CN113818249A - 一种接枝壳聚糖抗菌剂的合成及其对涤棉织物的整理工艺 - Google Patents
一种接枝壳聚糖抗菌剂的合成及其对涤棉织物的整理工艺 Download PDFInfo
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Abstract
本发明涉及一种壳聚糖接枝共聚物抗菌剂的合成及其对涤棉织物的整理工艺,所述抗菌剂的制备步骤为:(1)将壳聚糖与乙酸溶液混合,在35~65℃下搅拌30min~40min得到溶液A;(2)将双氧水加入溶液A中,在35~65℃下搅拌1h,得到溶液B;(3)将DMC、双氧水(30%wt)依次加入到溶液B中,随后将抗坏血酸溶于10ml水中,匀速滴加至溶液B中搅拌1.5h,得到溶液C;(4)重复步骤(3)得到溶液D;(5)取出溶液D,进行旋蒸冻干后收集。所述整理工艺的原料备选为:抗菌剂A1份、柠檬酸1.5份、次磷酸钠(丁烷四羧酸)1份、乳化剂1份、水100份。所得抗菌剂合成方法绿色、低能耗,且经过该抗菌剂整理后的涤棉混纺织物具有良好的抗菌性和耐洗性。
Description
技术领域
本发明涉及纺织品用反应性抗菌剂的合成与纺织品整理领域,具体为一种以壳聚糖与甲基丙烯酰氧乙基三甲基氯化铵合成的反应型阳离子抗菌单体及其对涤棉织物的抗菌整理。
背景技术
涤棉混纺织物柔软舒适,稳定性好,经水洗或拉扯后不易变形。薄涤棉混纺织物常用作夏季衣物的制作,但由于涤纶纤维吸湿透气性较差,伴随着人体分泌物与汗液的浸渍,微生物在适宜的环境下快速繁殖,使得织物产生异味,甚至会导致霉菌和变色,因此对涤棉织物进行抗菌整理是必要的。
目前,织物抗菌整理剂种类主要为无机抗菌剂、有机抗菌剂、天然抗菌剂三类。其中,天然抗菌剂主要来源为自然界中的植物、动物和微生物,抗菌效果好的同时具有良好的生物相容性与生物可降解性。
随着人们生活品质的提高,保护环境的理念愈发深入,自然生物类物质受到各领域研究人员的青睐。天然整理剂中壳聚糖最为普及,壳聚糖具有以下两种杀菌机理:(1)壳聚糖大分子的与带负电的细菌细胞膜产生静电吸附,使得细胞膜上电荷分布不均,细胞壁的合成与溶解平衡被破坏最终导致细菌破裂;(2) 壳聚糖大分子进入细胞中,细胞内带有负电的物质被-NH3+所吸附,导致微生物细胞失去活性而死亡。
虽然壳聚糖整理剂具有广谱抗菌性,但耐洗性差,同时由于壳聚糖水溶性差,难以采用传统轧烘焙整理方法对织物进行抗菌整理。为提高其耐洗性及长效抗菌性,国内外学者在此基础上研发了复合型壳聚糖抗菌剂、改性壳聚糖抗菌剂、纳米壳聚糖抗菌剂。
发明内容
本发明的目的是为了克服现有壳聚糖类抗菌整理剂水溶性差、整理后耐洗性差等问题,提供一种共聚物接枝壳聚糖的抗菌整理剂的合成方法与整理工艺。该合成方法采取自由基共聚反应,原料均绿色无害,且织物经过整理后具有长久有效的抗菌效果。
为实现上述目的,本发明采取以下技术方案:
1.一种共聚物接枝壳聚糖的抗菌剂A制备方法,包括以下步骤:
(1)将2g壳聚糖与20~40ml 1%乙酸溶液混合,在35~65℃下搅拌30min~40min至壳聚糖完全溶于乙酸溶液中,得到溶液A;
(2)将1ml~2ml双氧水加入溶液A中,在35~65℃下搅拌1h,得到溶液B;
(3)将1.5ml~2.5ml甲基丙烯酰氧乙基三甲基氯化铵(DMC)、1ml双氧水(30%wt)依次加入到溶液B中,随后将0.375g~1.55g抗坏血酸溶于10ml水中,置于恒压滴液漏斗,匀速滴加至溶液B中继续搅拌1.5h,得到溶液C;
(4)将0.375g~1.55g抗坏血酸溶于10ml水中,置于恒压滴液漏斗,匀速滴加至溶液C中继续搅拌 1.5h,得到溶液D;
(5)取出溶液D,进行旋蒸除去多余的水分后,置于真空干燥冷冻机中冻干12~18h,取出收集,得到抗菌剂A。
作为本发明的进一步优化的方案:
(1)将2g壳聚糖与40ml 1%乙酸溶液混合,在55℃下搅拌30min~40min至壳聚糖完全溶于乙酸溶液中,得到溶液A;
(2)将2ml双氧水加入溶液A中,在55℃下搅拌1h,得到溶液B;
(3)将2ml甲基丙烯酰氧乙基三甲基氯化铵(DMC)、1ml双氧水(30%wt)依次加入到溶液B中,随后将1.55g抗坏血酸溶于10ml水中,置于恒压滴液漏斗,匀速滴加至溶液B中继续搅拌1.5h,得到溶液C;
(4)将1.55g抗坏血酸溶于10ml水中,置于恒压滴液漏斗,匀速滴加至溶液C中继续搅拌1.5h,得到溶液D;
(5)取出溶液D,进行旋蒸除去多余的水分后,置于真空干燥冷冻机中冻干12~18h,取出收集,得到抗菌剂A,放入密封锥形瓶内保存。
2.一种涤棉混纺织物的抗菌整理工艺,包括以下步骤:
(1)进一步的配置整理液B,各物质用量按照重量份如下:
抗菌剂A 1份
柠檬酸1.5份
次磷酸钠(或丁烷四羧酸)1份
乳化剂OP-10 1份
水100份
(2)将涤棉织物用去离子水洗净,然后将洗净的涤棉织物浸泡在上述整理液中,50℃浸泡30min,一轧轧余率50%,二浸30min,二轧轧余率200%,取出后在80℃预烘5min,最后在140℃焙烘10min;
(3)取出织物,用流动的去离子水洗去织物表面未参与反应的残留物,自然风干。
本发明具有以下有益效果:
本发明通过双氧水和抗坏血酸的氧化还原体系中的自由基降解壳聚糖并将DMC单体成功接枝于壳聚糖上,该氧化还原体系活化能低,可在较低温度下引发接枝共聚。相较于原壳聚糖在中性溶液中溶解性较差,本发明中的抗菌剂在中性溶液中溶解性优异的同时抑菌效果显著。其次本发明中对涤棉混纺织物的抗菌整理工艺采用多元羧酸无甲醛整理剂,使用柠檬酸和丁烷四羧酸作为交联剂,绿色环保。经该抗菌剂整理后的涤棉织物白度变化不大,并且具有良好的抗菌性能和耐洗牢度。
附图说明
图1为本发明抗菌剂图;
图2为原壳聚糖和本发明抗菌剂的水溶性效果图,其中图2-1为原壳聚糖水溶性效果图;图2-2为本发明抗菌剂的水溶性效果图;
图3为本发明为由活菌计数法测得的不同浓度抗菌剂抗菌效果图;
图4为本发明中由振荡法测得的最佳抗菌整理工艺下整理涤棉混纺织物的抗菌效果图,其中图4-1为未整理涤棉织物的抗菌效果图;图4-2为整理后洗涤20次涤棉织物的抗菌效果图。
具体实施说明
下面结合具体实施方式对本发明的技术方案作进一步详细的说明,具体实施例仅是为了进一步详细说明本发明,不限制本发明的权利要求。
实施例1
一种共聚物接枝壳聚糖的抗菌剂A制备方法,包括以下步骤:
(1)按照表1称取各原料;
(2)将壳聚糖溶于乙酸溶液后,置于三颈烧瓶中,在55℃下用磁力搅拌机以转速190rpm搅拌30 min~45min至溶解均匀,得到溶液A;
(3)向溶液A中加入双氧水(a),在55℃下反应1h,得到溶液B;
(4)将甲基丙烯酰氧乙基三甲基氯化铵(DMC)、双氧水(30%wt)依次加入到溶液B中,随后将抗坏血酸溶于10ml水中,置于恒压滴液漏斗,匀速滴加至溶液B中继续搅拌1.5h,得到溶液C;
(5)将抗坏血酸溶于10ml水中,置于恒压滴液漏斗,匀速滴加至溶液C中继续搅拌1.5h,得到溶液D;
(6)取出溶液D,进行旋蒸除去多余的水分后,置于真空干燥冷冻机中冻干12~18h,取出收集,得到抗菌剂A,放入密封锥形瓶内保存。
表1 原料用量表/重量份
原料 | 实施例1 | 实施例2 | 实施例3 |
壳聚糖 | 2 | 2 | 2 |
1%乙酸 | 40 | 40 | 40 |
30%双氧水(a) | 1 | 2 | 2 |
DMC | 1.5 | 2 | 2.5 |
30%双氧水(b) | 1 | 1 | 1 |
抗坏血酸 | 1.55 | 1.55 | 1.55 |
30%双氧水(c) | 1 | 1 | 1 |
抗坏血酸 | 1.55 | 1.55 | 1.55 |
实施例2
各物质用量参照表1,制备方法同实施例1。
实施例3
各物质用量参照表1,制备方法同实施例1。
性能检测
取实施例2中的抗菌剂溶于去离子水中,水溶性如图2所示,水溶性优异。
取实施例2中的抗菌剂溶于去离子水中,配置成0.1、0.2、0.4、0.8、1g/L的溶液,对大肠杆菌的抑菌效果如图3所示。由浓度为1g/L的抗菌剂溶液的抑菌率达到100%。
实施例4
一种涤棉混纺织物的抗菌整理工艺,包括以下步骤:
(1)采用实施例2中制得的抗菌剂用于配置整理液;
(2)按照表2称取各原料:
表2 原料用量表/重量份
原料 | 实施例4 | 实施例5 | 实施例6 |
抗菌剂 | 1 | 0.625 | 0.016 |
柠檬酸 | 1 | 0 | 0 |
丁烷四羧酸 | 0 | 0.1 | 0.025 |
次磷酸钠 | 1.5 | 0.0625 | 0.016 |
乳化剂OP-10 | 1 | 1 | 1 |
去离子水 | 100 | 100 | 100 |
(2)将涤棉织物用去离子水洗净,然后将洗净的涤棉织物浸泡在上述整理液中,50℃浸泡30min,一轧轧余率50%,二浸30min,二轧轧余率200%,取出后在80℃预烘5min,最后在140℃焙烘10min;
(3)取出织物,用流动的去离子水洗去织物表面未参与反应的残留物,自然风干。
实施例5
各物质用量参照表2,制备方法同实施例4。
实施例6
各物质用量参照表2,制备方法同实施例4。
性能检测
将上述整理后的涤棉织物剪成尺寸为5cm×5cm的试样,采用ECE无磷标准洗涤剂进行洗涤:条件如下:水温40℃,溶液150ml,洗涤剂浓度0.2%,钢珠10粒,洗涤45min。此程序相当于5次水洗,重复洗涤直至洗涤20次。洗涤后取出试样,充分清洗样品以去除织物上残留的洗涤剂,45℃烘干。将洗涤前、后的待测试样与原织物分别剪成5mm×5mm的碎片,各称取0.75±0.05g作为一份试样,置于紫外灯下灭菌,备用。
取上述试样进行抗菌测试,图2为由振荡法测得的最佳抗菌整理工艺下整理涤棉混纺织物的抗菌效果图。由图4所示,经活菌计数法可知,整理后的涤棉织物洗涤20次后对大肠杆菌的抑菌率仍达到89.2%。
以上所述,仅为本发明较佳的具体实施方式,但本发明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发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (2)
1.一种壳聚糖接枝共聚物抗菌剂的制备方法,其特征在于:包括以下步骤:
(1)将2g壳聚糖与20~40ml 1%乙酸溶液混合,在35~65℃下搅拌30min~40min至壳聚糖完全溶于乙酸溶液中,得到溶液A;
(2)将1ml~2ml双氧水加入溶液A中,在35~65℃下搅拌1h,得到溶液B;
(3)将1.5ml~2.5ml甲基丙烯酰氧乙基三甲基氯化铵(DMC)、1ml双氧水(30%wt)依次加入到溶液B中,随后将0.375g~1.55g抗坏血酸溶于10ml水中,置于恒压滴液漏斗,匀速滴加至溶液B中继续搅拌1.5h,得到溶液C;
(4)将0.375g~1.55g抗坏血酸溶于10ml水中,置于恒压滴液漏斗,匀速滴加至溶液C中继续搅拌1.5h,得到溶液D;
(5)取出溶液D,进行旋蒸除去多余的水分后,置于真空干燥冷冻机中冻干12~18h,取出收集,得到抗菌剂A。
2.一种将权利要求书1中所制抗菌剂整理到涤棉混纺织物的整理工艺,其特征如下:包括以下步骤:
(1)进一步的配置整理液B,各物质用量按照重量份如下:
抗菌剂A 1份
柠檬酸1.5份
次磷酸钠(或丁烷四羧酸)1份
乳化剂OP-10 1份
水100份
(2)将涤棉织物用去离子水洗净,然后将洗净的涤棉织物浸泡在上述整理液中,50℃浸泡30min,一轧轧余率50%,二浸30min,二轧轧余率200%,取出后在80℃预烘5min,最后在140℃焙烘10min;
(3)取出织物,用流动的去离子水洗去织物表面未参与反应的残留物,自然风干。
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