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CN106146835B - 一种高分子季铵盐抗菌剂制备方法及应用 - Google Patents

一种高分子季铵盐抗菌剂制备方法及应用 Download PDF

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CN106146835B
CN106146835B CN201610552012.4A CN201610552012A CN106146835B CN 106146835 B CN106146835 B CN 106146835B CN 201610552012 A CN201610552012 A CN 201610552012A CN 106146835 B CN106146835 B CN 106146835B
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polyethyleneimine
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CN106146835A (zh
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徐福建
罗旭
胡杨
李杨
张桢焱
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Sichuan Daofang Traditional Chinese Medicine Development Co ltd
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Abstract

一种高分子季铵盐抗菌剂制备方法及应用，属于抗菌剂技术领域。该抗菌剂是由大分子量的聚乙烯亚胺(b‑PEI)与短链卤代烷进行季铵化反应制得。根据本发明所述方法制备的高分子季铵盐抗菌剂具有高效、持久、广谱的抗菌性能，同时具有安全性高，制备工艺简单等优点，可以作为抗菌添加剂，在医疗、卫生及环保领域具有潜在的商业应用前景。

Description

一种高分子季铵盐抗菌剂制备方法及应用
技术领域
本发明涉及一种高分子季铵盐抗菌剂、制备方法及应用，属于抗菌剂技术领域。
背景技术
近年来，随着科技的发展和人们生活水平的提高，人们对卫生和健康的要求越来越高，人们开始越来越关注高性能抗菌剂的开发和应用。
抗菌剂目前的种类繁多，其品种可分为三大类：无机抗菌剂，有机抗菌剂和天然抗菌剂。目前用于水体或医用消毒的杀菌剂大多为小分子物质，小分子杀菌剂不仅会残留余毒，抗菌时效短，而且会造成环境污染。而有机高分子抗菌剂具备抗菌性能持久、不挥发、不会渗入人或动物表皮等特点，已经成为抗菌剂领域的研究热点。中国专利CN 102870781 A制备了一种咪唑盐类高分子抗菌剂；中国专利CN 200910144560.3公开了一种胍盐类高分子抗菌剂；中国专利CN 105111356 A制备了一种水性生态合成革用高分子抗菌剂。但是这些抗菌剂制备工艺普遍比较复杂，热稳定性和加工性能较差，成本较高，使其难以大规模应用聚乙烯亚胺(PEI)是一种水溶性聚胺，分子链中拥有大量的胺基N原子。聚乙烯亚胺作为一种水溶性功能大分子，其特性引起国内外研究人员的广泛关注，目前已广泛应用于生物医学领域，如生物传感器的构建、药物释放、酶的固定、生物大分子的分离与纯化等多个方面都有应用。本发明通过一步法实现了对功能大分子聚乙烯亚胺的季铵化改性，制备出了具有强效抗菌性的高分子抗菌剂，工艺简单，成本低廉，易于实现大规模工业化生产。
发明内容
针对现有技术的不足，本发明提供了一种抗菌性能优异、工艺简单、成本低廉的高分子季铵盐抗菌剂及其制备方法。
为实现上述目的，本发明所采用的技术方案如下：
一种高分子季铵盐抗菌剂的制备方法，其特征在于：将短链卤代烷溶解于四氢呋喃中，将大分子量的聚乙烯亚胺溶解于四氢呋喃中；将两种溶液混合，控制聚乙烯亚胺上胺基与卤代烷的摩尔比为1.5:1～5:1，在50～65℃反应10～50h。
作为本发明的优选的实施方案，所述的聚乙烯亚胺为支化型聚乙烯亚胺，分子量为5000～40000g/mol。
作为本发明的优选的实施方案，所述的短链卤代烃可以是溴或者碘取代的C1～C6的烷烃，优选为单取代。
本发明的方法制备得到的高分子季铵盐抗菌剂作为广谱抗菌剂剂应用，用于大肠杆菌、金黄色葡萄球菌等多种细菌的抑菌杀菌剂。
与现有技术相比，本发明具有如下优点：
1.本发明提供了一种高分子季铵盐抗菌剂及其制备方法，该高分子季铵盐抗菌剂具有抗挥发与低残留毒性，大分子链具有大量的抗菌基团和良好的亲水性，使其具有优异的抗菌性能。
2.本发明提供了一种高分子季铵盐抗菌剂及其制备方法，本发明通过一步法实现了对功能大分子聚乙烯亚胺的季铵化改性，制备出了具有强效抗菌性的高分子抗菌剂，工艺简单，成本低廉，易于实现大规模工业化生产。
3.本发明提供的高分子季铵盐抗菌剂，制备工艺简单，稳定性较好，对大肠杆菌和金黄色葡萄球菌等多种细菌都具有良好的抑菌杀菌性。
附图说明
图1高分子季铵盐抗菌剂的抑菌效果图。
具体实施方式
下面通过实施例来进一步说明本发明，但并不局限于以下的实施例。在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，但凡在本发明的精神和原则之内，这些等价形式的改动、修改等均应包含在本发明的保护范围之内。
实施例1：
将1g聚乙烯亚胺溶于5mL四氢呋喃中，将2mL短链卤代烃1(溴己烷)溶于5mL四氢呋喃中。将聚乙烯亚胺溶液滴加到溴己烷溶液当中。维持50℃搅拌24h。反应结束后，乙醚沉淀产物，最后经过减压干燥得到季铵化的聚乙烯亚胺1。
实施例2：
将1g聚乙烯亚胺溶于5mL四氢呋喃中，将4mL短链卤代烃2(碘甲烷)溶于5mL四氢呋喃中。将聚乙烯亚胺溶液滴加到碘甲烷溶液当中，维持50℃搅拌24h。反应结束后，旋转蒸发除去溶剂四氢呋喃和未反应的碘甲烷，最后经过减压干燥得到季铵化的聚乙烯亚胺2。
实验例3：
本发明实施例1所制备的抗菌剂(季铵化的聚乙烯亚胺1)进行菌液共培养抑菌实验。检测用菌为大肠杆菌ATCC 25922。本实验采用等倍浓度稀释法测定最小抑菌浓度。具体方法如下：将待测材料溶解在去离子水中，最初浓度为4096μg/mL。然后，在96孔板中等倍稀释至1μg/mL。实验组中，每孔加入70μg不同浓度的抗菌材料。对照组中加入70μg的去离子水。将培养好的大肠杆菌在培养基里稀释至约2×106CFU/mL，随后，向实验组和对照组的每个孔中各加入70μg含菌的培养基。将96孔板在37℃下轻微震荡培养20h，然后用酶标仪读取各个孔在600nm处的吸收光强，吸收光强与对照组最接近的孔所对应的最大浓度即为最小抑菌浓度。结果示于图1。
实验例4
本发明实施例1所制备的抗菌剂(季铵化的聚乙烯亚胺1)和实施例2所制备的抗菌剂,进行菌液共培养抑菌实验，采用等倍浓度稀释法测定最小抑菌浓度，检测用菌为金黄色葡萄球菌。结果示于表1。
表1 季铵化的聚乙烯亚胺1和季铵化的聚乙烯亚胺2的抑菌结果

Claims (1)

1.一种高分子季铵盐抗菌剂的制备方法，其特征在于：将1g聚乙烯亚胺溶于5mL四氢呋喃中，将4mL短链卤代烃碘甲烷溶于5mL四氢呋喃中；将聚乙烯亚胺溶液滴加到碘甲烷溶液当中，维持50℃搅拌24h；反应结束后，旋转蒸发除去溶剂四氢呋喃和未反应的碘甲烷，最后经过减压干燥得到季铵化的聚乙烯亚胺；聚乙烯亚胺为支化型聚乙烯亚胺，分子量为5000～40000g/mol。
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CN109503834A (zh) * 2018-11-14 2019-03-22 北京化工大学 一种长链烷烃季铵化抗菌剂的制备方法及其产品和应用
CN109730964B (zh) * 2019-01-31 2022-04-26 四川大学 一种微环境响应型交联季铵盐胶束抗菌剂及其制备方法和应用
CN111763329A (zh) * 2020-05-25 2020-10-13 上海麟定生物科技有限公司 季铵化聚乙烯亚胺修饰的石墨烯量子点、制备方法及应用
CN111849328A (zh) * 2020-07-09 2020-10-30 绍兴百立盛新材料科技有限公司 一种抗病毒性透湿涂料的制备方法及应用
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CN118530682B (zh) * 2024-05-29 2025-08-26 广州市豪使特粘胶有限公司 一种耐候性抗菌粘合剂及其制备方法

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