CN115323778A - 壳聚糖-i型胶原氨基酸复合抗菌整理液及其制备方法和抗菌面料 - Google Patents

壳聚糖-i型胶原氨基酸复合抗菌整理液及其制备方法和抗菌面料 Download PDF

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CN115323778A
CN115323778A CN202210979855.8A CN202210979855A CN115323778A CN 115323778 A CN115323778 A CN 115323778A CN 202210979855 A CN202210979855 A CN 202210979855A CN 115323778 A CN115323778 A CN 115323778A
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柯开初
钟俊浩
柯晓芬
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Guangdong Runfengyi Textile Technology Co ltd
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Abstract

本发明公开了壳聚糖‑I型胶原氨基酸复合抗菌整理液，涉及纺织领域，包括以下原料：壳聚糖、I型胶原氨基酸、柠檬酸、聚丙烯酸钠、艾草提取液、节托莲提取液、改性聚乙二醇、植物多酚、玉米朊、改性蒙脱石、乙醇和水，通过壳聚糖和I型胶原氨基酸复合，提升壳聚糖的抑菌效果，加入艾草提取液、节托莲提取液和植物多酚，提高抗菌性能，节托莲与壳聚糖和I型胶原氨基酸复合物协同配合，进一步起到抑菌增效的作用，利用壳聚糖对面料的亲和性，在面料表面包覆壳聚糖，加入改性聚乙二醇和玉米朊，二者协同增效，能够与其他组分和面料的纤维化学键连接且连接强度大，并且能够形成多维均匀网络状结构，使抗菌成分更牢固附着在面料上，提升了抗菌耐久性。

Description

壳聚糖-I型胶原氨基酸复合抗菌整理液及其制备方法和抗菌 面料
技术领域
本发明涉及纺织领域，具体是壳聚糖-I型胶原氨基酸复合抗菌整理液及其制备方法和抗菌面料。
背景技术
随着人们生活水平的不断提高，在日常生活中，对于面料的舒适性和功能性也越来越关注。在人们生活的环境中生存着各种各样的微生物，其中，有些是对人体有益的，甚至是不可缺少的；另一些是有损于人体健康的，它们可以生存于人们日常使用的面料中，在温暖潮湿的环境中，便可大量的繁殖，严重影响着人们的身体健康，由此抗菌面料也越来越受到消费者的喜爱；
目前市场上主流的抗菌处理多采用抗菌整理液对面料进行浸轧，现有抗菌整理液多采用壳聚糖、纳米银离子等组分进行抗菌，但Ag+在空气中不稳定，易氧化发黑，与面料发生物理吸附，与面料间的结合能力差，面料耐洗涤性较差，而壳聚糖相对抗菌活性较低，也无法与面料稳定结合，抗菌耐久性低。
发明内容
本发明实施例的目的在于提供壳聚糖-I型胶原氨基酸复合抗菌整理液及其制备方法和抗菌面料，以解决现有抗菌整理液抗菌活性较低、抗菌耐久性低的问题。
壳聚糖-I型胶原氨基酸复合抗菌整理液，包括以下按照重量份的原料：壳聚糖10-20份、I型胶原氨基酸12-18份、柠檬酸1-5份、聚丙烯酸钠1-3份、艾草提取液5-9份、节托莲提取液4-8份、改性聚乙二醇7-12份、植物多酚1-3份、玉米朊3-7份、改性蒙脱石6-10份、乙醇20-30份和水100-120份。
在上述技术方案的基础上，本发明还提供以下可选技术方案：
在一种可选方案中：包括以下按照重量份的原料：壳聚糖12-18份、I型胶原氨基酸14-16份、柠檬酸2-4份、聚丙烯酸钠1.5-2.5份、艾草提取液6-8份、节托莲提取液5-7份4-8份、改性聚乙二醇8-11份、植物多酚1.5-2.5份、玉米朊4-6份、改性蒙脱石7-9份、乙醇23-27份和水105-115份。
在一种可选方案中：包括以下按照重量份的原料：壳聚糖15份、I型胶原氨基酸15份、柠檬酸3份、聚丙烯酸钠2份、艾草提取液7份、节托莲提取液6份6份、改性聚乙二醇9.5份、植物多酚2份、玉米朊5份、改性蒙脱石8份、乙醇25份和水110份。
在一种可选方案中：所述艾草提取液的制备方法如下：将干燥的艾草粉碎后加入反应装置，加5-10倍重量的水进行搅拌；然后加热反应装置以80-90℃进行加热1-2h，然后进行压榨，获得滤饼和去渣滤液；将去渣滤液进行一次纯化、浓缩、二次纯化，获得艾草提取液。
在一种可选方案中：所述节托莲提取液的制备方法如下：将节托莲进行水洗并晾干至叶片萎谢；将晾干后的节托莲在真空条件下进行微波干燥，微波干燥的微波功率为3000W，真空条件的真空度为-70～-60KPa，其中在微波干燥的过程中引入缓苏工艺；将经过微波干燥后的节托莲进行粉碎，在粉碎后的节托莲加入3-7倍重量的水，并进行超声波提取，得到节托莲提取液。
在一种可选方案中：所述改性聚乙二醇的制备方法如下：按照3:1:1称取木质素磺酸钠、硅烷偶联剂和三聚磷酸钾，并将之置于反应釜中，充分搅拌均匀得到混合物A，然后加入4-5倍混合物A重量的聚乙二醇，然后将反应釜内的温度升高至55～60℃，边搅拌边对反应釜内的混合料液进行紫外照射3～5h，得到所需改性聚乙二醇。
在一种可选方案中：所述植物多酚为牡丹酚、茶多酚、五倍子酚中的一种或多种组合。
在一种可选方案中：所述改性蒙脱石的制备方法如下：称取蒙脱石，采用碳酸镁溶液浸泡1-2h，用清水洗涤，然后放入-50～-40℃冷冻0.5-1h，然后通过红外辐射加热，红外辐射加热的温度控制在400-500℃，加热时间为1-2h，接着再放入-30～-20℃冷冻0.5-1h，取出后粉碎过筛，收集得到改性蒙脱石。
上述壳聚糖-I型胶原氨基酸复合抗菌整理液的制备方法，包括如下步骤：
将壳聚糖、I型胶原氨基酸、柠檬酸、聚丙烯酸钠、改性聚乙二醇以及玉米朊和乙醇混合均匀，得到混合物A；
将艾草提取液、节托莲提取液、植物多酚、改性蒙脱石和水充分混合均匀，得到混合物B；
将混合物A和混合物B置于50-60℃的温度下搅拌混合均匀，得到所需抗菌整理液。
一种抗菌面料，其制备方法包括如下步骤：
将涤纶纤维30-40份、棉纤维80-100份、甲壳素纤维10-16份进行混合后，按照现有技术中的混纺、整经、浆纱、穿经和织造等工序制得基布，备用；
制备抗菌整理液；
将基布二浸二轧抗菌整理液，同时对抗菌整理液施加按一定周期变化的电压而生成的振荡电场和通过永久磁铁或电磁铁而生成的静磁场构成的电磁场；
浸轧完成后，进行水洗，烘干，得到所需抗菌面料。
相较于现有技术，本发明实施例的有益效果如下：
通过壳聚糖和I型胶原氨基酸复合，将氨基酸接枝到壳聚糖上，壳聚糖上氨基增多，正电荷增多，提升壳聚糖的抑菌效果，通过加入艾草提取液、节托莲提取液、植物多酚以及改性蒙脱石，提高抗菌性能，其中，节托莲与壳聚糖和I型胶原氨基酸复合物协同配合，能够进一步起到抑菌增效的作用，通过加入改性蒙脱石，形成更多更小的微孔结构，有利于容纳、均匀分布更多的抗菌成分，提高抗菌效率和耐久性，并且利用壳聚糖对面料的亲和性，在面料表面包覆壳聚糖，通过加入改性聚乙二醇和玉米朊，二者协同增效，能够与其他组分和面料的纤维化学键连接且连接强度大，并且能够形成多维均匀网络状结构，使抗菌成分更牢固附着在面料上，提升了抗菌耐久性。
具体实施方式
以下实施例会对本发明进行详述。本发明所列举的各实施例仅用以说明本发明实施例，并非用以限制本发明的范围。对本发明实施例所作的任何显而易知的修饰或变更都不脱离本发明的精神与范围。
实施例1
本发明实施例中，称取以下按照重量份的原料：壳聚糖10份、I型胶原氨基酸12份、柠檬酸1份、聚丙烯酸钠1份、艾草提取液5份、节托莲提取液4份、改性聚乙二醇7份、植物多酚1份、玉米朊3份、改性蒙脱石6份、乙醇20份和水100份，将壳聚糖、I型胶原氨基酸、柠檬酸、聚丙烯酸钠、改性聚乙二醇以及玉米朊和乙醇混合均匀，得到混合物A；将艾草提取液、节托莲提取液、植物多酚、改性蒙脱石和水充分混合均匀，得到混合物B；将混合物A和混合物B置于50℃的温度下搅拌混合均匀，得到所需抗菌整理液。
其中，所述艾草提取液的制备方法如下：将干燥的艾草粉碎后加入反应装置，加8倍重量的水进行搅拌；然后加热反应装置以85℃进行加热1.5h，然后进行压榨，获得滤饼和去渣滤液；将去渣滤液进行一次纯化、浓缩、二次纯化，获得艾草提取液，通过添加艾草提取液，利用艾草的杀菌作用。
所述节托莲提取液的制备方法如下：将节托莲进行水洗并晾干至叶片萎谢；将晾干后的节托莲在真空条件下进行微波干燥，微波干燥的微波功率为3000W，真空条件的真空度为-65KPa，其中在微波干燥的过程中引入缓苏工艺；将经过微波干燥后的节托莲进行粉碎，在粉碎后的节托莲加入5倍重量的水，并进行超声波提取，得到节托莲提取液。
所述改性蒙脱石的制备方法如下：称取蒙脱石，采用碳酸镁溶液浸泡1.5h，用清水洗涤，然后放入-45℃冷冻0.8h，然后通过红外辐射加热，红外辐射加热的温度控制在450℃，加热时间为1.5h，接着再放入-25℃冷冻0.8h，取出后粉碎过筛，收集得到改性蒙脱石；
具体的，所述碳酸镁溶液浓度为2mol/L；
可以理解的是，通过碳酸镁处理蒙脱石，可以使蒙脱石剥离分散成更薄的单晶片，再进行冷冻-加热-冷冻的方式，使得蒙脱石进一步分散成更多更小的微孔结构，有利于容纳、均匀分布更多的抗菌成分，提高抗菌效率和耐久性。
所述改性聚乙二醇的制备方法如下：按照3:1:1称取木质素磺酸钠、硅烷偶联剂和三聚磷酸钾，并将之置于反应釜中，充分搅拌均匀得到混合物A，然后加入4.5倍混合物A重量的聚乙二醇，然后将反应釜内的温度升高至57℃，边搅拌边对反应釜内的混合料液进行紫外照射4h，得到所需改性聚乙二醇，经改性的聚乙二醇反应活性提高，能够更充分的与玉米朊反应，进一步提高与壳聚糖、面料等的连接强度，提高抗菌耐久性；
在具体实施中，硅烷偶联剂分子中的硅烷氧基对无机物具有反应性，有机官能基对有机物具有反应性，其能分别与木质素磺酸钠及三聚磷酸钾分子中的相关官能团发生化学反应而成键，从而使得木质素磺酸钠接枝到三聚磷酸钾分子上，增大了木质素磺酸钠分子与聚乙二醇的碰撞几率，在木质素磺酸钠及紫外照射的联合作用下能对聚乙二醇进行有效地活化，有效地提高了聚乙二醇的反应活性。
其中，所述植物多酚为五倍子酚。
通过本实施例中的抗菌整理液，来制备一种抗菌面料，其制备方法包括如下步骤：
将涤纶纤维35份、棉纤维90份、甲壳素纤维13份进行混合后，按照现有技术中的混纺、整经、浆纱、穿经和织造等工序制得基布，备用；
制备抗菌整理液；
将基布二浸二轧抗菌整理液，同时对抗菌整理液施加按一定周期变化的电压而生成的振荡电场和通过永久磁铁或电磁铁而生成的静磁场构成的电磁场，通过振荡电磁场使提高抗菌整理液的活性，更好的整理基布；
浸轧完成后，进行水洗，烘干，得到所需抗菌面料。
实施例2
本发明实施例与实施例1的不同之处在于，称取以下重量份的原料：壳聚糖12份、I型胶原氨基酸14份、柠檬酸2份、聚丙烯酸钠1.5份、艾草提取液6份、节托莲提取液5份、改性聚乙二醇8份、植物多酚1.5份、玉米朊4份、改性蒙脱石7份、乙醇23份和水105份，将壳聚糖、I型胶原氨基酸、柠檬酸、聚丙烯酸钠、改性聚乙二醇以及玉米朊和乙醇混合均匀，得到混合物A；将艾草提取液、节托莲提取液、植物多酚、改性蒙脱石和水充分混合均匀，得到混合物B；将混合物A和混合物B置于50℃的温度下搅拌混合均匀，得到所需抗菌整理液。
实施例3
本发明实施例与实施例1的不同之处在于，称取以下重量份的原料：壳聚糖15份、I型胶原氨基酸15份、柠檬酸3份、聚丙烯酸钠2份、艾草提取液7份、节托莲提取液6份、改性聚乙二醇9.5份、植物多酚2份、玉米朊5份、改性蒙脱石8份、乙醇25份和水110份，将壳聚糖、I型胶原氨基酸、柠檬酸、聚丙烯酸钠、改性聚乙二醇以及玉米朊和乙醇混合均匀，得到混合物A；将艾草提取液、节托莲提取液、植物多酚、改性蒙脱石和水充分混合均匀，得到混合物B；将混合物A和混合物B置于50-60℃的温度下搅拌混合均匀，得到所需抗菌整理液。
实施例4
本发明实施例与实施例1的不同之处在于，称取以下重量份的原料：壳聚糖18份、I型胶原氨基酸16份、柠檬酸4份、聚丙烯酸钠2.5份、艾草提取液8份、节托莲提取液7份、改性聚乙二醇11份、植物多酚2.5份、玉米朊6份、改性蒙脱石9份、乙醇27份和水115份，将壳聚糖、I型胶原氨基酸、柠檬酸、聚丙烯酸钠、改性聚乙二醇以及玉米朊和乙醇混合均匀，得到混合物A；将艾草提取液、节托莲提取液、植物多酚、改性蒙脱石和水充分混合均匀，得到混合物B；将混合物A和混合物B置于50-60℃的温度下搅拌混合均匀，得到所需抗菌整理液。
实施例5
本发明实施例与实施例1的不同之处在于，称取以下重量份的原料：壳聚糖20份、I型胶原氨基酸18份、柠檬酸5份、聚丙烯酸钠3份、艾草提取液9份、节托莲提取液8份、改性聚乙二醇12份、植物多酚3份、玉米朊7份、改性蒙脱石10份、乙醇30份和水120份，将壳聚糖、I型胶原氨基酸、柠檬酸、聚丙烯酸钠、改性聚乙二醇以及玉米朊和乙醇混合均匀，得到混合物A；将艾草提取液、节托莲提取液、植物多酚、改性蒙脱石和水充分混合均匀，得到混合物B；将混合物A和混合物B置于50-60℃的温度下搅拌混合均匀，得到所需抗菌整理液。
对比例1
在实施例3的基础上，将壳聚糖和I型胶原氨基酸替换为相同重量份的水。
对比例2
在实施例3的基础上，将节托莲提取液替换为相同重量份的水。
对比例3
在实施例3的基础上，将壳聚糖和I型胶原氨基酸以及节托莲提取液替换为相同重量份的水。
对比例4
在实施例3的基础上，将改性聚乙二醇替换为相同重量份的水。
对比例5
在实施例3的基础上，将玉米朊替换为相同重量份的水。
对比例6
在实施例3的基础上，将改性聚乙二醇和玉米朊替换为相同重量份的水。
对比例7
在实施例3的基础上，将改性聚乙二醇替换为相同重量份的普通聚乙二醇；
对比例8
在实施例3的基础上，将改性蒙脱石替换为相同重量份的普通蒙脱石；
对比例9
在实施例3的基础上，在制备抗菌面料时，不对抗菌整理液施加振荡电场和电磁场；
在相同的实验条件下，参照标准GBT20944.3-2008中的振荡法，以金黄色葡萄球菌(ATCC6538)、大肠杆菌(ATCC8739)和白色念珠菌(ATCC10231)为测试菌种，按GB/T20944.2-2007分别对上述实施例1-5以及对比例1-6制得的面料的抑菌率进行测试，其测试结果如表1所示：
Figure BDA0003799940270000071
Figure BDA0003799940270000081
从以上实施例1-5以及对比例1-3的结果可以看出，壳聚糖和I型胶原氨基酸以及节托莲提取液具有协同增效作用，能够提高整理液的抗菌性能；
从以上实施例1-5以及对比例4-6的结果可以看出，改性聚乙二醇和玉米朊存在协同增效作用，能够使得抗菌成分与面料附着更牢固，更紧密，有助于提高抗菌耐久性。
以上所述，仅为本公开的具体实施方式，但本公开的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本公开揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本公开的保护范围之内。因此，本公开的保护范围应以权利要求的保护范围为准。

Claims (10)

1.壳聚糖-I型胶原氨基酸复合抗菌整理液，其特征在于，包括以下按照重量份的原料：壳聚糖10-20份、I型胶原氨基酸12-18份、柠檬酸1-5份、聚丙烯酸钠1-3份、艾草提取液5-9份、节托莲提取液4-8份、改性聚乙二醇7-12份、植物多酚1-3份、玉米朊3-7份、改性蒙脱石6-10份、乙醇20-30份和水100-120份。
2.根据权利要求1所述的壳聚糖-I型胶原氨基酸复合抗菌整理液，其特征在于，包括以下按照重量份的原料：壳聚糖12-18份、I型胶原氨基酸14-16份、柠檬酸2-4份、聚丙烯酸钠1.5-2.5份、艾草提取液6-8份、节托莲提取液5-7份、改性聚乙二醇8-11份、植物多酚1.5-2.5份、玉米朊4-6份、改性蒙脱石7-9份、乙醇23-27份和水105-115份。
3.根据权利要求2所述的壳聚糖-I型胶原氨基酸复合抗菌整理液，其特征在于，包括以下按照重量份的原料：壳聚糖15份、I型胶原氨基酸15份、柠檬酸3份、聚丙烯酸钠2份、艾草提取液7份、节托莲提取液6份、改性聚乙二醇9.5份、植物多酚2份、玉米朊5份、改性蒙脱石8份、乙醇25份和水110份。
4.根据权利要求1所述的壳聚糖-I型胶原氨基酸复合抗菌整理液，其特征在于，所述艾草提取液的制备方法如下：将干燥的艾草粉碎后加入反应装置，加5-10倍重量的水进行搅拌；然后加热反应装置以80-90℃进行加热1-2h，然后进行压榨，获得滤饼和去渣滤液；将去渣滤液进行一次纯化、浓缩、二次纯化，获得艾草提取液。
5.根据权利要求1所述的壳聚糖-I型胶原氨基酸复合抗菌整理液，其特征在于，所述节托莲提取液的制备方法如下：将节托莲进行水洗并晾干至叶片萎谢；将晾干后的节托莲在真空条件下进行微波干燥，微波干燥的微波功率为3000W，真空条件的真空度为-70～-60KPa，其中在微波干燥的过程中引入缓苏工艺；将经过微波干燥后的节托莲进行粉碎，在粉碎后的节托莲加入3-7倍重量的水，并进行超声波提取，得到节托莲提取液。
6.根据权利要求1所述的壳聚糖-I型胶原氨基酸复合抗菌整理液，其特征在于，所述改性聚乙二醇的制备方法如下：按照3:1:1称取木质素磺酸钠、硅烷偶联剂和三聚磷酸钾，并将之置于反应釜中，充分搅拌均匀得到混合物A，然后加入4-5倍混合物A重量的聚乙二醇，然后将反应釜内的温度升高至55～60℃，边搅拌边对反应釜内的混合料液进行紫外照射3～5h，得到所需改性聚乙二醇。
7.根据权利要求1所述的壳聚糖-I型胶原氨基酸复合抗菌整理液，其特征在于，所述植物多酚为牡丹酚、茶多酚、五倍子酚中的一种或多种组合。
8.根据权利要求1所述的壳聚糖-I型胶原氨基酸复合抗菌整理液，其特征在于，所述改性蒙脱石的制备方法如下：称取蒙脱石，采用碳酸镁溶液浸泡1-2h，用清水洗涤，然后放入-50～-40℃冷冻0.5-1h，然后通过红外辐射加热，红外辐射加热的温度控制在400-500℃，加热时间为1-2h，接着再放入-30～-20℃冷冻0.5-1h，取出后粉碎过筛，收集得到改性蒙脱石。
9.如权利要求1-8任一所述的壳聚糖-I型胶原氨基酸复合抗菌整理液的制备方法，其特征在于，包括如下步骤：
将壳聚糖、I型胶原氨基酸、柠檬酸、聚丙烯酸钠、改性聚乙二醇以及玉米朊和乙醇混合均匀，得到混合物A；
将艾草提取液、节托莲提取液、植物多酚、改性蒙脱石和水充分混合均匀，得到混合物B；
将混合物A和混合物B置于50-60℃的温度下搅拌混合均匀，得到所需抗菌整理液。
10.一种抗菌面料，其特征在于，其制备方法包括如下步骤：
将涤纶纤维30-40份、棉纤维80-100份、甲壳素纤维10-16份进行混合后，按照现有技术中的混纺、整经、浆纱、穿经和织造等工序制得基布，备用；
采用如权利要求9的方法制备抗菌整理液；
将基布二浸二轧抗菌整理液，同时对抗菌整理液施加按一定周期变化的电压而生成的振荡电场和通过永久磁铁或电磁铁而生成的静磁场构成的电磁场；
浸轧完成后，进行水洗，烘干，得到所需抗菌面料。
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CN115678220B (zh) * 2022-11-15 2024-03-08 浙江中盛新材料股份有限公司 一种耐拉伸抗菌装饰膜及其制备方法

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