CN116903952A - 一种高盐高湿环境用防霉抗菌母粒及其制备方法 - Google Patents
一种高盐高湿环境用防霉抗菌母粒及其制备方法 Download PDFInfo
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Abstract
本申请涉及抗菌母粒领域,具体公开了一种高盐高湿环境用防霉抗菌母粒及其制备方法。一种高盐高湿环境用防霉抗菌母粒包括以下质量百分比的各组分:乙烯‑醋酸乙烯酯共聚物70‑80%、分散剂1‑5%、疏水剂1‑7%、有机防霉抗菌剂5‑15%、无机抗菌剂5‑15%;所述有机防霉抗菌剂选自三氯生、碘丙炔醇丁基氨甲酸酯、聚己缩胍盐酸盐中的一种或多种的组合;所述无机抗菌剂为纳米银/埃洛石复合抗菌剂。本申请的高盐高湿环境用防霉抗菌母粒具有在高盐高湿环境下具有优异的防霉抗菌效果的优点。
Description
技术领域
本申请涉及抗菌母粒领域,更具体地说,它涉及一种高盐高湿环境用防霉抗菌母粒及其制备方法。
背景技术
细菌和霉菌是微生物的两种主要类型,具有种类繁多、分布极广、生命力旺盛等特点,当环境条件为相对湿度大于65%、温度20℃-30℃、pH值3.0-6.0时,就会迅速吸收材料表面的营养物质而生长,造成材料的霉变和破坏。
目前,常在母粒中添加抗菌剂以获得具有抗菌效果的塑料制品。抗菌剂主要包括有机抗菌剂和无机抗菌剂,有机抗菌剂包括季铵盐类、咪唑类、吡啶类、有机金属类等;无机抗菌剂主要为银、铜、锌等无机物,主要利用其氧化活性和游离离子来杀伤菌类。
然而,由于高盐高湿环境下,抗菌物质易发生分解、且释放较快,大多数抗菌母粒所赋予塑料制品的防霉抗菌效果有限,故有待改善。
发明内容
为了提高高盐高湿环境下母粒的防霉抗菌效果,本申请提供一种高盐高湿环境用防霉抗菌母粒及其制备方法。
第一方面,本申请提供一种高盐高湿环境用防霉抗菌母粒,采用如下的技术方案:一种高盐高湿环境用的防霉抗菌母粒,包括以下质量百分比的各组分:
乙烯-醋酸乙烯酯共聚物70-80%、
分散剂1-5%、
疏水剂1-7%、
有机防霉抗菌剂5-15%、
无机抗菌剂5-15%;
所述有机防霉抗菌剂选自三氯生、碘丙炔醇丁基氨甲酸酯、聚己缩胍盐酸盐中的一种或多种的组合;
所述无机抗菌剂为纳米银/埃洛石复合抗菌剂。
通过采用上述技术方案,乙烯-醋酸乙烯酯共聚物,或称为EVA树脂,具有良好的化学稳定性、耐老化性,耐水性、耐腐蚀性和抗菌性能好,适用于高盐高湿环境;三氯生为广谱、高效抗菌剂,对革兰式阳性菌、真菌等具有高效的杀灭即抑制作用,能够吸附穿透细胞壁,与细胞质中的脂质和蛋白质反应,产生不可逆变性,防霉抗菌效果好,且在树脂体系中具有较高的稳定性,被释放后又能够在环境中较快分解,不易产生耐药性;碘丙炔醇丁基氨甲酸酯能够抑制真菌重要酶的活性,具有较高的抗霉防腐作用,且抗氧性能好;聚己缩胍盐酸盐能够吸附于细菌细胞表面的一些含磷化合物,破坏细胞壁,造成低分子量的细胞质内物质外漏,导致膜磷酯分离,影响蛋白质的聚集,造成膜穿透性增加,从而抑制细菌生长并导致细菌死亡,杀菌谱广,杀菌效率较低但长效抗菌效果好,且是通过机械吸附作用进行杀菌,细菌不易产生耐药性;
纳米银粒子能够破坏细胞膜的磷脂双分子层结构,改变细胞膜通透性,造成低分子量的细胞质内物质外漏,具有高效、广谱抗菌、长效抗菌作用,且不易产生耐药性;埃洛石耐盐性好,能够通过物理静电吸附在细菌细胞膜表面,影响细胞通透性,阻碍细菌与外界环境正常的物质交换,且埃洛石中的铝元素对细胞有一定的毒副作用,另一方面,埃洛石为中空管状结构,且两端开放,具有高吸附性,比表面积大,表面羟基丰富,能够作为载体材料对纳米银粒子起到很好的固定和分散效果,纳米银与埃洛石相复合作为无机抗菌剂,埃洛石作为纳米银的载体,促进纳米银在树脂体系中的分散,并对纳米银起到缓释作用,提高无机抗菌剂的抗菌长效性;
分散剂促进了防霉抗菌母粒各组份的均匀分散,有利于保证防霉抗菌母粒的稳定性;疏水剂提高了防霉抗菌母粒的疏水作用,减少了高盐高湿环境下液体在塑料制品表面积蓄的可能性,有利于减少细菌、霉菌在塑料制品表面的增殖,同时有利于减缓有机防霉抗菌剂的过快扩散至环境中的可能性,保证了长效抗菌效果;
综上所述,本申请通过选用乙烯-醋酸乙烯酯共聚物作为树脂基体,保证了防霉抗菌母粒及所制得的塑料制品在高盐高湿环境下的稳定性;通过有机防霉抗菌剂和无机抗菌剂相配合,使防霉抗菌母粒具有效果优异、广谱长效的抗菌防霉性能;通过疏水剂减少了环境中的水分在塑料制品表面凝聚成水珠的可能性,有利于抑制细菌、霉菌在塑料制品表面的增殖生长,并减少了有机防霉抗菌剂通过水介质而过快释放的可能性;通过分散剂保证了各组分的均匀分布,进一步保证了防霉抗菌母粒及所制得的塑料制品在高盐高湿环境下的抗菌稳定性;各组分相互配合、共同作用,使防霉抗菌母粒在高盐高湿环境下具有优异的防霉抗菌效果。
优选的,所述有机防霉抗菌剂为质量比为1:(0.2-0.5):(2-3)的三氯生、碘丙炔醇丁基氨甲酸酯和聚己缩胍盐酸盐。
通过采用上述技术方案,使防霉抗菌母粒具有更佳的抗菌防霉效果。
优选的,所述无机抗菌剂的制备方法为:
将埃洛石浸入1-4mol/L的盐酸溶液中,浸渍20-30min,滤出,洗涤,干燥;
将硝酸银溶解于无水乙醇中,配制为0.01-0.1mol/L的硝酸银溶液,将酸处理后的埃洛石浸入其中,超声分散,在30-40℃下浸渍12-48h,真空抽滤,洗涤,干燥,得到纳米银/埃洛石复合抗菌剂。
通过采用上述技术方案,稀盐酸浸渍有利于进一步扩大埃洛石的比表面积,并使表面活性基团更佳丰富,有利于纳米银粒子的负载;无水乙醇的将硝酸银缓慢还原为纳米银粒子,埃洛石对纳米银粒子不断吸附和负载,最终获得纳米银/埃洛石复合抗菌剂。
优选的,所述疏水剂包括全氟硅烷、聚四氟乙烯蜡中的一种或多种的组合。
优选的,以所述防霉抗菌母粒的原料总质量计,所述疏水剂包括2-4%全氟硅烷、2-3%聚四氟乙烯蜡。
通过采用上述技术方案,全氟硅烷能够促进无机抗菌剂与EVA树脂体系的相容性,提高树脂交联程度,提高柔韧性和弹性,并能够提高防霉抗菌母粒的耐盐性、耐腐蚀性和耐水性,即能够提高防霉抗菌母粒的疏水作用,提高防霉抗菌母粒及所制得的塑料制品在高盐高湿环境下的稳定性;聚四氟乙烯蜡能够起到润滑作用,促进无机抗菌剂的分散,同时能够扩散至防霉抗菌母粒及所制得的塑料制品表面,发挥良好的疏水作用。
优选的,所述分散剂选自聚乙烯吡咯烷酮、三乙醇胺、十二烷基苯磺酸盐、六偏磷酸盐、十二烷基硫酸盐、木质素磺酸盐中的一种或多种的组合。
通过采用上述技术方案,有利于促进各组分的均匀分散,提高防霉抗菌母粒在高盐高湿环境下的稳定性。
优选的,所述防霉抗菌母粒还包括1-5%防腐填料,所述防腐填料选自石墨烯、云母粉、玻璃鳞片中的一种或多种的组合。
通过采用上述技术方案,石墨烯结构稳定,耐腐蚀性能好,并且具有较强的吸附力,能够吸附EVA树脂和其他各组分,增强防霉抗菌母粒体系的稳定性,提高耐盐、耐腐蚀性能;云母粉具有优异的耐高温、耐酸碱、耐腐蚀性能,片状的云母粉在防霉抗菌母粒体系中形成基本平行的取向排列,阻挡水份或其他腐蚀性物质的渗入,同时具有较佳的抗紫外、红外性能,有利于减少防霉抗菌母粒中有机防霉抗菌剂等有机物质的受光分解,有利于保证抗菌效果;玻璃鳞片具有优异的抗腐蚀介质渗透性,有利于提高防霉抗菌母粒的防腐性能;
通过添加防腐填料,提高了防霉抗菌母粒在高盐高湿环境下的防腐性能,有利于提高抗菌母粒的作用稳定性,保证防霉抗菌效果。
优选的,所述防腐填料是经改性处理后得到,具体步骤为:
在超声环境下,将防腐填料浸入无水乙醇中,依次经过滤、烘干,得到改性处理后的防腐填料。
通过采用上述技术方案,有利于促进防腐填料在防霉抗菌母粒中的均匀分散。
第二方面,本申请提供一种高盐高湿环境用防霉抗菌母粒的制备方法,采用如下的技术方案:
一种高盐高湿环境用防霉抗菌母粒的制备方法,包括以下步骤:
按配比,将乙烯-醋酸乙烯酯共聚物、分散剂、疏水剂、有机防霉抗菌剂、无机抗菌剂混合搅拌,得到混合物;
将混合物经双螺杆挤出机熔融挤出成条,冷却,切粒,干燥,得到高盐高湿环境用防霉抗菌母粒。
优选的,包括以下步骤:
按配比,按配比,将乙烯-醋酸乙烯酯共聚物、分散剂、疏水剂、有机防霉抗菌剂、无机抗菌剂、防腐填料混合搅拌,得到混合物;
将混合物经双螺杆挤出机熔融挤出成条,冷却,切粒,干燥,得到高盐高湿环境用防霉抗菌母粒。
通过采用上述技术方案,能够制得具有优异的广谱长效防霉抗菌效果的防霉抗菌母粒。
综上所述,本申请具有以下有益效果:
1、由于本申请采用乙烯-醋酸乙烯酯共聚物作为树脂基体,保证了防霉抗菌母粒及所制得的塑料制品在高盐高湿环境下的稳定性;通过有机防霉抗菌剂和无机抗菌剂相配合,使防霉抗菌母粒具有效果优异、广谱长效的抗菌防霉性能;通过疏水剂减少了环境中的水分在塑料制品表面凝聚成水珠的可能性,有利于抑制细菌、霉菌在塑料制品表面的增殖生长,并减少了有机防霉抗菌剂通过水介质而过快释放的可能性;通过分散剂保证了各组分的均匀分布,进一步保证了防霉抗菌母粒及所制得的塑料制品在高盐高湿环境下的抗菌稳定性;各组分相互配合、共同作用,使防霉抗菌母粒在高盐高湿环境下具有优异的防霉抗菌效果;
2、本申请中优选采用质量比为1:(0.2-0.5):(2-3)的三氯生、碘丙炔醇丁基氨甲酸酯和聚己缩胍盐酸盐相复配作为有机防霉抗菌剂,三种化合物相互配合,能够赋予防霉抗菌母粒更佳的防霉抗菌性能;
3、本申请中优选添加防腐填料以进一步提高防霉抗菌母粒在高盐高湿环境下的防腐性能,提高抗菌母粒的作用稳定性,有利于保证防霉抗菌效果。
具体实施方式
以下结合实施例对本申请作进一步详细说明。
制备例
本制备例提供了一种无机抗菌剂,制备方法如下:
将埃洛石浸入2mol/L的盐酸溶液中,浸渍20min,滤出,水洗3次,70℃下烘干;
将硝酸银溶解于无水乙醇中,配制为0.05mol/L的硝酸银溶液,按照浴比1:20,将酸处理后的埃洛石浸入其中,超声分散,在40℃下浸渍12h,真空抽滤,用无水乙醇洗涤3次,60℃烘干,得到纳米银/埃洛石复合抗菌剂。
实施例
实施例1
一种高盐高湿环境用防霉抗菌母粒,包括以下质量的各组分:7.5kg乙烯-醋酸乙烯酯共聚物,0.3kg分散剂,0.4kg疏水剂,1kg有机防霉抗菌剂,0.8kg无机抗菌剂。
在本实施例中,乙烯-醋酸乙烯酯共聚物为牌号为UL7520的EVA树脂,分散剂为三乙醇胺,疏水剂为全氟癸基三甲氧基硅烷,有机防霉抗菌剂为聚己缩胍盐酸盐,无机抗菌剂由制备例1制得。
高盐高湿环境用防霉抗菌母粒的制备方法如下:
将上述质量的乙烯-醋酸乙烯酯共聚物、分散剂、疏水剂、有机防霉抗菌剂、无机抗菌剂依次加入高速混料机中搅拌,充分搅拌均匀后得到混合物;
将所述混合物加入到双螺杆挤出机中,经熔融挤出成条,将得到的丝条经水槽冷却后,输送至切粒机切粒,再输送入干燥器内干燥处理,冷却后到高盐高湿环境的防霉抗菌EVA色母粒。
实施例2
本实施例与实施例1的不同之处仅在于,高盐高湿环境用防霉抗菌母粒包括以下质量的各组分:7.8kg乙烯-醋酸乙烯酯共聚物,0.1kg分散剂,0.1kg疏水剂,0.5kg有机防霉抗菌剂,1.5kg无机抗菌剂。
实施例3
本实施例与实施例1的不同之处仅在于,高盐高湿环境用防霉抗菌母粒包括以下质量的各组分:7kg乙烯-醋酸乙烯酯共聚物,0.5kg分散剂,0.5kg疏水剂,1.5kg有机防霉抗菌剂,0.5kg无机抗菌剂。
实施例4
本实施例与实施例1的不同之处仅在于,有机防霉抗菌剂为三氯生。
实施例5
本实施例与实施例1的不同之处仅在于,有机防霉抗菌剂为碘丙炔醇丁基氨甲酸酯。
实施例6
本实施例与实施例1的不同之处仅在于,有机防霉抗菌剂为质量比为1:0.2:3的聚己缩胍盐酸盐、碘丙炔醇丁基氨甲酸酯、三氯生的组合。
实施例7
本实施例与实施例1的不同之处仅在于,有机防霉抗菌剂为质量比为1:0.4:2的聚己缩胍盐酸盐、碘丙炔醇丁基氨甲酸酯、三氯生的组合。
实施例8
本实施例与实施例1的不同之处仅在于,有机防霉抗菌剂为质量比为1:1:1的聚己缩胍盐酸盐、碘丙炔醇丁基氨甲酸酯、三氯生的组合。
实施例9
本实施例与实施例1的不同之处仅在于,疏水剂为聚四氟乙烯蜡。
实施例10
本实施例与实施例1的不同之处仅在于,疏水剂为0.2kg全氟癸基三甲氧基硅烷和0.2kg聚四氟乙烯蜡的组合。
实施例11
本实施例与实施例1的不同之处仅在于,分散剂为木质素磺酸盐。
实施例12
本实施例与实施例1的不同之处仅在于,高盐高湿环境用防霉抗菌母粒包括以下质量的各组分:7.2kg乙烯-醋酸乙烯酯共聚物,0.3kg分散剂,0.4kg疏水剂,1kg有机防霉抗菌剂,0.8kg无机抗菌剂,0.3kg防腐填料。
在本实施例中,防腐填料为石墨烯。
高盐高湿环境用防霉抗菌母粒的制备方法为:
将上述质量的乙烯-醋酸乙烯酯共聚物、分散剂、疏水剂、有机防霉抗菌剂、无机抗菌剂、防腐填料依次加入高速混料机中搅拌,充分搅拌均匀后得到混合物;
将所述混合物加入到双螺杆挤出机中,经熔融挤出成条,将得到的丝条经水槽冷却后,输送至切粒机切粒,再输送入干燥器内干燥处理,冷却后到高盐高湿环境的防霉抗菌EVA色母粒。
实施例13
本实施例与实施例12的不同之处仅在于,防腐填料为云母粉。
实施例14
本实施例与实施例12的不同之处仅在于,防腐填料为玻璃鳞片。
实施例15
本实施例与实施例12的不同之处仅在于,防腐填料为经过改性处理的防腐填料,改性方法如下:
在超声环境下,按照浴比1:20将防腐填料浸入无水乙醇中,再经过滤、烘干,得到改性处理后的防腐填料。
对比例
对比例1
本对比例与实施例1的不同之处仅在于,高盐高湿环境用防霉抗菌母粒包括以下质量的各组分:7.5kg乙烯-醋酸乙烯酯共聚物,0.3kg分散剂,0.4kg疏水剂,1.8kg有机防霉抗菌剂。
对比例2
本对比例与实施例1的不同之处仅在于,高盐高湿环境用防霉抗菌母粒包括以下质量的各组分:7.5kg乙烯-醋酸乙烯酯共聚物,0.3kg分散剂,0.4kg疏水剂,1.8kg无机抗菌剂。
对比例3
本对比例与实施例1的不同之处仅在于,高盐高湿环境用防霉抗菌母粒包括以下质量的各组分:7.9kg乙烯-醋酸乙烯酯共聚物,0.3kg分散剂,1kg有机防霉抗菌剂,0.8kg无机抗菌剂。
性能检测试验
将各实施例、对比例的防霉抗菌母粒与EVA树脂按照母粒:EVA树脂=5:100的比例混合,在注塑机上注塑成宽2cm、长4cm的标准塑料样条,进行如下测试:
测试一:抗菌效果测试:参照GB/T 31402-2015《塑料塑料表面抗菌性能试验方法》,以金黄色葡萄球菌ATCC 8739为测试对象,测试各实施例和对比例所制得的标准样条的抗菌率;
测试二:防霉效果测试:参照标准GB/T 24128-2009《塑料防霉性能试验方法》,以黑曲霉AS3.315为测试对象,测试各实施例和对比例所制得的标准样条上的霉菌生长情况并进行评级,其中0级为霉菌不生长,1级表示长霉面积<10%,2级表示长霉面积≥10%并<30%,3级表示长霉面积≥30%并<60%,4级表示长霉面积≥60%并≤100%;
测试三:高盐高湿环境测试:将各实施例和对比例所制得的标准样条浸泡于温度为28-30℃、pH为5、5wt%的氯化钠溶液中,浸泡7天后,观察各个样条上是否有霉斑生长,并参考测试二的方法进行评级,再进行试样上细菌回收,测定平均活菌数(CFU/cm2)。
表1
结合实施例1-3并结合表1,可以看出,参照本申请工卡的配方制得的防霉抗菌母粒,注塑后能够赋予塑料样条优异的防霉抗菌效果,并且在高盐高湿环境下,塑料样条仍具有较高的防霉抗菌性能。结合实施例1和对比例1-2并结合表1,表明有机防霉抗菌、无机抗菌剂相互配合能够提高塑料样条更佳的防霉抗菌效果。
结合实施例1、实施例6-8并结合表1,可以看出,聚己缩胍盐酸盐、三氯生对细菌的抑制效果较好,碘丙炔醇丁基氨甲酸酯对霉菌的抑制效果较好,参照本申请公开的配比将三者相复配时,能够赋予防霉抗菌母粒较高的防霉抗菌性能,高效、速效的三氯生与低效、长效的聚己缩胍盐酸盐相配合提高了塑料制品对细菌的抑制作用,碘丙炔醇丁基氨甲酸酯促进了塑料制品对霉菌的抑制作用。
结合实施例1、实施例9-10和对比例3并结合表1,可以看出,疏水剂的添加能够减少细菌、霉菌在塑料制品上的附着,有利于促进了高盐高湿环境下防霉抗菌母粒的防霉抗菌性能的提高。
结合实施例1、实施例12-14并结合表1,可以看出防腐填料的添加有利于提高塑料样条在高盐高湿环境下的防霉抗菌效果,其中,云母粉与玻璃鳞片能够抑制液体介质对塑料样条的渗透,使塑料样条具有更佳的防霉抗菌性能。
本具体实施例仅仅是对本申请的解释,其并不是对本申请的限制,本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改,但只要在本申请的权利要求范围内都受到专利法的保护。
Claims (10)
1.一种高盐高湿环境用防霉抗菌母粒,其特征在于,包括以下质量百分比的各组分:
乙烯-醋酸乙烯酯共聚物70-80%、
分散剂1-5%、
疏水剂1-7%、
有机防霉抗菌剂5-15%、
无机抗菌剂5-15%;
所述有机防霉抗菌剂选自三氯生、碘丙炔醇丁基氨甲酸酯、聚己缩胍盐酸盐中的一种或多种的组合;
所述无机抗菌剂为纳米银/埃洛石复合抗菌剂。
2.根据权利要求1所述的高盐高湿环境用防霉抗菌母粒,其特征在于:所述有机防霉抗菌剂为质量比为1:(0.2-0.5):(2-3)的三氯生、碘丙炔醇丁基氨甲酸酯和聚己缩胍盐酸盐。
3.根据权利要求1所述的高盐高湿环境用防霉抗菌母粒,其特征在于:所述无机抗菌剂的制备方法为:
将埃洛石浸入1-4mol/L的盐酸溶液中,浸渍20-30min,滤出,洗涤,干燥;
将硝酸银溶解于无水乙醇中,配制为0.01-0.1mol/L的硝酸银溶液,将酸处理后的埃洛石浸入其中,超声分散,在30-40℃下浸渍12-48h,真空抽滤,洗涤,干燥,得到纳米银/埃洛石复合抗菌剂。
4.根据权利要求1所述的高盐高湿环境用防霉抗菌母粒,其特征在于:所述疏水剂包括全氟硅烷、聚四氟乙烯蜡中的一种或多种的组合。
5.根据权利要求4所述的高盐高湿环境用防霉抗菌母粒,其特征在于:以所述防霉抗菌母粒的原料总质量计,所述疏水剂包括2-4%全氟硅烷、2-3%聚四氟乙烯蜡。
6.根据权利要求1所述的高盐高湿环境用防霉抗菌母粒,其特征在于:所述分散剂选自聚乙烯吡咯烷酮、三乙醇胺、十二烷基苯磺酸盐、六偏磷酸盐、十二烷基硫酸盐、木质素磺酸盐中的一种或多种的组合。
7.根据权利要求1所述的高盐高湿环境用防霉抗菌母粒,其特征在于:所述防霉抗菌母粒还包括1-5%防腐填料,所述防腐填料选自石墨烯、云母粉、玻璃鳞片中的一种或多种的组合。
8.根据权利要求7所述的高盐高湿环境用防霉抗菌母粒,其特征在于:所述防腐填料是经改性处理后得到,具体步骤为:
在超声环境下,将防腐填料浸入无水乙醇中,依次经过滤、烘干,得到改性处理后的防腐填料。
9.一种如权利要求1-8所述的高盐高湿环境用防霉抗菌母粒的制备方法,其特征在于:包括以下步骤:
按配比,将乙烯-醋酸乙烯酯共聚物、分散剂、疏水剂、有机防霉抗菌剂、无机抗菌剂混合搅拌,得到混合物;
将混合物经双螺杆挤出机熔融挤出成条,冷却,切粒,干燥,得到高盐高湿环境用防霉抗菌母粒。
10.根据权利要求9所述的高盐高湿环境用防霉抗菌母粒的制备方法,其特征在于:包括以下步骤:
按配比,按配比,将乙烯-醋酸乙烯酯共聚物、分散剂、疏水剂、有机防霉抗菌剂、无机抗菌剂、防腐填料混合搅拌,得到混合物;
将混合物经双螺杆挤出机熔融挤出成条,冷却,切粒,干燥,得到高盐高湿环境用防霉抗菌母粒。
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