CN116376134A - 一种耐油耐溶剂性的食品包装膜和制备方法 - Google Patents
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Abstract
本发明涉及包装膜技术领域，且公开了一种耐油耐溶剂性的食品包装膜和制备方法，以过氧化二异丙苯或过氧化二苯甲酰的引发下，以三烯丙基异氰脲酸酯作为交联剂，使聚乙烯、三烯丙基异氰脲酸酯，以及石墨烯表面修饰的烯丙基异氰脲酸酯结构发生熔融共交联，得到石墨烯交联聚乙烯食品包装膜。石墨烯纳米粒子在聚乙烯基体中形成化学交联，提高聚乙烯食品包装膜的阻隔性能。降低聚乙烯在有机溶剂中的溶胀度和溶解性，提高食品包装膜的耐油耐溶剂性。石墨烯纳米粒子化学键合在聚乙烯基体中，改善了石墨烯的分散性，使石墨烯对聚乙烯由更好的增强效果，提高了食品包装膜的拉伸性能和弹性模量等力学性能。
Description
技术领域
本发明涉及包装膜技术领域，具体为一种耐油耐溶剂性的食品包装膜和制备方法。
背景技术
聚乙烯具有无臭无毒、电绝缘性好等优点，在食品保鲜膜、包装膜等方面有着广泛的应用，提高聚乙烯膜材料阻隔性、力学强度、耐溶剂性等综合性能，有利于拓展聚乙烯膜在食品保鲜膜、包装膜等方面实际应用，石墨烯是一种性能优良的纳米材料，广泛应用在聚乙烯等高分子材料的改性中，如文献《石墨烯/低密度聚乙烯复合包装膜中2种抗氧化剂向食品模拟物异辛烷的迁移》，报道了石墨烯及石墨烯微片纳米粒子的吸附作用抑制了食品包装中的两种抗氧化剂向食品模拟物异辛烷中的迁移，避免食品添加剂扩散迁移到食品中而造成食品安全问题。对石墨烯进行功能化和表面修饰，可以使石墨烯更好地应用在聚乙烯等材料中，如文献《功能化石墨烯/聚乙烯复合材料薄膜的制备及表征》，报道了采用异佛尔酮二异氰酸酯对氧化石墨烯进行改性，再利用水合肼进行还原，得到的功能化石墨烯降低了聚乙烯材料的体积电阻率，提高了材料的抗静电性能。本发明旨在对氧化石墨烯表面功能化处理，对聚乙烯交联改性，提高聚乙烯食品包装膜的力学性能、阻隔性和耐溶剂性。
发明内容
(一)解决的技术问题
本发明提供了一种高强度高阻隔性的耐油耐溶剂性的食品包装膜和制备方法。
(二)技术方案
一种耐油耐溶剂性的食品包装膜，包括以下质量占比的原料组成：95.7-98.2％聚乙烯树脂、0.2-1％烯丙基异氰脲酸酯改性石墨烯、1-2％三烯丙基异氰脲酸酯、0.4-0.7％引发剂、0.2-0.6％抗氧剂。
优选的，所述引发剂为过氧化二苯甲酰或过氧化二异丙苯中的任一种。
优选的，所述耐油耐溶剂性的食品包装膜的制备方法，其特征在于：所述制备方法为：将聚乙烯树脂、烯丙基异氰脲酸酯改性石墨烯、三烯丙基异氰脲酸酯、引发剂、抗氧剂加入到双辊开炼机中，混炼温度160-180℃，时间10-20min；然后将物料在平板硫化机中进行模压，模压温度170-190℃，压力7-12MPa，时间8-15min，得到耐油耐溶剂性的食品包装膜。
优选的，所述烯丙基异氰脲酸酯改性石墨烯制备方法为：
(1)将氧化石墨烯加入到氯化亚砜中，加热回流进行酰氯化；得到的酰氯化石墨烯分散到反应溶剂中，在冰浴下加入二硫赤藓醇和三乙胺，搅拌溶解后升温至20-35℃反应24-48h，反应后离心分离，乙醇洗涤，得到多巯基石墨烯。
(2)将多巯基石墨烯分散到反应溶剂中，然后加入三烯丙基异氰脲酸酯和安息香二甲醚，搅拌溶解后在紫外灯下照射反应1-2h，离心分离，去离子水和乙醇洗涤，得到烯丙基异氰脲酸酯改性石墨烯。
优选的，所述(1)中反应溶剂包括四氢呋喃、二氯甲烷、三氯甲烷、丙酮、乙酸乙酯中的一种。
优选的，所述(1)中酰氯化石墨烯、二硫赤藓醇和三乙胺的质量比例为1:6-20:4-15。
优选的，所述(2)中反应溶剂包括丙酮、四氢呋喃、N,N-二甲基甲酰胺或N,N-二甲基乙酰胺中的一种。
优选的，所述(2)中多巯基石墨烯分散、三烯丙基异氰脲酸酯和安息香二甲醚的质量比例为1:2-7:0.02-0.08。
(三)有益的技术效果
利用二硫赤藓醇的羟基与酰氯化石墨烯发生酯化反应，在石墨烯表面修饰丰富的巯基，引入的巯基再与三烯丙基异氰脲酸酯的一个烯基发生巯基烯点击反应，得到烯丙基异氰脲酸酯改性石墨烯，从而在石墨烯表面修饰了大量的烯丙基异氰脲酸酯结构。
以过氧化二异丙苯或过氧化二苯甲酰的引发下，以三烯丙基异氰脲酸酯作为交联剂，使聚乙烯、三烯丙基异氰脲酸酯，以及石墨烯表面修饰的烯丙基异氰脲酸酯结构发生熔融共交联，得到石墨烯交联聚乙烯食品包装膜。石墨烯纳米粒子在聚乙烯基体中形成化学交联，均匀的分散在聚乙烯基体中，片层结构的石墨烯可以阻碍氧气气体分子和水蒸气的透过率，提高聚乙烯食品包装膜的阻隔性能。石墨烯化学交联聚乙烯后可以降低聚乙烯在有机溶剂中的溶胀度和溶解性，提高食品包装膜的耐油耐溶剂性。石墨烯纳米粒子化学键合在聚乙烯基体中，提高了石墨烯与聚乙烯的界面结合力，改善了石墨烯的分散性，使石墨烯对聚乙烯由更好的增强效果，提高了食品包装膜的拉伸性能和弹性模量等力学性能。得到综合性能优良的聚乙烯食品包装膜。
具体实施方式
实施例1
(1)将0.2g的氧化石墨烯加入到10mL的氯化亚砜中，加热回流进行酰氯化；得到的酰氯化石墨烯称取0.2g分散到30mL的四氢呋喃中，在冰浴下加入2.8g的二硫赤藓醇和2g的三乙胺，搅拌溶解后升温至20-35℃反应48h，反应后离心分离，乙醇洗涤，得到多巯基石墨烯。
(2)将0.2g的多巯基石墨烯分散到四氢呋喃中，然后加入1.4g的三烯丙基异氰脲酸酯和16mg的安息香二甲醚，搅拌溶解后在紫外灯下照射反应1h，离心分离，去离子水和乙醇洗涤，得到烯丙基异氰脲酸酯改性石墨烯。
(3)将质量占比为97.9％的聚乙烯树脂、0.2％的烯丙基异氰脲酸酯改性石墨烯、1％的三烯丙基异氰脲酸酯、0.5％的引发剂过氧化二异丙苯、0.4％的抗氧剂1010加入到双辊开炼机中，混炼温度180℃，时间10min；然后将物料在平板硫化机中进行模压，模压温度180℃，压力12MPa，时间10min，得到耐油耐溶剂性的食品包装膜。
实施例2
(1)将0.2g的酰氯化石墨烯分散到20mL的乙酸乙酯中，在冰浴下加入1.2g的二硫赤藓醇和0.8g的三乙胺，搅拌溶解后升温至25℃反应24-48h，反应后离心分离，乙醇洗涤，得到多巯基石墨烯。
(2)将0.2g的多巯基石墨烯分散到N,N-二甲基甲酰胺中，然后加入0.4g的三烯丙基异氰脲酸酯和4mg的安息香二甲醚，搅拌溶解后在紫外灯下照射反应2h，离心分离，去离子水和乙醇洗涤，得到烯丙基异氰脲酸酯改性石墨烯。
(3)将质量占比为97.1％的聚乙烯树脂、0.5％的烯丙基异氰脲酸酯改性石墨烯、1.5％的三烯丙基异氰脲酸酯、0.7％的引发剂过氧化二苯甲酰、0.2％的抗氧剂1076加入到双辊开炼机中，混炼温度180℃，时间15min；然后将物料在平板硫化机中进行模压，模压温度190℃，压力7MPa，时间8-15min，得到耐油耐溶剂性的食品包装膜。
实施例3
(1)将0.2g的酰氯化石墨烯分散到40mL的二氯甲烷中，在冰浴下加入4g的二硫赤藓醇和3g的三乙胺，搅拌溶解后升温至25℃反应36h，反应后离心分离，乙醇洗涤，得到多巯基石墨烯。
(2)将0.2g的多巯基石墨烯分散到丙酮中，然后加入1.4g的三烯丙基异氰脲酸酯和16mg的安息香二甲醚，搅拌溶解后在紫外灯下照射反应2h，离心分离，去离子水和乙醇洗涤，得到烯丙基异氰脲酸酯改性石墨烯。
(3)将质量占比为96.6％的聚乙烯树脂、0.8％的烯丙基异氰脲酸酯改性石墨烯、1.5％的三烯丙基异氰脲酸酯、0.7％的引发剂过氧化二苯甲酰、0.6％的抗氧剂1076加入到双辊开炼机中，混炼温度170℃，时间10min；然后将物料在平板硫化机中进行模压，模压温度180℃，压力12MPa，时间15min，得到耐油耐溶剂性的食品包装膜。
实施例4
(1)将0.2g的酰氯化石墨烯分散到20-40mL的丙酮中，在冰浴下加入1.2-4g的二硫赤藓醇和0.8-3g的三乙胺，搅拌溶解后升温至35℃反应24-48h，反应后离心分离，乙醇洗涤，得到多巯基石墨烯。
(2)将0.2g的多巯基石墨烯分散到丙酮中，然后加入0.8g的三烯丙基异氰脲酸酯和10mg的安息香二甲醚，搅拌溶解后在紫外灯下照射反应2h，离心分离，去离子水和乙醇洗涤，得到烯丙基异氰脲酸酯改性石墨烯。
(3)将质量占比为95.9％的聚乙烯树脂、1％的烯丙基异氰脲酸酯改性石墨烯、2％的三烯丙基异氰脲酸酯、0.7％的引发剂过氧化二苯甲酰、0.4％的抗氧剂1010加入到双辊开炼机中，混炼温度160℃，时间20min；然后将物料在平板硫化机中进行模压，模压温度190℃，压力10MPa，时间15min，得到耐油耐溶剂性的食品包装膜。
对比例1
(1)将0.2g的酰氯化石墨烯分散到20mL的四氢呋喃中，在冰浴下加入2.5g的二硫赤藓醇和1.5g的三乙胺，搅拌溶解后升温至35℃反应24-48h，反应后离心分离，乙醇洗涤，得到多巯基石墨烯。
(2)将质量占比为97.6％的聚乙烯树脂、0.2％的多巯基石墨烯、1％的三烯丙基异氰脲酸酯、0.6％的引发剂过氧化二异丙苯、0.6％的抗氧剂1010加入到双辊开炼机中，混炼温度180℃，时间15min；然后将物料在平板硫化机中进行模压，模压温度190℃，压力10MPa，时间10min，得到食品包装膜。
对比例2
(1)将质量占比为97.4％的聚乙烯树脂、0.2％的氧化石墨烯、1.5％的三烯丙基异氰脲酸酯、0.4％的引发剂过氧化二异丙苯、0.5％的抗氧剂1010加入到双辊开炼机中，混炼温度180℃，时间10min；然后将物料在平板硫化机中进行模压，模压温度190℃，压力10MPa，时间8min，得到食品包装膜。
参考ASTMF1249-90的方法，采用水蒸气透过率测试仪测定食品包装膜的水蒸气透过系数。参考GB/T 19789-2005的方法，采用氧气透过仪测定食品包装膜的氧气透过率。
参考准GB/T 1040.1-2006的方法，采用拉力试验机测定食品包装膜的拉伸性能。拉伸速率100mm/min，试样为长120mm，宽50，高4mm的样条。
称取0.500g的食品包装膜分别加入到N,N-二甲基甲酰胺、二甲亚砜、N-甲基吡咯烷酮溶剂中，浸泡24h后取出食品包装膜，观察溶胀溶解情况。
经过烯丙基异氰脲酸酯改性石墨烯交联后，聚乙烯食品包装膜在N,N-二甲基甲酰胺、二甲亚砜、N-甲基吡咯烷酮中均不发生溶胀和溶解的情况。
Claims (8)
1.一种耐油耐溶剂性的食品包装膜，其特征在于：所述食品包装膜包括以下质量占比的原料组成：95.7-98.2％聚乙烯树脂、0.2-1％烯丙基异氰脲酸酯改性石墨烯、1-2％三烯丙基异氰脲酸酯、0.4-0.7％引发剂、0.2-0.6％抗氧剂。
2.根据权利要求1所述的耐油耐溶剂性的食品包装膜，其特征在于：所述引发剂为过氧化二苯甲酰或过氧化二异丙苯中的任一种。
3.一种如权利要求1或2所述的耐油耐溶剂性的食品包装膜的制备方法，其特征在于：所述制备方法为：将聚乙烯树脂、烯丙基异氰脲酸酯改性石墨烯、三烯丙基异氰脲酸酯、引发剂、抗氧剂加入到双辊开炼机中，混炼温度160-180℃，时间10-20min；然后将物料在平板硫化机中进行模压，模压温度170-190℃，压力7-12MPa，时间8-15min，得到耐油耐溶剂性的食品包装膜。
4.根据权利要求3所述的耐油耐溶剂性的食品包装膜的制备方法，其特征在于：所述烯丙基异氰脲酸酯改性石墨烯制备方法为：
(1)将氧化石墨烯加入到氯化亚砜中，加热回流进行酰氯化；得到的酰氯化石墨烯分散到反应溶剂中，在冰浴下加入二硫赤藓醇和三乙胺，搅拌溶解后升温至20-35℃反应24-48h，反应后离心分离、洗涤，得到多巯基石墨烯；
(2)将多巯基石墨烯分散到反应溶剂中，然后加入三烯丙基异氰脲酸酯和安息香二甲醚，搅拌溶解后在紫外灯下照射反应1-2h，离心分离、洗涤，得到烯丙基异氰脲酸酯改性石墨烯。
5.根据权利要求4所述的耐油耐溶剂性的食品包装膜的制备方法，其特征在于：所述(1)中反应溶剂包括四氢呋喃、二氯甲烷、三氯甲烷、丙酮、乙酸乙酯中的一种。
6.根据权利要求4所述的耐油耐溶剂性的食品包装膜的制备方法，其特征在于：所述(1)中酰氯化石墨烯、二硫赤藓醇和三乙胺的质量比例为1:6-20:4-15。
7.根据权利要求4所述的耐油耐溶剂性的食品包装膜的制备方法，其特征在于：所述(2)中反应溶剂包括丙酮、四氢呋喃、N,N-二甲基甲酰胺或N,N-二甲基乙酰胺中的一种。
8.根据权利要求4所述的耐油耐溶剂性的食品包装膜的制备方法，其特征在于：所述(2)中多巯基石墨烯分散、三烯丙基异氰脲酸酯和安息香二甲醚的质量比例为1:2-7:0.02-0.08。
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