CN111996794A - 一种抗菌聚乳酸非织造材料的制备方法 - Google Patents
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Abstract
本发明涉及聚乳酸材料技术领域,具体涉及一种抗菌聚乳酸非织造材料的制备方法,包括如下步骤:步骤一、将聚乳酸非织造材料在常压介质阻挡放电(DBD)等离子体装置中进行表面改性处理;步骤二、将经常压等离子体处理后的聚乳酸非织造材料进行壳聚糖接枝整理;步骤三、将上述处理后的聚乳酸非织造材料浸渍到硝酸银溶液中进行抗菌整理。本发明工艺简单,原料绿色无污染,具有生物相容性和自然降解性,通过等离子体辅助方法对聚乳酸非织造材料进行表面修饰,并在其表面原位还原纳米银,提高纳米银负载效率,制备方法绿色环保,制备的聚乳酸非织造材料抗菌性能优异,对大肠杆菌和金黄色葡萄球菌的抑菌率达到99.9%。
Description
技术领域
本发明涉及聚乳酸材料技术领域,具体涉及一种抗菌聚乳酸非织造材料的制备方法。
背景技术
随着世界石油资源日益枯竭,以及白色污染日趋严重,寻找一种可再生的绿色能源逐渐引起了人们的关注。聚乳酸(PLA)材料以其良好的物理机械性能、优良的生物相容性、自然降解性被广泛地应用于医疗卫生、农林防护、纺织加工及包装材料等领域,是目前研究最广泛、最具有开发潜力的可生物降解材料。然而,PLA材料的性能还存在缺陷,最突出的是其表面缺乏极性官能团,惰性较高,亲水性很差,不容易与其他物质发生反应,这在很大程度上限制了PLA在生物医用功能性材料领域的进一步发展。
目前,针对PLA的改性方法有很多,主要包括共聚改性,共混改性,交联改性以及表面改性。在众多方法中,介质阻挡放电(DBD)等离子体在常压下即可产生,省去了繁杂的真空***,节能环保,处理效果稳定可靠。并且等离子体改性处理只作用于材料的浅表层,在不损伤材料基体性能的前提下,实现材料表面亲水性能、粘结性能和染色性能等多种性能的显著提高。纳米银具有强效、广谱的抗菌性,在抗菌纺织品的研发中引起了广泛关注。目前,比较常用的制备纳米银抗菌纺织品的方法是化学还原法,该方法是先将银离子吸附到纺织品上,再加入还原剂将银离子在纺织品上原位还原成纳米银,但这种方法需要加入还原剂,不利于环境的可持续发展。近年来,采用无还原剂的原位还原法已被学者研究报道,这种方法是利用纺织品自身的官能团将银离子吸附并原位还原成纳米银,无需加入其它还原剂,既简化了工艺过程,又降低了生产成本。
发明内容
针对以上问题,本发明提供了一种抗菌聚乳酸非织造材料的制备方法,以常压氩气DBD等离子体对PLA非织造材料进行预处理,采用环境友好的天然高分子材料壳聚糖对PLA进行表面接枝处理,在PLA非织造材料表面原位生成纳米银,使材料具有优异的抗菌性能。
为了实现上述目的,本发明采用的技术方案如下:
一种抗菌聚乳酸非织造材料的制备方法,具体包括以下步骤:
步骤一:对聚乳酸非织造材料进行表面改性处理,将聚乳酸非织造材料在常压介质阻挡放电等离子体装置中进行表面改性处理;
步骤二:对聚乳酸非织造材料进行壳聚糖接枝整理,配制壳聚糖溶液,将经等离子处理后的聚乳酸非织造材料投入壳聚糖溶液中进行壳聚糖接枝整理;
步骤三:对聚乳酸非织造材料进行抗菌整理,配制硝酸银溶液,将经壳聚糖接枝整理后的聚乳酸非织造材料投入硝酸银溶液中进行抗菌整理。
优选地,所述步骤(一)中,将聚乳酸非织造材料置于两平行极板之间,打开氩气阀,等离子体处理气氛为Ar和O2混合气体,Ar气的流量为1L/min,O2的流量为0.1L/min,处理功率为4KW,处理时间为60-120s。
优选地,所述步骤(二)中,将粉末状壳聚糖溶于2%醋酸溶液中,配制成壳聚糖溶液,壳聚糖溶液的质量分数为0.6%-1.1%,分子量为5×105,脱乙酰度89%-91%。
优选地,所述步骤(二)中,将经等离子体处理后的聚乳酸非织造材料投入壳聚糖溶液中,浴比1:40,恒温水浴温度为40-60℃,加热时间1h;随后用大量去离子水冲洗掉试样表面物理粘附的壳聚糖溶液,放入烘箱中,在45℃的条件下烘干2h待用。
优选地,所述步骤(三)中,将硝酸银溶解在去离子水中,配制成硝酸银溶液,硝酸银溶液的质量分数为0.5%-1.2%。
优选地,所述步骤(三)中,将经壳聚糖接枝整理后的聚乳酸非织造材料投入硝酸银溶液中,浴比1:40,反应温度为室温,反应时间为1h,采用去离子水水洗,水洗后烘干温度为30-60℃。
本发明所述的一种抗菌聚乳酸非织造材料的制备方法,与现有技术相比,具有如下有益效果:
1、经本发明整理后的PLA材料有良好的物理机械性能、且与还原剂壳聚糖一样具有优良的生物相容性、自然降解性,对人体安全性高,对环境无污染;
2、本发明对PLA采用DBD等离子体处理成功改善了其表面缺乏极性官能团,不容易与其他物质发生反应的缺陷。且等离子体处理节能环保,处理效果稳定可靠,改性处理也只作用于材料的浅表层,避免损伤材料基体性能;
3、本发明采用接枝壳聚糖原位还原纳米银的方法高效简便,能很好地将银纳米颗粒固定在织物表面,极大地提高了增大颗粒负载量。
附图说明
图1是本发明的工艺流程图;
图2是本发明PLA非织造材料整理前以及经抗菌整理后的外观示意图(a.PLA原样;b.壳聚糖-纳米银PLA整理样;c.等离子体-壳聚糖-纳米银PLA整理样);
图3是本发明PLA非织造材料经抗菌整理后的实验晕圈法效果图(a、b为壳聚糖-纳米银PLA非织造材料对大肠杆菌和金黄色葡萄球菌的抗菌效果图;c、d为等离子体-壳聚糖-纳米银PLA非织造材料对大肠杆菌和金黄色葡萄球菌的抗菌效果图)。
具体实施方式
下面结合附图与实施例对本发明的技术方案进行说明。
实施例一:
参照图1-图3,一种抗菌聚乳酸非织造材料的制备方法,具体包括以下步骤:
步骤一:将PLA非织造材料置于两平行极板之间,打开氩气阀,等离子体处理气氛为Ar和O2混合气体,Ar气的流量为1L/min,O2的流量为0.1L/min,处理功率为4KW,处理时间为90s。
步骤二:将粉末状壳聚糖溶于2%醋酸溶液中,配制成壳聚糖溶液,壳聚糖溶液的质量分数为0.8%,分子量为5×105,脱乙酰度90%;将经等离子体处理后的PLA非织造材料投入壳聚糖溶液中,浴比1:40,恒温水浴40℃,加热时间1h;随后用大量去离子水冲洗掉试样表面物理粘附的壳聚糖溶液,放入烘箱中,在45℃的条件下烘干2h待用。
步骤三:将粉末状硝酸银溶解在去离子水中,配制硝酸银溶液,质量分数为0.8%;将经接枝壳聚糖处理后的PLA非织造材料按投入硝酸银溶液中,浴比1:40,反应温度为室温,反应时间为1h,在45℃的条件下烘干2h。
本实施例中经抗菌整理后的PLA非织造材料对大肠杆菌的抑菌率达到96.1%,对金黄色葡萄球菌的抑菌率达到97.6%。
实施例二:
一种抗菌聚乳酸非织造材料的制备方法,具体包括以下步骤:
步骤一:将PLA非织造材料置于两平行极板之间,打开氩气阀,等离子体处理气氛为Ar和O2混合气体,Ar气的流量为1L/min,O2的流量为0.1L/min,处理功率为4KW,处理时间为120s。
步骤二:将粉末状壳聚糖溶于2%醋酸溶液中,配制成壳聚糖溶液,壳聚糖溶液的质量分数为1.1%,分子量为5×105,脱乙酰度89%;将经等离子体处理后的PLA非织造材料投入壳聚糖溶液中,浴比1:40,恒温水浴50℃,加热时间1h;随后用大量去离子水冲洗掉试样表面物理粘附的壳聚糖溶液,放入烘箱中,在45℃的条件下烘干2h待用。
步骤三:将粉末状硝酸银溶解在去离子水中,配制硝酸银溶液,质量分数为1.2%;将经接枝壳聚糖处理后的PLA非织造材料按投入硝酸银溶液中,浴比1:40,反应温度为室温,反应时间为1h,在45℃的条件下烘干2h。
本实施例中经抗菌整理后的PLA非织造材料对大肠杆菌的抑菌率达到97.5%,对金黄色葡萄球菌的抑菌率达到98.2%。
实施例三:
一种抗菌聚乳酸非织造材料的制备方法,具体包括以下步骤:
步骤一:将PLA非织造材料置于两平行极板之间,打开氩气阀,等离子体处理气氛为Ar和O2混合气体,Ar气的流量为1L/min,O2的流量为0.1L/min,处理功率为4KW,处理时间为100s;
步骤二:将粉末状壳聚糖溶于2%醋酸溶液中,配制成壳聚糖溶液,壳聚糖溶液的质量分数为1%,分子量为5×105,脱乙酰度90%;将经等离子体处理后的PLA非织造材料投入壳聚糖溶液中,浴比1:40,恒温水浴60℃,加热时间1h;随后用大量去离子水冲洗掉试样表面物理粘附的壳聚糖溶液,放入烘箱中,在45℃的条件下烘干2h待用。
步骤三:将粉末状硝酸银溶解在去离子水中,配制硝酸银溶液,质量分数为1%;将经接枝壳聚糖的PLA非织造材料按投入硝酸银溶液中,浴比1:40,反应温度为室温,反应时间为1h,在45℃的条件下烘干2h。
本实施例中经抗菌整理后的PLA非织造材料对大肠杆菌和金黄色葡萄球菌的抗菌性均高达99.9%。
以上对本发明的实施例进行了详细说明,但所述内容仅为本发明的较佳实施例,不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的均等变化与改进等,均应仍归属于本发明的专利涵盖范围之内。
Claims (6)
1.一种抗菌聚乳酸非织造材料的制备方法,其特征在于:具体包括以下步骤:
步骤一:对聚乳酸非织造材料进行表面改性处理,将聚乳酸非织造材料在常压介质阻挡放电等离子体装置中进行表面改性处理;
步骤二:对聚乳酸非织造材料进行壳聚糖接枝整理,配制壳聚糖溶液,将经等离子处理后的聚乳酸非织造材料投入壳聚糖溶液中进行壳聚糖接枝整理;
步骤三:对聚乳酸非织造材料进行抗菌整理,配制硝酸银溶液,将经壳聚糖接枝整理后的聚乳酸非织造材料投入硝酸银溶液中进行抗菌整理。
2.根据权利要求1所述的一种抗菌聚乳酸非织造材料的制备方法,其特征在于:所述步骤(一)中,将聚乳酸非织造材料置于两平行极板之间,打开氩气阀,等离子体处理气氛为Ar和O2混合气体,Ar气的流量为1L/min,O2的流量为0.1L/min,处理功率为4KW,处理时间为60-120s。
3.根据权利要求1所述的一种抗菌聚乳酸非织造材料的制备方法,其特征在于:所述步骤(二)中,将粉末状壳聚糖溶于2%醋酸溶液中,配制成壳聚糖溶液,壳聚糖溶液的质量分数为0.6%-1.1%,分子量为5×105,脱乙酰度89%-91%。
4.根据权利要求3所述的一种抗菌聚乳酸非织造材料的制备方法,其特征在于:所述步骤(二)中,将经等离子体处理后的聚乳酸非织造材料投入壳聚糖溶液中,浴比1:40,恒温水浴温度为40-60℃,加热时间1h;随后用大量去离子水冲洗掉试样表面物理粘附的壳聚糖溶液,放入烘箱中,在45℃的条件下烘干2h待用。
5.根据权利要求1所述的一种抗菌聚乳酸非织造材料的制备方法,其特征在于:所述步骤(三)中,将硝酸银溶解在去离子水中,配制成硝酸银溶液,硝酸银溶液的质量分数为0.5%-1.2%。
6.根据权利要求5所述的一种抗菌聚乳酸非织造材料的制备方法,其特征在于:所述步骤(三)中,将经壳聚糖接枝整理后的聚乳酸非织造材料投入硝酸银溶液中,浴比1:40,反应温度为室温,反应时间为1h,采用去离子水水洗,水洗后烘干温度为30-60℃。
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