CN114635280B - 一种医用抗病毒无纺布及其制备方法和应用 - Google Patents
一种医用抗病毒无纺布及其制备方法和应用 Download PDFInfo
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Abstract
本发明提供一种医用抗病毒无纺布及其制备方法和应用。本发明制备的医用抗病毒无纺布采用化学浸渍法得到,工艺简单,可操作性强,所得产品中陶瓷粉末成分为纳米级、含量可控,分布均匀,且该材料安全无刺激,具有高效防护性能,因而适合在防护用品领域大规模生产,具有良好的应用前景。
Description
技术领域
本发明涉及生活以及医用材料领域,具体涉及一种医用抗病毒无纺布及其制备方法和应用。
背景技术
近些年来,爆发过多起病毒传染病,如SARS、禽流感、甲型H1N1流感、新型冠状病毒肺炎等,多为呼吸道传染病。呼吸道传染病的主要传播途径为飞沫传播和接触性传播,对公众健康和社会稳定带来了严重的威胁。
普通医用口罩过滤层多由单层或多层熔喷无纺布制成,使含有害物的空气通过口罩的过滤层过滤后再被人吸入或者呼出,主要用于医务人员和相关人员对经空气传播的呼吸道传染病的防护,供医疗工作环境下,过滤空气中的颗粒物、阻隔飞沫、血液、体液、分泌物等用。
市面上已有的防护口罩要么防护力低下,尤其不具备针对流行病毒的过滤、防护力,要么制造工艺复杂、成本高昂,要么材料难以降解,环保性差,因此,亟需开发适用于高效过滤病毒的、安全环保的防护材料以及适于大规模生产和广泛应用的防护材料制备工艺。
发明内容
为解决现有技术中存在的问题,本发明提供一种医用抗病毒无纺布的制备方法,其特征在于,包括如下步骤:
步骤一,将锌盐溶于水中,获得溶液A;
步骤二,将铝盐溶于步骤一得到的溶液A,获得混合溶液B;
步骤三,将聚乳酸无纺布浸渍于步骤二得到的混合溶液B;
步骤四,加入碱性溶液;
步骤五,从溶液中取出被浸渍的聚乳酸无纺布,经后处理得到所述医用抗病毒无纺布。
根据本发明的实施方案,
步骤一中所述锌盐为硝酸锌,乙酸锌及其水合物,或葡萄糖酸锌中的一种或多种;步骤二中所述铝盐为硫酸铝,硝酸铝及其水合物中的一种或多种;
步骤三中,浸渍时长为10分钟至1小时,优选的,浸渍时长为15分钟至35分钟,例如,为20分钟,30分钟。
步骤四中,所述的碱性溶液为氨水,乙二胺的水溶液,三乙醇胺的水溶液中的一种或多种。所述步骤四中,加入碱性溶液后,搅拌均匀后,约5~20分钟,从溶液中取出聚乳酸无纺布。根据本发明的实施方案,所述碱性溶液为0.1mol/L氨水,0.2mol/L乙二胺,0.5mol/L三乙醇胺中的一种或多种;所述锌盐为Zn(NO3)2·6H2O,C4H6O4Zn·2H2O,葡萄糖酸锌中的一种或多种;所述铝盐为Al2(SO4)3·18H2O,Al2(SO4)3·16H2O,Al(NO3)3·9H2O中的一种或多种。
所述碱性溶液与溶液A的体积比为1:200~2000,优选的,为1:250~1500,更优选的,为1:250~600。
所述溶液A中,锌盐的浓度为0.5-30g/L,优选为1.0-20g/L,例如为1.8g/L,16g/L;
所述铝盐与锌盐的摩尔比为15:1~1:15,优选为10:1~1:12,例如为7:1~8:1,1:7-1:9。
步骤二中,所述聚乳酸无纺布可以根据需要采用常规尺寸,例如长、宽各选自10-30mm,例如选自180*180mm,195*195mm尺寸。
根据本发明的实施方案,步骤五中,取出被浸渍的聚乳酸无纺布后,经水冲洗,并干燥后得到所述医用抗病毒无纺布。所述干燥可以采用50~80℃鼓风干燥箱中干燥,干燥时间为12-36小时,优选的,为15-28小时。
根据本发明的实施方案,所述医用抗病毒无纺布的制备方法,包括如下步骤:
将Zn(NO3)2·6H2O溶于水中,搅拌均匀,获得Zn(NO3)2·6H2O溶液,再将Al2(SO4)3·18H2O溶于上述Zn(NO3)2·6H2O溶液,搅拌均匀,获得混合溶液,随后,将聚乳酸无纺布浸渍于该混合溶液,浸渍时长约为30min,加入0.2mol/L乙二胺,搅拌均匀后,约5-20分钟,从溶液中取出聚乳酸无纺布,用水洗净,并干燥。
所述方法中,各原料投料比以及后处理细节等均参照前文定义。
根据本发明的实施方案,所述医用抗病毒无纺布的制备方法,包括如下步骤:
将C4H6O4Zn·2H2O溶于水中,搅拌均匀,获得C4H6O4Zn·2H2O溶液,再将Al(NO3)3·9H2O溶于上述C4H6O4Zn·2H2O溶液,搅拌均匀,获得混合溶液,随后,将聚乳酸无纺布浸渍于该混合溶液,浸渍时长约为20min,加入0.1mol/L氨水,搅拌均匀后,约5-20分钟,从溶液中取出聚乳酸无纺布,用水洗净,并干燥。
所述方法中,各原料投料比以及后处理细节等均参照前文定义。
根据本发明的实施方案,所述医用抗病毒无纺布为含纳米陶瓷粉聚乳酸无纺布;所述纳米陶瓷粉为纳米氧化锌和纳米氧化铝复合陶瓷粉;所述纳米氧化锌的尺寸为20-100nm,优选为30-90nm,例如为40nm,80nm;所述纳米氧化铝的尺寸为40-150nm,优选为80-150nm,例如为90nm,120nm,140nm;所述纳米氧化铝与纳米氧化锌的摩尔比为15:1~1:15,优选为10:1~1:12。
本发明还提供一种根据所述方法得到的医用抗病毒无纺布。
本发明还提供所述抗病毒无纺布的用途,其特征在于,用于口罩,防护服等防护用品。
本发明还提供一种医用抗病毒口罩,其特征在于,含有所述医用抗病毒无纺布。
根据本发明的实施方案,所述医用抗病毒口罩由口罩体、口罩带组成,口罩体包括四层,第一层为聚乳酸无纺布层,第二层为所述医用抗病毒无纺布层(即含纳米陶瓷粉无纺布层),第三层为聚乳酸熔喷布层,第四层为聚乳酸无纺布层。
根据本发明的实施方案,所述口罩体第一层克重15-40gsm;第二层克重为50-200gsm;第三层克重为25-60gsm;第四层克重为30-80gsm。
根据本发明的实施方案,在一些实施方式中,所述口罩体从外到内依次包括四层,第一层为聚乳酸无纺布层;第二层为含纳米陶瓷粉聚乳酸无纺布层;第三层为聚乳酸熔喷布层;第四层为聚乳酸无纺布层;在一些实施方式中,所述口罩体从内到外依次包括四层,第一层为聚乳酸无纺布层;第二层为含纳米陶瓷粉聚乳酸无纺布层;第三层为聚乳酸熔喷布层;第四层为聚乳酸无纺布层。
根据本发明的实施方案,所述口罩带与第四层相连接;所述四层布体的周边通过超声波热合为一体。
有益效果
1)本发明制备得到的含纳米陶瓷粉聚乳酸无纺布层可以有效抑制病毒,尤其是2019-nCoV病毒;
2)本发明的含纳米陶瓷粉聚乳酸无纺布层采用化学浸渍法得到,工艺简单,可操作性强,所得产品中陶瓷粉末成分为纳米级、含量可控,分布均匀,且该材料安全无刺激,具有高效防护性能,因而适合在防护用品领域大规模生产,具有良好的应用前景;
3)发明人发现,由本发明得到的含纳米陶瓷粉聚乳酸无纺布层可进一步制备得到具有高效抗病毒能力的口罩,所述口罩制备原料价格低廉,制备工艺简单可控,在保证口罩对于病毒的防护力的同时,能够有效降低医用抗病毒口罩的生产成本;且口罩体的四层基体材料均为聚乳酸无纺布,可降解,绿色环保。
附图说明
图1为实施例1制得的含纳米陶瓷粉聚乳酸无纺布层的扫描电镜图;从左到右三幅图依次表示:(a)为在50um的比例下观察的图片;(b)为(a)中黑色选定区域在10um的比例下观察的图片;(c)为(b)中黑色选定区域在1um的比例下观察的图片,氧化锌的尺寸为80nm,氧化铝的尺寸为120nm。
图2为四层医用抗病毒口罩组成示意图。
具体实施方式
下文将结合具体实施例对本发明的技术方案做更进一步的详细说明。应当理解,下列实施例仅为示例性地说明和解释本发明,而不应被解释为对本发明保护范围的限制。凡基于本发明上述内容所实现的技术均涵盖在本发明旨在保护的范围内。
除非另有说明,以下实施例中使用的原料和试剂均为市售商品,或者可以通过已知方法制备。
实施例1
先将1.8g Zn(NO3)2·6H2O溶于1000mL纯化水中,搅拌均匀,获得Zn(NO3)2·6H2O溶液,再将30g Al2(SO4)3·18H2O溶于上述Zn(NO3)2·6H2O溶液,搅拌均匀,获得混合溶液,随后,将180*180mm聚乳酸无纺布浸渍于该混合溶液,浸渍时长为30min,加入0.2mol/L乙二胺2mL,搅拌均匀后,约5-20分钟,从溶液中取出聚乳酸无纺布,用纯化水冲洗干净,并于60℃鼓风干燥箱中干燥24h,即可获得含纳米陶瓷粉聚乳酸无纺布。通过X射线荧光光谱分析(XRF)对纳米陶瓷粉聚乳酸无纺布进行分析,氧化锌和氧化铝含量见表1。
表1纳米陶瓷粉聚乳酸无纺布中氧化锌和氧化铝含量
(w/w)% | |
Al2O3 | 90.2% |
ZnO | 9.8% |
实施例2
先将16g C4H6O4Zn·2H2O溶于1000mL纯化水中,搅拌均匀,获得C4H6O4Zn·2H2O溶液,再将3.5gAl(NO3)3·9H2O溶于上述C4H6O4Zn·2H2O溶液,搅拌均匀,获得混合溶液,随后,将195*195mm聚乳酸无纺布浸渍于该混合溶液,浸渍时长为20min,加入0.1mol/L氨水3mL,搅拌均匀后,约5-20分钟,从溶液中取出聚乳酸无纺布,用纯化水冲洗干净,并于70℃鼓风干燥箱中干燥18h,即可获得含纳米陶瓷粉聚乳酸无纺布。通过X射线荧光光谱分析(XRF)对纳米陶瓷粉聚乳酸无纺布进行分析,氧化锌和氧化铝含量见表2。
表2纳米陶瓷粉聚乳酸无纺布中氧化锌和氧化铝含量
(w/w)% | |
Al2O3 | 13.8% |
ZnO | 86.2% |
实施例3
一种医用抗病毒口罩由4层布体组成,从外到内,第一层为聚乳酸无纺布层(约20gsm);第二层为实施例1制得的含纳米陶瓷粉聚乳酸无纺布层(约55gsm);第三层为聚乳酸熔喷布层(约25gsm);第四层为聚乳酸无纺布层(约35gsm),四层布体的周边通过超声波热合为一体,再焊接耳带,制成口罩。
实施例4
一种医用抗病毒口罩由4层布体组成,从外到内,第一层为聚乳酸无纺布层(约25gsm);第二层为实施例2制得的含纳米陶瓷粉聚乳酸无纺布层(约80gsm);第三层为聚乳酸熔喷布层(约30gsm);第四层为聚乳酸无纺布层(约50gsm),四层布体的周边通过超声波热合为一体,再焊接耳带,制成口罩。
实施例5
通过扫描电镜对实施例1制得的含纳米陶瓷粉聚乳酸无纺布层进行检测,氧化锌的尺寸为40nm,氧化铝的尺寸为90nm;对实施例2制得的含纳米陶瓷粉聚乳酸无纺布层进行检测,氧化锌的尺寸为80nm,氧化铝的尺寸为120nm。
实施例6
将实施例1制得的含纳米陶瓷粉聚乳酸无纺布层按照ANSI/AAMI PB70:2012进行检测,含纳米陶瓷粉聚乳酸无纺布对2019-nCoV病毒的过滤效率为99.0%。
实验方法如下:
所有操作在生物安全防护三级实验室(P3)进行。
a.测试材料紫外线消毒正反面各照射30分钟。
b.用无血清MEM培养基稀释新冠病毒液滴度至200TCID50/ml,配值6ml/管,共4管。
c.每管留取1ml病毒液,加热60度灭活1小时,备用。
d.在将稀释的毒液5ml置于15ml离心管中,取灭菌的测试材料盖在离心管口上,用橡皮筋扎紧并用封口膜进行加固。管口朝下倒置离心管,并将管子倒立于一个新的无菌的50ml离心管内。在安全柜内静置24小时。
e.次日,小心吸取测试材料上的滤过液20ul于无菌的EP管中,加1ml 5%FBS的MEM培养基混匀,并加于已铺有Vero细胞的24孔培养板孔中。
f.同法,吸取10ml管子中未滤过的毒液20ul,加1ml 5%FBS的MEM培养基混匀,并加于已铺有Vero细胞的24孔培养板孔中。(对照)
g.同法,取热灭活的毒液20ul,加1ml 5%FBS的MEM培养基混匀,并加于已铺有Vero细胞的24孔培养板孔中。(对照)
h.培养72小时,取培养上清液200ul,磁珠法提取核酸,荧光RT-PCR法检测新冠病毒的核酸水平。
i.实验结果如下,每个样本重复4次
注:FAM、VIC、Red代表用3种不同荧光探针分别标记SARS-CoV-2的3个不同序列,FAM标记RdRP基因,VIC标记N基因,Red标记E基因。定量计算用FAM通道的RdRP基因。
根据以上结果计算,在原液浓度为200TCID 50/ml的情况下,新冠病毒经过纳米陶瓷粉聚乳酸无纺布过滤24h后,滤出液的病毒载量约为原来的1.0%即2.0TCID 50/ml,纳米陶瓷粉聚乳酸无纺布对新冠病毒的过滤效率为99.0%。
实施例7
将实施例4制得的医用抗病毒口罩按照YY/T 1497-2016进行检测,结果显示对Phi-X174噬菌体病毒过滤效率≥70%。
实施例8
按照实施例1的制备方法,仅减少加入铝盐的步骤,得到含纳米氧化锌无纺布材料,依据实施例6的检测方法按照ANSI/AAMI PB70:2012进行检测,测得含纳米氧化锌无纺布材料对2019-nCoV病毒的过滤效率为72.0%。
实施例9
按照实施例4制备口罩的方法,减少第二层,即所述口罩从外到内,第一层为聚乳酸无纺布层;第二层为聚乳酸熔喷布层;第三层为聚乳酸无纺布层,三层布体的周边通过超声波热合为一体,再焊接耳带,制成口罩。将所得到的口罩按照YY/T 1497-2016进行检测,结果显示对Phi-X174噬菌体病毒过滤效率为44%。
实施例10
按照实施例4制备口罩的方法,将第二层替换为聚乳酸无纺布层,即所述口罩从外到内,第一层为聚乳酸无纺布层;第二层为聚乳酸无纺布层;第三层为聚乳酸熔喷布层;第四层为聚乳酸无纺布层,四层布体的周边通过超声波热合为一体,再焊接耳带,制成口罩。将所得到的口罩按照YY/T 1497-2016进行检测,结果显示对Phi-X174噬菌体病毒过滤效率为57%。
以上,对本发明的实施方式进行了说明。但是,本发明不限定于上述实施方式。凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (11)
1.一种医用抗病毒无纺布的制备方法,其特征在于,包括如下步骤:
步骤一,将锌盐溶于水中,获得溶液A;
步骤二,将铝盐溶于步骤一得到的溶液A,获得混合溶液B;
步骤三,将聚乳酸无纺布浸渍于步骤二得到的混合溶液B;
步骤四,加入碱性溶液;
步骤五,从溶液中取出被浸渍的聚乳酸无纺布,经后处理得到所述医用抗病毒无纺布;
步骤一中所述锌盐为硝酸锌,乙酸锌及其水合物中的一种或多种;步骤二中所述铝盐为硫酸铝,硝酸铝及其水合物中的一种或多种;
步骤三中,浸渍时长为10分钟至1小时;
步骤四中,所述的碱性溶液为氨水,乙二胺的水溶液,三乙醇胺的水溶液中的一种或多种;
所述铝盐与锌盐的摩尔比为7:1~8:1,1:7-1:9。
2.根据权利要求1所述的制备方法,其特征在于,步骤三中,浸渍时长为15分钟至35分钟。
3.根据权利要求1所述的制备方法,其特征在于,步骤三中,浸渍时长为为20分钟或30分钟。
4.根据权利要求1所述的制备方法,其特征在于,所述碱性溶液为0.1mol/L氨水,0.2mol/L乙二胺,0.5mol/L三乙醇胺中的一种或多种;所述锌盐为Zn(NO3)2·6H2O,C4H6O4Zn·2H2O中的一种或多种;所述铝盐为Al2(SO4)3•18H2O, Al2(SO4)3•16H2O,Al(NO3)3•9H2O中的一种或多种。
5.根据权利要求1所述的制备方法,其特征在于,所述碱性溶液与溶液A的体积比为1:200~2000。
6.根据权利要求1所述的制备方法,其特征在于,所述溶液A中,锌盐的浓度为0.5-30g/L。
7.根据权利要求1-6任一项所述的制备方法得到的医用抗病毒无纺布。
8.根据权利要求7所述的医用抗病毒无纺布的用途,其特征在于,用于口罩,防护服。
9.一种口罩,其特征在于,含有权利要求7所述的医用抗病毒无纺布。
10.根据权利要求9所述的口罩,其特征在于,所述口罩由口罩体、口罩带组成,口罩体包括四层,第一层为聚乳酸无纺布层,第二层为根据权利要求7所述的医用抗病毒无纺布,第三层为聚乳酸熔喷布层,第四层为聚乳酸无纺布层。
11.根据权利要求10所述的口罩,其特征在于,所述口罩体从外到内依次包括四层,第一层为聚乳酸无纺布层;第二层为根据权利要求7所述的医用抗病毒无纺布;第三层为聚乳酸熔喷布层;第四层为聚乳酸无纺布层。
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