CN112647294B - 一种具有优异耐洗性的抗菌性棉织物及其制备工艺 - Google Patents
一种具有优异耐洗性的抗菌性棉织物及其制备工艺 Download PDFInfo
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Abstract
本发明公布了一种具有优异耐洗性的抗菌棉织物及其制备工艺。该棉织物所涉及的材料包括羧甲基壳聚糖、(3‑羧丙基)三甲基氯化铵以及原始棉织物。所述耐洗抗菌棉织物的制备工艺为:(1)将洁净棉织物浸渍于配置好的羧甲基壳聚糖溶液中,控制增重后干热酯化;(2)将负载羧甲基壳聚糖的棉织物浸渍于配置好的(3‑羧丙基)三甲基氯化铵溶液中,经辊轧增重后加热反应。本发明用简单的浸渍、辊轧和加热工艺对棉织物进行抗菌改性,所得棉织物抗菌性能优异,耐洗性好且未对棉织物的固有性能造成损害,同时整理工艺简单,生产成本低,绿色环保,适用于工业生产。
Description
技术领域
本发明属于生物新材料领域,具体涉及一种具有优异耐洗性的抗菌性棉织物及其制备工艺。
技术背景
棉织物的透气性、柔软性和舒适性使其成为生产贴身衣物和床上用品的理想材料。此外,因为它们含有许多亲水基团所以具有良好的吸水能力。但是亲水性和透气性也容易为细菌的生存和繁殖提供合适的环境。细菌分泌物不仅有一种强烈而独特的气味,也会影响棉织物的外观和强度。这将会导致健康危害和经济损失。因此,棉织物的抗菌整理越来越受到重视。用于纺织工业的典型抗菌剂包括金属离子、金属氧化物、卤胺和季铵盐等。然而,当单独使用某种抗菌剂时,它们存在抑菌率有限和耐久性不足等问题。
壳聚糖是由甲壳素脱乙酰化产生的,无毒,可被人体产生的溶菌酶降解。壳聚糖还具有生物相容性,已广泛用于药物输送载体、密封膜和渗透膜等。在纺织领域,它还经常被用作棉织物染色、纺织品印花和抗收缩整理的预处理剂。羧甲基壳聚糖衍生物通过羧甲基基团对壳聚糖链上的羟基进行改性来提高水溶性。羧甲基壳聚糖含有许多游离的羧基和氨基,其羧基可以与棉织物的羟基酯化,将羧甲基壳聚糖连接到棉织物表面。羧甲基壳聚糖的氨基在酸性条件下可转化为季铵盐,但其改性的棉织物仅表现出相对较弱的抗菌性能。为了进一步增强抗菌效果,我们前期采用羧甲基壳聚糖作为粘结剂固定银和铜纳米粒子,尽管对金黄色葡萄球菌和大肠杆菌达到了99.9%以上的高抑菌率,但是由无机颗粒改性的棉织物的抗菌耐久性是有限的,这表现为在30次洗涤循环后它们的抗菌活性明显降低。同时,金属纳米粒子释放的金属离子也是对环境的潜在威胁。羧甲基壳聚糖将卤胺固定在棉织物上,虽然与不含羧甲基壳聚糖粘合剂的对照样品相比,抑菌率显著增加,但洗涤后需要进行卤素填充操作以再次获得理想的抗菌效果,过程繁琐,成本高。
(3-羧丙基)三甲基氯化铵,是甜菜碱盐酸盐的烷基衍生物。其结构中的阳离子铵有望起到有效的抑菌作用,其结构中的羧基与接枝在棉纤维上的羧甲基壳聚糖的氨基反应,从而将含阳离子铵的抗菌剂共价接枝到棉织物上。
综上所述,棉织物具有柔韧性好,透气性好,吸水性好,生物相容性好以及廉价易得的特性,作为生物材料使用具有明显的优势。但是抑菌率不高和抑菌耐洗性差两大缺点阻碍了其进一步的应用。本发明提供一套简易可行的方法,将羧甲基壳聚糖和(3-羧丙基)三甲基氯化铵共价接枝到棉织物表面。该方法所用原料安全易得,操作步骤简单,整理剂与棉织物之间的连接稳定。
发明内容
本发明解决的技术问题为:首先通过羧甲基壳聚糖的羧基与棉纤维表面的羟基之间的酯化反应,将羧甲基壳聚糖固定在棉纤维表面,然后将(3-羧丙基)三甲基氯化铵通过酰胺化反应连接到羧甲基壳聚糖链上。在提高抗菌棉织物的耐洗性的同时也增加了改性棉织物的安全性、降低了生产成本。包括如下操作步骤:
(1)将洁净织物在羧甲基壳聚糖水溶液中浸渍,辊轧,并加热酯化;
(2)将(1)中所得棉织物浸入(3-羧丙基)三甲基氯化铵水溶液中,经浸渍、辊轧,干热处理得到羧甲基壳聚糖和(3-羧丙基)三甲基氯化铵修饰的耐洗性抗菌棉织物。
进一步,步骤(1)所述羧甲基壳聚糖的分子质量为1-15 kDa,脱乙酰度为50-95%,取代度为60-90%,所述羧甲基壳聚糖水溶液的浓度为0.5-2 wt%,浸渍时间为2-10 min,辊轧增重70-100%,加热酯化温度控制在140-180 ℃,加热时间为5-180 min。
进一步,步骤(2)所述(3-羧丙基)三甲基氯化铵浓度为2-10 wt%,浸渍时间为2-10min,辊轧增重70-100%,加热温度控制在140-180 ℃,加热时间为5-180 min。与已有技术相比较,本发明不使用任何有机溶剂,所使用试剂生物相容性好,整个过程绿色无污染,不存在有毒有害分子残留问题,非常适合制备生物材料。
本发明将羧甲基壳聚糖、(3-羧丙基)三甲基氯化铵共价接枝到棉织物上。接枝了羧甲基壳聚糖的棉织物对大肠杆菌和金黄色葡萄球菌几乎没有抑制作用,继续接枝(3-羧丙基)三甲基氯化铵的抗菌性棉织物对这两种细菌抑菌率达到99.9%,赋予棉织物较高的抗菌性能。羧甲基壳聚糖起到一个连接的作用,没有接枝羧甲基壳聚糖仅负载(3-羧丙基)三甲基氯化铵的棉织物在洗涤10次后,抗菌率下降到40%。负载了羧甲基壳聚糖和(3-羧丙基)三甲基氯化铵的棉织物,在经过120次洗涤以后,对大肠杆菌和金黄色葡萄球菌的抑菌率均达到98%,显著提高了棉织物的抗菌耐洗性。
具体实施方式
以下结合具体的实施例对本发明的技术方案进一步地说明。
实施例1
将洁净棉织物在0.5 wt%羧甲基壳聚糖水溶液中浸渍10 min,辊轧增重100%后180℃加热5 min,用去离子水洗涤后干燥。
制得的改性棉织物由棉织物和羧甲基壳聚糖构筑而成,羧甲基壳聚糖分子量为5kDa,脱乙酰度为95%,取代度为80%,通过对改性棉织物进行红外分析,在1720 cm-1和1572cm-1处有分别有明显的C=O伸缩振动吸收峰和N-H弯曲振动吸收峰,说明羧甲基壳聚糖成功接枝于棉纤维表面。所得抗菌棉织物对大肠杆菌和金黄色葡萄球菌没有明显杀灭效果。接枝羧甲基壳聚糖的棉织物的水汽透过率为775 g/m2/d,吸水率为145%,抗拉强度为32.1MPa,与原始棉织物相比无明显差异。
实施例2
将洁净棉织物在5 wt%的(3-羧丙基)三甲基氯化铵水溶液中浸渍4 min,辊轧增重100%后180 ℃加热5 min,用去离子水洗涤后干燥。
制得的抗菌棉织物由棉织物和(3-羧丙基)三甲基氯化铵构筑而成,通过对改性棉织物进行红外分析,在1425 cm-1处出现CH3-N+的弯曲振动吸收峰,所得抗菌棉织物对大肠杆菌和金黄色葡萄球菌的抑菌率均达到90%以上,经过10次严格洗涤周期后,抑菌率降低至40%。负载了(3-羧丙基)三甲基氯化铵的改性棉织物的水汽透过率为792 g/m2/d,吸水率为161%,抗拉强度为29.3 MPa。
实施例3
将洁净棉织物在0.5 wt%羧甲基壳聚糖水溶液中浸渍10 min,辊轧增重100%后180℃加热5 min,用去离子水洗涤后干燥;
将接枝了羧甲基壳聚糖的棉织物在5 wt%的(3-羧丙基)三甲基氯化铵水溶液中浸渍4 min,辊轧增重100%后180 ℃加热5 min,用去离子水洗涤后干燥。
制得的抗菌棉织物由棉织物、羧甲基壳聚糖和(3-羧丙基)三甲基氯化铵构筑而成,羧甲基壳聚糖分子量为5 kDa,脱乙酰度为95%,取代度为80%,通过对改性棉织物进行红外分析,在1720 cm-1、1572 cm-1和1425 cm-1处分别出现C=O伸缩振动吸收峰、N-H弯曲振动吸收峰和CH3-N+的弯曲振动吸收峰,所得抗菌棉织物对大肠杆菌和金黄色葡萄球菌的抑菌率均达到99.9%以上,且经过120次严格的洗涤周期,抑菌率均为98%以上。抗菌棉织物的水汽透过率为779 g/m2/d,吸水性为158%,抗拉强度为30.1 MPa。
实施例4
将洁净棉织物在1 wt%羧甲基壳聚糖水溶液中浸渍8 min,辊轧增重90%后170 ℃加热10 min,用去离子水洗涤后干燥;
将接枝了羧甲基壳聚糖的棉织物在2 wt%的(3-羧丙基)三甲基氯化铵水溶液中浸渍10 min,辊轧增重90%后170 ℃加热10 min,用去离子水洗涤后干燥。
制得的抗菌棉织物由棉织物、羧甲基壳聚糖和(3-羧丙基)三甲基氯化铵构筑而成,羧甲基壳聚糖分子量为1 kDa,脱乙酰度为85%,取代度为60%,通过对改性棉织物进行红外分析,在1720 cm-1、1572 cm-1和1425 cm-1处分别出现C=O伸缩振动吸收峰、N-H弯曲振动吸收峰和CH3-N+的弯曲振动吸收峰,所得抗菌棉织物对大肠杆菌和金黄色葡萄球菌的抑菌率均达到85%以上,且经过120次严格的洗涤周期,抑菌率均为80%以上。棉织物的水汽透过率为763 g/m2/d,吸水性为150%,抗拉强度为31.7 MPa。
实施例5
将洁净棉织物在1.5 wt%羧甲基壳聚糖水溶液中浸渍5 min,辊轧增重80%后160℃加热30 min,用去离子水洗涤后干燥。
将2中接枝了羧甲基壳聚糖的棉织物在8 wt%的(3-羧丙基)三甲基氯化铵水溶液中浸泡6 min,轧制增重80%后160 ℃加热30 min,用去离子水洗涤后干燥。
制得的抗菌棉织物由棉织物、羧甲基壳聚糖和(3-羧丙基)三甲基氯化铵构筑而成,羧甲基壳聚糖分子量为10 kDa,脱乙酰度为75%,取代度为70%,通过对改性棉织物进行红外分析,在1720 cm-1、1572 cm-1和1425 cm-1处分别出现C=O伸缩振动吸收峰、N-H弯曲振动吸收峰和CH3-N+的弯曲振动吸收峰,所得抗菌棉织物对大肠杆菌和金黄色葡萄球菌的抑菌率均达到99.9%以上,且经过120次严格的洗涤周期,抑菌率均为98%以上。棉织物的水汽透过率为751 g/m2/d,吸水率为164%,抗拉强度为26.9 MPa。
实施例6
将洁净棉织物在2 wt%羧甲基壳聚糖水溶液中浸渍2 min,辊轧增重70%后140 ℃加热180 min, 用去离子水洗涤后干燥。
将1中接枝了羧甲基壳聚糖的棉织物在10 wt%的(3-羧丙基)三甲基氯化铵水溶液中浸渍2 min,辊轧增重70%后140 ℃加热180 min,用去离子水洗涤后干燥。
制得的抗菌棉织物由棉织物、羧甲基壳聚糖和(3-羧丙基)三甲基氯化铵构筑而成,羧甲基壳聚糖分子量为15 kDa,脱乙酰度为50%,取代度为95%,通过对改性棉织物进行红外分析,在1720 cm-1、1572 cm-1和1425 cm-1处分别出现C=O伸缩振动吸收峰、N-H弯曲振动吸收峰和CH3-N+的弯曲振动吸收峰,所得抗菌棉织物对大肠杆菌和金黄色葡萄球菌的抑菌率均达到99.9%以上,且经过120次严格的洗涤周期,抑菌率均为98%以上。棉织物的水汽透过率为745 g/m2/d,吸水性为165%,抗拉强度为25.5 MPa。
Claims (4)
1.一种具有优异耐洗性的抗菌棉织物,由棉织物、羧甲基壳聚糖和(3-羧丙基)三甲基氯化铵构成,其特征在于:所述羧甲基壳聚糖分子量为15 kDa,脱乙酰度为50%,取代度为95%。
2.一种具有优异耐洗性的抗菌性棉织物的制备工艺,其特征在于由如下两个步骤组合:
将洁净棉织物在羧甲基壳聚糖水溶液中浸渍,辊轧,并加热酯化;
将(1)中所得棉织物浸入(3-羧丙基)三甲基氯化铵水溶液中,经浸渍、辊轧,干热处理得到羧甲基壳聚糖和(3-羧丙基)三甲基氯化铵修饰的耐洗性抗菌棉织物。
3.如权利要求2所述的一种具有优异耐洗性的抗菌性棉织物的制备工艺,其特征在于,步骤(1)所述羧甲基壳聚糖的分子质量为1-15 kDa,脱乙酰度为50-95%,取代度为60-90%,所述羧甲基壳聚糖水溶液的浓度为0.5-2 wt%,浸渍时间为2-10 min,辊轧增重70-100%,加热酯化温度控制在140-180 ℃,加热时间为5-180 min。
4.如权利要求2所述的一种具有优异耐洗性的抗菌性棉织物的制备工艺,其特征在于,步骤(2)所述(3-羧丙基)三甲基氯化铵浓度为2-10 wt%,浸渍时间为2-10 min,辊轧增重70-100%,加热温度控制在140-180 ℃,加热时间为5-180 min。
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