CN111849328A - 一种抗病毒性透湿涂料的制备方法及应用 - Google Patents

一种抗病毒性透湿涂料的制备方法及应用 Download PDF

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CN111849328A
CN111849328A CN202010657689.0A CN202010657689A CN111849328A CN 111849328 A CN111849328 A CN 111849328A CN 202010657689 A CN202010657689 A CN 202010657689A CN 111849328 A CN111849328 A CN 111849328A
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antiviral
polyethyleneimine
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quaternary ammonium
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金伟伟
娄琪超
徐意
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Shaoxing Bailisheng New Material Technology Co ltd
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Abstract

本发明公开了一种抗病毒性透湿涂料的制备方法及在制备抗病毒性透湿膜中应用，包括以下步骤：1)聚乙烯亚胺和卤代烃经过反应得到聚乙烯亚胺季铵盐；2)在水性聚合物中配合聚乙烯亚胺季铵盐和草酸，得到抗病毒性透湿涂料。将抗病毒性透湿涂料附着于多孔基膜后，进行加热处理。多孔基膜作为透湿膜的基材，得到抗病毒性透湿膜。本发明的透湿膜具备抗病毒能力，而且加入季铵盐聚合物对水蒸气透过率的影响不明显，因此本发明的抗病毒透湿膜不仅具有高透湿率的特点，还具有优异的抗病毒性能，有阻隔气溶胶、抑制病毒、水蒸气透过率高的功能，可用于制备医疗防护服。

Description

一种抗病毒性透湿涂料的制备方法及应用
技术领域
本发明涉及抗病毒性透湿材料领域，具体涉及一种抗病毒性透湿涂料的制备方法及在制备抗病毒性透湿膜中应用。
背景技术
随着环境污染的增大，以及人类对自然环境的影响加剧，细菌和病毒的扩散和传播也愈来愈明显。全世界每年死于病毒的人数已超过400万人，严重威胁人类的健康。近年来病毒性传染并如SARS病毒、Ebola病毒、H1N1病毒、NCP病毒等等，均对社会产生严重的影响。
医疗防护服作为抵御病毒的基本物资，保障着医护人员的身体健康。防护服面料以透气膜为隔离层，通过与无纺布复合而成为面料。现有防护服的透气膜主要为聚乙烯薄膜，成本低廉，然而其透湿性较差，穿戴一段时间后就会引起水分冷凝，舒适度较差。同时，该薄膜的强度较低，较易撕裂，存在潜在的安全隐患。而热塑性聚氨酯薄膜具有较高的透湿率，可以明显提高面料的舒适性。
然而以聚乙烯薄膜、热塑性聚氨酯薄膜为代表的高性能防护服材料并不具备抗病毒效果，病毒可以沉积在防护服表面，在更换防护服时存在间接传染的可能性。因此，发明一种抗病毒、高透湿的隔离材料具有很大的意义。
发明内容
本发明的目的在于，提供了一种抗病毒性透湿涂料的制备方法及在制备抗病毒性透湿膜中应用，该涂料能够形成耐水性优异的抗病毒性透湿膜。
以下说明本发明的要点。
一种抗病毒性透湿涂料的制备方法，包括以下步骤：
1)聚乙烯亚胺和卤代烃经过反应得到聚乙烯亚胺季铵盐；
2)在水性聚合物中配合聚乙烯亚胺季铵盐和草酸，得到抗病毒性透湿涂料。
本发明中通过在水性聚合物中配合聚乙烯亚胺季铵盐和草酸而成，所述水性聚合物与所述聚乙烯亚胺季铵盐的固体成分重量比为1：0.01～0.2。所述的水性聚合物具有较高的亲水性，可以提供良好的透湿性。所述的聚乙烯亚胺季铵盐为多链季铵盐，具有极高的抗病毒性，可以在短时间内杀灭病毒。所述的草酸可以与聚乙烯亚胺季铵盐形成大分子复合物，能够显著减少聚乙烯亚胺季铵盐在水中的溶出，实现长期的抗病毒功效。
步骤1)中，所述的聚乙烯亚胺的数均分子量为3000～100000。
所述的卤代是具有碳原子数为4～12的溴代烃或碘代烃。所述的卤代烃为溴丁烷、溴己烷、溴辛烷、碘丁烷中的一种或两种以上(包括两种)；
步骤1)中，聚乙烯亚胺和卤代烃经过反应得到聚乙烯亚胺季铵盐，具体包括以下步骤：
在保护性气体下，将聚乙烯亚胺、卤代烃、碳酸钾加入到乙醇中，搅拌加热回流，冷却后过滤去除固体，并将滤液去除挥发物，得到聚乙烯亚胺季铵盐。
所述的保护性气体采用氮气保护
所述的聚乙烯亚胺、卤代烃、碳酸钾的重量比为5～15：5～40：5～15，最优选为10：10～20：10。
70℃～90℃搅拌加热回流6～10h，最优选的，80℃搅拌加热回流8h。
将滤液在100℃～120下去除挥发物，最优选的，将滤液在110℃下去除挥发物.
步骤2)中，所述的水性聚合物经水性异氰酸酯交联而成，所述水性聚合物与水性异氰酸酯的固体成分重量比为1：0.05～0.2。未交联的水性聚合物使用时易被水溶解，而异氰酸酯交联则会提高材料的稳定性，长期保持高透湿性。所述的水性聚合物优选为聚乙烯醇、聚氨酯乳液、羟乙基纤维素、羟丙基纤维素中的一种或两种以上(包括两种)。所述的水性聚合物优选为聚乙烯醇，进一步优选聚合度为1700～2500、水解度为88～99％的聚乙烯醇。
所述的聚乙烯亚胺季铵盐以聚乙烯亚胺和卤代烃合成而成，所述聚乙烯亚胺与卤代烃的重量比为1：0.05～0.2。
将水性聚合物溶解在水中，冷却后，再加入异氰酸酯、聚乙烯亚胺季铵盐和草酸，搅拌均匀并真空脱泡，得到抗病毒性透湿涂料
在水性聚合物中配合聚乙烯亚胺季铵盐和草酸，得到抗病毒性透湿涂料，具体包括：
将水性聚合物溶解在水中，冷却后，再加入异氰酸酯、聚乙烯亚胺季铵盐和草酸，搅拌均匀并真空脱泡，得到抗病毒性透湿涂料。
所述的水性聚合物、水、异氰酸酯、聚乙烯亚胺季铵盐、草酸的用量之比为2～15g：70～120mL：5～20g：0.3～3g：0.3～3g，最优选为5～10g：90～95ml：10g：1g：1g。
所述的抗病毒性透湿涂料在制备抗病毒性透湿膜中的应用，抗病毒性透湿膜的形成方法，将所述的抗病毒性透湿涂料附着于多孔基膜后，进行加热处理。多孔基膜作为透湿膜的基材，不仅提供多孔基材，而且提供相应的力学性能。优选高强度的湿法聚乙烯薄膜。
一种抗病毒性透湿膜，其由所述的抗病毒性透湿膜的形成方法形成。
最优选的，一种抗病毒性透湿膜的制备方法，包括以下步骤：
1)在氮气保护下，将聚乙烯亚胺、碘丁烷、溴辛烷、碳酸钾加入到乙醇中，80℃搅拌加热回流8h。，冷却后过滤去除固体，并在氮气保护下，将滤液在110℃下负压去除挥发物，得到聚乙烯亚胺季铵盐；
所述的聚乙烯亚胺的数均分子量为25000；
所述的聚乙烯亚胺、碘丁烷、溴辛烷、碳酸钾的重量比为10：10：10：10；
2)将聚氨酯乳液添加到水中，冷却，再加入异氰酸酯、聚乙烯亚胺季铵盐和草酸，搅拌均匀并真空脱泡，得到抗病毒透湿涂料；将该抗病毒透湿涂料以40um的厚度涂布到聚丙烯微孔膜上，并通过60℃的烘箱干燥1min，得到抗病毒性透湿膜；
所述的聚氨酯乳液、水、异氰酸酯、聚乙烯亚胺季铵盐、草酸的用量之比为10g：90ml：10g：1g：1g。
该最优方案得到的抗病毒性透湿膜的水蒸气透过率g/(24h·m2)为18654.1，平均病毒灭活对数值为4.17，不仅具有高透湿率的特点，还具有优异的抗病毒性能。
与现有技术相比，本发明具有如下优点：
根据本发明，抗病毒性透湿涂料中的季铵盐与水***联聚合物之间具有氢键，从而防止季铵盐在水中溶出。因此，能够防止由于季铵盐的溶出而导致抗病毒性下降。
本发明的透湿膜具备抗病毒能力，而且加入季铵盐聚合物对水蒸气透过率的影响不明显，因此本发明的抗病毒透湿膜不仅具有高透湿率的特点，还具有优异的抗病毒性能。
本发明将该抗病毒性透湿涂料涂布到多孔基膜上，可得到致密的抗病毒性透湿膜，具有阻隔气溶胶、抑制病毒、水蒸气透过率高的功能，可用于制备医疗防护服。
具体实施方式
以下详细说明本发明的实施方式。
本发明的抗病毒性透湿涂料以高透湿性聚合物结合抗病毒组分设计而成。由于透湿膜直接接触水分，因此需要避免透湿聚合物和抗病毒组分的溶解。本发明采用经水性异氰酸酯交联的水性聚合物为成膜物质，并以聚乙烯亚胺季铵盐为抗病毒组分，从而兼顾致密性、透湿性、抗病毒性的平衡。
本发明的抗病毒性涂膜的形成方法中，使本发明的抗病毒性透湿涂料附着于多孔基膜之后，进行加热处理来形成抗病毒性涂膜。
以下，列举实施例来更具体地说明本发明。
实施例1
在氮气保护下，将10g聚乙烯亚胺(德国巴斯夫BASF lupasol WF，数均分子量为25000)、10g溴丁烷、10g碳酸钾加入到乙醇中，80℃搅拌加热回流8h。冷却后过滤去除固体，并在氮气保护下将滤液在110℃下去除挥发物，得到聚乙烯亚胺季铵盐A。
将5g聚乙烯醇1799溶解在95ml的热水中，冷却至室温25℃，再加入10g异氰酸酯、1g聚乙烯亚胺季铵盐A和1g草酸，搅拌均匀并真空脱泡，得到本发明的抗病毒透湿涂料。将该抗病毒透湿涂料以30um的厚度涂布到PET无纺布上，并通过60℃的烘箱干燥1min，得到本发明的抗病毒透湿膜。
实施例2
在氮气保护下，将10g聚乙烯亚胺(德国巴斯夫BASF lupasol WF，数均分子量为25000)、10g溴丁烷、10g溴己烷、10g碳酸钾加入到乙醇中，80℃搅拌加热回流8h。冷却后过滤去除固体，并在氮气保护下，将滤液在110℃下负压去除挥发物，得到聚乙烯亚胺季铵盐B。
将10g聚氨酯乳液(安徽安大华泰，AH1618)添加到90ml的水中，冷却至室温，再加入10g异氰酸酯、1g聚乙烯亚胺季铵盐和1g草酸，搅拌均匀并真空脱泡，得到本发明的抗病毒透湿涂料。将该抗病毒透湿涂料以30um的厚度涂布到PET无纺布上，并通过60℃的烘箱干燥1min，得到本发明的抗病毒透湿膜。
实施例3
在氮气保护下，将10g聚乙烯亚胺(德国巴斯夫BASF lupasol WF，数均分子量为25000)、10g溴丁烷、10g溴辛烷、10g碳酸钾加入到乙醇中，80℃搅拌加热回流8h。冷却后过滤去除固体，并在氮气保护下将滤液在110℃负压下去除挥发物，得到聚乙烯亚胺季铵盐C。
将5g羟乙基纤维素(山东创耀，HEC-60000)分散在95ml的水中，并用少量氨水完全溶解，再加入10g异氰酸酯、1g聚乙烯亚胺季铵盐和1g草酸，搅拌均匀并真空脱泡，得到本发明的抗病毒透湿涂料。将该抗病毒透湿涂料以20um的厚度涂布到PP无纺布上，并通过60℃的烘箱干燥1min，得到本发明的抗病毒透湿膜。
实施例4
在氮气保护下，将10g聚乙烯亚胺(德国巴斯夫BASF lupasol WF，数均分子量为25000)、10g溴己烷、10g溴辛烷、10g碳酸钾加入到乙醇中，80℃搅拌加热回流8h。冷却后过滤去除固体，并在氮气保护下，将滤液在110℃下负压去除挥发物，得到聚乙烯亚胺季铵盐D。
将5g羟丙基纤维素(肥城雨田化工)溶解在95ml的水中，再加入10g异氰酸酯、1g聚乙烯亚胺季铵盐D和1g草酸，搅拌均匀并真空脱泡，得到本发明的抗病毒透湿涂料。将该抗病毒透湿涂料以20um的厚度涂布到PE微孔膜上，并通过60℃的烘箱干燥1min，得到本发明的抗病毒透湿膜。
实施例5
在氮气保护下，将10g聚乙烯亚胺(德国巴斯夫BASF lupasol WF，数均分子量为25000)、10g碘丁烷、10g溴辛烷、10g碳酸钾加入到乙醇中，80℃搅拌加热回流8h。冷却后过滤去除固体，并在氮气保护下，将滤液在110℃下负压去除挥发物，得到聚乙烯亚胺季铵盐E。
将10g聚氨酯乳液(安徽安大华泰，AH1618)添加到90ml的水中，冷却至室温，再加入10g异氰酸酯、1g聚乙烯亚胺季铵盐E和1g草酸，搅拌均匀并真空脱泡，得到本发明的抗病毒透湿涂料。将该抗病毒透湿涂料以40um的厚度涂布到PP微孔膜上，并通过60℃的烘箱干燥1min，得到本发明的抗病毒透湿膜。
对比例1
将10g聚氨酯乳液添加到90ml的水中，冷却至室温，再加入10g异氰酸酯，搅拌均匀并真空脱泡，得到透湿涂料。将该透湿涂料以30um的厚度涂布到PET无纺布上，并通过60℃的烘箱干燥1min，得到抗病毒透湿膜。
需说明的是，对于以下的实施例和比较例，采用《ISO 18184-2014抗病毒纺织品测试》评价本发明对冠状病毒HCoV-229E的抗病毒性，采用《GB/T 12704.2-2009纺织品织物透湿性试验方法第2部分：蒸发法》的方法B评价本发明的透湿性。
表1抗病毒透湿膜的水蒸气透过率测试结果
水蒸气透过率g/(24h·m<sup>2</sup>)
实施例1 18651.3
实施例2 17824.6
实施例3 16918.3
实施例4 18683.4
实施例5 18654.1
对比例2 16607.7
表2抗病毒透湿膜的冠状病毒HCoV-229E的杀灭作用和杀灭负对数值
Figure BDA0002577336610000071
注：三次实验的平均灭活对数值≥4，可判断对病毒有灭活作用。
结论：与对比例1相比，实施例1-5的透湿膜具备抗病毒能力，而且加入季铵盐聚合物对水蒸气透过率的影响不明显，因此可以本发明的抗病毒透湿膜不仅具有高透湿率的特点，还具有优异的抗病毒性能。

Claims (10)

1.一种抗病毒性透湿涂料的制备方法，其特征在于，包括以下步骤：
1)聚乙烯亚胺和卤代烃经过反应得到聚乙烯亚胺季铵盐；
2)在水性聚合物中配合聚乙烯亚胺季铵盐和草酸，得到抗病毒性透湿涂料。
2.根据权利要求1所述的抗病毒性透湿涂料的制备方法，其特征在于，步骤1)中，所述的聚乙烯亚胺的数均分子量为3000～100000。
3.根据权利要求1所述的抗病毒性透湿涂料的制备方法，其特征在于，步骤1)中，所述的卤代是具有碳原子数为4～12的溴代烃或碘代烃。
4.根据权利要求1所述的抗病毒性透湿涂料的制备方法，其特征在于，步骤1)中，聚乙烯亚胺和卤代烃经过反应得到聚乙烯亚胺季铵盐，具体包括：
在保护性气体下，将聚乙烯亚胺、卤代烃、碳酸钾加入到乙醇中，搅拌加热回流，冷却后过滤去除固体，并将滤液去除挥发物，得到聚乙烯亚胺季铵盐。
5.根据权利要求4所述的抗病毒性透湿涂料的制备方法，其特征在于，所述的聚乙烯亚胺、卤代烃、碳酸钾的重量比为5～15：5～40：5～15。
6.根据权利要求4所述的抗病毒性透湿涂料的制备方法，其特征在于，70℃～90℃搅拌加热回流6～10h；
将滤液在100℃～120下去除挥发物。
7.根据权利要求1所述的抗病毒性透湿涂料的制备方法，其特征在于，步骤2)中，在水性聚合物中配合聚乙烯亚胺季铵盐和草酸，得到抗病毒性透湿涂料，具体包括：
将水性聚合物溶解在水中，冷却后，再加入异氰酸酯、聚乙烯亚胺季铵盐和草酸，搅拌均匀并真空脱泡，得到抗病毒性透湿涂料。
8.根据权利要求7所述的抗病毒性透湿涂料的制备方法，其特征在于，所述的水性聚合物、水、异氰酸酯、聚乙烯亚胺季铵盐、草酸的用量之比为2～15g：70～120mL：5～20g：0.3～3g：0.3～3g。
9.根据权利要求1～8任一项所述的抗病毒性透湿膜在制备抗病毒性透湿膜中的应用。
10.根据权利要求9所述的应用，其特征在于，具体包括：将所述的抗病毒性透湿涂料附着于多孔基膜后，进行加热处理，得到抗病毒性透湿膜。
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