CN115198525A - 一种基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法及应用 - Google Patents
一种基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法及应用 Download PDFInfo
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Abstract
本发明涉及一种基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法及应用,首先将棉织物浸渍在甜菜碱和金属盐溶液中,再经等离子体处理得到甜菜碱和纳米金属粒子双重抗菌棉织物。等离子体可以引发双键甜菜碱在棉织物表面接枝聚合,形成致密的抗菌薄膜;还可以从金属盐中还原纳米金属粒子并负载在棉织物上,纳米金属粒子与棉织物结合紧密,不易分离。该法操作简单,反应迅速,同时无需使用任何有机溶剂,复合绿色环保的理念,制备得到的双重抗菌棉织物抗菌性能优异,同时具有较好的防紫外线性能。
Description
本发明涉及一种基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法及应用,属于纺织加工技术领域。
背景技术
棉织物因其舒适性、透气性、柔韧性、生物降解性、吸水性等优良性能而广受欢迎。但是,棉织物具有的多孔蓬松的结构和较高的比表面积为细菌和真菌生长提供了理想的条件(如湿度,温度和营养),在棉织物中,病原体繁殖迅速,散发出令人不快的气味,导致织物脱色和价值缩水,加速感染的交叉传播,危及人体健康。为了解决这些问题,人们致力于通过添加各种抗菌剂(如无机抗菌剂、双胍、季铵盐、卤胺、壳聚糖等)来改善棉织物的抗菌活性。
目前,由于病原微生物耐药性的不断增强,市场对抗菌材料的需求不断变高,单一抗菌剂难以达到理想的抗菌效果,因此开发多重抗菌新型材料已经成为现在的研究热点。
发明内容
本发明的目的在于解决上述不足,提供一种基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法,通过等离子体引发含双键的甜菜碱单体在棉织物表面接枝聚合,同时通过等离子体还原可以在棉织物表面制备纳米金属颗粒,由此制得的抗菌棉织物不仅具有优良的抗菌性能,同时具有良好的紫外防护性能。该方法具有反应条件温和、反应速度快、成本低,绿色环保的独特优势。
本发明技术方案:
一种基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法,包括如下步骤:
(1)配制一定浓度的甜菜碱水溶液和金属盐水溶液,二者按1∶1混合制得整理液,然后浸入棉织物,室温下避光震荡。
(2)取出织物并晾干后置于等离子体改性处理仪的真空腔中,抽真空至一定压强,通入工作气体,放电形成等离子体进行处理,处理完成后充分水洗并烘干至恒重。
进一步的,步骤(1)所述甜菜碱为甲基丙烯酰乙基磺基甜菜碱或2-甲基丙烯酰氧乙基羧酸基甜菜碱,甜菜碱水溶液的质量分数为1~20%。
进一步的,步骤(1)所述的金属盐为硝酸银、硝酸铜、硝酸锌、乙酸银、乙酸铜、乙酸锌、硫酸铜、硫酸锌、氯化银、氯化铜、氯化锌中的一种,金属盐水溶液质量分数为0.1~2%。
进一步的,步骤(1)所述浸入棉织物的浴比为1∶10N1∶100,室温下避光震荡10~60min。
进一步的,步骤(2)所述等离子体改性处理仪为HD-1B型冷等离子体改性处理仪,工作气体为空气、氩气氮气和氧气中的一中或几种的混合。
进一步的,步骤(2)所述等离子体改性处理抽真空至压强为5~50Pa,处理时间为1~5min,处理功率为100~500W。
进一步的,步骤(2)所述等离子体改性处理后充分水洗并烘干至恒重,干燥温度为40~60℃。
本发明的有益效果:本发明提供了一种基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法,将棉织物先浸渍在甜菜碱和金属盐的混合溶液中,然后通过等离子体处理,引发合有双键的甜菜碱在棉织物表面接枝聚合,同时,等离子体可以从金属盐溶液中还原产生纳米金属粒子并负载到棉织物上。该法工艺流程短、反应速度快,可在棉织物表面产生均匀的纳米粒子,且环境友好,无需使用有机溶剂。通过改法制备的棉织物具有较好的的抗菌活性和防紫外性能。
附图说明
图1为等离子体改性处理示意图。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合具体实施例和附图,对本发明实施例中的技术方案进行清楚、完整地描述。
实施例1:
一种基于等离子体技术制备抗菌棉织物的方法,包括如下步骤:
(1)配制5wt%的甲基丙烯酰乙基磺基甜菜碱水溶液,然后浸入棉织物,浴比1∶50,室温下避光震荡30min。
(2)取出织物并晾干后置于等离子体改性处理仪的真空腔中,抽真空至压强为20Pa,通入氩气,放电形成等离子体进行处理,处理功率为300W,处理时间为3min,等离子体处理完成后,将织物充分水洗并45℃烘干。
增重率测试。用等离子体处理前后织物的重量变化来评价等离子处理还原的金属粒子在棉织物上的负载量,增重率(G%)按如式I进行计算:
其中,M为等离子体处理后织物的重量(g),N为等离子体处理前织物的重量(g)。
制备的抗菌棉织物增重率为3.49%。
实施例2:
(1)配制5wt%的甲基丙烯酰乙基磺基甜菜碱水溶液和0.2wt%硝酸银水溶液,二者按体积比1∶1混合制得整理液,然后浸入棉织物,浴比1∶50,室温下避光震荡30min。
(2)取出织物并晾干后置于等离子体改性处理仪的真空腔中,抽真空至压强为20Pa,通入氩气,放电形成等离子体进行处理,处理功率为300W,处理时间为3min,等离子体处理完成后,将织物充分水洗并45℃烘干。测试增重率为4.52%。
实施例3:
步骤(1)中,配制5%的甲基丙烯酰乙基磺基甜菜碱水溶液和0.2%的硝酸铜水溶液,其余同实施例2,测试增重率为5.88%。
实施例4:
步骤(1)中,配制5%的甲基丙烯酰乙基磺基甜菜碱水溶液和0.2%的硝酸锌水溶液,其余同实施例2,测试增重率为5.26%。
实施例5:
步骤(1)中,配制5%的甲基丙烯酰乙基磺基甜菜碱水溶液和0.25%的硝酸银水溶液,其余同实施例2,测试增重率为4.86%。
实施例6:
步骤(1)中,配制5%的甲基丙烯酰乙基磺基甜菜碱水溶液和0.3%的硝酸银水溶液,其余同实施例2,测试增重率为5.38%。
实施例7:
步骤(1)中,配制5%的甲基丙烯酰乙基磺基甜菜碱水溶液和0.35%的硝酸银水溶液,其余同实施例2,测试增重率为5.76%。
实施例8:
步骤(1)中,配制5%的甲基丙烯酰乙基磺基甜菜碱水溶液和0.4%的硝酸银水溶液,其余同实施例2,测试增重率为6.12%。
最低抑菌浓度(MlC)测定
采用比浊法来测定双键甜菜碱、硝酸银、硝酸铜和硝酸锌溶液的MIC,将一定量甜菜碱溶于去离子水中,配制成浓度为384g/L的抗菌剂溶液,选用菌种为大肠杆菌,制备1×106-CFU/mL细菌悬浮液备用;取8个无菌试管,在第1个试管中加入1.6mL细菌悬浮液,其余试管分别加入1mL,取0.4mL的抗菌剂溶液加入到第1个试管中,摇匀后,从第1个试管中取1mL混合液加入第2个试管,摇匀后再从第2个试管中取1mL加入第3个试管,以此类推稀释到第7个试管,从第7个试管中取出1mL并舍弃,此时试管第1~7中甜菜碱单体浓度依次为76.8、38.4、19.2、9.6、4.8、2.4、1.2g/L;将上述接种好细菌的8个试管在37℃培养24h。
按上述方法,制备Ag+浓度为0.4096、0.2048、0.1024、0.0512、0.0256、0.0128、0.0064g/L的7个试管,第8个试管中不添加抗菌剂溶液,在37℃培养24h。
按上述方法,制备Cu2+浓度为2.56、1.28、0.64、0.32、0.16、0.08、0.04g/L的7个试管,第8个试管中不添加抗菌剂溶液,在37℃培养24h。
按上述方法,制备Zn2+浓度为5.12、2.56、1.28、0.64、0.32、0.16、0.08g/L的7个试管,第8个试管中不添加抗菌剂溶液,在37℃培养24h。
经测试,双键甜菜碱、Ag+、Cu2+、Zn2+对大肠杆菌的MIC分别为19.2g/L、0.0512g/L、0.16g/L和0.64g/L。
抑菌浓度指数(FIC)测定
采用棋盘稀释法,将上述四种抗菌原液分别取2×MIC、1×MIC、0.5×MIC、0.25×MIC、0.125×MIC浓度,取无菌96孔板,取50μL不同浓度的两种溶液分别排列在96版的横向和纵向中形成不同浓度组合的混合液,随后在每个孔中加入100μL的1×106-CFU/mL细菌悬浮液,在37℃培养24h。FIC的计算公式如下:
FIC=A混合使用时的MIC/A单独使用时的MIC+B混合使用时的MIC/B单独使用时的MIC。
FIC的测试结果如表1所示:
表1FIC结果
Ag<sup>+</sup> | Cu<sup>2+</sup> | Zn<sup>2+</sup> | |
双键甜菜碱 | 0.326 | 0.459 | 0.487 |
可以看出,FIC<0.5,表明甜菜碱和Ag+、Cu2+、Zn2+在等离子体技术处理下具有抗菌协同作用,其中Ag+的协同作用最强。
织物的抗菌性能测试:
根据修正后的AATCC100-2012抗菌测试标准,对实施例1、实施例2、实施例3、实施例4进行抗菌性能测试,以未处理的棉织物作为空白对照样。选用革兰氏阴性菌(大肠杆菌O157:H7)和革兰氏阳性菌(金黄色葡萄球菌)为测试菌种,大肠杆菌O157:H7和金黄色葡萄球菌的接种浓度分别1.7×106CFU/sample和2.1×106CFU/sample。抗菌测试结果分别显示在表2中。
表2织物的抗菌性能测试结果
抗菌测试结果显示,未负载纳米金属粒子的棉织物对大肠杆菌和金黄色葡萄球菌有一定杀菌率可能是因为甜菜碱可以抑制细菌在织物表面吸附和沉积,从而阻止细菌生物膜的形成。相比未负载纳米金属粒子的棉织物,负载了纳米金属粒子的棉织物的抗菌效率显著提升,尤其是浸渍在硝酸银溶液中的棉织物,通过等离子体将Ag+还原为Ag纳米粒子并负载在棉织物上,在5min就可以杀死全部的大肠杆菌和金黄色葡萄球菌,这是因为在等离子体作用下纳米Ag可以与细菌的细胞壁结合,破坏细胞膜使细胞渗液死亡,与细菌细胞的酶蛋白结合,影响细胞新陈代谢,使细菌窒息或缺营养死亡。不同实施例之间的抗菌效果有差异是因为纳米Ag的抗菌效果优于纳米Cu和纳米Zn。
防紫外性能测试
根据GB/T 18830-2009《纺织品防紫外线性能测试标准》对制备的棉织物进行测试,采用YG(B)912E型纺织品防紫外性能测试仪进行测试,测试样品为实施例2、实施例5、实施例6、实施例7和实施例8,以原棉织物为对照,结果如表3所示。
表3紫外防护性能测试结果
样品 | 增重率(%) | 紫外防护系(UPF) |
原棉织物 | -- | 8.62 |
实施例2 | 4.52 | 16.28 |
实施例5 | 4.68 | 58.40 |
实施例6 | 5.38 | 72.15 |
实施例7 | 5.76 | 85.93 |
实施例8 | 6.12 | 86.45 |
从表2中可以看出,随着硝酸银浓度增加,织物的增重率增加,织物的UPF值增加,这是因为纳米银尺寸小,接触面积大,可以吸收大量紫外线;另外银存在于织物表面是的织物颜色变深,深色织物对紫外线也有一定的吸收作用,因此,织物的防紫外性能较好。
Claims (9)
1.一种基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法,其特征在于:由以下步骤组成:
(1)配制一定浓度的甜菜碱水溶液和金属盐水溶液,二者按体积比1∶1混合制得整理液,然后浸入棉织物,室温下避光震荡;
(2)取出棉织物并晾干后置于等离子体改性处理仪的真空腔中,抽真空至一定压强,通入工作气体,放电形成等离子体进行处理,处理完成后充分水洗并烘干至恒重。
2.根据权利要求1所述的基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法,其特征在于:步骤(1)中,所述甜菜碱为甲基丙烯酰乙基磺基甜菜碱或2-甲基丙烯酰氧乙基羧酸基甜菜碱,甜菜碱水溶液的质量分数为1~20%。
3.据权利要求1或2所述的基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法,其特征在于:步骤(1)所述的金属盐为硝酸银、硝酸铜、硝酸锌、乙酸银、乙酸铜、乙酸锌、硫酸铜、硫酸锌、氯化银、氯化铜、氯化锌中的一种,金属盐水溶液质量分数为0.1~2%。
4.据权利要求1或2所述的基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法,其特征在于:步骤(1)所述浸入棉织物,浴比为1∶10~1∶100,室温下避光震荡10~60min。
5.据权利要求1或2所述的基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法,其特征在于:步骤(2)所述等离子体改性处理仪为HD-1B型冷等离子体改性处理仪,工作气体为空气、氩气、氮气和氧气中的一中或几种的混合。
6.据权利要求1或2所述的基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法,其特征在于:步骤(2)中,所述抽真空至一定压强,抽真空至压强为5~50Pa。
7.据权利要求6所述的基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法,其特征在于:步骤(2)中,所述放电形成等离子体进行处理,等离子体处理时间为1~5min,处理功率为100~500W。
8.据权利要求1或2所述的基于等离子体技术制备甜菜碱和纳米金属粒子双重抗菌棉织物的方法,其特征在于:步骤(2)中,处理完成后充分水洗并烘干至恒重,干燥温度为40~60℃。
9.权利要求1所述的方法得到的产品在制备抗菌棉织物中的应用。
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