CN113521372A - 一种抗菌型医用涂布无纺布的制备方法 - Google Patents
一种抗菌型医用涂布无纺布的制备方法 Download PDFInfo
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- CN113521372A CN113521372A CN202110662733.1A CN202110662733A CN113521372A CN 113521372 A CN113521372 A CN 113521372A CN 202110662733 A CN202110662733 A CN 202110662733A CN 113521372 A CN113521372 A CN 113521372A
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Abstract
本发明公开了一种抗菌型医用涂布无纺布的制备方法，首先，利用硅烷偶联剂对纳米氧化锌晶须和纳米二氧化钛晶须进行改性，将改性晶须混入纺丝原液中纺丝并制成无纺布基体；在氧化石墨烯上负载可持续释放的Ag+得到改性氧化石墨烯，将改性氧化石墨烯、月桂酸酐加入到涂层A中并涂覆在无纺布基体的下表面；将抗菌微胶囊、多孔淀粉混合加入到涂层B中并涂覆到无纺布基体的上表面，经过紫外灯照射得到抗菌型涂布无纺布；本发明通过涂层A、涂层B、无纺布基体的协同作用，制备得到的抗菌型医用涂布无纺布抗菌性能优异，止血作用最强，抗拉伸断裂强度高，遇水可溶，具有非常广阔的应用前景。
Description
技术领域
本发明涉及无纺布技术领域，具体是一种抗菌型医用涂布无纺布的制备方法。
背景技术
无纺布作为一种常用的医疗器械，被广泛运用于一次性口罩、实验服、伤口包扎等情况，目前市面上用于伤口包扎的无纺布仅仅是通过压迫血管来减少血液流失，进行止血，而血液的主要成分为蛋白质，无纺布在吸收血液后，不及时更换就极易造成细菌的滋生从而引发伤口的进一步感染，但是频繁更换无纺布又会造成药物敷料的浪费，且更换过程也十分麻烦，尤其是身边没有专业人士帮忙更换无纺布的话，就很容易导致伤口包扎不完全，增加伤口感染和撕裂的风险。
其次，无纺布在吸收血液后，血液将伤口和无纺布粘附在一起，在更换无纺布时极易扯破伤口，造成伤口的二次撕裂，减缓伤口愈合进程；传统无纺布的抗拉强度也比较差，稍微使点力气便容易断裂，因此人们亟需一种具有强效抗菌作用、抗拉强度高不易断裂、能促进伤口愈合，拆换无纺布时不会对伤口造成撕裂的医用涂布无纺布。
发明内容
本发明的目的在于提供一种抗菌型医用涂布无纺布及其制备方法，以解决现有技术中的问题。
为实现上述目的，本发明提供如下技术方案：
一种抗菌型医用涂布无纺布，所述各原料组分如下：以重量份计，无纺布基体90-100份、涂层A15-25份、涂层B15-25份。
本发明将涂层A涂覆在无纺布基体的下表面，将涂层B涂覆在无纺布基体的上表面，涂层A、涂层B、无纺布基体中均含有抑菌、抗菌物质，在使用时需要将医用无纺布下表面贴附在伤口处，涂层B可有效抑制外部细菌的入侵，预防感染，涂层A可有效抑制伤口内部细菌的滋生，加速伤口愈合，利用涂层A、涂层B、无纺布基体的协同作用，可有效抑菌，加快伤口愈合，降低感染风险。
优选地，所述无纺布基体包括各原料组分如下：以重量份计，改性晶须20-30份、纺丝液70-90份、氯乙酸8-12份、丙烯酸8-12份、二苯甲酮8-12份；所述纺丝液为聚氨酯、聚丙烯、聚羟基乙酸中的一种或多种。
本发明在纺丝液中特别添加有改性晶须，可有效增加医用无纺布的拉伸强度，避免传统医用无纺布拉伸强度不足容易断裂的问题；本发明中添加的晶须为纳米氧化锌晶须和纳米二氧化钛晶须，具有一定的光催化能力和抑菌效果；本发明在制得无纺布A后，将无纺布A先浸没在氢氧化钠中进行碱化处理，又浸没在氯乙酸、丙烯酸、二苯甲酮中进行醚化处理，制得的无纺布基体在具有止血作用的同时还具有可溶的特性，用水可直接溶解无纺布基体，减少了在更换无纺布时因为血液凝固在无纺布上而造成伤口二次撕裂的情况；丙烯酸、二苯甲酮作为催化剂，促进了无纺布基体上羧基的增加，在后期涂覆涂层A时，促进涂层A中改性氧化石墨烯表面环氧基发生开环，从而能将改性氧化石墨烯接枝在无纺布基体表面而不容易脱落。
本发明利用硅烷偶联剂对纳米氧化锌晶须、纳米二氧化钛晶须进行改性，硅烷偶联剂水解产生硅羟基，硅羟基发生脱水缩合，与纳米氧化锌晶须、纳米二氧化钛晶须表面上的羟基发生反应，将纳米氧化锌晶须、纳米二氧化钛晶须表面的羟基替换为硝基,纳米氧化锌晶须、纳米二氧化钛晶须之间的氢键作用力减弱，由于静电相互原理，纳米氧化锌晶须、纳米二氧化钛晶须便均匀分散在纺丝液中而不发生团聚；同时，由于纳米氧化锌晶须、纳米二氧化钛晶须的存在，可以使制得的改性纱线具有粗糙的表面，更有利于后期涂层A、涂层B涂覆的时候形成物理锁扣，增加涂层A、涂层B在无纺布基体上的附着力。
优选地，所述改性晶须包括各原料组分如下：以重量份计，纳米氧化锌晶须20-30份、纳米二氧化钛晶须20-30份、硅烷偶联剂10-16份。
优选地，所述涂层A包括各原料组分如下：以重量份计，改性氧化石墨烯20-30份、月桂酸酐12-14份、冰醋酸10-20份、涂层基料30-60份。
优选地，所述改性氧化石墨烯包括各原料组分如下：以重量份计，氧化石墨烯50-60份、乙酸锌8-10份、氢氧化钠10-20份、硝酸银15-25份。
本发明中的涂层A特别添加有改性氧化石墨烯，在超声分散条件下，乙酸锌中的Zn+被静电吸附到部分改性氧化石墨烯表面的氨基上，同时氢氧化钠发生还原反应，氢氧化钠中的OH-离子与改性氧化石墨烯表面的Zn+反应生成ZnO核，Ag+被吸附在改性氧化石墨烯表面的ZnO核上，且Ag+能持续释放，避免了传统银离子杀菌剂不能够持续杀菌的问题，且不容易脱落；本发明还在涂层A中添加了月桂酸酐，利用涂层A中壳聚糖与月桂酸酐的取代反应，将壳聚糖分子上氨基中的氮原子用月桂酸酐进行取代，制备得到的壳聚糖在保留其辅助伤口愈合、杀菌、凝血作用的同时还具备一定的疏水功能，防止涂层B中多孔淀粉对血液的过多吸附。
优选地，所述涂层B包括各原料组分如下：以重量份计，抗菌微胶囊20-30份、多孔淀粉30-40份、无水碳酸钠10-20份、三偏磷酸钠10-16份、涂层基料40-60份。
优选地，所述抗菌微胶囊包括各原料组分如下：以重量份计，乙基纤维素20-40份、植物提取液20-30份、乳化剂10-18份、明胶30-50份、十二烷基硫酸钠16-18份；所述植物提取液为紫雏菊提取液、生姜提取液、葡萄籽提取液中的一种或多种；所述乳化剂为司班80。
本发明中的涂层B涂覆在无纺布基体的上表面，涂层B中特别添加有抗菌微胶囊和多孔淀粉，利用多孔淀粉来吸收伤口流出的血液，促进血液中血小板、白细胞在伤口处的聚集，加快伤口止血过程；抗菌微胶囊以具有抗菌作用的植物提取液为芯材，以乙基纤维素、明胶为壁材，将抗菌微胶囊分散在涂料B中，抗菌微胶囊表面含有的氨基与涂层A中改性氧化石墨烯表面的部分羧基发生缩合反应，在涂层A与涂层B中形成交联结构，增加了涂层A、涂层B在无纺布基体表面的粘附力，同时，抗菌微胶囊的添加一方面可以通过释放抗菌物质来抵抗外源细菌对伤口的侵袭，另一方面可以通过植物提取液掩盖药物带来的刺激性气味，使人心情愉悦。
优选地，所述涂层基料包括各原料组分如下：以重量份计，壳聚糖40-60份、胶黏剂15-25份、琼脂10-14份；所述胶黏剂为VAE乳液；所述多孔淀粉为木薯多孔淀粉、玉米多孔淀粉、小麦多孔淀粉中的一种或多种。
一种抗菌型医用涂布无纺布的制备方法，包括以下步骤：
（1）制备无纺布基体；
A.制备改性晶须；
B.制备无纺布；
C.制备无纺布基体；
（2）制备涂层A；
A.制备改性氧化石墨烯；
B.合成涂层A；
C.下表面涂覆；
（3）制备涂层B；
A. 制备抗菌微胶囊；
B．合成涂层B；
C. 上表面涂覆，得到抗菌型无纺布。
具体包括以下步骤：
（1）制备无纺布基体：
A.制备改性晶须：将纳米氧化锌晶须、纳米二氧化钛晶须加入到乙醇溶液中混合均匀，加入硅烷偶联剂，调节pH值为4-6，继续搅拌反应30-60min，得到改性晶须；
B.制备无纺布：将N，N-二甲基甲酰胺加入到纺丝液中搅拌混匀，提升转速至1100-1300r/min并加入改性晶须，静电纺丝，得到改性纱线，将改性纱线制成无纺布A；
C.制备无纺布基体：
a)将无纺布A在乙醇中浸泡15-25min，于20-28℃条件下，加入氢氧化钠溶液，继续搅拌反应10-20min，取出晾干，得到无纺布B；
b)将氢氧化钠置于氯乙酸溶液中搅拌溶解，再依次加入丙烯酸、二苯甲酮搅拌均匀，调节pH值为6-8，再放入无纺布B浸泡1-2h，取出，乙醇洗涤，置于紫外灯下固化3-6h，得到无纺布基体；
（2）制备涂层A；
A.制备改性氧化石墨烯：将氧化石墨烯置于乙醇溶液中超声分散25-35min，依次加入乙酸锌、氢氧化钠溶液搅拌反应1-2h，升高温度至145-165℃，加入硝酸银继续搅拌，恒温反应20-24h，去离子水洗涤干燥，于90-110℃条件下置于尿素溶液中搅拌反应20-40min，再次用去离子水洗涤干燥得到改性氧化石墨烯；
B.合成涂层A：室温条件下，将壳聚糖加入到乙酸溶液中搅拌溶解，升高温度至50-60℃，加入月桂酸酐、乙醇溶液继续搅拌，恒温反应10-15h后，依次加入冰醋酸、涂层基料、改性氧化石墨烯搅拌得到涂层A；
C.下表面涂覆：将涂层A涂覆在无纺布基体的下表面，反应8-10h后，置于120-150℃紫外灯下固化3-6小时；
（3）制备涂层B：
A.制备抗菌微胶囊：将乙基纤维素置于二氯甲烷中搅拌溶解，加入植物提取液、乳化剂，于1100-1300r/min转速下搅拌30-40min，加入熔化的明胶、十二烷基硫酸钠于200-400r/min转速下进行低速搅拌，得到抗菌微胶囊；
B.合成涂层B：在50-60℃条件下，将壳聚糖、多孔淀粉、去离子水混合均匀，并依次加入无水碳酸钠、三偏磷酸钠搅拌反应1-2h，调节pH为5-7，依次加入胶黏剂、抗菌微胶囊、琼脂搅拌得到涂层B；
C.上表面涂覆：将涂层B涂覆在无纺布基体的上表面，于120-150℃紫外灯下固化3-6小时，得到抗菌型无纺布。
与现有技术相比，本发明的有益效果是：
本发明中的涂层B可有效抑制外部细菌的入侵，预防感染，涂层A可有效抑制伤口内部细菌的滋生，加速伤口愈合，利用涂层A、涂层B、无纺布基体的协同作用，可有效抑菌，加快伤口愈合，降低感染风险。
本发明中的无纺布基体具有可溶的特性，用水可直接溶解，减少了在更换无纺布时因为血液凝固在无纺布上而造成伤口二次撕裂的情况。
本发明中的涂层A涂覆在无纺布基体的下表面，涂层A中的改性氧化石墨烯上负载的Ag+离子能够维持较长时间的释放，可达到长期有效抑菌的目的，且涂层A中的壳聚糖具有一定的疏水性，避免了涂层B中多孔淀粉对血液过多的吸附。
本发明中的涂层B涂覆在无纺布基体的上表面，涂层B中的多孔淀粉有利于吸附血液，加快止血过程；抗菌微胶囊表面的羧基可与涂层A中改性氧化石墨烯表面的氨基发生缩合形成交联，增大涂层在无纺布基体上的附着力，不仅可以抵抗外源细菌对伤口的侵袭，另一方面还可以通过植物提取液掩盖药物带来的刺激性气味，使人心情愉悦。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
（1）制备无纺布基体：
A.制备改性晶须：将纳米氧化锌晶须、纳米二氧化钛晶须加入到乙醇溶液中混合均匀，加入硅烷偶联剂，调节pH值为4，继续搅拌反应30min，得到改性晶须；
B.制备无纺布：将N，N-二甲基甲酰胺加入到纺丝液中搅拌混匀，提升转速至1100r/min并加入改性晶须，静电纺丝，得到改性纱线，将改性纱线制成无纺布A；
C.制备无纺布基体：
a)将无纺布A在乙醇中浸泡15min，于20℃条件下，加入氢氧化钠溶液，继续搅拌反应10min，取出晾干，得到无纺布B；
b)将氢氧化钠置于氯乙酸溶液中搅拌溶解，再依次加入丙烯酸、二苯甲酮搅拌均匀，调节pH值为6，再放入无纺布A浸泡1h，取出，乙醇洗涤，置于紫外灯下固化3h，得到无纺布基体；
（2）制备涂层A；
A.制备改性氧化石墨烯：将氧化石墨烯置于乙醇溶液中超声分散25min，依次加入乙酸锌、氢氧化钠溶液搅拌反应1h，升高温度至145℃，加入硝酸银继续搅拌，恒温反应20h，去离子水洗涤干燥，于90℃条件下置于尿素溶液中搅拌反应20min，再次用去离子水洗涤干燥得到改性氧化石墨烯；
B.合成涂层A：室温条件下，将壳聚糖加入到乙酸溶液中搅拌溶解，升高温度至50℃，加入月桂酸酐、乙醇溶液继续搅拌，恒温反应10h后，依次加入冰醋酸、涂层基料、改性氧化石墨烯搅拌得到涂层A；
C.下表面涂覆：将涂层A涂覆在无纺布基体的下表面，反应8h后，置于120℃紫外灯下固化3小时；
（3）制备涂层B：
A.制备抗菌微胶囊：将乙基纤维素置于二氯甲烷中搅拌溶解，加入植物提取液、乳化剂，于1100r/min转速下搅拌30min，加入熔化的明胶、十二烷基硫酸钠于200r/min转速下进行低速搅拌，得到抗菌微胶囊；
B.合成涂层B：在50℃条件下，将壳聚糖、多孔淀粉、去离子水混合均匀，并依次加入无水碳酸钠、三偏磷酸钠搅拌反应1h，调节pH为5，依次加入胶黏剂、抗菌微胶囊、琼脂搅拌得到涂层B；
C.上表面涂覆：将涂层B涂覆在无纺布基体的上表面，于120℃紫外灯下固化3小时，得到抗菌型无纺布。
一种抗菌型医用涂布无纺布，各原料组分如下：以重量份计，无纺布基体90份、涂层A15份、涂层B15份。
无纺布基体包括各原料组分如下：以重量份计，改性晶须20份、纺丝液70份、氯乙酸8份、丙烯酸8份、二苯甲酮8份；
改性晶须包括各原料组分如下：以重量份计，纳米氧化锌晶须20份、纳米二氧化钛晶须20份、硅烷偶联剂10份。
涂层A包括各原料组分如下：以重量份计，改性氧化石墨烯20份、月桂酸酐12份、冰醋酸10份、涂层基料30份。
改性氧化石墨烯包括各原料组分如下：以重量份计，氧化石墨烯50份、乙酸锌8份、氢氧化钠10份、硝酸银15份。
涂层B包括各原料组分如下：以重量份计，抗菌微胶囊20份、多孔淀粉30份、无水碳酸钠10份、三偏磷酸钠10份、涂层基料40份。
抗菌微胶囊包括各原料组分如下：以重量份计，乙基纤维素20份、植物提取液20份、乳化剂10-份、明胶30份、十二烷基硫酸钠16份；
涂层基料包括各原料组分如下：以重量份计，壳聚糖40份、胶黏剂15份、琼脂10份。
实施例2
（1）制备无纺布基体：
A.制备改性晶须：将纳米氧化锌晶须、纳米二氧化钛晶须加入到乙醇溶液中混合均匀，加入硅烷偶联剂，调节pH值为5，继续搅拌反应40min，得到改性晶须；
B.制备无纺布：将N，N-二甲基甲酰胺加入到纺丝液中搅拌混匀，提升转速至1200r/min并加入改性晶须，静电纺丝，得到改性纱线，将改性纱线制成无纺布A；
C.制备无纺布基体：
a)将无纺布A在乙醇中浸泡20min，于24℃条件下，加入氢氧化钠溶液，继续搅拌反应15min，取出晾干，得到无纺布B；
b)将氢氧化钠置于氯乙酸溶液中搅拌溶解，再依次加入丙烯酸、二苯甲酮搅拌均匀，调节pH值为7，再放入无纺布A浸泡1.5h，取出，乙醇洗涤，置于紫外灯下固4.5h，得到无纺布基体；
（2）制备涂层A；
A.制备改性氧化石墨烯：将氧化石墨烯置于乙醇溶液中超声分散30min，依次加入乙酸锌、氢氧化钠溶液搅拌反应1.5h，升高温度至155℃，加入硝酸银继续搅拌，恒温反应22h，去离子水洗涤干燥，于100℃条件下置于尿素溶液中搅拌反应30min，再次用去离子水洗涤干燥得到改性氧化石墨烯；
B.合成涂层A：室温条件下，将壳聚糖加入到乙酸溶液中搅拌溶解，升高温度至55℃，加入月桂酸酐、乙醇溶液继续搅拌，恒温反应13h后，依次加入冰醋酸、涂层基料、改性氧化石墨烯搅拌得到涂层A；
C.下表面涂覆：将涂层A涂覆在无纺布基体的下表面，反应9h后，置于135℃紫外灯下固化4.5小时；
（3）制备涂层B：
A.制备抗菌微胶囊：将乙基纤维素置于二氯甲烷中搅拌溶解，加入植物提取液、乳化剂，于1200r/min转速下搅拌35min，加入熔化的明胶、十二烷基硫酸钠于300r/min转速下进行低速搅拌，得到抗菌微胶囊；
B.合成涂层B：在55℃条件下，将壳聚糖、多孔淀粉、去离子水混合均匀，并依次加入无水碳酸钠、三偏磷酸钠搅拌反应1.5h，调节pH为6，依次加入胶黏剂、抗菌微胶囊、琼脂搅拌得到涂层B；
C.上表面涂覆：将涂层B涂覆在无纺布基体的上表面，于135℃紫外灯下固化4.5小时，得到抗菌型无纺布。
一种抗菌型医用涂布无纺布，各原料组分如下：以重量份计，无纺布基体95份、涂层A20份、涂层B20份。
无纺布基体包括各原料组分如下：以重量份计，改性晶须25份、纺丝液80份、氯乙酸10份、丙烯酸10份、二苯甲酮10份。
改性晶须包括各原料组分如下：以重量份计，纳米氧化锌晶须25份、纳米二氧化钛晶须25份、硅烷偶联剂13份。
涂层A包括各原料组分如下：以重量份计，改性氧化石墨烯25份、月桂酸酐13份、冰醋酸15份、涂层基料45份。
改性氧化石墨烯包括各原料组分如下：以重量份计，氧化石墨烯55份、乙酸锌9份、氢氧化钠15份、硝酸银20份。
涂层B包括各原料组分如下：以重量份计，抗菌微胶囊25份、多孔淀粉35份、无水碳酸钠15份、三偏磷酸钠13份、涂层基料50份。
抗菌微胶囊包括各原料组分如下：以重量份计，乙基纤维素30份、植物提取液25份、乳化剂15份、明胶40份、十二烷基硫酸钠17份；
涂层基料包括各原料组分如下：以重量份计，壳聚糖50份、胶黏剂20份、琼脂12份。
实施例3
（1）制备无纺布基体：
A.制备改性晶须：将纳米氧化锌晶须、纳米二氧化钛晶须加入到乙醇溶液中混合均匀，加入硅烷偶联剂，调节pH值为6，继续搅拌反应60min，得到改性晶须；
B.制备无纺布：将N，N-二甲基甲酰胺加入到纺丝液中搅拌混匀，提升转速至1300r/min并加入改性晶须，静电纺丝，得到改性纱线，将改性纱线制成无纺布A；
C.制备无纺布基体：
a)将无纺布A在乙醇中浸泡25min，于28℃条件下，加入氢氧化钠溶液，继续搅拌反应20min，取出晾干，得到无纺布B；
b)将氢氧化钠置于氯乙酸溶液中搅拌溶解，再依次加入丙烯酸、二苯甲酮搅拌均匀，调节pH值为8，再放入无纺布A浸泡2h，取出，乙醇洗涤，置于紫外灯下固化6h，得到无纺布基体；
（2）制备涂层A；
A.制备改性氧化石墨烯：将氧化石墨烯置于乙醇溶液中超声分散35min，依次加入乙酸锌、氢氧化钠溶液搅拌反应2h，升高温度至165℃，加入硝酸银继续搅拌，恒温反应24h，去离子水洗涤干燥，于110℃条件下置于尿素溶液中搅拌反应40min，再次用去离子水洗涤干燥得到改性氧化石墨烯；
B.合成涂层A：室温条件下，将壳聚糖加入到乙酸溶液中搅拌溶解，升高温度至60℃，加入月桂酸酐、乙醇溶液继续搅拌，恒温反应15h后，依次加入冰醋酸、涂层基料、改性氧化石墨烯搅拌得到涂层A；
C. 下表面涂覆：将涂层A涂覆在无纺布基体的下表面，反应10h后，置于150℃紫外灯下固化6小时；
（3）制备涂层B：
A.制备抗菌微胶囊：将乙基纤维素置于二氯甲烷中搅拌溶解，加入植物提取液、乳化剂，于1300r/min转速下搅拌40min，加入熔化的明胶、十二烷基硫酸钠于400r/min转速下进行低速搅拌，得到抗菌微胶囊；
B.合成涂层B：在60℃条件下，将壳聚糖、多孔淀粉、去离子水混合均匀，并依次加入无水碳酸钠、三偏磷酸钠搅拌反应2h，调节pH为7，依次加入胶黏剂、抗菌微胶囊、琼脂搅拌得到涂层B；
C.上表面涂覆：将涂层B涂覆在无纺布基体的上表面，于150℃紫外灯下固化6小时，得到抗菌型无纺布。
一种抗菌型医用涂布无纺布，各原料组分如下：以重量份计，无纺布基体100份、涂层A25份、涂层B25份。
无纺布基体包括各原料组分如下：以重量份计，改性晶须30份、纺丝液90份、氯乙酸12份、丙烯酸12份、二苯甲酮12份。
改性晶须包括各原料组分如下：以重量份计，纳米氧化锌晶须30份、纳米二氧化钛晶须30份、硅烷偶联剂16份。
涂层A包括各原料组分如下：以重量份计，改性氧化石墨烯30份、月桂酸酐14份、冰醋酸120份、涂层基料60份。
改性氧化石墨烯包括各原料组分如下：以重量份计，氧化石墨烯60份、乙酸锌10份、氢氧化钠20份、硝酸银25份。
涂层B包括各原料组分如下：以重量份计，抗菌微胶囊30份、多孔淀粉40份、无水碳酸钠20份、三偏磷酸钠16份、涂层基料60份。
抗菌微胶囊包括各原料组分如下：以重量份计，乙基纤维素40份、植物提取液30份、乳化剂18份、明胶50份、十二烷基硫酸钠18份；
涂层基料包括各原料组分如下：以重量份计，壳聚糖60份、胶黏剂25份、琼脂14份。
实施例4
其余各项参数均参考实施例1。
（1）制备无纺布基体：
A.制备无纺布：将N，N-二甲基甲酰胺加入到纺丝液中搅拌混匀，提升转速至1100r/min，静电纺丝，得到改性纱线，将改性纱线制成无纺布A；
B.制备无纺布基体：将无纺布A在乙醇中浸泡15min，于20℃条件下，加入氢氧化钠溶液，继续搅拌反应10min，取出晾干，得到无纺布基体；
（2）制备涂层A；
A.制备改性氧化石墨烯：将氧化石墨烯置于乙醇溶液中超声分散25min，依次加入乙酸锌、氢氧化钠溶液搅拌反应1h，升高温度至145℃，加入硝酸银继续搅拌，恒温反应20h，去离子水洗涤干燥，于90℃条件下置于尿素溶液中搅拌反应20min，再次用去离子水洗涤干燥得到改性氧化石墨烯；
B.合成涂层A：室温条件下，将壳聚糖加入到乙酸溶液中搅拌溶解，升高温度至50℃，加入月桂酸酐、乙醇溶液继续搅拌，恒温反应10h后，依次加入冰醋酸、涂层基料、改性氧化石墨烯搅拌得到涂层A；
C.下表面涂覆：将涂层A涂覆在无纺布基体的下表面，反应8h后，置于120℃紫外灯下固化3小时；
（3）制备涂层B：
A.制备抗菌微胶囊：将乙基纤维素置于二氯甲烷中搅拌溶解，加入植物提取液、乳化剂，于1100r/min转速下搅拌30min，加入熔化的明胶、十二烷基硫酸钠于200r/min转速下进行低速搅拌，得到抗菌微胶囊；
B.合成涂层B：在50℃条件下，将壳聚糖、多孔淀粉、去离子水混合均匀，并依次加入无水碳酸钠、三偏磷酸钠搅拌反应1h，调节pH为5，依次加入胶黏剂、抗菌微胶囊、琼脂搅拌得到涂层B；
C.上表面涂覆：将涂层B涂覆在无纺布基体的上表面，于120℃紫外灯下固化3小时，得到抗菌型无纺布。
实施例5
其余各项参数均参考实施例1。
（1）制备无纺布基体：
A.制备改性晶须：将纳米氧化锌晶须、纳米二氧化钛晶须加入到乙醇溶液中混合均匀，加入硅烷偶联剂，调节pH值为4，继续搅拌反应30min，得到改性晶须；
B.制备无纺布：将N，N-二甲基甲酰胺加入到纺丝液中搅拌混匀，提升转速至1100r/min并加入改性晶须，静电纺丝，得到改性纱线，将改性纱线制成无纺布A；
C.制备无纺布基体：
a)将无纺布A在乙醇中浸泡15min，于20℃条件下，加入氢氧化钠溶液，继续搅拌反应10min，取出晾干，得到无纺布B；
b)将氢氧化钠置于氯乙酸溶液中搅拌溶解，再依次加入丙烯酸、二苯甲酮搅拌均匀，调节pH值为6，再放入无纺布A浸泡1h，取出，乙醇洗涤，置于紫外灯下固化3h，得到无纺布基体；
（2）制备涂层A；
A.室温条件下，将壳聚糖加入到乙酸溶液中搅拌溶解，升高温度至50℃，加入月桂酸酐、乙醇溶液继续搅拌，恒温反应10h后，依次加入冰醋酸、涂层基料搅拌得到涂层A；
B.下表面涂覆：将涂层A涂覆在无纺布基体的下表面，反应8h后，置于120℃紫外灯下固化3小时；
（3）制备涂层B：
A.制备抗菌微胶囊：将乙基纤维素置于二氯甲烷中搅拌溶解，加入植物提取液、乳化剂，于1100r/min转速下搅拌30min，加入熔化的明胶、十二烷基硫酸钠于200r/min转速下进行低速搅拌，得到抗菌微胶囊；
B.合成涂层B：在50℃条件下，将壳聚糖、多孔淀粉、去离子水混合均匀，并依次加入无水碳酸钠、三偏磷酸钠搅拌反应1h，调节pH为5，依次加入胶黏剂、抗菌微胶囊、琼脂搅拌得到涂层B；
C.上表面涂覆：将涂层B涂覆在无纺布基体的上表面，于120℃紫外灯下固化3小时，得到抗菌型无纺布。
实施例6
其余各项参数均参考实施例1。
（1）制备无纺布基体：
A.制备改性晶须：将纳米氧化锌晶须、纳米二氧化钛晶须加入到乙醇溶液中混合均匀，加入硅烷偶联剂，调节pH值为4，继续搅拌反应30min，得到改性晶须；
B.制备无纺布：将N，N-二甲基甲酰胺加入到纺丝液中搅拌混匀，提升转速至1100r/min并加入改性晶须，静电纺丝，得到改性纱线，将改性纱线制成无纺布A；
C.制备无纺布基体：
a)将无纺布A在乙醇中浸泡15min，于20℃条件下，加入氢氧化钠溶液，继续搅拌反应10min，取出晾干，得到无纺布B；
b)将氢氧化钠置于氯乙酸溶液中搅拌溶解，再依次加入丙烯酸、二苯甲酮搅拌均匀，调节pH值为6，再放入无纺布A浸泡1h，取出，乙醇洗涤，置于紫外灯下固化3h，得到无纺布基体；
（2）制备涂层A；
A.制备改性氧化石墨烯：将氧化石墨烯置于乙醇溶液中超声分散25min，依次加入乙酸锌、氢氧化钠溶液搅拌反应1h，升高温度至145℃，加入硝酸银继续搅拌，恒温反应20h，去离子水洗涤干燥，于90℃条件下置于尿素溶液中搅拌反应20min，再次用去离子水洗涤干燥得到改性氧化石墨烯；
B.合成涂层A：室温条件下，将壳聚糖加入到乙酸溶液中搅拌溶解，升高温度至50℃，恒温反应10h后，依次加入冰醋酸、涂层基料、改性氧化石墨烯搅拌得到涂层A；
C.下表面涂覆：将涂层A涂覆在无纺布基体的下表面，反应8h后，置于120℃紫外灯下固化3小时；
（3）制备涂层B：
A.制备抗菌微胶囊：将乙基纤维素置于二氯甲烷中搅拌溶解，加入植物提取液、乳化剂，于1100r/min转速下搅拌30min，加入熔化的明胶、十二烷基硫酸钠于200r/min转速下进行低速搅拌，得到抗菌微胶囊；
B.合成涂层B：在50℃条件下，将壳聚糖、多孔淀粉、去离子水混合均匀，并依次加入无水碳酸钠、三偏磷酸钠搅拌反应1h，调节pH为5，依次加入胶黏剂、抗菌微胶囊、琼脂搅拌得到涂层B；
C.上表面涂覆：将涂层B涂覆在无纺布基体的上表面，于120℃紫外灯下固化3小时，得到抗菌型无纺布。
实施例7
其余各项参数均参考实施例1。
（1）制备无纺布基体：
A.制备改性晶须：将纳米氧化锌晶须、纳米二氧化钛晶须加入到乙醇溶液中混合均匀，加入硅烷偶联剂，调节pH值为4，继续搅拌反应30min，得到改性晶须；
B.制备无纺布：将N，N-二甲基甲酰胺加入到纺丝液中搅拌混匀，提升转速至1100r/min并加入改性晶须，静电纺丝，得到改性纱线，将改性纱线制成无纺布A；
C.制备无纺布基体：
a)将无纺布A在乙醇中浸泡15min，于20℃条件下，加入氢氧化钠溶液，继续搅拌反应10min，取出晾干，得到无纺布B；
b)将氢氧化钠置于氯乙酸溶液中搅拌溶解，再依次加入丙烯酸、二苯甲酮搅拌均匀，调节pH值为6，再放入无纺布A浸泡1h，取出，乙醇洗涤，置于紫外灯下固化3h，得到无纺布基体；
（2）制备涂层A；
A.制备改性氧化石墨烯：将氧化石墨烯置于乙醇溶液中超声分散25min，依次加入乙酸锌、氢氧化钠溶液搅拌反应1h，升高温度至145℃，加入硝酸银继续搅拌，恒温反应20h，去离子水洗涤干燥，于90℃条件下置于尿素溶液中搅拌反应20min，再次用去离子水洗涤干燥得到改性氧化石墨烯；
B.合成涂层A：室温条件下，将壳聚糖加入到乙酸溶液中搅拌溶解，升高温度至50℃，加入月桂酸酐、乙醇溶液继续搅拌，恒温反应10h后，依次加入冰醋酸、涂层基料、改性氧化石墨烯搅拌得到涂层A；
C.下表面涂覆：将涂层A涂覆在无纺布基体的下表面，反应8h后，置于120℃紫外灯下固化3小时，得到抗菌型无纺布。
实施例8
其余各项参数均参考实施例1。
（1）制备无纺布基体：
A.制备改性晶须：将纳米氧化锌晶须、纳米二氧化钛晶须加入到乙醇溶液中混合均匀，加入硅烷偶联剂，调节pH值为4，继续搅拌反应30min，得到改性晶须；
B.制备无纺布：将N，N-二甲基甲酰胺加入到纺丝液中搅拌混匀，提升转速至1100r/min并加入改性晶须，静电纺丝，得到改性纱线，将改性纱线制成无纺布A；
C.制备无纺布基体：
a)将无纺布A在乙醇中浸泡15min，于20℃条件下，加入氢氧化钠溶液，继续搅拌反应10min，取出晾干，得到无纺布B；
b)将氢氧化钠置于氯乙酸溶液中搅拌溶解，再依次加入丙烯酸、二苯甲酮搅拌均匀，调节pH值为6，再放入无纺布A浸泡1h，取出，乙醇洗涤，置于紫外灯下固化3h，得到无纺布基体。
（2）制备涂层B：
A.制备抗菌微胶囊：将乙基纤维素置于二氯甲烷中搅拌溶解，加入植物提取液、乳化剂，于1100r/min转速下搅拌30min，加入熔化的明胶、十二烷基硫酸钠于200r/min转速下进行低速搅拌，得到抗菌微胶囊；
B.合成涂层B：在50℃条件下，将壳聚糖、多孔淀粉、去离子水混合均匀，并依次加入无水碳酸钠、三偏磷酸钠搅拌反应1h，调节pH为5，依次加入胶黏剂、抗菌微胶囊、琼脂搅拌得到涂层B；
C.上表面涂覆：将涂层B涂覆在无纺布基体的上表面，于120℃紫外灯下固化3小时，得到抗菌型无纺布。
实施例4-8为对比实验，其中实施例4中在涂层A中添加有改性氧化石墨烯，在涂层B中添加有抗菌微胶囊和多孔淀粉，直接将涂层A、涂层B涂覆在普通无纺布上得到抗菌型涂布无纺布；实施例5在涂层A中未添加改性氧化石墨烯，其余参数均不变，将涂层A、涂层B涂覆在无纺布基体上；实施例6中涂层A中的壳聚糖未通过添加月桂酸酐进行改性，其余参数均不变，将涂层A、涂层B涂覆在无纺布基体上；实施例7中的无纺布基体只涂覆有涂层A，其余参数均不变；实施例8中无纺布基体只涂覆有涂层B,其余参数均不变；将实施例1-8中制得的无纺布样品进行以下实验：
抗菌性能测试：按照GB/20944,。3-2008《纺织品抗菌性能的评价第3部分：振荡法》进行测试。
无纺布溶解性能测试：将无纺布样品置于蒸馏水中摇晃使其充分润湿，静置观察无纺布完全溶解为均一溶液所需要的时间，若静置反应一周后无纺布完全溶解为均一透明的溶液则说明无纺布可溶，若一周后无纺布仍为完整状态则认为不溶解。
止血效果测试：将若干小鼠样品腹部进行脱毛处理，并进行麻醉，取仰卧位固定于实验用鼠板上，固定好小鼠的四肢和头部，用酒精对小鼠腹部进行消毒处理，于肋弓下沿腹中线作一长约2cm的纵行切口，沿腹中线剪开腹肌，挤压腹部至肝中叶从切口处被挤出，吸干肝脏周围腹腔液后，待血液充满肝叶面，立即覆盖无纺布样品并开始计时，直至出血停止，记录出血时间及出血量。出血时间为血液充满肝叶开始至出血停止，出血量为前后无纺布样品重量差。
力学性能测试：拉伸强度测试按照标准ASTMD638在万能拉力试验机上进行测试。拉伸试验速率为45mm/min。
| 各项性能 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 | 实施例7 | 实施例8 | 传统无纺布 |
| 止血时间/s | 62 | 63 | 63 | 65 | 65 | 79 | 81 | 77 | 153 |
| 出血量/g | 0.93 | 0.94 | 0.94 | 1.04 | 1.01 | 1.32 | 1.41 | 1.25 | 1.43 |
| 抑菌率/% | 99.6 | 99.4 | 99.5 | 89.7 | 68.3 | 75.3 | 59.9 | 59.4 | 26.5 |
| 拉伸断裂强度/N | 289 | 289 | 288 | 108 | 167 | 279 | 276 | 245 | 102 |
| 完全溶解时间/h | 8.17 | 8.18 | 8.25 | 未溶解 | 8.37 | 8.33 | 8.41 | 8.41 | 未溶解 |
根据表中数据可知，实施例1-3的实验数据结果均比较理想，其中实施例1得到的数据结果较实施例1-2来看，略胜一筹，故参考实施例1中的各项参数进行了实施例4-8的实验，其中实施例4中在涂层A中添加有改性氧化石墨烯，在涂层B中添加有抗菌微胶囊和多孔淀粉，直接将涂层A、涂层B涂覆在普通无纺布上得到的抗菌型涂布无纺布止血时间和止血量较实施例1-3相比稍差，但抑菌率一般，仅有89%，拉伸断裂强度与传统无纺布相似，拉伸断裂强度较差，且无纺布不能在水中溶解；实施例5在涂层A中未添加改性氧化石墨烯，其余参数均不变，将涂层A、涂层B涂覆在无纺布基体上得到的抗菌型涂布无纺布拉伸断裂强度一般，抑菌效果较差，其余各项参数与传统无纺布相比有显著进步；实施例6中涂层A中的壳聚糖未通过添加月桂酸酐进行改性，其余参数均不变，将涂层A、涂层B涂覆在无纺布基体上得到的抗菌型医用涂布无纺布止血时间与实施例1-3相比略长，出血量较多，其余各项参数结果均比较理想；实施例7中的无纺布基体只涂覆有涂层A，其余参数均不变，得到的抗菌型医用涂布无纺布，出血量较大，且止血时间较长，抑菌性能也很差，仅有59.9%，其余各项性能较传统无纺布有所改进；实施例8中无纺布基体只涂覆有涂层B,其余参数均不变，制备得到的抗菌型医用涂布无纺布止血时间、出血量均一般，抑菌性能较差，拉伸断裂强度较实施例1-3相比有所降低，其余各项性能表现良好。
通过以上数据我们可以得出以下结论：普通无纺布拉伸断裂强度、抑菌性能较差，吸附血液以后极易滋生细菌，且粘黏在伤口上以后强行取下容易造成伤口二次撕裂的问题。本发明通过在纺丝原液中添加纳米氧化锌晶须和纳米二氧化钛晶须来增加无纺布基体的力学性能，增加抗菌型医用涂布无纺布的拉伸断裂强度，同时纳米氧化锌晶须和纳米二氧化钛晶须也具有一定的抑菌能力；本发明在氧化石墨烯上负载Ag+对氧化石墨烯进行改性进一步增加无纺布的杀菌、抗菌性能，在壳聚糖中添加月桂酸酐来增加涂层A的疏水性能和凝血性能，加快伤口愈合和增强无纺布抗菌能力；本发明在涂层B中添加有抗菌微胶囊和多孔淀粉，利用多孔淀粉来加快血液吸收，促进伤口愈合，利用抗菌微胶囊释放天然抗菌成分来增强杀菌作用。结果表明，利用涂层A、涂层B、无纺布基体协同作用得到的抗菌型医用涂布无纺布的抗菌效果做好，止血作用最强，吸血量最小，抗拉伸断裂强度高，遇水可溶，具有非常广阔的应用前景。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
Claims (1)
1.一种抗菌型医用涂布无纺布的制备方法，其特征在于，具体包括以下步骤：
（1）制备无纺布基体：
A. 制备改性晶须：将纳米氧化锌晶须、纳米二氧化钛晶须加入到乙醇溶液中混合均匀，加入硅烷偶联剂，调节pH值为5，继续搅拌反应40min，得到改性晶须；
B. 制备无纺布：将N，N-二甲基甲酰胺加入到纺丝液中搅拌混匀，提升转速至1200r/min并加入改性晶须，静电纺丝，得到改性纱线，将改性纱线制成无纺布A；
C. 制备无纺布基体：
a) 将无纺布A在乙醇中浸泡20min，于24℃条件下，加入氢氧化钠溶液，继续搅拌反应15min，取出晾干，得到无纺布B；
b) 将氢氧化钠置于氯乙酸溶液中搅拌溶解，再依次加入丙烯酸、二苯甲酮搅拌均匀，调节pH值为7，再放入无纺布A浸泡1.5h，取出，乙醇洗涤，置于紫外灯下固4.5h，得到无纺布基体；
（2）制备涂层A；
A.制备改性氧化石墨烯：将氧化石墨烯置于乙醇溶液中超声分散30min，依次加入乙酸锌、氢氧化钠溶液搅拌反应1.5h，升高温度至155℃，加入硝酸银继续搅拌，恒温反应22h，去离子水洗涤干燥，于100℃条件下置于尿素溶液中搅拌反应30min，再次用去离子水洗涤干燥得到改性氧化石墨烯；
B.合成涂层A：室温条件下，将壳聚糖加入到乙酸溶液中搅拌溶解，升高温度至55℃，加入月桂酸酐、乙醇溶液继续搅拌，恒温反应13h后，依次加入冰醋酸、涂层基料、改性氧化石墨烯搅拌得到涂层A；
C.下表面涂覆：将涂层A涂覆在无纺布基体的下表面，反应9h后，置于135℃紫外灯下固化4.5小时；
（3）制备涂层B：
A. 制备抗菌微胶囊：将乙基纤维素置于二氯甲烷中搅拌溶解，加入植物提取液、乳化剂，于1200r/min转速下搅拌35min，加入熔化的明胶、十二烷基硫酸钠于300r/min转速下进行低速搅拌，得到抗菌微胶囊；
B. 合成涂层B：在55℃条件下，将壳聚糖、多孔淀粉、去离子水混合均匀，并依次加入无水碳酸钠、三偏磷酸钠搅拌反应1.5h，调节pH为6，依次加入胶黏剂、抗菌微胶囊、琼脂搅拌得到涂层B；
上表面涂覆：将涂层B涂覆在无纺布基体的上表面，于135℃紫外灯下固化4.5小时，得到抗菌型无纺布；
所述各原料组分如下：以重量份计，无纺布基体95份、涂层A20份、涂层B20份；
无纺布基体包括各原料组分如下：以重量份计，改性晶须25份、纺丝液80份、氯乙酸10份、丙烯酸10份、二苯甲酮10份；
改性晶须包括各原料组分如下：以重量份计，纳米氧化锌晶须25份、纳米二氧化钛晶须25份、硅烷偶联剂13份；
涂层A包括各原料组分如下：以重量份计，改性氧化石墨烯25份、月桂酸酐13份、冰醋酸15份、涂层基料45份；
改性氧化石墨烯包括各原料组分如下：以重量份计，氧化石墨烯55份、乙酸锌9份、氢氧化钠15份、硝酸银20份；
涂层B包括各原料组分如下：以重量份计，抗菌微胶囊25份、多孔淀粉35份、无水碳酸钠15份、三偏磷酸钠13份、涂层基料50份；
抗菌微胶囊包括各原料组分如下：以重量份计，乙基纤维素30份、植物提取液25份、乳化剂15份、明胶40份、十二烷基硫酸钠17份；
涂层基料包括各原料组分如下：以重量份计，壳聚糖50份、胶黏剂20份、琼脂12份。
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