CN111844943A - 一种抗菌组合层以及包含其的抗菌防护口罩 - Google Patents

一种抗菌组合层以及包含其的抗菌防护口罩 Download PDF

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CN111844943A
CN111844943A CN202010768366.9A CN202010768366A CN111844943A CN 111844943 A CN111844943 A CN 111844943A CN 202010768366 A CN202010768366 A CN 202010768366A CN 111844943 A CN111844943 A CN 111844943A
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antibacterial
layer
lipase
montmorillonite
composite
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刘坤
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Sichuan Lezhi Guijun Hygienic Material Co ltd
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    • A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
    • A41D2500/00—Materials for garments
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Abstract

本发明涉及抗菌口罩技术领域，公开了一种抗菌组合层，包括抗菌外层和抗菌内层；所述抗菌外层为淀粉基聚乳酸复合材料，所述抗菌外层负载有无机纳米抗菌剂；所述抗菌内层吸附有脂肪酶。还公开了一种包含抗菌层的抗菌防护口罩，包括顺次相接的防尘外层、过滤层、抗菌组合层和亲肤层，抗菌组合层中的抗菌外层与过滤层贴合，抗菌组合层中的抗菌内层与亲肤层贴合。本发明能够避免细菌尸体或细菌分泌物污染抗菌材料，持续发挥抗菌效果，绿色可降解，抗菌效果佳。

Description

一种抗菌组合层以及包含其的抗菌防护口罩
技术领域
本发明属于防护口罩的技术领域，具体地说，涉及一种抗菌组合层以及包含其的抗菌防护口罩。
背景技术
空气和水的污染、病毒或其它细菌的大量繁衍，给人们的健康带来巨大的威胁。口罩是用来使人类免受病菌侵袭的一种便捷的保护措施。
传统的抗菌口罩有纱布口罩和非织造材料制得的口罩，由于非织造纤维具有复杂的纤维堆积结构以及纤维的三维随机分布，使材料中含有大量微小空隙，微粒围绕纤维经过各种类型的弯曲通道或路径，可极大降低气流通过时的阻力，同时由于具有较快的生产速度、优异的结构性能使得其在口罩过滤市场的应用较为广泛。
由于绿色可持续发展的要求，当前非织造纤维材料中，绿色可降解的高分子材料逐渐成为口罩等防护材料的重点研究方向。其中，聚乳酸高分子材料具备可降解性，且降解产物为二氧化碳和水的优势，而得到应用。由于聚乳酸不具备抗菌特性，因而常在聚乳酸树脂中加入抗菌剂或者对聚乳酸树脂进行改性处理，用以使得聚乳酸树脂具备抗菌特性。
公开号为CN111286175A的专利，就公开了一种满足上述应用需求的可降解抗菌口罩。该专利公开了可降解纺丝原料、可降解纤维膜及可降解防护罩，其技术方案是在聚合物基材上负载纳米非金属光催化材料，用以达到抗菌和可降解的双重功效。细菌或病毒被纳米非金属光催化材料在抑菌过程中，防护罩会受到死亡菌体及菌体破裂后释放的细胞内物质的污染，从而造成杀菌能力下降。当前也有通过设置多层防护层的口罩用以增强杀菌效果。然而，若未将菌体污染物除去，菌体污染物容易通过外防护层侵入内防护层，造成内防护层无法发挥杀菌效果。
因此，寻求一种在防护过程中能够除去菌体污染物、持续发挥杀菌效果的抗菌口罩尤为重要。
发明内容
经过大量的研究，我们发现，将抗菌层设置为双层结构，外层结构为包含有聚乳酸的复合材料，内层结构为吸附有脂肪酶的复合材料。抗菌层在抗菌的过程中，菌体分泌物会吸附于外层结构上，通过脂肪酶与聚乳酸作用，能够加速降解聚乳酸，避免菌体分泌物污染内层结构，进而达到持续的抗菌效果。
因此，本发明的第一个目的在于，提供一种抗菌组合层，包括抗菌外层和抗菌内层；所述抗菌外层为淀粉基聚乳酸复合材料，所述抗菌外层负载有无机纳米抗菌剂；所述抗菌内层吸附有酯酶。
本发明的第二个目的在于，提供一种抗菌防护口罩，包括顺次相接的防尘外层、过滤层、抗菌组合层和亲肤层，抗菌组合层中的抗菌外层与过滤层贴合，抗菌组合层中的抗菌内层与亲肤层贴合。
本申请设置有抗菌组合层，抗菌外层负载有无机纳米抗菌剂，复合抗菌层在使用过程中，抗菌外层负载的无机纳米抗菌剂起着抗菌作用，将菌体阻挡于抗菌外层的表面，随着抗菌的持续作用，菌体的尸体或者菌体破碎后形成的分泌物覆盖于抗菌外层。由于抗菌内层中吸附有脂肪酶，在抗菌组合层作用过程中，抗菌内层逐步释放出游离脂肪酶，游离脂肪酶作用于聚乳酸分子，使得聚乳酸分子逐渐分解，以致抗菌外层逐渐脱落，从而露出抗菌内层，抗菌内层再持续发挥抗菌作用，这是由于聚乳酸中含有酯键，脂肪酸能够作用于酯键，加速聚乳酸分子的降解。
本申请的抗菌外层为淀粉基聚乳酸复合材料，淀粉为变性淀粉，变性淀粉能够与聚乳酸分子发生交联，起着对聚乳酸分子的改性作用，进而提升聚乳酸分子的稳定性和拉伸强度。
本申请以抗菌组合层、过滤层和亲肤层制成的抗菌防护口罩，能够提升防护口罩的抗菌效果。
本发明的有益效果表现在：
能够避免细菌尸体或细菌分泌物污染抗菌材料，持续发挥抗菌效果，绿色可降解，抗菌效果佳。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将对本发明实施例中的技术方案进行清楚、完整地描述。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
第一，本发明提供了一种抗菌组合层，包括抗菌外层和抗菌内层；所述抗菌外层为淀粉基聚乳酸复合材料，所述抗菌外层负载有无机纳米抗菌剂，所述淀粉为变性淀粉；所述抗菌内层吸附有脂肪酶。
本发明中，淀粉为玉米淀粉。
本发明中，抗菌外层中玉米淀粉、增塑剂、无机纳米抗菌剂和聚乳酸树脂的质量比为0.05:0.01～0.06:0.01～0.05:1。
本发明中，无机纳米抗菌剂为TiO2纳米微球或TiO2-Ag复合纳米微球。其中，TiO2-Ag复合纳米微球的制备方法为：钛酸四丁酯和无水乙醇按1:1的体积均匀混合形成第一混合液；冰醋酸和去离子水按1:4的体积比混合后加入到无水乙醇中，冰醋酸与无水乙醇的体积比为1:5，pH调节至3，加入AgNO3，使得Ag与TiO2的质量比为2.5～3:1，均匀混合后得到第二混合液；将第一混合液缓慢加入第二混合液中，并进行超声10min处理，并烘干至恒重得到TiO2-Ag复合纳米微球。TiO2-Ag复合纳米微球通过将TiO2和Ag混合于一起，用以提升抗菌特性。
本发明中，脂肪酶为根霉菌酯肪酶、猪胰腺酯肪酶或梭基酯酶，或者组合物。
本发明中，抗菌外层的制备方法为，将玉米淀粉、增塑剂、无机纳米抗菌剂和聚乳酸树脂按0.05:0.01～0.06:0.1～0.3:1的质量比加入密炼机中混合，于双螺杆挤出机中熔融造粒，得到颗粒物，再将颗粒物放入纺丝机中进行纺丝处理。采用常规的纺丝工艺处理即可，增塑剂为甘油或者PEG-200。
本发明中，抗菌内层为苎麻-聚丙烯-蒙脱土复合材料，抗菌内层吸附有脂肪酶，抗菌内层的表面涂覆有壳聚糖。
蒙脱土属于2:1型的层状硅酸盐，因其突出的阳离子交换能力和良好的吸附性能而非常适合于吸附材料。将蒙脱土作为载体中能够制备出高效安全、具有缓释性的复合材料。蒙脱土同样是一种对脂肪酶有着很好的固化作用，将蒙脱土作为吸附载体吸附脂肪酶，能够制备出高效安全、具有缓释性的抗菌材料。在抗菌组合层的抗菌过程中，抗菌外层首先作用于菌体，随着抗菌作用的持续作用，抗菌内层中蒙脱土释放出脂肪酶，脂肪酶逐步作用于聚乳酸中的酯键，从而达到对聚乳酸的降解。苎麻具有一定的疏水性、抗菌性以及是一种多孔材料，将苎麻与聚丙烯混合形成的复合材料能够起着抗菌作用，且由于有的细菌为亲水性菌体，在苎麻的作用下能够避免细菌在抗菌内层的表面形成细菌生物膜。由于壳聚糖涂覆于抗菌内层的表面，壳聚糖是同样具有抗菌作用的物质，且壳聚糖能够抑制非亲水性的菌体进入抗菌内层中。壳聚糖为亲水性胶体，能够缓慢溶胀聚乳酸分子，从而达到对聚乳酸树脂的进一步降解，能够使得聚乳酸分子脱落，避免菌体分泌物通过抗菌外层渗入抗菌内层中。
本发明中，抗菌内层的制备方法为，将蒙脱土与聚丙烯树脂A加入密炼机内混合，得到改性蒙脱土，将改性蒙脱土加入质量分数为0.2％的脂肪酶溶液中，超声吸附30min，得到吸附有脂肪酶的蒙脱土；再将苎麻、聚丙烯树脂B、吸附有脂肪酶的蒙脱土、硅烷偶联剂和抗氧化剂加入密炼机中混合，于双螺杆挤出机中熔融造粒，得到颗粒物，再将颗粒物放入纺丝机中进行纺丝处理。采用常规的纺丝工艺处理即可。蒙脱土、聚丙烯树脂A、脂肪酶、苎麻、聚丙烯树脂B、硅烷偶联剂和抗氧化剂的质量比为15:1～3:0.1～0.6:10～15:60～70:0.5:0.5。抗氧化剂为抗氧剂1010。
本发明中在抗菌内层的表面喷涂壳聚糖，壳聚糖占抗菌内层质量的5％～15％。
本发明中，为了进一步增强抗菌效果，在蒙脱土中加入纳米银抗菌剂，纳米银抗菌剂的加入质量与蒙脱土的质量比为3～5:15。
第二，本发明提供了一种抗菌防护口罩，包括顺次相接的防尘外层、过滤层、抗菌组合层和亲肤层，抗菌组合层中的抗菌外层与过滤层贴合，抗菌组合层中的抗菌内层与亲肤层贴合。
实施例1
一种抗菌组合层，包括抗菌外层和抗菌内层。抗菌外层为淀粉基聚乳酸复合材料，抗菌外层负载有无机纳米抗菌剂，淀粉为玉米淀粉。抗菌内层为苎麻-聚丙烯-蒙脱土复合材料，抗菌内层吸附有脂肪酶，抗菌内层的表面涂覆有壳聚糖。
抗菌外层的制备方法为，将玉米淀粉、增塑剂、无机纳米抗菌剂和聚乳酸树脂按0.05:0.03:0.2:1的质量比加入密炼机中混合，于双螺杆挤出机中熔融造粒，得到颗粒物，再将颗粒物放入纺丝机中进行纺丝处理。采用常规的纺丝工艺处理即可。增塑剂为甘油，无机纳米抗菌剂为TiO2。
抗菌内层的制备方法为，将蒙脱土与聚丙烯树脂A加入密炼机内混合，得到改性蒙脱土，将改性蒙脱土加入质量分数为0.2％的脂肪酶溶液中，超声吸附30min，得到吸附有脂肪酶的蒙脱土；再将苎麻、聚丙烯树脂B、吸附有脂肪酶的蒙脱土、硅烷偶联剂和抗氧化剂加入密炼机中混合，于双螺杆挤出机中熔融造粒，得到颗粒物，再将颗粒物放入纺丝机中进行纺丝处理。采用常规的纺丝工艺处理即可。蒙脱土、聚丙烯树脂A、脂肪酶、苎麻、聚丙烯树脂B、硅烷偶联剂和抗氧化剂的质量比为15:2:0.3:12:65:0.5:0.5。抗氧化剂为抗氧剂1010，脂肪酶为根霉菌酯肪酶。
实施例2
本实施例与实施例1的区别在于，抗菌外层中玉米淀粉、增塑剂、无机纳米抗菌剂和聚乳酸树脂的质量比为0.05:0.03:0.3:1。
实施例3
本实施例与实施例1的区别在于，抗菌外层中玉米淀粉、增塑剂、无机纳米抗菌剂和聚乳酸树脂的质量比为0.05:0.06:0.1:1。
实施例4
本实施例与实施例1的区别在于，无机纳米抗菌剂为TiO2-Ag复合纳米微球。TiO2-Ag复合纳米微球的制备方法为，钛酸四丁酯和无水乙醇按1:1的体积均匀混合形成第一混合液；冰醋酸和去离子水按1:4的体积比混合后加入到无水乙醇中，冰醋酸与无水乙醇的体积比为1:5，pH调节至3，加入AgNO3，使得Ag与TiO2的质量比为2.5:1，均匀混合后得到第二混合液；将第一混合液缓慢加入第二混合液中，并进行超声10min处理，并烘干至恒重得到TiO2-Ag复合纳米微球。
实施例5
本实施例与实施例1的区别在于，抗菌内层中蒙脱土、聚丙烯树脂A、脂肪酶、苎麻、聚丙烯树脂B、硅烷偶联剂和抗氧化剂的质量比为15:1:0.6:15:70:0.5:0.5。
实施例6
本实施例与实施例1的区别在于，抗菌内层中蒙脱土、聚丙烯树脂A、脂肪酶、苎麻、聚丙烯树脂B、硅烷偶联剂和抗氧化剂的质量比为15:3:0.1:10:60:0.5:0.5。
实施例7
本实施例与实施例1的区别在于，抗菌内层中还包括纳米银抗菌剂，纳米银抗菌剂和改性蒙脱土一起加入脂肪酶溶液中，得到吸附有脂肪酶、纳米银抗菌剂的蒙脱土，纳米银抗菌剂与蒙脱土的质量比为5:15。
实施例8
本实施例与实施例1的区别在于，脂肪酶还可以选用猪胰腺酯肪酶或梭基酯酶，或者它们的组合物。
实施例9
本实施例与实施例4的区别在于，TiO2-Ag复合纳米微球的制备方法为，钛酸四丁酯和无水乙醇按1:1的体积均匀混合形成第一混合液；冰醋酸和去离子水按1:4的体积比混合后加入到无水乙醇中，冰醋酸与无水乙醇的体积比为1:5，pH调节至3，加入AgNO3，使得Ag与TiO2的质量比为3:1，均匀混合后得到第二混合液；将第一混合液缓慢加入第二混合液中，并进行超声10min处理，并烘干至恒重得到TiO2-Ag复合纳米微球。
实施例10
本实施例与实施例7的区别在于，纳米银抗菌剂与蒙脱土的质量比为3:15。
实施例11
一种抗菌防护口罩，包括顺次相接的防尘外层、过滤层、实施例1至10中任意一项的抗菌组合层和亲肤层，抗菌组合层中的抗菌外层与过滤层贴合，抗菌组合层中的抗菌内层与亲肤层贴合。
对比例1
一种抗菌组合层，包括双层抗菌层。抗菌层为淀粉基聚乳酸复合材料，抗菌层负载有TiO2抗菌剂，淀粉为玉米淀粉。抗菌层的制备方法同实施例1中抗菌外层的制备方法。
对比例2
一种抗菌组合层，包括第一抗菌层和第二抗菌层，第一抗菌层同实施例1中的抗菌外层。第二抗菌层与实施例1中的抗菌内层相较，没有吸附脂肪酶。
对比例3
一种抗菌组合层，包括双层抗菌层，抗菌层为苎麻-聚丙烯-蒙脱土复合材料，抗菌内层的表面涂覆有壳聚糖。抗菌内层的制备方法同实施例1中国抗菌内层的制备方法。
对比例4
一种抗菌组合层，与实施例1的区别在于，抗菌外层中中玉米淀粉、增塑剂、无机纳米抗菌剂和聚乳酸树脂的质量比为0.05:0.08:0.5:1；抗菌内层中蒙脱土、聚丙烯树脂A、脂肪酶、苎麻、聚丙烯树脂B、硅烷偶联剂和抗氧化剂的质量比为15:5:0.8:18:75:0.5:0.5。
对比例5
一种抗菌组合层，与实施例1的区别在于，抗菌外层中玉米淀粉、增塑剂、无机纳米抗菌剂和聚乳酸树脂的质量比为0.05:0.01:0.05:1；抗菌内层的蒙脱土、聚丙烯树脂A、脂肪酶、苎麻、聚丙烯树脂B、硅烷偶联剂和抗氧化剂的质量比为15:0.5:0.1:8:58:0.5:0.5。
试验例
样品：实施例1至7，对比例1至对比例5。
参照《GB15979-2002一次性卫生用品卫生标准》附录C《产品杀菌性能、抑菌性能与稳定性测试方法》对样品的抗菌层进行杀菌率试验，作用时间为5分钟。实验结果如表1所示。
表1不同样品的杀菌效果结果
Figure BDA0002615550220000091
由表1可知，实施例组的各样品的杀菌效果均优于对比例组的杀菌效果。(1)实施例组与对比例1至3相比，通过采用脂肪酶对聚乳酸树脂的降解作用，能够避免细菌分泌物污染抗菌层，从而提升杀菌效果。(2)实施例组与对比例4至5相比，实施例组中抗菌内层和抗菌外层中各物质的含量限定在实施例组的范围内，能够达到更佳的抗菌效果。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种抗菌组合层，其特征在于，包括抗菌外层和抗菌内层；
所述抗菌外层为淀粉基聚乳酸复合材料，所述抗菌外层负载有无机纳米抗菌剂；所述抗菌内层吸附有脂肪酶。
2.根据权利要求1所述的抗菌组合层，其特征在于，所述抗菌外层的制备方法为，将淀粉、增塑剂、无机纳米抗菌剂和聚乳酸树脂按0.05:0.01～0.06:0.1～0.3:1的质量比加入密炼机中混合，于双螺杆挤出机中熔融造粒，得到颗粒物，再将颗粒物放入纺丝机中进行纺丝处理。
3.根据权利要求1所述的抗菌组合层，其特征在于，无机纳米抗菌剂为TiO2纳米微球或TiO2-Ag复合纳米微球。
4.根据权利要求3所述的抗菌组合层，其特征在于，TiO2-Ag复合纳米微球的制备方法为，钛酸四丁酯和无水乙醇按1:1的体积均匀混合形成第一混合液；冰醋酸和去离子水按1:4的体积比混合后加入到无水乙醇中，冰醋酸与无水乙醇的体积比为1:5，pH调节至3，加入AgNO3，使得Ag与TiO2的质量比为2.5～3:1，均匀混合后得到第二混合液；将第一混合液缓慢加入第二混合液中，并进行超声处理，并烘干至恒重得到TiO2-Ag复合纳米微球。
5.根据权利要求1所述的抗菌组合层，其特征在于，所述脂肪酶为根霉菌酯肪酶、猪胰腺酯肪酶或梭基酯酶。
6.根据权利要求1或2所述的抗菌组合层，其特征在于，抗菌内层为苎麻-聚丙烯-蒙脱土复合材料，抗菌内层的表面涂覆有壳聚糖。
7.根据权利要求6所述的抗菌组合层，其特征在于，所述抗菌外层的制备方法为，将蒙脱土与聚丙烯树脂A加入密炼机内混合，得到改性蒙脱土，将改性蒙脱土加入质量分数为0.2％的脂肪酶溶液中，超声吸附，得到吸附有脂肪酶的蒙脱土；再将苎麻、聚丙烯树脂B、吸附有脂肪酶的蒙脱土、硅烷偶联剂和抗氧化剂加入密炼机中混合，于双螺杆挤出机中熔融造粒，得到颗粒物，再将颗粒物放入纺丝机中进行纺丝处理。
8.根据权利要求7所述的抗菌组合层，其特征在于，所述抗菌内层中蒙脱土、聚丙烯树脂A、脂肪酶、苎麻、聚丙烯树脂B、硅烷偶联剂和抗氧化剂的质量比为15:1～3:0.1～0.6:10～15:60～70:0.5:0.5。
9.根据权利要求6所述的抗菌组合层，其特征在于，在蒙脱土中加入纳米银抗菌剂，纳米银抗菌剂的加入质量与蒙脱土的质量比为3～5:15。
10.一种抗菌防护口罩，其特征在于，包括顺次相接的防尘外层、过滤层、权利要求1至5或7至9中任意一项所述的抗菌组合层和亲肤层，抗菌组合层中的抗菌外层与过滤层贴合，抗菌组合层中的抗菌内层与亲肤层贴合。
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