CN110512352A - 一种长效抗菌非织造布的制备方法 - Google Patents

一种长效抗菌非织造布的制备方法 Download PDF

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CN110512352A
CN110512352A CN201910737373.XA CN201910737373A CN110512352A CN 110512352 A CN110512352 A CN 110512352A CN 201910737373 A CN201910737373 A CN 201910737373A CN 110512352 A CN110512352 A CN 110512352A
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葛彦
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Abstract

本发明公开了一种长效抗菌非织造布的制备方法，包括：(1)将N,N‑二(十八烷基丙胺基)甘氨酸与氨丙基三乙氧基硅烷进行了缩合反应，得到有机‑无机复合脂质；(2)将抗菌剂包裹在有机无机复合脂质形成的稳定硅质体中，得到抗菌硅质体溶液；(2)以壳聚糖和聚氧化乙烯为原料通过静电纺丝，得到壳聚糖/聚氧化乙烯非织造布；(4)将壳聚糖/聚氧化乙烯非织造布浸泡在含有四聚磷酸的抗菌硅质体溶液中进行接枝反应，然后采用低温等离子体进行表面处理，低温风干，即得长效抗菌非织造布。本发明制备方法提供的抗菌非织造布具有持久的、广谱性的抗菌效果，具备良好的缓释抗菌和舒适性能，生物相容性好，并带有一定的植物芳香味。

Description

一种长效抗菌非织造布的制备方法
技术领域
本发明涉及纺织工程领域，具体涉及一种长效抗菌非织造布的制备方法。
背景技术
壳聚糖是天然高分子生物多糖甲壳素脱乙酰化产物，具有优良的耐溶剂性和耐碱性，良好的生物相容性与皮肤亲和性，抑菌性、成膜性、透气性、吸水性、保湿性好，可止血、促进伤口愈合等优点，可制成非织造布用作医学材料。采用壳聚糖纳米纤维制作的医用非织造布，其超细的直径和极大的孔隙率可以有效地过滤带病微粒等物质。但是，作为抗菌性的纳米纤维，如果仅仅将抗菌剂与高聚物简单的静电混纺，则不可避免的会出现抗菌药物的突释现象。
因此，在不影响壳聚糖纳米纤维非织造布透气性和孔隙率的前提下赋予非织造布抗菌特性，必须进行抗菌整理。而且壳聚糖、聚氧化乙烯具有一定的水溶性，形成材料后会溶胀崩解，也会造成释放后期的突释效应。另外，现有的抗菌纤维由于抗菌剂与纤维的结合牢度不佳，因此限制了其抗菌作用的持久性。
发明内容
为解决以上技术问题，本发明的目的在于提供一种长效抗菌非织造布的制备方法，使非织造布具有持久的、广谱性的抗菌效果，具备良好的缓释抗菌和舒适性能，生物相容性好。
本发明提供了一种长效抗菌非织造布的制备方法，包括如下步骤：
S1.将10～20g N,N-二(十八烷基丙胺基)甘氨酸溶于100ml三乙胺或者吡啶中，再加入10～20g氨丙基三乙氧基硅烷，在-10～10℃下加入4～8g缩合剂反应4～8h，反应完毕后经硅胶柱层析收集获得有机-无机复合脂质；
S2.将所述有机-无机复合脂质溶于三氯甲烷中，蒸发除去三氯甲烷得到类脂质薄膜，向所述类脂质薄膜中加入抗菌剂，搅拌混匀并迅速加热到45～50℃，维持10～30s同时在水浴中进行超声，之后冷却至4℃后静置，经脂质体挤出器挤出，得到抗菌硅质体溶液；
S3：将壳聚糖和聚氧化乙烯完全溶解于乙酸溶液，搅拌均匀，得到纺丝液，采用所述纺丝液进行静电纺丝，得到壳聚糖/聚氧化乙烯纳米纤维；
S4：向所述抗菌硅质体溶液中加入四聚磷酸，然后将所述壳聚糖/聚氧化乙烯纳米纤维浸泡在含四聚磷酸的抗菌硅质体溶液中，进行接枝反应，然后采用低温等离子体进行表面处理，低温风干，即得长效抗菌非织造布。
优选的，步骤S1中，所述缩合剂包括六氟磷酸苯并三唑-1-基-氧基三吡咯烷基磷、二环己基碳二亚胺和N,N'-羰基二咪唑中的一种或几种。
优选的，步骤S2中，所述有机-无机复合脂质与三氯甲烷混合的质量体积比为100～200:10mg/mL。
优选的，步骤S2中，所述抗菌剂包括茶树精油、尤加利精油和牛至精油中的一种或几种。
优选的，步骤S2中，所述脂质体挤出器采用聚碳酸酯滤膜，所述聚碳酸酯滤膜的孔径为0.5～1.0μm。
优选的，步骤S3中，所述壳聚糖的规格为粘均分子量5.0×105，脱乙酰度为80～85％，所述聚氧化乙烯的规格为平均分子量1.0×106。
优选的，步骤S3中，壳聚糖和聚氧化乙烯的总浓度为10～30g/L，壳聚糖与聚氧化乙烯的质量比为1:1～4。
优选的，步骤S3中，所述乙酸溶液的浓度为90v/v％。
优选的，步骤S4中，所述四聚磷酸浓度为20～40g/L，浸泡的浴比为1:100～300，浸泡温度为0～4℃，浸泡12～24h。
优选的，步骤S4中，低温等离子体处理的条件为：气体采用氮气或氧气，处理功率为250～300W，压强50～60Pa，处理时间为10～15min。
本发明通过将制备得到的壳聚糖/聚氧化乙烯纳米纤维浸入含有四聚磷酸的抗菌硅质体溶液中，利用使抗菌硅质体溶液中的抗菌剂通过硅质体与纳米纤维在四聚磷酸的桥接下结合，牢度较高，可以保持长效抗菌。
附图说明
图1是本发明实施例和对比例整理方法得到的非织造布的抑菌时间曲线对比图。
具体实施方式
根据下述实施例，可以更好地理解本发明。然而，本领域的技术人员容易理解，实施例所描述的内容仅用于说明本发明，而不应当也不会限制权利要求书中所详细描述的本发明。
实施例1
一种长效抗菌非织造布的制备方法，包括如下步骤：
1、制备有机-无机复合脂质：将15g N,N-二(十八烷基丙胺基)甘氨酸溶于100ml三乙胺中，再加入15g氨丙基三乙氧基硅烷，在0℃下加入6g缩合试剂六氟磷酸苯并三唑-1-基-氧基三吡咯烷基磷反应6h，反应完毕后经硅胶柱层析收集获得有机-无机复合脂质；
2、制备抗菌硅质体：称取0.15g有机-无机复合脂质，将有机-无机复合脂质溶于10ml三氯甲烷中，蒸发除去三氯甲烷得到类脂质薄膜；将100ml含30g/L茶树精油溶液加入到所得类脂质薄膜中，搅拌混匀并迅速加热到50℃，热激20s同时水浴超声，冷却至4℃后静置，经聚碳酸酯滤膜脂质体挤出器挤出，滤膜的孔径为1.0μm，得到抗菌硅质体溶液；
3、将0.5g壳聚糖(粘均分子量5.0×105，脱乙酰度为80％)和1.5g聚氧化乙烯(平均分子量1.0×106)完全溶解于100ml 90％(v/v)乙酸溶液，搅拌均匀，得到纺丝液；
4、采用纺丝液进行静电纺丝，使用的注射器规格为10ml，针头规格为平头，7号针；静电纺丝条件为，电压15KV，距离8cm，进样速率1ml/h，温度30℃得到壳聚糖/聚氧化乙烯纳米纤维；
5、在抗菌硅质体溶液中加入30g/L四聚磷酸，将壳聚糖/聚氧化乙烯纳米纤维浸入该溶液，浸泡的浴比为1:200，浸泡温度为4℃，浸泡24h，进行接枝反应；
6、将经接枝反应的纳米纤维采用低温等离子体进行表面处理，低温风干，低温等离子体处理的条件为：气体采用氮气，处理功率为300W，压强60Pa，处理时间为15min。风干温度4℃，相对湿度为20％，即得长效抗菌非织造布。
实施例2
一种长效抗菌非织造布的制备方法，包括如下步骤：
1、制备有机-无机复合脂质：将10g N,N-二(十八烷基丙胺基)甘氨酸溶于100ml吡啶中，再加入10g氨丙基三乙氧基硅烷，在-10℃下加入4g缩合试剂二环己基碳二亚胺反应4h，反应完毕后经硅胶柱层析收集获得有机-无机复合脂质；
2、制备抗菌硅质体：称取0.1g有机-无机复合脂质，将有机-无机复合脂质溶于10ml三氯甲烷中，蒸发除去三氯甲烷得到类脂质薄膜；将150ml含20g/L尤加利精油溶液加入到所得类脂质薄膜中，搅拌混匀并迅速加热到45℃，热激10s同时水浴超声，冷却至4℃后静置，经聚碳酸酯滤膜脂质体挤出器挤出，滤膜的孔径为0.5μm，得到抗菌硅质体溶液；
3、将0.5g壳聚糖(粘均分子量5.0×105，脱乙酰度为85％)和0.5g聚氧化乙烯(平均分子量1.0×106)完全溶解于100ml 90％(v/v)乙酸溶液，搅拌均匀，得到纺丝液；
4、采用纺丝液进行静电纺丝，使用的注射器规格为10ml，针头规格为平头，7号针；静电纺丝条件为，电压12KV，距离7cm，进样速率0.3ml/h，温度25℃得到壳聚糖/聚氧化乙烯纳米纤维；
5、在抗菌硅质体溶液中加入20g/L四聚磷酸，将壳聚糖/聚氧化乙烯纳米纤维浸入该溶液，浸泡的浴比为1:100，浸泡温度为0℃，浸泡12h，进行接枝反应；
6、将经接枝反应的纳米纤维采用低温等离子体进行表面处理，低温风干，低温等离子体处理的条件为：气体采用氧气，处理功率为250W，压强50Pa，处理时间为10min。风干温度4℃，相对湿度为10％，即得长效抗菌非织造布。
实施例3
一种长效抗菌非织造布的制备方法，包括如下步骤：
1、制备有机-无机复合脂质：将20g N,N-二(十八烷基丙胺基)甘氨酸溶于100ml三乙胺中，再加入20g氨丙基三乙氧基硅烷，在10℃下加入8g缩合试剂N,N'-羰基二咪唑反应8h，反应完毕后经硅胶柱层析收集获得有机-无机复合脂质；
2、制备抗菌硅质体：称取0.2g有机-无机复合脂质，将有机-无机复合脂质溶于10ml三氯甲烷中，蒸发除去三氯甲烷得到类脂质薄膜；将25ml含40g/L尤加利精油溶液加入到所得类脂质薄膜中，搅拌混匀并迅速加热到50℃，热激30s同时水浴超声，冷却至4℃后静置，经聚碳酸酯滤膜脂质体挤出器挤出，滤膜的孔径为1.0μm，得到抗菌硅质体溶液；
3、将0.6g壳聚糖(粘均分子量5.0×105，脱乙酰度为85％)和2.4g聚氧化乙烯(平均分子量1.0×106)完全溶解于100ml 90％(v/v)乙酸溶液，搅拌均匀，得到纺丝液；
4、采用纺丝液进行静电纺丝，使用的注射器规格为10ml，针头规格为平头，7号针；静电纺丝条件为，电压20KV，距离10cm，进样速率1.0ml/h，温度35℃得到壳聚糖/聚氧化乙烯纳米纤维；
5、在抗菌硅质体溶液中加入40g/L四聚磷酸，将壳聚糖/聚氧化乙烯纳米纤维浸入该溶液，浸泡的浴比为1:300，浸泡温度为4℃，浸泡24h，进行接枝反应；
6、将经接枝反应的纳米纤维采用低温等离子体进行表面处理，低温风干，低温等离子体处理的条件为：气体采用氮气，处理功率为300W，压强60Pa，处理时间为15min。风干温度10℃，相对湿度为30％，即得长效抗菌非织造布。
对比例1
一种硅质体抗菌非织造布的制备方法，包括如下步骤：
1、制备有机-无机复合脂质：将15g N,N-二(十八烷基丙胺基)甘氨酸溶于100ml三乙胺中，再加入15g氨丙基三乙氧基硅烷，在0℃下加入6g缩合试剂六氟磷酸苯并三唑-1-基-氧基三吡咯烷基磷反应6h，反应完毕后经硅胶柱层析收集获得有机-无机复合脂质；
2、制备抗菌硅质体：称取150mg有机-无机复合脂质，将有机-无机复合脂质溶于10ml三氯甲烷中，蒸发除去三氯甲烷得到类脂质薄膜；将100ml 30g/L茶树精油溶液加入到所得类脂质薄膜中，搅拌混匀并迅速加热到50℃，热激20s同时水浴超声，冷却至4℃后静置，经聚碳酸酯滤膜脂质体挤出器挤出，滤膜的孔径为1.0μm，得到抗菌硅质体溶液；
3、将0.5g壳聚糖(粘均分子量5.0×105，脱乙酰度为80％)和1.5g聚氧化乙烯(平均分子量1.0×106)完全溶解于100ml 90％(v/v)乙酸溶液，搅拌均匀，得到纺丝液；
4、采用纺丝液进行静电纺丝，使用的注射器规格为10ml，针头规格为平头，7号针；静电纺丝条件为，电压15KV，距离8cm，进样速率1ml/h，温度30℃得到壳聚糖/聚氧化乙烯纳米纤维；
5、将壳聚糖/聚氧化乙烯纳米纤维浸入抗菌硅质体溶液，浸泡的浴比为1:200，浸泡温度为4℃，浸泡24h，进行接枝反应；
6、将经接枝反应的纳米纤维低温风干，风干温度4℃，相对湿度为20％，即得硅质体抗菌非织造布。对比例2：
一种抗菌非织造布的制备方法，包括如下步骤：
1、将0.6g壳聚糖(粘均分子量5.0×105，脱乙酰度为85％)和2.4g聚氧化乙烯(平均分子量1.0×106)完全溶解于100ml 90％(v/v)乙酸溶液，搅拌均匀，得到纺丝液；
2、采用纺丝液进行静电纺丝，使用的注射器规格为10ml，针头规格为平头，7号针；静电纺丝条件为，电压20KV，距离10cm，进样速率1.0ml/h，温度35℃得到壳聚糖/聚氧化乙烯纳米纤维；
3、将壳聚糖/聚氧化乙烯纳米纤维浸入25ml 40g/L尤加利精油溶液，浸泡的浴比为1:300，浸泡温度为4℃，浸泡24h，进行接枝反应；
4、将经接枝反应的纳米纤维采用低温等离子体进行表面处理，低温风干，低温等离子体处理的条件为：气体采用氮气，处理功率为300W，压强60Pa，处理时间为15min。风干温度10℃，相对湿度为30％，即得抗菌非织造布。
测试例：抗菌测试
将1g实施例1-3和对比例1-2制备的非织造布放入透析袋中置于200ml 1.2M磷酸钠缓冲液，磁力搅拌进行释放。经过一段时间释放后，取出非织造布利用AATCC100-2004标准检验非织造布对金黄色葡萄球菌的抑菌效果，具体如图1所示。根据图1可以发现，与对比例相比，本发明实施例制备的非织造布，抗菌性能更持久。
以上所述仅是本发明的优选实施方式，应当指出，对于本领域普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (10)

1.一种长效抗菌非织造布的制备方法，其特征在于，包括如下步骤：
S1.将10～20g N,N-二(十八烷基丙胺基)甘氨酸溶于100ml三乙胺或者吡啶中，再加入10～20g氨丙基三乙氧基硅烷，在-10～10℃下加入4～8g缩合剂反应4～8h，反应完毕后经硅胶柱层析收集获得有机-无机复合脂质；
S2.将所述有机-无机复合脂质溶于三氯甲烷中，蒸发除去三氯甲烷得到类脂质薄膜，向所述类脂质薄膜中加入抗菌剂，搅拌混匀并迅速加热到45～50℃，维持10～30s同时在水浴中进行超声，之后冷却至4℃后静置，经脂质体挤出器挤出，得到抗菌硅质体溶液；
S3：将壳聚糖和聚氧化乙烯完全溶解于乙酸溶液，搅拌均匀，得到纺丝液，采用所述纺丝液进行静电纺丝，得到壳聚糖/聚氧化乙烯纳米纤维；
S4：向所述抗菌硅质体溶液中加入四聚磷酸，然后将所述壳聚糖/聚氧化乙烯纳米纤维浸泡在含四聚磷酸的抗菌硅质体溶液中，进行接枝反应，然后采用低温等离子体进行表面处理，低温风干，即得长效抗菌非织造布。
2.根据权利要求1所述的长效抗菌非织造布的制备方法，其特征在于，步骤S1中，所述缩合剂包括六氟磷酸苯并三唑-1-基-氧基三吡咯烷基磷、二环己基碳二亚胺和N,N'-羰基二咪唑中的一种或几种。
3.根据权利要求1所述的长效抗菌非织造布的制备方法，其特征在于，步骤S2中，所述有机-无机复合脂质与三氯甲烷混合的质量体积比为100～200:10mg/mL。
4.根据权利要求1所述的长效抗菌非织造布的制备方法，其特征在于，步骤S2中，所述抗菌剂包括茶树精油、尤加利精油和牛至精油中的一种或几种。
5.根据权利要求1所述的长效抗菌非织造布的制备方法，其特征在于，步骤S2中，所述脂质体挤出器采用聚碳酸酯滤膜，所述聚碳酸酯滤膜的孔径为0.5～1.0μm。
6.根据权利要求1所述的长效抗菌非织造布的制备方法，其特征在于，步骤S3中，所述壳聚糖的规格为粘均分子量5.0×105，脱乙酰度为80～85％，所述聚氧化乙烯的规格为平均分子量1.0×106。
7.根据权利要求1所述的长效抗菌非织造布的制备方法，其特征在于，步骤S3中，壳聚糖和聚氧化乙烯的总浓度为10～30g/L，壳聚糖与聚氧化乙烯的质量比为1:1～4。
8.根据权利要求1所述的长效抗菌非织造布的制备方法，其特征在于，步骤S3中，所述乙酸溶液的浓度为90v/v％。
9.根据权利要求1所述的一种长效抗菌非织造布的制备方法，其特征在于，步骤S4中，所述四聚磷酸浓度为20～40g/L，浸泡的浴比为1:100～300，浸泡温度为0～4℃，浸泡12～24h。
10.根据权利要求1所述的一种长效抗菌非织造布的制备方法，其特征在于，步骤S4中，低温等离子体处理的条件为：气体采用氮气或氧气，处理功率为250～300W，压强50～60Pa，处理时间为10～15min。
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