CN109364286A - 一种氧化石墨烯复合纳米纤维结构敷料及制备方法 - Google Patents
一种氧化石墨烯复合纳米纤维结构敷料及制备方法 Download PDFInfo
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- CN109364286A CN109364286A CN201811220706.3A CN201811220706A CN109364286A CN 109364286 A CN109364286 A CN 109364286A CN 201811220706 A CN201811220706 A CN 201811220706A CN 109364286 A CN109364286 A CN 109364286A
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- graphene oxide
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- oxide composite
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Abstract
本发明提供一种氧化石墨烯复合纳米纤维结构敷料及制备方法,先将纳米二氧化钛,沸石与PVA溶液混合搅拌均匀形成浆料,涂敷于承托层表面,干燥前喷涂一层0.2~2%的海藻酸钠溶液,40~75℃干燥,形成薄层,然后在薄层表面覆盖一层纳米纤维,接着涂覆由氧化石墨烯,海藻酸钠,透明质酸锌,维生素B2,维生素B12组成的浆料,干燥,喷洒少量锌盐溶液固化。本发明基于石墨烯的物理杀菌机理,结合纳米纤维膜的透气阻隔作用,负载有效成份制成结构敷料,通过各层对组织渗出液的吸收和消毒,保持伤口无菌状态,并提供必要营养物质,以避免伤口的二次感染,促进愈合,制备方法简单。
Description
技术领域
本发明涉及医用材料技术领域,具体涉及一种氧化石墨烯复合纳米纤维敷料及制备方法。
背景技术
皮肤受到创伤后使组织出现离断形成伤口,伤口局部有不同程度的组织坏死和血管断裂出血,数小时内便出现炎症反应,表现为充血、浆液渗出及白细胞游出,故局部红肿,并可能引起感染等并发症。伤口的修复是组织连续性和功能恢复的过程。伤口敷料是一种在伤口表面覆盖一层可以辅助身体促进伤口愈合的功能性医用辅料。它可以临时隔离伤口与外界环境,避免受到外部环境的感染。同时敷料中负载特定物质可以促进伤口愈合。
在伤口愈合过程中,病菌是导致伤口感染恶化的主要原因。研究表明,石墨烯具有抗菌和抑菌性能,其层状结构表面丰富的官能团还可以通过负载有效组分进一步对付病菌或病毒。
专利申请号为201810369012的发明专利涉及一种具有抑菌抗瘢痕双重作用的氧化石墨烯伤口敷料的制备方法,以氧化石墨烯作为原料,经过超声振荡分散、固液分离、药物负载三个基本程序而得到产品。该发明制备的氧化石墨烯敷料厚度可控,比表面积大,吸附性优良,强度和柔韧性好,无毒无菌,抑菌、抗瘢痕形成,对人体无刺激,与皮肤伤口无粘结性,环保;制备方法简单,操作方便,生产成本较低。该发明制备的伤口敷料可广泛用于常规及微创整形手术的伤口愈合及抗瘢痕形成,皮肤烧伤、挫伤等创面的愈合及抗瘢痕形成。该专利敷料无法给予伤口保湿性及营养供给以促进组织愈合,只起到在结构上隔离伤口,在抗菌方面防止感染的作用,并靠患者自身免疫能力自行愈合。
发明内容
为解决上述技术问题,本发明提供一种氧化石墨烯复合纳米纤维结构敷料,本发明基于石墨烯的物理杀菌机理,结合纳米纤维膜的透气阻隔作用,负载有效成份制成结构敷料,通过各层对组织渗出液的吸收和消毒,保持伤口无菌状态,并提供必要营养物质,以避免伤口的二次感染,促进愈合,制备方法简单。
本发明提供一种氧化石墨烯复合纳米纤维结构敷料,由三层结构组成,三层结构为承托层、中间层、内层,承托层、中间层、内层由上到下逐层设置。承托层厚度基本为布料本身厚度,中间层厚度为0.10~10微米、内层厚度为0.1~2微米,承托层、中间层、内层面积相同。
优选的是,所述承托层与空气接触,承托层采用普通医用网格物或织物中的至少一种制作而成。
上述任一方案优选的是,所述织物为无纺布。
上述任一方案优选的是,所述承托层上部涂覆有纳米二氧化钛、PVA、沸石粉制成的浆料。浆料的制备方法为:将聚乙烯醇粉末(PVA)用90~100℃的去离子水配成溶解质量浓度为0.1~6%溶液,然后加入纳米二氧化钛、沸石粉形成悬浊液,混合搅拌,迅速涂敷。为了防止悬浊液分层,涂敷时悬浊液不停地搅拌。二氧化钛、沸石粉与PVA的用量比为1:0.2~3:0.01~0.1。所述用量指质量。
上述任一方案优选的是,所述纳米二氧化钛、沸石粉与PVA的用量比为1:0.2~3:0.01~0.1。
上述任一方案优选的是,所述纳米二氧化钛、沸石粉与PVA的用量比为1:0.2:0.01。
上述任一方案优选的是,所述纳米二氧化钛、沸石粉与PVA的用量比为1:1:0.05。
上述任一方案优选的是,所述纳米二氧化钛、沸石粉与PVA的用量比为1:2:0.05。
上述任一方案优选的是,所述纳米二氧化钛、沸石粉与PVA的用量比为1:3:0.1。
上述任一方案优选的是,所述中间层采用纳米纤维制作而成,纳米纤维为PVA、PEO、PCL中的至少一种。
上述任一方案优选的是,所述内层与伤口接触,内层由氧化石墨烯、海藻酸钠、透明质酸锌、维生素B2、维生素B12制成的浆料涂覆而成。浆料的质量组成如下:水100份,氧化石墨烯0.2~8份,海藻酸钠0.1~3份,透明质酸锌0.05~4份,维生素B2为0.01~0.2份,维生素B12为0.01~0.1份;将上述组分混合搅拌均匀,形成氧化石墨烯和其他组分溶液组成的浆料。
本发明还提供一种氧化石墨烯复合纳米纤维结构敷料的制备方法,包括以下步骤:
(1)承托层的制备:将纳米二氧化钛、沸石与PVA溶液混合均匀形成浆料,涂敷于无纺布、织物或网格物表面,干燥前喷涂海藻酸钠溶液,干燥;
(2)中间层的制备:将纳米纤维覆盖在步骤(1)制备好的承托层表面;
(3)内层的制备:将氧化石墨烯、海藻酸钠、透明质酸锌、维生素B2、维生素B12、组成的浆料涂覆在中间层表面,干燥,再喷洒少量锌盐溶液,固化。
上述任一方案优选的是,所述步骤(1)中纳米二氧化钛、沸石粉与PVA的用量比为1:0.2~3:0.01~0.1。
上述任一方案优选的是,所述步骤(1)中承托层与空气接触,承托层采用网格物或织物中的至少一种制作而成。
上述任一方案优选的是,所述织物为无纺布。
上述任一方案优选的是,所述步骤(1)中喷涂的海藻酸钠溶液质量浓度为0.2~2%,喷涂量为20-100ml/m2。海藻酸钠为白色或淡黄色粉末,几乎无臭无味。海藻酸钠溶于水,不溶于乙醇、乙醚、氯仿等有机溶剂。溶于水后成粘稠状液体,1%水溶液pH值为6-8。当pH=6-9时粘性稳定,加热至80℃以上时则粘性降低。海藻酸钠无毒,LD50>5000mg/kg。海藻酸钠微溶于水,不溶于大部分有机溶剂。它溶于碱性溶液,使溶液具有粘性。海藻酸钠粉末遇水变湿,微粒的水合作用使其表面具有粘性。然后微粒迅速粘合在一起形成团块,团块很缓慢的完全水化并溶解。如果水中含有其它与海藻酸盐竞争水合的化合物,则海藻酸钠更难溶解于水中。水中的糖、淀粉或蛋白质会降低海藻酸钠的水合速率,混合时间有必要延长。单价阳离子的盐(如NaCl)在浓度高于0.5%时也会有类似的作用。海藻酸钠在1%的蒸馏水溶液中的pH值约为7.2。海藻酸钠具有吸湿性,平衡时所含水分的多少取决于相对湿度。干燥的海藻酸钠在密封良好的容器内于25℃及以下温度储存相当稳定。海藻酸钠溶液在pH5~9时稳定。
上述任一方案优选的是,所述步骤(1)中在40~75℃干燥25~60min。
上述任一方案优选的是,所述步骤(2)中纳米纤维为PVA、PEO、PCL中的至少一种。
上述任一方案优选的是,所述步骤(3)中干燥温度为35~65℃,干燥时间为30~50min。
上述任一方案优选的是,所述步骤(3)中锌盐溶液为氯化锌、醋酸锌、硝酸锌、柠檬酸锌溶液中的至少一种,质量浓度1%~2%,喷洒量为10~60ml/m2。
上述任一方案优选的是,所述步骤(3)中固化温度为35~75℃,固化时间为20~75min。
本发明的上述技术方案的有益效果如下:本发明提供一种氧化石墨烯复合纳米纤维结构敷料的制备方法,首先将纳米二氧化钛,沸石与PVA溶液混合搅拌均匀形成浆料,涂敷于承托层表面,干燥前喷涂一层0.2~2%的海藻酸钠溶液,40~75℃干燥,形成薄层,然后在薄层表面覆盖一层纳米纤维,接着涂覆由氧化石墨烯,海藻酸钠,透明质酸锌,维生素B2,维生素B12组成的浆料,干燥,喷洒少量锌盐溶液固化。本发明基于石墨烯的物理杀菌机理,结合纳米纤维膜的透气阻隔作用,负载有效成份制成结构敷料,通过各层对组织渗出液的吸收和消毒,保持伤口无菌状态,并提供必要营养物质,以避免伤口的二次感染,促进愈合,制备方法简单。
附图说明
图1为本发明的氧化石墨烯复合纳米纤维结构敷料的结构示意图。
具体实施方式
为使本发明要解决的技术问题、技术方案和优点更加清楚,下面将结合附图及具体实施例进行详细描述。
实施例1
氧化石墨烯复合纳米纤维结构敷料的制备方法如下,如图1所示:
(1)承托层100的制备:将纳米二氧化钛、沸石与PVA(用量比为1:0.2:0.03)溶液混合搅拌均匀形成浆料,涂敷于无纺布、织物或网格物表面,干燥前喷涂一层1%的海藻酸钠溶液50ml/m2,50℃干燥30min,形成薄层。
(2)中间层200的制备:在步骤(1)制备的薄层表面覆盖纳米纤维膜PVA200。纤维膜的克重为2g/m2。
(3)内层300的制备:在中间层上部涂覆由氧化石墨烯,海藻酸钠,透明质酸锌,维生素B2,维生素B12和水,组成的浆料。浆料的质量组成如下:水100份,氧化石墨烯0.5份,海藻酸钠0.25份,透明质酸锌0.06份,维生素B2为0.015份,维生素B12为0.01份。将这些组分混合搅拌均匀,形成氧化石墨烯和其他组分溶液组成的浆料。40℃干燥25min,再喷洒少量氯化锌溶液(15ml/m2),在40℃固化35min。
实施例2
氧化石墨烯复合纳米纤维结构敷料的制备方法如下:
(1)承托层100的制备:将纳米二氧化钛、沸石与PVA(1:1:0.02)溶液混合搅拌均匀形成浆料,涂敷于无纺布,织物或网格物表面,干燥前喷涂一层0.2%的海藻酸钠溶液(25ml/m2),45℃干燥25min,形成薄层。
(2)中间层200的制备:在薄层表面覆盖纳米纤维膜PVA。纤维膜的克重为2g/m2。
(3)内层300的制备:在中间层上部涂覆由氧化石墨烯,海藻酸钠,透明质酸锌,维生素B2,维生素B12组成的浆料,浆料的组成如下:水100份,氧化石墨烯3份,海藻酸钠1.6份,透明质酸锌2.6份,维生素B2为0.10份,维生素B12为0.08份。将这些组分混合搅拌均匀形成氧化石墨烯和其他组分溶液组成的浆料。40℃干燥25min,再喷洒少量氯化锌溶液(15ml/m2),在40℃固化35min。
实施例3
氧化石墨烯复合纳米纤维结构敷料的制备方法如下:
(1)承托层100的制备:将纳米二氧化钛、沸石与PVA(1:2.8:0.08)溶液混合搅拌均匀形成浆料,涂敷于无纺布,织物或网格物表面,干燥前喷涂一层0.5%的海藻酸钠溶液(80ml/m2),70℃干燥45min,形成薄层。
(2)中间层200的制备:在薄层表面覆盖纳米纤维膜PVA。纤维膜的克重为3.5g/m2。
(3)内层300的制备:在中间层上部涂覆由氧化石墨烯,海藻酸钠,透明质酸锌,维生素B2,维生素B12等组成的浆料,浆料的组成如下:水100份,氧化石墨烯7.3份,海藻酸钠2.4份,透明质酸锌3.7份,维生素B2为0.17份,维生素B12为0.08份。将这些组分混合搅拌均匀形成氧化石墨烯和其他组分溶液组成的浆料。50℃干燥35min,再喷洒少量氯化锌溶液(55ml/m2),在60℃固化55min。
上述实施例所得的结构性敷料按照AATCC-100-2012试验法进行抗菌率测试抗菌性能如表1所示:
表1本发明制备的结构性敷料抗菌性能测试结果
本发明实施例结构敷料根据GB/T12704-1991织物透湿量测定方法透湿杯法,测定本发明制得复合面料的性能,透湿性能如表2所示:
表2本发明实施例结构敷料的透湿性能测试结果
*其中,人体无汗日透湿量约2500g/m2·24h。
从上述结果可以看出,石墨烯的含量显著影响透湿率,含量越高,透湿率明显下降。从透湿量看,所得敷料透湿性能良好,明显高于人体无汗时水分蒸发量2500ml/m2·24h。更结合纳米纤维膜的透气阻隔作用,使敷料具备较好透气性。同时抗菌数据显示敷料对于金黄色葡萄球菌的抗菌性能随着石墨烯的含量增加而呈现一定增强的趋势,其均表现出很好的抗菌性能。
以上详细描述了本发明的较佳具体实施例。应当理解,本领域的普通技术人员无需创造性劳动就可以根据本发明的构思作出诸多修改和变化。因此,凡本技术领域中技术人员依本发明的构思在现有技术的基础上通过逻辑分析、推理或者有限的实验可以得到的技术方案,皆应在由权利要求书所确定的保护范围内。
Claims (10)
1.一种氧化石墨烯复合纳米纤维结构敷料,其特征在于,包括三层结构,三层结构为承托层、中间层、内层,承托层、中间层、内层由上到下逐层设置。
2.如权利要求1所述的一种氧化石墨烯复合纳米纤维结构敷料,其特征在于,所述承托层与空气接触,承托层采用普通医用网格物或织物中的至少一种制作而成。
3.如权利要求1所述的一种氧化石墨烯复合纳米纤维结构敷料,其特征在于,所述承托层上部涂覆有纳米二氧化钛、PVA、沸石粉制成的浆料。
4.如权利要求1所述的一种氧化石墨烯复合纳米纤维结构敷料,其特征在于,所述中间层采用纳米纤维制作而成,纳米纤维为PVA、PEO、PCL中的至少一种。
5.如权利要求1所述的一种氧化石墨烯复合纳米纤维结构敷料,其特征在于,所述内层与伤口接触,内层由氧化石墨烯、海藻酸钠、透明质酸锌、维生素B2、维生素B12制成的浆料涂覆而成。
6.一种氧化石墨烯复合纳米纤维结构敷料的制备方法,其特征在于,包括以下步骤:
(1)承托层的制备:将纳米二氧化钛、沸石与PVA溶液混合均匀形成浆料,涂敷于无纺布、织物或网格物表面,干燥前喷涂海藻酸钠溶液,干燥;
(2)中间层的制备:将纳米纤维覆盖在步骤(1)制备好的承托层表面;
(3)内层的制备:将氧化石墨烯、海藻酸钠、透明质酸锌、维生素B2、维生素B12、组成的浆料涂覆在中间层表面,干燥,再喷洒少量锌盐溶液,固化。
7.如权利要求6所述的一种氧化石墨烯复合纳米纤维结构敷料的制备方法,其特征在于,所述步骤(1)中纳米二氧化钛、沸石粉与PVA的用量比为1:0.2~3:0.01~0.1。
8.如权利要求6所述的一种氧化石墨烯复合纳米纤维结构敷料的制备方法,其特征在于,所述步骤(1)中喷涂的海藻酸钠溶液为0.2~2%,喷涂量为20~100ml/m2。
9.如权利要求6所述的一种氧化石墨烯复合纳米纤维结构敷料的制备方法,其特征在于,所述步骤(2)中纳米纤维为PVA、PEO、PCL中的至少一种。
10.如权利要求6所述的一种氧化石墨烯复合纳米纤维结构敷料的制备方法,其特征在于,所述步骤(3)中锌盐溶液为氯化锌、醋酸锌、硝酸锌、柠檬酸锌溶液中的至少一种,喷洒量为10~60ml/m2。
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