CN107456598A - 一种新型纳米银活性炭纤维多功能医用材料的制备方法 - Google Patents
一种新型纳米银活性炭纤维多功能医用材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种纳米银活性炭纤维多功能医用材料的制备方法，属于医用敷料制备技术领域。本发明对活性炭纤维(Activated Carbon Fiber，ACF)表面改性和纳米银(Nanometer Silver，Ag)表面修饰，通过静电自组装使两者有机结合，研制出纳米银活性炭纤维(Ag/ACF)止血、抗菌、促愈合医用材料，国际上尚无同类产品问世。利用ACF强的吸附创面渗出物，激活凝血机制，加速止血的效应，结合纳米银高的抗菌、抑菌性和不产生耐药性解决已用材料的局限性。研究尺寸稳定在10nm左右的表面带负电性纳米Ag、大比表面积带正电性ACF以及通过静电自组装Ag/ACF医用材料的制备；评价Ag/ACF医用材料止血、抗菌、促愈合功效及Ag与ACF的“协同作用”机制。
Description
技术领域
本发明涉及一种纳米银活性炭纤维多功能医用材料的制备方法，属于医用敷料制备技术领域。
背景技术
活性炭纤维(activated carbon fiber，ACF)敷料是近年开发的一种新型高分子医用敷料，具有比表面积大，有效吸附容量高，吸附、脱附速度快，易再生，含灰量低，化学稳定性强，良好的柔韧性和强度等特性。活性炭纤维强的吸附作用和表面存在多种官能团，可与创面中的多种凝血因子发生氧化还原反应，激活凝血机制，具有加速止血的效应。ACF敷料通过其活性炭纤维强大的吸附性和表面丰富的微孔结构，将组织液、脓汁、细菌及致病微生物吸入微孔内，改变生存环境使其死亡，减轻炎性反应，加速创面愈合。
为防止伤口感染，以往许多敷料使用时加入抗生素，而抗生素的长期大剂量使用会产生耐药性，时至今日，一些细菌已很难用抗生素杀灭。在使用核生化武器的特殊战争条件下，伤员的创面污染情况可能更为复杂，进一步加剧了感染伤口创面的治疗难度。组织创面的现场包扎止血及防治感染是战伤、创伤急救的首要步骤。选择性能良好的包扎敷料可以有效提高创面止血的效率并降低后期感染并发症的发生率。目前，创伤现场急救措施基本沿用几十年前的传统方法，创面包扎敷料缺乏现代科技含量，治疗功能落后，敷料体积笨重，显然难以适应现代抢救装备的需要。为此，世界各国学者对创面敷料的改进进行了大量研究，但进展缓慢，特别是原材料的革新更是乏善可陈。因此，研发一种适应当前战伤医学和创伤医学需求、具有强大止血、杀菌、促愈合多功能的新型医用敷料已是迫在眉睫的现实课题。
银及其化合物以其独特的、优良的抗菌和抑菌性能已经在医学、卫生等领域得到了广泛应用。银可以阻断细菌内电子传输，增加细菌DNA稳定性从而削弱细菌的细胞复制银，还可破坏细菌的结构和受体功能，形成不可溶的无效代谢化合物，从而有助于感染的预防和控制，银还可以减少伤口表面的炎症促进伤口愈合，至今没有一种细菌可以逃过离子化银的杀灭作用。另外，还没有任何病例报告银离子或金属银有致敏性。载银抗菌医用敷料就是结合银的抗菌性和医用敷料的优良性能，发挥抗菌作用，可有效控制难愈性创面的细菌生长、减轻创面局部感染；吸附创面分泌物，改善创面局部的微环境，促进创面的上皮化和再上皮化，促进伤口的愈合，含银敷料已成为医用敷料发展的一个重要方向。
大量资料表明，仍在医疗领域广泛使用的棉质纱布、绷带等传统敷料，已难以满足临床治疗和各种灾害现场的需要。如何通过改进医用敷料的性能、提高其抑菌杀菌能力、预防或治疗创面感染、加速创面愈合进程，应对耐药菌感染带来的困局是当今医学界研究的热点。尽管世界各国研制开发的新型医用敷料层出不穷，但由于价格昂贵或性能单一等原因，目前尚没有一种新型敷料取得真正意义上的广泛使用。因此，研制并生产低成本、高性能的多功能医用敷料具有深远的意义。
鉴于上述背景，本发明针对现代战伤、灾害创伤组织创面的自身发展规律及特点，对相关创面敷料材料进行了科学论证，借鉴活性炭纤维表面多种官能团具有激活凝血机制、加速止血以及吸附、过滤灭菌的传统优势，结合纳米银杀菌无耐药性物理特性，提出将两者物质进行有机结合，形成新型具有多功能复合敷料。通过静电自组装制成的复合敷料安全可靠，体积小巧，作用强大，材料价廉，资源广泛，适于规模生产。
发明内容
本发明的主要目的在于，获得尺寸在10nm以下、稳定的表面带负电性纳米Ag，大比表面积表面带正电性ACF以及纳米银活性炭纤维医用材料的制备工艺参数；研制出可商用的纳米银活性炭纤维复合物止血、抗菌、促愈合敷料产品；为研制新型高效止血、抗菌、促愈合的现场救护医用材料提供临床研究的理论基础和经验积累。
为解决上述技术问题，本发明是采用如下所述的技术方案来实现的：
(1)银纳米粒子的合成、表面修饰及性质表征：采用硼氢化物或柠檬酸钠还原硝酸银的方法，制备不同尺寸的银纳米粒子(2～50nm)，选择具有负电性、碳原子数为3，8，11和 16的ω-巯基烷酸作为银纳米粒子的稳定分子，制备表面单层修饰的负电性银纳米粒子。采用XRD、HRTEM、UV-Vis、XPS和FT-IR等方法对合成的粒子的尺寸、形态、和表面修饰分子进行表征，并测定银纳米粒子的表面Zeta电位。
(2)活性炭纤维表面改性：采用ZnCl2、H3PO4、KOH等化学活化纤维素基、PAN基、酚醛基、沥青基、聚乙烯醇基、苯乙烯/烯烃共聚物和木质素纤维为前驱体制备活性炭纤维，制备不同比表面积和孔道结构且可医用的ACF作为基材，通过改变其表面酸、碱性，提高表面正电性。通过氧化或还原引入亲水性官能团或除去某些表面憎水性官能团，制备易于与带负电性纳米银颗粒的复合，优良的亲水性，减小与创面的粘连的活性炭纤维底材。采用FESEM、比表面积分析仪(BET)和FT-IR的方法对合成活性炭纤维尺寸、孔道结构、形态进行表征。
(3)纳米银活性炭纤维复合物止血、抗菌、促愈合医用敷料的制备：①将表面单层修饰的负电性银纳米粒子溶液通过雾化方式喷涂在活性炭纤维上，再切割，成型，最后用臭氧消毒制备成敷料。②将活性炭纤维通过快速提拉的方式通过表面单层修饰的负电性银纳米粒子溶液利用静电自组装制备成敷料样品，烘干、切割，成型、臭氧消毒后得纳米银活性炭纤维复合物止血、抗菌、促愈合医用敷料。
本发明的应用方法：将本发明制得的高止血医用敷料贴于伤口处，每1～2天更换一次即可。该医用敷料抗牵拉能力和组织亲附力好，可使创面保持湿润，避免更换敷料时伤口发生损伤，可有效防止灰尘和微生物的侵入，预防交叉感染，促进伤口愈合，能在2～3min内快速止血。
本发明所述的纳米银活性炭纤维止血、抗菌、促愈合敷料与现有的同类产品相比具有如下特点：
(1)止血性能：活性炭纤维表面存在多种官能团，可与创面中的多种凝血因子发生氧化还原反应，激活凝血机制，具有加速止血的效应。
(2)杀菌性能：一方面，活性炭纤维具有强大的吸附和过滤作用，能将常见有害细菌如金黄色葡萄球菌、大肠杆菌、绿脓杆菌、肺炎杆菌等牢固结合、沉淀；能对生化武器中的炭疽杆菌、芥子气等起到有效的过滤防御作用。另一方面，敷料中的纳米银释放出的银粒子能够透过细胞壁，可将吸附于碳纤维表面的菌体内蛋白凝固、使细菌失活，且灭菌能力持久、不易产生耐药性。因此，该复合敷料具有双重灭菌功效。
(3)吸附性能：在产生相同吸附作用条件下，本发明复合型敷料较传统纱布敷料的重量及体积均减小100倍以上，携带方便；而其抑菌杀菌及止血效果却增大数十倍，功效显著。
附图说明
图1为纳米银活性炭纤维医用敷料的制备技术路线。
具体实施方式
纳米银活性炭纤维医用敷料的制备技术路线见图1。首先采用硼氢化物或柠檬酸钠还原硝酸银的方法，制备不同尺寸的银纳米粒子(2～50nm)，选择具有负电性、碳原子数为3， 8，11和16的ω-巯基烷酸作为金纳米粒子的稳定分子，制备表面单层修饰的负电性银纳米粒子。采用XRD、HRTEM、UV-Vis、XPS和FT-IR等方法对合成的粒子的尺寸、形态、和表面修饰分子进行表征，并测定银纳米粒子的表面Zeta电位。采用ZnCl2、H3PO4、KOH 等化学活化纤维素基、PAN基、酚醛基、沥青基、聚乙烯醇基、苯乙烯/烯烃共聚物和木质素纤维为前驱体活性碳纤维，制备的不同比表面积和孔道结构且可医用的ACF作为基材，通过改变其表面酸、碱性，提高表面正电性，通过氧化或还原引入亲水性官能团或除去某些表面憎水性官能团，制备易于与带负电性纳米银颗粒的复合，亲水性优良，减小与创面的粘连的活性碳纤维底材。采用FESEM、比表面积分析仪(BET)和FT-IR等方法对合成活性碳纤维尺寸、孔道结构、形态进行表征。最后纳米银活性炭纤维复合物止血、抗菌、促愈合医用敷料的制备：①将表面单层修饰的负电性银纳米粒子溶液通过雾化方式喷涂在活性炭纤维上，再切割，成型，最后用臭氧消毒制备成敷料。②将活性炭纤维通过快速提拉的方式通过表面单层修饰的负电性银纳米粒子溶液利用静电自组装制备成敷料样品，烘干、切割，成型、臭氧消毒后得纳米银活性炭纤维复合物止血、抗菌、促愈合医用敷料。
将本发明制得的高止血、抗菌、促愈合医用敷料贴于伤口处，每1天更换一次即可。该医用敷料抗牵拉能力和组织亲附力好，可使创面保持湿润，避免更换敷料时伤口发生损伤，可有效防止灰尘和微生物的侵入，预防交叉感染，促进伤口愈合，能在2min内快速止血。
Claims (1)
1.一种纳米银活性炭纤维多功能医用材料的制备方法，其特征在于具体制备步骤为：
(1)银纳米粒子的合成、表面修饰及性质表征：采用硼氢化物或柠檬酸钠还原硝酸银的方法，制备不同尺寸的银纳米粒子(2～50nm)，选择具有负电性、碳原子数为3，8，11和16的ω-巯基烷酸作为银纳米粒子的稳定分子，制备表面单层修饰的负电性银纳米粒子。采用XRD、HRTEM、UV-Vis、XPS和FT-IR等方法对合成的粒子的尺寸、形态、和表面修饰分子进行表征，并测定银纳米粒子的表面Zeta电位。
(2)活性炭纤维表面改性：采用ZnCl2、H3PO4、KOH等化学活化纤维素基、PAN基、酚醛基、沥青基、聚乙烯醇基、苯乙烯/烯烃共聚物和木质素纤维为前驱体制备活性炭纤维，制备不同比表面积和孔道结构且可医用的ACF作为基材，通过改变其表面酸、碱性，提高表面正电性。通过氧化或还原引入亲水性官能团或除去某些表面憎水性官能团，制备易于与带负电性纳米银颗粒的复合，优良的亲水性，减小与创面的粘连的活性炭纤维底材。采用FESEM、比表面积分析仪(BET)和FT-IR的方法对合成活性炭纤维尺寸、孔道结构、形态进行表征。
(3)纳米银活性炭纤维复合物止血、抗菌、促愈合医用敷料的制备：①将表面单层修饰的负电性银纳米粒子溶液通过雾化方式喷涂在活性炭纤维上，再切割，成型，最后用臭氧消毒制备成敷料。②将活性炭纤维通过快速提拉的方式通过表面单层修饰的负电性银纳米粒子溶液利用静电自组装制备成敷料样品，烘干、切割，成型、臭氧消毒后得纳米银活性炭纤维复合物止血、抗菌、促愈合医用敷料。
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