CN106436322A - 一种家纺面料用抗菌整理剂的制备方法 - Google Patents
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Abstract
本发明涉及了一种家纺面料用抗菌整理剂的制备方法，向反应釜中加入表面改性纳米氧化锌粉末、乳化剂、去离子水，升温至70℃；缓慢地向反应釜中滴加1‑丁基‑3‑乙烯基咪唑硝酸盐、3‑乙烯基苯胺和引发剂水溶液，滴加完后，在78℃保温反应3h，将反应釜温度降至45～50℃，加入0.3份硝酸银与20份去离子水的溶液，搅拌均匀后，迅速加入0.3份硼氢化钠与20份去离子水的溶液，进行还原反应；过200目筛，得家纺面料用抗菌整理剂。本发明采用咪唑单体在改性后的纳米二氧化钛离子表面接枝的方法，使咪唑限制在基体中，将无机和有机抗菌剂进行复合，实现了抗菌剂的安全、持久、高效性。
Description
技术领域
本发明涉及一种家纺面料用抗菌整理剂的制备方法，尤其是一种家纺面料用抗菌整理剂，属于纺织品助剂领域
背景技术
家纺面料用抗菌剂按其成分可大致分为天然生物类、有机类和无机类三大类抗菌剂。
天然生物类抗菌剂有来源于虾、蟹壳的脱乙酞甲壳质，也有中草药、银杏、江南竹、日芥子等的萃取液，以天然原材料作为抗菌剂，受到原料来源和加工条件的制约，目前还不能实现大规模生产。
有机抗菌剂主要是有机酸、酯、醇、酚等物质。有机抗菌剂用于抗菌的历史较长，但是其耐热性，稳定性较差，其分解产物和挥发物可能对人体有害，因而应用受到限制。对细菌抑制作用较强的无机抗菌剂脱颖而出。
目前无机抗菌剂通常是由具有抗菌活性的金属离子和载体组成的体系。与有机抗菌剂相比，它具有较好的耐热性和安全性，而且资源丰富，应用范围广，是纤维、塑料、建材等生活制品最适宜的抗菌剂品种，有望替代有机抗菌剂。纳米材料是近年来新问世的一种高新材料，这类材料因其所特有的小尺寸效应、表面效应、量子尺寸效应、量子隧道效应等特性，从而拥有完全不同于常规材料的奇特的力学性能、光学性能、热学性能、磁学性能、催化性能等。因此，纳米材料将成为下一代新材料的基础。
近年来，以氧化锌为代表的光催化材料得到了广泛的研究，由于纳米氧化锌光催化复合材料应用技术和工艺简单，成本低廉，利用自然光即可催化分解细菌和污染物，具有高催化活性、良好的化学稳定性和热稳定性、无二次污染、无刺激性、安全无毒等特点，能长期有益于自然生态环境，所以是最具有开发前景的绿色环保纳米材料之一。但其使用受光源限制。
因而，研究开发不受光源限制、本身无毒、没有二次污染危险的含纳米氧化锌光催化复合抗菌剂，具有较大应用意义。
发明内容
针对现有抗菌剂的不足，本发明所要解决的技术问题是提供一种家纺面料用抗菌整理剂的制备方法，尤其是以纳米氧化锌、咪唑类抗菌单体为主要抗菌剂组分，采用聚合方法制备家纺面料用抗菌整理剂，将咪唑类抗菌剂接枝到纳米氧化锌上，使咪唑类抗菌剂限制在基体中，既克服了咪唑类抗菌剂作为有机抗菌剂存在的缺陷，又提高抗菌剂的抗菌长效性和有效性。
为实现上述目的，本发明采用的技术方案为：
一种家纺面料用抗菌整理剂的制备方法，各组分以质量份计，包括以下步骤：
步骤一 向反应釜中加入8份表面改性纳米氧化锌粉末、7份十六烷基三甲基溴化铵、5份OP-10、243份去离子水，搅拌均匀，升温至70℃；以20份去离子水溶解0.3份过硫酸钠成引发剂水溶液；
步骤二 缓慢地向反应釜中滴加23份咪唑抗菌单体1-丁基-3-乙烯基咪唑硝酸盐、4份3-乙烯基苯胺和引发剂水溶液，滴加完后，在78℃保温反应3h，
步骤三 将反应釜温度降至45～50℃，加入0.3份硝酸银与20份去离子水的溶液，搅拌均匀后，迅速加入0.3份硼氢化钠与20份去离子水的溶液，进行还原反应；过200目筛，得家纺面料用抗菌整理剂。
所述表面改性纳米氧化锌的制备方法为：
7份纳米氧化锌加到盛有30份无水乙醇和10份水的广口瓶中，超声分散30分钟，升温至40℃，恒温匀速搅拌30分钟，盐酸调节pH值5.5，待搅拌稳定后通过滴管从瓶口加入由20份无水乙醇溶解的0.5～1.2份硅烷偶联剂γ-(甲基丙烯酰氧)丙基三甲氧基硅烷，反应1小时后，取出过滤、洗涤、烘干、研磨，制得表面改性纳米氧化锌粉末。
氧化锌因其全新的纳米特性体现出许多新的物理化学性能，使它在众多领域表现出巨大的应用前景。但由于纳米氧化锌的小尺寸效应、表面效应等使其作为无机物直接添加到有机材料中有想当大的困难：①氧化锌表面亲水疏油，呈现极性，在材料中难于均匀分散；②颗粒具有较大的比表面积和较高的表面能，使它们极易团聚，不易在有机介质中分散，与聚合物配伍性能差，直接影响纳米氧化锌的实际功效。为了降低纳米氧化锌表面极性，消除表面高能势，提高纳米氧化锌在有机介质中的分散能力和亲和力，扩大其应用范围，需要对其进行表面改性。使用偶联剂对纳米氧化锌粉体进行改性的方法较为普遍。偶联剂是一种由亲水的极性基团和亲油的非极性基团两部分组成的双亲化合物，其分子中的亲水基团与纳米粉体表面的羟基反应，使纳米颗粒表面亲水性转变成亲油性，从而达到改善纳米粉体与有机相液体的相容性。
本发明采用咪唑类抗菌单体在改性后的纳米氧化锌离子表面接枝的方法，使咪唑类抗菌单体限制在基体中，并在分子链上生成纳米银，将无机和有机抗菌剂进行复合，克服了纳米氧化锌光触媒在光线暗处没有抗菌性和咪唑类抗菌剂安全性差、会产生微生物耐药性，化学稳定性差、耐热性差等缺点，实现了抗菌剂的安全、持久、高效性。
具体实施方法：
下列实施方案，仅是举例说明，不是仅有的，所以，一切在本发明范围内或是做与本发明相似的改变均包含于本发明之内。
实施例1
一种家纺面料用抗菌整理剂的制备方法，各组分以质量份计，包括以下步骤：
步骤一 向反应釜中加入8份表面改性纳米氧化锌粉末、7份十六烷基三甲基溴化铵、5份OP-10、243份去离子水，搅拌均匀，升温至70℃；以20份去离子水溶解0.3份过硫酸钠成引发剂水溶液；
步骤二 缓慢地向反应釜中滴加23份咪唑抗菌单体1-丁基-3-乙烯基咪唑硝酸盐、4份3-乙烯基苯胺和引发剂水溶液，滴加完后，在78℃保温反应3h，
步骤三 将反应釜温度降至45～50℃，加入0.3份硝酸银与20份去离子水的溶液，搅拌均匀后，迅速加入0.3份硼氢化钠与20份去离子水的溶液，进行还原反应；过200目筛，得家纺面料用抗菌整理剂。
所述表面改性纳米氧化锌的制备方法为：
7份纳米氧化锌加到盛有30份无水乙醇和10份水的广口瓶中，超声分散30分钟，升温至40℃，恒温匀速搅拌30分钟，盐酸调节pH值5.5，待搅拌稳定后通过滴管从瓶口加入由20份无水乙醇溶解的0.5～1.2份硅烷偶联剂γ-(甲基丙烯酰氧)丙基三甲氧基硅烷，反应1小时后，取出过滤、洗涤、烘干、研磨，制得表面改性纳米氧化锌粉末。
Claims (2)
1.一种家纺面料用抗菌整理剂的制备方法，其特征在于，各组分以质量份计，包括以下步骤：
步骤一 向反应釜中加入8份表面改性纳米氧化锌粉末、7份十六烷基三甲基溴化铵、5份OP-10、243份去离子水，搅拌均匀，升温至70℃；以20份去离子水溶解0.3份过硫酸钠成引发剂水溶液；
步骤二 缓慢地向反应釜中滴加23份咪唑抗菌单体1-丁基-3-乙烯基咪唑硝酸盐、4份3-乙烯基苯胺和引发剂水溶液，滴加完后，在78℃保温反应3h，
步骤三 将反应釜温度降至45～50℃，加入0.3份硝酸银与20份去离子水的溶液，搅拌均匀后，迅速加入0.3份硼氢化钠与20份去离子水的溶液，进行还原反应；过200目筛，得家纺面料用抗菌整理剂。
2.如权利要求1所述的一种家纺面料用抗菌整理剂，其特征在于：所述表面改性纳米氧化锌的制备方法为，
7份纳米氧化锌加到盛有30份无水乙醇和10份水的广口瓶中，超声分散30分钟，升温至40℃，恒温匀速搅拌30分钟，盐酸调节pH值5.5，待搅拌稳定后通过滴管从瓶口加入由20份无水乙醇溶解的0.5～1.2份硅烷偶联剂γ-(甲基丙烯酰氧)丙基三甲氧基硅烷，反应1小时后，取出过滤、洗涤、烘干、研磨，制得表面改性纳米氧化锌粉末。
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