CN108930156A - 一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法 - Google Patents
一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法 Download PDFInfo
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Abstract
本发明公开了一种用卤胺‑氨基化复合改性棉纤维制作长效抗菌家居用品的方法，将磁性棉纤维‑聚苯胺复合材料与氯化的接枝水溶性卤胺前置体的棉纤维、纳米银原位生成整理的氨基化棉纤维进行混纺，得到所述家居用品。采用浸渍‑干燥‑固化的方法将水溶性卤胺前置体接枝到预处理棉纤维上，通过次氯酸钠漂白溶液的浸泡氯化制备出具有抗菌功效的棉纤维，并且有良好的耐洗性和稳定性。通过氧化活化棉纤维并接枝端氨基超支化聚合物制备了氨基化改性棉纤维，利用改性棉纤维中丰富氨基对银离子的络合、还原作用原位控制生成纳米银，实现了对棉织物的高效抗菌整理；氨基化棉纤维原位生成的纳米银粒径小，且氨基化棉纤维整理后纳米银的耐洗牢度较高。
Description
技术领域
本发明属于家居用品技术领域，具体涉及一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法。
背景技术
棉纤维是一种重要的工业原料，作为自然界最纯净的纤维素在轻工、化学、医药、国防等工业领域得到广泛应用。但是，棉纤维致密的结晶结构和较高的聚合度导致其结晶度较高，限制了其有效利用。因此，降低棉纤维结晶度，提高其反应性能显得尤为重要。氢氧化钠-尿素水体系是一种成本较低、无毒无污染、绿色环保的非衍生化纤维素溶剂，对纤维素的溶解能力较强。
纳米银是一种具有高效杀菌性能的无机纳米材料，并且由于其无毒、抗菌持久稳定、不易产生抗药性等特点，在纺织领域常被用作抗菌整理剂。利用纳米银对纺织品进行抗菌整理有多种方法，如浸渍吸附、多层沉积、聚合物混合涂层等。在这些方法中简单的物理吸附往往牢度不够，使用交联剂固着或聚合物涂层来增加其牢度又会造成织物原有的优异手感、对人体肌肤的亲和力等丧失，并且这些化学试剂的使用不仅会污染环境，整理到织物上还会对人体产生潜在的危害。同时，纳米银在保存和整理应用过程中往往会产生团聚现象。近年来，原位生成纳米银抗菌整理技术以其高效、简便、环保等特性日益受到广大研究人员的重视。
发明内容
本发明的目的是针对现有的问题，提供了一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法，依照该方法制作的家居用品具有良好的长效抗菌能力、耐洗性和稳定性，且能吸收电磁波辐射。
本发明是通过以下技术方案实现的：
一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法，其特征在于，包括如下步骤：
（1）氢氧化钠-尿素水体系预处理棉纤维的工艺：
向质量比为8:14的氢氧化钠和尿素中加入水，搅拌20-25min溶解均匀，放入低温恒温水浴锅中预冷至-4℃，加入棉纤维搅拌预处理，用100目的滤袋过滤，用蒸溜水洗涤至滤水呈中性，均分成3份待用；
（2）棉纤维接枝水溶性卤胺前置体：
将1/3的（1）中所得预处理棉纤维浸泡在接枝溶液中15-20min浸湿，然后在78-82℃鼓风干燥箱中干燥固化1-2h，再浸泡于0.5%的洗涤剂中15-20min，用去离子水冲洗后放入65-70℃的真空干燥箱中干燥1-2h；
（3）氨基化棉纤维的纳米银原位生成整理：
按浴比1:50将氨基化棉纤维浸渍于0.1 mol/L的硝酸银水溶液中，在96-98℃下搅拌1-2min后水洗，常温晾干；
（4）家居用品的制备：
将四氧化三铁纳米颗粒与棉纤维-聚苯胺复合材料按质量比1:1加入到无水乙醇中，超声分散完全，机械搅拌3-4h得磁性棉纤维-聚苯胺复合材料；
将其与所得氯化的接枝水溶性卤胺前置体的棉纤维、纳米银原位生成整理的氨基化棉纤维进行混纺，得到所述家居用品。
进一步的，步骤（2）中接枝溶液的制备：向1-2份卤胺前置体四甲基呱啶醇中加入9-10份甲苯，升温至88-92℃磁力搅拌溶解，滴加3-4份交联剂KH560，边滴加边搅拌，滴加0.7-0.8份三乙胺，升温至135-145℃反应23-25h后，在54-56℃下减压蒸馏除去甲苯溶剂，加入去离子水搅拌溶解，得到质量分数为5%的接枝溶液；水溶性卤胺前置体为2,2,6,6-四甲基-4-呱啶醇。
进一步的，步骤（3）中棉纤维的氨基化改性：按浴比1:30将1/3的权1步骤（1）中所得预处理棉纤维浸渍于浓度为2g/L的高碘酸钠水溶液中，在40-43℃下避光震荡20-30min后，用大量去离子水洗涤，再按浴比1:50浸渍于5g/L的端氨基超支化聚合物HBP-NH2水溶液中，室温下震荡55-60min后，多次水洗，室温下晾干，制得氨基化棉纤维。
进一步的，步骤（4）中棉纤维-聚苯胺的原位聚合：向1/3的权1步骤（1）中所得预处理棉纤维中1:500加入蒸馏水，剧烈搅拌直至分散完全，加入1mol/L的盐酸和0.5mL苯胺，低速搅拌，滴加浓度为2%的过硫酸铵水溶液，机械搅拌23-24h得到聚合产物，真空抽滤分离掉上层清液，多次冲洗直至滤液澄清，真空干燥得到棉纤维-聚苯胺复合材料。
进一步的，步骤（4）中接枝水溶性卤胺前置体的棉纤维的氯化：
向浓度为1%的次氯酸钠溶液中滴加盐酸溶液（4mol/L）调节pH为7.5，将接枝水溶性卤胺前置体的棉纤维在其中浸泡40-45min后，用去离子水冲洗多次，最后于44-46℃鼓风干燥箱内干燥1-2h。
本发明相比现有技术具有以下优点：
（1）利用氢氧化钠-尿素水体系对棉纤维进行预处理，可有效降低纤维素的结晶度，提高其反应活性，促进其进一步应用；对棉纤维进行适度预处理并抑制其溶解，随着预处理程度的加深，纤维的润胀性能逐渐增加，而平均聚合度逐渐减小；纤维的表面形貌被逐渐破坏，表面的微细纤维不断减少，扭曲和弯折程度也不断增力。
（2）利用交联剂KH560，采用浸渍-干燥-固化的方法将水溶性卤胺前置体（2,2,6,6-四甲基-4-呱啶醇）接枝到预处理棉纤维上，通过次氯酸钠漂白溶液的浸泡氯化制备出具有抗菌功效的棉纤维，并表现出非常好的耐洗性和稳定性。
（3）通过氧化活化棉纤维并接枝端氨基超支化聚合物制备了氨基化改性棉纤维，利用改性棉纤维中丰富氨基对银离子的络合、还原作用原位控制生成纳米银，实现了对棉织物的高效抗菌整理；氨基化棉纤维原位生成的纳米银粒径小，且氨
基化棉纤维整理后纳米银的耐洗牢度较高。
（4）以棉纤维为模板，采用原位聚合的方法制备出棉纤维-聚苯胺复合材料，
再通过物理吸附四氧化三铁纳米颗粒，得到电磁改性的棉纤维复合吸波材料，吸波性能好；HCl掺杂的聚苯胺能够均匀包覆在棉纤维的表面，磁性复合材料保持了棉纤维的原有结构，使得磁性复合材料可以吸收电磁波；
将磁性棉纤维-聚苯胺复合材料与所得氯化的接枝水溶性卤胺前置体的棉纤维、纳米银原位生成整理的氨基化棉纤维进行混纺，制作家居用品，具有良好的长效抗菌能力和耐洗性，且能吸收来自于家用电器的电磁波辐射。
具体实施方式
实施例1
一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法，其特征在于，包括如下步骤：
（1）氢氧化钠-尿素水体系预处理棉纤维的工艺：
向质量比为8:14的氢氧化钠和尿素中加入水，搅拌20min溶解均匀，放入低温恒温水浴锅中预冷至-4℃，加入棉纤维搅拌预处理，用100目的滤袋过滤，用蒸溜水洗涤至滤水呈中性，均分成3份待用；
（2）棉纤维接枝水溶性卤胺前置体：
将1/3的（1）中所得预处理棉纤维浸泡在接枝溶液中15min浸湿，然后在78-82℃鼓风干燥箱中干燥固化1h，再浸泡于0.5%的洗涤剂中15min，用去离子水冲洗后放入65-70℃的真空干燥箱中干燥1h；
（3）氨基化棉纤维的纳米银原位生成整理：
按浴比1:50将氨基化棉纤维浸渍于0.1 mol/L的硝酸银水溶液中，在96-98℃下搅拌1min后水洗，常温晾干；
（4）家居用品的制备：
将四氧化三铁纳米颗粒与棉纤维-聚苯胺复合材料按质量比1:1加入到无水乙醇中，超声分散完全，机械搅拌3h得磁性棉纤维-聚苯胺复合材料；
将其与所得氯化的接枝水溶性卤胺前置体的棉纤维、纳米银原位生成整理的氨基化棉纤维进行混纺，得到所述家居用品。
进一步的，步骤（2）中接枝溶液的制备：向1份卤胺前置体四甲基呱啶醇中加入9份甲苯，升温至88-92℃磁力搅拌溶解，滴加3份交联剂KH560，边滴加边搅拌，滴加0.7份三乙胺，升温至135-145℃反应23h后，在54-56℃下减压蒸馏除去甲苯溶剂，加入去离子水搅拌溶解，得到质量分数为5%的接枝溶液；水溶性卤胺前置体为2,2,6,6-四甲基-4-呱啶醇。
进一步的，步骤（3）中棉纤维的氨基化改性：按浴比1:30将1/3的权1步骤（1）中所得预处理棉纤维浸渍于浓度为2g/L的高碘酸钠水溶液中，在40-43℃下避光震荡20min后，用大量去离子水洗涤，再按浴比1:50浸渍于5g/L的端氨基超支化聚合物HBP-NH2水溶液中，室温下震荡55min后，多次水洗，室温下晾干，制得氨基化棉纤维。
进一步的，步骤（4）中棉纤维-聚苯胺的原位聚合：向1/3的权1步骤（1）中所得预处理棉纤维中1:500加入蒸馏水，剧烈搅拌直至分散完全，加入1mol/L的盐酸和0.5mL苯胺，低速搅拌，滴加浓度为2%的过硫酸铵水溶液，机械搅拌23h得到聚合产物，真空抽滤分离掉上层清液，多次冲洗直至滤液澄清，真空干燥得到棉纤维-聚苯胺复合材料。
进一步的，步骤（4）中接枝水溶性卤胺前置体的棉纤维的氯化：
向浓度为1%的次氯酸钠溶液中滴加盐酸溶液（4mol/L）调节pH为7.5，将接枝水溶性卤胺前置体的棉纤维在其中浸泡40min后，用去离子水冲洗多次，最后于44-46℃鼓风干燥箱内干燥1h。
实施例2
一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法，其特征在于，包括如下步骤：
（1）氢氧化钠-尿素水体系预处理棉纤维的工艺：
向质量比为8:14的氢氧化钠和尿素中加入水，搅拌25min溶解均匀，放入低温恒温水浴锅中预冷至-4℃，加入棉纤维搅拌预处理，用100目的滤袋过滤，用蒸溜水洗涤至滤水呈中性，均分成3份待用；
（2）棉纤维接枝水溶性卤胺前置体：
将1/3的（1）中所得预处理棉纤维浸泡在接枝溶液中20min浸湿，然后在78-82℃鼓风干燥箱中干燥固化2h，再浸泡于0.5%的洗涤剂中20min，用去离子水冲洗后放入65-70℃的真空干燥箱中干燥2h；
（3）氨基化棉纤维的纳米银原位生成整理：
按浴比1:50将氨基化棉纤维浸渍于0.1 mol/L的硝酸银水溶液中，在96-98℃下搅拌2min后水洗，常温晾干；
（4）家居用品的制备：
将四氧化三铁纳米颗粒与棉纤维-聚苯胺复合材料按质量比1:1加入到无水乙醇中，超声分散完全，机械搅拌4h得磁性棉纤维-聚苯胺复合材料；
将其与所得氯化的接枝水溶性卤胺前置体的棉纤维、纳米银原位生成整理的氨基化棉纤维进行混纺，得到所述家居用品。
进一步的，步骤（2）中接枝溶液的制备：向2份卤胺前置体四甲基呱啶醇中加入10份甲苯，升温至88-92℃磁力搅拌溶解，滴加4份交联剂KH560，边滴加边搅拌，滴加0.8份三乙胺，升温至135-145℃反应25h后，在54-56℃下减压蒸馏除去甲苯溶剂，加入去离子水搅拌溶解，得到质量分数为5%的接枝溶液；水溶性卤胺前置体为2,2,6,6-四甲基-4-呱啶醇。
进一步的，步骤（3）中棉纤维的氨基化改性：按浴比1:30将1/3的权1步骤（1）中所得预处理棉纤维浸渍于浓度为2g/L的高碘酸钠水溶液中，在40-43℃下避光震荡30min后，用大量去离子水洗涤，再按浴比1:50浸渍于5g/L的端氨基超支化聚合物HBP-NH2水溶液中，室温下震荡60min后，多次水洗，室温下晾干，制得氨基化棉纤维。
进一步的，步骤（4）中棉纤维-聚苯胺的原位聚合：向1/3的权1步骤（1）中所得预处理棉纤维中1:500加入蒸馏水，剧烈搅拌直至分散完全，加入1mol/L的盐酸和0.5mL苯胺，低速搅拌，滴加浓度为2%的过硫酸铵水溶液，机械搅拌24h得到聚合产物，真空抽滤分离掉上层清液，多次冲洗直至滤液澄清，真空干燥得到棉纤维-聚苯胺复合材料。
进一步的，步骤（4）中接枝水溶性卤胺前置体的棉纤维的氯化：
向浓度为1%的次氯酸钠溶液中滴加盐酸溶液（4mol/L）调节pH为7.5，将接枝水溶性卤胺前置体的棉纤维在其中浸泡45min后，用去离子水冲洗多次，最后于44-46℃鼓风干燥箱内干燥2h。
按照本发明方法制作的家居用品，具有良好的长效抗菌能力、耐洗性和稳定性，且能吸收来自于家用电器的电磁波辐射；对金黄色葡萄球菌和大肠杆菌的抑菌率为99.99%以上，经多次强力洗涤后对金黄色葡萄球菌和大肠杆菌任具有99%以上的抗菌率。
Claims (5)
1.一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法，其特征在于，包括如下步骤：
（1）氢氧化钠-尿素水体系预处理棉纤维的工艺：
向质量比为8:14的氢氧化钠和尿素中加入水，搅拌20-25min溶解均匀，放入低温恒温水浴锅中预冷至-4℃，加入棉纤维搅拌预处理，用100目的滤袋过滤，用蒸溜水洗涤至滤水呈中性，均分成3份待用；
（2）棉纤维接枝水溶性卤胺前置体：
将1/3的（1）中所得预处理棉纤维浸泡在接枝溶液中15-20min浸湿，然后在78-82℃鼓风干燥箱中干燥固化1-2h，再浸泡于0.5%的洗涤剂中15-20min，用去离子水冲洗后放入65-70℃的真空干燥箱中干燥1-2h；
（3）氨基化棉纤维的纳米银原位生成整理：
按浴比1:50将氨基化棉纤维浸渍于0.1 mol/L的硝酸银水溶液中，在96-98℃下搅拌1-2min后水洗，常温晾干；
（4）家居用品的制备：
将四氧化三铁纳米颗粒与棉纤维-聚苯胺复合材料按质量比1:1加入到无水乙醇中，超声分散完全，机械搅拌3-4h得磁性棉纤维-聚苯胺复合材料；
将其与所得氯化的接枝水溶性卤胺前置体的棉纤维、纳米银原位生成整理的氨基化棉纤维进行混纺，得到所述家居用品。
2.根据权利要求1所述的一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法，其特征在于，步骤（2）中接枝溶液的制备：
向1-2份卤胺前置体四甲基呱啶醇中加入9-10份甲苯，升温至88-92℃磁力搅拌溶解，滴加3-4份交联剂KH560，边滴加边搅拌，滴加0.7-0.8份三乙胺，升温至135-145℃反应23-25h后，在54-56℃下减压蒸馏除去甲苯溶剂，加入去离子水搅拌溶解，得到质量分数为5%的接枝溶液；
水溶性卤胺前置体为2,2,6,6-四甲基-4-呱啶醇。
3.根据权利要求1所述的一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法，其特征在于，步骤（3）中棉纤维的氨基化改性：
按浴比1:30将1/3的权1步骤（1）中所得预处理棉纤维浸渍于浓度为2g/L的高碘酸钠水溶液中，在40-43℃下避光震荡20-30min后，用大量去离子水洗涤，再按浴比1:50浸渍于5g/L的端氨基超支化聚合物HBP-NH2水溶液中，室温下震荡55-60min后，多次水洗，室温下晾干，制得氨基化棉纤维。
4.根据权利要求1所述的一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法，其特征在于，步骤（4）中棉纤维-聚苯胺的原位聚合：
向1/3的权1步骤（1）中所得预处理棉纤维中1:500加入蒸馏水，剧烈搅拌直至分散完全，加入1mol/L的盐酸和0.5mL苯胺，低速搅拌，滴加浓度为2%的过硫酸铵水溶液，机械搅拌23-24h得到聚合产物，真空抽滤分离掉上层清液，多次冲洗直至滤液澄清，真空干燥得到棉纤维-聚苯胺复合材料。
5.根据权利要求1所述的一种用卤胺-氨基化复合改性棉纤维制作长效抗菌家居用品的方法，其特征在于，步骤（4）中接枝水溶性卤胺前置体的棉纤维的氯化：
向浓度为1%的次氯酸钠溶液中滴加盐酸溶液（4mol/L）调节pH为7.5，将接枝水溶性卤胺前置体的棉纤维在其中浸泡40-45min后，用去离子水冲洗多次，最后于44-46℃鼓风干燥箱内干燥1-2h。
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| CN112962316A (zh) * | 2021-02-04 | 2021-06-15 | 刘娇 | 一种导电安全面料及其制备方法 |
| CN113684688A (zh) * | 2021-09-14 | 2021-11-23 | 佛山市海邦纺织有限公司 | 一种吸湿速干抗菌棉面料的制备方法 |
| CN115323786A (zh) * | 2022-08-22 | 2022-11-11 | 东莞市日东智能装备有限公司 | 一种免缝高抗菌窗帘及其加工工艺 |
| CN116536919A (zh) * | 2023-04-25 | 2023-08-04 | 南通明富纺织品有限公司 | 一种抗菌保暖型色织布及其制备工艺 |
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