CN113235186A - 一种抗菌聚乳酸纳米纤维的制备方法 - Google Patents
一种抗菌聚乳酸纳米纤维的制备方法 Download PDFInfo
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Abstract
本发明公开了一种抗菌聚乳酸纳米纤维的制备方法。首先将聚乳酸、海藻酸钠、聚乙二醇、硝酸银分散于溶剂中制备纺丝液,然后采用静电辅助的溶液喷射纺丝方法来制备聚乳酸纳米纤维,最后通过紫外光辐照,还原纤维组分中的硝酸银,得到抗菌聚乳酸纳米纤维。本发明通过引入海藻酸钠(SA)组分来提高纳米纤维的亲水性和在静电辅助拉丝过程中的导向力,能够有效提高纳米纤维尺寸的均匀性。本发明制备的聚乳酸纤维亲水性明显改善,尺寸分布均匀,成型好,抗菌能力强。
Description
技术领域
本发明涉及纳米纤维技术领域,具体涉及一种抗菌聚乳酸纳米纤维的制备方法。
背景技术
纳米纤维具有较高的孔隙率,由纳米纤维构建的纳米纤维膜具有三维网络结构,因而在组织工程、医用材料等领域具有潜在应用前景。聚乳酸(PLA)是一种可天然降解的材料,来源丰富并且可以再生。
将PLA纺丝为纳米纤维,目前已有较多文献报道。PLA的纺丝一般采用熔融纺丝、静电纺丝或者溶液喷射法进行。如曲良俊(申请号201310194327.2)以熔融纺丝法制备一种聚乳酸/银复合导电纤维,纤维的电导率可达2.4S/cm。沈文等(申请号201910307469 .2)以氯仿和二甲基亚砜作为溶剂,采用静电纺丝法制备了一种隔菌聚乳酸超细纳米纤维,发现聚乳酸纳米纤维可有效地起到隔菌抗感染的作用,增强药物或抗生素的释放,促进伤口的愈合。张瑾等(申请号201910050604.X)基于溶液喷射纺丝方法得到了一种抗菌纳米纤维膜,纤维膜中的银盐可均匀缓慢释放银离子,具有持久杀菌效果。
静电纺丝是借助于高压电场形成纤维,而溶液喷射纺丝是借助于高压气流的导向力,在高速气流牵引作用下对纺丝溶液拉伸细化并且使溶剂在空气中快速挥发,从而得到更细的纤维。溶液喷射法作为一种新型纺丝技术,其优点在于安全、能耗低、方便易行等。与常规的静电纺丝和熔融纺丝相比,其缺点也较为明显,由于高速气流的变化和喷射溶液的变化,纤维的尺寸分布不均匀。对静电辅助的溶液喷射纺丝而言,如何获得尺寸均一的纤维至关重要。
为了提高纤维的应用范围和使用效果,赋予纤维特殊的功能性也是市场需求之一,如超强纤维、抗菌纤维、高水蒸气通透纤维等。为了提高聚乳酸纤维的抗菌能力,一般向材料中加入有机抗菌剂、纳米二氧化钛粒子、纳米氧化锌、季铵盐、银盐或纳米银等。由于PLA具有疏水的特性,很难吸收生物组织渗出液,其抗菌效果往往不理想。
发明内容
本发明的目的在于提供一种抗菌聚乳酸纳米纤维的制备方法,解决聚乳酸纤维尺寸均匀性以及聚乳酸纤维在组织工程中难以有效抗菌的问题。
本发明采用静电辅助的溶液喷射纺丝方法来制备抗菌聚乳酸纳米纤维,通过引入海藻酸钠(SA)组分来提高纳米纤维的亲水性和在静电辅助拉丝过程中的导向力,能够有效提高纳米纤维尺寸的均匀性,并且通过紫外光辐照,还原纤维组分中的硝酸银,得到纳米银抗菌活性组分。
本发明抗菌聚乳酸纤维制备方法具体步骤如下:
1)按照重量份数依次取聚乳酸4-10份、海藻酸钠1-4份、聚乙二醇1份、硝酸银0.3-2份、溶剂82-94份,备用;
2)将步骤1)中的聚乳酸、海藻酸钠、聚乙二醇、硝酸银分散于溶剂中,强力搅拌均匀后,得到纺丝液,备用;
3)采用静电辅助的溶液喷射纺丝方法将步骤2)的纺丝液制成聚乳酸纳米纤维;
4)用紫外光辐照步骤3)制得的聚乳酸纳米纤维,将组分中的硝酸银还原得到纳米银抗菌活性组分,最终得到抗菌聚乳酸纳米纤维。
进一步的,步骤1)和步骤2)中所述溶剂为丙酮和二甲基甲酰胺的混合,丙酮和二甲基甲酰胺的体积比为9:1。
进一步的,步骤3)静电辅助溶液喷射纺丝的工艺过程中,纺丝液的供料速率为10mL/h、纺丝针孔为0.5 mm、高速气流牵伸风量为20 slpm、纺丝箱温度为70℃。
进一步的,步骤4)中用紫外光辐照时间为5分钟,紫外灯功率为20kW。
本发明的优点及有益效果:
1、采用丙酮和二甲基甲酰胺混合作为溶剂,可有效溶解聚乳酸、海藻酸钠和硝酸银三种原料;并且丙酮和二甲基甲酰胺均为有机溶剂,在静电辅助溶液喷射纺丝的过程中易于挥发,更利于纺丝液成丝。
2、添加海藻酸钠(SA)组分,一方面增加了纳米纤维的亲水性,另一方面可有效提高纳米纤维尺寸的均匀性。由于海藻酸钠分子链含有大量的羧基极性基团,在外加电场作用下,含有海藻酸钠的聚乳酸液滴不仅受到来自于纺丝喷嘴的压力,还受到强电场的作用力,在两种强的作用力下,聚乳酸液滴被迅速拉为线状,由于有机溶剂的迅速挥发,从而得到具有尺寸均匀性的聚乳酸纤维。
3、本发明中的银离子还原为纳米银,一方面降低了银离子的重金属离子毒害,另一方面降低银离子的迁移,使纤维具有更长久的抗菌能力。
综上所述,本发明方法制备的抗菌聚乳酸纳米纤维,尺寸分布均匀,成型好,亲水性明显改善,抗菌能力强。
具体实施方式
为更好的理解本发明,下面结合实例对本发明做进一步说明,但是本发明要求保护范围并不局限于实施例的表述范围。
实施例1
1)按照重量份数依次取聚乳酸4份、海藻酸钠1份、聚乙二醇1份、硝酸银0.3份、溶剂94份,备用。溶剂为丙酮和二甲基甲酰胺按体积比9:1混合制得;
2)将聚乳酸、海藻酸钠、聚乙二醇、硝酸银分别加入到溶剂中,搅拌均匀后得到纺丝液,备用;
3)采用静电辅助的溶液喷射纺丝方法将步骤2)的纺丝液制成聚乳酸纳米纤维。其中,静电电压为5kV、纺丝液的供料速率为:10ml/h、纺丝针孔为0.5 mm、高速气流牵伸风量为20 slpm、纺丝箱温度为70℃;
4)用紫外光辐照步骤3)制得的聚乳酸纳米纤维,辐照时间为5分钟,紫外灯功率为20kW。将组分中的硝酸银还原得到纳米银抗菌活性组分,最终得到抗菌聚乳酸纳米纤维。
实施例2
1)按照重量份数依次取聚乳酸10份、海藻酸钠4份、聚乙二醇1份、硝酸银2份、溶剂83份,备用。溶剂为丙酮和二甲基甲酰胺按体积比9:1混合制得;
2)将聚乳酸、海藻酸钠、聚乙二醇、硝酸银分别加入到溶剂中,搅拌均匀后得到纺丝液,备用;
3)采用静电辅助的溶液喷射纺丝方法将步骤2)的纺丝液制成聚乳酸纳米纤维。其中,静电电压为5kV、纺丝液的供料速率为:10ml/h、纺丝针孔为0.5 mm、高速气流牵伸风量为20 slpm、纺丝箱温度为70℃;
4)用紫外光辐照步骤3)制得的聚乳酸纳米纤维,辐照时间为5分钟,紫外灯功率为20kW。将组分中的硝酸银还原得到纳米银抗菌活性组分,最终得到抗菌聚乳酸纳米纤维。
实施例3
1)按照重量份数依次取聚乳酸8份、海藻酸钠2份、聚乙二醇1份、硝酸银1份、溶剂88份,备用。溶剂为丙酮和二甲基甲酰胺按体积比9:1混合制得;
2)将聚乳酸、海藻酸钠、聚乙二醇、硝酸银分别加入到溶剂中,搅拌均匀后得到纺丝液,备用;
3)采用静电辅助的溶液喷射纺丝方法将步骤2)的纺丝液制成聚乳酸纳米纤维。其中,静电电压为5kV、纺丝液的供料速率为:10ml/h、纺丝针孔为0.5 mm、高速气流牵伸风量为20 slpm、纺丝箱温度为70℃;
4)用紫外光辐照步骤3)制得的聚乳酸纳米纤维,辐照时间为5分钟,紫外灯功率为20kW。将组分中的硝酸银还原得到纳米银抗菌活性组分,最终得到抗菌聚乳酸纳米纤维。
对比例1
不添加静电场,直接以溶液喷射纺丝法制备抗菌聚乳酸纳米纤维,其他工艺参数与实施例3一致。
对比例2
不添加海藻酸钠,其他工艺参数与实施例2一致。
对比例3
改变静电场电压为15kV,其他工艺参数与实施例2一致。
对比例4
改变静电场电压为20kV,其他工艺参数与实施例2一致。
对各实施例和对比例制得的纤维样品进行纤维直径分布范围测量和抑菌性能测试,抑菌性能具体测试方法如下:
将样品对金葡球菌的抗菌性能进行测试,取尺寸为1cm×1cm样品,利用紫外光消毒30min。然后取10μL金葡球菌菌液滴在样品表面,接着滴加1mL PBS缓冲液使样品保持湿润状态,在37℃恒温培养箱中培育2h后,将样品取出,置于5mL PBS缓冲液冲中震荡,然后取适量的经过震荡后得到的PBS溶液稀释1000倍,滴在凝胶培养皿表面进行细菌培养,24小时进行平板菌落计数,对抗菌膜的抗菌活性进行评价,测量和测试结果如下表所示:
对比上表发现,改变溶液中聚乳酸浓度会导致纤维的直径变化,其他条件一定的条件下,聚乳酸的浓度越高,纤维直径越大。同时,静电场电压和海藻酸钠的含量会影响纤维直径的分布,其他条件不变的情况下,引入海藻酸钠使得纤维直径分布均匀,海藻酸钠含量大,纤维的直径分布越均匀。在实验范围内,静电场电压15kV使纤维直径分布最窄。纤维的抗菌性能受电场影响不大,电场电压越大,使得纺丝液中银离子团聚,会稍微降低材料的抗菌性能。
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,虽然本发明已以较佳实施例揭露如上,然而并非用以限定本发明,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,当可利用上述揭示的技术内容作出些许更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明技术方案的范围内。
Claims (5)
1.一种抗菌聚乳酸纳米纤维的制备方法,其特征在于包括以下步骤:
1)按照重量份数依次取聚乳酸4-10份、海藻酸钠1-4份、聚乙二醇1份、硝酸银0.3-2份、溶剂82-94份,备用;
2)将步骤1)中的聚乳酸、海藻酸钠、聚乙二醇、硝酸银分散于溶剂中,搅拌均匀后得到纺丝液,备用;
3)采用静电辅助的溶液喷射纺丝方法将步骤2)的纺丝液制成聚乳酸纳米纤维;
4)用紫外光辐照步骤3)制得的聚乳酸纳米纤维,将组分中的硝酸银还原得到纳米银抗菌活性组分,最终得到抗菌聚乳酸纳米纤维。
2.根据权利要求1所述的抗菌聚乳酸纳米纤维的制备方法,其特征在于步骤1)和步骤2)中所述溶剂为丙酮和二甲基甲酰胺的混合。
3.根据权利要求2所述的抗菌聚乳酸纳米纤维的制备方法,其特征在于丙酮和二甲基甲酰胺的体积比为9:1。
4.根据权利要求1所述的抗菌聚乳酸纳米纤维的制备方法,其特征在于步骤3)静电辅助溶液喷射纺丝的工艺过程中,纺丝液的供料速率为10mL/h、纺丝针孔为0.5 mm、高速气流牵伸风量为20slpm、纺丝箱温度为70℃。
5.根据权利要求1所述的抗菌聚乳酸纳米纤维的制备方法,其特征在于步骤4)中用紫外光辐照时间为5分钟,紫外灯功率为20kW。
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