CN102175732B - 一种席夫碱配合物修饰碳纳米管电极的制备方法 - Google Patents

一种席夫碱配合物修饰碳纳米管电极的制备方法 Download PDF

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CN102175732B
CN102175732B CN 201010581529 CN201010581529A CN102175732B CN 102175732 B CN102175732 B CN 102175732B CN 201010581529 CN201010581529 CN 201010581529 CN 201010581529 A CN201010581529 A CN 201010581529A CN 102175732 B CN102175732 B CN 102175732B
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CN102175732A (zh
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刘峥
王松梅
张小鸽
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Suzhou Shengze science and Technology Pioneer Park Development Co.,Ltd.
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Guilin University of Technology
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Abstract

本发明公开了一种席夫碱配合物修饰碳纳米管电极的制备方法。截取约4cm长的铜棒(φ＝2.0mm)，把铜棒两端磨平，并清洗干净；将直径4mm的碳棒磨细，切下约1mm厚的碳片塞入直径为3.5mm、长为4cm的玻璃管中；碳片与玻璃管顶端留出1mm的距离，从另一端插入上述铜棒做引线，顶端用石蜡固定。称取0.013-0.017g电活性物质吡啶-4-甲醛缩甘氨酸席夫碱镍(Ⅱ)配合物，0.035-0.075g碳纳米管，0.01-0.05g固体石蜡，加热熔化，迅速搅拌，填入上述玻璃管预留的1mm碳片薄层处，冷却后在称量纸上抛光，即制得吡啶-4-甲醛缩甘氨酸席夫碱镍(Ⅱ)配合物修饰碳纳米管电极。本发明制作方法简单，制备的电极对甲醛有较高的电催化氧化活性，可应用于环境样品中甲醛的分析测定。

Description

一种席夫碱配合物修饰碳纳米管电极的制备方法
技术领域
本发明属电化学技术领域，特别涉及一种席夫碱配合物修饰碳纳米管电极的制备方法。
背景技术
目前，席夫碱及其配合物种类繁多，结构多样，有许多独特的性能，在分析化学、医药领域、催化领域、腐蚀领域、光致变色等许多方面应用非常广泛。在分析化学领域，含硫Schiff碱作为良好配体，可以用来鉴别、鉴定金属离子并可借助色谱分析、荧光分析、光度分析等手段达到对某些有机小分子和金属离子的定量分析，且效果十分理想，但席夫碱配合物修饰碳纳米管电极对甲醛电催化氧化的研究则少有报道。甲醛是无色、具有强烈气味的刺激性气体，其35％～40％的水溶液通称福尔马林。甲醛是原浆毒物，能与蛋白质结合，吸入后会对人体产生很大危害。因此，对甲醛的环境监测方法与技术的研究一直引起广泛的关注。化学修饰电极因其测试速度快、准确度高、便于携带等特点越来越得到人们的重视，因此，研究新型化学修饰剂的制备及相关电极的制作方法至关重要。
发明内容
本发明的目的是提供一种能分析检测甲醛的席夫碱配合物修饰碳纳米管电极的制备方法。
具体步骤为：
截取约4cm长的铜棒(φ＝2.0mm)，把铜棒两端磨平，并清洗干净；将直径4mm的碳棒磨细，切下约1mm厚的碳片塞入直径为3.5mm、长为4cm的玻璃管中；碳片与玻璃管顶端留出1mm的距离，从另一端插入上述铜棒做引线，顶端用石蜡固定。称取0.013-0.017g电活性物质吡啶-4-甲醛缩甘氨酸席夫碱镍(Ⅱ)配合物，0.035-0.075g碳纳米管，0.01-0.05g固体石蜡，加热熔化，迅速搅拌，填入上述玻璃管预留的1mm碳片薄层处，冷却后在称量纸上抛光，即制得吡啶-4-甲醛缩甘氨酸席夫碱镍(Ⅱ)配合物修饰碳纳米管电极。
本发明以吡啶-4-甲醛为原料，制备了新的吡啶-4-甲醛缩甘氨酸席夫碱镍(Ⅱ)配合物，并以此作为化学修饰剂或电活性物质，研制了吡啶-4-甲醛缩甘氨酸席夫碱镍(Ⅱ)配合物修饰碳纳米管电极，发现该电极对甲醛有较好的电催化氧化活性。在甲醛浓度为0.1g/L～0.5g/L范围内，甲醛的浓度与氧化峰电流成线性关系，这表明可利用这一修饰碳纳米管电极对甲醛作定量分析。
本发明制备了4种吡啶-4-甲醛席夫碱镍(Ⅱ)配合物修饰剂，用循环伏安法测出含有甲醛的氧化峰电流值与不含甲醛的氧化峰电流值之差，即修饰碳纳米管电极对甲醛的电催化氧化电流，结果表明4种吡啶-4-甲醛席夫碱镍(Ⅱ)配合物都有一定的催化活性，其中吡啶-4-甲醛缩甘氨酸席夫碱镍(Ⅱ)配合物对甲醛的电催化氧化活性最高，是一种理想的电活性物质。
本发明制作方法简单，制备的电极对甲醛有较高的电催化氧化活性，可应用于环境样品中甲醛的分析测定。
具体实施方式
实施例：
截取约4cm长的铜棒(φ＝2.0mm)，把铜棒两端磨平，并清洗干净；将直径4mm的碳棒磨细，切下约1mm厚的碳片塞入直径为3.5mm、长为4cm的玻璃管中；碳片与玻璃管顶端留出1mm的距离，从另一端插入上述铜棒做引线，该顶端用石蜡固定。称取0.015g电活性物质吡啶-4-甲醛缩甘氨酸席夫碱镍(Ⅱ)配合物，0.055g碳纳米管，0.03g固体石蜡，加热熔化，迅速搅拌，填入上述玻璃管预留的1mm碳片薄层处，冷却后在称量纸上抛光，即制得吡啶-4-甲醛缩甘氨酸席夫碱镍(Ⅱ)配合物修饰碳纳米管电极。

Claims (1)

1.一种席夫碱配合物修饰碳纳米管电极的制备方法，其特征在于：截取约4cm长的铜棒，φ＝2.0mm，把铜棒两端磨平，并清洗干净；将直径4mm的碳棒磨细，切下约1mm厚的碳片塞入直径为3.5mm、长为4cm的玻璃管中；碳片与玻璃管顶端留出1mm的距离，从另一端插入上述铜棒做引线，顶端用石蜡固定；称取0.013-0.017g电活性物质吡啶-4-甲醛缩甘氨酸席夫碱镍(Ⅱ)配合物，0.035-0.075g碳纳米管，0.01-0.05g固体石蜡，加热熔化，迅速搅拌，填入上述玻璃管预留的1mm碳片薄层处，冷却后在称量纸上抛光，即制得吡啶-4-甲醛缩甘氨酸席夫碱镍(Ⅱ)配合物修饰碳纳米管电极。
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CN102621203B (zh) * 2012-03-22 2014-04-16 桂林理工大学 一种席夫碱修饰铜电极的制备方法
CN102914577B (zh) * 2012-11-19 2014-07-30 桂林理工大学 用于无标记h-IGg阻抗型免疫传感器的氧化还原探针的制备方法
CN103467371B (zh) * 2013-09-27 2014-12-03 桂林理工大学 2-辛酮缩2,6-吡啶二甲酰肼及其应用
CN105403611B (zh) * 2015-10-18 2017-12-12 桂林理工大学 一种检测l半胱氨酸浓度的方法
CN108163838B (zh) * 2017-12-30 2020-01-14 武汉工程大学 一种西佛碱铜配合物修饰碳纳米管及其制备方法和应用
CN110148720B (zh) * 2019-05-13 2021-07-06 中南民族大学 串晶结构席夫碱聚合物/碳纳米管复合电极材料及其制法

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