CN107938328A - 一种纳米抑菌整理剂的制备方法 - Google Patents
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Abstract
一种纳米抑菌整理剂的制备方法，属于织物整理剂技术领域。包括以下步骤：取纳米二氧化硅、纳米氧化锌和纳米氧化钛溶于无水乙醇，然后加入硅烷偶联剂进行搅拌反应；取薰衣草、蒲公英和黄连分别进行热风干燥，干燥后将薰衣草、蒲公英和黄连分别粉碎后混匀，然后加入去离子水，加热回流，冷却离心后收集上清液；取甲基丙烯酸十二氟庚酯、苯乙烯、十二烷基苯磺酸钠和纳米铁加入搅拌后的混合液中超声分散；然后加入抗坏血酸和上清液，升温后进行搅拌反应；将搅拌均匀后的整理剂自然冷却，得抗菌整理剂。经过本发明制备得到的抑菌整理剂具备非常优异的抑菌性能。
Description
技术领域
本发明属于织物整理剂技术领域，具体涉及一种纳米抑菌整理剂的制备方法。
背景技术
整理，是印染加工进入市场的最后一道工序，因此，它的目的是消除前道工序所造成的不良影响，同时赋予织物新的功能，而使用整理剂则是增加功能的主要手段。近年来，随着人们生活水平的提高，消费观念的更新，市场管理的规范化，尤其是纺织品贸易的全球化，激烈的竞争使纺织品生产者不得不改进产品的性能来迎合市场，而且要“快速响应”，既要响应花色、款式，还要有特殊的品质，这样就促进了各种功能性整理剂的发展。例如：臭氧层出现空洞，使地面紫外光辐射量增加，因而刺激皮肤癌变，由此也就促使科技工作者研制成功了抗紫外光的整理剂。再者，新产品、新的工业技术要求新的整理剂。例如，抗静电剂的使用，则是因为合成纤维产量的上升而提出的，而集成电路芯片生产工人的服装，对抗静电效果的要求更高，从而也促进了抗静电剂的发展。环境保护，这是今年来又一个强有力的潮流，这是推动整理剂更新换代的主要力量之一，于是出现了一些环保整理剂，如无醛固色剂、无醛免烫整理剂等等。所有这些都促进了整理剂的发展，以适应市场的需求，满足消费者的需求。
抗菌整理剂主要可以分为无机、有机和天然三种。早期抗菌剂基本都属于有机系列，大多是含氮、硫、氯等元素的各类复杂化合物，其主要品种有：季铵盐类、双胍类、醇类、酚类、醛类、有机金属类、砒啶类、噻吩类等。该类抗菌剂短期杀菌效果好，但大多都有耐热稳定性差、寿命短等缺点。进入21世纪，尤其是近几年来，绿色消费观念的不断兴起，促进了适应环保要求的抗菌整理剂的发展，使越来越多的产品在其加工、应用及功能消失后均不会对人类健康和生态环境造成危害。由于天然抗菌剂资源丰富、生物可降解、吸收性能好，而无机纳米抗菌剂用量少、高效、安全无毒，因此，开发环境友好的无机纳米抗菌剂和天然抗菌剂，将会成为绿色抗菌剂的研究主题。然而现有的织物抗菌整理剂的抗菌效果并不理想。
发明内容
解决的技术问题：针对上述技术问题，本发明提供一种纳米抑菌整理剂的制备方法，能够很好的杀灭对人体和衣物有害的微生物。
技术方案：一种纳米抑菌整理剂的制备方法，所述制备方法包括以下步骤：
步骤一.称取3-5质量份纳米二氧化硅、1-2质量份纳米氧化锌和0.2-1质量份纳米氧化钛溶于40-50质量份无水乙醇，然后加入1.5-2.4质量份硅烷偶联剂，40-45℃温度、300-380r/min转速下搅拌反应2-3h；
步骤二.取3-6质量份薰衣草、5-8质量份蒲公英和0.5-1.5质量份黄连分别进行热风干燥5-10min，干燥温度为81-85℃，干燥后将薰衣草、蒲公英和黄连分别粉碎至50-100目，然后将粉碎后的薰衣草、蒲公英和黄连混匀后加入40-50质量份去离子水，在50-60℃温度下回流1-2h，然后将温度降至20-30℃，在6000-8000r/min转速下离心5-10min，收集上清液；
步骤三.取3-5质量份甲基丙烯酸十二氟庚酯、2-4质量份苯乙烯、1-2质量份十二烷基苯磺酸钠和0.1-0.3质量份纳米铁加入步骤一搅拌后的混合液中超声分散5-10min；
步骤四.向步骤三分散后的混合液中加入3-5质量份抗坏血酸和步骤二制备的上清液，然后在78-90℃温度下搅拌反应3-5h；
步骤五.将搅拌均匀后的整理剂自然冷却，得抗菌整理剂。
作为优选，所述步骤一中称取4质量份纳米二氧化硅、1.5质量份纳米氧化锌和0.5质量份纳米氧化钛溶于45质量份无水乙醇，然后加入2质量份硅烷偶联剂，40℃温度、350r/min转速下搅拌反应2.5h。
作为优选，所述步骤二中取4质量份薰衣草、6质量份蒲公英和1质量份黄连分别进行热风干燥10min，干燥温度为85℃，干燥后将薰衣草、蒲公英和黄连分别粉碎至50-100目，然后将粉碎后的薰衣草、蒲公英和黄连混匀后加入48质量份去离子水，在56℃温度下回流2h，然后将温度降至30℃，在7500r/min转速下离心10min，收集上清液。
作为优选，所述步骤三中取4质量份甲基丙烯酸十二氟庚酯、2质量份苯乙烯、1.2质量份十二烷基苯磺酸钠和0.15质量份纳米铁加入步骤一搅拌后的混合液中超声分散8min。
作为优选，所述步骤四中向步骤三分散后的混合液中加入4质量份抗坏血酸和步骤二制备的上清液，然后在80℃温度下搅拌反应5h。
有益效果：本发明所述纳米抑菌整理剂在纳米二氧化硅、纳米氧化锌和纳米氧化钛等纳米氧化物的基础上，还加入了蒲公英、薰衣草、黄连提取液，提高了织物的抑菌性能，本发明的抑菌整理剂在对金黄色葡萄球菌的抑菌率达到89.9-98.3％，高于大多数的抑菌整理剂的抑菌效果，肺炎伯雷氏菌的抑菌率为87.6-95.4％，同时对白色念珠菌的抑菌率也高达85.4-92.1％。
具体实施方式
实施例1
一种纳米抑菌整理剂的制备方法，所述制备方法包括以下步骤：
步骤一.称取3质量份纳米二氧化硅、1质量份纳米氧化锌和0.2质量份纳米氧化钛溶于40质量份无水乙醇，然后加入1.5质量份硅烷偶联剂，40℃温度、300r/min转速下搅拌反应2h；
步骤二.取3质量份薰衣草、5质量份蒲公英和0.5质量份黄连分别进行热风干燥5min，干燥温度为81℃，干燥后将薰衣草、蒲公英和黄连分别粉碎至50目，然后将粉碎后的薰衣草、蒲公英和黄连混匀后加入40质量份去离子水，在50℃温度下回流1h，然后将温度降至20℃，在6000r/min转速下离心5min，收集上清液；
步骤三.取3质量份甲基丙烯酸十二氟庚酯、2质量份苯乙烯、1质量份十二烷基苯磺酸钠和0.1质量份纳米铁加入步骤一搅拌后的混合液中超声分散5min；
步骤四.向步骤三分散后的混合液中加入3质量份抗坏血酸和步骤二制备的上清液，然后在78℃温度下搅拌反应3h；
步骤五.将搅拌均匀后的整理剂自然冷却，得抗菌整理剂。
实施例2
一种纳米抑菌整理剂的制备方法，所述制备方法包括以下步骤：
步骤一.称取5质量份纳米二氧化硅、2质量份纳米氧化锌和1质量份纳米氧化钛溶于50质量份无水乙醇，然后加入2.4质量份硅烷偶联剂，45℃温度、380r/min转速下搅拌反应3h；
步骤二.取6质量份薰衣草、8质量份蒲公英和1.5质量份黄连分别进行热风干燥10min，干燥温度为85℃，干燥后将薰衣草、蒲公英和黄连分别粉碎至100目，然后将粉碎后的薰衣草、蒲公英和黄连混匀后加入50质量份去离子水，在60℃温度下回流2h，然后将温度降至30℃，在8000r/min转速下离心10min，收集上清液；
步骤三.取5质量份甲基丙烯酸十二氟庚酯、4质量份苯乙烯、2质量份十二烷基苯磺酸钠和0.3质量份纳米铁加入步骤一搅拌后的混合液中超声分散10min；
步骤四.向步骤三分散后的混合液中加入5质量份抗坏血酸和步骤二制备的上清液，然后在90℃温度下搅拌反应5h；
步骤五.将搅拌均匀后的整理剂自然冷却，得抑菌整理剂。
实施例3
一种纳米抑菌整理剂的制备方法，所述制备方法包括以下步骤：
步骤一.称取4质量份纳米二氧化硅、1.5质量份纳米氧化锌和0.5质量份纳米氧化钛溶于45质量份无水乙醇，然后加入2质量份硅烷偶联剂，40℃温度、350r/min转速下搅拌反应2.5h；
步骤二.取4质量份薰衣草、6质量份蒲公英和1质量份黄连分别进行热风干燥10min，干燥温度为85℃，干燥后将薰衣草、蒲公英和黄连分别粉碎至50-100目，然后将粉碎后的薰衣草、蒲公英和黄连混匀后加入48质量份去离子水，在56℃温度下回流2h，然后将温度降至30℃，在7500r/min转速下离心10min，收集上清液；
步骤三.取4质量份甲基丙烯酸十二氟庚酯、2质量份苯乙烯、1.2质量份十二烷基苯磺酸钠和0.15质量份纳米铁加入步骤一搅拌后的混合液中超声分散8min；
步骤四.向步骤三分散后的混合液中加入4质量份抗坏血酸和步骤二制备的上清液，然后在80℃温度下搅拌反应5h；
步骤五.将搅拌均匀后的整理剂自然冷却，得抑菌整理剂。
对比例1
同实施例3，区别在于不添加纳米氧化锌和纳米氧化钛，具体制备方法如下：
步骤一.称取4质量份纳米二氧化硅溶于45质量份无水乙醇，然后加入2质量份硅烷偶联剂，40℃温度、350r/min转速下搅拌反应2.5h；
步骤二.取4质量份薰衣草、6质量份蒲公英和1质量份黄连分别进行热风干燥10min，干燥温度为85℃，干燥后将薰衣草、蒲公英和黄连分别粉碎至50-100目，然后将粉碎后的薰衣草、蒲公英和黄连混匀后加入48质量份去离子水，在56℃温度下回流2h，然后将温度降至30℃，在7500r/min转速下离心10min，收集上清液；
步骤三.取4质量份甲基丙烯酸十二氟庚酯、2质量份苯乙烯、1.2质量份十二烷基苯磺酸钠和0.15质量份纳米铁加入步骤一搅拌后的混合液中超声分散8min；
步骤四.向步骤三分散后的混合液中加入4质量份抗坏血酸和步骤二制备的上清液，然后在80℃温度下搅拌反应5h；
步骤五.将搅拌均匀后的整理剂自然冷却，得抑菌整理剂。
对比例2
同实施例3，区别在于将纳米铁替换成溴化铁，具体制备方法如下：
步骤一.称取4质量份纳米二氧化硅、1.5质量份纳米氧化锌和0.5质量份纳米氧化钛溶于45质量份无水乙醇，然后加入2质量份硅烷偶联剂，40℃温度、350r/min转速下搅拌反应2.5h；
步骤二.取4质量份薰衣草、6质量份蒲公英和1质量份黄连分别进行热风干燥10min，干燥温度为85℃，干燥后将薰衣草、蒲公英和黄连分别粉碎至50-100目，然后将粉碎后的薰衣草、蒲公英和黄连混匀后加入48质量份去离子水，在56℃温度下回流2h，然后将温度降至30℃，在7500r/min转速下离心10min，收集上清液；
步骤三.取4质量份甲基丙烯酸十二氟庚酯、2质量份苯乙烯、1.2质量份十二烷基苯磺酸钠和0.15质量份溴化铁加入步骤一搅拌后的混合液中超声分散8min；
步骤四.向步骤三分散后的混合液中加入4质量份抗坏血酸和步骤二制备的上清液，然后在80℃温度下搅拌反应5h；
步骤五.将搅拌均匀后的整理剂自然冷却，得抑菌整理剂。
将实施例1-3和对比例1-2制备的抑菌整理剂进行性能测试。具体测试方法如下：
将上述实施例1-3和对比例1-2中制备的抑菌整理剂取50kg分别倒入料槽中，棉白色布料宽幅160cm，长度20m，轧液率70-80％，车速50-60m/min，120℃干燥，170℃烘焙30s。
上述方法制备的纳米抑菌织物按照FZ/T73023-2006《抗菌针织品》洗涤方法洗涤50次后，对比前后样品色差小。采用GB/T21510-2008《纳米无机材料抗菌性能测试方法》中振荡法测定抗菌性能，接触时间24h，测试金黄色葡萄球菌(G+)，肺炎伯雷氏菌(G-)，白色念珠菌(真菌)等微生物抑菌率如下表，织物符合国家抗菌织物3A标准。
| 金黄色葡萄球菌/％ | 肺炎伯雷氏菌/％ | 白色念珠菌/％ | |
| 实施例1 | 89.9 | 87.6 | 85.4 |
| 实施例2 | 93.5 | 91.6 | 89.7 |
| 实施例3 | 98.3 | 95.4 | 92.1 |
| 对比例1 | 75.3 | 70.1 | 68.9 |
| 对比例2 | 78.5 | 76.3 | 72.9 |
实施例3的纳米抑菌织物对金黄色葡萄球菌的抑菌率达到98.3％，高于大多数的抑菌整理剂的抑菌效果，肺炎伯雷氏菌的抑菌率为95.4％，同时对白色念珠菌的抑菌率也高达92.1％。
Claims (5)
1.一种纳米抑菌整理剂的制备方法，其特征在于，所述制备方法包括以下步骤：
步骤一.称取3-5质量份纳米二氧化硅、1-2质量份纳米氧化锌和0.2-1质量份纳米氧化钛溶于40-50质量份无水乙醇，然后加入1.5-2.4质量份硅烷偶联剂，40-45℃温度、300-380r/min转速下搅拌反应2-3 h；
步骤二. 取3-6质量份薰衣草、5-8质量份蒲公英和0.5-1.5质量份黄连分别进行热风干燥5-10 min，干燥温度为81-85℃，干燥后将薰衣草、蒲公英和黄连分别粉碎至50-100目，然后将粉碎后的薰衣草、蒲公英和黄连混匀后加入40-50质量份去离子水，在50-60℃温度下回流1-2 h，然后将温度降至20-30℃，在6000-8000 r/min转速下离心5-10min，收集上清液；
步骤三. 取3-5质量份甲基丙烯酸十二氟庚酯、2-4质量份苯乙烯、1-2质量份十二烷基苯磺酸钠和0.1-0.3质量份纳米铁加入步骤一搅拌后的混合液中超声分散5-10 min；
步骤四. 向步骤三分散后的混合液中加入3-5质量份抗坏血酸和步骤二制备的上清液，然后在78-90℃温度下搅拌反应3-5 h；
步骤五.将搅拌均匀后的整理剂自然冷却，得抗菌整理剂。
2.根据权利要求1所述的一种纳米抑菌整理剂的制备方法，其特征在于，所述步骤一中称取4质量份纳米二氧化硅、1.5质量份纳米氧化锌和0.5质量份纳米氧化钛溶于45质量份无水乙醇，然后加入2质量份硅烷偶联剂，40℃温度、350 r/min转速下搅拌反应2.5 h。
3.根据权利要求1所述的一种纳米抑菌整理剂的制备方法，其特征在于，所述步骤二中取4质量份薰衣草、6质量份蒲公英和1质量份黄连分别进行热风干燥10 min，干燥温度为85℃，干燥后将薰衣草、蒲公英和黄连分别粉碎至50-100目，然后将粉碎后的薰衣草、蒲公英和黄连混匀后加入48质量份去离子水，在56℃温度下回流2 h，然后将温度降至30℃，在7500 r/min转速下离心10 min，收集上清液。
4.根据权利要求1所述的一种纳米抑菌整理剂的制备方法，其特征在于，所述步骤三中取4质量份甲基丙烯酸十二氟庚酯、2质量份苯乙烯、1.2质量份十二烷基苯磺酸钠和0.15质量份纳米铁加入步骤一搅拌后的混合液中超声分散8 min。
5.根据权利要求1所述的一种纳米抑菌整理剂的制备方法，其特征在于，所述步骤四中向步骤三分散后的混合液中加入4质量份抗坏血酸和步骤二制备的上清液，然后在80℃温度下搅拌反应5 h。
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| CN108823965A (zh) * | 2018-07-09 | 2018-11-16 | 合肥洁诺医疗用品有限公司 | 一种擦拭纸用改性无纺布的制备方法 |
| CN109957970A (zh) * | 2019-03-29 | 2019-07-02 | 苏州经贸职业技术学院 | 丝绸天然纳米功能整理剂的制备方法 |
| CN111454426A (zh) * | 2020-04-25 | 2020-07-28 | 泉州西米露新材料科技有限公司 | 环保可降解的芳香型聚氨酯发泡材料及其制备方法 |
| CN113684677A (zh) * | 2021-09-07 | 2021-11-23 | 广东职业技术学院 | 一种抗菌服装面料及其制备方法 |
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