CN113445152A - 一种基于定岛超纤改性制备压电抗菌口罩滤材的方法 - Google Patents

一种基于定岛超纤改性制备压电抗菌口罩滤材的方法 Download PDF

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CN113445152A
CN113445152A CN202110438807.3A CN202110438807A CN113445152A CN 113445152 A CN113445152 A CN 113445152A CN 202110438807 A CN202110438807 A CN 202110438807A CN 113445152 A CN113445152 A CN 113445152A
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CN113445152B (zh
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王睿
谭雪玲
胡丹
毛佳伟
张晓飞
陈静
陈意
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CHENGDU PRODUCT QUALITY SUPERVISION AND INSPECTION INSTITUTE
SICHUAN INSTITUTE PRODUCT QUALITY SUPERVISION INSPECTION AND RESEARCH
Chengdu Products Quality Inspection Research Institute Co ltd
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Abstract

本发明涉及一种基于定岛超纤改性制备压电抗菌口罩滤材的方法。所述方法利用尼龙11和聚偏氟乙烯改性定岛超纤，在特定聚氨酯填充材料的帮助下，实现改性定岛超纤的高压极化，进而产生1～2V的压电。利用该方法制成的口罩滤材可以替代传统熔喷布滤材，并且可以将人体活动产生的力转化为超低电压以发挥杀菌功能，无须添加任何小分子抗菌剂，产品对人体无害，丢弃后也不会因抗菌剂环境累积而产生细菌耐药性。

Description

一种基于定岛超纤改性制备压电抗菌口罩滤材的方法
技术领域
本发明属于日用防护品技术领域，具体涉及一种基于定岛超纤改性制备压电抗菌口罩滤材的方法。
背景技术
个人防护口罩一般为多层结构，内外侧为单层纺粘层，中间为单层或多层熔喷布。熔喷布俗称口罩的“心脏”，具有良好的过滤性、屏蔽性、绝热性和吸油性。熔喷布的主要原料为聚丙烯(PP)，采用高速热空气流对模头喷丝孔挤出的PP熔体细流进行牵伸，形成超细纤维，并收集在凝网帘或滚筒上，靠纤维自身粘合形成无纺布，可以有效过滤细菌、粉尘；含有细菌的飞沫靠近熔喷布后，也会被静电吸附在表面，无法透过。因此，熔喷布是生产个人防护口罩的必要原料；如熔喷布资源不足，个人防护口罩产能将受到严重影响。因此，开发能有效替代熔喷布的口罩滤材，是缓解社会在非常时期对个人防护口罩巨大需求的重要途径。
除熔喷工艺外，海岛法是制造超细纤维无纺布的另一种重要方法，在合成革、清洁用品领域已有广泛应用。海岛法工艺分为定岛、不定岛两种。由于定岛法克服了非定岛超细纤维在纤维粗细、长度方面不可控的缺陷，因此制造的无纺布综合性能更好，理论上可替代熔喷布用于制造口罩滤材。
然而，传统定岛超纤孔隙大、孔隙率高，对细菌、粉尘的过滤效率低。此外，传统定岛超纤也无抗菌功能。通过添加小分子抗菌剂可赋予产品抗菌性，但小分子抗菌剂大多具有生理毒性，与人体皮肤接触时会引起过敏、炎症等副作用；这些口罩被丢弃后，小分子抗菌剂还会在环境中积累，导致细菌产生耐药性。
故基于此，提出本发明技术方案。
发明内容
为了解决现有技术存在的问题，本发明提供了一种基于定岛超纤改性制备压电抗菌口罩滤材的方法。所述压电抗菌口罩滤材的抗菌功能的实现没有使用任何小分子抗菌剂，而是靠人体活动伸缩拉扯滤材生产的超低电压杀死细菌。制成的口罩滤材对人体无害，丢弃后不会污染环境，不会导致细菌耐药性产生。
本发明的方案是，提供一种基于定岛超纤改性制备压电抗菌口罩滤材的方法，包括如下步骤：
(1)将尼龙6母料与尼龙11母料依次混合、烘干、挤出，得尼龙混合母粒；
(2)将所述尼龙混合母粒与碱溶性对苯二甲酸乙二醇酯分别熔融、复合、喷丝、挤出，得定岛复合纤维；
(3)将所述定岛复合纤维依次开松除尘、梳理、混合杂乱、铺网、预针刺、主针刺，得到具有三维网络结构的无纺布；
(4)将溶剂型聚氨酯、聚偏氟乙烯溶于N,N-二甲基甲酰胺，加热搅拌后冷却，得填充剂；
(5)将所述具有三维网络结构的无纺布浸渍于所述填充剂中，再经湿法凝固、水洗、碱减量、水洗、烘干，得改性定岛超纤；
(6)将所述改性定岛超纤进行剖层，再加电压极化，即得压电抗菌口罩滤材。
优选地，步骤(1)中，所述尼龙6母料为5～10重量份；所述尼龙11母料为3～5重量份。
优选地，步骤(1)中，所述烘干的温度为80～120℃，烘干的时间为8～12h。
优选地，步骤(2)中，所述尼龙混合母粒为5～10重量份；所述碱溶性对苯二甲酸乙二醇酯为5～10重量份。
优选地，步骤(4)中，所述溶剂型聚氨酯的硬段为异佛尔酮二异氰酸酯、氢化甲苯二异氰酸酯、氢化二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯中的一种或多种；所述溶剂型聚氨酯的软段为数均分子量为6000～8000的聚己二酸丁二醇酯二醇、聚己二酸乙二醇酯二醇、聚碳酸亚乙酯二醇、聚碳酸亚丙酯二醇中的一种或多种。
优选地，步骤(4)中，所述溶剂型聚氨酯为5～10重量份；所述聚偏氟乙烯为5～10重量份；所述N,N-二甲基甲酰胺为100重量份。
优选地，步骤(4)中，所述加热的温度为70～90℃，搅拌的时间为2～3h。
优选地，步骤(6)中，所述极化的温度为70～100℃，极化的时间为15～45min，极化的电压为3～10kV。
基于相同的技术构思，本发明的再一方案是，提供一种由上述制备方法得到的压电抗菌口罩滤材。
本发明所涉及的方法的原理是：
据研究表明，1～2V的电压即可造成细菌的细胞膜穿孔，同时破坏细菌的代谢系统，从而杀死细菌。这种超低压电场对人体无害，杀菌机制也不同于小分子抗菌剂，细菌也很难通过改变自身膜结构产生耐药性。
聚偏氟乙烯和尼龙11在经过高压电场(3～10kV)极化后，其内部分子能够形成单轴取向，进而表现出压电性，但各自产生的压电难以超过1V，无法起到杀菌作用。本发明以尼龙11改性定岛超纤的岛组分，以聚偏氟乙烯作为定岛超纤填充剂，两者协同，在高压电场极化后正反两面之间可以产生1～2V的压电，使改性后的定岛超纤具有压电杀菌功能。
然而，由于定岛超纤孔隙大、孔隙率高，容易被高压电场击穿，导致极化失败。本发明以湿法聚氨酯对定岛超纤进行填充，可以提升产品对细菌、粉尘的过滤性。更为重要的时，填充后的定岛超纤能经受的电场电压上限会提升。本发明在大量实验后发现，只有当填充聚氨酯为脂肪族聚氨酯，且软段为数均分子量为6000～8000的聚己二酸丁二醇酯二醇、聚己二酸乙二醇酯二醇、聚碳酸亚乙酯二醇、聚碳酸亚丙酯二醇中的一种或多种时，改性后的定岛超纤才具备较高的电阻率，才能经受3～10kV的高压电场极化。极化后的口罩滤材产品，可将人体活动伸缩拉扯滤材的动能转化为电场，滤材正反两面的电压达到1～2V，起到压电杀菌作用。
本发明的有益效果为：
本发明所述基于定岛超纤改性制备压电抗菌口罩滤材的方法，最终得到的压电抗菌口罩滤材其抗菌功能的实现没有使用任何小分子抗菌剂，而是靠人体活动伸缩拉扯滤材生产的超低电压杀死细菌。制成的口罩滤材对人体无害，丢弃后不会污染环境，不会导致细菌耐药性产生。
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，下面将对本发明的技术方案进行详细的描述。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做出创造性劳动的前提下所得到的所有其它实施方式，都属于本发明所保护的范围。
实施例1
本实施例提供一种基于定岛超纤改性制备压电抗菌口罩滤材的方法，包括如下步骤：
(1)将500g尼龙6母料与300g尼龙11母料混合均匀，并在 80℃条件下烘干8h，再利用双螺杆挤出机将其挤出制备，得尼龙混合母粒；
(2)取500g所述尼龙混合母粒与500g碱溶性对苯二甲酸乙二醇酯切片干燥，再各自通过螺杆高温熔融挤出熔体，由不同分配管进入复合纺丝组件，两种熔体在组件内分为细流再汇合，最后经过喷丝板纺丝挤出，得定岛复合纤维；
(3)将所述定岛复合纤维依次开松除尘、梳理、混合杂乱、铺网、预针刺、主针刺，得到具有三维网络结构的无纺布；
(4)将500g溶剂型聚氨酯(硬段为异佛尔酮二异氰酸酯、软段为数均分子量为6000的聚己二酸丁二醇酯二醇)、500g分子量为30 万的聚偏氟乙烯溶于10kg的N,N-二甲基甲酰胺中，在70℃加热搅拌2小时，再冷却至常温，得到填充剂；
(5)将所述具有三维网络结构的无纺布浸渍于所述填充剂中，再经湿法凝固、水洗、碱减量、水洗、烘干，得厚度为2mm的改性定岛超纤；
(6)将所述改性定岛超纤剖成0.5mm，再利用油浴电晕复合电压极化装置对剖层后的改性定岛超纤进行极化，极化温度为70℃，极化时间为15min，极化电压为6kV，即可获得压电抗菌口罩滤材。
经检验，所得压电抗菌口罩滤材符合GB/T32610—2016《日常防护型口罩技术规范》相关要求(过滤效率级别：III级；防护效果级别：D级)，在施力并产生10％伸缩率的条件下，滤材正反两面能产生的压电电压为1.3～1.7V，对大肠杆菌15min灭杀率50～70％。
实施例2
本实施例提供一种基于定岛超纤改性制备压电抗菌口罩滤材的方法，包括如下步骤：
(1)将800g尼龙6母料与400g尼龙11母料混合均匀，并在 100℃条件下烘干8h，再利用双螺杆挤出机将其挤出制备，得尼龙混合母粒；
(2)取800g所述尼龙混合母粒与800g碱溶性对苯二甲酸乙二醇酯切片干燥，再各自通过螺杆高温熔融挤出熔体，由不同分配管进入复合纺丝组件，两种熔体在组件内分为细流再汇合，最后经过喷丝板纺丝挤出，得定岛复合纤维；
(3)将所述定岛复合纤维依次开松除尘、梳理、混合杂乱、铺网、预针刺、主针刺，得到具有三维网络结构的无纺布；
(4)将800g溶剂型聚氨酯(硬段为异佛尔酮二异氰酸酯、软段为数均分子量为7000的聚己二酸丁二醇酯二醇)、800g分子量为50 万的聚偏氟乙烯溶于10kg的N,N-二甲基甲酰胺中，在80℃加热搅拌3小时，再冷却至常温，得到填充剂；
(5)将所述具有三维网络结构的无纺布浸渍于所述填充剂中，再经湿法凝固、水洗、碱减量、水洗、烘干，得厚度为3mm的改性定岛超纤；
(6)将所述改性定岛超纤剖成0.4mm，再利用油浴电晕复合电压极化装置对剖层后的改性定岛超纤进行极化，极化温度为90℃，极化时间为30min，极化电压为8kV，即可获得压电抗菌口罩滤材。
经检验，所得压电抗菌口罩滤材符合GB/T32610—2016《日常防护型口罩技术规范》相关要求(过滤效率级别：III级；防护效果级别：D级)，在施力并产生10％伸缩率的条件下，滤材正反两面能产生的压电电压为1.5-1.8V，对大肠杆菌15min灭杀率60～75％。
实施例3
本实施例提供一种基于定岛超纤改性制备压电抗菌口罩滤材的方法，包括如下步骤：
(1)将1000g尼龙6母料与500g尼龙11母料混合均匀，并在 120℃条件下烘干12h，再利用双螺杆挤出机将其挤出制备，得尼龙混合母粒；
(2)取1000g所述尼龙混合母粒与1000g碱溶性对苯二甲酸乙二醇酯切片干燥，再各自通过螺杆高温熔融挤出熔体，由不同分配管进入复合纺丝组件，两种熔体在组件内分为细流再汇合，最后经过喷丝板纺丝挤出，得定岛复合纤维；
(3)将所述定岛复合纤维依次开松除尘、梳理、混合杂乱、铺网、预针刺、主针刺，得到具有三维网络结构的无纺布；
(4)将1000g溶剂型聚氨酯(硬段为异佛尔酮二异氰酸酯、软段为数均分子量为8000的聚己二酸丁二醇酯二醇)、1000g分子量为 60万的聚偏氟乙烯溶于10kg的N,N-二甲基甲酰胺中，在90℃加热搅拌3小时，再冷却至常温，得到填充剂；
(5)将所述具有三维网络结构的无纺布浸渍于所述填充剂中，再经湿法凝固、水洗、碱减量、水洗、烘干，得厚度为3mm的改性定岛超纤；
(6)将所述改性定岛超纤剖成0.3mm，再利用油浴电晕复合电压极化装置对剖层后的改性定岛超纤进行极化，极化温度为100℃，极化时间为45min，极化电压为10kV，即可获得压电抗菌口罩滤材。
经检验，所得压电抗菌口罩滤材符合GB/T32610—2016《日常防护型口罩技术规范》相关要求(过滤效率级别：III级；防护效果级别：D级)，在施力并产生10％伸缩率的条件下，滤材正反两面能产生的压电电压为1.6-1.9V，对大肠杆菌15min灭杀率70～80％。
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应以所述权利要求的保护范围为准。

Claims (9)

1.一种基于定岛超纤改性制备压电抗菌口罩滤材的方法，其特征在于，包括如下步骤：
(1)将尼龙6母料与尼龙11母料依次混合、烘干、挤出，得尼龙混合母粒；
(2)将所述尼龙混合母粒与碱溶性对苯二甲酸乙二醇酯分别熔融、复合、喷丝、挤出，得定岛复合纤维；
(3)将所述定岛复合纤维依次开松除尘、梳理、混合杂乱、铺网、预针刺、主针刺，得到具有三维网络结构的无纺布；
(4)将溶剂型聚氨酯、聚偏氟乙烯溶于N,N-二甲基甲酰胺，加热搅拌后冷却，得填充剂；
(5)将所述具有三维网络结构的无纺布浸渍于所述填充剂中，再经湿法凝固、水洗、碱减量、水洗、烘干，得改性定岛超纤；
(6)将所述改性定岛超纤进行剖层，再加电压极化，即得压电抗菌口罩滤材。
2.根据权利要求1所述基于定岛超纤改性制备压电抗菌口罩滤材的方法，其特征在于，步骤(1)中，所述尼龙6母料为5～10重量份；所述尼龙11母料为3～5重量份。
3.根据权利要求1所述基于定岛超纤改性制备压电抗菌口罩滤材的方法，其特征在于，步骤(1)中，所述烘干的温度为80～120℃，烘干的时间为8～12h。
4.根据权利要求1所述基于定岛超纤改性制备压电抗菌口罩滤材的方法，其特征在于，步骤(2)中，所述尼龙混合母粒为5～10重量份；所述碱溶性对苯二甲酸乙二醇酯为5～10重量份。
5.根据权利要求1所述基于定岛超纤改性制备压电抗菌口罩滤材的方法，其特征在于，步骤(4)中，所述溶剂型聚氨酯的硬段为异佛尔酮二异氰酸酯、氢化甲苯二异氰酸酯、氢化二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯中的一种或多种；所述溶剂型聚氨酯的软段为数均分子量为6000～8000的聚己二酸丁二醇酯二醇、聚己二酸乙二醇酯二醇、聚碳酸亚乙酯二醇、聚碳酸亚丙酯二醇中的一种或多种。
6.根据权利要求1所述基于定岛超纤改性制备压电抗菌口罩滤材的方法，其特征在于，步骤(4)中，所述溶剂型聚氨酯为5～10重量份；所述聚偏氟乙烯为5～10重量份；所述N,N-二甲基甲酰胺为100重量份。
7.根据权利要求1所述基于定岛超纤改性制备压电抗菌口罩滤材的方法，其特征在于，步骤(4)中，所述加热的温度为70～90℃，搅拌的时间为2～3h。
8.根据权利要求1所述基于定岛超纤改性制备压电抗菌口罩滤材的方法，其特征在于，步骤(6)中，所述极化的温度为70～100℃，极化的时间为15～45min，极化的电压为3～10kV。
9.权利要求1～8任一所述制备方法得到的压电抗菌口罩滤材。
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