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CN113287812B - 一种抗菌抗病毒可降解口罩及其制备方法 - Google Patents

一种抗菌抗病毒可降解口罩及其制备方法 Download PDF

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Publication number
CN113287812B
CN113287812B CN202110534082.8A CN202110534082A CN113287812B CN 113287812 B CN113287812 B CN 113287812B CN 202110534082 A CN202110534082 A CN 202110534082A CN 113287812 B CN113287812 B CN 113287812B
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Prior art keywords
woven fabric
antiviral
antibacterial
cellulose
reaction
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CN202110534082.8A
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CN113287812A (zh
Inventor
邓超
肖惠宁
勇强
法扎德·塞迪
靳向煜
李程程
魏海英
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Nanjing Forestry University
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Nanjing Forestry University
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Priority to CN202110534082.8A priority Critical patent/CN113287812B/zh
Priority to US18/561,291 priority patent/US12193532B2/en
Priority to PCT/CN2021/097606 priority patent/WO2022241842A1/zh
Publication of CN113287812A publication Critical patent/CN113287812A/zh
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    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
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    • A41—WEARING APPAREL
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    • A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
    • A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
    • A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
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Abstract

一种抗菌抗病毒可降解口罩及其制备方法，由外而内依次分别为面层、芯层和接触面部的里层，所述面层为抗菌抗病毒纤维素水刺无纺布，所述芯层为聚丙烯熔喷无纺布，所述里层为聚丙烯纺粘无纺布或可降解天然棉织物。该口罩能够同时具有抗菌抗病毒的功能，同时材料可降解，能够有效缓解聚丙烯等不可降解石油基纤维材料带来的环境污染压力。

Description

一种抗菌抗病毒可降解口罩及其制备方法
技术领域
本发明涉及纺织技术领域，尤其涉及一种抗菌抗病毒可降解口罩及其制备方法。
背景技术
KN95过滤式口罩、外科口罩等因其能有效吸附过滤细菌和病毒气溶胶颗粒，已成为疫情期间重要的防护用品。然而，口罩由于自身缺乏抗菌和抗病毒活性，使得细菌或病毒在口罩面层存活时间较长(长至7天)，导致其使用寿命较短，需要经常更换并大量处置。另外，目前市场上口罩的加工原材料主要是聚丙烯等石油基材料，由于这类材料的不可降解性，废弃口罩造成了巨大的环境污染。
目前，随着疫情的持续发展以及口罩废弃物的日益增加，开发抗菌抗病毒可降解的功能型口罩成为一种迫切需求。当前有关抗菌抗病毒口罩的研究主要有以下几类：1)采用氯化钠盐对口罩面层进行涂层；2)运用石墨烯沉积技术对口罩面层进行改性；3)将金属纳米颗粒喷涂到口罩面层从而赋予口罩抗菌抗病毒性能；4)采用光敏剂对口罩面层进行化学修饰，使口罩在光照射下产生生物杀灭活性氧，从而提供光诱导的生物杀灭功能。
尽管已有不同的研究方法赋予口罩抗菌、抗病毒性能，但是这些方法可能存在金属离子泄露对人体造成伤害的风险或使用条件受限制，且口罩制备所用原材料没有改变，仍然无法有效解决口罩用即弃造成的环境污染问题。
发明内容
解决的技术问题：本发明提供一种抗菌抗病毒可降解口罩及其制备方法，该口罩能够同时具有抗菌抗病毒的功能，同时材料可降解，能够有效缓解聚丙烯等不可降解石油基纤维材料带来的环境污染压力。
技术方案：一种抗菌抗病毒可降解口罩，所述口罩包括三层结构，由外而内依次分别为面层(1)、芯层(2)和接触面部的里层(3)，所述面层(1)为抗菌抗病毒纤维素水刺无纺布，所述芯层(2)为聚丙烯熔喷无纺布，所述里层(3)为聚丙烯纺粘无纺布或可降解天然棉织物；所述芯层(2)聚丙烯熔喷无纺布，纤维细度为1～3μm，面密度为20～60g/m2；所述里层(3)聚丙烯纺粘无纺布，纤维细度为20～30μm，面密度为20～45g/m2；所述可降解天然棉织物，面密度为20～45 g/m2。
上述面层(1)纤维素水刺无纺布为梳理水刺无纺布或湿法水刺无纺布，其面密度为 20～70g/m2。
上述面层(1)纤维素梳理水刺无纺布由纤维素纤维依次经过开松、梳理、水刺加固成，最后经烘箱烘干制成。
上述纤维素纤维的长度为28～58mm。
上述面层(1)纤维素湿法水刺无纺布由60～80％的木浆纤维与20～40％的纤维素纤维通过打浆混合均匀后，依次经混浆、上浆、湿法成网、水刺加固成型，最后经烘箱烘干制成。
上述木浆纤维的长度为1～5mm，纤维素纤维长度为6～16mm。
上述面层(1)抗菌抗病毒纤维素水刺无纺布的制备包括如下步骤：S1，将环己基异氰酸酯、有机溶剂按照质量比1:(5～10)混合，并加入均相催化剂配制成反应溶液，所述均相催化剂为4-二甲氨基吡啶、三乙胺或二月桂酸二丁基锡，将真空干燥过的纤维素水刺无纺布浸泡于所述反应溶液中，加热0.5～24h进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥； S2，将聚合物、二氧六环有机溶剂按照质量比1:7混合，配制成反应溶液，将步骤S1得到的纤维素水刺无纺布浸泡于所述反应溶液中3-10min，反应结束用乙醇洗涤并干燥，再将上述无纺布正反面经紫外光照固化，单面照射3～10min；S3，将改性胍盐或硫酸新霉素溶于溶剂配制成反应溶液，反应溶液浓度0.01～200mg/mL，酸碱度pH≥7，将步骤S2得到的纤维素水刺无纺布浸泡于所述反应溶液中，在pH≥7的碱性溶液中60～100℃下恒温反应4～24h进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥，制得抗菌抗病毒纤维素水刺无纺布。
优选的，在步骤S1中，所述加热反应的过程为：在60～120℃下恒温反应0.5～24h；步骤 S1中，所述有机溶剂包括N,N-二甲基甲酰胺、乙腈、二氧六环、4-二甲氨基吡啶中的任意一种或至少两种组合；步骤S1中，所述催化剂包括三乙胺、二月桂酸二丁基锡中的任意一种或至少两种组合。
在步骤S2中，所述聚合物的结构为：
Figure BDA0003069068200000031
其中m＝1-5，n＝10-80；所述聚合物通过单体TMA和BPEMA按摩尔比95:5混合后，在引发剂偶氮二异丁腈作用下聚合而成，具体制备如下：将TMA和BPEMA溶于二氧六环并装入圆底烧瓶，同时加入偶氮二异丁腈引发剂，在氮气保护，80℃条件下聚合反应8h，反应结束用己烷将聚合物洗出并干燥，单体TMA和BPEMA的结构式如下：
TMA：
Figure BDA0003069068200000032
BPEMA：
Figure BDA0003069068200000033
在步骤S3中所述反应溶剂包括去离子水、乙醇、二甲基亚砜中的任意一种或至少两种组合。
上述芯层(2)聚丙烯熔喷无纺布，在风量85L/min条件下，压降≤95Pa，对0.25～0.3μm大小的NaCl颗粒物拦截效率≥99％；在风量32L/min条件下，压降≤35Pa，对0.25～0.3μm大小的NaCl颗粒物拦截效率≥95％。
有益效果：(1)本发明所提供的口罩为三层结构，其中面层采用改性胍盐或硫酸新霉素接枝共聚的抗菌抗病毒纤维素无纺布，利用改性胍盐或硫酸新霉素的快速抗菌抗病毒特性，将经呼吸等从外环境在口罩面层上滞留的病毒或细菌迅速灭活，从而防止病毒或细菌微生物穿过口罩进入人体造成危害，同时防止人手触碰引起的交叉感染，可避免对环境造成二次污染。此外，口罩面层的可降解性能够有效缓解聚丙烯等不可降解石油基纤维材料带来的环境污染压力。芯层采用高效低阻的聚丙烯熔喷无纺布，能够通过其静电吸附作用等有效拦截吸附 PM2.5颗粒物及细菌病毒等微生物，形成第二道防护屏障。里层采用具有亲肤特性的聚丙烯纺粘无纺布或可降解天然棉织物，以增加实际佩戴口罩过程中的舒适性及贴合性。采用可降解的面层和里层，保证了大部分口罩材料的可降解性，从而进一步减少环境污染。本发明的重点在面层的功能化制备。
(2)本发明采用改性胍盐和硫酸新霉素作为抗菌抗病毒活性因子，改性胍盐具有较强的抗菌抗病毒性能、低细胞毒性和高生物相容性，广泛应用于医药、包装、食品和农业等领域；硫酸新霉素是一种水溶性氨基糖苷类抗生素，对革兰氏阳性和阴性菌株均表现出有效的抗菌活性，且具有一定的抗病毒特性，它可以抑制病毒RNA的复制和翻译从而使病毒失活。通过将改性胍盐或硫酸新霉素共价接枝在纤维素水刺无纺布表面，能够避免石墨烯、金属离子等抗菌剂改性的口罩在使用过程中因泄露或迁移对人体造成伤害的风险，同时能够使口罩具有高效持久的抗菌抗病毒特性、防尘防雾霾作用，有效灭活病原微生物，因此能够有效预防 HCoV-229E、SARS-CoV-2等冠状病毒的传播感染。
(3)本发明所采用的改性胍盐和硫酸新霉素具有广泛的抗菌谱和持久的抗菌活性，具有抗菌效率高、水溶性好且拥有高效抗病毒特性等优点。改性胍盐通过破坏细菌和病毒的细胞膜或衣壳而有效灭活细菌和病毒，从而导致细胞质的渗漏，或干扰病毒基因组含量或结构单元，并导致病毒完全分解。硫酸新霉素附着在细胞壁表面从而使细胞表面的酶失活，随后细胞壁被破坏，硫酸新霉素进入细胞内与DNA结合，从而使生物体失活，以起到杀菌抗病毒作用。
(4)本发明制得的抗菌抗病毒口罩对HCoV-229E的抗病毒活性率高达98.21％，对COVID-19冠状病毒SARS-CoV-2的抗病毒活性率高达99.84％，对革兰氏阴性的大肠杆菌、革兰氏阳性的金黄色葡萄球菌的抑菌率高达99.99％，液滴接触角高达120.9°。
附图说明
图1为本发明提供的抗菌抗病毒口罩各功能层组合示意图；
图2为本发明聚合物氢谱图；
图3为本发明TMA的氢谱图；
图4为本发明BPEMA的氢谱图。
具体实施方式
为了使本发明的目的、技术方案和优点更加清楚明白，以下结合具体实施例对本发明进行进一步详细说明；应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明；除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
另外，还需要说明的是，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。
参照图1，本发明提供一种抗菌抗病毒口罩，所述口罩包括三层结构，由外而内依次分别为面层1、芯层2和接触面部的里层3，所述面层1为抗菌抗病毒纤维素水刺无纺布，所述芯层2为高效低阻的聚丙烯熔喷无纺布，所述里层3为拒水亲肤性的聚丙烯纺粘无纺布或可降解天然棉织物。
所述面层1纤维素水刺无纺布为梳理水刺无纺布或湿法水刺无纺布(浙江宝仁和中科技有限公司)，其面密度为20～70g/m2。
所述面层1纤维素梳理水刺无纺布由纤维素纤维依次经过开松、梳理、水刺加固成，最后经烘箱烘干制成；所述纤维素纤维的长度为28～58mm。
所述面层1纤维素湿法水刺无纺布由60～80％的木浆纤维与20～40％的纤维素纤维通过打浆混合均匀后，依次经混浆、上浆、湿法成网、水刺加固成型，最后经烘箱烘干制成；所述木浆纤维的长度为1～5mm，纤维素纤维长度为6～16mm。
所述面层1抗菌抗病毒纤维素水刺无纺布的制备方法，步骤如下：
S1，将环己基异氰酸酯、有机溶剂混合并加入催化剂配制成反应溶液，将真空干燥过的纤维素水刺无纺布浸泡于所述反应溶液中，加热一定时间进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥；
S2，将聚合物、二氧六环有机溶剂混合配制成反应溶液，将步骤S1得到的纤维素水刺无纺布浸泡于所述反应溶液中一定时间，反应结束用乙醇洗涤并干燥，再将上述无纺布正反面经紫外光照固化一定时间；
S3，将改性胍盐或硫酸新霉素溶于不同的溶剂配制成不同浓度的反应溶液，将步骤S2 得到的纤维素水刺无纺布浸泡于所述反应溶液中，在不同的酸碱性溶液中加热一定时间进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥，制得抗菌抗病毒纤维素水刺无纺布。
优选地，在步骤S1中，所述加热反应的过程为：在60～120℃下恒温反应0.5～24h。
优选地，步骤S1中，所述有机溶剂包括N,N-二甲基甲酰胺、乙腈、二氧六环、4-二甲氨基吡啶中的任意一种或至少两种组合；
优选地，步骤S1中，所述催化剂包括三乙胺、二月桂酸二丁基锡中的任意一种或至少两种组合。
优选地，在步骤S2中，所述聚合物的结构为：
Figure BDA0003069068200000061
其中m＝1-5，n＝10-80；
优选地，在步骤S2中，浸泡时间为3-10min，所述紫外光照固化时间为单面3～10min。
优选地，在步骤S3中，所述反应过程为：在反应溶液浓度2～200mg/mL，酸碱度pH6-10， 60～100℃下恒温反应4～24h。
优选地，步骤S3中，所述反应溶剂包括去离子水、乙醇、二甲基亚砜中的任意一种或至少两种组合。
所述芯层2高效低阻聚丙烯熔喷无纺布(宣城广能非织造有限公司)，纤维细度为1～3μm，面密度为20～60g/m2；在风量85L/min条件下，压降≤95Pa，对0.25～0.3μm大小的NaCl颗粒物拦截效率≥99％；在风量32L/min条件下，压降≤35Pa，对0.25～0.3μm大小的NaCl颗粒物拦截效率≥95％。
所述里层3聚丙烯纺粘无纺布(东华大学制备)，纤维细度为20～30μm，面密度为20～45g/m2。
以下具体实施方式中，按照ISO 18184:2019标准通过病毒滴度TCID50测试对制得的抗菌抗病毒口罩的抗病毒性能进行测试。
下面通过具体的实施例子并结合附图对本发明做进一步的详细描述。
实施例1
参照图1，本实施例提供一种抗菌抗病毒口罩，所述口罩包括三层结构，由外而内依次分别为面层1、芯层2和接触面部的里层3，所述面层1为抗菌抗病毒纤维素湿法水刺无纺布，所述芯层2为高效低阻的聚丙烯熔喷无纺布，所述里层3为拒水亲肤性的聚丙烯纺粘无纺布或可降解天然棉织物。
所述面层1纤维素湿法水刺无纺布的面密度为60g/m2，由75％的木浆纤维与25％的纤维素纤维通过打浆混合均匀后，依次经混浆、上浆、湿法成网、水刺加固成型，最后经烘箱烘干制成；所述木浆纤维的长度为2～4mm，纤维素纤维长度为12mm。
所述面层1抗菌抗病毒纤维素湿法水刺无纺布的制备方法，步骤如下：
S1，将4mL环己基异氰酸酯、20mL的N,N-二甲基甲酰胺混合并加入50μL二月桂酸二丁基锡配制成反应溶液，将真空干燥过的纤维素湿法水刺无纺布浸泡于所述反应溶液中，100℃条件下恒温反应1h进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥；
S2，将210mg聚合物、30mL二氧六环有机溶剂混合配制成反应溶液，将步骤S1得到的纤维素湿法水刺无纺布浸泡于所述反应溶液中5min，反应结束用乙醇洗涤并干燥，再将上述无纺布经紫外光照固化，正反面各5min；
S3，将改性胍盐溶于去离子水配制成浓度为200mg/mL的反应溶液，将步骤S2得到的纤维素湿法水刺无纺布浸泡于所述反应溶液中，在pH>7的溶液中80℃条件下恒温反应24h进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥，制得抗菌抗病毒纤维素湿法水刺无纺布。
在步骤S2中，所述聚合物的结构为：
Figure BDA0003069068200000071
其中m＝1，n＝14；所述聚合物通过单体TMA和BPEMA按摩尔比95:5混合后，在引发剂偶氮二异丁腈作用下聚合而成，具体制备如下：将TMA和BPEMA溶于二氧六环并装入圆底烧瓶，同时加入偶氮二异丁腈引发剂，在氮气保护，80℃条件下聚合反应8h，反应结束用己烷将聚合物洗出并干燥，测得的氢谱结构如图2所示。
所述单体TMA的结构为：
Figure BDA0003069068200000081
制备过程如下：将硫脲和中性氧化铝按摩尔比1:3混合研磨均匀，再将甲基丙烯酸缩水甘油酯以硫脲摩尔质量的二分之一缓慢加入到上述均匀混合物中，再进一步研磨。放置1小时后，用乙酸乙酯将单体TMA洗出，测得的氢谱结构如图3所示。
所述单体BPEMA的结构为：
Figure BDA0003069068200000082
制备过程如下：
i)将4-羟基二苯甲酮和碳酸乙烯酯(摩尔比1:1)，甲苯，碘化钠混合，在100℃条件下加热得到澄清溶液，然后温度升高到180℃，反应持续2h。最后冷却反应，加入100mL甲苯和25mL水提取有机相产物，有机相再水洗两次，用MgSO4干燥，除去溶剂，得到的4-(2- 羟乙氧基)二苯甲酮。
ii)将得到的4-(2-羟乙氧基)二苯甲酮和三乙胺(摩尔比2:3)溶于二氯甲烷中，在氮气环境下冰浴冷却上述反应混合物。然后，将溶于二氯甲烷的甲基丙烯酰氯滴加到上述反应混合物中，反应在室温下持续一整夜，然后转移到分液漏斗中，用冷水，碳酸氢钠水溶液，水洗涤，再用MgSO4干燥，过滤除去溶剂，得到单体BPEMA，测得的氢谱结构如图4所示。
所述芯层2高效低阻聚丙烯熔喷无纺布，纤维细度为2.5μm，面密度为40g/m2；所述里层3 聚丙烯纺粘无纺布，纤维细度为24μm，面密度为25g/m2。
本实施例1制成的抗菌抗病毒口罩对冠状病毒HCoV-229E的抗病毒活性率高达95.96％，对 COVID-19冠状病毒SARS-CoV-2的抗病毒活性率高达99.72％，对大肠杆菌、金黄色葡萄球菌的抑菌率高达99.99％，液滴接触角高达118.7°。
实施例2
本实施例提供一种抗菌抗病毒口罩，与实施例1相比，不同之处在于：步骤S3中将改性胍盐溶于去离子水配制成浓度为100mg/mL的反应溶液，其余与实施例1均相同。
实施例3
本实施例提供一种抗菌抗病毒口罩，与实施例1相比，不同之处在于：步骤S3中将改性胍盐溶于去离子水配制成浓度为25mg/mL的反应溶液，其余与实施例1均相同。
实施例4
本实施例提供一种抗菌抗病毒口罩，与实施例1相比，不同之处在于：步骤S3中将改性胍盐溶于去离子水配制成浓度为5mg/mL的反应溶液，其余与实施例1均相同。
实施例5
本实施例提供一种抗菌抗病毒口罩，与实施例1相比，不同之处在于：所述面层1抗菌抗病毒纤维素湿法水刺无纺布的制备方法，步骤如下：
S1，将4mL环己基异氰酸酯、20mL的N,N-二甲基甲酰胺混合并加入50μL二月桂酸二丁基锡配制成反应溶液，将真空干燥过的纤维素湿法水刺无纺布浸泡于所述反应溶液中，100℃条件下恒温反应1h进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥；
S2，将210mg聚合物、30mL二氧六环有机溶剂混合配制成反应溶液，将步骤S1得到的纤维素湿法水刺无纺布浸泡于所述反应溶液中5min，反应结束用乙醇洗涤并干燥，再将上述无纺布经紫外光照固化，正反面各5min；
S3，将硫酸新霉素溶于去离子水配制成浓度为200mg/mL的反应溶液，将步骤S2得到的纤维素湿法水刺无纺布浸泡于所述反应溶液中，在pH>7的溶液中80℃条件下恒温反应24h 进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥，制得抗菌抗病毒纤维素湿法水刺无纺布。
其余与实施例1均相同。
本实施例制成的抗菌抗病毒口罩对HCoV-229E的抗病毒活性率高达97.85％，对SARS-CoV-2的抗病毒活性率高达99.29％，对大肠杆菌、金黄色葡萄球菌的抑菌率高达99.99％，液滴接触角高达119.6°。
实施例6
本实施例提供一种抗菌抗病毒口罩，与实施例5相比，不同之处在于：步骤S3中将硫酸新霉素溶于去离子水配制成浓度为100mg/mL的反应溶液，其余与实施例5均相同。
实施例7
本实施例提供一种抗菌抗病毒口罩，与实施例5相比，不同之处在于：步骤S3中将硫酸新霉素溶于去离子水配制成浓度为25mg/mL的反应溶液，其余与实施例5均相同。
实施例8
本实施例提供一种抗菌抗病毒口罩，与实施例5相比，不同之处在于：步骤S3中将硫酸新霉素溶于去离子水配制成浓度为5mg/mL的反应溶液，其余与实施例5均相同。
对比例1
本实施例提供一种抗菌抗病毒口罩，与实施例1相比，不同之处在于：所述面层1抗菌抗病毒纤维素湿法水刺无纺布的制备方法，步骤如下：
S1，将210mg聚合物、30mL二氧六环有机溶剂混合配制成反应溶液，将纤维素湿法水刺无纺布浸泡于所述反应溶液中5min，反应结束用乙醇洗涤并干燥，再将上述无纺布经紫外光照固化，正反面各5min；
S2，将改性胍盐溶于去离子水配制成浓度为200mg/mL的反应溶液，将步骤S1得到的纤维素湿法水刺无纺布浸泡于所述反应溶液中，在pH>7的溶液中80℃条件下恒温反应24h进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥，制得抗菌抗病毒纤维素湿法水刺无纺布。
其余与实施例1均相同。
本对比例制成的抗菌抗病毒口罩对HCoV-229E的抗病毒活性率高达96.03％，对SARS-CoV-2的抗病毒活性率高达99.84％，对大肠杆菌、金黄色葡萄球菌的抑菌率高达99.99％，液滴接触角65.4°。
对比例2
本实施例提供一种抗菌抗病毒口罩，与实施例5相比，不同之处在于：所述面层1抗菌抗病毒纤维素湿法水刺无纺布的制备方法，步骤如下：
S1，将210mg聚合物、30mL二氧六环有机溶剂混合配制成反应溶液，将纤维素湿法水刺无纺布浸泡于所述反应溶液中5min，反应结束用乙醇洗涤并干燥，再将上述无纺布经紫外光照固化，正反面各5min；
S2，将硫酸新霉素溶于去离子水配制成浓度为200mg/mL的反应溶液，将步骤S1得到的纤维素湿法水刺无纺布浸泡于所述反应溶液中，在pH>7的溶液中80℃条件下恒温反应24h 进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥，制得抗菌抗病毒纤维素湿法水刺无纺布。
其余与实施例5均相同。
本对比例制成的抗菌抗病毒口罩对HCoV-229E的抗病毒活性率高达98.21％，对SARS-CoV-2的抗病毒活性率高达99.35％，对大肠杆菌、金黄色葡萄球菌的抑菌率高达99.99％，液滴接触角57.5°。
将上述实施例和对比例提供的抗菌抗病毒纤维素湿法水刺无纺布制成的口罩进行抗菌、抗病毒性能及过滤效率测试，结果如表1所示。
表1
Figure BDA0003069068200000111
由表1可知，本发明制备的口罩具有优异的抗菌抗病毒性能，对大肠杆菌和金黄色葡萄球菌的抗菌率高达99.99％，对HCoV-229E的抗病毒活性高达98.21％，对SARS-CoV-2的抗病毒活性高达99.35％，对空气中的PM2.5颗粒过滤效率高达99％；
对比实施例1-4和实施例5-8可以看出，所述实施例采用本发明所述抗菌抗病毒口罩，抗菌抗病毒效果随着改性胍盐或硫酸新霉素的接枝反应浓度增加而增加；
对比实施例1(实施例5)和对比例1(对比例2)可以看出，虽然没有经过疏水改性的抗菌抗病毒口罩抗病毒效果更好一些，但是接触角较小，自清洁性能较差，说明经疏水改性的抗菌抗病毒纤维素湿法水刺无纺布适合作为口罩的面层材料，而未经疏水改性的无纺布可作为口罩的内层材料，从而制备得到的口罩具有优异的抗菌抗病毒性能、过滤效率。
以上所述，仅为本发明的说明实施例，并非对本发明任何形式上和实质上的限制，应当指出，对于本技术领域的普通技术人员，在不脱离本发明方法的前提下，做出的若干改进和补充也应视为本发明的保护范围；凡熟悉本专业的技术人员，在不脱离本发明精神和范围的情况下，利用以上所揭示的技术内容做出的些许更改、修饰与演变的等同变化，均为本发明的等效实施例；同时，凡依据本发明的实质技术对上述实施例所做的任何等同变化的更改、修饰与演变，均仍属于本发明的保护范围。

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1.一种抗菌抗病毒可降解口罩的制备方法，其特征在于，所述口罩包括三层结构，由外而内依次分别为面层(1)、芯层(2)和接触面部的里层(3)，所述面层(1)为抗菌抗病毒纤维素水刺无纺布，所述芯层(2)为聚丙烯熔喷无纺布，所述里层(3)为聚丙烯纺粘无纺布或可降解天然棉织物；所述芯层(2)聚丙烯熔喷无纺布，纤维细度为1~3μm，面密度为20~60g/m2；所述里层(3)聚丙烯纺粘无纺布，纤维细度为20~30μm，面密度为20~45g/m2；所述可降解天然棉织物，面密度为 20~45 g/m2，所述面层(1)抗菌抗病毒纤维素水刺无纺布的制备包括如下步骤：S1，将环己基异氰酸酯、有机溶剂按照质量比1:（5~10）混合，并加入均相催化剂配制成反应溶液，所述均相催化剂为4-二甲氨基吡啶、三乙胺或二月桂酸二丁基锡，将真空干燥过的纤维素水刺无纺布浸泡于所述反应溶液中，加热0.5~24h进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥；S2，将聚合物、二氧六环有机溶剂按照质量比1:7混合，配制成反应溶液，将步骤S1得到的纤维素水刺无纺布浸泡于所述反应溶液中3-10min，反应结束用乙醇洗涤并干燥，再将上述无纺布正反面经紫外光照固化，单面照射3~10min；S3，将改性胍盐或硫酸新霉素溶于溶剂配制成反应溶液，反应溶液浓度0.01~200mg/mL，酸碱度pH≥7，将步骤S2得到的纤维素水刺无纺布浸泡于所述反应溶液中，在pH≥7的碱性溶液中60~100℃下恒温反应4~24h进行共价接枝反应，反应结束用乙醇和去离子水洗涤并干燥，制得抗菌抗病毒纤维素水刺无纺布；在步骤S2中，所述聚合物的结构为：
Figure DEST_PATH_IMAGE002
，其中m=1-5，n=10-80；所述聚合物通过单体TMA和BPEMA按摩尔比95:5混合后，在引发剂偶氮二异丁腈作用下聚合而成，具体制备如下：将TMA和BPEMA溶于二氧六环并装入圆底烧瓶，同时加入偶氮二异丁腈引发剂，在氮气保护，80℃条件下聚合反应8h，反应结束用己烷将聚合物洗出并干燥，单体TMA和BPEMA的结构式如下：
TMA：
Figure DEST_PATH_IMAGE004
BPEMA：
Figure DEST_PATH_IMAGE006
。
2.根据权利要求1所述抗菌抗病毒可降解口罩的制备方法，其特征在于：在步骤S1中，所述加热反应的过程为：在60~120℃下恒温反应0.5~24h；步骤S1中，所述有机溶剂包括N,N-二甲基甲酰胺、乙腈、二氧六环、4-二甲氨基吡啶中的任意一种或至少两种组合；步骤S1中，所述催化剂包括三乙胺、二月桂酸二丁基锡中的任意一种或至少两种组合。
3.根据权利要求1所述抗菌抗病毒可降解口罩的制备方法，其特征在于：在步骤S3中所述反应溶剂包括去离子水、乙醇、二甲基亚砜中的任意一种或至少两种组合。
4.根据权利要求1所述抗菌抗病毒可降解口罩的制备方法，其特征在于：所述面层(1)纤维素水刺无纺布为梳理水刺无纺布或湿法水刺无纺布，其面密度为20~70g/m2。
5.根据权利要求1所述抗菌抗病毒可降解口罩的制备方法，其特征在于：所述面层(1)纤维素梳理水刺无纺布由纤维素纤维依次经过开松、梳理、水刺加固成，最后经烘箱烘干制成。
6.根据权利要求5所述抗菌抗病毒可降解口罩的制备方法，其特征在于：所述纤维素纤维的长度为28~58mm。
7.根据权利要求1所述抗菌抗病毒可降解口罩的制备方法，其特征在于：所述面层(1)纤维素湿法水刺无纺布由60~80%的木浆纤维与20~40%的纤维素纤维通过打浆混合均匀后，依次经混浆、上浆、湿法成网、水刺加固成型，最后经烘箱烘干制成。
8.根据权利要求7所述抗菌抗病毒可降解口罩的制备方法，其特征在于：所述木浆纤维的长度为1~5mm，纤维素纤维长度为6~16mm。
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