CN116333380A - 一种用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球的制备方法及应用 - Google Patents
一种用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球的制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球的制备方法及应用。其制备方法包括以下步骤:将壳聚糖溶解在冰醋酸溶液中,在氮气气氛下依次添加硝酸银、硒代硫酸钠搅拌均匀,以戊二醛为交联剂,通过反相乳液交联法加入液体石蜡、司班‑80、戊二醛反应即得。本发明制得的纳米硒化银壳聚糖微球添加至异戊橡胶中抗菌性能优良,且具有良好的物理机械性能、抗菌持久性能。
Description
技术领域
本发明涉及橡胶材料技术领域,具体涉及一种用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球的制备方法及应用。
背景技术
天然橡胶是最早使用的医用弹性体,由于其含有一种高致敏性植物蛋白,所用配合剂N-亚硝胺等对人体的刺激反应较大,易使人体皮肤表面出现瘙痒、发红等过敏现象,所以天然橡胶只有经过纯化改性后才能用于人体。异戊橡胶是由异戊二烯合成的一种橡胶,主要成分为顺-1,4-聚异戊二烯,与天然橡胶分子结构相同,性能相近,具备与天然橡胶同样良好的加工工艺性能,最重要的是异戊橡胶中不含有天然橡胶中易使人致敏的蛋白质成分,基本可代替NR,近年来逐步成为医疗卫生、食品、日常用品方面的重要原料。
壳聚糖是一种重要的天然生物降解高分子,是天然多糖中唯一的碱性多糖,也是少数具有荷电性的天然产物之一。分子中含有反应活性高且能与金属离子配位的氨基和羟基,在酸性介质中带正电荷聚电解质性质的结构可与细菌的阴离子化合物相互作用。壳聚糖与无机材料或金属材料(如金和银纳米粒子)的复合材料也可以提供特定的性能,如广谱抗菌活性和光催化活性。
在医疗环境中存在许多的细菌,细菌可通过材料侵染与之接触的人体组织。银纳米颗粒(AgNPs)是研究最广泛的抗菌无机纳米颗粒之一,因为其具有强大的广谱抗菌活性。十多年来,银纳米粒子已在化妆品、纺织品、医药和医疗产品中商业化使用。尽管如此,人们仍然担心它们对哺乳动物细胞的毒性、对环境的影响以及由于AgNPs的广泛使用而可能产生的耐药性。因此,人们一直在努力探索新型无机纳米材料的抗菌应用。最近硒元素因其抗菌作用而备受关注,且纳米硒对哺乳动物的细胞毒性最低。
利用反相乳液交联法可制备纳米硒化银壳聚糖微球。硒化物可减少银元素所带来的细胞毒性,硒又能增加银的广谱抗菌性;将纳米硒化银包裹于壳聚糖微球添加至异戊橡胶中,可依靠壳聚糖微球的缓释作用从而提高材料抗菌性能的长久性。因此,有必要合成使用纳米硒化银壳聚糖微球来制备抗菌异戊橡胶材料。
发明内容
为了解决现有技术的缺点和不足之处提供用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球的制备方法及应用。
本发明目的通过以下技术方案实现:
本发明的首要目的在于提供一种用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球。其制备原料包括壳聚糖0.5~3质量份、硝酸银1~3mL、硒代硫酸钠3~6mL、液体石蜡100~200ml、Span-80 5~20ml、戊二醛5~20ml。
进一步地,所用硒代硫酸钠溶液(Na2SeSO3)溶液由硒粉与亚硫酸钠溶液在90~100℃下回流反应8~11h得到。
本发明的目的之二在于提供一种用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球的制备方法,该方法包括如下步骤:将0.2~3g壳聚糖溶解在3%冰醋酸溶液中超声分散1~2h;在氮气气氛下将1~3mL硝酸银溶液在搅拌下滴加至上述壳聚糖溶液中混合均匀,再滴入3~6mLNa2SeSO3溶液反应30~40min;随后将100~200ml液体石蜡、5~20ml司班-80添加至上述溶液反应30~40min后加入5~20ml戊二醛,在40~60℃下搅拌反应5小时;最后用乙醇清洗、过滤、干燥,即得纳米硒化银壳聚糖微球。
本发明的另一目的在于提供上述抗菌异戊橡胶的应用,该方法原料来源广泛、制备的异戊橡胶具有良好的抗菌性能,并能保持优异的抗菌持久性。
所述纳米硒化银壳聚糖微球应用于制备抗菌异戊橡胶,所述抗菌异戊橡胶材料的制备按质量份计,包括氧化锌(ZnO)4~5质量份、硬脂酸(SA)1~2质量份、促进剂NS 1~2质量份、纳米硒化银壳聚糖微球(CS-Ag2Se)0.25~3质量份、硫磺1~3质量份、异戊橡胶(IR)100质量份。
上述应用包含如下步骤:
(1)配方:氧化锌(ZnO)4~5质量份、硬脂酸(SA)1~2质量份、促进剂NS 1~2质量份、纳米硒化银壳聚糖微球(CS-Ag2Se)0.25~3质量份、硫磺1~3质量份、异戊橡胶(IR)100质量份;
(2)混炼:将称取的氧化锌、硬脂酸、促进剂NS、纳米硒化银壳聚糖微球、硫磺、异戊橡胶IR加入开炼机混炼,具体加料顺序为:先加入异戊橡胶,待其包辊塑炼光滑均匀后加入氧化锌、硬脂酸,均匀分散后加入促进剂NS,再加入纳米硒化银壳聚糖微球,最后加入硫磺,左右割刀数次,打三角包、打卷数次,得到混炼胶,记为IR/CS-Ag2Se。
(3)将混炼胶通过平板硫化机进行硫化,冷却、停放,制得抗菌异戊橡胶。
上述应用中,步骤(3)中,采用的硫化时间为150~160℃,优选150℃。
与现有技术相比,本发明具有以下优点及有益效果:
(1)本发明制得的纳米硒化银壳聚糖微球应用于异戊橡胶,一方面能够减少同种天然橡胶带来的过敏问题,另一方面制得的纳米硒化银壳聚糖微球应用于异戊橡胶,在不降低异戊橡胶的硫化及物理机械性能的基础上,能够少量高效提高异戊橡胶的抗菌性能。
(2)本发明制得的抗菌异戊橡胶,不仅具有良好的抗菌效果,并且能够在其应用场合下保持有效的抗菌持久性。
具体实施方式
下面结合具体实施例对本发明进行进一步详细的解释和说明。
实施例1
一种用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球,其制备方法包括以下步骤:
(1)将0.5g壳聚糖溶解在3%冰醋酸溶液中超声分散1h;
(2)在氮气气氛下将1mL硝酸银溶液在搅拌下滴加至上述壳聚糖溶液中混合均匀后,再滴加3mLNa2SeSO3溶液反应30min;
(3)随后将100ml液体石蜡、10ml司班-80、10ml戊二醛添加至上述溶液中,在40℃下搅拌反应5小时;
(4)最后用乙醇清洗、过滤、干燥,即得纳米硒化银壳聚糖微球。
一种混炼胶,其制备方法包括以下步骤:
(1)配方:氧化锌(ZnO)5质量份、硬脂酸(SA)2质量份、促进剂NS 1质量份、纳米硒化银壳聚糖微球0.25质量份、硫磺2.25质量份、异戊橡胶100质量份;
(2)混炼:将称取的氧化锌、硬脂酸、促进剂NS、纳米硒化银壳聚糖微球、硫磺、异戊橡胶IR加入开炼机混炼,具体加料顺序为:先加入异戊橡胶,待其包辊塑炼光滑均匀后加入氧化锌、硬脂酸,均匀分散后加入促进剂NS,再加入纳米硒化银壳聚糖微球,最后加入硫磺,左右割刀数次,打三角包、打卷数次,得到混炼胶,记为IR/CS-Ag2Se-0.25。
将混炼胶在150℃下通过平板硫化机进行硫化,冷却、停放,制得抗菌异戊橡胶。
实施例2
一种用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球,其制备方法包括以下步骤:
(1)将0.5g壳聚糖溶解在3%冰醋酸溶液中超声分散1h;
(2)在氮气气氛下将1mL硝酸银溶液在搅拌下滴加至上述壳聚糖溶液中混合均匀后,再滴加3mLNa2SeSO3溶液反应30min;
(3)随后将100ml液体石蜡、10ml司班-80、10ml戊二醛添加至上述溶液中,在40℃下搅拌反应5小时;
(4)最后用乙醇清洗、过滤、干燥,即得纳米硒化银壳聚糖微球。
一种混炼胶,其制备方法包括以下步骤:
(1)配方:氧化锌(ZnO)5质量份、硬脂酸(SA)2质量份、促进剂NS 1质量份、纳米硒化银壳聚糖微球0.5质量份、硫磺2.25质量份、异戊橡胶100质量份;
(2)混炼:将称取的氧化锌、硬脂酸、促进剂NS、纳米硒化银壳聚糖微球、硫磺、异戊橡胶IR加入开炼机混炼,具体加料顺序为:先加入异戊橡胶,待其包辊塑炼光滑均匀后加入氧化锌、硬脂酸,均匀分散后加入促进剂NS,再加入纳米硒化银壳聚糖微球,最后加入硫磺,左右割刀数次,打三角包、打卷数次,得到混炼胶,记为IR/CS-Ag2Se-0.5。
将混炼胶在150℃下通过平板硫化机进行硫化,冷却、停放,制得抗菌异戊橡胶。
实施例3:
一种用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球,其制备方法包括以下步骤:
(1)将0.5g壳聚糖溶解在3%冰醋酸溶液中超声分散1h;
(2)在氮气气氛下将1mL硝酸银溶液在搅拌下滴加至上述壳聚糖溶液中混合均匀后,再滴加3mLNa2SeSO3溶液反应30min;
(3)随后将100ml液体石蜡、10ml司班-80、10ml戊二醛添加至上述溶液中,在40℃下搅拌反应5小时;
(4)最后用乙醇清洗、过滤、干燥,即得纳米硒化银壳聚糖微球。
一种混炼胶,其制备方法包括以下步骤:
(4)配方:氧化锌(ZnO)5质量份、硬脂酸(SA)2质量份、促进剂NS 1质量份、纳米硒化银壳聚糖微球0.75质量份、硫磺2.25质量份、异戊橡胶100质量份;
(5)混炼:将称取的氧化锌、硬脂酸、促进剂NS、纳米硒化银壳聚糖微球、硫磺、异戊橡胶IR加入开炼机混炼,具体加料顺序为:先加入异戊橡胶,待其包辊塑炼光滑均匀后加入氧化锌、硬脂酸,均匀分散后加入促进剂NS,再加入纳米硒化银壳聚糖微球,最后加入硫磺,左右割刀数次,打三角包、打卷数次,得到混炼胶,记为IR/CS-Ag2Se-0.75。
将混炼胶在150℃下通过平板硫化机进行硫化,冷却、停放,制得抗菌异戊橡胶。
实施例4:
一种用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球,其制备方法包括以下步骤:
(1)将0.5g壳聚糖溶解在3%冰醋酸溶液中超声分散1h;
(2)在氮气气氛下将1mL硝酸银溶液在搅拌下滴加至上述壳聚糖溶液中混合均匀后,再滴加3mLNa2SeSO3溶液反应30min;
(3)随后将100ml液体石蜡、10ml司班-80、10ml戊二醛添加至上述溶液中,在40℃下搅拌反应5小时;
(4)最后用乙醇清洗、过滤、干燥,即得纳米硒化银壳聚糖微球。
一种混炼胶,其制备方法包括以下步骤:
(1)配方:氧化锌(ZnO)5质量份、硬脂酸(SA)2质量份、促进剂NS 1质量份、纳米硒化银壳聚糖微球1质量份、硫磺2.25质量份、异戊橡胶100质量份;
(2)混炼:将称取的氧化锌、硬脂酸、促进剂NS、纳米硒化银壳聚糖微球、硫磺、异戊橡胶IR加入开炼机混炼,具体加料顺序为:先加入异戊橡胶,待其包辊塑炼光滑均匀后加入氧化锌、硬脂酸,均匀分散后加入促进剂NS,再加入纳米硒化银壳聚糖微球,最后加入硫磺,左右割刀数次,打三角包、打卷数次,得到混炼胶,记为IR/CS-Ag2Se-1。
将混炼胶在150℃下通过平板硫化机进行硫化,冷却、停放,制得抗菌异戊橡胶。
对比例1:
一种混炼胶,其制备方法包括以下步骤:
(1)配方:氧化锌(ZnO)5质量份、硬脂酸(SA)2质量份、促进剂NS 1质量份、硫磺2.25质量份、异戊橡胶100质量份;
(2)混炼:将称取的氧化锌、硬脂酸、促进剂NS、纳米硒化银壳聚糖微球、硫磺、异戊橡胶IR加入开炼机混炼,具体加料顺序为:先加入异戊橡胶,待其包辊塑炼光滑均匀后加入氧化锌、硬脂酸,均匀分散后加入促进剂NS,再加入纳米硒化银壳聚糖微球,最后加入硫磺,左右割刀数次,打三角包、打卷数次,得到混炼胶,记为IR/CS-Ag2Se。
将混炼胶在150℃下通过平板硫化机进行硫化,冷却、停放,制得抗菌异戊橡胶。
其与实施例1、实施例2、实施例3、实施例4的区别在于不添加所制备纳米硒化银壳聚糖微球,其他组分、用量、制备方法均与实施例1、实施例2、实施例3、实施例4相同。
性能测试:
(1)硫化特性:采用U-Can UR-2010SD无转子硫化仪在170℃下测试混炼胶的硫化特性;
(2)拉伸强度:采用UT-2080拉力试验机测试混炼胶的拉伸强度,按照“GB/T 528-2009硫化橡胶或热塑性橡胶拉伸应力应变性能的测定”公开的测定方法进行测试;
(3)撕裂强度:采用UT-2080拉力试验机测试混炼胶的撕裂强度,按照“GB/T 528-2009硫化橡胶或热塑性橡胶拉伸应力应变性能的测定”公开的测定方法进行测试;
(4)抗菌率:参照“GB/T 31402-2015塑料塑料表面抗菌性能实验办法”公开的测定方法,以革兰氏阴性菌(大肠杆菌)和革兰氏阳性菌(金黄色葡萄球菌)为测试菌种,进行抗菌性能的测试;
(5)平板菌落计数法测试:将革兰氏阴性菌、革兰氏阳性菌的菌种分别接种于75mL的肉汤培养基中于150rpm下培养24h后将菌液浓度稀释至1×106CFU/mL。样品放入六孔板,将浓度为1×106CFU/mL的菌液滴到样品表面用盖玻片盖好,培养24h后用PBS溶液将试样上的菌液洗脱并进行梯度稀释,选取适宜稀释倍数的稀释液涂覆到平板培养基上,在37℃的恒温恒湿培养箱中培养24h,观察菌落生长情况并对菌落进行计数,根据菌落的数量计算抗菌率(结果如表1所示)。
表1
由表1可知:随着纳米硒化银壳聚糖微球份数的添加,异戊橡胶材料的抗菌率有所提高,这是由于随着纳米硒化银壳聚糖微球份数的增加,纳米硒化银壳聚糖微球在异戊橡胶中分散密度更大使得与细菌的接触范围更广接触面积更大,因此对细菌的抑制性越大使得抗菌率提高。相比之下材料对革兰氏阴性菌展现出比革兰氏阳性菌更好的抑制作用,这是由于两种细菌结构不同的原因所导致的,革兰氏阳性细菌(金黄色葡萄球菌)的细胞壁比革兰氏阴性细菌(大肠杆菌)的细胞壁要更厚、更硬,使得对革兰氏阴性菌更容易穿透,从而抑制性更强抗菌效果更好。
上述实施例为本发明,但本发明的实施方式并不受上述实施例的限制,其他任何未背离本发明原理下对本发明作出的任何改进、修饰、替代、组合以及对本发明所选原料的替换、辅助助剂的添加等均应为等效的置换方式,都包含在本发明的保护和公开范围之内。
Claims (10)
1.一种用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球,其特征在于,所述纳米硒化银壳聚糖微球制备原料包括:壳聚糖0.5~3质量份、硝酸银1~3mL、硒代硫酸钠溶液3~6mL、液体石蜡100~200ml、Span-805~20ml和戊二醛5~20ml。
2.权利要求1所述用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球的制备方法,其特征在于,包括如下步骤:将0.2~3g壳聚糖溶解在3%冰醋酸溶液中超声分散1~2h;在氮气气氛下将1~3mL硝酸银溶液在搅拌下滴加至上述壳聚糖溶液中混合均匀,再滴入3~6mL硒代硫酸钠溶液反应;随后将100~200ml液体石蜡、5~20ml Span-80添加至上述溶液反应后,加入5~20ml戊二醛,在40~60℃下搅拌反应5小时;最后用乙醇清洗、过滤、干燥,即得纳米硒化银壳聚糖微球。
3.根据权利要求2所述用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球的制备方法,其特征在于,所述滴入3~6mL硒代硫酸钠溶液反应的反应时间为30~40min。
4.根据权利要求2所述用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球的制备方法,其特征在于,所述将100~200ml液体石蜡、5~20ml Span-80添加至上述溶液反应的反应时间为30~40min。
5.根据权利要求2所述用于制备抗菌异戊橡胶的纳米硒化银壳聚糖微球的制备方法,其特征在于,所述硒代硫酸钠溶液(Na2SeSO3)溶液由硒粉与亚硫酸钠溶液在90~100℃下回流反应8~11h得到。
6.权利要求1所述用于纳米硒化银壳聚糖微球用于制备抗菌异戊橡胶,其特征在于,所述抗菌异戊橡胶材料的制备,包括氧化锌ZnO、硬脂酸SA、促进剂NS、纳米硒化银壳聚糖微球CS-Ag2Se、硫磺S、异戊橡胶。
7.根据权利要求4所述应用,其特征在于,配方按质量份计,包括氧化锌ZnO4~5质量份、硬脂酸SA1~2质量份、促进剂NS 1~2质量份、纳米硒化银壳聚糖微球CS-Ag2Se0.25~3质量份、硫磺1~3质量份、异戊橡胶IR100质量份。
8.根据权利要求4~5所述应用,其特征在于,制备抗菌异戊橡胶包含如下步骤:将称取的氧化锌、硬脂酸、促进剂NS、纳米硒化银壳聚糖微球、硫磺、异戊橡胶IR加入开炼机混炼,具体加料顺序为:先加入异戊橡胶,待其包辊塑炼光滑均匀后加入氧化锌、硬脂酸,均匀分散后加入促进剂NS,再加入纳米硒化银壳聚糖微球,最后加入硫磺,左右割刀数次,打三角包、打卷数次,得到混炼胶,记为IR/CS-Ag2Se,将混炼胶通过平板硫化机进行硫化,冷却、停放,制得抗菌异戊橡胶。
9.根据权利要求6所述应用,其特征在于,采用的硫化温度为150~160℃。
10.根据权利要求6所述应用,其特征在于,采用的硫化温度为150℃。
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