CN109529093A - 一种用于创口灭菌止血的海藻酸纤维及其制备方法 - Google Patents

一种用于创口灭菌止血的海藻酸纤维及其制备方法 Download PDF

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CN109529093A
CN109529093A CN201811267852.1A CN201811267852A CN109529093A CN 109529093 A CN109529093 A CN 109529093A CN 201811267852 A CN201811267852 A CN 201811267852A CN 109529093 A CN109529093 A CN 109529093A
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alginic acid
essential oil
acid fibre
wormwood essential
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辛斌杰
袁蓉
王蕾
李庭晓
刘岩
郑元生
陈卓明
许颖琦
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Shanghai University of Engineering Science
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Abstract

本发明公开了一种用于创口灭菌止血的海藻酸纤维及其制备方法,旨在提高海藻酸纤维抗菌、止血、止痛的效果,其技术方案要点是:一种用于创口灭菌止血的海藻酸纤维,包括海藻酸纤维,其特征在于,所述海藻酸纤维内设置有若干银离子及艾草精油微胶囊。本发明达到有效提高海藻酸纤维抗菌、止血、止痛的效果。

Description

一种用于创口灭菌止血的海藻酸纤维及其制备方法
技术领域
该发明属于功能纺织品领域,特别是涉及一种用于创口灭菌止血的海藻酸纤维及其制备方法。
背景技术
随生物医学与材料科学等新兴学科的发展,,新材料与药物结合成为21世纪研究热点。由于各学科的相互交叉,将药物材料与纺织纤维相结合制备具有优异的缓释保健医疗性能的功能纺织品已成为纺织材料领域研究热潮。
艾草,又名灸草,菊科蒿属植物。全草入药,有温经止血、散寒止痛、抗过敏、抗菌消炎等作用,艾叶是艾草发挥效用的部分,艾叶油,即艾草精油,其中含有能够止血、镇痛作用的苦艾醇、苦艾酮。然而精油具有易挥发,有效时间短的缺点,现利用复凝聚法将艾草精油作为芯材包覆于由阿拉伯树胶与明胶制成的囊材中,实现缓慢释放精油的作用。
海藻酸纤维是一种天然生物高分子材料,资源丰富,具有快速凝胶性能和优良的生物相容性及生物降解性,被广泛用于药物缓释、医用敷料、组织工程支架等领域。
因此需要提出一种新的方案来将艾草精油添加到海藻酸纤维中以提高海藻酸纤维抗菌、止痛、止血的性能。
发明内容
针对上述问题,本发明的目的是提供一种用于创口灭菌止血的海藻酸纤维及其制备方法,达到有效提高海藻酸纤维抗菌、止血、止痛的效果。
本发明的上述技术目的是通过以下技术方案得以实现的:一种用于创口灭菌止血的海藻酸纤维,包括海藻酸纤维,其特征在于,所述海藻酸纤维内设置有若干银离子及艾草精油微胶囊,所述艾草精油微胶囊内存有艾草精油。
进一步,所述艾草精油微胶囊粒径为500~2000nm。
进一步,一种用于创口灭菌止血的海藻酸纤维的制备方法,其特征在于,包括如下步骤:
步骤1、阿拉伯树胶与明胶溶解于去离子水中,滴加艾草精油与分散剂进行乳化;
步骤2、将乳化后的溶液用醋酸溶液调节PH=3-4,进行复凝聚过程,使囊材包覆于精油表面;
步骤3、复凝聚后的溶液降温置于冷冻搅拌机搅拌,使氢氧化钠溶液调节PH=9-10,进行低温碱化,将溶液回复室温加入体积比为10ml/l的25%戊二醛并搅拌,再加入单宁酸搅拌,然后进行冷冻干燥,从而得到艾草精油微胶囊粉末;
步骤4、将海藻碾碎、水洗、除杂、强碱水萃取,澄清后得粗海藻酸盐溶液,经氯化钙沉淀得带色的海藻酸纤维,经脱色、脱味处理后用酸处理,除去可溶性杂质得海藻酸纤维沉淀,然后与碳酸钠作用得海藻酸钠,经干燥、粉碎、过筛,制得海藻酸钠粉末;
步骤5、通过海藻酸纤维制备海藻酸钠纺丝溶液,并在海藻酸钠纺丝溶液中加入水溶性磺胺嘧啶钠与艾草精油微胶囊,经喷丝孔后进入含硝酸银的2%氯化钙的凝固浴,发生离子交换将水溶性的海藻酸钠转换成不溶于水的海藻酸纤维,硝酸银与磺胺嘧啶钠反应后在海藻酸纤维内形成银离子颗粒。
进一步,步骤1中,阿拉伯树胶与明胶在去离子水中质量分数为0.9%-1.1%,艾草精油质量分数2.8%-3.2%,分散剂质量分数0.9%-1.1%,搅拌速率为8000转/分钟,搅拌时间为30分钟。
进一步,步骤2中,所述醋酸溶液浓度为10wt%,搅拌速率为3000~4000转/分钟,搅拌时间为30分钟。
进一步,步骤3中,复凝聚后的溶液逐渐降温至0~5℃,温度达到后用10%氢氧化钠溶液调节至复凝聚后的溶液PH为9-10,并且在温度保持5℃以下,搅拌转速为2000-3000转/分钟,搅拌时间为20分钟。
进一步,步骤3中,搅拌时间为30分钟;移到40℃恒温水浴锅中,搅拌时间3h;再加入单宁酸用量比例为10g/l,搅拌时间为4.5h。将固化后的体系在转速为5000转/分钟条件下离心10min,冷冻干燥得到艾草精油微胶囊粉末。
进一步,步骤5中,海藻酸钠溶液浓度10%-12%,海藻酸钠溶液中艾草精油微胶囊浓度为1wt%,纺丝温度75℃,凝固浴浓度6wt%,拉伸倍数为1.5。
与现有技术相比,本发明具有以下优势:
1)本发明通过高浓度海藻酸钠溶液进行湿法纺丝,提升低浓度海藻酸钠纺丝得到的纤维的强力;
2)本发明采用微胶囊化技术对艾草精油进行处理,使精油被包裹于囊材中,形成微胶囊,有效延长精油扩散时间,增强缓释性能;充分固化增强艾草精油微胶囊物理性能;
3)采用微胶囊化技术对艾草精油进行处理,使精油被包裹于囊材中,形成微胶囊,有效延长精油扩散时间,增强缓释性能,充分固化增强艾草精油微胶囊物理性能;
4)本发明采用载银离子颗粒的海藻酸纤维包覆艾草精油微胶囊,增加缓释效果,同时银离子与艾草精油同时发挥作用,提升灭菌效果;
5)本发明采用海藻酸纤维内部包覆及在凝固浴反应形成银离子产物,使有效成分牢固度增加,提高耐水洗性,提升纤维质量,拓展其应用领域,增加商业价值。
附图说明
图1为实施例一的结构示意图;
图2为实施例二及实施例三的流程图。
图中:1、海藻酸纤维;2、银离子;3、艾草精油微胶囊。
具体实施方式
下面结合附图和实施例,对本发明进行详细描述。
实施例一:一种用于创口灭菌止血的海藻酸纤维,如图1所示,包括海藻酸纤维1,海藻酸纤维1内含有若干银离子2颗粒及艾草精油微胶囊3,艾草精油微胶囊3内存有艾草精油。其中海藻酸纤维1由海藻酸钠溶液经湿法纺丝工艺制得,银离子2颗粒分别以加入纺丝液及凝固浴的方式结合海藻酸纤维1,艾草精油微胶囊3由阿拉伯树胶为囊材,艾草精油为芯材以复凝聚法制得,并且制得的艾草精油微胶囊3粒径为500-2000nm,从而保证艾草精油微胶囊3表面积,有利于药物释放,并且较小的直径方便纺丝;然后将制得的艾草精油微胶囊3加入海藻酸钠纺丝液,从而加工成用于创口灭菌止血的海藻酸纤维。
在海藻酸纤维1内含有艾草微胶囊和银离子2颗粒,达到提高灭菌效果,同时通过艾草胶囊内的艾草精油达到温经止血、散寒止痛、抗过敏、抗菌消炎等作用;并且由于海藻酸纤维1包覆住艾草精油微胶囊3,艾草精油微胶囊3包覆艾草精油,可以达到增加缓释效果,增加艾草精油作用时间。
实施例二:一种用于实施例一所述的一种创口灭菌止血的海藻酸纤维1的制备方法。如图2所示,先进行艾草精油微胶囊3制备:首先将树胶阿拉伯胶与明胶按4%比例加热溶解于去离子水中,加入艾草精油及分散剂,然后进行搅拌,先以转速10000r/min搅拌20s,然后以转速2000r/min搅拌30min,之后用10%醋酸调节PH至3,用磁力搅拌机搅拌30min,转速2000r/min,将体系降温至1℃,加入10%氢氧化钠溶液至PH为9,冷冻搅拌机搅拌速率2000r/min,搅拌时间20min后,回复室温加入25%戊二醛搅拌3小时及单宁酸搅拌4小时,搅拌完毕后放入冷冻干燥机干燥12小时,从而制备完成艾草微胶囊,并且制备的艾草微胶囊粒径在为500-2000nm区间内。
然后制备海藻酸纤维1:首先将海藻碾碎、水洗、除杂、强碱水萃取,澄清后得粗海藻酸盐溶液,经氯化钙沉淀得带色的海藻酸纤维1,经脱色、脱味处理后用酸处理,除去可溶性杂质得海藻酸纤维1沉淀,然后与碳酸钠作用得海藻酸钠,经干燥、粉碎、过筛,制得海藻酸钠粉末。
然后通过海藻酸钠粉末制备质量分数为11%的海藻酸钠纺丝溶液,将艾草精油微胶囊3与磺胺嘧啶钠分别按1wt%与2wt%的比例加入11wt%的海藻酸钠纺丝液中,在75℃的温度下,由湿法纺丝装置的喷丝孔喷出,进入45℃含硝酸银的2wt%氯化钙凝固浴,硝酸银量与纺丝液中磺胺嘧啶钠相同,4%的三氟甲磺酸钠为催化剂,凝固浴30min。从而制备完成海藻酸纤维1,并且在海藻酸纤维1,并且在海藻酸纤维1内包含有艾草精油微胶囊3和银离子2颗粒。
实施例二:一种用于实施例一所述的一种创口灭菌止血的海藻酸纤维1的制备方法。如图2所示,先进行艾草精油微胶囊3制备:首先将树胶阿拉伯胶与明胶按4%比例加热溶解于去离子水中,加入艾草精油及分散剂,进行搅拌,先以转速8000r/min搅拌30s,然后以转速4000r/min搅拌30min,再用10%醋酸调节PH至4,用磁力搅拌机搅拌30min,转速3000r/min,并将将体系降温至1℃,加入10%氢氧化钠溶液至PH为10,冷冻搅拌机搅拌速率3000r/min,搅拌时间30min后,回复室温加入25%戊二醛搅拌3小时及单宁酸搅拌4小时,搅拌完毕后放入冷冻干燥机干燥12小时,从而制备完成艾草微胶囊,并且制备的艾草微胶囊粒径在为500-2000nm区间内。
然后制备海藻酸纤维1:首先将海藻碾碎、水洗、除杂、强碱水萃取,澄清后得粗海藻酸盐溶液,经氯化钙沉淀得带色的海藻酸纤维1,经脱色、脱味处理后用酸处理,除去可溶性杂质得海藻酸纤维1沉淀,然后与碳酸钠作用得海藻酸钠,经干燥、粉碎、过筛,制得海藻酸钠粉末。
将艾草精油微胶囊3与磺胺嘧啶钠分别按1wt%与2wt%的比例加入11wt%的海藻酸钠纺丝液中,在75℃的温度下,由湿法纺丝装置的喷丝孔喷出,进入45℃含硝酸银的2wt%氯化钙凝固浴,硝酸银量与纺丝液中磺胺嘧啶钠相同,4%的三氟甲磺酸钠为催化剂,凝固浴30min。从而制备完成海藻酸纤维1,并且在海藻酸纤维1,并且在海藻酸纤维1内包含有艾草精油微胶囊3和银离子2颗粒。
以上所述仅是本发明的优选实施方式,本发明的保护范围并不仅局限于上述实施例,凡属于本发明思路下的技术方案均属于本发明的保护范围。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理前提下的若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。

Claims (8)

1.一种用于创口灭菌止血的海藻酸纤维,包括海藻酸纤维(1),其特征在于,所述海藻酸纤维(1)内设置有若干银离子颗粒(2)及艾草精油微胶囊(3),所述艾草精油微胶囊内存有艾草精油。
2.根据权利要求1所述的一种用于创口灭菌止血的海藻酸纤维,其特征在于,所述艾草精油微胶囊(3)粒径为500~2000nm。
3.一种用于创口灭菌止血的海藻酸纤维的制备方法,其特征在于,包括如下步骤:
步骤1、阿拉伯树胶与明胶溶解于去离子水中,滴加艾草精油与分散剂进行乳化;
步骤2、将乳化后的溶液用醋酸溶液调节PH=3-4,进行复凝聚过程,使囊材包覆于艾草精油表面;
步骤3、复凝聚后的溶液降温置于低温环境下并通过搅拌机搅拌,使氢氧化钠溶液调节PH=9-10,进行低温碱化,将溶液回复室温加入体积比为10ml/l的25%戊二醛并搅拌,再加入单宁酸搅拌,然后进行冷冻干燥,从而得到艾草精油微胶囊(3)粉末;
步骤4、将海藻碾碎、水洗、除杂、强碱水萃取,澄清后得粗海藻酸盐溶液,经氯化钙沉淀得带色的海藻酸纤维(1),经脱色、脱味处理后用酸处理,除去可溶性杂质得海藻酸纤维(1)沉淀,然后与碳酸钠作用得海藻酸钠,经干燥、粉碎、过筛,制得海藻酸钠粉末;
步骤5、通过海藻酸钠粉末制备海藻酸钠纺丝溶液,并在海藻酸钠纺丝溶液中加入水溶性磺胺嘧啶钠与艾草精油微胶囊(3),经喷丝孔后进入含硝酸银的2%氯化钙的凝固浴,发生离子交换将水溶性的海藻酸钠转换成不溶于水的海藻酸纤维(1),硝酸银与磺胺嘧啶钠反应后在海藻酸纤维内形成银离子颗粒(2)。
4.根据权利要求3所述的一种用于创口灭菌止血的海藻酸纤维的制备方法,其特征在于,步骤1中,阿拉伯树胶与明胶在去离子水中质量分数为0.9%-1.1%,艾草精油质量分数2.8%-3.2%,分散剂质量分数0.9%-1.1%,搅拌速率为8000转/分钟,搅拌时间为30分钟。
5.根据权利要求3所述的一种用于创口灭菌止血的海藻酸纤维的制备方法,其特征在于,步骤2中,所述醋酸溶液浓度为10wt%,搅拌速率为3000~4000转/分钟,搅拌时间为30分钟。
6.根据权利要求3所述的一种用于创口灭菌止血的海藻酸纤维的制备方法,其特征在于,步骤3中,复凝聚后的溶液逐渐降温至0~5℃,温度达到后用10%氢氧化钠溶液调节至复凝聚后的溶液PH为9-10,并且在温度保持5℃以下,搅拌转速为2000-3000转/分钟,搅拌时间为20分钟。
7.根据权利要求3所述的一种用于创口灭菌止血的海藻酸纤维的制备方法,其特征在于,步骤3中,搅拌时间为30分钟;移到40℃恒温水浴锅中,搅拌时间3h;再加入单宁酸用量比例为10g/l,搅拌时间为4.5h。将固化后的体系在转速为5000转/分钟条件下离心10min,冷冻干燥得到艾草精油微胶囊(3)粉末。
8.根据权利要求3所述的一种用于创口灭菌止血的海藻酸纤维的制备方法,其特征在于,步骤5中,海藻酸钠溶液浓度10%-12%,海藻酸钠溶液中艾草精油微胶囊(3)浓度为1wt%,纺丝温度75℃,凝固浴浓度6wt%,拉伸倍数为1.5。
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