CN105803777B - 一种抗菌材料的制造方法 - Google Patents
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Abstract
本发明提供一种抗菌材料的制造方法，通过对抗菌液和基布的原料和工艺的改进，获得兼具透气性、快速抗菌和持久抗菌的抗菌材料。包括以下步骤：步骤1.抗菌液的制备；步骤2.抗菌基材的制造；步骤3.过滤成型。主要采用聚乳酸热塑性聚合物静电纺丝工艺制成纤维膜后对具有良好抗菌性能的抗菌液抽真空过滤，在基材表面附着抗菌物质，然后烘干制成抗菌材料。
Description
技术领域
本发明涉及一种抗菌材料的制造方法。
背景技术
抗菌材料是指自身具有杀灭或抑制微生物功能的一类新型功能材料。在医疗领域、家庭用品、家用电器、食品包装等领域有极其广阔的应用前景，在人们对环境卫生要求日益提高的今天，抗菌材料的应用受到更加广泛的关注。目前的抗菌整理技术主要有三类1.共混纺丝法：先将抗菌剂加入纺丝材料中制成抗菌纤维，然后制成抗菌纺织品。该法抗菌效果持久，耐洗性好，但技术含量高，难度大，涉及领域广，抗菌剂要求高；常用来生产合成类纤维产品。2. 后整理法：在织物印染后整理过程中加入抗菌剂(常被称为抗菌整理剂)，然后制成各种抗菌纺织品。该法加工处理较为简单，而耐洗性及抗菌效果持久性较差。3.复合整理法:先将抗菌剂加入到纺丝材料中制成抗菌纤维，在织物印染后整理过程中加入抗菌整理剂，然后制成抗菌纺织品，这种方法仅在具有高抗菌性能要求的特殊产品中使用，限制了使用范围。目前的方法都难以同时达到透气透湿、耐久抗菌的性能。
发明内容
为解决以上问题，本发明采用以下技术方案：
步骤1.抗菌液的制备
第一步，分别配制质量百分比浓度为5-10%的甲基纤维素水溶液和质量百分比浓度为8-11％的硫酸铜溶液，备用；
第二步，在微波震荡或者高速搅拌下，向上述铜盐溶液中，缓慢加入壳聚糖，并保持微波震荡或者高速搅拌30-120min，得到混合溶液A； 其中，壳聚糖在混合溶液A中的质量分数为7-10％；
第三步，在超声波震荡或者高速搅拌下，按体积比7︰4~5︰9的比例，将上述混合溶液A缓慢加入到上述甲基纤维素水溶液中；
然后，在40℃下，按与铜离子的摩尔比为1︰1.2的比例，加入抗坏血酸反应30~45min，然后加入质量分数为2-3%果胶、5-8%海藻酸钠得到混合液，然后将所得液体负压除泡、静置，再陈化36h，得到抗菌液；
步骤2.抗菌基材的制造
1)将质量比为1∶1～50的聚乳酸和热塑性聚合物溶解于有机溶剂中形成纺丝溶液；
2)将聚乳酸热塑性聚合物纺丝溶液置入静电纺丝机注射器中，在8～30kV电压下，于接收电极上得到聚乳酸聚合物复合纤维膜；
3)在50～100℃的真空条件下去除有机溶剂，得聚乳酸聚合物复合纤维膜；
本发明提供的制备方法步骤1)中的热塑性聚合物为聚醚酮酮、聚醚醚酮、聚醚酰亚胺、聚砜、聚醚砜、酚酞改性聚醚砜、聚苯硫醚、聚苯醚或聚酰胺。
本发明提供的制备方法步骤1)中的有机溶剂为四氢呋喃、二氯乙烷、四氯乙烷、二氯甲烷、三氯甲烷、N，N-二甲基甲酰胺、N，N-二甲基乙酰胺或N，N-二甲基吡咯烷酮。
本发明提供的制备方法步骤2)中的接收电极与发射电极间的距离为8～23cm。
本发明提供的制备方法步骤2)中静电纺丝机制得的聚乳酸聚合物复合纤维的直径为 10～50nm。
本发明提供的制备方法步骤3)中制得的聚乳酸聚合物复合纤维膜的厚度为5～50μm，宽度为5～40cm。
步骤3.过滤成型
用步骤2制得的聚乳酸聚合物复合纤维膜过滤步骤1的抗菌凝胶液，每平方厘米过滤量为3-9ml，底部采用抽滤机进行室温下抽滤，抽滤机以1-2分米/分钟的速度进行往复运动，过滤时间为1-2小时，过滤完成后通过160～180℃烘道，保留时间15分钟，出烘道经冷却后制得。
与最接近的现有技术比，本发明提供的技术方案具有以下有益效果：
1)本发明提供的聚乳酸聚合物复合纤维膜因其具有多孔结构，利于聚氨酯加热时在层间的流动，提高材料内部结构的均匀性；
2)聚乳酸聚合物复合纤维膜因其具有多孔结构保证了材料的透气性优异；
3）以甲基纤维素为连续相，掺杂沉积纳米氧化亚铜，制备出生物相容性好、 透气性好、抗菌性能优异的复合抗菌膜医用材料。
4）产品的透气性、吸水性好，，具有快速抗菌，和耐久抗菌性能好。
5）工艺流程短、工艺控制简便，生产成本低廉。
具体实施方式
实施例1
步骤1.抗菌液的制备
第一步，分别配制质量百分比浓度为5%的甲基纤维素水溶液和质量百分比浓度为8％的硫酸铜溶液，备用；
第二步，在微波震荡或者高速搅拌下，向上述铜盐溶液中，缓慢加入壳聚糖，并保持微 波震荡或者高速搅拌30-120min，得到混合溶液A； 其中，壳聚糖在混合溶液A中的质量分数为10％；
第三步，在超声波震荡或者高速搅拌下，按体积比7︰4的比例，将上述混合溶液A缓慢加入到上述甲基纤维素水溶液中；
然后，在40℃下，按与铜离子的摩尔比为1︰1.2的比例，加入抗坏血酸反应45min，然后加入质量分数为2-3%果胶、5-8%海藻酸钠得到混合液，然后将所得凝胶负压除泡、静置，再陈化36h，得到抗菌液；
步骤2.抗菌基材的制备
1)将质量比为1∶1～50的聚乳酸和聚酰胺溶解于有机溶剂中形成纺丝溶液；
2)将聚乳酸热塑性聚合物纺丝溶液置入静电纺丝机注射器中，在8～30kV电压下，于接收电极上得到聚乳酸聚合物复合纤维膜；
3)在50～100℃的真空条件下去除有机溶剂，得聚乳酸聚合物复合纤维膜；
步骤3.过滤成型
用步骤2制得的聚乳酸聚合物复合纤维膜过滤步骤1的抗菌液，每平方厘米过滤量为3-9ml，底部采用抽滤机进行抽滤，抽滤机以1-2分米/分钟的速度进行往复运动，过滤时间为1-2小时，过滤完成后附着有聚氨酯树脂的复合纤维膜通过160℃烘道，保留时间15分钟，出烘道经冷却后制得。
实施例2
步骤1.抗菌液的制备
第一步，分别配制质量百分比浓度为10%的甲基纤维素水溶液和质量百分比浓度为11％的硫酸铜溶液，备用；
第二步，在微波震荡或者高速搅拌下，向上述铜盐溶液中，缓慢加入壳聚糖，并保持微 波震荡或者高速搅拌120min，得到混合溶液A； 其中，壳聚糖在混合溶液A中的质量分数为10％；
第三步，在超声波震荡或者高速搅拌下，按体积比7︰4的比例，将上述混合溶液A缓慢加入到上述甲基纤维素水溶液中；
然后，在40℃下，按与铜离子的摩尔比为1︰1.2的比例，加入抗坏血酸反应45min，然后加入质量分数为2-3%果胶、5-8%海藻酸钠得到混合液，然后将所得凝胶负压除泡、静置，再陈化36h，得到抗菌液；
步骤2.抗菌基材的制备
1)将质量比为1∶1～50的聚乳酸和聚砜溶解于四氢呋喃中形成纺丝溶液；
2)将聚乳酸热塑性聚合物纺丝溶液置入静电纺丝机注射器中，在8～30kV电压下，于接收电极上得到聚乳酸聚合物复合纤维膜；
3)在50～100℃的真空条件下去除有机溶剂，得聚乳酸聚合物复合纤维膜；
步骤3.过滤成型
用步骤2制得的聚乳酸聚合物复合纤维膜过滤步骤1的抗菌液，每平方厘米过滤量为3-9ml，底部采用抽滤机进行抽滤，抽滤机以1-2分米/分钟的速度进行往复运动，过滤时间为1-2小时，过滤完成后通过130℃烘道，保留时间15分钟，出烘道经冷却后制得。
比较例1
步骤2基布采用聚酯超细纤维膜，其他步骤同实施例1。
比较例2
步骤1中抗菌液由壳聚糖5～9份、噻菌灵0.1～1份、聚乙二醇0.1～3份、甲基乙内酰脲类化合物0.1～2份、过氧乙酸2～5份组成。其他步骤同实施例2。
对具体实施例进行性能测试，采用本领域常规测试方法，测试结果如表1所示，实验表明本发明的抗菌材料能在保持良好透气性的情况下，实现快速发挥抗菌效果以及良好的抗菌耐久性。
表1 抗菌材料透气性能
| 实施例1 | 实施例2 | 比较例1 | 比较例2 | |
| 透气性（dm<sup>3</sup>/min） | 2.8 | 2.7 | 0.95 | 0.8 |
表2 抗菌材料的未洗涤抗菌率
注：抗菌率“***”：≥99%，“**”：≥90%，“*”≥50%，“—”： <50%
表3 经50次洗涤后抗菌材料的抗菌率
Claims (1)
1.一种抗菌材料的制作方法，具体包括如下步骤：
步骤1.抗菌液的制备
第一步，分别配制质量百分比浓度为5-10%的甲基纤维素水溶液和质量百分比浓度为8-11％的硫酸铜溶液，备用；
第二步，在微波震荡或者高速搅拌下，向上述铜盐溶液中，缓慢加入壳聚糖，并保持微波震荡或者高速搅拌30-120min，得到混合溶液A； 其中，壳聚糖在混合溶液A中的质量分数为7-10％；
第三步，在超声波震荡或者高速搅拌下，按体积比7︰4~5︰9的比例，将上述混合溶液A缓慢加入到上述甲基纤维素水溶液中；
然后，在40℃下，按与铜离子的摩尔比为1︰1.2的比例，加入抗坏血酸反应30~45min，然后加入质量分数为2-3%果胶、5-8%海藻酸钠得到混合液，然后将所得液体负压除泡、静置，再陈化36h，得到抗菌液；
步骤2. 聚乳酸聚合物复合纤维膜的制造
1)将质量比为1∶1～50的聚乳酸和热塑性聚合物溶解于有机溶剂中形成纺丝溶液；热塑性聚合物为聚醚酮酮、聚醚醚酮、聚醚酰亚胺、 聚砜、聚醚砜、酚酞改性聚醚砜、聚苯硫醚、聚苯醚或聚酰胺；
2)将聚乳酸热塑性聚合物纺丝溶液置入静电纺丝机注射器中，在8～30kV电压下，于接收电极上得到聚乳酸聚合物复合纤维膜；
3)在50～100℃的真空条件下去除有机溶剂，得聚乳酸聚合物复合纤维膜；
步骤3.过滤成型
用步骤2制得的聚乳酸聚合物复合纤维膜过滤步骤1的抗菌液，每平方厘米过滤量为3-9ml，底部采用抽滤机进行室温下抽滤，抽滤机以1-2分米/分钟的速度进行往复运动，过滤时间为1-2小时，过滤完成后通过160～180℃烘道，保留时间15分钟，出烘道经冷却后制得。
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