CN110172818A - 一种无纺布等离子体接枝壳寡糖衍生物的表面抗菌改性方法 - Google Patents

一种无纺布等离子体接枝壳寡糖衍生物的表面抗菌改性方法 Download PDF

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CN110172818A
CN110172818A CN201910368226.XA CN201910368226A CN110172818A CN 110172818 A CN110172818 A CN 110172818A CN 201910368226 A CN201910368226 A CN 201910368226A CN 110172818 A CN110172818 A CN 110172818A
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chitosan oligosaccharide
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吴鹏
刘源森
徐长安
唐旭
林凌
刘维维
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Third Institute of Oceanography MNR
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Abstract

本发明涉及一种无纺布等离子体接枝壳寡糖及其衍生物的表面抗菌改性的方法，采用壳寡糖及其衍生物作为无纺布的表面接枝材料，将无纺布通过常压空气介质阻挡放电等离子体表面改性，然后以共价键结合壳寡糖及其衍生物。

Description

一种无纺布等离子体接枝壳寡糖衍生物的表面抗菌改性方法
技术领域
本发明属于一种无纺布等离子体接枝壳寡糖衍生物的表面抗菌改性的方法，属于特种纤维制备的技术领域。
背景技术
壳聚糖(Chitosan)是由氨基葡萄糖和N-乙酰氨基葡萄糖通过β-1,4-糖苷键连接而成的，含量仅次于纤维素的第二大天然生物多糖。壳聚糖具有生物无毒性、可自然降解性、生物相容性好等特点，此外，壳聚糖还呈现出了一定的抗菌活性，已有大量研究证实，壳聚糖能够抑制多种微生物的生长繁殖。壳寡糖(Chitooligosaccharide)是壳聚糖主链经物理、化学或酶降解断裂后得到的聚合度为2-10的低分子量碱性氨基寡糖。壳寡糖除了具有壳聚糖所具有的优良生理性质之外，与壳聚糖相比较，其水溶性更好，功能作用范围更广，生物活性更高。
高分子纤维无纺布在许多领域有广泛应用，通过改性赋予抗菌性能，可以进一步拓展其用途。通常抗菌纤维可以通过抗菌剂与高分子聚合物共混纺丝制备得到。但是抗菌剂与聚合物共混纺丝时，成纤条件以及抗菌剂在纤维中的分布相对比较难控制。共混纺丝得到的纤维内部的抗菌剂不能与细菌接触，大量的抗菌剂起不到抗菌作用，抗菌剂的利用效率低。另外，无机抗菌剂(银、铜、锌等金属)用于纤维还存在抗菌剂迁移等问题，一方面抗菌效果不能保持良好的持久性，另一方面，无机抗菌剂的溶出容易对环境造成二次污染。
发明内容
本发明主要解决的技术问题是提供一种无纺布等离子体接枝壳寡糖衍生物的表面抗菌改性的方法。
本发明的技术方案如下：
(1)将无纺布置于等离子体装置上，开放环境下将等离子体喷射到无纺布表面，使无纺布在等离子体氛围中运动，电极间距离为1～3mm，处理功率为10～100KJ/m2，频率为20～50KHz，处理时间为5～30s，产生表面改性；
(2)将经等离子处理的无纺布通过滚轮输送至壳寡糖及其衍生物接枝液中，然后通过挤出滚轮去除未接枝的壳寡糖及其衍生物，挤出压力设置在1～5bar。然后将接枝好的无纺布在40～60℃下真空干燥至恒重。
所述壳寡糖衍生物的制备步骤为：
1)氯曲酸合成：曲酸与亚硫酰氯在冰浴反应下生成氯曲酸；
2)将1-2mol的氯曲酸溶解在1mol的壳寡糖水溶液里，在25-35℃下边搅拌边反应3-5h后冷却至室温；
3)加入20mL丙酮进入混合溶液里终止反应，生成棕色沉淀，然后过滤分离产品；
(4)乙醇索氏提取法脱除多余丙酮，12h；
(5)最后，用再生纤维素膜在蒸馏水内透析24h，干燥得到真空纯化的壳寡糖-氯曲酸衍生物。
所述等离子体发生器中的等离子源包括选择以下至少一种源：介质阻挡放电DBD等离子源、表面放电SD等离子源、等离子炬源、电弧等离子炬、滑动电弧等离子管等离子源、螺旋共振器等离子源、微波等离子源或大气压等离子体喷射APPJ源。
所述离子源中的等离子体选自He、Ar、Ne、Xe、空气、N2、O2、H2O或CO2。
所述无纺布为聚烯烃、聚卤代烯烃、聚硅氧烷、聚醚、聚酰胺、聚酯、聚碳酸酯、聚氨酯、环氧树脂、聚丙烯腈、聚丙烯酸类高分子、聚苯醚、聚酸酐、聚-α-氨基酸、聚苯硫醚、聚醚砜中的一种或是其中两种或多种的共混物；或是可降解高分子聚-L-乳酸、聚-(D,L)-乳酸、聚羟基丁酸、聚己内酯、聚丁内酯、聚戊内酯、聚酯二氧杂环己烷中的一种或者是至少以下两种单体的共聚物：L-乳酸、D,L-乳酸、羟基乙酸、3-羟基丁酸、3-羟基戊酸、己内酯、丁内酯、戊内酯、或是其中两种或多种的混纺无纺布。
本发明与现有抗菌改性技术相比，具有如下优点：
(1)壳寡糖衍生物抗菌剂具有不挥发，化学稳定性好，安全性高等优点。壳寡糖衍生物抗菌改性的无纺布抗菌性能优异，在高效过滤材料、生物医学材料、防护材料等领域有广泛的应用前景。
(2)采用等离子体接枝聚合、短时间照射，将壳寡糖衍生物分子以共价键键合到无纺布纤维表面，抗菌基团的密度大，抗菌剂的利用效率高，抗菌性能大大提高，对金色葡萄球菌和大肠杆菌的抑菌效果可达99％。
(3)无纺布纤维表面改性所用设备投资费用低，发明成本低、操作简单、适用性强、处理效果好、质量可靠等优点。大量缩短改性时间，降低化学品用量和产品成本，减少环境污染，适用于工业化生产。
具体实施方式：
现结合实施例对本发明作进一步描述：
壳寡糖衍生物的制备步骤为：
(1)氯曲酸合成：曲酸与亚硫酰氯在冰浴反应下生成氯曲酸；
(2)将1-2mol的氯曲酸溶解在1mol的壳寡糖水溶液里，在25-35℃下边搅拌边反应3-5h后冷却至室温；
(3)加入20mL丙酮进入混合溶液里终止反应，生成棕色沉淀，然后过滤分离产品；
(4)乙醇索氏提取法脱除多余丙酮；
(5)用再生纤维素膜在蒸馏水内透析24h，干燥得到真空纯化的壳寡糖-氯曲酸衍生物。
实施例1
(1)将无纺布置于等离子处理仪上，开放环境下将等离子体喷射到无纺布表面，使无纺布在等离子体氛围中运动，电极间距离为1mm，处理功率为25KJ/m2，频率为20KHz，处理时间为5s，产生表面改性；
(2)将经等离子处理的无纺布通过滚轮输送至2g/L的质量分数1.5％的壳寡糖衍生物接枝水溶液中，然后通过挤出滚轮去除未接枝的壳寡糖及其衍生物，挤出压力设置在2bar。然后将接枝好的无纺布在40℃下真空干燥至恒重。
(3)用大肠杆菌(肠道菌代表)、金黄色葡萄球菌(化脓菌代表)同时进行振荡烧瓶试验。不加样片组活菌计数1×105CFU/mL，且样本振荡前后平均菌落数差值为4.3％(＜10％)，试验有效。用平板计数法对剩余活菌数量进行统计，记为VS，处理前的记为VC。根据处理前后的差值，计算抑菌率(％)＝(VC-VS)/Vc×100％。试验组与对照组的大肠杆菌抑菌率差值为35.3％(＞26％)，金色葡萄球菌的抑菌率差值为43.5％(＞26％)，说明壳寡糖衍生物改性无纺布对大肠杆菌和金色葡萄球菌有抑菌作用。
实施例2
(1)将无纺布置于等离子体装置上，开放环境下将等离子体喷射到无纺布表面，使无纺布在等离子体氛围中运动，电极间距离为1.5mm，处理功率为45KJ/m2，频率为26KHz，处理时间为10s，产生表面改性；
(2)将经等离子处理的无纺布通过滚轮输送至3g/L的壳寡糖及其衍生物接枝液中，然后通过挤出滚轮去除未接枝的壳寡糖及其衍生物，挤出压力设置在3bar。然后将接枝好的无纺布在50℃下真空干燥至恒重。
(3)用大肠杆菌(肠道菌代表)、金黄色葡萄球菌(化脓菌代表)同时进行振荡烧瓶试验。不加样片组活菌计数1×105CFU/mL，且样本振荡前后平均菌落数差值为4.3％(＜10％)，试验有效。用平板计数法对剩余活菌数量进行统计，记为VS，处理前的记为VC。根据处理前后的差值，计算抑菌率(％)＝(VC-VS)/Vc×100％。试验组与对照组的大肠杆菌抑菌率差值为45.3％(＞26％)，金色葡萄球菌的抑菌率差值为63.5％(＞26％)，说明壳寡糖衍生物改性无纺布对大肠杆菌和金色葡萄球菌有抑菌作用。
实施例3
(1)将无纺布置于等离子体装置上，开放环境下将等离子体喷射到无纺布表面，使无纺布在等离子体氛围中运动，电极间距离为2mm，处理功率为55KJ/m2，频率为30KHz，处理时间为15s，产生表面改性；
(2)将经等离子处理的无纺布通过滚轮输送至3g/L的壳寡糖及其衍生物接枝液中，然后通过挤出滚轮去除未接枝的壳寡糖及其衍生物，挤出压力设置在4bar。然后将接枝好的无纺布在60℃下真空干燥至恒重。
(3)用大肠杆菌(肠道菌代表)、金黄色葡萄球菌(化脓菌代表)同时进行振荡烧瓶试验。不加样片组活菌计数1×105CFU/mL，且样本振荡前后平均菌落数差值为4.3％(＜10％)，试验有效。用平板计数法对剩余活菌数量进行统计，记为VS，处理前的记为VC。根据处理前后的差值，计算抑菌率(％)＝(VC-VS)/Vc×100％。试验组与对照组的大肠杆菌抑菌率差值为38.5％(＞26％)，金色葡萄球菌的抑菌率差值为51.2％(＞26％)，说明壳寡糖衍生物改性无纺布对大肠杆菌和金色葡萄球菌抑制效果显著。

Claims (5)

1.一种无纺布等离子体接枝壳寡糖衍生物表面抗菌改性方法，其特征在于步骤如下：
将无纺布置于等离子体装置上，开放环境下将等离子体喷射到无纺布表面，使无纺布在等离子体氛围中运动，电极间距离为1～3mm，处理功率为10～100KJ/m2，频率为20～50KHz，处理时间为5～30s，产生表面改性；
将经等离子处理的无纺布通过滚轮输送至壳寡糖衍生物接枝液中，然后通过挤出滚轮去除未接枝的壳寡糖衍生物，挤出压力设置在1～5bar，然后将接枝好的无纺布在40～60℃下真空干燥至恒重。
2.根据权利要求1所述无纺布等离子体接枝壳寡糖衍生物表面抗菌改性方法，其特征在于所述等离子体装置的等离子源为介质阻挡放电DBD等离子源、表面放电SD等离子源、等离子炬源、电弧等离子炬、滑动电弧等离子管等离子源、螺旋共振器等离子源、微波等离子源或大气压等离子体喷射APPJ源。
3.根据权利要求2所述无纺布等离子体接枝壳寡糖及其衍生物的表面抗菌改性的方法，其特在于所述等离子源中的等离子体选自He、Ar、Ne、Xe、空气、N2、O2、H2O或CO2。
4.根据权利要求1所述无纺布等离子体接枝壳寡糖衍生物表面抗菌改性方法，其特在于所述无纺布为聚烯烃、聚卤代烯烃、聚硅氧烷、聚醚、聚酰胺、聚酯、聚碳酸酯、聚氨酯、环氧树脂、聚丙烯腈、聚丙烯酸类高分子、聚苯醚、聚酸酐、聚-α-氨基酸、聚苯硫醚、聚醚砜中的一种或是其中两种或多种的共混物；或是可降解高分子聚-L-乳酸、聚-(D,L)-乳酸、聚羟基丁酸、聚己内酯、聚丁内酯、聚戊内酯、聚酯二氧杂环己烷中的一种或者是至少以下两种单体的共聚物：L-乳酸、D,L-乳酸、羟基乙酸、3-羟基丁酸、3-羟基戊酸、己内酯、丁内酯、戊内酯、或是其中两种或多种的混纺无纺布。
5.根据权利要求1所述无纺布等离子体接枝壳寡糖衍生物表面抗菌改性方法，其特征在于壳寡糖衍生物的制备步骤为：
（1）氯曲酸合成：曲酸与亚硫酰氯在冰浴反应下生成氯曲酸；
（2）将1-2mol的氯曲酸溶解在1mol的壳寡糖水溶液里，在25-35℃下边搅拌边反应3-5h后冷却至室温；
（3）加入20mL丙酮进入混合溶液里终止反应，生成棕色沉淀，然后过滤分离产品；
（4）乙醇索氏提取法脱除多余丙酮；
（5）用再生纤维素膜在蒸馏水内透析24h，干燥得到真空纯化的壳寡糖-氯曲酸衍生物。
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