀分散液;
(2)将二硫锡铅/N-甲基吡咯烷酮分散液用注射泵以5ml/h的速度沿容器壁注射到盛水容器中,在水表面形成一层均匀透明的二硫锡铅超薄膜;
(3)用传送装置将等离子体处理的聚酰胺薄膜导入步骤2中的盛水容器中并导出,二硫锡铅超薄膜覆盖在导出的聚酰胺薄膜表面;
(4)将多个覆盖有二硫锡铅超薄膜的聚酰胺薄膜堆叠,并热压在一起,得到二硫锡铅/聚酰胺纳米叠层阻隔薄膜。
实施例9
(1)将石墨烯分散在N,N二甲基甲酰胺中,形成浓度为0.3mg/ml的均匀分散液;
(2)将石墨烯/N,N二甲基甲酰胺分散液用注射泵以10ml/h的速度沿容器壁注射到盛水容器中,在水表面形成一层均匀透明的石墨烯超薄膜;
(3)用传送装置将等离子体处理的聚酯薄膜导入步骤2中的盛水容器中并导出,石墨烯超薄膜覆盖在导出的聚酯薄膜表面;
(4)将多个覆盖有石墨烯超薄膜的聚酯薄膜堆叠,并热压在一起,得到石墨烯/聚酯纳米叠层阻隔薄膜。

Claims (9)

1.一种无机纳米片/塑料纳米叠层阻隔薄膜的制备方法,其特征在于:所述纳米叠层阻隔薄膜由在水表面形成的无机纳米片超薄膜和塑料膜交替堆叠而成;具体制备步骤如下:
(1)将无机纳米片分散在能与水互溶的有机溶剂中,形成均匀分散液;
(2)将均匀的无机纳米片分散液沿容器壁缓慢注射到盛水容器中,无机纳米片在水表面形成一层均匀透明的超薄膜;
(3)将亲水处理的塑料膜导入水中并导出,使得水表面的无机纳米片超薄膜转移覆盖到塑料膜表面;
(4)将多个覆盖有无机纳米片超薄膜的塑料膜堆叠并加热或者加压成为一体,形成无机纳米片/塑料叠层阻隔薄膜。
2.根据权利要求1所述的纳米叠层阻隔薄膜的制备方法,其特征在于所述的无机纳米片包括石墨烯、二硫化钼(MoS2)、氮化硼(BN)、硫化钨(WS2)、硒化钼(MoSe2)、碲化钼(MoTe2)、硒化钽(TaSe2)、硒化铌(NbSe)、碲化镍(NiTe2)、碲化铋(Bi2Te3)、二硒化钨(WSe2)、二碲化钨(WTe2)、硫化镓(GaS)、硫化铪(HfSe2)、硒化铟(In2Se3)、硫锡铅(PbSnS2)、硒化铂(PtSe2)、硫化铼(ReS2)、硫化锡(SnS2)、硒化锡(SnSe2)、硫化钽(TaS2)、硫化钛(TiS2)、硒化钛(TiSe2)或硒化钒(VSe2)、粘土、云母中的一种或者几种。
3.根据权利要求1所述的纳米叠层阻隔薄膜的制备方法,其特征在于所述的无机纳米片分散在能与水互溶的有机溶剂中,所述有机溶剂包括N-甲基吡咯烷酮、N,N二甲基甲酰胺、N,N-二甲基乙酰胺、N-乙烯基吡咯烷酮、甲醇、乙醇、异丙醇、丙酮、二甲基亚砜中的一种或者几种。
4.根据权利要求1所述的纳米叠层阻隔薄膜的制备方法,其特征在于所述的无机纳米片超薄膜在水表面形成,厚度在0.34~10纳米。
5.根据权利要求1所述的纳米叠层阻隔薄膜的制备方法,其特征在于所述的塑料膜的材料为热塑性聚合物,包括但不限于聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、聚偏二氯乙烯、聚酰胺、聚酯、聚乙烯醇、乙烯-乙烯醇共聚物或聚氨酯。
6.根据权利要求1所述的纳米叠层阻隔薄膜的制备方法,其特征在于步骤(3)中所述的亲水处理包括等离子体处理、紫外臭氧清洗处理。。
7.根据权利要求1所述的纳米叠层阻隔薄膜的制备方法,其特征在于步骤(1)中均匀分散液的浓度为0.001-2mg/ml,优选为0.1-1mg/ml。
8.根据权利要求1所述的纳米叠层阻隔薄膜的制备方法,其特征在于所述纳米叠层阻隔薄膜中无机纳米片的重量百分含量不超过10%。
9.权利要求1-8任一项所述的方法制备的纳米叠层阻隔薄膜的用途,用于密封产品的包装。
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