CN111208185B - 一种复合纳米材料的制备方法 - Google Patents
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Abstract
本发明公开一种复合纳米材料的制备方法。将镍盐、钴盐、铁盐、亚铁盐以及阳离子交联剂加入去离子水中，磁力搅拌分散均匀后缓慢加入水合肼、l氢氧化钠、聚丙烯酸钠，搅拌均匀后得到混合液；将上述混合液转移到不锈钢反应釜中，在110～140℃温度下反应12～24h；反应结束后，自然冷却至室温，将所得产物过滤、蒸馏水冲洗、烘干得到Ni‑Co/Fe3O4复合纳米材料。本发明采用亲水性高分子聚合物聚丙烯酸钠与交联剂在水溶液中交联形成凝胶，限制了Ni‑Co/Fe3O4复合纳米材料的生长，能获得尺寸小,分散性好的Ni‑Co/Fe3O4复合纳米材料，并具有优异的葡萄糖传感性能。
Description
技术领域
本发明属于电化学传感技术领域，涉及一种复合纳米材料的制备方法，具体是一种Ni-Co/Fe3O4葡萄糖传感用纳米复合材料的制备方法。
背景技术
糖尿病作为一种全球性的慢性疾病，源于胰岛素缺乏症，其特点是血糖水平升高。此外，糖尿病会导致一系列继发性并发症例如心脏病，失明或肾衰竭。通过对糖尿病患者血糖含量的准确检测，可以有效地对糖尿病进行监测和治疗，因此葡萄糖的定量分析在临床医学上具有十分重要的意义。电化学传感器方法尤其是无酶葡萄糖电化学传感器由于不受酶易变性失活的影响，并具有灵敏度高、检出限低、操作简便的优点在葡萄糖的定量分析中扮演了重要的角色。进一步，电极活性材料的成分和结构无疑对无酶葡萄糖电化学传感器的性能有至关重要的作用。最近，双金属材料尤其是双金属与其他材料形成复合纳米结构由于其出色的催化性能、优异的生物相容性和出色的稳定性在葡萄糖无酶传感检测方面受到越来越多的关注。P.Vennila等(Ni-Co/Fe3O4 flower-like nanocomposite highlysensitive selective enzyme free glucose sensor applications，Journal of alloysand compounds,2017,703,633-642)采用湿化学方法制备了Ni、Co与Fe3O4复合纳米材料，并应用于葡萄糖传感检测，但获得的Ni-Co/Fe3O4复合纳米颗粒的尺寸大小为亚微米级并且严重团聚，限制了其葡萄糖传感性能。
发明内容
本发明目的在于针对现有Ni-Co/Fe3O4复合纳米颗粒尺寸大且严重团聚的不足，提供一种Ni-Co/Fe3O4复合纳米材料的制备方法。
本发明的一种Ni-Co/Fe3O4纳米复合材料的制备方法具体包括步骤：
1)将1～3mmol的镍盐、2～6mmol钴盐、0.2～0.6mol铁盐、0.1～0.3mol亚铁盐以及0.05～0.1mmol阳离子交联剂加入50～100ml去离子水中，磁力搅拌分散均匀后缓慢加入0.03～0.06mol的水合肼、0.03～0.06mol氢氧化钠、0.5～1.0g聚丙烯酸钠，搅拌均匀后得到混合液；
2)将上述混合液转移到不锈钢反应釜中，在110～140℃温度下反应12～24h；
3)反应结束后，自然冷却至室温，将所得产物过滤、蒸馏水冲洗、烘干得到Ni-Co/Fe3O4复合纳米材料。
所述的镍盐为Ni(NO3)2·6H2O、NiCl2·6H2O或NiCl2；
所述的钴盐为Co(NO3)2·6H2O、CoCl2·6H2O或CoCl2；
所述的铁盐为FeCl3或FeCl3·6H2O；
所述的亚铁盐为FeCl2·4H2O、FeCl2或FeSO4·7H2O；
所述的阳离子交联剂为十二烷基三甲基溴化铵，十四烷基三甲基溴化铵或十六烷基三甲基溴化铵；
所述的聚丙烯酸钠，分子量为500～700万。
本发明采用亲水性高分子聚合物聚丙烯酸钠与阳离子交联剂在水溶液中交联形成凝胶，限制了结晶材料的生长，能获得尺寸小,分散性良好的Ni-Co/Fe3O4复合纳米材料，并具有优异的葡萄糖传感性能。
具体实施方式
下面结合具体实施例对本发明做进一步的分析。
实施例1：
称取1mmolNiCl2·6H2O、2mmol CoCl2·6H2O、0.2mol FeCl3、0.1mol FeCl2·4H2O以及0.05mmol十二烷基三甲基溴化铵加入到50ml去离子水中。磁力搅拌分散均匀后缓慢加入0.03mol水合肼和0.03mol氢氧化钠。然后再加入0.5g聚丙烯酸钠，并搅拌均匀。将所得溶液转移到不锈钢反应釜中，在温度110℃下反应时间24h。反应结束后，自然冷却至室温，将所得产物过滤、蒸馏水冲洗、烘干得到Ni-Co/Fe3O4复合纳米材料。
实施例2：
称取3mmol Ni(NO3)2·6H2O、6mmol Co(NO3)2·6H2O、0.6mol FeCl3·6H2O、0.3molFeSO4·7H2O以及0.1mmol十二烷基三甲基溴化铵加入到100ml去离子水中。磁力搅拌分散均匀后缓慢加入0.06mol的水合肼和0.06mol氢氧化钠。然后再加入1.0g聚丙烯酸钠，并搅拌均匀。将所得溶液转移到不锈钢反应釜中，在温度140℃下反应时间12h。反应结束后，自然冷却至室温，将所得产物过滤、蒸馏水冲洗、烘干得到Ni-Co/Fe3O4复合纳米材料。
实施例3：
称取2mmol NiCl2、4mmol CoCl2、0.4mol FeCl3·6H2O、0.2mol FeCl2·4H2O以及0.08mmol十二烷基三甲基溴化铵加入到80ml去离子水中。磁力搅拌分散均匀后缓慢加入0.05mol的水合肼和0.05mol氢氧化钠。然后再加入0.7g聚丙烯酸钠，并搅拌均匀。将所得溶液转移到不锈钢反应釜中，在温度130℃下反应时间17h。反应结束后，自然冷却至室温，将所得产物过滤、蒸馏水冲洗、烘干得到Ni-Co/Fe3O4复合纳米材料。
实施例4：
称取1.5mmol Ni(NO3)2·6H2O、3mmol Co(NO3)2·6H2O、0.3mol FeCl3·6H2O、0.15mol FeCl2·4H2O以及0.06mmol十四烷基三甲基溴化铵加入到60ml去离子水中。磁力搅拌分散均匀后缓慢加入0.04mol水合肼和0.05mol氢氧化钠。然后再加入0.7g聚丙烯酸钠，并搅拌均匀。将所得溶液转移到不锈钢反应釜中，在温度120℃下反应时间20h。反应结束后，自然冷却至室温，将所得产物过滤、蒸馏水冲洗、烘干得到Ni-Co/Fe3O4复合纳米材料。
实施例5：
称取2.5mmol NiCl2·6H2O、5mmolCoCl2·6H2O、0.4mol FeCl3·6H2O、0.2molFeCl2以及0.09mmol十二烷基三甲基溴化铵加入到90ml去离子水中。磁力搅拌分散均匀后缓慢加入0.045mol的水合肼和0.05mol氢氧化钠。然后再加入0.8g聚丙烯酸钠，并搅拌均匀。将所得溶液转移到不锈钢反应釜中，在温度135℃下反应时间15h。反应结束后，自然冷却至室温，将所得产物过滤、蒸馏水冲洗、烘干得到Ni-Co/Fe3O4复合纳米材料。
实施例6：
称取1.8mmol Ni(NO3)2·6H2O、2.2mmol Co(NO3)2·6H2O、0.34mol FeCl3、0.2molFeSO4·7H2O以及0.07mmol十六烷基三甲基溴化铵加入到70ml去离子水中。磁力搅拌分散均匀后缓慢加入0.04mol水合肼和0.04mol氢氧化钠。然后再加入0.7g聚丙烯酸钠，并搅拌均匀。将所得溶液转移到不锈钢反应釜中，在温度125℃下反应时间17h。反应结束后，自然冷却至室温，将所得产物过滤、蒸馏水冲洗、烘干得到Ni-Co/Fe3O4复合纳米材料。
性能分析实验：
葡萄糖传感性能使用CHI630D电化学分析工作站的三电极体系进行测试。将5mg上述实施例Ni-Co/Fe3O4复合纳米材料样品溶于5mL无水乙醇中，并加入20μLNafion溶液，超声振荡直到样品完全分散到溶液中。取20μL的样品分散液涂抹到已清理的裸玻碳电极上，待其晾干即获得工作电极。对电极为铂电极，参比电极为银/氯化银电极。电解质溶液为0.1M的氢氧化钠溶液。所有电化学测试使用的溶液都需用高纯氮去氧至少15min以去除溶液中的溶解氧且提高葡萄糖催化氧化效率，计时电流法设定恒定电压0.5V。手动操作移液枪完成葡萄糖的连续加入。样品的颗粒粒度使用激光粒度分析仪分析。
表1为各实例样品的颗粒粒度和葡萄糖传感性能
上述实施例并非是对于本发明的限制，本发明并非仅限于上述实施例，只要符合本发明要求，均属于本发明的保护范围。
Claims (5)
1.一种复合纳米材料的制备方法，其特征在于包括以下步骤：
1）将1～3 mmol的镍盐、2～6 mmol钴盐、0.2～0.6 mol 铁盐、0.1～0.3 mol 亚铁盐以及0.05～0.1mmol阳离子交联剂加入去离子水中，磁力搅拌分散均匀后缓慢加入0.03～0.06 mol的水合肼、0.03～0.06 mol氢氧化钠、0.5～1.0g分子量为500～700万的聚丙烯酸钠，搅拌均匀后得到混合液；所述阳离子交联剂为十二烷基三甲基溴化铵，十四烷基三甲基溴化铵或十六烷基三甲基溴化铵；
2）将上述混合液转移到不锈钢反应釜中，在110～140℃温度下反应12～24h；
3）反应结束后，自然冷却至室温，将所得产物过滤、蒸馏水冲洗、烘干得到Ni-Co/ Fe3O4复合纳米材料。
2.如权利要求1所述的一种复合纳米材料的制备方法，其特征在于所述的镍盐为Ni（NO3）2·6H2O、NiCl2·6H2O或NiCl2。
3.如权利要求1-2任一所述的一种复合纳米材料的制备方法，其特征在于所述的钴盐为Co（NO3）2·6H2O、CoCl2·6H2O或CoCl2。
4.如权利要求3所述的一种复合纳米材料的制备方法，其特征在于所述的铁盐为FeCl3或FeCl3·6H2O。
5.如权利要求4所述的一种复合纳米材料的制备方法，其特征在于所述的亚铁盐为FeCl2·4H2O、FeCl2或FeSO4·7H2O。
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