CN114230810A - 一种抗菌可生物降解智能响应水凝胶及其制备方法 - Google Patents
一种抗菌可生物降解智能响应水凝胶及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种抗菌可生物降解智能响应水凝胶,以重量份数计,其组分包括:1‑3份黄酮类物质、6‑12份壳聚糖、3‑5份聚乙二醇、2‑4份腐殖酸钠、5‑8份聚合单体、0.05‑0.2份纳米氧化物、0.05‑0.1份引发剂、0.08‑0.15份交联剂;还公开对应制备方法,能有效针对不同环境迅速做出响应,可生物降解,高效发挥抗菌作用,除此之外本发明加入腐殖酸钠抗菌成分,还可以有效地净化空气,吸附环境中的异味,达到多重功效。
Description
技术领域
本发明属于化工生活品应用技术领域,具体涉及一种抗菌可生物降解智能响应水凝胶及其制备方法。
背景技术
抗菌剂是一类可以在一定时间内,使某些微生物的生长和繁殖保持在必要水平以下的化学试剂。其主要机制有四种:干扰细胞壁的合成;损伤细菌细胞膜、破坏细胞膜的屏障作用;影响细菌蛋白质的合成,细菌丧失生长繁殖的物质基础;影响细菌核酸代谢。
现存的抗菌除臭剂主要为有机抗菌剂,其有效成分主要为咪唑,噻唑,香草醛,季铵盐类物质,使用该类抗菌材料,能当下对细菌微生物产生致命作用,但吸附与缓释性能较为薄弱,使用后残留物质会对河流,生物,土壤造成潜在危害且难以富集回收再利用。而这些有机物的耐热性较差,潮湿环境易于水解,有效期短,吸附与缓释作用差。潮湿环境下较干燥环境更易于滋生细菌等微生物,而大量使用该类抗菌剂会对细菌本身产生抗药性。为克服现存缺陷,本发明提供一种抗菌可生物降解智能响应凝胶,采用绿色可降解原料在较为温和的条件下合成一种可生物降解产品,成本低,绿色安全,具有强效的抗菌、吸附、缓释作用。
发明内容
针对现有技术的以上缺陷或改进需求,本发明目的在于提供一种智能响应可生物降解抗菌水凝胶。该法易于操作,成本低,可生物降解,对环境友好且有针对性对细菌等微生物产生抑制作用。
为实现上述目的,按照本发明的另一个方面,本发明提供了一种抗菌可生物降解智能响应水凝胶,以重量份数计,其组分包括:1-3份黄酮类物质、6-12份壳聚糖、3-5份聚乙二醇、2-4份腐殖酸钠、5-8份聚合单体、0.05-0.2 份纳米氧化物、0.05-0.1份引发剂、0.08-0.15份交联剂。
上述抗菌可生物降解智能响应水凝胶的制备方法,包括如下步骤:
1)将1-3份黄酮类物质溶于乙醚中备用,黄酮和乙醚的固液比为(1-3) g:(10-20)mL;
2)将6-12份壳聚糖溶于水中,壳聚糖和水的固液比为(1-2)g:(100-500) mL;
加入3-5份聚乙二醇充分搅拌得到壳聚糖溶液备用;
3)将2-4份腐植酸钠溶于水中,腐殖酸钠与水的固液比为(1-3)g: (100-300)mL;得到腐植酸钠溶液备用;
4)向三口烧瓶中加入体积比为1~5:1~5:1~5的1)、2)、3)中得到的溶液乳化30min,加入5-8份聚合单体、0.05-0.2份的纳米氧化物,40℃下搅拌30min,滴加0.05-0.1份份引发剂与0.08-0.15份交联剂;升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
进一步的,黄酮类物质具体为姜黄素、二氢黄酮、异黄酮、黄酮醇中的一种。
进一步的,所述黄酮类物质具体为姜黄素、二氢黄酮、异黄酮、黄酮醇中的两种或两种以上的混合。
进一步的,所述壳聚糖具体为壳聚糖季铵盐。
进一步的,所述聚乙二醇具体为聚乙二醇-400。
进一步的,聚合单体为丙烯酸、丙烯酰胺、丙烯腈中的一种。
进一步的,所述纳米氧化物具体为:纳米SiO2、纳米ZnO、纳米TiO2 中的一种。
进一步的,所述引发剂具体为:过硫酸钾、过硫酸钠、过硫酸铵中的一种。
进一步的,所述交联剂具体为:过氧化苯甲酰、N,N-二甲基双丙烯酰胺中的一种。
总体而言,通过本发明的所构思的以上技术方案与现有技术相比,能够取得下列有益效果:
(1)本发明的抗菌可生物降解智能响应水凝胶,以缓释凝胶为载体,加入黄酮类物质,壳聚糖季铵盐,腐植酸钠,聚合单体通过多元接支共聚反应得到一种可针对不同环境做出智能响应。在干燥环境下缓慢持久释放抗菌成分,避免因高剂量使用抗菌药物而产生抗药性,在潮湿环境下因凝胶吸收环境中的水分有一定溶胀改变使得气孔张开抗菌成分释放速度加快,能有效针对不同环境迅速做出响应,高效发挥抗菌作用,除此之外本发明加入腐殖酸钠抗菌成分,还可以有效地净化空气,吸附环境中的异味,达到多重功效。
(2)本发明的抗菌可生物降解智能响应水凝胶,对环境友好,可生物降解,对不同环境可做到智能响应,有强效的抗菌作用。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明的进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明的,并不用于限定本发明的。此外,下面所描述的本发明的各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。
本发明所述的一种抗菌可生物降解智能响应水凝胶,以重量份数记,其组分包括:1-3份黄酮类物质、6-12份壳聚糖、3-5份聚乙二醇、2-4份腐殖酸钠、5-8份聚合单体、0.05-0.2份纳米氧化物0.05-0.1份引发剂、0.08-0.15 份交联剂。
具体制备方法包括:
1)将1-3份黄酮类物质溶于10-20ml乙醚中备用;
2)将6-12份壳聚糖溶于水中(固液比为(1-2):(50-200)),加入 3-5份聚乙二醇充分搅拌得到糖溶液备用;
3)将2-4份腐植酸钠溶于水中(固液比为(1-3):(100-300)),得到的腐植酸钠溶液备用;
4)向三口烧瓶中加入体积比为(1-5):(1-5):(1-5)的1)、2)、3)溶液乳化30min,加入聚合单体、0.05-0.2份纳米氧化物,40℃下搅拌30min,滴加0.05-0.1份份引发剂与0.08-0.15份交联剂。升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
以下结合具体实施例对本发明作进一步说明。
实施例1:
本发明公开了一种抗菌可生物降解智能响应水凝胶的制备方法,包括以下步骤:
1)将1份姜黄素溶于10ml乙醚中备用;
2)将6份壳聚糖季铵盐溶于水(固液比为1:50)中,加入3份聚乙二醇-400充分搅拌得到壳聚糖季铵盐溶液备用;
3)将2份腐植酸钠溶于水中(固液比为1:100),得到腐殖酸钠溶液备用;
4)向三口烧瓶中加入体积比为1:1:1的1)、2)、3)溶液乳化30min,加入2份丙烯酰胺、0.05份的纳米SiO2,40℃下搅拌30min,滴加0.05份过硫酸钾与0.08份N,N-二甲基双丙烯酰胺。升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
实施例2:
本发明公开了一种抗菌可生物降解智能响应水凝胶的制备方法,包括以下步骤:
1)将2份二氢黄酮溶于12ml乙醚中备用;
2)将8份壳聚糖季铵盐溶于水中(固液比为2:50),加入3份聚乙二醇-400充分搅拌得到壳聚糖季铵盐溶液备用;
3)将3份腐植酸钠溶于水中(固液比为3:100),得到腐植酸钠溶液备用;
4)向三口烧瓶中加入体积比为2:1:1的1)、2)、3)溶液乳化30min,加入丙烯酰胺、0.08份纳米SiO2,40℃下搅拌30min,滴加0.05份过硫酸钾与0.08份N,N-二甲基双丙烯酰胺。升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
实施例3:
本发明公开了一种抗菌可生物降解智能响应水凝胶的制备方法,包括以下步骤:
1)将1份异黄酮溶于11ml乙醚中备用;
2)将10份壳聚糖季铵盐溶于水中(固液比为1:80),加入2份聚乙二醇充分搅拌得到壳聚糖季铵盐溶液备用;
3)将3份腐植酸钠溶于水中(固液比为2:118),得到腐植酸钠溶液备用;
4)向三口烧瓶中加入体积比为3:1:1的1)、2)、3)溶液乳化30min,加入丙烯酸、0.1份纳米ZnO,40℃下搅拌30min,滴加0.06份过硫酸铵与 0.1份N,N-二甲基双丙烯酰胺。升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
实施例4:
本发明公开了一种抗菌可生物降解智能响应水凝胶的制备方法,包括以下步骤:
1)将3份黄酮醇溶于20ml乙醚中备用;
2)将12份壳聚糖季铵盐溶于水中(固液比为1:180),加入4份聚乙二醇充分搅拌得到壳聚糖季铵盐溶液备用;
3)将4份腐植酸钠溶于水中(固液比为3:220),得到腐植酸钠溶液备用;
4)向三口烧瓶中加入体积比为1:2:1的1)、2)、3)溶液乳化30min,加入丙烯腈、0.12份纳米ZnO,40℃下搅拌30min,滴加0.1份过硫酸铵与 0.15份N,N-二甲基双丙烯酰胺。升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
实施例5:
本发明公开了一种抗菌可生物降解pH响应水凝胶的制备方法,包括以下步骤:
1)将2份姜黄素、二氢黄酮(质量比为1:1)溶于13ml乙醚中备用;
2)将9份壳聚糖季铵盐溶于水中(固液比为2:75),加入2份聚乙二醇充分搅拌得到壳聚糖季铵盐溶液备用;
3)将2份腐植酸钠溶于水中(固液比为3:170),得到腐殖酸钠溶液备用;
4)向三口烧瓶中加入体积比为2:1:3的1)、2)、3)溶液乳化30min,加入丙烯酰胺、0.15份纳米SiO2,40℃下搅拌30min,滴加0.07份过硫酸铵与0.09份N,N-二甲基双丙烯酰胺。升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
实施例6:
本发明公开了一种抗菌可生物降解智能响应水凝胶的制备方法,包括以下步骤:
1)将1份姜黄素、二氢黄酮、异黄酮(质量比为1:1:1)的混合物溶于 20ml乙醚中备用;(混合这种方法在权利要求中没有体现)
2)将6份壳聚糖季铵盐溶于水中(固液比为2:130),加入2份聚乙二醇充分搅拌得到壳聚糖季铵盐溶液备用;
3)将2份腐植酸钠水中(固液比为2:155),得到腐殖酸钠溶液备用;
4)向三口烧瓶中加入体积比为4:3:5的1)、2)、3)溶液乳化30min,加入丙烯酸、0.18份纳米ZnO,40℃下搅拌30min,滴加0.1份过硫酸钾与 0.12份N,N-二甲基双丙烯酰胺。升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
实施例7:
本发明公开了一种抗菌可生物降解智能响应水凝胶的制备方法,包括以下步骤:
1)将3份姜黄素、二氢黄酮、异黄酮(质量比为3:2:1)的混合物溶于 10mL乙醚中备用;
2)将12份壳聚糖季铵盐溶于水中(固液比为1:70),加入4份聚乙二醇充分搅拌得到壳聚糖季铵盐溶液备用;
3)将3份腐植酸钠溶于水中(固液比为2:170),得到腐殖酸钠溶液备用;
4)向三口烧瓶中加入体积比为5:4:5的1)、2)、3)溶液乳化30min,加入5份丙烯酰胺、0.09份纳米TiO2,40℃下搅拌30min,滴加0.09份过硫酸钾与0.1份N,N-二甲基双丙烯酰胺。升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
实施例8:
本发明公开了一种抗菌可生物降解智能响应水凝胶的制备方法,包括以下步骤:
1)将2份姜黄素、二氢黄酮、异黄酮(质量比1:2:1)溶于16ml乙醚中备用;
2)将7份壳聚糖季铵盐溶于水中(固液比为2:220),加入2份聚乙二醇充分搅拌得到壳聚糖季铵盐溶液备用;
3)将腐植酸钠溶于水中(固液比3:250),得到腐殖酸钠溶液备用;
4)向三口烧瓶中加入体积比为3:1:5的1)、2)、3)溶液乳化30min,加入3份丙烯酸、0.08份纳米ZnO,40℃下搅拌30min,滴加0.1份过硫酸铵与0.12份N,N-二甲基双丙烯酰胺。升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
实施例9
本发明公开了一种抗菌可生物降解智能响应水凝胶的制备方法,包括以下步骤:
1)将1份姜黄素、二氢黄酮、异黄酮(质量比为3:5:2)溶于11ml乙醚中备用;
2)将7份壳聚糖季铵盐溶于水中(固液比为2:190),加入4份聚乙二醇充分搅拌得到壳聚糖季铵盐溶液备用;
3)将腐植酸钠溶于水中(固液比为3:290),得到1%的腐植酸钠溶液备用;
4)向三口烧瓶中加入体积比为4:3:2的1)、2)、3)溶液乳化30min,加入丙烯腈、0.16份纳米TiO2,40℃下搅拌30min,滴加0.08份过硫酸钾与0.14份N,N-二甲基双丙烯酰胺。升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
针对以上几种案例制得的一种抗菌可生物降解智能响应水凝胶与市场上购买的抗菌剂(杀菌除臭剂)进行对比实验,试验结果如下所示:
一种抗菌可生物降解智能响应水凝胶测试数据:
1.抗菌试验
实验采用滤纸片法,对6mm的圆形滤纸片进行160℃、2h干热灭菌,将灭菌滤纸片放入一种抗菌可生物降解智能响应水凝胶或杀菌除臭剂中充分浸透,取出放置于无菌平皿内,自然挥干待用。
将斜面保藏菌接种到牛肉膏蛋白胨琼脂培养基,放入37℃的恒温培养箱,培养24h。取活化好的菌种,用无菌生理盐水制成105cfu/mL的菌悬液。
取上述配制好的菌悬液0.1mL,滴入固体培养基表面,用无菌涂布器均匀涂布于其上,用无菌镊子夹取浸渍色素溶液一种抗菌可生物降解智能响应水凝胶或杀菌除臭剂挥干后的滤纸片,放入平皿中。用浸渍蒸馏水挥干后的做空白对照。每个样品做3个重复。将平板放入细菌培养箱中,37℃培养24h后,取出观察,测量抑菌圈直径,取平均值。
实施案例1~9制得的一种抗菌可生物降解智能响应水凝胶和杀菌除臭剂(普通车内抗菌剂,市售)抗菌性见表1
表1抗菌性测试结果
从实验数据可以看出,市场上杀菌除臭剂的抗菌效果低于抗菌可生物降解智能响应水凝胶,实施案例1~9对金葡萄球菌与大肠杆菌均具有显著的抗菌能力。实施案例1-4与5-9对比,实施例1-4中分别采用单一黄酮类天然抗菌物质,实施例中5-9中采用了黄酮类复配作用,制备出性能更加优异的抗菌凝胶。可知,这种抗菌可生物降解智能响应水凝胶中的黄酮类天然抗菌物质、壳聚糖季铵盐与腐植酸钠三者协同作用,更有助于抑菌、杀菌。
2.降解实验测试
本发明申请中抗菌可生物降解智能响应水凝胶降解性能的测试方法如下:
称取真空干燥处理后的抗菌可生物降解智能响应水凝胶m1 g埋于具有保水能力和相对湿度为50%的土壤中培养,加入pH为2.0的硫酸溶液,并保持恒定pH,30天后取出凝胶冲洗表面杂物经真空干燥处理后称重,记录水凝胶质量m2g,按下式计算抗菌可生物降解智能响应水凝胶的降解率:
降解率测试结果如表2所示。
性能指标 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 |
90天降解率% | 53.6 | 52.7 | 56.6 | 52.4 | 57.2 |
180天降解率% | 80.6 | 76.9 | 77.6 | 76.8 | 78.3 |
性能指标 | 实施例6 | 实施例7 | 实施例8 | 实施例9 | 抗菌除臭剂 |
90天降解率% | 52.6 | 53.4 | 53.2 | 54.8 | 13.72 |
180天降解率% | 76.6 | 77.2 | 79.2 | 72.8 | 32.8 |
本实验数据可以看出用本发明的抗菌可生物降解智能响应水凝胶在使用一段时间后易于降解,在产品发挥自身作用后,可自身降解,比传统杀虫剂更加环保,而市售产品抗菌除臭剂基本上没有缓释作用,使用完会残留大量的有机成分,对周围环境安全造成隐患。
本发明主要以缓释凝胶为载体,加入黄酮类物质,壳聚糖季铵盐,腐植酸钠,聚合单体通过多元接支共聚反应得到一种可针对不同环境做出智能响应。在干燥环境下缓慢持久释放抗菌成分,避免因高剂量使用抗菌药物而产生抗药性,在潮湿环境下因凝胶吸收环境中的水分有一定溶胀改变使得气孔张开抗菌成分释放速度加快,能有效针对不同环境迅速做出响应,智能高效发挥抗菌作用,除此之外本发明加入腐殖酸钠抗菌成分,还可以有效地净化空气,吸附环境中的异味,达到多重功效。
黄酮广泛存在于自然界植物中,分子中存在酚羟基,甲氧基,异戊烯基等活性基团,能够有效抗菌,且可以降解。壳聚糖季铵盐是一种水溶性较强抗菌可生物降解大分子,是经过壳聚糖经化学修饰的助剂产品,具有优异的抗菌性,成膜性,吸附性等特点。腐殖酸钠是自然界广泛存在的大分子有机质,参与者全球碳循环,分子结构为芳环和脂环,存在羧基,羟基,羰基,甲氧基等活性基团,腐殖酸钠是一种腐殖酸的钠盐,具有强效吸附、除臭的作用,除此之外也具有抗菌、抗病毒等多重药效,纳米氧化物是一类尺寸小、比表面积大,表面的键态和颗粒内部不同及表面原子配位不等的特点,从而导致表面的活性部位增加,够有效提高其吸附、除异味等性能。
本发明方法简单,利用本方法合成智能响应抗菌水凝胶,对环境友好,可生物降解,对不同环境可做到智能响应,有强效的抗菌作用。本发明制备方法,以壳聚糖、腐殖酸钠、黄酮类物质三者为凝胶提供抗菌、吸附等活性成分,壳聚糖、聚乙二醇、腐植酸、黄酮、聚合单体发生接枝聚合反应经过搅拌得到可完全降解棕黑色凝胶物。
本发明的抗菌可生物降解智能响应水凝胶可有效缓解空气环境中的细菌微生物,降低一些因细菌感染发生的疾病。本产品较市售产品(抗菌除臭剂)给安全且可以长效发挥作用,使用可生物降解。对环境无污染隐患,是一种具有高性价的抗菌、抑菌产品。
本领域的技术人员容易理解,以上所述仅为本发明的较佳实施例而已,并不用于限制本发明的,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种抗菌可生物降解智能响应水凝胶,其特征在于,以重量份数计,其组分包括:1-3份黄酮类物质、6-12份壳聚糖、3-5份聚乙二醇、2-4份腐殖酸钠、5-8份聚合单体、0.05-0.2份纳米氧化物、0.05-0.1份引发剂、0.08-0.15份交联剂。
2.权利要求1所述的一种抗菌可生物降解智能响应水凝胶的制备方法,其特征在于,包括如下步骤:
1)将1-3份黄酮类物质溶于乙醚中备用,黄酮和乙醚的固液比为(1-3)g:(10-20)mL;
2)将6-12份壳聚糖溶于水中,壳聚糖和水的固液比为(1-2)g:(100-500)mL;
加入3-5份聚乙二醇充分搅拌得到壳聚糖溶液备用;
3)将2-4份腐植酸钠溶于水中,腐殖酸钠与水的固液比为(1-3)g:(100-300)mL;得到腐植酸钠溶液备用;
4)向三口烧瓶中加入体积比为1~5:1~5:1~5的1)、2)、3)中得到的溶液乳化30min,加入5-8份聚合单体、0.05-0.2份的纳米氧化物,40℃下搅拌30min,滴加0.05-0.1份份引发剂与0.08-0.15份交联剂;升温至80℃续搅拌至出现凝胶状产物;
5)将凝胶状产物分别用无水乙醇和水洗涤三次,60℃真空干燥24h。
3.根据权利要求2所述的一种抗菌可生物降解智能响应水凝胶的制备方法,其特征在于,黄酮类物质具体为姜黄素、二氢黄酮、异黄酮、黄酮醇中的一种。
4.根据权利要求2所述的一种抗菌可生物降解智能响应水凝胶的制备方法,其特征在于,所述黄酮类物质具体为姜黄素、二氢黄酮、异黄酮、黄酮醇中的两种或两种以上的混合。
5.根据权利要求2所述的一种抗菌可生物降解智能响应水凝胶的制备方法,其特征在于,所述壳聚糖具体为壳聚糖季铵盐。
6.根据权利要求2所述的一种抗菌可生物降解智能响应水凝胶的制备方法,其特征在于,所述聚乙二醇具体为聚乙二醇-400。
7.根据权利要求2所述的一种抗菌可生物降解智能响应水凝胶的制备方法,其特征在于,聚合单体为丙烯酸、丙烯酰胺、丙烯腈中的一种。
8.根据权利要求2所述的一种抗菌可生物降解智能响应水凝胶的制备方法,其特征在于,所述纳米氧化物具体为:纳米SiO2、纳米ZnO、纳米TiO2中的一种。
9.根据权利要求2所述的一种抗菌可生物降解智能响应水凝胶的制备方法,其特征在于,所述引发剂具体为:过硫酸钾、过硫酸钠、过硫酸铵中的一种。
10.根据权利要求2-9任一权利要求所述的一种抗菌可生物降解智能响应水凝胶的制备方法,其特征在于,所述交联剂具体为:过氧化苯甲酰、N,N-二甲基双丙烯酰胺中的一种。
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