CN111869951A - 一种口罩过滤层的制备方法 - Google Patents

一种口罩过滤层的制备方法 Download PDF

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CN111869951A
CN111869951A CN202010579504.9A CN202010579504A CN111869951A CN 111869951 A CN111869951 A CN 111869951A CN 202010579504 A CN202010579504 A CN 202010579504A CN 111869951 A CN111869951 A CN 111869951A
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mask
trfe
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spraying
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CN111869951B (zh
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汤玉斐
邢国鑫
刘照伟
赵康
郑婉星
康玲
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Shanxi Jie Kanghui Medical Equipment Co ltd
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Xian University of Technology
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Abstract

本发明公开了一种口罩过滤层的制备方法，具体按照以下步骤实施：步骤1、静电纺丝制备P(VDF‑TrFE)高压电纤维膜；步骤2、对步骤1得到的P(VDF‑TrFE)高压电纤维膜采用双喷法进行改性处理，得到改性纤维毡；步骤3、将步骤2得到的改性纤维毡进行热固化处理；步骤4、将步骤3热固化处理后的改性纤维毡进行浸泡制孔及无害化处理，得到可重复使用的自供电口罩高效过滤层，解决了现有技术中存在的口罩过滤效果差的问题。

Description

一种口罩过滤层的制备方法
技术领域
本发明属于复合纤维制备技术领域，涉及一种口罩过滤层的制备方法。
背景技术
流行病(流感、新型冠状肺炎等)传染的机理主要是通过飞沫来传播病毒。病人喷出的飞沫中的大颗粒一般很快可以落地，而含有小于100纳米病毒的细小喷沫易形成气溶胶，在空气中随流漂移，极容易被他人吸入呼吸系统或经碰触到粘膜而被传染。口罩过滤的原理主要是利用静电吸附以及纤维排列后对超细颗粒和飞沫的阻隔。但在传统熔喷布口罩使用过程中，细菌病毒在静电层的沉积以及哈气(水汽)等会导致荷电层静电的消除，损伤其过滤效果。现有的口罩过滤层存在过滤效果较差、寿命短、质量大、能耗高等缺点。
中国专利《一种多层口罩》(申请号：202020612909.3，申请公布号：CN 210611090U，公布日：2020.05.26)提出一种多层口罩，其主体由外到内依次为第一无纺布层、熔喷布过滤层、第二无纺布层、亲肤棉层，可以改善长时间使用过程中熔喷布过滤层的受潮问题，利于熔喷布过滤层长时间使用中保持阻隔性能，也能保证使用的舒适度。但其未能充分利用静电吸附作用，隔离效果不高，且不能循环使用。
中国专利《一种可循环使用的防护型口罩》(申请号：202010212588.2，申请公布号：CN 111202286 A，公布日：2020.05.29)设计了一种可循环使用的防护型口罩，其中间层采用膨体高分子量四氟乙烯共聚分散树脂的微孔材料，其孔径<75纳米，对粒径为75纳米的细小颗粒的过滤性能超过95％，能够用于新冠肺炎病原体病毒的防护。虽然这种口罩可以重复使用，但中间层的过滤完全依赖于孔径，只能利用机械阻隔作用，过滤效果较差。
中国专利《充电式加热口罩及其加工方法》(申请号：202010180203.9，申请公布号：CN 111213933 A，公布日：2020.06.02)设计了一种加热口罩，通过在两层口罩层集成加热结构，并与现有医用口罩配合使用，供电后实现对医用口罩的加热，既保证佩戴温度适宜，还可以避免破坏医用口罩内的静电荷，提高病毒吸附力。此外，摘下口罩将温度调至56℃至60℃左右加热30分钟，可以彻底杀灭病毒，循环再用。但其存在质量大、能耗高、佩戴不方便的问题。
中国专利《一种电化学口罩》(申请号：202010183610.5，申请公布号：CN111109719 A，公布日：2020.05.08)提出一种多层口罩，其主体由外到内依次为外表层、中间过滤层和电化学膜电极层，可以吸收呼吸蒸汽中的水分，并通过电化学膜电极层将其电解为氧气和氢气，解决了口罩佩戴过程中呼吸蒸汽引起口罩失效的问题；同时，氧气回供人体，为口罩佩戴者增氧。但存在质量大、能耗高、佩戴不方便以及过滤效果差的问题。
发明内容
本发明的目的是提供一种口罩过滤层的制备方法，解决了现有技术中存在的口罩过滤效果差的问题。
本发明所采用的技术方案是，一种口罩过滤层的制备方法，具体按照以下步骤实施：
步骤1、静电纺丝制备P(VDF-TrFE)高压电纤维膜；
步骤2、对步骤1得到的P(VDF-TrFE)高压电纤维膜采用双喷法进行改性处理，得到改性纤维毡；
步骤3、将步骤2得到的改性纤维毡进行热固化处理；
步骤4、将步骤3热固化处理后的改性纤维毡进行浸泡制孔及无害化处理，得到可重复使用的自供电口罩高效过滤层。
本发明的特点还在于：
步骤1具体按照以下实施：将P(VDF-TrFE)、水溶性聚合物、无机填料和溶剂混合成的均匀纺丝液置入推进泵中，进行静电纺丝以获得P(VDF-TrFE)高压电纤维膜。
步骤1中，静电纺丝参数为：纺丝电压为18～22kv，接收距离为15cm～18cm，纺丝温度在20℃～30℃，湿度在10％～30％，推进泵推进速度为0.3mL/h～0.5mL/h，每张纤维膜纺丝时间为2～3h。
步骤1中纺丝液按质量百分比的物质组成为，P(VDF-TrFE)为17％～20％，水溶性聚合物为8％～10％，无机填料为1％～5％，溶剂65％～74％，以上组分质量总和为100％，水溶性聚合物为聚乙烯吡咯烷酮、聚乙烯醇等中的任意一种，无机填料为MWCNTs、ZnO、BaTiO3、BiFeO3等中的任意一种，溶剂为二甲基甲酰胺(DMF)、二甲基乙酰胺(DMAc)、N-甲基吡咯烷酮(NMP)、丙酮、二甲基亚砜、四氢呋喃等中的任意一种或多种。
步骤2具体按照以下实施，将步骤1得到的P(VDF-TrFE)高压电纤维膜垂直固定在两个喷涂喷笔之间，进行由聚乙烯亚胺(PEI)、光催化颗粒、粘结剂、氧化剂、溶剂组成的混合溶液的双向喷涂，得到改性纤维毡。
步骤2中，喷涂喷笔的驱动气体为氮气或氩气，气压为0.2～0.3MPa，喷涂距离为5～8cm，喷涂浓度为0.3～1.0mL/cm2。
步骤2中混合溶液按质量百分比的物质组成为：聚乙烯亚胺(PEI)为1.5％～3％，粘接剂为0.5～2％，光催化颗粒为7％～15％，氧化剂为1％～2％，溶剂为78％～90％，以上组分总和为100％，粘接剂为多巴胺、单宁酸、(3-胆丙基)三甲氧基硅烷、没食子酸等中的一种或两种，光催化颗粒为纳米TiO2、ZnO、CdS中的任意一种或多种，氧化剂为过硫酸铵、高碘酸钠、过氧化氢、硫酸铜等中的任意一种或多种，溶剂为三(羟甲基)氨基甲烷(Tris-HCl)、去离子水、乙酸、无水乙醇中的任意一种或多种。混合溶液pH为7.8～8.5。
步骤3具体按照以下实施，将步骤2得到的改性纤维毡在烘箱中热固化处理后，冷却至室温。
步骤3中的热固化处理温度为70～90℃，热固化时间为1～3h。
步骤4具体按照以下实施，将步骤3热固化处理后的改性纤维毡浸泡在足量的去离子水和乙醇混合溶液中，充分振荡清洗后干燥，得到可重复使用的自供电口罩高效过滤层，其中去离子水和乙醇体积比为3:1，浸泡时间为0.5～1d，干燥温度为50～70℃，干燥时间为2～4h。
本发明的有益效果是：本发明的目的是提供一种口罩过滤层的制备方法，解决了现有口罩过滤效果较差、寿命短、能耗高的问题，结合简单的静电纺丝和双喷涂工艺能得到纤维直径小、柔韧性好、压电性能优异的改性多孔纤维毡，其对细菌病毒有良好的机械阻隔能力，在人呼吸(微小风压)下就能持续产生优异的压电效应，达到自供电效果，充分发挥静电吸附作用，并协同PEI的荷正电性能，高效吸附负电性细菌病毒，大大提高过滤效果；多孔结构能增加纤维的比表面积，增强吸附能力，也能在保证致密度的前提下减小呼吸阻力；此外，在使用完口罩后，可经由紫外灯照射，利用光催化剂颗粒的光催化氧化能力达到杀菌消毒的效果，实现可循环使用。
附图说明
图1是本发明一种口罩过滤层的制备方法的过滤层及单根纤维形貌示意图。
图中，1.P(VDF-TrFE)纤维，2.孔洞，3.光催化剂颗粒，4.粘结剂颗粒及其上接枝的PEI。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。
本发明一种口罩过滤层的制备方法，具体按照以下步骤实施：
步骤1、静电纺丝制备P(VDF-TrFE)高压电纤维膜；
步骤1具体按照以下实施：将P(VDF-TrFE)、水溶性聚合物、无机填料和溶剂混合成的均匀纺丝液置入推进泵中，进行静电纺丝以获得P(VDF-TrFE)高压电纤维膜。
步骤1中，静电纺丝参数为：纺丝电压为18～22kv，接收距离为15cm～18cm，纺丝温度在20℃～30℃，湿度在10％～30％，推进泵推进速度为0.3mL/h～0.5mL/h，每张纤维膜纺丝时间为2～3h。
步骤1中纺丝液按质量百分比的物质组成为，P(VDF-TrFE)为17％～20％，水溶性聚合物为8％～10％，无机填料为1％～5％，溶剂65％～74％，以上组分质量总和为100％，水溶性聚合物为聚乙烯吡咯烷酮、聚乙烯醇等中的任意一种，无机填料为MWCNTs、ZnO、BaTiO3、BiFeO3等中的任意一种，溶剂为二甲基甲酰胺(DMF)、二甲基乙酰胺(DMAc)、N-甲基吡咯烷酮(NMP)、丙酮、二甲基亚砜、四氢呋喃等中的任意一种或多种。
步骤2、对步骤1得到的P(VDF-TrFE)高压电纤维膜采用双喷法进行改性处理，得到改性纤维毡；
步骤2具体按照以下实施，将步骤1得到的P(VDF-TrFE)高压电纤维膜垂直固定在两个喷涂喷笔之间，进行由聚乙烯亚胺(PEI)、光催化颗粒、粘结剂、氧化剂、溶剂组成的混合溶液的双向喷涂，得到改性纤维毡。
步骤2中，喷涂喷笔的驱动气体为氮气或氩气，气压为0.2～0.3MPa，喷涂距离为5～8cm，喷涂浓度为0.3～1.0mL/cm2。
步骤2中混合溶液按质量百分比的物质组成为：聚乙烯亚胺(PEI)为1.5％～3％，粘接剂为0.5～2％，光催化颗粒为7％～15％，氧化剂为1％～2％，溶剂为78％～90％，以上组分总和为100％，粘接剂为多巴胺、单宁酸、(3-胆丙基)三甲氧基硅烷、没食子酸等中的一种或两种，光催化颗粒为纳米TiO2、ZnO、CdS中的任意一种或多种，氧化剂为过硫酸铵、高碘酸钠、过氧化氢、硫酸铜等中的任意一种或多种，溶剂为三(羟甲基)氨基甲烷(Tris-HCl)、去离子水、乙酸、无水乙醇中的任意一种或多种。混合溶液pH为7.8～8.5。
步骤3、将步骤2得到的改性纤维毡进行热固化处理；
步骤3具体按照以下实施，将步骤2得到的改性纤维毡在烘箱中热固化处理后，冷却至室温。
步骤3中的热固化处理温度为70～90℃，热固化时间为1～3h。
步骤4、将步骤3热固化处理后的改性纤维毡进行浸泡制孔及无害化处理，得到可重复使用的自供电口罩高效过滤层。
步骤4具体按照以下实施，将步骤3热固化处理后的改性纤维毡浸泡在足量的去离子水和乙醇混合溶液中，充分振荡清洗后干燥，得到可重复使用的自供电口罩高效过滤层，其中去离子水和乙醇体积比为3:1，浸泡时间为0.5～1d，干燥温度为50～70℃，干燥时间为2～4h。
本发明一种口罩过滤层的制备方法通过添加无机纳米填料来降低电纺P(VDF-TrFE)纤维直径、提高纤维的β相含量，从而增强纤维的压电性能，使其在压力下持续产生良好的压电效应，达到自供电效果，充分发挥静电吸附作用；选择合适的纺丝液及电纺时间、电压来保证纤维的小直径和纤维毡的致密性，实现有效机械阻隔细菌病毒的目的；通过选用合适的粘结剂与氧化剂，将聚乙烯亚胺和光催化剂快速牢固负载到纤维毡表面，并以热固化处理来增强结合强度，使纤维毡具有荷正电吸附负电性的细菌病毒和紫外光下杀菌消毒的效果；浸泡制孔及无害化处理可以去除可溶性聚合物，得到多孔结构，达到增强吸附能力和降低呼吸阻力的目的，也能消除制备过程中残留的有害物质及固定不牢固的物质，保证膜通量和安全性。
本发明一种口罩过滤层的制备方法，结合简单的静电纺丝和双喷涂工艺能得到纤维直径小、柔韧性好、压电性能优异的改性多孔纤维毡，其对细菌病毒有良好的机械阻隔能力，在人呼吸(微小风压)下就能持续产生优异的压电效应，达到自供电效果，充分发挥静电吸附作用，并协同PEI的荷正电性能，高效吸附负电性细菌病毒，大大提高过滤效果；多孔结构能增加纤维的比表面积，增强吸附能力，也能在保证致密度的前提下减小呼吸阻力；此外，在使用完口罩后，可经由紫外灯照射，利用光催化剂颗粒的光催化氧化能力达到杀菌消毒的效果，实现可循环使用。本发明在提高口罩过滤效果和使用寿命方面有很好的应用前景。
实施例1
将1.7g P(VDF-TrFE)、0.8g聚乙烯吡咯烷酮、0.1g BaTiO3、5.4g二甲基甲酰胺和2g丙酮混合成的均匀纺丝液置入推进泵中，调节纺丝电压为18kv，接收距离为15cm，纺丝温度为20℃，湿度为30％，推进泵推进速度为0.5mL/h，静电纺丝2h获得P(VDF-TrFE)高压电纤维膜。
将P(VDF-TrFE)纤维膜垂直固定在两个喷涂喷笔之间，在0.2MPa的氮气压力下，保持8cm的喷涂距离和1.0mL/cm2的喷涂浓度，进行由0.15g聚乙烯亚胺、0.05g多巴胺、0.7gTiO2颗粒、0.1g过氧化氢、9g三(羟甲基)氨基甲烷组成的混合溶液(pH＝8.5)的双向喷涂，得到改性纤维毡。
将改性纤维毡在90℃下热固化处理1h，冷却至室温后，浸泡在足量的去离子水和乙醇(体积比为3:1)的混合溶液中1d，充分振荡清洗后在50℃下干燥2h，得到可重复使用的自供电口罩高效过滤层。
实施例2
将2gP(VDF-TrFE)、1g聚乙烯吡咯烷酮、0.5g MWCNTs、5.2g二甲基乙酰胺和1.3g丙酮混合成的均匀纺丝液置入推进泵中，调节纺丝电压为22kv，接收距离为18cm，纺丝温度为30℃，湿度为10％，推进泵推进速度为0.3mL/h，静电纺丝2h获得P(VDF-TrFE)高压电纤维膜。
将P(VDF-TrFE)纤维膜垂直固定在两个喷涂喷笔之间，在0.3MPa的氮气压力下，保持5cm的喷涂距离和0.3mL/cm2的喷涂浓度，进行由0.3g聚乙烯亚胺、0.2g单宁酸、1.5gZnO颗粒、0.2g过硫酸铵、7.8g三(羟甲基)氨基甲烷组成的混合溶液(pH＝7.8)的双向喷涂，得到改性纤维毡。
将改性纤维毡在90℃下热固化处理3h，冷却至室温后，浸泡在足量的去离子水和乙醇(体积比为3:1)的混合溶液中0.5d，充分振荡清洗后在70℃下干燥2h，得到可重复使用的自供电口罩高效过滤层。
实施例3
将1.8g P(VDF-TrFE)、0.9g聚乙烯醇、0.3g ZnO、5.6gN-甲基吡咯烷酮和1.4g二甲基亚砜混合成的均匀纺丝液置入推进泵中，调节纺丝电压为20kv，接收距离为15cm，纺丝温度为30℃，湿度为10％，推进泵推进速度为0.4mL/h，静电纺丝2h获得P(VDF-TrFE)高压电纤维膜。
将P(VDF-TrFE)纤维膜垂直固定在两个喷涂喷笔之间，在0.2MPa的氮气压力下，保持5cm的喷涂距离和0.6mL/cm2的喷涂浓度，进行由0.3g聚乙烯亚胺、0.2g多巴胺、1.5gTiO2颗粒、0.16g过氧化氢、0.04g硫酸铜、7.8g三(羟甲基)氨基甲烷组成的混合溶液(pH＝8.5)的双向喷涂，得到改性纤维毡。
将改性纤维毡在70℃下热固化处理3h，冷却至室温后，浸泡在足量的去离子水和乙醇(体积比为3:1)的混合溶液中1d，充分振荡清洗后在70℃下干燥2h，得到可重复使用的自供电口罩高效过滤层。
实施例4
将2g P(VDF-TrFE)、1g聚乙烯醇、0.4g BiFeO3、5.5g二甲基甲酰胺和1.1g丙酮混合成的均匀纺丝液置入推进泵中，调节纺丝电压为20kv，接收距离为15cm，纺丝温度为30℃，湿度为10％，推进泵推进速度为0.3mL/h，静电纺丝2h获得P(VDF-TrFE)高压电纤维膜。
将P(VDF-TrFE)纤维膜垂直固定在两个喷涂喷笔之间，在0.3MPa的氩气压力下，保持5cm的喷涂距离和0.8mL/cm2的喷涂浓度，进行由0.2g聚乙烯亚胺、0.1g单宁酸、0.1g(3-胆丙基)三甲氧基硅烷、1gTiO2颗粒、0.1g过氧化氢、8.5g三(羟甲基)氨基甲烷组成的混合溶液(pH＝7.8)的双向喷涂，得到改性纤维毡。
将改性纤维毡在80℃下热固化处理2h，冷却至室温后，浸泡在足量的去离子水和乙醇(体积比为3:1)的混合溶液中1d，充分振荡清洗后在70℃下干燥2h，得到可重复使用的自供电口罩高效过滤层。
实施例5
将1.7g P(VDF-TrFE)、0.8g聚乙烯吡咯烷酮、0.1g BaTiO3、5.4g N，N-二甲基甲酰胺与2g四氢呋喃混合成的均匀纺丝液置入推进泵中，调节纺丝电压为20kv，接收距离为15cm，纺丝温度为30℃，湿度为10％，推进泵推进速度为0.5mL/h，静电纺丝3h获得P(VDF-TrFE)高压电纤维膜。
将P(VDF-TrFE)纤维膜垂直固定在两个喷涂喷笔之间，在0.3MPa的氮气压力下，保持8cm的喷涂距离和0.8mL/cm2的喷涂浓度，进行由0.3g聚乙烯亚胺、0.1g多巴胺、0.1g没食子酸、1gTiO2颗粒、0.2g过氧化氢、8.3g三(羟甲基)氨基甲烷组成的混合溶液(pH＝8.5)的双向喷涂，得到改性纤维毡。
将改性纤维毡在90℃下热固化处理1h，冷却至室温后，浸泡在足量的去离子水和乙醇(体积比为3:1)的混合溶液中1d，充分振荡清洗后在50℃下干燥2h，得到可重复使用的自供电口罩高效过滤层。
表1为传统熔喷布过滤层和实施例1～5所得可重复使用的自供电口罩高效过滤层的纤维直径、d33、对负电性达旦黄截留率和使用时长。
Figure BDA0002552642940000101
Figure BDA0002552642940000111
从表中可以看出，传统熔喷布过滤层的直径一般在1～5μm，对负电性达旦黄截留率为95％～97％，且使用寿命较短；而可重复使用的自供电口罩高效过滤层的纤维直径为0.4～0.8μm，机械阻隔效果好，d33在-41～-43pC/N，压电性能优异，对达旦黄截留率可达到98％～99.9％，具有较好的隔离吸附作用，使用寿命也比熔喷布高，此外通过紫外灯照射后可以循环使用。因此，本发明在提高口罩过滤效果和使用寿命方面有很好的应用前景。
图1是本发明一种口罩过滤层的制备方法的过滤层及单根纤维形貌示意图。从图1可以看到，在P(VDF-TrFE)纤维1上分布着许多孔洞2，纤维毡的上下表面区域的纤维上负载有PEI4和光催化剂颗粒3。

Claims (10)

1.一种口罩过滤层的制备方法，其特征在于，具体按照以下步骤实施：
步骤1、静电纺丝制备P(VDF-TrFE)高压电纤维膜；
步骤2、对步骤1得到的P(VDF-TrFE)高压电纤维膜采用双喷法进行改性处理，得到改性纤维毡；
步骤3、将步骤2得到的改性纤维毡进行热固化处理；
步骤4、将步骤3热固化处理后的改性纤维毡进行浸泡制孔及无害化处理，得到可重复使用的自供电口罩高效过滤层。
2.根据权利要求1所述的一种口罩过滤层的制备方法，其特征在于，所述步骤1具体按照以下实施：将P(VDF-TrFE)、水溶性聚合物、无机填料和溶剂混合成的均匀纺丝液置入推进泵中，进行静电纺丝以获得P(VDF-TrFE)高压电纤维膜。
3.根据权利要求2所述的一种口罩过滤层的制备方法，其特征在于，所述步骤1中，静电纺丝参数为：纺丝电压为18～22kv，接收距离为15cm～18cm，纺丝温度在20℃～30℃，湿度在10％～30％，推进泵推进速度为0.3mL/h～0.5mL/h，每张纤维膜纺丝时间为2～3h。
4.根据权利要求2所述的一种口罩过滤层的制备方法，其特征在于，所述步骤1中纺丝液按质量百分比的物质组成为，P(VDF-TrFE)为17％～20％，水溶性聚合物为8％～10％，无机填料为1％～5％，溶剂65％～74％，以上组分质量总和为100％，水溶性聚合物为聚乙烯吡咯烷酮、聚乙烯醇等中的任意一种，无机填料为MWCNTs、ZnO、BaTiO3、BiFeO3等中的任意一种，溶剂为二甲基甲酰胺(DMF)、二甲基乙酰胺(DMAc)、N-甲基吡咯烷酮(NMP)、丙酮、二甲基亚砜、四氢呋喃等中的任意一种或多种。
5.根据权利要求1所述的一种口罩过滤层的制备方法，其特征在于，所述步骤2具体按照以下实施，将步骤1得到的P(VDF-TrFE)高压电纤维膜垂直固定在两个喷涂喷笔之间，进行由聚乙烯亚胺(PEI)、光催化颗粒、粘结剂、氧化剂、溶剂组成的混合溶液的双向喷涂，得到改性纤维毡。
6.根据权利要求5所述的一种口罩过滤层的制备方法，其特征在于，所述步骤2中，所述喷涂喷笔的驱动气体为氮气或氩气，气压为0.2～0.3MPa，喷涂距离为5～8cm，喷涂浓度为0.3～1.0mL/cm2。
7.根据权利要求5所述的一种口罩过滤层的制备方法，其特征在于，所述步骤2中混合溶液按质量百分比的物质组成为：聚乙烯亚胺(PEI)为1.5％～3％，粘接剂为0.5～2％，光催化颗粒为7％～15％，氧化剂为1％～2％，溶剂为78％～90％，以上组分总和为100％，粘接剂为多巴胺、单宁酸、(3-胆丙基)三甲氧基硅烷、没食子酸等中的一种或两种，光催化颗粒为纳米TiO2、ZnO、CdS中的任意一种或多种，氧化剂为过硫酸铵、高碘酸钠、过氧化氢、硫酸铜等中的任意一种或多种，溶剂为三(羟甲基)氨基甲烷(Tris-HCl)、去离子水、乙酸、无水乙醇中的任意一种或多种。混合溶液pH为7.8～8.5。
8.根据权利要求1所述的一种口罩过滤层的制备方法，其特征在于，所述步骤3具体按照以下实施，将步骤2得到的改性纤维毡在烘箱中热固化处理后，冷却至室温。
9.根据权利要求8所述的一种口罩过滤层的制备方法，其特征在于，所述步骤3中的热固化处理温度为70～90℃，热固化时间为1～3h。
10.根据权利要求1所述的一种口罩过滤层的制备方法，其特征在于，所述步骤4具体按照以下实施，将步骤3热固化处理后的改性纤维毡浸泡在足量的去离子水和乙醇混合溶液中，充分振荡清洗后干燥，得到可重复使用的自供电口罩高效过滤层，其中去离子水和乙醇体积比为3:1，浸泡时间为0.5～1d，干燥温度为50～70℃，干燥时间为2～4h。
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