CN117430825A - 一种氧化石墨烯/聚氨丙基双胍复合材料及其制备方法与抗菌应用 - Google Patents
一种氧化石墨烯/聚氨丙基双胍复合材料及其制备方法与抗菌应用 Download PDFInfo
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Abstract
本发明公开了一种氧化石墨烯/聚氨丙基双胍复合材料及其制备方法与抗菌应用。由聚氨丙基双胍接枝氧化石墨烯制成，聚氨丙基双胍和氧化石墨烯的摩尔比为1:1~10。本发明利用聚氨丙基双胍中氨基与氧化石墨烯中羧基进行反应，达到聚氨丙基双胍接枝氧化石墨烯,从而在氧化石墨烯表面修饰了双胍官能团,实现了对石墨烯的表面功能化改性。经测试，聚氨丙基双胍接枝氧化石墨烯制备的抗菌乳液湿磨在人造石英石表面，干燥后其抗菌效果可以达到99.99%，在洗刷5000次后其抗菌效果仍然可以达到99%。
Description
技术领域
本发明涉及石墨烯技术领域，具体地说，涉及一种氧化石墨烯/聚氨丙基双胍复合材料及其制备方法与抗菌应用。
背景技术
天然石材，如石英石广泛应用于公共建筑和室内装修领域，是一种无放射性污染、可重复利用的绿色新型建筑室内装饰材料。同时，在食品、制药、餐饮等行业对环境中的细菌有着严格的要求，当温度和湿度处于适宜细菌生存的区间，经常有人员和设备流动的区域便容易滋生细菌，因此需要一种能够有效抑制细菌滋生的方法。比如，在室内装饰材料中添加抗菌剂，赋予其抗菌的功能，然而与之而来的便是持久性抗菌的难题，室内装饰材料常常面临着频繁的洗刷、磨损，许多抗菌剂在抗菌过程中效果减弱直至失效，不能满足长期抗菌的需求。
氧化石墨烯片层含有较多极性基团，如羟基、羧基和环氧基团等，使其表面具有良好的亲水性和生物相容性，具有高度可调控性和可修饰性，可以通过调节接枝条件和比例来控制接枝量和接枝位置，从而实现对材料性能的精确调控。同时，作为二维材料，氧化石墨烯可通过其几纳米的厚度物理切割细菌，因此拥有一定的抗菌功能。
聚氨丙基双胍（PAPB），末端胍基具有很高的活性，容易被呈负电性的各类细菌、病毒所吸附，低浓度条件下，聚氨丙基双胍对革兰氏阳性、阴性细菌都有较强的抑制作用。将其作为抗菌组分添加到石英石中，初期虽然能够呈现优异的抗菌效果，然而经过长期的使用后，石英石的抗菌效果明显下滑。因此，室内装饰材料领域迫切需要抗菌效果优异且能够持久抗菌的抗菌剂。
发明内容
本发明的目的在于克服上述现有技术存在的不足，提供一种在人造石英石表面抗菌性强、抗菌耐久性长的氧化石墨烯/聚氨丙基双胍复合材料及其制备的抗菌乳液。
为了实现上述目的，本发明采用如下技术方案：
一种氧化石墨烯/聚氨丙基双胍复合材料，由聚氨丙基双胍接枝氧化石墨烯制成，聚氨丙基双胍和氧化石墨烯的摩尔比为1~25:1。
上述氧化石墨烯/聚氨丙基双胍复合材料的制备方法，包括如下步骤：取聚氨丙基双胍、氧化石墨烯，比例为1~25:1，在超声波中分散混合，然后加入2-吡咯酮和二苯基硅烷，比例为1~10 :1~10，将上述混合液置于60~120℃油浴锅中保持10~120 min，同时用微波照射10~60min；将得到的溶液过滤，在 65 ℃下真空干燥得到聚氨丙基双胍接枝氧化石墨烯（GO-PAPB）。
一种含有氧化石墨烯/聚氨丙基双胍复合材料的抗菌乳液，由如下重量份数的组分组成：
氧化石墨烯/聚氨丙基双胍复合材料0.5-2，
黄原胶0.5-2，
硅酸镁铝1-3，
吐温-80 2-4，
PVP K30 2-4，
水8-12。
上述抗菌乳液的制备方法，包括如下步骤：取氧化石墨烯/聚氨丙基双胍复合材料、黄原胶、硅酸镁铝和水，超声波分散，加入吐温-80和PVP K30，经高速剪切乳化，制得含有氧化石墨烯/聚氨丙基双胍复合材料的抗菌乳液。
与现有技术相比，本发明具有如下有益效果：本发明利用聚氨丙基双胍中氨基与氧化石墨烯中羧基进行反应，达到聚氨丙基双胍接枝氧化石墨烯,从而在氧化石墨烯表面修饰了双胍官能团,实现了对石墨烯的表面功能化改性。聚氨丙基双胍接枝到氧化石墨烯上，接枝后的材料既在氧化石墨烯的物理切割抗菌的基础上，增添胍基的抗菌性能，又拥有氧化石墨烯的高比表面积、高稳定性，聚氨丙基双胍与氧化石墨烯发生协同作用，使其能够在建筑装饰材料中保持极强的抗菌性和耐久性，经测试，聚氨丙基双胍接枝氧化石墨烯（GO-PAPB）制备的抗菌乳液湿磨在人造石英石表面，干燥后其抗菌效果可以达到99.99%，在洗刷5000次后其抗菌效果仍然可以达到99%。
附图说明
图1为未修饰的氧化石墨烯红外光谱；
图2为实施例1 的聚氨丙基双胍修饰后的氧化石墨烯红外光谱；
图3为实施例2 的聚氨丙基双胍修饰后的氧化石墨烯红外光谱。
具体实施方式
实施例1：
取0.85 mmol/L 氧化石墨烯，6.3 mmol/L 聚氨丙基双胍，加入2mL去离子水，在超声波中分散混合，然后加入1.2 mmol/L 2-吡咯酮和0.55 mmol/L二苯基硅烷，将上述混合液至于80℃油浴锅中保持10 min，同时用微波照射10 min，频率在2450 Hz。将得到的溶液过滤，在 65 ℃下真空干燥得到聚氨丙基双胍接枝氧化石墨烯（GO-PAPB）。
从图1、图2中可以看出，与未修饰的氧化石墨烯（GO）红外图谱对比，修饰后的氧化石墨烯（GO-PAPB）在1695.00 cm-1处C＝O的伸缩振动峰减弱，是因为GO表面部分-COOH基团断裂，由于氮原子上未共用电子对与羰基的p-π共轭，使C=O伸缩振动频率降低。同时可以看到，相对于GO，GO-PAPB在1718cm-1，1689 cm-1处出现伸缩振动双峰，为酰胺Ⅰ带C=O峰，同时在1626 cm-1处有一较峰，即酰胺Ⅱ带。此吸收较弱，并靠近νC=O的NH2的面内变形振动，说明聚氨丙基双胍-NH2与氧化石墨烯-COOH脱水形成酰基-O=C-NH2-，聚氨丙基双胍成功接枝到氧化石墨烯（GO-PAPB）。
按照重量份，取1份黄原胶，2份硅酸镁铝，1份GO-PAPB，20份水，超声波分散，加入3份吐温-80和3份PVP K30，1份甲基三乙氧基硅烷，高速剪切乳化，制得GO-PAPB抗菌乳液。
抗菌测试：将抗菌GO-PAPB抗菌乳液湿磨在人造石英石表面，用量10 g/m2，自然干燥7天，样品由广东省微生物分析检测中心按《ISO 22196:2011塑料与其他无孔表面的抗菌性测定》规定的方法检测其抗菌效果，结果如表1所示，表1 是氧化石墨烯修饰前后的抗菌效果对比；从表1可以看出GO-PAPB的抗菌效果比PAPB有明显提升。
耐久性测试：抗细菌耐久性能按照GB/T 9266-2009《建筑涂料涂层耐洗刷性的测定》，洗刷次数为 5000 次，然后再进行抗菌测试，结果如2所示，表2是经过5000次洗刷后，氧化石墨烯修饰前后的抗菌耐久性对比，从表2可以看出，GO-PAPB在洗刷5000次后其仍然具有较强的抗菌效果，而PAPB在洗刷5000次后抗菌效果下降明显。
实施例2：
取0.85 mmol/L 氧化石墨烯，18.9 mmol/L 聚氨丙基双胍，加入6 mL去离子水，在超声波中分散混合，然后加入1.2 mmol/L 2-吡咯酮和0.55 mmol/L 二苯基硅烷，将上述混合液至于100℃油浴锅中保持20 min，同时用微波照射20 min，频率在2450Hz。将得到的溶液过滤，在 65 ℃下真空干燥得到聚氨丙基双胍接枝氧化石墨烯。
从图3中可以看出，在1770～1720cm-1波段未见与苯环相连的-COOH峰，该工艺条件下，氧化石墨烯上-COOH全部与聚氨丙基双胍末端-NH2脱水缩合。在1690cm-1处有一尖吸收峰，为酰胺Ⅰ带C=O峰，结合1638cm-1处较弱吸收峰，即酰胺Ⅱ带，可判定为形成了酰基-O=C-NH2-，聚氨丙基双胍成功接枝到氧化石墨烯。
按照重量份，取1份黄原胶，2份硅酸镁铝，1份GO-PAPB，20份水，超声波分散，加入3份吐温-80和3份PVP K30，1份甲基三乙氧基硅烷，高速剪切乳化，制得GO-PAPB抗菌乳液。
抗菌测试：将抗菌GO-PAPB抗菌乳液湿磨在人造石英石表面，用量10 g/m2，自然干燥7天，样品由广东省微生物分析检测中心按《ISO 22196:2011塑料与其他无孔表面的抗菌性测定》规定的方法检测。结果如表1所示，表1 是氧化石墨烯修饰前后的抗菌效果对比；从表1可以看出GO-PAPB的抗菌效果比PAPB有明显提升。
耐久性测试：抗细菌耐久性能按照GB/T 9266-2009《建筑涂料涂层耐洗刷性的测定》，洗刷次数为 5000 次，然后再进行抗菌测试，结果如2所示，表2是经过5000次洗刷后，氧化石墨烯修饰前后的抗菌耐久性对比，从表2可以看出，GO-PAPB在洗刷5000次后其仍然具有较强的抗菌效果，而PAPB在洗刷5000次后抗菌效果下降明显。
对比例1：
取1份黄原胶，2份硅酸镁铝，1份GO，20份水，超声波分散，加入3份吐温-80和3份PVP K30，1份甲基三乙氧基硅烷，高速剪切乳化，制得GO乳液。
将上述乳液湿磨在人造石英石表面，用量10 g/m2，自然干燥7天，样品由广东省微生物分析检测中心按《ISO 22196:2011塑料与其他无孔表面的抗菌性测定》规定的方法检测其抗菌性，结果如表1。抗细菌耐久性能按照，GB/T 9266-2009《建筑涂料 涂层耐洗刷性的测定》，洗刷次数为 5000 次，测试其抗菌耐久性，结果如表2。
对比例2：
取1份黄原胶，2份硅酸镁铝，1份PAPB，20份水，超声波分散，加入3份吐温-80和3份PVP K30，1份甲基三乙氧基硅烷，高速剪切乳化，制得PAPB乳液。
将抗菌PAPB乳液湿磨在人造石英石表面，用量10 g/m2，自然干燥7天，样品由广东省微生物分析检测中心按《ISO 22196:2011塑料与其他无孔表面的抗菌性测定》规定的方法检测其抗菌性，结果如表1。抗细菌耐久性能按照，GB/T 9266-2009《建筑涂料 涂层耐洗刷性的测定》，洗刷次数为 5000 次，测试其抗菌耐久性，结果如表2。
。
Claims (4)
1.一种氧化石墨烯/聚氨丙基双胍复合材料，其特征在于由聚氨丙基双胍接枝氧化石墨烯制成，聚氨丙基双胍和氧化石墨烯的摩尔比为1~25:1。
2.权利要求1所述氧化石墨烯/聚氨丙基双胍复合材料的制备方法，其特征在于包括如下步骤：取聚氨丙基双胍、氧化石墨烯，比例为1~25:1，在超声波中分散混合，然后加入2-吡咯酮和二苯基硅烷，比例为1~10 :1~10，将上述混合液置于60~120℃油浴锅中保持10~120min，同时用微波照射10~60min；将得到的溶液过滤，在65 ℃下真空干燥得到聚氨丙基双胍接枝氧化石墨烯。
3.一种含有氧化石墨烯/聚氨丙基双胍复合材料的抗菌乳液，其特征在于由如下重量份数的组分组成：
权利要求1所述氧化石墨烯/聚氨丙基双胍复合材料0.5-2，
黄原胶0.5-2，
硅酸镁铝1-3，
吐温-80 2-4，
PVP K30 2-4，
水8-12。
4.权利要求3所述抗菌乳液的制备方法，其特征在于包括如下步骤：取氧化石墨烯/聚氨丙基双胍复合材料、黄原胶、硅酸镁铝和水，超声波分散，加入吐温-80和PVP K30，经高速剪切乳化，制得含有氧化石墨烯/聚氨丙基双胍复合材料的抗菌乳液。
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