CN110565375B - 一种酶促蛋白质纤维原位染色及抗菌整理的方法 - Google Patents

一种酶促蛋白质纤维原位染色及抗菌整理的方法 Download PDF

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CN110565375B
CN110565375B CN201910876679.3A CN201910876679A CN110565375B CN 110565375 B CN110565375 B CN 110565375B CN 201910876679 A CN201910876679 A CN 201910876679A CN 110565375 B CN110565375 B CN 110565375B
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王平
农叶琳
周舟
于蓉
丁书林
袁久刚
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Jiangnan University
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Abstract

本发明公开了一种酶促蛋白质纤维原位染色及抗菌整理的方法，先借助1‑乙基‑(3‑二甲基氨基丙基)碳二亚胺盐酸盐和N‑羟基琥珀酰亚胺，将含酚羟基的酪胺接枝到蛋白质纤维上；再借助于漆酶，催化蛋白质纤维大分子与苯胺类小分子接枝聚合，实现蛋白质纤维原位染色和抗菌整理。具体包括以下步骤：(1)蛋白质纤维表面接枝酪胺；(2)漆酶催化蛋白质纤维和苯胺类小分子接枝聚合。与蛋白质纤维酸性染料染色和化学法抗菌整理相比，本发明述及的方法具有酶催化效率高、反应条件缓和、蛋白质纤维染色深度和色牢度较高，且抗菌效果优良的优点。

Description

一种酶促蛋白质纤维原位染色及抗菌整理的方法
技术领域
本发明涉及一种酶促蛋白质纤维原位染色及抗菌整理的方法，属于生态染整加工技术领域。
背景技术
蛋白质纤维染色中常用的染料包括酸性染料、酸性媒介染料和酸性含媒染料等。酸性染料颜色鲜艳、匀染性好，但由于染料与纤维间氢键和范德华力较弱，故染物湿处理牢度低。与酸性染料相比，酸性媒介染料和酸性含媒染料染色中纤维制品染色深度和色牢度增加，但颜色鲜艳度不够，且酸性媒介染料染色中需添加金属媒染剂，不仅影响纺织品的安全性，还易产生环境污染，增加印染废水处理的负担。由此可见，上述三类酸性染料进行蛋白质纤维染色中均存在一定的不足。
蛋白质类纤维易成为细菌、霉菌等微生物的养分，使这类纺织品发生霉变，甚至可能转为疾病传播的载体。常用抗菌整理剂包括无机银离子类、有机季铵盐类和和天然高分子类等，采用的整理工艺多以浸渍、高温焙烘等方法进行。这些整理剂在赋予蛋白质纤维抗菌效果的同时，也部分存在着与纤维结合不牢固、高温焙烘中纤维强力受损或泛黄，整理废液污染环境等弊端。因此，需开发和应用反应条件缓和、抗菌整理效果好、纤维损伤较少的抗菌整理方法。
生物酶法具有安全、高效、专一和环境友好等优点，以酶法对蛋白质纤维进行染整加工，不仅能保持纤维原有的优良特性，且能赋予纤维制品特定的颜色外观和功能性。漆酶能催化氧化酚类(如儿茶素、丁香酸)或芳胺类小分子(如苯胺、对苯二胺)聚合，形成的大分子不仅有一定的颜色外观，且具有一定的功能性(如抗菌、抗氧化、导电等)。
蛋白质纤维大分子中含一定数量的酪氨酸，漆酶能催化氧化酪氨酸上的酚羟基，生成反应性较强的醌类活性基。这些醌类活性基不仅可引发蛋白质纤维分子间交联，而且也能与苯胺或对苯二胺小分子发生接枝聚合，形成与蛋白质纤维相连接的聚苯胺类大分子。聚苯胺类大分子不仅具有一定的色外观，也具有抗菌、抗氧化和导电效果，这为漆酶催化蛋白质纤维的原位染色及功能化整理提供了新方法。另一方面，由于蛋白质纤维分子中酪氨酸数量有限，且多数分布在由疏水性较强的丙氨酸和甘氨酸组成的大分子链中，这在一定程度上影响了漆酶对酪氨酸的可及度，降低了漆酶催化苯胺或对苯二胺与蛋白质纤维接枝聚合的效果。
根据上述情况，可以在蛋白质纤维上接枝含酚羟基的酪胺，旨在增加蛋白质纤维表面的酚羟基数量，提高蛋白质纤维的反应性。在此基础上，再借助漆酶，催化氧化蛋白质纤维上的酚羟基形成较多醌类活性基，不仅能促进蛋白质纤维分子间交联、苯胺类小分子自聚，而且能催化蛋白质纤维与苯胺类小分子的自由基发生接枝聚合(即：促使蛋白质纤维与聚苯胺类大分子通过共价键连接)，增加酶促蛋白质纤维原位染色和抗菌整理效果。
发明内容
发明目的：本发明的目的在于提供一种酶促蛋白质纤维原位染色及抗菌整理的方法，使用本发明不仅可在低温缓和条件下使蛋白质纤维着色，且纤维制品具有较好的抗菌效果。
技术方案：为解决上述技术问题，本发明提供如下技术方案：
一种酶促蛋白质纤维原位染色及抗菌整理的方法，先利用1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐和N-羟基琥珀酰亚胺，将含酚羟基的酪胺接枝到蛋白质纤维上；再利用漆酶催化蛋白质纤维大分子与苯胺类小分子接枝聚合，实现蛋白质纤维原位染色和抗菌整理。
一种酶促蛋白质纤维原位染色及抗菌整理的方法，包括如下步骤：
(1)蛋白质纤维表面接枝酪胺：将蛋白质纤维、酪胺、1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐和N-羟基琥珀酰亚胺同浴处理；反应后蛋白质纤维以去离子水在25～ 40℃清洗10～15分钟；
(2)漆酶催化蛋白质纤维和苯胺类小分子接枝聚合：经步骤(1)处理后的蛋白质纤维浸渍在苯胺类小分子溶液中，添加漆酶进行催化氧化和聚合反应；反应后将蛋白质纤维以去离子水在90～95℃清洗10～15分钟，然后50℃烘干；
步骤(1)中，所述反应处方为：酪胺5～20g/L，1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐2.5～5g/L，N-羟基琥珀酰亚胺2.5～5g/L，浴比1:20；反应条件：pH 5～7、温度25～40℃、时间4～24小时；所述蛋白质纤维包括真丝和羊毛。
步骤(2)中，所述反应处方组成为：苯胺类小分子1～4g/L，漆酶0.1～1U/mL，浴比1:20；反应条件：pH 4～5.5，温度25～50℃，时间8～12小时；所述苯胺类小分子包括苯胺和对苯二胺。
有益效果：
与蛋白质纤维酸性染料染色和化学法抗菌整理相比，本发明有以下优点：
(1)酶催化效率高，借助漆酶催化氧化苯胺类小分子聚合，同时实现蛋白质纤维与苯胺类小分子的自由基接枝聚合，具有专一性强和反应效率高的优点；
(2)反应条件缓和，在低温近中性条件下，借助酶法完成蛋白质纤维原位染色和抗菌整理，避免了采用常规酸性染料染色和化学法抗菌整理温度高、能耗大、且纤维易产生损伤的诸多弊端；
(3)染色效果和抗菌性能改善明显，以本发明述及的方法进行酶促蛋白质纤维处理，加工的蛋白质纤维制品染色深度和色牢度较高、抗菌效果优良。
具体实施方式
一种酶促蛋白质纤维原位染色及抗菌整理的方法，先借助1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐和N-羟基琥珀酰亚胺，将含酚羟基的酪胺接枝到蛋白质纤维上；再借助于漆酶，催化苯胺类小分子与蛋白质纤维大分子接枝聚合，实现蛋白质纤维原位染色和抗菌整理。具体实施例如下：
实施例1
选用真丝为原料的真丝织物进行处理：
(1)真丝表面接枝酪胺：将真丝、酪胺、1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐和N-羟基琥珀酰亚胺同浴处理；反应后真丝以去离子水在25℃清洗10分钟；
(2)漆酶催化真丝和苯胺接枝聚合：经步骤(1)处理后的真丝浸渍在苯胺溶液中，添加漆酶进行催化氧化和聚合反应；反应后将真丝以去离子水在90℃清洗10分钟，然后50℃烘干；
步骤(1)中，所述反应处方为：酪胺5g/L，1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐2.5g/L，N-羟基琥珀酰亚胺2.5g/L，浴比1:20；反应条件：pH 5、温度25℃、时间4小时；
步骤(2)中，所述反应处方组成为：苯胺1g/L，漆酶0.1U/mL，浴比1:20；反应条件：pH 4，温度25℃，时间8小时。
试样1：未经处理的真丝；
试样2：未经步骤(1)处理，仅经步骤(2)处理；
试样3：经步骤(1)、(2)处理。
采用分光测色仪测定试样的染色深度K/S，参照GB/T 3920-2008测定试样的湿摩擦牢度，参照GB/T 20944.3-2008测定试样对大肠杆菌的抑菌率。其中，试样1、试样2 和试样3的染色深度分别为0.25、12.1和15.8；试样2和试样3的湿摩擦牢度等级分别3级、4～5级；试样1、试样2和试样3的抑菌率为2.5％、68.5％和82.5％。
实施例2
选用羊毛为原料的羊毛织物进行处理：
(1)羊毛表面接枝酪胺：将羊毛织物、酪胺、1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐和N-羟基琥珀酰亚胺同浴处理；反应后羊毛织物以去离子水在25℃清洗10分钟；
(2)漆酶催化羊毛和对苯二胺接枝聚合：经步骤(1)处理后的羊毛织物浸渍在对苯二胺溶液中，添加漆酶进行催化氧化和聚合反应；反应后将羊毛织物以去离子水在90℃清洗10分钟，然后50℃烘干；
步骤(1)中，所述反应处方为：酪胺20g/L，1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐5g/L，N-羟基琥珀酰亚胺5g/L，浴比1:20；反应条件：pH 7、温度40℃、时间 24小时；
步骤(2)中，所述反应处方组成为：对苯二胺4g/L，漆酶1U/mL，浴比1:20；反应条件：pH 5.5，温度50℃，时间12小时。
试样4：未经处理的羊毛织物；
试样5：未经步骤(1)处理，仅经步骤(2)处理；
试样6：经步骤(1)、(2)处理。
采用分光测色仪测定试样的染色深度K/S，参照GB/T 3920-2008测定试样的湿摩擦牢度，参照GB/T 20944.3-2008测定试样对大肠杆菌的抑菌率。其中，试样4、试样5 和试样6的染色深度分别为0.85、26.2、29.5；试样5和试样6的湿摩擦牢度等级分别2～3级、4级；试样4、试样5和试样6的抑菌率为5.9％、75.5％和92.1％。
通过对实施例数据分析：
未经处理试样1和试样4的颜色较浅、抗菌率低于10％；
未经步骤(1)接枝酪胺处理，仅经步骤(2)处理的试样2和试样5的染色深度中等，湿摩擦牢度分别为3级和2～3级，抗菌率均低于80％；
经步骤(1)和(2)组合处理后，试样3和试样6染色深度K/S较高，湿摩擦牢度等级增加，抗菌率均高于80％，表明：接枝酪胺增加了蛋白质纤维中酚羟基的数量，提高了蛋白质纤维的反应性，促进了漆酶催化氧化蛋白质纤维与苯胺类小分子接枝聚合，使聚苯胺或聚苯二胺大分子能与蛋白质纤维通过共价键相连接，获得了较好的酶促原位染色和抗菌整理效果。
虽然本发明已以较佳实施例公开如上，但其并非用以限定本发明，任何熟悉此技术的人，在不脱离本发明的精神和范围内，都可做各种的改动与修饰，因此本发明的保护范围应该以权利要求书所界定的为准。

Claims (8)

1.一种酶促蛋白质纤维原位染色及抗菌整理的方法，其特征在于，先利用1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐和 N-羟基琥珀酰亚胺，将含酚羟基的酪胺接枝到蛋白质纤维上；再利用漆酶，催化蛋白质纤维大分子与苯胺类小分子接枝聚合，实现蛋白质纤维原位染色和抗菌整理。
2.根据权利要求1所述的酶促蛋白质纤维原位染色及抗菌整理的方法，其特征在于，包括如下步骤：
（1）蛋白质纤维表面接枝酪胺：将蛋白质纤维、酪胺、1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐和 N-羟基琥珀酰亚胺同浴处理；清洗；
（2）漆酶催化蛋白质纤维和苯胺类小分子接枝聚合：经步骤（1）处理后的蛋白质纤维浸渍在苯胺类小分子溶液中，添加漆酶进行催化氧化和聚合反应；清洗；烘干。
3.根据权利要求2所述的酶促蛋白质纤维原位染色及抗菌整理的方法，其特征在于，步骤（1）中，反应体系中配方如下：酪胺 5～20 g/L，1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐2.5～5 g/L， N-羟基琥珀酰亚胺 2.5～5 g/L，浴比1:20；
反应条件如下：pH 5～7、温度25～40℃、时间4～24 小时。
4.根据权利要求2所述的酶促蛋白质纤维原位染色及抗菌整理的方法，其特征在于，步骤（1）中，反应结束后蛋白质纤维在25～40℃去离子水中清洗10～15分钟。
5.根据权利要求1或2所述的酶促蛋白质纤维原位染色及抗菌整理的方法，其特征在于，所述的蛋白质纤维包括真丝、羊毛。
6.根据权利要求2所述的酶促蛋白质纤维原位染色及抗菌整理的方法，其特征在于，步骤（2）中，反应体系如下：苯胺类小分子 1～4 g/L，漆酶 0.1～1 U/mL，浴比1:20；反应条件如下：pH 4～5.5、温度25～50℃、时间8～12小时。
7.根据权利要求1、2或6所述的酶促蛋白质纤维原位染色及抗菌整理的方法，其特征在于，所述苯胺类小分子包括苯胺、对苯二胺。
8.根据权利要求2所述的酶促蛋白质纤维原位染色及抗菌整理的方法，其特征在于，步骤（2）中，反应结束后将蛋白质纤维在90～95℃去离子水中清洗10～15分钟。
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