CN108273496A - 一种基于细菌纤维素的仿生酶的制备方法及其应用 - Google Patents
一种基于细菌纤维素的仿生酶的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种基于细菌纤维素的仿生酶的制备方法及其应用。其特征在于利用细菌纤维素高温碳化合成碳纤维,并利用细菌纤维素的多孔结构及高的持水能力,通过水的交换功能在细菌纤维素中装载高浓度的高锰酸钾溶液。再经过冷冻干燥形成细菌纤维素/高锰酸钾气凝胶。然后利用高温煅烧使细菌纤维素碳化形成碳纤维,同时高锰酸钾被高温分解生成氧化锰纳米颗粒。本方法制备的碳纤维/氧化锰复合纳米材料具有较好的仿生酶活性,可以催化超氧负离子的歧化反应,应用于超氧负离子传感器的制备,在生物及医学领域具有较高的应用价值。而且本方法成本低、操作简单,便于大批量生产及推广应用。
Description
技术领域
本发明涉及一种细菌纤维素的仿生酶的制备方法,利用天然细菌纤维素负载高锰酸钾通过高温煅烧形成碳纤维/氧化锰复合纳米纤维材料,属于高分子基功能复合材料的技术。
背景技术
碳纤维是一种新型碳基纳米材料,具有极好的机械强度、很大的体积质量比、多孔网络结构。碳纤维具有纳米尺寸的直径,具有纳米材料的一般性能,碳纤维表面的边界位点可以促进表面电子转移,用于电化学器械或电化学分析。制备碳纤维的方法很多,其中最常用的是电纺丝法,可以利用聚合物溶液或熔融物合成几个纳米到几微米直径的纳米纤维。近年来,专家们发展了一些更为简单地方法制备碳纳米纤维。有的利用一些天然的植物纤维,如:棉花、树叶、细菌纤维素等材料,经化学或物理方法处理合成碳纤维用于能源及传感领域。
细菌纤维素是一种由特定的细菌如Acetobacter、Agrobacterium等产出的有机聚合物材料。与普通的植物纤维素相比,细菌纤维素具有纯度高、直径小、机械强度高、持水性好等优点,是合成其他纳米材料的理想载体。例如,利用细菌纤维素作为模板,可以合成银纳米颗粒掺杂的复合纳米纤维;合成细菌纤维/CdTe量子点复合材料用于制备pH及葡萄糖传感器;或者利用高温煅烧的方法合成碳纤维用检测Cd(II)、Pb(II)等金属离子。但是利用细菌纤维素合成碳纤维基的复合材料研究较少,对碳纤维/氧化锰复合纳米材料的相关研究还未见报道。
本专利提供以细菌纤维素和高锰酸钾为原料制备碳纤维/氧化锰复合纳米材料的制备方法及其在超氧负离子检测中的应用。
发明内容
本发明的目的是提供一种基于细菌纤维素的仿生酶的制备方法,可以简单有效制备出碳纤维/氧化锰复合纳米纤维材料。该复合纳米材料具有仿生酶的催化活性,对超氧阴离子的歧化反应具有较强的催化作用,可以用于生物医学研究及生物传感器的制备。
基于细菌纤维素的仿生酶的制备方法,包含如下制备步骤:
(1)提供一种天然细菌纤维素;
(2)将天然细菌纤维素在磁力搅拌下,用10%乙醇水溶液浸泡之后,再用去离子水浸泡并更换去离子水,以去除含有的有机溶剂及其它杂质;
(3)将步骤(2)得到的细菌纤维素浸料在高锰酸钾溶液中浸泡,在磁力搅拌下反应1天,装载高锰酸钾,将反应后的细菌纤维素用去离子水清洗冲洗3-5次,去除过量的高锰酸钾,得到细菌纤维素/高锰酸钾水凝胶;
(4)将步骤(3)得到细菌纤维素/高锰酸钾水凝胶放入液氮中冷冻,再放入冷冻干燥箱(-80 ℃,0.021 Mpa)中冷冻干燥,制得细菌纤维/高锰酸钾气凝胶;
(5)将步骤(4)得到的细菌纤维素/高锰酸钾气凝胶在管式炉中氮气保护下高温煅烧,形成碳纤维/氧化锰复合纳米材料,即得到基于细菌纤维素的仿生酶。
进一步,所述步骤(2)的用10%乙醇水溶液浸泡的时间为1小时,用去离子水中浸泡时间为3天,更换去离子水的次数为3-6次。
进一步,所述步骤(3)的高锰酸钾溶液的浓度为1~40 mM,高锰酸钾溶液中浸泡的时间为12~24小时。
优选的,所述步骤(3)的高锰酸钾溶液的浓度为20mM。
进一步,所述步骤(4)的在液氮中冷冻的时间为30分钟,冷冻干燥时间为12~24小时。
优选的,所述步骤(5)的高温煅烧的过程为,升温速度为2 ºC/分钟,在250 ºC 保持1小时,接着在450 ºC保持1小时,最后在800 ºC保持2小时。
根据上述制备方法得到的碳纤维/氧化锰复合纳米材料,在仿生酶的活性和催化超氧负离子的歧化反应的生物及医学的应用。
本发明的有益效果是:
(1)本发明提供的碳纤维/氧化锰复合纳米材料是经过高温处理高锰酸钾加载的细菌纤维素形成的,合成成本低有利于推广应用。
(2)本发明获得的碳纤维/氧化锰复合纳米材料中碳纤维的直径大约为10~30nm。
(3)本发明获得的碳纤维/氧化锰复合纳米材料,当高锰酸钾浓度为20mM时,得到的复合材料中氧化锰质量分数为1.6~ 3.5%时,氧化锰的颗粒大小为30~70nm。
(4)本发明获得的碳纤维/氧化锰复合纳米材料对超氧负离子的歧化反应具有较强的催化性能,对于生物医学研究及生物传感器的制备具有很大的应用价值。
(5)本发明提供的制备简单可行,易于操作,拓宽了细菌纤维素及纳米氧化锰的应用领域,赋予了细菌纤维素新的应用领域,制备的复合材料具有很高的经济价值。
附图说明
为了使本发明的目的和技术方案有益效果更加清楚,本发明提供如下附图:
图1为实施例1的碳纤维/氧化锰复合纳米材料的合成方法。
图2为实施例1的碳纤维/氧化锰复合纳米材料的扫描电子显微镜微观形貌图。
图3为实施例1的碳纤维/氧化锰复合纳米材料的透射电子显微镜微观形貌图。
图4为实施例1的碳纤维/氧化锰复合纳米材料的粉末衍射图谱。
图5为实施例1的碳纤维/氧化锰复合纳米材料对超氧负离子的电化学响应图。
图6为实施例1的碳纤维/氧化锰复合纳米材料对超氧负离子的检测标准曲线。
具体实施方式
下面结合具体实施方式对本发明进行详细说明。
实施例1
合成步骤示意图如图1所示,具体为:
(1)将细菌纤维素原料切成3cm×3cm×0.5cm小块,先在10%乙醇水溶液中浸泡1小时,然后在去离子水中浸泡3天,以除去含有的有机溶剂及其他杂质。
(2)在磁力搅拌作用下,将细菌纤维素在20mM高锰酸钾溶液中浸泡1天。然后取出并用去离子水清洗冲洗3-5次,除去过量的高锰酸钾,得到细菌纤维/高锰酸钾水凝胶。
(3)将细菌纤维素/高锰酸钾水凝胶在液氮中冷冻30分钟,然后置于冷冻干燥箱中(-80 ℃,0.021 Mpa)冷冻干燥24小时,制得细菌纤维/高锰酸钾气凝胶。
(4)将细菌纤维素/高锰酸钾气凝胶在管式炉中(氮气保护下),以800 ºC高温煅烧2小时。然后自然冷却到室温,即得到碳纤维/氧化锰复合纳米材料。
通过图2 的扫描电子显微镜图、图3的透射电镜图和图4的粉末衍射图谱可以看到碳纤维/氧化锰复合纳米材料的微观形貌和特征峰,说明成功制备出了碳纤维/氧化锰复合纳米材料。
接着将1mg合成的碳纤维/氧化锰复合纳米材料与50 μL nafion加入到450 μL乙醇中超声分散,然后取5μL混合溶液滴到磨好的玻碳电极表面,室温下干燥2小时。然后用以0.64 V的恒定电位,进行电化学响应和对超氧负离子的检测的实验。图5为碳纤维/氧化锰复合纳米材料对超氧负离子的电化学响应图,图6为碳纤维/氧化锰复合纳米材料对超氧负离子的检测标准曲线,通过图5和图6可以证明碳纤维/氧化锰复合纳米材料可以很好检测生物体系中肿瘤细胞释放的超氧根负离子,所以碳纤维/氧化锰复合纳米材料具有在仿生酶和催化超氧负离子的歧化反应的生物及医学的应用。
Claims (7)
1.一种基于细菌纤维素的仿生酶的制备方法,包含如下制备步骤:
(1)提供一种天然细菌纤维素;
(2)将天然细菌纤维素在磁力搅拌下,用10%乙醇水溶液浸泡之后,再用去离子水浸泡并更换去离子水,以去除含有的有机溶剂及其它杂质;
(3)将步骤(2)得到的细菌纤维素浸料在高锰酸钾溶液中浸泡,在磁力搅拌下反应1天,装载高锰酸钾,将反应后的细菌纤维素用去离子水清洗冲洗3-5次,去除过量的高锰酸钾,得到细菌纤维素/高锰酸钾水凝胶;
(4)将步骤(3)得到细菌纤维素/高锰酸钾水凝胶放入液氮中冷冻,再放入冷冻干燥箱(-80 ℃,0.021 Mpa)中冷冻干燥,制得细菌纤维/高锰酸钾气凝胶;
(5)将步骤(4)得到的细菌纤维素/高锰酸钾气凝胶在管式炉中氮气保护下高温煅烧,形成碳纤维/氧化锰复合纳米材料,即得到基于细菌纤维素的仿生酶。
2.根据权利要求1所述的一种基于细菌纤维素的仿生酶的制备方法,其特征在于,所述步骤(2)的用10%乙醇水溶液浸泡的时间为1小时,用去离子水中浸泡时间为3天,更换去离子水的次数为3-6次。
3.根据权利要求1所述的一种基于细菌纤维素的仿生酶的制备方法,其特征在于,所述步骤(3)的高锰酸钾溶液的浓度为1~40 mM,高锰酸钾溶液中浸泡的时间为12~24小时。
4.根据权利要求3所述的一种基于细菌纤维素的仿生酶的制备方法,其特征在于,所述步骤(3)的高锰酸钾溶液的浓度为20mM。
5.根据权利要求1所述的一种基于细菌纤维素的仿生酶的制备方法,其特征在于,所述步骤(4)的在液氮中冷冻的时间为30分钟,冷冻干燥时间为12~24小时。
6.根据权利要求1所述的一种基于细菌纤维素的仿生酶的制备方法,其特征在于,所述步骤(5)的高温煅烧的过程为,升温速度为2 ºC/分钟,在250 ºC 保持1小时,接着在450 ºC保持1小时,最后在800 ºC保持2小时。
7.权利要求1~6任意一项所述的基于细菌纤维素的仿生酶的制备方法得到的碳纤维/氧化锰复合纳米材料,在仿生酶的活性和催化超氧负离子的歧化反应的生物及医学的应用。
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