CN114073786A - 吸液抗菌3d纳米纤维复合医用敷料及其制备方法 - Google Patents
吸液抗菌3d纳米纤维复合医用敷料及其制备方法 Download PDFInfo
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- CN114073786A CN114073786A CN202010810131.1A CN202010810131A CN114073786A CN 114073786 A CN114073786 A CN 114073786A CN 202010810131 A CN202010810131 A CN 202010810131A CN 114073786 A CN114073786 A CN 114073786A
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- polyvinyl alcohol
- antibacterial
- chitosan
- medical dressing
- nanofiber
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- Materials For Medical Uses (AREA)
Abstract
本申请提出一种吸液抗菌3D纳米纤维复合医用敷料及其制备方法,其包括复合的吸湿抗菌层和保护层;吸湿抗菌层包括抗菌药物和聚乙烯醇/壳聚糖纳米短纤维;聚乙烯醇/壳聚糖纳米短纤维经静电纺丝、交联和均质化处理得到;吸湿抗菌层是抗菌药物和聚乙烯醇/壳聚糖纳米短纤维的均质液经预冻成型、真空冷冻干燥、热处理、真空干燥得到的三维多级网孔材料;保护层是聚己内酯和聚乳酸经静电纺丝得到。使用时,该敷料与皮肤直接贴合的是一层具有多级网孔结构的吸湿抗菌层,使其具有很好的吸液性、保湿性、空气通透性、贴合性和生物相容性,同时发挥优异的抗菌能力;保护层具有良好的力学性能、透气性和隔菌防水能力,对创面提供很好的保护作用。
Description
技术领域
本申请涉及一种医用敷料,尤其涉及一种吸液抗菌3D纳米纤维复合医用敷料及其制备方法。
背景技术
皮肤是人体最大的器官,具有调节体温、维持机体内环境稳定、排泄、抵御外界微生物入侵、防止水分蒸发等重要功能。人体皮肤受损后,不仅会造成机体本身免疫功能失调,同时抵御外界侵害的防御能力也显著降低,在多种因素的作用下,创面容易发生局部感染,甚至引起全身感染。医用敷料是一类用于覆盖创面的医用材料,可以代替受损皮肤起到暂时性屏障作用。在医用敷料使用过程中,伤口愈合存在三个难题亟待解决:不断渗出的组织液、被伤口感染的风险和利于创面愈合的湿润环境。因此,一种理想的医用敷料,应该既能够有效吸收组织渗出液,又能保证创面具有一定的湿度,而且具有抗菌、隔菌性能以防止伤口感染。
目前国内的敷料普遍存在产品种类和功能单一、功能性缺陷等问题。专利CN201310441908.1公开的一种含纳米银的聚乙烯醇/壳聚糖纳米纤维膜敷料的制备方法。该方法以聚乙烯醇、壳聚糖、纳米银为原料,利用静电纺丝技术制备纳米纤维膜,然后经交联制得敷料。该方法制备的纳米纤维膜敷料虽然能够为伤口提供湿润环境,但纤维膜结构单一且厚度只有几个毫米,对伤口渗液的吸收能力有限,易导致伤口被渗出液浸泡影响伤口愈合;同时其机械性可控性也较差,影响敷料的使用效果。专利CN201710978882.2公开了一种吸湿抗菌3D纳米纤维医用敷料及其制备方法。该方法以PCL-PEG-PCL为原料,利用静电纺丝技术制备纳米纤维薄膜,然后利用高速搅拌切割得到纳米短纤维,将纳米短纤维和抗菌药物的均质液经快速冷冻、真空冷冻干燥和热处理得到三维多级网孔材料。该方法中使用的高分子材料仅为合成高分子,无法实现与天然高分子材料复合的优势互补,且与复合材料相比生物相容性较差。此外该敷料仅为三维多级网孔结构,虽然能够实现纤维间大孔结构与多孔小间隙协同作用而赋予材料很强的吸液能力,但无法保护创面免除外界灰尘、细菌等的入侵,致使伤口感染风险较大,难以满足医用敷料的要求。
发明内容
鉴于上述问题,本申请旨在提出一种吸液抗菌3D纳米纤维复合医用敷料,其不但能有效吸收组织的渗出液,而且能够保证创面的湿度,此外,还具有良好的生物相容性、抗菌和隔菌性能。
本申请的吸液抗菌3D纳米纤维复合医用敷料,其包括吸湿抗菌层和保护层;该吸湿抗菌层和保护层复合在一起;
所述吸湿抗菌层为包括抗菌药物和聚乙烯醇/壳聚糖纳米短纤维;
所述保护层包括聚乳酸/聚己内酯纳米纤维膜。
优选地,所述聚乙烯醇/壳聚糖纳米短纤维经静电纺丝、交联和均质化处理方法得到;所述吸湿抗菌层是抗菌药物和聚乙烯醇/壳聚糖纳米短纤维的均质液经预冻成型、真空冷冻干燥、热处理、真空干燥得到的三维多级网孔材料;
所述聚乳酸/聚己内酯纳米纤维膜是经静电纺丝得到的。
优选地,所述抗菌药物为银化合物、双胍盐、抗生素中的至少一种;所述银化合物为Ag2SO4、AgNO3和磺胺嘧啶银中的至少一种;所述双胍盐为聚六亚甲基双胍盐酸盐、壳聚糖双胍盐酸盐中的至少一种;所述抗生素为盐酸环丙沙星、庆大霉素、盐酸四环素、盐酸万古霉素中的至少一种。
优选地,所述均质化处理方法包括高速分散切割、超声波均质、冷冻切割中的至少一种。
优选地,所述聚乙烯醇/壳聚糖纳米短纤维的长度为10-500000nm。
本申请还旨在提出一种制备吸液抗菌3D纳米纤维复合医用敷料的方法,其包括:
步骤1,将壳聚糖和聚乙烯醇分别溶解,然后混合并搅拌均匀,得到聚乙烯醇/壳聚糖纺丝溶液;
步骤2,将步骤1中制备的聚乙烯醇/壳聚糖纺丝溶液转移至静电纺丝设备的注射器内,设置控制电压、纺丝速度、接收距离,进行纺丝,采用铝箔接收,得到聚乙烯醇/壳聚糖纳米纤维膜;
步骤3,将步骤2中制备的聚乙烯醇/壳聚糖纳米纤维膜在交联剂中交联,在真空干燥箱中干燥,切成小块,加至溶剂中,均质化处理,得到聚乙烯醇/壳聚糖纳米短纤维的均质液;
步骤4,将步骤3中的聚乙烯醇/壳聚糖纳米短纤维的均质液与抗菌药物混合并搅拌均匀后,低温冷冻,使溶液完全凝固,然后真空冷冻干燥,热处理,最后再进行真空干燥,得到具有三维多级网孔结构的抗菌吸湿层;
步骤5,将聚乳酸和聚己内酯分别溶解,然后混合并搅拌均匀,得到聚乳酸/聚己内酯纺丝溶液;
步骤6,将步骤5中制备的聚乳酸/聚己内酯纺丝液转移至静电纺丝设备的注射器内,设置控制电压、纺丝速度、接收距离,在所述抗菌吸湿层上进行静电纺丝得到聚乳酸/聚己内酯纳米纤维保护层,经室温真空干燥得到3D纳米纤维复合医用敷料。
优选地,所述步骤1中,壳聚糖的质量浓度为3-7%,聚乙烯醇的质量浓度为5-10%,壳聚糖溶液和聚乙烯醇溶液按照体积比20:80-30:70进行混合;
所述步骤3中,交联剂浓度为25-50%;
所述步骤3中,均质化处理方法包括高速分散切割、超声波均质、冷冻切割中的至少一种。
优选地,所述高速分散切割速度为6-15Krpm,时间为3-30min;高速分散切割过程是经由均质机的搅拌叶片高速转动对溶液中小块纤维膜进行切割形成短纤维,使短纤维长度在0-50000nm且均匀地分布在溶液中而形成均质液。
所述超声波均质功率为400-1200w,频率为18-21KHz,时间为10-30min;超声波均质过程是利用超声波在含有小块纳米纤维膜的溶液中的空化作用来达到均质效果的,使短纤维长度在10-500000nm且均匀地分布在溶液中。
所述冷冻切割是在低温恒温器中-20℃条件下进行;冷冻切割过程为先将含小块纳米纤维膜溶液-80℃条件下冷冻,转移至低温恒温器中-20℃条件下切割得到10-500000nm短纤维,将短纤维加入到溶剂中搅拌均匀而得到均质液。
优选地,所述步骤3中,聚乙烯醇/壳聚糖纳米短纤维的均质液中聚乙烯醇/壳聚糖纳米短纤维的含量为10-30mg/ml,溶剂为水、酒精、叔丁醇、甘油等中的至少一种。溶剂的使用能够为聚乙烯醇/壳聚糖纳米短纤维提供一个相对稳定的液相环境,不会影响聚乙烯醇/壳聚糖纳米短纤维的化学性质。
优选地,所述步骤4中,与聚乙烯醇/壳聚糖纳米短纤维均质液混合的抗菌药物含量为0.05-200mg/ml;
所述步骤5中,聚乳酸和聚己内酯按照质量比70:30-90:10进行混合,聚乳酸和聚己内酯的质量分数为8-11%。
本申请的吸液抗菌3D纳米纤维复合医用敷料不仅可以促进伤口愈合,同时还可以保护创面。吸湿抗菌层是由聚乙烯醇/壳聚糖纳米短纤维和抗菌药物形成的具有多级网孔结构的材料,具有很好的吸液能力和锁水能力,吸液后很好的贴合伤口,同时保持伤口湿润,具有良好的空气通透性,壳聚糖和抗菌物质的协同抗菌更有利于促进伤口愈合。保护层是具有高孔隙率、高比表面积的电纺聚乳酸/聚己内酯纳米纤维薄膜,具有良好的生物相容性、生物降解性、力学性能、透气性和隔菌防水能力,在使用过程中能够对创面起到很好的保护作用。本申请的吸液抗菌3D纳米纤维复合医用敷料选用的材料均具有良好的生物相容性和生物降解性,制备完成后基本无有机溶剂的残留,不需要特殊处理便可投入使用。
附图说明
图1为本申请的吸液抗菌3D纳米纤维复合医用敷料的制备方法流程图。
具体实施方式
下面,结合附图对本申请的吸液抗菌3D纳米纤维复合医用敷料及其制备方法进行详细说明。
本申请的吸液抗菌3D纳米纤维复合医用敷料包括吸湿抗菌层和保护层,吸湿抗菌层和保护层复合在一起。吸湿抗菌层用于与创口贴合;保护层位于吸湿抗菌层外侧,隔菌防水,对创面提供很好的保护作用。吸湿抗菌层包括抗菌药物和聚乙烯醇/壳聚糖纳米短纤维。聚乙烯醇/壳聚糖纳米短纤维经静电纺丝、交联和均质化处理得到。吸湿抗菌层是抗菌药物和聚乙烯醇/壳聚糖纳米短纤维的均质液经预冻成型、真空冷冻干燥、热处理、真空干燥得到的三维多级网孔材料。保护层包括聚乳酸/聚己内酯纳米纤维膜。聚乳酸/聚己内酯纳米纤维膜是经静电纺丝得到的纳米纤维膜。
本申请的吸液抗菌3D纳米纤维复合医用敷料的吸湿抗菌层选用聚乙烯醇和壳聚糖为主要原料,聚乙烯醇/壳聚糖具有良好的消炎止血、抗粘连、抗菌活性、生物相容性和生物可降解性,作为抗菌药物的载体,实现载体与药物的协同抗菌、长效抗菌。保护层选用聚己内酯和聚乳酸为主要原料,聚乳酸/聚己内酯具有良好的力学性能、疏水性、生物相容性和生物降解性。吸湿抗菌层直接与皮肤贴合,是具有三维多级网孔结构的材料,具有很高的孔隙率,能够大量吸收伤口渗出液并原位保留,防止皮肤浸渍且保持伤口湿润,适用于组织液渗液量较大的伤口,且纳米短纤维重组形成的独特网孔结构赋予吸湿抗菌层良好的力学性能,在吸收水分后材料变得柔软且与伤口紧密贴合,克服了二维纳米纤维膜吸液能力有限和贴合伤口欠佳的问题。保护层是静电纺丝聚合物膜材料,该膜材料的高孔隙率、高比表面积使其能够有效阻隔灰尘、细菌等入侵伤口,避免伤口感染,同时赋予伤口很好的的透气透湿性,保证创面能够接触到外界新鲜的氧气,保护创面液体不至于过快蒸发变干,提供一个相对湿润的修复环境;具有良好的的疏水性、生物相容性、生物降解性、力学性能,在使用过程中能够对创面起到很好的保护作用。
抗菌药物可以是银化合物、双胍盐、抗生素中的至少一种。银化合物为Ag2SO4、AgNO3和磺胺嘧啶银中的至少一种;双胍盐为聚六亚甲基双胍盐酸盐、壳聚糖双胍盐酸盐中的至少一种;所述抗生素为盐酸环丙沙星、庆大霉素、盐酸四环素、盐酸万古霉素中的至少一种。由于吸湿抗菌层中含有抗菌药物,药物能够避免伤口因细菌感染而导致的伤口恶化问题的发生,为伤口的愈合提供良好的环境保障。
本申请的吸液抗菌3D纳米纤维复合医用敷料的制备方法包括以下步骤:
步骤1,将壳聚糖和聚乙烯醇分别溶于在乙酸溶液、水中,搅拌至完全溶解,混合壳聚糖溶液和聚乙烯醇溶液,得到聚乙烯醇/壳聚糖纺丝溶液;壳聚糖的质量浓度为3-7%,乙酸溶液体积分数为1-3%,聚乙烯醇的质量浓度为5-10%,壳聚糖溶液和聚乙烯醇溶液按照体积比20:80-30:70进行混合。
步骤2,将步骤1中制备的聚乙烯醇/壳聚糖纺丝液转移至静电纺丝设备的注射器内,在注射器前端加上内径为0.1mm-1mm的不锈钢针头,控制电压为15kV-23kV,纺丝速度为0.1mL/h-0.5mL/h,接收距离为10cm-20cm的条件下进行纺丝,采用铝箔接收,得到聚乙烯醇/壳聚糖纳米纤维膜。
步骤3,将步骤2中制备的聚乙烯醇/壳聚糖纳米纤维膜在戊二醛蒸汽中室温交联4-5h,在45-55℃真空干燥箱中干燥72h,切成小块,加至溶剂中,均质化处理,得到聚乙烯醇/壳聚糖纳米短纤维的均质液;戊二醛溶液浓度为25-50%,均质化处理方法包括高速分散切割、超声波均质、冷冻切割中的至少一种。
高速分散切割过程是经由均质机的搅拌叶片高速转动对溶液中小块纤维膜进行切割形成短纤维,使短纤维长度在0-50000nm且均匀地分布在溶液中而形成均质液。高速分散机切割优选速度为6-15Krpm,时间为3-30min。
超声波均质过程是利用超声波在含有小块纳米纤维膜的溶液中的空化作用来达到均质效果的,使短纤维长度在10-500000nm且均匀地分布在溶液中。超声波均质优选功率为400-1200w,频率为18-21KHz,时间为10-30min。
冷冻切割过程为先将含小块纳米纤维膜溶液-80℃条件下冷冻,转移至低温恒温器中-20℃条件下切割得到10-500000nm短纤维,将短纤维加入到溶剂中搅拌均匀而得到均质液。冷冻切割优选在低温恒温器中-20℃条件下进行。
聚乙烯醇/壳聚糖纳米短纤维的均质液中聚乙烯醇/壳聚糖纳米短纤维的含量为10-30mg/ml,溶剂为水、酒精、叔丁醇、甘油等中的至少一种。本申请选用的溶剂能够为聚乙烯醇/壳聚糖纳米短纤维提供一个相对稳定的液相环境,不会影响聚乙烯醇/壳聚糖纳米短纤维的化学性质。
步骤4,将步骤3中的聚乙烯醇/壳聚糖纳米短纤维的均质液与抗菌药物混合并搅拌均匀,置于密封容器内,在-80℃下冷冻4-8h,使溶液完全凝固,然后真空冷冻干燥24-36h,取出,在80-100℃下热处理1-3h,最后真空干燥12-48h,得到具有三维多级网孔结构的抗菌吸湿层。
与聚乙烯醇/壳聚糖纳米短纤维均质液混合的抗菌药物含量为0.05~200mg/ml,所述抗菌药物为银化合物、双胍盐、抗生素中的至少一种。银化合物为Ag2SO4、AgNO3和磺胺嘧啶银中的至少一种;双胍盐为聚六亚甲基双胍盐酸盐、壳聚糖双胍盐酸盐中的至少一种;抗生素为盐酸环丙沙星、庆大霉素、盐酸四环素、盐酸万古霉素中的至少一种。
步骤5,将聚乳酸和聚己内酯分别溶于六氟异丙醇中,搅拌至完全溶解,混合并搅拌均匀,得到聚乳酸/聚己内酯纺丝溶液。聚乳酸和聚己内酯按照质量比70:30~90:10进行混合,聚乳酸和聚己内酯的质量分数为8~11%。
步骤6,将步骤5中制备的聚乳酸/聚己内酯纺丝液转移至静电纺丝设备的注射器内,在注射器前端加上内径为0.5mm-1mm的不锈钢针头,控制电压为10kV-20kV,纺丝速度为0.5mL/h-2mL/h,接收距离为10cm-25cm,在抗菌吸湿层上进行静电纺丝得到聚乳酸/聚己内酯纳米纤维保护层,经室温真空干燥得到3D纳米纤维复合医用敷料。
实施例1
(1)制备聚乙烯醇/壳聚糖纳米纤维膜:将0.3g壳聚糖溶于10mL 1%乙酸溶液中,将1g聚乙烯醇溶于10mL超纯水中,搅拌至完全溶解,取壳聚糖溶液和聚乙烯醇溶液按照体积比20:80混合,得到质量分数为8.6%的聚乙烯醇/壳聚糖纺丝溶液。将纺丝溶液转移至静电纺丝设备的10mL注射器内,在注射器前端加上内径为1mm的不锈钢针头,控制电压为15kV,纺丝速度为0.1mL/h,接收距离为10cm条件下进行纺丝,铝箔接收聚乙烯醇/壳聚糖纳米纤维膜。
(2)改性聚乙烯醇/壳聚糖纳米纤维膜:在浓度为50%戊二醛蒸汽中室温交联4h,在50℃真空干燥箱中干燥72h,切成小块。
(3)制备聚乙烯醇/壳聚糖纳米短纤维:称取2g聚乙烯醇/壳聚糖纳米纤维加至100mL体积分数为25%叔丁醇溶液中,然后在切割速度为8Krpm条件下高速分散切割20min,得到浓度为20mg/mL聚乙烯醇/壳聚糖纳米短纤维的均质液。
(4)制备混合的均质化溶液:将50mg盐酸四环素加至聚乙烯醇/壳聚糖纳米短纤维的均质液中并搅拌均匀。
(5)制备三维多级网孔材料:将混合均匀的均质液迅速转移至密封容器内,迅速置于-80℃下冷冻4h,然后冷冻真空干燥24h,取出,在90℃恒温条件下加热2h,最后真空干燥12h,得到具有三维多级网孔结构的抗菌吸湿层。
(6)制备聚乳酸/聚己内酯纳米纤维膜:取1g聚乳酸和4g聚己内酯分别溶于20mL六氟异丙醇中,搅拌至完全溶解,然后按照体积比80:20混合聚乳酸溶液和聚己内酯溶液,配成质量分数为10%聚乳酸/聚己内酯纺丝溶液。将纺丝溶液转移至静电纺丝设备的15mL注射器内,在注射器前端加上内径为0.6mm的不锈钢针头,控制电压为14kV,纺丝速度为0.5mL/h,接收距离为15cm条件下,在具有三维多级网孔结构的抗菌吸湿层上进行静电纺丝,得到聚乳酸/聚己内酯纳米纤维保护层,得到3D纳米纤维复合医用敷料。
实施例2
(1)制备聚乙烯醇/壳聚糖纳米纤维膜:将0.7g壳聚糖溶于10mL 3%乙酸溶液中,将0.7g聚乙烯醇溶于10mL超纯水中,搅拌至完全溶解,取壳聚糖溶液和聚乙烯醇溶液按照体积比30:70混合,得到质量分数为7%的聚乙烯醇/壳聚糖纺丝溶液。将纺丝溶液转移至静电纺丝设备的10mL注射器内,在注射器前端加上内径为0.84mm的不锈钢针头,控制电压为20kV,纺丝速度为0.1mL/h,接收距离为15cm条件下进行纺丝,铝箔接收聚乙烯醇/壳聚糖纳米纤维膜。
(2)改性聚乙烯醇/壳聚糖纳米纤维膜:将聚乙烯醇/壳聚糖纳米纤维膜在浓度为50%戊二醛蒸汽中室温交联5h,在55℃真空干燥箱中干燥72h,切成小块。
(3)制备聚乙烯醇/壳聚糖纳米短纤维:称取2.5g聚乙烯醇/壳聚糖纳米纤维加至100mL体积分数为25%叔丁醇溶液中,然后在切割速度为10Krpm条件下高速分散切割15min,得到浓度为25mg/mL聚乙烯醇/壳聚糖纳米短纤维的均质液。
(4)制备混合的均质化溶液:将0.2g聚六亚甲基双弧盐酸盐加至聚乙烯醇/壳聚糖纳米短纤维的均质液中并搅拌均匀。
(5)制备三维多级网孔材料:将混合均匀的均质液迅速转移至密封容器内,迅速置于-80℃下冷冻8h,然后冷冻真空干燥36h,取出,在95℃恒温条件下加热1.5h,最后真空干燥12h,得到具有三维多级网孔结构的抗菌吸湿层。
(6)制备聚乳酸/聚己内酯纳米纤维膜:取1g聚乳酸和11g聚己内酯分别溶于20mL六氟异丙醇中,搅拌至完全溶解,然后按照体积比90:10混合聚乳酸溶液和聚己内酯溶液,配成质量分数为10%聚乳酸/聚己内酯纺丝溶液。将纺丝溶液转移至静电纺丝设备的15mL注射器内,在注射器前端加上内径为0.9mm的不锈钢针头,控制电压为15kV,纺丝速度为1.5mL/h,接收距离为15cm条件下,在具有三维多级网孔结构的抗菌吸湿层上进行静电纺丝,得到聚乳酸/聚己内酯纳米纤维保护层,得到3D纳米纤维复合医用敷料。
除非另有定义,本申请中使用的所有技术和/或科学术语具有与由本发明所涉及的领域的普通技术人员通常理解的相同含义。本申请中提到的材料、方法和实施例仅为说明性的,而非限制性的。
虽然已结合具体实施方式对本发明进行了描述,在本申请的发明主旨下,本领域的技术人员可以进行适当的替换、修改和变化,这种替换、修改和变化仍属于本申请的保护范围。
Claims (10)
1.一种吸液抗菌3D纳米纤维复合医用敷料,其包括吸湿抗菌层和保护层;该吸湿抗菌层和保护层复合在一起;
所述吸湿抗菌层包括抗菌药物和聚乙烯醇/壳聚糖纳米短纤维;
所述保护层包括聚乳酸/聚己内酯纳米纤维膜。
2.如权利要求1所述的吸液抗菌3D纳米纤维复合医用敷料,其特征在于:
所述聚乙烯醇/壳聚糖纳米短纤维经静电纺丝、交联和均质化处理方法得到;所述吸湿抗菌层是抗菌药物和聚乙烯醇/壳聚糖纳米短纤维的均质液经预冻成型、真空冷冻干燥、热处理、真空干燥得到的三维多级网孔材料;
所述聚乳酸/聚己内酯纳米纤维膜是经静电纺丝得到的。
3.如权利要求1所述的吸液抗菌3D纳米纤维复合医用敷料,其特征在于:
所述抗菌药物为银化合物、双胍盐、抗生素中的至少一种;
所述银化合物为Ag2SO4、AgNO3和磺胺嘧啶银中的至少一种;
所述双胍盐为聚六亚甲基双胍盐酸盐、壳聚糖双胍盐酸盐中的至少一种;
所述抗生素为盐酸环丙沙星、庆大霉素、盐酸四环素、盐酸万古霉素中的至少一种。
4.如权利要求2所述的吸液抗菌3D纳米纤维复合医用敷料,其特征在于:
所述均质化处理方法包括高速分散切割、超声波均质、冷冻切割中的至少一种。
5.如权利要求1所述的吸液抗菌3D纳米纤维复合医用敷料,其特征在于:
所述聚乙烯醇/壳聚糖纳米短纤维的长度为10-500000nm。
6.一种制备吸液抗菌3D纳米纤维复合医用敷料的方法,其包括:
步骤1,将壳聚糖和聚乙烯醇分别溶解,然后混合并搅拌均匀,得到聚乙烯醇/壳聚糖纺丝溶液;
步骤2,将步骤1中制备的聚乙烯醇/壳聚糖纺丝溶液转移至静电纺丝设备的注射器内,设置控制电压、纺丝速度、接收距离,进行纺丝,采用铝箔接收,得到聚乙烯醇/壳聚糖纳米纤维膜;
步骤3,将步骤2中制备的聚乙烯醇/壳聚糖纳米纤维膜在交联剂中交联,在真空干燥箱中干燥,切成小块,加至溶剂中,均质化处理,得到聚乙烯醇/壳聚糖纳米短纤维的均质液;
步骤4,将步骤3中的聚乙烯醇/壳聚糖纳米短纤维的均质液与抗菌药物混合并搅拌均匀后,低温冷冻,使溶液完全凝固,然后真空冷冻干燥,热处理,最后再进行真空干燥,得到具有三维多级网孔结构的抗菌吸湿层;
步骤5,将聚乳酸和聚己内酯分别溶解,然后混合并搅拌均匀,得到聚乳酸/聚己内酯纺丝溶液;
步骤6,将步骤5中制备的聚乳酸/聚己内酯纺丝液转移至静电纺丝设备的注射器内,设置控制电压、纺丝速度、接收距离,在所述抗菌吸湿层上进行静电纺丝得到聚乳酸/聚己内酯纳米纤维保护层,经室温真空干燥得到3D纳米纤维复合医用敷料。
7.如权利要求6所述的制备吸液抗菌3D纳米纤维复合医用敷料的方法,其特征在于:
所述步骤1中,壳聚糖的质量浓度为3-7%,聚乙烯醇的质量浓度为5-10%,壳聚糖溶液和聚乙烯醇溶液按照体积比20:80-30:70进行混合;
所述步骤3中,交联剂浓度为25-50%;
所述步骤3中,均质化处理方法包括高速分散切割、超声波均质、冷冻切割中的一种或两种。
8.如权利要求7所述的制备吸液抗菌3D纳米纤维复合医用敷料的方法,其特征在于:
所述高速分散切割速度为6-15Krpm,时间为3-30min;
所述超声波均质功率为400-1200w,频率为18-21KHz,时间为10-30min;
所述冷冻切割是在低温恒温器中-20℃条件下进行。
9.如权利要求6所述的制备吸液抗菌3D纳米纤维复合医用敷料的方法,其特征在于:
所述步骤3中,聚乙烯醇/壳聚糖纳米短纤维的均质液中聚乙烯醇/壳聚糖纳米短纤维的含量为10-30mg/ml,溶剂为水、酒精、叔丁醇、甘油等中的至少一种。
10.如权利要求6所述的制备吸液抗菌3D纳米纤维复合医用敷料的方法,其特征在于:
所述步骤4中,与聚乙烯醇/壳聚糖纳米短纤维均质液混合的抗菌药物含量为0.05-200mg/ml;
所述步骤5中,聚乳酸和聚己内酯的按照质量比70:30-90:10进行混合,聚聚乳酸和聚己内酯的质量分数为8-11%。
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CN115382002A (zh) * | 2022-08-25 | 2022-11-25 | 东华大学 | 一种兼具智能抗菌及感染指示的海绵敷料及其制备方法 |
CN116370685A (zh) * | 2022-12-30 | 2023-07-04 | 武汉理工大学 | 一种快速促愈合的抗菌纳米纤维敷料及其制备方法 |
WO2025077051A1 (zh) * | 2023-10-12 | 2025-04-17 | 五邑大学 | 一种复合纤维基防护材料及其制备方法和应用 |
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