CN109295704A - 一种载银粘胶纤维制备方法及其应用 - Google Patents

一种载银粘胶纤维制备方法及其应用 Download PDF

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CN109295704A
CN109295704A CN201810992244.0A CN201810992244A CN109295704A CN 109295704 A CN109295704 A CN 109295704A CN 201810992244 A CN201810992244 A CN 201810992244A CN 109295704 A CN109295704 A CN 109295704A
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朱云峰
冯浪
管超
杨菁菁
朱圣清
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Abstract

本发明提供一种具有抗菌性能的载银粘胶纤维制备方法包括三个步骤，(1)粘胶纤维的前处理：将粘胶纤维浸入去离子水中并超声浸洗30min,拧干后在乙醇溶液中超声浸洗20‑30min，拧干,干燥。(2)纳米银溶胶的制备：取制备的晶种,去离子水,硝酸银溶液,浓度为4‑12mM的抗坏血酸反应制备纳米银溶胶。(3)载银粘胶纤维的制备：粘胶纤维和纳米银溶胶的质量(g)体积(mL)比为1:(20‑80)，将粘胶纤维浸泡在制备的纳米银溶胶中4‑7天捞出，拧干，然后将样品置于真空干燥箱内以100℃的温度烘干，得到具有抗菌性能的粘胶纤维。

Description

一种载银粘胶纤维制备方法及其应用
技术领域
本发明属于材料领域，具体涉及一种载银粘胶纤维制备方法及其应用材料。
背景技术
粘胶纤维是从天然的棉短绒、植物秸秆等富含纤维素的原材料中提取出纤维素，再经过化学加工而得到的纤维素纤维。粘胶纤维与多数天然纤维拥有相似的性能，具有优良的生物相容性和吸附性，所以其表面常常被大量微生物附着，同时吸附了大量的水分和其他物质后为各种微生物生长提供了有利的条件，因此限制了它的应用。金属银具有很优异的抗菌性能，当银粒子处于纳米尺寸时，其抗菌性能将大大提高。
发明内容
本发明提供一种载银粘胶纤维制备方法，该方法包括以下步骤：(1)粘胶纤维的前处理：将粘胶纤维浸入去离子水中浸洗20-30min,拧干后，放入乙醇溶液中浸洗20-30min，拧干,烘干，得烘干粘胶纤维；(2)纳米银溶胶的制备：用浓度为6-14mM的硼氢化钠溶液1mL，1-7mM的壳聚糖溶液3mL，0.75-1.75mM硝酸银溶液10mL，高速搅拌反应制备纳米银晶种，然后取制备的纳米银晶种、去离子水、硝酸银溶液、浓度为4-12mM的抗坏血酸反应制备纳米银溶胶；
(3)载银粘胶纤维的制备：将粘胶纤维和纳米银溶胶按照质量体积比为1g:(20-80)mL的比例取各原料，然后将粘胶纤维浸泡在制备的纳米银溶胶中4-7天捞出，拧干，烘干，得到具有抗菌性能的黏胶纤维。
优选的本发明步骤(1)所述的浸洗为超声浸洗。
优选的本发明步骤(1)所述的烘干温度为100℃。
优选的本发明步骤(2)所述的纳米银溶胶的为：在反应温度为20-80℃，搅拌速度为200-600r/min的条件下，先后分别加入浓度为6-14mM的硼氢化钠溶液1mL，1-7mM的壳聚糖溶液3mL，0.75-1.75mM硝酸银溶液10mL，高速搅拌反应20min制备纳米银晶种，取制备的纳米银晶种2mL,去离子水10mL,硝酸银溶液30mL,浓度为10mM的抗坏血酸0.5mL反应制备纳米银溶胶。
优选的本发明步骤(2)所述的纳米银溶胶的为：在反应温度为20℃，搅拌速度为400r/min的条件下，先后分别加入浓度为10mM的硼氢化钠溶液1mL，2.5mM的壳聚糖溶液3mL，1.25mM硝酸银溶液10mL，高速搅拌反应20min制备纳米银晶种。
优选的本发明步骤(3)所述的载银粘胶纤维的制备为：将粘胶纤维和纳米银溶胶按照质量体积比为1g:40mL的比例取各原料，将粘胶纤维浸泡在制备的纳米银溶胶中7天捞出，拧干，烘干，得到具有抗菌性能的黏胶纤维。
优选的本发明步骤(3)所述的烘干为置于真空干燥箱内100℃烘干。
优选的本发明所述的壳聚糖作为反应的保护剂和还原剂。
优选的本发明所述纳米银的制备过程中的硝酸银溶液的加入方式可以用恒压滴液漏斗滴加，也可以用滴管缓慢加入。
优选的本发明所述的粘胶纤维是从富含纤维素的原材料中提取出纤维素，再经过化学加工而得到的纤维素纤维，所述富含纤维素的原材料为天然的棉短绒或植物秸秆。
本发明所述的载银粘胶纤维制备方法制备的粘胶纤维在医用敷料中的应用。
本专利首先采用化学还原法制备一定粒径的纳米银溶胶，然后将粘胶纤维浸泡在制备的纳米银溶胶中制备载银粘胶纤维。与其他方法相比，其优越性在于:(1)通过改变相应的实验参数可以控制纳米银的颗粒大小，制备的纳米银颗粒粒径比较均匀，稳定性较好。(2)通过控制浴比可以使溶胶中的纳米银颗粒被完全吸附到粘胶纤维上，使得资源被充分的利用并且满足清洁生产；(3)纳米银颗粒和粘胶纤维之间形成了配位键使得纳米银吸附更加牢固，不易脱落；(4)本方法采用壳聚糖作为保护剂，壳聚糖本身就具备抗菌效果并且是无毒，使制备的纳米颗粒的稳定性很好，不易团聚，保证了纳米颗粒粒径的均一；(5)壳聚糖是无毒的生化试剂且本身具备一定的灭菌性能，将其用作制备纳米银可加强材料的灭菌性能；(6)本方法制备载银粘胶纤维分为纳米银溶胶的制备和粘胶纤维的浸泡吸附两个部分，实验流程简单，易于操作，设备简单，制备周期短。
附图说明
图1：为实施例1的紫外光谱图。
图2：为实施例1的透射电镜图及其粒径分布情况。
图3：为实施例1载银粘胶纤维的扫描电镜图片。
具体实施方式
下面通过实施例对本发明进行具体描述，有必要在此指出的是本实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，该领域的技术熟练人员可以根据上述发明的内容做出一些非本质的改进和调整。
实施例1：粘胶纤维制备
(1)粘胶纤维的前处理：将粘胶纤维用去离子水中超声浸洗20-30min,然后将粘胶纤维拧干后用相同的方法在乙醇溶液中超声浸洗30min拧干,然后在100℃的条件下烘干待用。
(2)纳米银溶胶的制备：在反应温度为20℃下，搅拌速度为400r/min的条件下先后分别加入浓度为10mM的硼氢化钠溶液1mL，2.5mM的壳聚糖溶液3mL，1.25mM硝酸银溶液10mL，高速搅拌反应20min制备晶种。然后取制备的晶种2mL,去离子水10mL,硝酸银溶液30mL,浓度为10mM的抗坏血酸0.5mL反应制备纳米银溶胶。
(3)载银粘胶纤维的制备：将粘胶纤维和纳米银溶胶按照质量体积比为1g:40mL的比例取各原料，将粘胶纤维浸泡在制备的纳米银溶胶中7天捞出，拧干，然后将样品置于真空干燥箱内以100℃的温度烘干，得到具有抗菌性能的粘胶纤维。
实施例2：粘胶纤维制备
(1)粘胶纤维的前处理：将粘胶纤维用去离子水中超声浸洗30min,然后将粘胶纤维拧干后用相同的方法在乙醇溶液中超声浸洗30min拧干,然后在100℃的条件下烘干待用。
(2)纳米银溶胶的制备：在反应温度为20℃下，搅拌速度为400r/min的条件下先后分别加入浓度为14mM的硼氢化钠溶液1mL，2.5mM的壳聚糖溶液3mL，1.25mM硝酸银溶液10mL，高速搅拌反应20min制备晶种。然后取制备的晶种2mL,去离子水10mL,硝酸银溶液30mL,浓度为10mM的抗坏血酸0.05mL反应制备纳米银溶胶。
(3)载银粘胶纤维的制备：将粘胶纤维和纳米银溶胶按照质量体积比为1g:40mL的比例取各原料，将粘胶纤维浸泡在制备的纳米银溶胶中7天捞出，拧干，然后将样品置于真空干燥箱内以100℃的温度烘干，得到具有抗菌性能的粘胶纤维。
实施例3：粘胶纤维制备
(1)粘胶纤维的前处理：将粘胶纤维用去离子水中超声浸洗30min,然后将粘胶纤维拧干后用相同的方法在乙醇溶液中超声浸洗30min拧干,然后在100℃的条件下烘干待用。
(2)纳米银溶胶的制备：在反应温度为20℃下，搅拌速度为400r/min的条件下先后分别加入浓度为10mM的硼氢化钠溶液1mL，2.5mM的壳聚糖溶液3mL，1.25mM硝酸银溶液10mL，高速搅拌反应20min制备晶种。然后取制备的晶种2mL,去离子水10mL,硝酸银溶液30mL,浓度为10mM的抗坏血酸0.5mL反应制备纳米银溶胶；
(3)载银粘胶纤维的制备：将粘胶纤维和纳米银溶胶按照质量体积比为1g:40mL的比例取各原料，将粘胶纤维浸泡在制备的纳米银溶胶中7天捞出，拧干，然后将样品置于真空干燥箱内以100℃的温度烘干，得到具有抗菌性能的粘胶纤维。
试验例：对实施例1-3制备的样品进行性能测试，具体结果见表1
表1：实施例1-3制备的载银粘胶纤维的载银量和抗菌性能
实施例1-3所制备的载银粘胶纤维载银量较高，分别为1395mg/kg、1507mg/kg和1898mg/kg，较高的载银量进一步保证了载银活性炭纤维的抗菌性能，实施例1-3所制备的载银活性炭纤维对白色念珠菌、金黄色葡萄球菌和大肠杆菌的24小时抗菌率菌达到99％以上，具有较好的抗菌性能。

Claims (10)

1.一种载银粘胶纤维制备方法，其特征在于，该方法包括以下步骤：
(1)粘胶纤维的前处理：将粘胶纤维浸入去离子水中浸洗20-30min,拧干后，放入乙醇溶液中浸洗20-30min，拧干,烘干，得烘干粘胶纤维；
(2)纳米银溶胶的制备：用浓度为6-14mM的硼氢化钠溶液1mL，1-7mM的壳聚糖溶液3mL，0.75-1.75mM硝酸银溶液10mL，高速搅拌反应制备纳米银晶种，然后取制备的纳米银晶种、去离子水、硝酸银溶液、浓度为4-12mM的抗坏血酸反应制备纳米银溶胶；
(3)载银粘胶纤维的制备：将粘胶纤维和纳米银溶胶按照质量体积比为1g:(20-80)mL的比例取各原料，然后将粘胶纤维浸泡在制备的纳米银溶胶中4-7天捞出，拧干，烘干，得到具有抗菌性能的黏胶纤维。
2.根据权利要求1所述的载银粘胶纤维制备方法，其特征在于，步骤(1)所述的浸洗为超声浸洗。
3.根据权利要求1所述的载银粘胶纤维制备方法，其特征在于，步骤(1)所述的烘干温度为100℃。
4.根据权利要求1所述的载银粘胶纤维制备方法，其特征在于，步骤(2)所述的纳米银溶胶为：在反应温度为20-80℃，搅拌速度为200-600r/min的条件下，先后分别加入浓度为6-14mM的硼氢化钠溶液1mL，1-7mM的壳聚糖溶液3mL，0.75-1.75mM硝酸银溶液10mL，高速搅拌反应20min制备纳米银晶种，取制备的纳米银晶种2mL,去离子水10mL,硝酸银溶液30mL,浓度为10mM的抗坏血酸0.5mL反应制备纳米银溶胶。
5.根据权利要求4所述的载银粘胶纤维制备方法，其特征在于，步骤(2)所述的纳米银溶胶的为：在反应温度为20℃，搅拌速度为400r/min的条件下，先后分别加入浓度为10mM的硼氢化钠溶液1mL，2.5mM的壳聚糖溶液3mL，1.25mM硝酸银溶液10mL，高速搅拌反应20min制备纳米银晶种。
6.根据权利要求1所述的载银粘胶纤维制备方法，其特征在于，步骤(3)所述的载银粘胶纤维的制备为：将粘胶纤维和纳米银溶胶按照质量体积比为1g:40mL的比例取各原料，将粘胶纤维浸泡在制备的纳米银溶胶中7天捞出，拧干，烘干，得到具有抗菌性能的黏胶纤维。
7.根据权利要求1所述的载银粘胶纤维制备方法，其特征在于，步骤(3)所述的烘干为置于真空干燥箱内100℃烘干。
8.根据权利要求1-7任一项所述的载银粘胶纤维制备方法，其特征在于，所述的粘胶纤维是从富含纤维素的原材料中提取出纤维素，再经过化学加工而得到的纤维素纤维。
9.根据权利要求8所述的载银粘胶纤维制备方法，其特征在于，所述富含纤维素的原材料为天然的棉短绒或植物秸秆。
10.根据权利要求1-7任一项所述的载银粘胶纤维制备方法制备的粘胶纤维在医用敷料中的应用。
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