CN110172784B - 一种梯度结构多层微纳米纤维复合敷料的制备方法 - Google Patents

一种梯度结构多层微纳米纤维复合敷料的制备方法 Download PDF

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CN110172784B
CN110172784B CN201910425173.0A CN201910425173A CN110172784B CN 110172784 B CN110172784 B CN 110172784B CN 201910425173 A CN201910425173 A CN 201910425173A CN 110172784 B CN110172784 B CN 110172784B
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CN110172784A (zh
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杜磊
徐煜
王文召
李涛
邹奉元
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Blue Sky Smart Technology Group Co ltd
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Abstract

本发明公开了一种梯度结构多层微纳米纤维复合敷料的制备方法，包括以下步骤(1)配制静电纺丝前驱液；(2)利用两台纺丝机进行纺丝，纺丝前将静电纺丝前驱液分别装入纺丝机的纺丝喷头中，并设定纺丝参数；两台纺丝机处于同一水平面且纺丝喷头彼此相对，以滚筒为接收装置，放置在纺丝机中间；(3)纺丝时，接收装置两端的纺丝喷头以一定的速度向下移动，所得到的微纳米纤维复合敷料在组分构成和空间结构均具有梯度结构。本发明利用静电场非均匀分布这一特点，以“递进交叉对喷法”可一步实现制备组分和孔径均为梯度结构的微纳米纤维复合敷料制备。该方法可以对孔径结构进行可控调节，又可在不同组分上负载不同药物，协同加速创面修复。

Description

一种梯度结构多层微纳米纤维复合敷料的制备方法
技术领域
本发明属于生物医用纺织品领域，具体涉及一种梯度结构多层微纳米纤维复合敷料的制备方法。
背景技术
人体的皮肤是维持人体内环境稳定和阻止病原体侵入的有效屏障。当皮肤创伤发生后，皮肤正常的生理功能将遭到破坏。创伤修复是一个动态且复杂的过程，其中包括炎症反应、肉芽重建、以及组织塑形三个阶段。医用敷料既可起到皮肤屏障功能的部分作用，保护人体免受到更大的损伤；又可为创伤修复提供一个有利的微环境，进而加速创伤愈合。理想的敷料应具备如下属性：要能够在对渗出液的吸收控制的同时，还能为肉芽组织重建提供一个湿润的环境；要提供有序的孔径结构，引导成纤维细胞增殖。此外还要赋予敷料抗菌活性和有效促进成纤维细胞增殖迁移的性能。
通过对加工工艺进行设计和控制，制备出具有特定结构、理化性能的功能敷料是当前的研究热点，也是国产高性能敷料打破国外市场垄断的必由之路。在众多敷料加工手段中，静电纺丝技术早已被公认为是制备功能性敷料的首选方法之一。但目前静电纺丝敷料较多的研究还是聚焦于制备随机排列或者定向排列的均质结构的纤维膜。然而，具有梯度结构的多层微纳米复合纤维敷料，才能最大程度仿生细胞外基质的结构，更加利于加速细胞和组织的生长，促进受损皮肤修复。
发明内容
本发明的目的在于提供一种梯度结构多层微纳米纤维复合敷料的制备方法，利用静电场非均匀分布这一特点，以“递进交叉对喷法”可一步实现制备组分构成和空间结构均为梯度结构的微纳米纤维复合敷料制备。该方法可以对孔径结构进行可控调节，又可在不同组分上负载不同药物，协同加速创面修复。
为了解决上述技术问题，采用如下技术方案：
一种梯度结构多层微纳米纤维复合敷料的制备方法，其特征在于包括如下步骤：
(1)以亲水性高聚物、疏水性高聚物及药物为原料配制成静电纺丝前驱液；
(2)利用两台纺丝机进行纺丝，分别制备疏水性微米纤维和亲水性纳米纤维；纺丝前将静电纺丝前驱液分别装入纺丝机的纺丝喷头中，并设定纺丝参数；两台纺丝机处于同一水平面且纺丝喷头彼此相对，以滚筒为接收装置，放置在纺丝机中间；
(3)纺丝时，接收装置两端的纺丝喷头以一定的速度向下移动。此时，在接收辊上指定区域所接收到纤维的比例不断变化，随着纺丝时间增长，所得到的微纳米纤维复合敷料在组分构成和空间结构均具有梯度结构。
优选后，在制备静电纺丝前驱液时，将亲水性高聚物、疏水性高聚物分别溶解于纯水和有机溶剂中，磁力搅拌至完全溶解，并将药物加入溶液中，使亲水性高聚物、疏水性高聚物和所述药物混合均匀，配制成静电纺丝前驱液。本发明在制备前驱液中通过纯水与有机溶剂作为溶剂混合亲水性高聚物、疏水性高聚物及药物。
优选后，所述的亲水性高聚物为聚乙烯醇、聚氧化乙烯或聚乙烯吡络烷酮中的一种。上述亲水性高聚物具有良好可纺性，同时溶液具有较高的粘度，防止药物团聚，有利于药物的均匀分散，保证药物活性，赋予其缓释效果。
优选后，所述的疏水性高聚物为聚己内酯、聚氨酯或聚乳酸中的一种。上述疏水性高聚物溶液具有较高的粘度，有利于药物的均匀分散，保证药物活性。
优选后，所述的有机溶剂为二氯甲烷、三氯甲烷、二甲基甲酰胺、二甲基亚砜或四氢呋喃中的一种。上述有机溶剂对于疏水性高聚物具有良好的溶解性。
优选后，所述的药物为抗菌性药物、维生素、生长因子中的一种或多种。抗菌性药物负载于亲水性纳米纤维上，具有抗菌功能，率先释放，在炎症反应发挥作用，防止伤口感染；维生素及生长因子负载于疏水性微米纤维上，随后释放，促进成纤维细胞生长。两种或多种药物负载，协同加速创伤修复。
优选后，所述的抗菌性药物为纳米银、纳米二氧化钛、氧化锌、四环素、环丙沙星盐酸或头孢唑啉中的一种；所述的维生素为维生素C、维生素B6、或维生素B12中的一种；所述的生长因子为重组人表皮生长因子或血管内皮生长因子。
优选后，所述步骤(2)中的纺丝参数为：纺丝电压为10-16kV，接收距离为12-15cm，接收辊的转速为150-400rpm，纺丝液的推进速率为8-16μL/min，纺丝时间为4-8h；并对纺丝参数进行微调，使亲水性纳米纤维和疏水性微米纤维在相同的纺丝时间内所接收的膜具有相同的宽度。通过调整纺丝参数，使得亲水性纳米纤维和疏水性微米纤维在相同的纺丝时间内所接收的膜具有相同的宽度，以提高复合敷料的使用效果。
优选后，所述步骤(2)中还需要调节亲水性纳米纤维和疏水性微米纤维的在接收装置上的接收位置，使两个纺丝喷头之间的水平位置为膜宽度的一半。
优选后，在纺丝结束后，将纺制所得的多层微纳米纤维复合敷料，在75％乙醇蒸汽进行交联，交联温度为25℃-35℃，交联时间为12h-36h，并在真空干燥箱中干燥24h。通过蒸汽进行交联，提高了纤维复合敷料的水稳定性。
由于采用上述技术方案，具有以下有益效果：
本发明为一种梯度结构多层微纳米纤维复合敷料的制备方法，利用静电场非均匀分布这一特点，以“递进交叉对喷法”可一步实现制备组分构成和空间结构均为梯度结构的微纳米纤维复合敷料制备。该方法可以对孔径结构进行可控调节，又可在不同组分上负载不同药物，亲水性纳米纤维可负载亲水性抗菌药物，疏水性微米纤维负载促进成纤维细胞生长的药物，协同加速创面修复。
由亲水性纳米纤维接触伤口有效吸收创面溢出液；疏水性微米纤维位于敷料表面，可有效阻隔外界污染物。
呈梯度变化的孔径结构既能够促进细胞的迁移、增殖，又能够增强蛋白质与细胞表面的沟通。
该方法得到的纳米纤维复合物赋予敷料多重功能，同时该方法也为梯度结构纳米纤维复合物的可控制备提供有益借鉴。
一步法的制备过程操作简便，制备速度快，适合于量产，具有显著的经济效益与社会效益。
附图说明
下面结合附图对本发明做进一步说明：
图1为“递进式交叉对喷”微/纳米纤维装置示意图；
图2为两个纺丝喷头均以一定速度向下滑动；W区域内，微/纳米纤维沉积比例动态变化。
图3图三为所制得多层微纳米纤维复合敷料电镜照片，可见其孔径和组分呈现梯度变化。
具体实施方式
如图1至图3所示，本发明的多层微纳米纤维复合敷料由利用静电纺丝技术所制备的亲水性高聚物纳米纤维和疏水性高聚物微米纤维共同构成。亲水性纳米纤维可负载亲水性抗菌药物，接触创面；疏水性微米纤维负载促进成纤维细胞生长的药物，隔绝外界污染物，协同加速创面修复。利用静电场非均匀分布这一特点，本发明以“递进交叉对喷法”一步实现制备组分和孔径均为梯度结构的微/纳米纤维复合敷料。
一种梯度结构多层微纳米纤维复合敷料的制备方法，
(1)以亲水性高聚物、疏水性高聚物及药物为原料配制成静电纺丝前驱液；在制备静电纺丝前驱液时，将亲水性高聚物、疏水性高聚物分别溶解于纯水和有机溶剂中，磁力搅拌至完全溶解，并将药物加入溶液中，使亲水性高聚物、疏水性高聚物和所述药物混合均匀，配制成静电纺丝前驱液。本发明在制备前驱液中通过纯水与有机溶剂作为溶剂混合亲水性高聚物、疏水性高聚物及药物。
其中，所述的亲水性高聚物为聚乙烯醇、聚氧化乙烯或聚乙烯吡络烷酮中的一种。上述亲水性高聚物具有良好可纺性，同时溶液具有较高的粘度，防止药物团聚，有利于药物的均匀分散，保证药物活性，赋予其缓释效果。
所述的疏水性高聚物为聚己内酯、聚氨酯或聚乳酸中的一种。上述疏水性高聚物具有较高的粘度，有利于药物的均匀分散，保证药物活性。
所述的有机溶剂为二氯甲烷、三氯甲烷、二甲基甲酰胺、二甲基亚砜或四氢呋喃中的一种。上述有机溶剂对于疏水性高聚物具有良好的溶解性。
所述的药物为抗菌性药物、维生素、生长因子中的一种或多种。抗菌性药物分为纳米粒子与抗生素，纳米粒子可以为纳米银、纳米二氧化钛或氧化锌；抗生素可以为四环素、环丙沙星盐酸或头孢唑啉；维生素可以为维生素C、维生素B6或维生素B12；生长因子可以为重组人表皮生长因子或血管内皮生长因子。抗菌性药物负载于亲水性纳米纤维上，具有抗菌功能；维生素及生长因子负载于疏水性微米纤维上，促进成纤维细胞生长的药物，实现多药物负载，协同加速创伤修复。
(2)利用两台纺丝机1进行纺丝(如图1所示)，分别制备疏水性微米纤维和亲水性纳米纤维，两台纺丝机1均由高压电源2供电；纺丝前将静电纺丝前驱液分别装入纺丝机1的10mL纺丝喷头3的针管中，并设定纺丝参数，纺丝参数为：纺丝电压为10-16kV，接收距离为12-15cm，接收辊的转速为150-400rpm，纺丝液的推进速率为8-16μL/min，纺丝时间为4-8h；并对纺丝参数进行微调，使亲水性纳米纤维和疏水性微米纤维在相同的纺丝时间内所接收的膜具有相同的宽度。通过调整纺丝参数，使得亲水性纳米纤维和疏水性微米纤维在相同的纺丝时间内所接收的膜具有相同的宽度，以提高复合敷料的使用效果。
两台纺丝机1处于同一水平面且纺丝喷头3彼此相对，以滚筒为接收装置4，放置在纺丝机1中间；最后需要调节亲水性纳米纤维和疏水性微米纤维的在接收装置4上的接收位置，使两个纺丝喷头3之间的水平位置为膜宽度的一半。
(3)纺丝时，接收装置4两端的纺丝喷头3以一定的速度向下移动，接收装置4进行同步的旋转。此时，在接收辊上指定区域所接收到纤维的比例不断变化，随着纺丝时间增长，所得到的微纳米纤维复合敷料在组分构成和空间结构均具有梯度结构。
(4)在纺丝结束后，将纺制所得的多层微纳米纤维复合敷料，在75％乙醇蒸汽进行交联，交联温度为25℃-35℃，交联时间为12h-36h，并在真空干燥箱中干燥24h。通过蒸汽进行交联，提高了纤维复合敷料的水稳定性。
以上仅为本发明的具体实施例，但本发明的技术特征并不局限于此。任何以本发明为基础，为解决基本相同的技术问题，实现基本相同的技术效果，所作出地简单变化、等同替换或者修饰等，皆涵盖于本发明的保护范围之中。

Claims (8)

1.一种梯度结构多层微纳米纤维复合敷料的制备方法，其特征在于包括如下步骤：
(1)以亲水性高聚物与疏水性高聚物及药物为原料配制成静电纺丝前驱液；
(2)利用两台纺丝机进行纺丝，分别制备疏水性微米纤维和亲水性纳米纤维；纺丝前将静电纺丝前驱液分别装入纺丝机的纺丝喷头中，并设定纺丝参数；两台纺丝机处于同一水平面且纺丝喷头彼此相对，以滚筒为接收装置，放置在纺丝机中间；
其中，纺丝电压为10-16kV，接收距离为12-15cm，接收辊的转速为150-400rpm，纺丝液的推进速率为8-16μL/min，纺丝时间为4-8h；并对纺丝参数进行微调，使亲水性纳米纤维和疏水性微米纤维在相同的纺丝时间内所接收的膜具有相同的宽度；还需要调节亲水性纳米纤维和疏水性微米纤维的在接收装置上的接收位置，使两个纺丝喷头之间的水平位置为膜宽度的一半；
(3)纺丝时，接收装置两端的纺丝喷头以一定的速度向下移动，此时，在接收辊上指定区域所接收到纤维的比例不断变化，随着纺丝时间增长，所得到的微纳米纤维复合敷料在组分构成和空间结构均具有梯度结构。
2.根据权利要求1所述的一种梯度结构多层微纳米纤维复合敷料的制备方法，其特征在于：在制备静电纺丝前驱液时，将亲水性高聚物、疏水性高聚物分别溶解于纯水和有机溶剂中，磁力搅拌至完全溶解，并将药物加入溶液中，使亲水性高聚物、疏水性高聚物和所述药物混合均匀，配制成静电纺丝前驱液。
3.根据权利要求2所述的一种梯度结构多层微纳米纤维复合敷料的制备方法，其特征在于：所述的亲水性高聚物为聚乙烯醇、聚氧化乙烯或聚乙烯吡络烷酮中的一种。
4.根据权利要求2所述的一种梯度结构多层微纳米纤维复合敷料的制备方法，其特征在于：所述的疏水性高聚物为聚己内酯、聚氨酯或聚乳酸中的一种。
5.根据权利要求2、3、4任意一项所述的一种梯度结构多层微纳米纤维复合敷料的制备方法，其特征在于：所述的有机溶剂为二氯甲烷、三氯甲烷、二甲基甲酰胺、二甲基亚砜或四氢呋喃中的一种。
6.根据权利要求2所述的一种梯度结构多层微纳米纤维复合敷料的制备方法，其特征在于：所述的药物为抗菌性药物、维生素、生长因子中的一种或多种。
7.根据权利要求6所述的一种梯度结构多层微纳米纤维复合敷料的制备方法，其特征在于：所述的抗菌性药物为纳米银、纳米二氧化钛、氧化锌、四环素、环丙沙星盐酸或头孢唑啉中的一种；所述的维生素为维生素C、维生素B6、或维生素B12中的一种；所述的生长因子为重组人表皮生长因子或血管内皮生长因子。
8.根据权利要求1所述的一种梯度结构多层微纳米纤维复合敷料的制备方法，其特征在于：在纺丝结束后，将纺制所得的多层微纳米纤维复合敷料，在75％乙醇蒸汽进行交联，交联温度为25℃-35℃，交联时间为12h-36h，并在真空干燥箱中干燥24h。
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