CN113797909B - 碳点诱导合成Co9S8/C双功能纳米酶的方法 - Google Patents
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Abstract
本发明提供一种碳点诱导合成Co9S8/C双功能纳米酶的方法，该方法将超小的Co9S8纳米颗粒掺入到由CDs拼接形成的多孔二维碳纳米片中。所制备的纳米材料孔结构丰富，具有大的比表面积和出色的双功能纳米酶性能，可以在不施加任何外部能量的情况下模拟过氧化物酶(POD)和氧化酶(OXD)的催化活性，可作为抗坏血酸(AA)的比色传感器，具有较好的抗干扰能力和优异的灵敏度。
Description
技术领域
本发明属于新材料领域，具体涉及一种碳点诱导合成Co9S8/C双功能纳米酶的方法。
背景技术
催化反应的进行需要变价金属离子，如Fe2+/3+，Co2+/3+，Cu1+/2+和Ce3+/4+等，因此，许多含有变价元素的纳米材料表现出模拟酶活性，有望成为天然酶的替代品。天然酶通常制造和储存昂贵，转移不稳定，对恶劣环境敏感。过渡金属Co可形成多种硫化物，如CoS，CoS2,Co2S3，Co3S4和Co9S8等，但其催化活性普遍较低。这主要源于两个方面的原因：首先，它们的纳米粒子不容易赋予小纳米尺寸和均匀分布，限制了活性位点的可及性。其次，与碳基材的弱锚定力使其纳米颗粒不稳定且容易团聚，导致耐久性差。纳米空间限域法在某种程度上克服了上述问题，然而，其制备程序复杂、繁琐、低效且昂贵。
作为一类新的零维(0D)荧光纳米材料，碳点(CDs)因其优秀的电子、光学、物理化学性质以及低成本在如生物医学、化学传感、光催化、电催化，发光二极管，太阳能电池，锂/钠离子电池等领域得到了广泛的应用。从结构上看，CDs由一个羧酸、醇和胺等极性基团组成的壳所包裹的碳核组成。CDs表面的这些杂原子基团从反应性、结合性和氧化还原性质等方面决定了CDs与周围环境的相互作用。例如，通过这些表面基团，CDs可以与大量金属离子(如Fe3+、Ni2+、Cu2+、Ru3+、Co2+)络合，使金属前体稳定的吸附其上。因此，CDs可用作多功能载体或纳米尺寸的模板，以防止在纳米复合材料的制备过程中发生严重的聚集。此外，先前的工作已经证明，CDs可以在高温下拼接成二维(2D)碳纳米片，并导致在其表面形成的产物受到限制。这种策略不仅抑制了新形成的纳米结构的团聚，而且促进了它们在使用中的性能稳定性。
发明内容
为提高钴硫化物的催化活性，克服现有方法复杂、繁琐、低效且昂贵的缺点，提出一种碳点诱导合成Co9S8/C双功能纳米酶的方法，将超小的Co9S8纳米颗粒掺入到由CDs拼接形成的多孔二维碳纳米片中，获得具有大的比表面积、高性能的双功能纳米酶。
为解决上述技术问题，本发明采用的技术方案是：
碳点诱导合成Co9S8/C双功能纳米酶的方法，采用以下步骤：
步骤1将0.075～0.125g CDs粉末加入到15mL无水乙醇或去离子水中，在25℃～35℃、频率20～30KHz环境下超声分散0.5～1h，配制成浓度为5～8.3g/L的碳点溶液；
步骤2将0.075～0.125g氨基磺酸钴溶于15mL体积浓度为25v/v％的氨水溶液中，在25℃～35℃、频率20～30KHz环境下超声分散0.5～1h，配制成浓度为5～8.3g/L的氨基磺酸钴-氨水混合溶液；
步骤3将步骤1得到的碳点溶液在剧烈搅拌下滴加到步骤2得到的氨基磺酸钴-氨水混合溶液中，并持续搅拌0.5～1h，然后将混合溶液放置于电热鼓风干燥箱中，在温度为70～90℃环境下烘干得到固体粉末；
步骤4将步骤3得到的固体粉末研磨0.25～0.5h；
步骤5将由步骤4研磨后的固体粉末放置于管式炉中，以氩气或氮气为保护气体，在温度550～750℃下煅烧2～4h，管式炉升温速率为2～8℃/min，氩气气流量为10～30sccm；然后将管式炉自然冷却到室温，最终得到Co9S8/C双功能纳米酶。
所述CDs粉末依据专利ZL201610534465.4公开的利用煤质沥青制备多色发光可调碳点的方法，采用甲酸与双氧水选择性刻蚀煤沥青获得。
本发明公开碳点诱导合成Co9S8/C双功能纳米酶的方法简便，所制备的纳米材料孔结构丰富，具有大的比表面积和出色的双功能纳米酶性能，可以在不施加任何外部能量的情况下模拟过氧化物酶(POD)和氧化酶(OXD)的催化活性，可作为抗坏血酸(AA)的比色传感器，具有较好的抗干扰能力和优异的灵敏度。
附图说明
图1为本发明制备获得Co9S8/C双功能纳米酶的X射线衍射图谱；
图2为本发明制备获得Co9S8/C双功能纳米酶的透射电镜测试结果；
图3为本发明制备获得Co9S8/C双功能纳米酶的高分辨透射电镜测试结果；
图4为本发明制备获得Co9S8/C双功能纳米酶在添加双氧水(H2O2)的情况下氧化3,3',5,5'-四甲基联苯胺(TMB)底物后溶液的紫外-可见吸收光谱；
图5为本发明制备获得Co9S8/C双功能纳米酶在不添加双氧水(H2O2)的情况下氧化3,3',5,5'-四甲基联苯胺(TMB)底物后溶液的紫外-可见吸收光谱；
图6为Co9S8/C+H2O2+TMB反应体系，固定Co9S8/C和TMB浓度，催化反应速度与双氧水(H2O2)浓度之间的关系；
图7为Co9S8/C+H2O2+TMB反应体系，固定Co9S8/C和H2O2浓度，催化反应速度与TMB浓度之间的关系；
图8为Co9S8/C+TMB反应体系，固定Co9S8/C浓度，催化反应速度与TMB浓度之间的关系；
图9为Co9S8/C+H2O2+TMB反应体系中，加入不同浓度抗坏血酸(AA)后，紫外-可见吸收光谱的叠加图；
图10为Co9S8/C+H2O2+TMB反应体系中，加入不同浓度抗坏血酸(AA)后，反应溶液652nm处吸光度的变化量与AA浓度的关系的线性拟合结果。
具体实施方式
以下结合附图介绍本发明详细技术方案：
碳点诱导合成Co9S8/C双功能纳米酶的方法，采用以下步骤：
步骤1将0.075～0.125g CDs粉末加入到15mL无水乙醇或去离子水中，在25℃～35℃、频率20～30KHz环境下超声分散0.5～1h，配制成浓度为5～8.3g/L的碳点溶液；
步骤2将0.075～0.125g氨基磺酸钴(Co(SO3NH2)2·xH2O)溶于15mL体积浓度为25v/v％的氨水溶液中，在25℃～35℃、频率20～30KHz环境下超声分散0.5～1h，配制成浓度为5～8.3g/L的氨基磺酸钴-氨水混合溶液；
步骤3将步骤1得到的碳点溶液在剧烈搅拌下滴加到步骤2得到的氨基磺酸钴-氨水混合溶液中，并持续搅拌0.5～1h，然后将混合溶液放置于电热鼓风干燥箱中，在温度为70～90℃环境下烘干得到固体粉末；
步骤4将步骤3得到的固体粉末研磨0.25～0.5h；
步骤5将由步骤4研磨后的固体粉末放置于管式炉中，以氩气或氮气为保护气体，在温度550～750℃下煅烧2～4h，管式炉升温速率为2～8℃/min，氩气气流量为10～30sccm；然后将管式炉自然冷却到室温，最终得到Co9S8/C双功能纳米酶。
所述CDs粉末依据专利ZL201610534465.4公开的利用煤质沥青制备多色发光可调碳点的方法，采用甲酸与双氧水选择性刻蚀煤沥青获得。
实施例1
碳点诱导合成Co9S8/C双功能纳米酶的方法，采用以下步骤：
步骤1将0.1g CDs粉末加入到15mL无水乙醇或去离子水中，在35℃、频率30KHz环境下超声分散1h，配制成浓度为6.7g/L的碳点溶液；
步骤2将0.1g氨基磺酸钴溶于15mL体积浓度为25v/v％的氨水溶液中，在35℃、频率30KHz环境下超声分散1h，配制成浓度为6.7g/L的氨基磺酸钴-氨水混合溶液；
步骤3将步骤1得到的碳点溶液在剧烈搅拌下滴加到步骤2得到的氨基磺酸钴-氨水混合溶液中，并持续搅拌1h，然后将混合溶液放置于电热鼓风干燥箱中，在温度为90℃环境下烘干得到固体粉末；
步骤4将步骤3得到的固体粉末研磨0.5h；
步骤5将由步骤4研磨后的固体粉末放置于管式炉中，以氩气或氮气为保护气体，在温度700℃下煅烧4h，管式炉升温速率为5℃/min，氩气气流量为30sccm；然后将管式炉自然冷却到室温，最终得到Co9S8/C双功能纳米酶。
对制备获得的Co9S8/C双功能纳米酶进行表征。本发明制备获得Co9S8/C双功能纳米酶的X射线衍射图谱见图1，图谱显示的衍射峰与Co9S8标准卡片(PDF#75-2023)相一致。
本发明制备获得Co9S8/C双功能纳米酶的透射电镜测试结果见图2，从图中可以看到黑色纳米颗粒均匀分布在浅黑色碳基底上。
本发明制备获得Co9S8/C双功能纳米酶的高分辨透射电镜测试结果如图3所示，图中测得晶粒晶格条纹距离为0.29nm，与Co9S8(311)晶面间距相符，说明黑色颗粒是Co9S8纳米颗粒。
本发明制备获得Co9S8/C双功能纳米酶在添加双氧水(H2O2)的情况下氧化3,3',5,5'-四甲基联苯胺(TMB)底物后溶液的紫外-可见吸收光谱见图4，说明其具有类过氧化物酶活性。
本发明制备获得Co9S8/C双功能纳米酶在不添加双氧水(H2O2)的情况下氧化3,3',5,5'-四甲基联苯胺(TMB)底物后溶液的紫外-可见吸收光谱如图5所示，说明其具有类氧化物酶活性。
本发明制备获得Co9S8/C双功能纳米酶的类过氧化物酶催化反应动力学模型见图6和图7，由图可见，其类过氧化物酶催化反应动力学模型遵循典型Michaelis-Menten动力学模型。
本发明制备获得Co9S8/C双功能纳米酶的类氧化物酶催化反应动力学模型见图8，由图可见，其类氧化物酶催化反应动力学模型也遵循典型Michaelis-Menten动力学模型。
图9和图10说明本发明制备获得Co9S8/C双功能纳米酶可以用作比色检测AA。
Claims (2)
1.碳点诱导合成Co9S8/C双功能纳米酶的方法，其特征在于：采用以下步骤：
步骤1将0.075～0.125g CDs粉末加入到15mL无水乙醇或去离子水中，在25℃～35℃、频率20～30KHz环境下超声分散0.5～1h，配制成浓度为5～8.3g/L的碳点溶液；
步骤2将0.075～0.125g氨基磺酸钴溶于15mL体积浓度为25v/v％的氨水溶液中，在25℃～35℃、频率20～30KHz环境下超声分散0.5～1h，配制成浓度为5～8.3g/L的氨基磺酸钴-氨水混合溶液；
步骤3将步骤1得到的碳点溶液在剧烈搅拌下滴加到步骤2得到的氨基磺酸钴-氨水混合溶液中，并持续搅拌0.5～1h，然后将混合溶液放置于电热鼓风干燥箱中，在温度为70～90℃环境下烘干得到固体粉末；
步骤4将步骤3得到的固体粉末研磨0.25～0.5h；
步骤5将由步骤4研磨后的固体粉末放置于管式炉中，以氩气或氮气为保护气体，在温度550～750℃下煅烧2～4h，管式炉升温速率为2～8℃/min，氩气气流量为10～30sccm；然后将管式炉自然冷却到室温，最终得到Co9S8/C双功能纳米酶。
2.根据权利要求1所述的碳点诱导合成Co9S8/C双功能纳米酶的方法，其特征在于：所述CDs粉末利用煤质沥青制备多色发光可调碳点的方法，采用甲酸与双氧水选择性刻蚀煤沥青获得。
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