CN106421873A - 一种功能性医用敷料及其制备方法 - Google Patents

一种功能性医用敷料及其制备方法 Download PDF

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CN106421873A
CN106421873A CN201611034732.8A CN201611034732A CN106421873A CN 106421873 A CN106421873 A CN 106421873A CN 201611034732 A CN201611034732 A CN 201611034732A CN 106421873 A CN106421873 A CN 106421873A
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medical dressing
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polyamino
monomer
silver
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史丙华
姜志华
何杰
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CHANGSHA HAIRUN BIOTECH Co Ltd
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Abstract

一种功能性医用敷料及其制备方法，其首先将多氨基单体以冰水浴冷却；然后用漏斗在氮气保护下向多氨基单体中滴加乙烯基单体和溶剂，滴加完毕后常温下反应4小时生成淡黄色中间体，将中间体放置到旋转蒸发仪上减压除去溶剂，再升温、减压、得到多氨基超支化聚合物；再在多氨基超支化聚合物中添加改性剂升温、减压、得到封闭空间网络结构聚酰胺树状大分子聚合物；接着在封闭空间网络结构聚酰胺树状大分子聚合物溶液中加入银离子化合物溶液使其络合还原得到稳定的纳米银溶液；最后将成卷纯棉无纺布或脱脂纱布通过盛有上述纳米银溶液的浸液槽，再经过压扎、热风烘干、裁切、包装、钴60辐照灭菌，即得。

Description

一种功能性医用敷料及其制备方法
技术领域
本发明涉及一种医疗用功能性敷料，特别是一种功能性医用敷料及其制备方法。
背景技术
医用敷料是暂时覆盖烧伤、溃疡、创伤等伤口的一类临床医用材料，其主要作用是控制伤口的渗出液及保护伤口免受细菌及尘粒等外源污染。
银纳米材料由于尺寸小、比表面积大，具有独特的光、电、磁、热、抗菌等性能，在化学检测、生物成像以及抗菌制剂等方面都有广泛的应用。纳米银具有极强的纳米活性，表现出超长的抗菌能力，在极低的浓度下即可杀灭常见的细菌、真菌、支原体等致病微生物。跟抗生素相比，纳米银具有杀菌作用不受PH值影响、广谱抗菌、无耐药性、效力持久、遇水杀菌力更强、安全环保等特点，是理想的抗菌材料，可广泛应用于众多行业。目前已用于抗菌织物，凝胶，抗菌原液，微粉等产品，并可广泛应用于妇科感染、浅部真菌感染、创伤护理、水处理、卫生材料、日用消费品等领域。由于它没有耐药性是极佳的抗生素的替代品，是一种安全天然的非抗生素类高效杀菌剂。
含银敷料是一种用于慢性难愈性伤口的理想、安全、经济的换药敷料。但市面大部分含银敷料由于银离子本身易氧化等特点从而使敷料本身易变色失去抑菌效果，及银释放不可控易导致银沉积且抑菌效果不持久。
发明内容
本发明所要解决的技术问题是，针对现有技术不足，提供一种不易氧化，不易变色，且银释放可控的功能性医用敷料及其制备方法。
为解决上述技术问题，本发明采用的技术方案是：一种功能性医用敷料的制备方法，其包括下列步骤：
1)将多氨基单体以冰水浴冷却到5－10℃；
2)用漏斗在氮气保护下向步骤1)得到的多氨基单体中滴加乙烯基单体和溶剂，滴加完毕后常温下反应4小时生成淡黄色中间体，将中间体放置到旋转蒸发仪上减压除去溶剂，再升温到120℃－140℃减压反应2－4小时得到多氨基超支化聚合物；
3)在多氨基超支化聚合物中添加改性剂升温到140－150℃继续减压反应1－4小时得到封闭空间网络结构聚酰胺树状大分子聚合物；
4)在封闭空间网络结构聚酰胺树状大分子聚合物中加入银离子化合物使其络合还原得到稳定的纳米银溶液；
5)将成卷纯棉无纺布或脱脂纱布以10－12m/min的速度通过盛有上述纳米银溶液的浸液槽，再经过压扎、110－120℃热风烘干、裁切、包装、钴60辐照灭菌，即得。
所述多氨基单体为二乙烯三胺、三乙烯四胺、四乙烯五胺或五乙烯六胺。
所述乙烯基单体为丙烯酸、丙烯酸甲酯、甲基丙烯酸甲酯或丙烯酸乙酯。
所述溶剂为甲醇、三氯甲烷、或N,N-二甲基甲酰胺。
所述银离子化合物为硝酸银、醋酸银。
所述改性剂为丁二酸酐、马来酸酐。
所述步骤2)中多氨基单体与乙烯基单体的摩尔比1:1-1:3，所述步骤3)中多氨基单体与改性剂的摩尔比1:0.1-1:1。
为解决上述技术问题，本发明还提供了一种上述方法制备的功能性医用敷料。
本发明通过设计合成一种阳离子类型的封闭空间网络结构聚酰胺树状大分子聚合物稳定的纳米银水溶液，再用其对材质为棉/麻基材(脱脂纱布、纯棉无纺布等)进行浸润，因棉/麻基材主要化学成分为纤维素，而纤维素含有大量的羟基等极性基团，其吸水后在水中产生电离，因此带上一定的负电荷，与阳离子类型的封闭空间网络结构聚酰胺树状大分子聚合物稳定的纳米银通过静电吸附使具有抑菌作用的纳米银紧密附着在棉/麻基材上而不容易脱色，同时其封闭空间网络结构使纳米银稳定释放保证敷料抑菌效果持久，然后再经过压扎、(100-150℃)烘干、裁切、灭菌(钴60灭菌或环氧乙烷灭菌)，即得到色泽均一亮丽、色牢度好不易脱色、抑菌效果好且持久、生物相容性好的敷料。
本发明工艺简单，适合工业化及连续生产；所得功能性敷料无需染色上色、色泽均一亮丽、色牢度好不易脱色；银离子逐步释放、避免银离子沉积、抑菌持久、且生物相容性好。
具体实施方式
实施例1：
称取103.2g二乙烯三胺置于500ml三口烧瓶中冰水浴冷却；用恒压漏斗在氮气保护下缓慢滴加87.0g丙烯酸甲酯和200ml甲醇的混合溶液，滴加完毕后常温下反应4小时生成淡黄色中间体，将上述中间体转移到茄形瓶中在旋转蒸发仪上减压除去甲醇，在升温到120℃减压反应4小时得到多氨基超支化聚合物，加入10g的丁二酸酐升温到140℃继续减压反应4小时得到封闭空间网络结构聚酰胺树状大分子聚合物。
将500ml质量分数为0.1％硝酸银溶液缓慢滴加到500ml质量分数为0.1％的上述聚酰胺树状大分子聚合物水溶液中，滴加完毕后在搅拌条件下将溶液加热到90℃再冷却至室温，即得到稳定的纳米银溶液。
将成卷脱脂纱布以10m/mim速度通过盛有以上纳米银溶液的浸液槽再经过压扎、120℃热风烘干、裁切、包装、钴60辐照灭菌即得到银含量1200ppm的金黄色功能性敷料。
实施例2：
称取51.6g二乙烯三胺置于250ml三口烧瓶中冰水浴冷却；用恒压漏斗在氮气保护下缓慢滴加43.0g丙烯酸甲酯和100ml甲醇的混合溶液，滴加完毕后常温下反应4小时生成淡黄色中间体，将上述中间单体转移到茄形瓶中在旋转蒸发仪上减压除去甲醇，再升温到140℃减压反应2小时得到多氨基超支化聚合物，加入10g的马来酸酐升温到150℃继续减压反应2小时得到封闭空间网络结构聚酰胺树状大分子聚合物。
将500ml质量分数为0.01％醋酸银溶液缓慢滴加到500ml质量分数为0.01％的上述聚酰胺树状大分子聚合物水溶液中，滴加完毕后在搅拌条件下将溶液加热至沸腾再冷却至室温，即得到稳定的纳米银溶液。
将成卷脱脂纱布以10m/mim速度通过盛有以上纳米银溶液的浸液槽再经过压扎、120℃热风烘干、裁切、包装、钴60辐照灭菌即得到银含量600ppm金黄色功能性敷料。
实施例3：
称取122.6g四乙烯五胺置于500ml三口烧瓶中冰水浴冷却；用恒压漏斗在氮气保护下缓慢滴加57.5g丙烯酸甲酯和200ml三氯甲烷的混合溶液，滴加完毕后常温下反应4小时生成淡黄色中间体，将上述中间单体转移到茄形瓶中在旋转蒸发仪上减压除去三氯甲烷，在升温到140℃减压反应2小时得到多氨基超支化聚合物，加入13.4g的丁二酸酐升温到150℃继续减压反应1小时得到封闭空间网络结构聚酰胺树状大分子聚合物。
将500ml质量分数为0.005％硝酸银溶液缓慢滴加到500ml质量分数为0.005％的上述聚酰胺树状大分子聚合物水溶液中，滴加完毕后将溶液常温反应48小时，即得到稳定的纳米银溶液。
将成卷纯棉无纺布以12m/mim速度通过盛有以上纳米银溶液的浸液槽再经过压扎、110℃热风烘干、裁切、包装、钴60辐照灭菌即得到银含量600ppm金黄色功能性敷料。
下面对实施例1－实施例3所得功能性敷料进行脱色及抑菌试验，得到实验结果如下：
表1实例中样品经过以下处理脱色情况
表2实例中样品经过纯化水浸泡不同时间后清洗烘干再测其抑菌效果

Claims (8)

1.一种功能性医用敷料的制备方法，其特征在于包括下列步骤：
1)将多氨基单体以冰水浴冷却到5－10℃；
2)用漏斗在氮气保护下向步骤1)得到的多氨基单体中滴加乙烯基单体和溶剂，滴加完毕后常温下反应4小时生成淡黄色中间体，将中间体放置到旋转蒸发仪上减压除去溶剂，再升温到120℃－140℃减压反应2－4小时得到多氨基超支化聚合物；
3)在多氨基超支化聚合物中添加改性剂升温到140－150℃继续减压反应1－4小时得到封闭空间网络结构聚酰胺树状大分子聚合物；
4)在封闭空间网络结构聚酰胺树状大分子聚合物中加入银离子化合物使其络合还原得到稳定的纳米银溶液；
5)将成卷纯棉无纺布或脱脂纱布以10－12m/min的速度通过盛有上述纳米银溶液的浸液槽，再经过压扎、110－120℃热风烘干、裁切、包装、钴60辐照灭菌，即得。
2.根据权利要求1所述的一种功能性医用敷料的制备方法，其特征在于，所述多氨基单体为二乙烯三胺、三乙烯四胺、四乙烯五胺或五乙烯六胺。
3.根据权利要求1所述的一种功能性医用敷料的制备方法，其特征在于，所述乙烯基单体为丙烯酸、丙烯酸甲酯、甲基丙烯酸甲酯或丙烯酸乙酯。
4.根据权利要求1所述的一种功能性医用敷料的制备方法，其特征在于，所述溶剂为甲醇、三氯甲烷、或N,N-二甲基甲酰胺。
5.根据权利要求1所述的一种功能性医用敷料的制备方法，其特征在于，所述银离子化合物为硝酸银、醋酸银。
6.据权利要求1所述的一种功能性医用敷料的制备方法，其特征在于，所述改性剂为丁二酸酐、马来酸酐。
7.根据权利要求1所述的一种功能性医用敷料的制备方法，其特征在于，所述步骤2)中多氨基单体与乙烯基单体的摩尔比1:1-1:3，所述步骤3)中多氨基单体与改性剂的摩尔比1:0.1-1:1。
8.一种权利要求1所述方法制备的一种功能性医用敷料。
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