CN111976242A - 一种抗介质高阻隔共挤膜及其制备方法 - Google Patents
一种抗介质高阻隔共挤膜及其制备方法 Download PDFInfo
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- CN111976242A CN111976242A CN202010852610.XA CN202010852610A CN111976242A CN 111976242 A CN111976242 A CN 111976242A CN 202010852610 A CN202010852610 A CN 202010852610A CN 111976242 A CN111976242 A CN 111976242A
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Abstract
本申请公开了一种抗介质高阻隔共挤膜,由基材层、抗介质层、增韧层、粘合层、内层共挤得到的复合薄膜;所述外层为包装时与外界接触,所述抗介质层按照重量组份计包括:酚醛树脂30‑40份、环氧树脂15‑23份、环氧丙烯酸酯10‑13份、过氧化二异丙苯4‑6份、十八烷基胺纳米蒙脱土5‑8份、纳米二氧化钛3‑4份、纳米氧化锌2‑3份、抗介质助剂1‑3份、双氰胺4‑6份、1‑羟基环己基苯乙酮8‑10份、油酰胺1‑2份、羟基乙叉二膦酸5‑7份、甲醇溶剂13‑25份。本发明还提出一种抗介质高阻隔共挤膜的制备方法。本发明的阻隔共挤膜具有优异的抗介质性能。
Description
技术领域
本发明属于阻隔膜材料制备技术领域,具体涉及一种抗介质高阻隔共挤膜及其制备方法。
背景技术
高阻隔薄膜是把气体阻隔性很强的材料与热缝合性、水分阻隔性很强的聚烯烃同时进行挤出而成,是多层结构的薄膜。因为对水蒸气和氧气具有优异的阻隔性能,从而多被用于药品、食品、化妆品等包装领域以及用于制备真空绝热板。
早期技术中的阻隔薄膜,其结构从外至内依次是:PET膜(聚对苯二甲酸乙二醇酯膜)、铝箔和PE膜(聚乙烯膜),其中,位于外层的PET膜具有良好的耐磨和耐候性能,位于中间层的铝箔具有较好的阻气性能,位于内层的PE膜熔点较低,适于对其进行熔融热封从而实现对真空绝热板的真空封装。但是,这种阻隔薄膜的缺点在于,由于用作中间层的铝箔具有较大的热导率,因此该阻隔薄膜内部的横向热损较大。
作为应用最多的高阻隔性材料EVOH,这种材料的薄膜类型除了非拉伸型外,还有双向拉伸型、铝蒸镀型、黏合剂涂覆型等,双向拉伸型中还有耐热型的用于无菌包装制品。EVOH的阻隔性能取决于乙烯的含量,一般来说当乙烯含量增加时候,气体阻隔性下降,但易于加工。EVOH显著特点是对气体具有极好的阻隔性和极好加工性,另外透明性、光泽性、机械强度、伸缩性、耐磨性、耐寒性和表面强度都非常优异。
而现有技术中的高阻隔膜,耐腐蚀性差,抗介质能力弱,韧性也无法满足实际使用时的需求,故此亟需开发一种抗介质高阻隔共挤膜来解决现有技术中的问题。
发明内容
本发明的目的是提供一种抗介质高阻隔共挤膜及其制备方法,以提高共挤膜的抗介质性能。
为了解决以上技术问题,本发明采用以下技术方案:
一种抗介质高阻隔共挤膜,由基材层、抗介质层、增韧层、粘合层、内层共挤得到的复合薄膜;所述外层为包装时与外界接触,所述抗介质层按照重量组份计包括:酚醛树脂30-40份、环氧树脂15-23份、环氧丙烯酸酯10-13份、过氧化二异丙苯4-6份、十八烷基胺纳米蒙脱土5-8份、纳米二氧化钛3-4份、纳米氧化锌2-3份、抗介质助剂1-3份、双氰胺4-6份、1-羟基环己基苯乙酮8-10份、油酰胺1-2份、羟基乙叉二膦酸5-7份、甲醇溶剂13-25份;
所述基材层为聚酰胺树脂和抗紫外助剂按重量比80:15制备而成;
所述增韧层按照重量组份计包括:聚丙烯15-20份、聚乙烯9-11份、增韧改性剂4-6份、抗氧化剂1-3份、乙烯基三胺4-6份、芥酸酰胺1-2份、丝素蛋白-聚氨酯水凝胶5-8份;
所述粘合层按照重量组份计包括:酚醛树脂30-40份、氧化淀粉3-5份、马来酸酐1-3份、腰果油10-14份、茶油5-8份、间苯二胺4-6份、乙醇溶剂12-24份。
优选地,所述抗介质助剂由聚氨酯、氧化锌粉和丙酮按重量比60-80:15-25:10-20混合而成。
优选地,所述抗紫外助剂的原料按重量份包括:聚氨酯15-25份、聚苯硫醚6-9份、丙烯酸丁酯4-8份、纳米氧化锌3-6份、纳米二氧化钛1-4份、蒙脱土2-5份、凹凸棒石黏土1-5份、无机硅藻土2-5份、十二烷基苯磺酸钠4-6份、二月桂酸二丁基锡2-5份、聚磷酸铵1-4份、丙烯酰胺3-5份、过硫酸铵1-5份、水8-16份、N,N-亚甲基双丙烯酰胺4-8份、丙三醇二乙酸酯3-6份、硅烷偶联剂KH-550 1-4份。
优选地,所述抗紫外助剂如下工艺进行制备:将聚氨酯、聚苯硫醚和丙烯酸丁酯混合均匀,升温至110-130℃,保温20-40min,接着加入纳米氧化锌、纳米二氧化钛、蒙脱土、凹凸棒石黏土、无机硅藻土、十二烷基苯磺酸钠、二月桂酸二丁基锡、聚磷酸铵、丙烯酰胺、过硫酸铵、水、N,N-亚甲基双丙烯酰胺、丙三醇二乙酸酯和硅烷偶联剂KH-550混合均匀,继续升温至150-190℃,保温20-40min,接着于1500-2500r/min转速搅拌1-3h,接着于80-90℃干燥1-4h,接着粉碎成20-40目的粉末颗粒得到抗紫外助剂。
优选地,所述增韧改性剂的原料按重量份包括:玻璃鳞片15-25份、蒸馏水10-20份、马来酸酐4-8份、过硫酸铵2-5份、苯乙烯1-5份、木质纤维粉4-8份、黄麻纤维3-6份、氧化锌2-8份、多壁碳纳米管4-6份、二氯乙烷2-5份、硅烷偶联剂KH-560 1-5份、过氧化二异丙苯2-6份、羟基硅油4-8份。
优选地,所述增韧改性剂按如下工艺进行制备:在氮气保护下,将玻璃鳞片、蒸馏水和马来酸酐混合均匀,然后升温至80-90℃,保温10-30min,然后加入过硫酸铵混合均匀,搅拌5-15min后加入苯乙烯混合均匀,接着于850-1250r/min转速搅拌50-70min,然后升温至85-95℃,抽提40-50h,接着于真空烘箱中,65-75℃烘至恒重,冷却至室温得到物料a;将木质纤维粉、黄麻纤维、氧化锌、多壁碳纳米管和二氯乙烷混合均匀,超声处理1-3h,接着加入物料a、硅烷偶联剂KH-560、过氧化二异丙苯和羟基硅油混合均匀,于650-850r/min转速搅拌20-40min,接着升温至80-90℃,回流20-30h,冷却至室温得到增韧改性剂。
本发明还提出一种所述的抗介质高阻隔共挤膜的制备方法,包括以下步骤:
S1、制备基材层:将所述聚酰胺树脂以颗粒状加入挤出机中,经过挤出机挤出成型得到基材层;
S2、制备抗介质层:将所述酚醛树脂、环氧树脂、环氧丙烯酸酯和过氧化二异丙苯按照上述组份混合均匀,并在110-120℃恒温下,以150-250转/分钟机械搅拌1-3,之后依次加入所述、1-羟基环己基苯乙酮、油酰胺、羟基乙叉二膦酸和甲醇溶剂,搅拌均匀后加入双氰胺成型30-60min,再利用造粒机进行造粒,挤出机挤出成型,得到抗介质层;
S3、制备增韧层:将所述聚丙烯、聚乙烯、芥酸酰胺、丝素蛋白-聚氨酯水凝胶按照上述组份混合均匀,并在50-60℃恒温下,以60-120转/分钟机械搅拌60-90min,之后依次加入所述增韧改性剂和抗氧化剂,搅拌均匀后加入所述乙烯基三胺固化成型30-60min,再利用造粒机进行造粒,挤出机挤出成型,得到增韧层;
S4、制备粘合层:将所述腰果油和茶油加入到所述乙醇溶剂中,以500-700转/分钟搅拌5-10min,得到油乳液;将所述油乳液加入到所述酚醛树脂和氧化淀粉中,以800-1000转/分钟搅拌10-20min,至完全融合,再依次加入所述马来酸酐和间苯二胺搅拌均匀后,固化30-60min,经造粒机进行造粒,挤出机挤出成型,得到粘合层;
S5、共挤成膜:按照基材层、抗介质层、增韧层、粘合层和内层这种次序进行叠放,得到复合膜,将所述复合膜通过挤出机挤出成型,即得抗介质高阻隔共挤膜。
与现有技术相比,本发明的有益效果是:
防紫外线改性助剂以聚氨酯为基础树脂,纳米氧化锌、纳米二氧化钛、蒙脱土、凹凸棒石黏土和无机硅藻土作为防紫外线补强填料体系,利用了该防紫外线补强填料体系中大量的锌元素以及钛元素,使得太阳光紫外线在照射到阻隔膜时,锌元素以及钛元素对紫外线的吸收作用,大大提高了阻隔膜的抗紫外线性能,延长阻隔膜的使用寿命,进一步提高了阻隔膜的抗紫外线性能,且在硅烷偶联剂KH-550对防紫外线补强填料体系的表面羟基进行接枝改性,实现了防紫外线补强填料体系与基础树脂的结合,得到的防紫外线改性助剂运用到本发明的阻隔膜的制备中,有效提高粉阻隔膜的耐紫外线性能,进一步提高了阻隔膜的抗紫外线性能。
通过在氮气保护下,将玻璃鳞片、蒸馏水和马来酸酐混合均匀,然后升温保温,然后加入过硫酸铵混合均匀,搅拌后加入苯乙烯混合均匀,接着搅拌,然后升温,抽提,接着于真空烘箱中,烘至恒重,冷却至室温得到物料a;将木质纤维粉、黄麻纤维、氧化锌、多壁碳纳米管和二氯乙烷混合均匀,超声处理,接着加入物料a、硅烷偶联剂KH-560、过氧化二异丙苯和羟基硅油混合均匀,搅拌,接着升温,回流,冷却至室温得到,其中以玻璃鳞片作为黏性基料,以马来酸酐为接枝单体,以过硫酸铵、苯乙烯和过氧化二异丙苯为引发剂,以木质纤维粉、黄麻纤维、氧化锌、多壁碳纳米管为增韧补强填料,以羟基硅油为溶剂,以硅烷偶联剂KH-560接枝改性剂,通过将以木质纤维粉、黄麻纤维、氧化锌、多壁碳纳米管进行表面改性,得到改性后的填料与马来酸酐结合,并将得到的韧性增强改性助剂运用到本发明的阻隔膜的制备中,得到的阻隔膜具有优异的韧性。
另外,因酚醛树脂分子链上由大量的酚羟基,由于与苯环的共轭效应,时的酚醛基具有弱酸性,因而与水分子中含有对电子的氧原子产生较强的溶剂化作用,而环氧树脂中的脂羟基与烷基碳原子相连,不存在共轭体系,与水分子的溶剂作用较弱,因此,含有酚醛树脂的涂膜在蒸馏水中吸水率较高,同样在强碱性介质中,由于酚醛树脂中酚羟基的弱酸性,能够与氢氧化钠作用生成酚钠,酚醛树脂的加入改善了涂层的交联结构和交联键,因而使得涂层在纯水和强酸性介质中具有较强的抗介质渗透能力,且在高温碱溶液中的稳定性更好。
再者,添加的十八烷基胺纳米蒙脱土能提高碳碳键的转化率,对酯键的水解有促进作用,使共挤膜耐介质渗透性能变差。
最后,抗介质助剂由聚氨酯、氧化锌粉和丙酮混合而成,可以利用氧化锌粉实现提高涂层的耐腐蚀电化学性能,进而有效提高涂层的抗介质性能。
具体实施方式
为便于更好地理解本发明,通过以下实例加以说明,这些实例属于本发明的保护范围,但不限制本发明的保护范围。
在实施例中,一种抗介质高阻隔共挤膜,其特征在于,由基材层、抗介质层、增韧层、粘合层、内层共挤得到的复合薄膜;所述外层为包装时与外界接触,所述抗介质层按照重量组份计包括:酚醛树脂30-40份、环氧树脂15-23份、环氧丙烯酸酯10-13份、过氧化二异丙苯4-6份、十八烷基胺纳米蒙脱土5-8份、纳米二氧化钛3-4份、纳米氧化锌2-3份、抗介质助剂1-3份、双氰胺4-6份、1-羟基环己基苯乙酮8-10份、油酰胺1-2份、羟基乙叉二膦酸5-7份、甲醇溶剂13-25份;
所述基材层为聚酰胺树脂和抗紫外助剂按重量比80:15制备而成;
所述增韧层按照重量组份计包括:聚丙烯15-20份、聚乙烯9-11份、增韧改性剂4-6份、抗氧化剂1-3份、乙烯基三胺4-6份、芥酸酰胺1-2份、丝素蛋白-聚氨酯水凝胶5-8份;
所述粘合层按照重量组份计包括:酚醛树脂30-40份、氧化淀粉3-5份、马来酸酐1-3份、腰果油10-14份、茶油5-8份、间苯二胺4-6份、乙醇溶剂12-24份。
在本实施例中,所述抗介质助剂由聚氨酯、氧化锌粉和丙酮按重量比60-80:15-25:10-20混合而成。
在本实施例中,所述抗紫外助剂如下工艺进行制备:按重量份将15-25份聚氨酯、6-9份聚苯硫醚和4-8份丙烯酸丁酯混合均匀,升温至110-130℃,保温20-40min,接着加入3-6份纳米氧化锌、1-4份纳米二氧化钛、2-5份蒙脱土、1-5份凹凸棒石黏土、2-5份无机硅藻土、4-6份十二烷基苯磺酸钠、2-5份二月桂酸二丁基锡、1-4份聚磷酸铵、3-5份丙烯酰胺、1-5份过硫酸铵、8-16份水、4-8份N,N-亚甲基双丙烯酰胺、3-6份丙三醇二乙酸酯和1-4份硅烷偶联剂KH-550混合均匀,继续升温至150-190℃,保温20-40min,接着于1500-2500r/min转速搅拌1-3h,接着于80-90℃干燥1-4h,接着粉碎成20-40目的粉末颗粒得到抗紫外助剂。
所述增韧改性剂按如下工艺进行制备:在氮气保护下,按重量份将15-25份玻璃鳞片、10-20份蒸馏水和4-8份马来酸酐混合均匀,然后升温至80-90℃,保温10-30min,然后加入2-5份过硫酸铵混合均匀,搅拌5-15min后加入1-5份苯乙烯混合均匀,接着于850-1250r/min转速搅拌50-70min,然后升温至85-95℃,抽提40-50h,接着于真空烘箱中,65-75℃烘至恒重,冷却至室温得到物料a;将4-8份木质纤维粉、3-6份黄麻纤维、2-8份氧化锌、4-6份多壁碳纳米管和2-5份二氯乙烷混合均匀,超声处理1-3h,接着加入物料a、1-5份硅烷偶联剂KH-560、2-6份过氧化二异丙苯和4-8份羟基硅油混合均匀,于650-850r/min转速搅拌20-40min,接着升温至80-90℃,回流20-30h,冷却至室温得到增韧改性剂。
本发明还提出一种所述的抗介质高阻隔共挤膜的制备方法,包括以下步骤:
S1、制备基材层:将所述聚酰胺树脂以颗粒状加入挤出机中,经过挤出机挤出成型得到基材层;
S2、制备抗介质层:将所述酚醛树脂、环氧树脂、环氧丙烯酸酯和过氧化二异丙苯按照上述组份混合均匀,并在110-120℃恒温下,以150-250转/分钟机械搅拌1-3,之后依次加入所述、1-羟基环己基苯乙酮、油酰胺、羟基乙叉二膦酸和甲醇溶剂,搅拌均匀后加入双氰胺成型30-60min,再利用造粒机进行造粒,挤出机挤出成型,得到抗介质层;
S3、制备增韧层:将所述聚丙烯、聚乙烯、芥酸酰胺、丝素蛋白-聚氨酯水凝胶按照上述组份混合均匀,并在50-60℃恒温下,以60-120转/分钟机械搅拌60-90min,之后依次加入所述增韧改性剂和抗氧化剂,搅拌均匀后加入所述乙烯基三胺固化成型30-60min,再利用造粒机进行造粒,挤出机挤出成型,得到增韧层;
S4、制备粘合层:将所述腰果油和茶油加入到所述乙醇溶剂中,以500-700转/分钟搅拌5-10min,得到油乳液;将所述油乳液加入到所述酚醛树脂和氧化淀粉中,以800-1000转/分钟搅拌10-20min,至完全融合,再依次加入所述马来酸酐和间苯二胺搅拌均匀后,固化30-60min,经造粒机进行造粒,挤出机挤出成型,得到粘合层;
S5、共挤成膜:按照基材层、抗介质层、增韧层、粘合层和内层这种次序进行叠放,得到复合膜,将所述复合膜通过挤出机挤出成型,即得抗介质高阻隔共挤膜。
实施例1
一种抗介质高阻隔共挤膜,其特征在于,由基材层、抗介质层、增韧层、粘合层、内层共挤得到的复合薄膜;所述外层为包装时与外界接触,所述抗介质层按照重量组份计包括:酚醛树脂35份、环氧树脂18份、环氧丙烯酸酯12份、过氧化二异丙苯5份、十八烷基胺纳米蒙脱土6份、纳米二氧化钛3.5份、纳米氧化锌2.5份、抗介质助剂2份、双氰胺5份、1-羟基环己基苯乙酮9份、油酰胺1.5份、羟基乙叉二膦酸6份、甲醇溶剂18份;
所述基材层为聚酰胺树脂和抗紫外助剂按重量比80:15制备而成;
所述增韧层按照重量组份计包括:聚丙烯18份、聚乙烯10份、增韧改性剂5份、抗氧化剂2份、乙烯基三胺5份、芥酸酰胺1.5份、丝素蛋白-聚氨酯水凝胶6.5份;
所述粘合层按照重量组份计包括:酚醛树脂35份、氧化淀粉4份、马来酸酐2份、腰果油12份、茶油6份、间苯二胺5份、乙醇溶剂19份。
在本实施例中,所述抗介质助剂由聚氨酯、氧化锌粉和丙酮按重量比70:18:15混合而成。
在本实施例中,所述抗紫外助剂如下工艺进行制备:按重量份将15份聚氨酯、9份聚苯硫醚和4份丙烯酸丁酯混合均匀,升温至130℃,保温20min,接着加入6份纳米氧化锌、1份纳米二氧化钛、5份蒙脱土、1份凹凸棒石黏土、2份无机硅藻土、6份十二烷基苯磺酸钠、2份二月桂酸二丁基锡、1份聚磷酸铵、5份丙烯酰胺、1份过硫酸铵、16份水、4份N,N-亚甲基双丙烯酰胺、6份丙三醇二乙酸酯和1份硅烷偶联剂KH-550混合均匀,继续升温至150℃,保温40min,接着于1500r/min转速搅拌3h,接着于80℃干燥4h,接着粉碎成20目的粉末颗粒得到抗紫外助剂。
所述增韧改性剂按如下工艺进行制备:在氮气保护下,按重量份将15份玻璃鳞片、20份蒸馏水和4份马来酸酐混合均匀,然后升温至90℃,保温10min,然后加入5份过硫酸铵混合均匀,搅拌15min后加入1份苯乙烯混合均匀,接着于1250r/min转速搅拌50min,然后升温至95℃,抽提40h,接着于真空烘箱中,75℃烘至恒重,冷却至室温得到物料a;将4份木质纤维粉、6份黄麻纤维、2份氧化锌、6份多壁碳纳米管和2份二氯乙烷混合均匀,超声处理3h,接着加入物料a、5份硅烷偶联剂KH-560、2份过氧化二异丙苯和8份羟基硅油混合均匀,于650r/min转速搅拌40min,接着升温至80℃,回流30h,冷却至室温得到增韧改性剂。
本发明还提出一种所述的抗介质高阻隔共挤膜的制备方法,包括以下步骤:
S1、制备基材层:将所述聚酰胺树脂以颗粒状加入挤出机中,经过挤出机挤出成型得到基材层;
S2、制备抗介质层:将所述酚醛树脂、环氧树脂、环氧丙烯酸酯和过氧化二异丙苯按照上述组份混合均匀,并在110℃恒温下,以250转/分钟机械搅拌1,之后依次加入所述、1-羟基环己基苯乙酮、油酰胺、羟基乙叉二膦酸和甲醇溶剂,搅拌均匀后加入双氰胺成型60min,再利用造粒机进行造粒,挤出机挤出成型,得到抗介质层;
S3、制备增韧层:将所述聚丙烯、聚乙烯、芥酸酰胺、丝素蛋白-聚氨酯水凝胶按照上述组份混合均匀,并在50℃恒温下,以120转/分钟机械搅拌60min,之后依次加入所述增韧改性剂和抗氧化剂,搅拌均匀后加入所述乙烯基三胺固化成型60min,再利用造粒机进行造粒,挤出机挤出成型,得到增韧层;
S4、制备粘合层:将所述腰果油和茶油加入到所述乙醇溶剂中,以500转/分钟搅拌10min,得到油乳液;将所述油乳液加入到所述酚醛树脂和氧化淀粉中,以800转/分钟搅拌20min,至完全融合,再依次加入所述马来酸酐和间苯二胺搅拌均匀后,固化30min,经造粒机进行造粒,挤出机挤出成型,得到粘合层;
S5、共挤成膜:按照基材层、抗介质层、增韧层、粘合层和内层这种次序进行叠放,得到复合膜,将所述复合膜通过挤出机挤出成型,即得抗介质高阻隔共挤膜。
实施例2
一种抗介质高阻隔共挤膜,其特征在于,由基材层、抗介质层、增韧层、粘合层、内层共挤得到的复合薄膜;所述外层为包装时与外界接触,所述抗介质层按照重量组份计包括:酚醛树脂30份、环氧树脂23份、环氧丙烯酸酯10份、过氧化二异丙苯6份、十八烷基胺纳米蒙脱土5份、纳米二氧化钛4份、纳米氧化锌2份、抗介质助剂3份、双氰胺4份、1-羟基环己基苯乙酮10份、油酰胺1份、羟基乙叉二膦酸7份、甲醇溶剂13份;
所述基材层为聚酰胺树脂和抗紫外助剂按重量比80:15制备而成;
所述增韧层按照重量组份计包括:聚丙烯15份、聚乙烯11份、增韧改性剂4份、抗氧化剂3份、乙烯基三胺4份、芥酸酰胺2份、丝素蛋白-聚氨酯水凝胶5份;
所述粘合层按照重量组份计包括:酚醛树脂35份、氧化淀粉4份、马来酸酐2份、腰果油12份、茶油6份、间苯二胺5份、乙醇溶剂18份。
在本实施例中,所述抗介质助剂由聚氨酯、氧化锌粉和丙酮按重量比70:20:15混合而成。
在本实施例中,所述抗紫外助剂如下工艺进行制备:按重量份将15份聚氨酯、69份聚苯硫醚和4份丙烯酸丁酯混合均匀,升温至130℃,保温20min,接着加入6份纳米氧化锌、1份纳米二氧化钛、5份蒙脱土、1份凹凸棒石黏土、5份无机硅藻土、4份十二烷基苯磺酸钠、5份二月桂酸二丁基锡、1份聚磷酸铵、5份丙烯酰胺、1份过硫酸铵、16份水、4份N,N-亚甲基双丙烯酰胺、6份丙三醇二乙酸酯和1份硅烷偶联剂KH-550混合均匀,继续升温至190℃,保温20min,接着于2500r/min转速搅拌1h,接着于90℃干燥1h,接着粉碎成40目的粉末颗粒得到抗紫外助剂。
所述增韧改性剂按如下工艺进行制备:在氮气保护下,按重量份将15份玻璃鳞片、20份蒸馏水和4份马来酸酐混合均匀,然后升温至90℃,保温10min,然后加入5份过硫酸铵混合均匀,搅拌5min后加入5份苯乙烯混合均匀,接着于850r/min转速搅拌70min,然后升温至85℃,抽提450h,接着于真空烘箱中,65℃烘至恒重,冷却至室温得到物料a;将8份木质纤维粉、3份黄麻纤维、8份氧化锌、4份多壁碳纳米管和5份二氯乙烷混合均匀,超声处理1h,接着加入物料a、5份硅烷偶联剂KH-560、2份过氧化二异丙苯和8份羟基硅油混合均匀,于650r/min转速搅拌40min,接着升温至80℃,回流30h,冷却至室温得到增韧改性剂。
本发明还提出一种所述的抗介质高阻隔共挤膜的制备方法,包括以下步骤:
S1、制备基材层:将所述聚酰胺树脂以颗粒状加入挤出机中,经过挤出机挤出成型得到基材层;
S2、制备抗介质层:将所述酚醛树脂、环氧树脂、环氧丙烯酸酯和过氧化二异丙苯按照上述组份混合均匀,并在110℃恒温下,以250转/分钟机械搅拌1次,之后依次加入所述、1-羟基环己基苯乙酮、油酰胺、羟基乙叉二膦酸和甲醇溶剂,搅拌均匀后加入双氰胺成型30min,再利用造粒机进行造粒,挤出机挤出成型,得到抗介质层;
S3、制备增韧层:将所述聚丙烯、聚乙烯、芥酸酰胺、丝素蛋白-聚氨酯水凝胶按照上述组份混合均匀,并在60℃恒温下,以60转/分钟机械搅拌90min,之后依次加入所述增韧改性剂和抗氧化剂,搅拌均匀后加入所述乙烯基三胺固化成型30min,再利用造粒机进行造粒,挤出机挤出成型,得到增韧层;
S4、制备粘合层:将所述腰果油和茶油加入到所述乙醇溶剂中,以500转/分钟搅拌10min,得到油乳液;将所述油乳液加入到所述酚醛树脂和氧化淀粉中,以800转/分钟搅拌20min,至完全融合,再依次加入所述马来酸酐和间苯二胺搅拌均匀后,固化30min,经造粒机进行造粒,挤出机挤出成型,得到粘合层;
S5、共挤成膜:按照基材层、抗介质层、增韧层、粘合层和内层这种次序进行叠放,得到复合膜,将所述复合膜通过挤出机挤出成型,即得抗介质高阻隔共挤膜。
实施例3
一种抗介质高阻隔共挤膜,其特征在于,由基材层、抗介质层、增韧层、粘合层、内层共挤得到的复合薄膜;所述外层为包装时与外界接触,所述抗介质层按照重量组份计包括:酚醛树脂40份、环氧树脂15份、环氧丙烯酸酯13份、过氧化二异丙苯4份、十八烷基胺纳米蒙脱土8份、纳米二氧化钛3份、纳米氧化锌3份、抗介质助剂1份、双氰胺6份、1-羟基环己基苯乙酮8份、油酰胺2份、羟基乙叉二膦酸5份、甲醇溶剂13份;
所述基材层为聚酰胺树脂和抗紫外助剂按重量比80:15制备而成;
所述增韧层按照重量组份计包括:聚丙烯20份、聚乙烯9份、增韧改性剂6份、抗氧化剂1份、乙烯基三胺6份、芥酸酰胺1份、丝素蛋白-聚氨酯水凝胶8份;
所述粘合层按照重量组份计包括:酚醛树脂30份、氧化淀粉5份、马来酸酐1份、腰果油14份、茶油5份、间苯二胺6份、乙醇溶剂12份。
在本实施例中,所述抗介质助剂由聚氨酯、氧化锌粉和丙酮按重量比60:25:10混合而成。
在本实施例中,所述抗紫外助剂如下工艺进行制备:按重量份将15份聚氨酯、9份聚苯硫醚和4份丙烯酸丁酯混合均匀,升温至130℃,保温20min,接着加入6份纳米氧化锌、1份纳米二氧化钛、5份蒙脱土、5份凹凸棒石黏土、2份无机硅藻土、6份十二烷基苯磺酸钠、2份二月桂酸二丁基锡、4份聚磷酸铵、3份丙烯酰胺、5份过硫酸铵、8份水、8份N,N-亚甲基双丙烯酰胺、6份丙三醇二乙酸酯和1份硅烷偶联剂KH-550混合均匀,继续升温至1190℃,保温20min,接着于2500r/min转速搅拌1h,接着于90℃干燥1h,接着粉碎成40目的粉末颗粒得到抗紫外助剂。
所述增韧改性剂按如下工艺进行制备:在氮气保护下,按重量份将25份玻璃鳞片、10份蒸馏水和8份马来酸酐混合均匀,然后升温至90℃,保温10min,然后加入5份过硫酸铵混合均匀,搅拌5min后加入5份苯乙烯混合均匀,接着于850r/min转速搅拌70min,然后升温至85℃,抽提50h,接着于真空烘箱中,65℃烘至恒重,冷却至室温得到物料a;将8份木质纤维粉、3份黄麻纤维、8份氧化锌、4份多壁碳纳米管和5份二氯乙烷混合均匀,超声处理1h,接着加入物料a、5份硅烷偶联剂KH-560、2份过氧化二异丙苯和8份羟基硅油混合均匀,于650r/min转速搅拌40min,接着升温至80℃,回流30h,冷却至室温得到增韧改性剂。
本发明还提出一种所述的抗介质高阻隔共挤膜的制备方法,包括以下步骤:
S1、制备基材层:将所述聚酰胺树脂以颗粒状加入挤出机中,经过挤出机挤出成型得到基材层;
S2、制备抗介质层:将所述酚醛树脂、环氧树脂、环氧丙烯酸酯和过氧化二异丙苯按照上述组份混合均匀,并在120℃恒温下,以150-转/分钟机械搅拌3,之后依次加入所述、1-羟基环己基苯乙酮、油酰胺、羟基乙叉二膦酸和甲醇溶剂,搅拌均匀后加入双氰胺成型30min,再利用造粒机进行造粒,挤出机挤出成型,得到抗介质层;
S3、制备增韧层:将所述聚丙烯、聚乙烯、芥酸酰胺、丝素蛋白-聚氨酯水凝胶按照上述组份混合均匀,并在60℃恒温下,以60转/分钟机械搅拌90min,之后依次加入所述增韧改性剂和抗氧化剂,搅拌均匀后加入所述乙烯基三胺固化成型30min,再利用造粒机进行造粒,挤出机挤出成型,得到增韧层;
S4、制备粘合层:将所述腰果油和茶油加入到所述乙醇溶剂中,以700转/分钟搅拌5min,得到油乳液;将所述油乳液加入到所述酚醛树脂和氧化淀粉中,以1000转/分钟搅拌10min,至完全融合,再依次加入所述马来酸酐和间苯二胺搅拌均匀后,固化60min,经造粒机进行造粒,挤出机挤出成型,得到粘合层;
S5、共挤成膜:按照基材层、抗介质层、增韧层、粘合层和内层这种次序进行叠放,得到复合膜,将所述复合膜通过挤出机挤出成型,即得抗介质高阻隔共挤膜。
对实施例1-3中的抗介质高阻隔共挤膜的性能进行检测,得到的数据如表1所示,
表1:
其中,防紫外线改性助剂以聚氨酯为基础树脂,纳米氧化锌、纳米二氧化钛、蒙脱土、凹凸棒石黏土和无机硅藻土作为防紫外线补强填料体系,利用了该防紫外线补强填料体系中大量的锌元素以及钛元素,使得太阳光紫外线在照射到阻隔膜时,锌元素以及钛元素对紫外线的吸收作用,大大提高了阻隔膜的抗紫外线性能,延长阻隔膜的使用寿命,进一步提高了阻隔膜的抗紫外线性能,且在硅烷偶联剂KH-550对防紫外线补强填料体系的表面羟基进行接枝改性,实现了防紫外线补强填料体系与基础树脂的结合,得到的防紫外线改性助剂运用到本发明的阻隔膜的制备中,有效提高粉阻隔膜的耐紫外线性能,进一步提高了阻隔膜的抗紫外线性能。
通过在氮气保护下,将玻璃鳞片、蒸馏水和马来酸酐混合均匀,然后升温保温,然后加入过硫酸铵混合均匀,搅拌后加入苯乙烯混合均匀,接着搅拌,然后升温,抽提,接着于真空烘箱中,烘至恒重,冷却至室温得到物料a;将木质纤维粉、黄麻纤维、氧化锌、多壁碳纳米管和二氯乙烷混合均匀,超声处理,接着加入物料a、硅烷偶联剂KH-560、过氧化二异丙苯和羟基硅油混合均匀,搅拌,接着升温,回流,冷却至室温得到,其中以玻璃鳞片作为黏性基料,以马来酸酐为接枝单体,以过硫酸铵、苯乙烯和过氧化二异丙苯为引发剂,以木质纤维粉、黄麻纤维、氧化锌、多壁碳纳米管为增韧补强填料,以羟基硅油为溶剂,以硅烷偶联剂KH-560接枝改性剂,通过将以木质纤维粉、黄麻纤维、氧化锌、多壁碳纳米管进行表面改性,得到改性后的填料与马来酸酐结合,并将得到的韧性增强改性助剂运用到本发明的阻隔膜的制备中,得到的阻隔膜具有优异的韧性。
另外,因酚醛树脂分子链上由大量的酚羟基,由于与苯环的共轭效应,时的酚醛基具有弱酸性,因而与水分子中含有对电子的氧原子产生较强的溶剂化作用,而环氧树脂中的脂羟基与烷基碳原子相连,不存在共轭体系,与水分子的溶剂作用较弱,因此,含有酚醛树脂的涂膜在蒸馏水中吸水率较高,同样在强碱性介质中,由于酚醛树脂中酚羟基的弱酸性,能够与氢氧化钠作用生成酚钠,酚醛树脂的加入改善了涂层的交联结构和交联键,因而使得涂层在纯水和强酸性介质中具有较强的抗介质渗透能力,且在高温碱溶液中的稳定性更好。
再者,添加的十八烷基胺纳米蒙脱土能提高碳碳键的转化率,对酯键的水解有促进作用,使共挤膜耐介质渗透性能变差。
最后,抗介质助剂由聚氨酯、氧化锌粉和丙酮混合而成,可以利用氧化锌粉实现提高涂层的耐腐蚀电化学性能,进而有效提高涂层的抗介质性能。
以上内容不能认定本发明具体实施只局限于这些说明,对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思前提下,还可以做出若干简单推演或替换,都应当视为属于本发明由所提交的权利要求书确定的专利保护范围。
Claims (7)
1.一种抗介质高阻隔共挤膜,其特征在于,由基材层、抗介质层、增韧层、粘合层、内层共挤得到的复合薄膜;所述外层为包装时与外界接触,所述抗介质层按照重量组份计包括:酚醛树脂30-40份、环氧树脂15-23份、环氧丙烯酸酯10-13份、过氧化二异丙苯4-6份、十八烷基胺纳米蒙脱土5-8份、纳米二氧化钛3-4份、纳米氧化锌2-3份、抗介质助剂1-3份、双氰胺4-6份、1-羟基环己基苯乙酮8-10份、油酰胺1-2份、羟基乙叉二膦酸5-7份、甲醇溶剂13-25份;
所述基材层为聚酰胺树脂和抗紫外助剂按重量比80:15制备而成;
所述增韧层按照重量组份计包括:聚丙烯15-20份、聚乙烯9-11份、增韧改性剂4-6份、抗氧化剂1-3份、乙烯基三胺4-6份、芥酸酰胺1-2份、丝素蛋白-聚氨酯水凝胶5-8份;
所述粘合层按照重量组份计包括:酚醛树脂30-40份、氧化淀粉3-5份、马来酸酐1-3份、腰果油10-14份、茶油5-8份、间苯二胺4-6份、乙醇溶剂12-24份。
2.如权利要求1所述的一种抗介质高阻隔共挤膜,其特征在于,所述抗介质助剂由聚氨酯、氧化锌粉和丙酮按重量比60-80:15-25:10-20混合而成。
3.如权利要求1所述的一种抗介质高阻隔共挤膜,其特征在于,所述抗紫外助剂的原料按重量份包括:聚氨酯15-25份、聚苯硫醚6-9份、丙烯酸丁酯4-8份、纳米氧化锌3-6份、纳米二氧化钛1-4份、蒙脱土2-5份、凹凸棒石黏土1-5份、无机硅藻土2-5份、十二烷基苯磺酸钠4-6份、二月桂酸二丁基锡2-5份、聚磷酸铵1-4份、丙烯酰胺3-5份、过硫酸铵1-5份、水8-16份、N,N-亚甲基双丙烯酰胺4-8份、丙三醇二乙酸酯3-6份、硅烷偶联剂KH-550 1-4份。
4.如权利要求3所述的一种抗介质高阻隔共挤膜,其特征在于,所述抗紫外助剂如下工艺进行制备:将聚氨酯、聚苯硫醚和丙烯酸丁酯混合均匀,升温至110-130℃,保温20-40min,接着加入纳米氧化锌、纳米二氧化钛、蒙脱土、凹凸棒石黏土、无机硅藻土、十二烷基苯磺酸钠、二月桂酸二丁基锡、聚磷酸铵、丙烯酰胺、过硫酸铵、水、N,N-亚甲基双丙烯酰胺、丙三醇二乙酸酯和硅烷偶联剂KH-550混合均匀,继续升温至150-190℃,保温20-40min,接着于1500-2500r/min转速搅拌1-3h,接着于80-90℃干燥1-4h,接着粉碎成20-40目的粉末颗粒得到抗紫外助剂。
5.如权利要求1所述的一种抗介质高阻隔共挤膜,其特征在于,所述增韧改性剂的原料按重量份包括:玻璃鳞片15-25份、蒸馏水10-20份、马来酸酐4-8份、过硫酸铵2-5份、苯乙烯1-5份、木质纤维粉4-8份、黄麻纤维3-6份、氧化锌2-8份、多壁碳纳米管4-6份、二氯乙烷2-5份、硅烷偶联剂KH-560 1-5份、过氧化二异丙苯2-6份、羟基硅油4-8份。
6.如权利要求5所述的一种抗介质高阻隔共挤膜,其特征在于,所述增韧改性剂按如下工艺进行制备:在氮气保护下,将玻璃鳞片、蒸馏水和马来酸酐混合均匀,然后升温至80-90℃,保温10-30min,然后加入过硫酸铵混合均匀,搅拌5-15min后加入苯乙烯混合均匀,接着于850-1250r/min转速搅拌50-70min,然后升温至85-95℃,抽提40-50h,接着于真空烘箱中,65-75℃烘至恒重,冷却至室温得到物料a;将木质纤维粉、黄麻纤维、氧化锌、多壁碳纳米管和二氯乙烷混合均匀,超声处理1-3h,接着加入物料a、硅烷偶联剂KH-560、过氧化二异丙苯和羟基硅油混合均匀,于650-850r/min转速搅拌20-40min,接着升温至80-90℃,回流20-30h,冷却至室温得到增韧改性剂。
7.一种如权利要求1-6任一项所述的抗介质高阻隔共挤膜的制备方法,其特征在于,包括以下步骤:
S1、制备基材层:将所述聚酰胺树脂以颗粒状加入挤出机中,经过挤出机挤出成型得到基材层;
S2、制备抗介质层:将所述酚醛树脂、环氧树脂、环氧丙烯酸酯和过氧化二异丙苯按照上述组份混合均匀,并在110-120℃恒温下,以150-250转/分钟机械搅拌1-3,之后依次加入所述、1-羟基环己基苯乙酮、油酰胺、羟基乙叉二膦酸和甲醇溶剂,搅拌均匀后加入双氰胺成型30-60min,再利用造粒机进行造粒,挤出机挤出成型,得到抗介质层;
S3、制备增韧层:将所述聚丙烯、聚乙烯、芥酸酰胺、丝素蛋白-聚氨酯水凝胶按照上述组份混合均匀,并在50-60℃恒温下,以60-120转/分钟机械搅拌60-90min,之后依次加入所述增韧改性剂和抗氧化剂,搅拌均匀后加入所述乙烯基三胺固化成型30-60min,再利用造粒机进行造粒,挤出机挤出成型,得到增韧层;
S4、制备粘合层:将所述腰果油和茶油加入到所述乙醇溶剂中,以500-700转/分钟搅拌5-10min,得到油乳液;将所述油乳液加入到所述酚醛树脂和氧化淀粉中,以800-1000转/分钟搅拌10-20min,至完全融合,再依次加入所述马来酸酐和间苯二胺搅拌均匀后,固化30-60min,经造粒机进行造粒,挤出机挤出成型,得到粘合层;
S5、共挤成膜:按照基材层、抗介质层、增韧层、粘合层和内层这种次序进行叠放,得到复合膜,将所述复合膜通过挤出机挤出成型,即得抗介质高阻隔共挤膜。
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Denomination of invention: A high barrier co extruded film with anti dielectric properties and its preparation method Granted publication date: 20221028 Pledgee: Bank of Beijing Limited by Share Ltd. Hangzhou branch Pledgor: ZHONGSU NEW MATERIALS TECHNOLOGY (HANGZHOU) CO.,LTD. Registration number: Y2024330000182 |