CN114657647B - 一种抗菌导电海藻酸盐纤维的制备方法与应用 - Google Patents
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Abstract
本发明公开了一种抗菌导电海藻酸盐纤维的制备方法,主要是将海藻酸钠溶液注入低温凝固液中,使其迅速凝胶化并在凝固液中长时间浸渍盐析,海藻酸钠溶液在钙离子作用下有序聚集浓缩成初生丝条,再经过牵伸取向细化获得良好机械性能,然后浸入锌盐凝固液中盐析并且再次牵伸,从而获得高强度的抗菌导电海藻酸盐纤维。该纤维生物相容性好,机械性能强,具有抗菌导电功能,在手术缝合线、人工韧带和柔性传感器等方面有应用前景。
Description
技术领域
本发明属于高分子纤维材料领域,具体涉及一种抗菌导电海藻酸盐纤维的制备方法与应用。
背景技术
海藻酸钠是一种天然多糖类高分子化合物,主要从天然海藻中提取,是一种绿色可再生资源且产量巨大。海藻酸钠具有良好的生物相容性、生物可降解性和安全无毒,已被广泛应用于纺织、食品、医药等领域。海藻酸钠水溶液浓度低、粘度高,在金属钙离子作用下会发生凝胶化,故通常将海藻酸钠溶液挤出到氯化钙溶液中凝固成纤维,但这种条件下得到的海藻酸盐纤维强度不高。因此,海藻酸盐纤维主要加工成无纺布,用于面膜、医用纱布和绷带等产品。提高海藻酸盐纤维的强度就能进一步拓展其应用领域和价值。
以高浓度海藻酸钠溶液能制备高强度的海藻酸盐纤维,但海藻酸钠不能通过直接溶解得到高浓度溶液,只能通过稀的海藻酸钠溶液逐渐浓缩得到高浓度溶液。2019年的文献Advanced Materials第31期1902381号发表的名称为“Cooking-Inspired VersatileDesign of an Ultrastrong and Tough Polysaccharide Hydrogel through ProgrammedSupramolecular Interactions”,通过煮沸的方式将海藻酸钠溶液熬制成高浓度溶液,并制备了高强度的凝胶体材料。但这种方式并不是适合纺丝。专利CN1986921A公开了一种海藻纤维凝胶纺丝工艺,将海藻酸钠溶于氢氧化钠和次氯酸钠的溶液中,得到浓度5~25%的海藻酸钠溶液,但从实施例中发现,海藻酸钠溶液的浓度最高是10%,显然25%浓度不能通过直接溶解得到。近来的研究表明,高分子溶液通过冷冻固化后,再浸入盐溶液中浸泡,由于Hofmeister效应,这些高分子会聚集成高强度的凝胶体。因此,在盐溶液中浸泡同样实现了高分子溶液的浓缩,这对通过稀的海藻酸钠溶液制备高强度纤维提供了有力条件。
发明内容
本发明的目的在于提供一种抗菌导电海藻酸盐纤维的制备方法,使海藻酸盐纤维具有抗菌导电功能的同时,还具有高强的机械性能。为了实现上述发明目的,本发明使海藻酸钠溶液迅速凝胶化,并使海藻酸钠凝胶丝进一步冷冻盐析,形成结构更紧密的聚集体,经牵伸使海藻酸盐大分子取向细化,再经吸附锌离子和牵伸细化,得到具有抗菌导电功能的高强度海藻酸盐纤维。该纤维具有良好的生物特性和功能性,在手术缝合线、人工韧带以及柔性传感器等方面有应用潜力。
本发明提供的技术方案是采用如下方法制备抗菌导电海藻酸盐纤维:
S1.分别将海藻酸钠和聚乙烯醇溶解混合,得到混合溶液A;
S2.将钙盐溶于低级醇和低级多元醇的混合溶剂中得到凝固液B,并将凝固液B的温度控制在0~10℃,所述钙盐为氯化钙、硝酸钙、磷酸二氢钙、乳酸钙、甲酸钙、高氯酸钙等中的任意一种,所述低级多元醇为乙二醇、丙三醇、丁二醇、三乙醇胺中的任意一种,所述低级醇为甲醇、乙醇、异丙醇中的任意一种;
S3.将S1所得的溶液A注入凝固液B中浸渍盐析,得到凝胶化纤维;
S4.将S3所得凝胶化纤维牵伸,并浸入含锌盐的丙酮溶剂C中二次盐析,所述锌盐为氯化锌、硫酸锌、硝酸锌、乙酸锌中的任意一种;
S5.将S4所得纤维水洗,再牵伸,干燥,即得抗菌导电海藻酸盐纤维。
进一步地,S1所述溶液A中海藻酸钠的浓度3~5 wt%,聚乙烯醇的浓度0.1~2 wt%。
进一步地,S2所述凝固液B中钙盐的浓度5~20 wt%,所述低级多元醇的浓度为1~3wt%,其余为低级醇。
进一步地,S3所述海藻酸溶液注射直径为2~5 mm,成型丝条在0~10℃的凝固液B中浸渍盐析时间12~24h。
进一步地,S4所述纤维牵伸倍数为1.5~3倍。
进一步地,S4所述锌盐的浓度为5~10 wt%,纤维在溶剂C中浸渍盐析时间1~6h。
进一步地,S5中纤维牵伸倍数为1.2~3倍。
另外,本发明还提供了上述制备方法得到的一种抗菌导电海藻酸盐纤维在手术缝合线、人工韧带、柔性传感器中的应用。
本发明的有益效果在于:
1)海藻酸钠稀溶液在低温凝固液中迅速凝胶化形成丝条,使丝条在凝固液中盐析较长时间,海藻酸钠大分子在钙离子作用下逐渐有序聚集、浓缩,再在牵伸作用下取向细化,从而获得高强机械性能。
2)以锌盐的丙酮溶剂对海藻酸盐纤维丝条进行第二次盐析,使纤维表层螯合了锌离子,从而使纤维具有抗菌性,同时避免了纤维中钙离子的解离。由于离子导电原因,纤维在一定湿度下具有良好导电性。
3)本发明的制备方法工艺条件简单,生产成本低。制备的海藻酸盐纤维具有高强度、抗菌性和弱导电性,而且生物相容性好,在手术缝合线、人工韧带和可植入传感器等方面有潜在应用价值。
具体实施方式
下面结合具体实施例对本发明作进一步详细地描述,但本发明的实施方式不限于此。
实施例1
将0.6g海藻酸钠溶于14.38ml水,将0.02g聚乙烯醇溶于5ml水,再将它们混合均匀,得到混合溶液A。将10g氯化钙和2g丙三醇溶于188g乙醇中,得到凝固液B,再将凝固液B置于4℃冷藏。将溶液A通过2mm喷嘴注入凝固液B中,使初生丝条在其中盐析24h。将10氯化锌溶于190g丙酮溶剂中,得到凝固液C。将盐析的丝条牵伸1.5倍,然后置于凝固液C中盐析1h。然后,将二次盐析的海藻酸盐纤维经过水洗,再次牵伸2倍,再风干,即得抗菌导电海藻酸盐纤维。
实施例2
将1g海藻酸钠溶于13.6ml水,将0.4g聚乙烯醇溶于5ml水,再将它们混合均匀,得到混合溶液A。将40g甲酸钙和6g乙二醇溶于154g异丙醇中,得到凝固液B,再将凝固液B置于0℃冷藏。将溶液A通过3mm喷嘴注入凝固液B中,使初生丝条在其中盐析12h。将20硫酸锌溶于180g丙酮溶剂中,得到凝固液C。将盐析的丝条牵伸3倍,然后置于凝固液C中盐析3h。然后,将二次盐析的海藻酸盐纤维经过水洗,再次牵伸1.2倍,再风干,即得抗菌导电海藻酸盐纤维。
实施例3
将0.8g海藻酸钠溶于14ml水,将0.2g聚乙烯醇溶于5ml水,再将它们混合均匀,得到混合溶液A。将20g氯化钙和6g丙三醇溶于174g甲醇中,得到凝固液B,再将凝固液B置于10℃冷藏。将溶液A通过5mm喷嘴注入凝固液B中,使初生丝条在其中盐析16h。将10氯化锌溶于190g丙酮溶剂中,得到凝固液C。将盐析的丝条牵伸2倍,然后置于凝固液C中盐析6h。然后,将二次盐析的海藻酸盐纤维经过水洗,再次牵伸2倍,再风干,即得抗菌导电海藻酸盐纤维。
实施例4
将1g海藻酸钠溶于14.8ml水,将0.2g聚乙烯醇溶于4ml水,再将它们混合均匀,得到混合溶液A。将10g高氯酸钙和6g丙三醇溶于184g乙醇中,得到凝固液B,再将凝固液B置于4℃冷藏。将溶液A通过3mm喷嘴注入凝固液B中,使初生丝条在其中盐析20h。将20硫酸锌溶于180g丙酮溶剂中,得到凝固液C。将盐析的丝条牵伸3倍,然后置于凝固液C中盐析2h。然后,将二次盐析的海藻酸盐纤维经过水洗,再次牵伸1.5倍,再风干,即得抗菌导电海藻酸盐纤维。
实施例1-4的海藻酸盐纤维的线密度和断裂强度的测试结果见表1。可以看出,海藻酸盐纤维具有良好的断裂强度和断裂伸长率,适合应用于手术缝合线、人工韧带和柔性传感器方面。
表1 海藻酸盐纤维的各项性能指标
Claims (7)
1.一种抗菌导电海藻酸盐纤维的制备方法,包括如下步骤:
S1.分别将海藻酸钠和聚乙烯醇溶解混合,得到混合溶液A;
S2.将钙盐溶于低级醇和低级多元醇的混合溶剂中得到凝固液B,并将凝固液B的温度控制在0~4℃,所述钙盐为氯化钙、硝酸钙、磷酸二氢钙、乳酸钙、甲酸钙、高氯酸钙中的任意一种,所述低级多元醇为乙二醇、丙三醇、丁二醇、三乙醇胺中的任意一种,所述低级醇为甲醇、乙醇、异丙醇中的任意一种;
S3.将S1所得的溶液A注入0~4℃冷藏的凝固液B中浸渍盐析12~24h,得到凝胶化纤维;
S4.将S3所得凝胶化纤维牵伸,并浸入含锌盐的丙酮溶剂C中二次盐析,所述锌盐为氯化锌、硫酸锌、硝酸锌、乙酸锌中的任意一种;
S5.将S4所得纤维水洗,再次牵伸,干燥,即得抗菌导电海藻酸盐纤维,所述抗菌导电海藻酸盐纤维具有高强的机械性能,应用于手术缝合线、人工韧带和柔性传感器。
2. 根据权利要求1所述的一种抗菌导电海藻酸盐纤维的制备方法,其特征在于,S1所述溶液A中海藻酸钠的浓度3~5 wt%,聚乙烯醇的浓度0.1~2 wt%。
3. 根据权利要求1所述的一种抗菌导电海藻酸盐纤维的制备方法,其特征在于,S2所述凝固液B中钙盐的浓度5~20 wt%,所述低级多元醇的浓度为1~3 wt%,其余为低级醇。
4. 根据权利要求1所述的一种抗菌导电海藻酸盐纤维的制备方法,其特征在于,S3所述溶液A注射直径为2~5 mm。
5.根据权利要求1所述的一种抗菌导电海藻酸盐纤维的制备方法,其特征在于,S4所述纤维牵伸倍数为1.5~3倍。
6. 根据权利要求1所述的一种抗菌导电海藻酸盐纤维的制备方法,其特征在于,S4所述锌盐的浓度为5~10 wt%,纤维在溶剂C中浸渍盐析时间1~6h。
7.根据权利要求1所述的一种抗菌导电海藻酸盐纤维的制备方法,其特征在于,S5中纤维牵伸倍数为1.2~2倍。
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