CN106496552A - 一种三元纳米复合材料石墨烯‑聚苯胺‑聚氨基苯磺酸的制备方法 - Google Patents
一种三元纳米复合材料石墨烯‑聚苯胺‑聚氨基苯磺酸的制备方法 Download PDFInfo
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Abstract
本发明公开了一种三元纳米复合材料氧化石墨烯‑聚苯胺‑聚氨基苯磺酸的制备方法,本发明所述方法制备得到的复合材料对AP有较大的电流响应,且修饰电极的稳定性好,适合作为AP的传感材料。
Description
技术领域
本发明涉及复合材料技术领域,尤其涉及一种三元纳米复合材料石墨烯-聚苯胺-聚氨基苯磺酸的制备方法。
背景技术
电化学生物传感器是结合生物特异性识别过程和电化学来实现检测的传感器件。具体为将酶或模拟材料作为生物敏感基元,用电化学修饰电极作为信号转换器,通过捕捉目标物与敏感基元之间的反应所产生的可测信号,此信号与目标信号浓度成正比,实现对电活性目标物定量测定。电化学生物传感器具有构造简单、成本低廉、灵敏度高、选择性高和稳定性好等优点。
酶生物传感器的直接电化学特性表现为电子在敏感基元的活性中心与电极表面间的直接传递,然而不借助任何传递媒介或试剂的直接电子传递是很困难的。因为生物酶往往都是大分子,其氧化还原活性中心深深地包囊在分子的内部。电化学传感器性能的好坏与修饰电极的材料密切相关。导电性良好的物质基于其优异的特性,能在电极与酶间起到促进直接电子传递的作用。
石墨烯具有π-π共轭结构,大的比表面积和好的生物相容性,应该在酶生物传感器领域有着广泛的用途。
发明内容
本发明的目的在于提出一种三元纳米复合材料石墨烯-聚苯胺-聚氨基苯磺酸的制备方法,能够作为模拟酶具备出色的电催化活性。
为达此目的,本发明采用以下技术方案:
一种三元纳米复合材料氧化石墨烯-聚苯胺-聚氨基苯磺酸的制备方法,包括:
(1)在冰浴条件下,机械搅拌条件下,在98%浓硫酸中加入鳞片石墨粉,再加入占石墨粉50-80wt%的硝酸钠,和占石墨烯2-4倍重量的高锰酸钾,冰浴下反应30-120min;
(2)加热至30-40℃恒温4-5h,加入去离子水和双氧水,搅拌1-3h,加入5%浓度的HCl离心洗涤直至无硫酸根离子,得到氧化石墨烯粉末;
(3)将所述氧化石墨烯粉末超声分散配置成为0.3-1g/L的均匀悬浮液,依次加入苯胺和间氨基苯磺酸、质子酸HCl和引发剂过硫酸铵;苯胺与间氨基苯磺酸的质量比为4:1-6:1;
(4)常温搅拌下进行反应,反应结束并冷却至室温;
(5)离心分离得到沉淀物,用乙醇洗涤所述沉淀物,得到氧化石墨烯-聚苯胺-聚氨基苯磺酸三元纳米复合材料。
本发明对于现有技术的贡献,主要集中在提供一种全新的工艺步骤,至于各个工艺条件,不如各物质的用量与比例,本领域技术人员可以在现有技术的基础上,结合具体要求,自行确定,本发明不再就其赘述。
本发明所述方法制备得到的产物,经FTIR分析,其在1030和620cm-1处有-SO3的红外吸收峰,证明间氨基苯磺酸与苯胺成功共聚,掺杂在聚合物中。
本发明制备得到的三元纳米复合材料,氧化石墨烯表面被一层共聚物薄膜包覆,通过TEM和SEM发现聚合物在氧化石墨烯表面生长的颗粒均一,无团聚现象。
本发明所述方法制备得到的复合材料对AP有较大的电流响应,且修饰电极的稳定性好,适合作为AP的传感材料。
具体实施方式
下面通过具体实施方式来进一步说明本发明的技术方案。
实施例1
一种三元纳米复合材料氧化石墨烯-聚苯胺-聚氨基苯磺酸的制备方法,包括:
(1)在冰浴条件下,机械搅拌条件下,在98%浓硫酸中加入鳞片石墨粉,再加入占石墨粉50wt%的硝酸钠,和占石墨烯2倍重量的高锰酸钾,冰浴下反应30min;
(2)加热至30℃恒温4h,加入去离子水和双氧水,搅拌1h,加入5%浓度的HCl离心洗涤直至无硫酸根离子,得到氧化石墨烯粉末;
(3)将所述氧化石墨烯粉末超声分散配置成为0.3g/L的均匀悬浮液,依次加入苯胺和间氨基苯磺酸、质子酸HCl和引发剂过硫酸铵;苯胺与间氨基苯磺酸的质量比为4:1;
(4)常温搅拌下进行反应,反应结束并冷却至室温;
(5)离心分离得到沉淀物,用乙醇洗涤所述沉淀物,得到氧化石墨烯-聚苯胺-聚氨基苯磺酸三元纳米复合材料。
实施例2
一种三元纳米复合材料氧化石墨烯-聚苯胺-聚氨基苯磺酸的制备方法,包括:
(1)在冰浴条件下,机械搅拌条件下,在98%浓硫酸中加入鳞片石墨粉,再加入占石墨粉80wt%的硝酸钠,和占石墨烯4倍重量的高锰酸钾,冰浴下反应120min;
(2)加热至40℃恒温5h,加入去离子水和双氧水,搅拌3h,加入5%浓度的HCl离心洗涤直至无硫酸根离子,得到氧化石墨烯粉末;
(3)将所述氧化石墨烯粉末超声分散配置成为1g/L的均匀悬浮液,依次加入苯胺和间氨基苯磺酸、质子酸HCl和引发剂过硫酸铵;苯胺与间氨基苯磺酸的质量比为6:1;
(4)常温搅拌下进行反应,反应结束并冷却至室温;
(5)离心分离得到沉淀物,用乙醇洗涤所述沉淀物,得到氧化石墨烯-聚苯胺-聚氨基苯磺酸三元纳米复合材料。
实施例3
一种三元纳米复合材料氧化石墨烯-聚苯胺-聚氨基苯磺酸的制备方法,包括:
(1)在冰浴条件下,机械搅拌条件下,在98%浓硫酸中加入鳞片石墨粉,再加入占石墨粉70wt%的硝酸钠,和占石墨烯3倍重量的高锰酸钾,冰浴下反应60min;
(2)加热至35℃恒温4.5h,加入去离子水和双氧水,搅拌2h,加入5%浓度的HCl离心洗涤直至无硫酸根离子,得到氧化石墨烯粉末;
(3)将所述氧化石墨烯粉末超声分散配置成为0.7g/L的均匀悬浮液,依次加入苯胺和间氨基苯磺酸、质子酸HCl和引发剂过硫酸铵;苯胺与间氨基苯磺酸的质量比为5:1;
(4)常温搅拌下进行反应,反应结束并冷却至室温;
(5)离心分离得到沉淀物,用乙醇洗涤所述沉淀物,得到氧化石墨烯-聚苯胺-聚氨基苯磺酸三元纳米复合材料。
实施例1-3所述方法制备得到的三元复合对AP有较大的电流响应,且修饰电极的稳定性好,适合作为AP的传感材料。
Claims (1)
1.一种三元纳米复合材料氧化石墨烯-聚苯胺-聚氨基苯磺酸的制备方法,包括:
(1)在冰浴条件下,机械搅拌条件下,在98%浓硫酸中加入鳞片石墨粉,再加入占石墨粉50-80wt%的硝酸钠,和占石墨烯2-4倍重量的高锰酸钾,冰浴下反应30-120min;
(2)加热至30-40℃恒温4-5h,加入去离子水和双氧水,搅拌1-3h,加入5%浓度的HCl离心洗涤直至无硫酸根离子,得到氧化石墨烯粉末;
(3)将所述氧化石墨烯粉末超声分散配置成为0.3-1g/L的均匀悬浮液,依次加入苯胺和间氨基苯磺酸、质子酸HCl和引发剂过硫酸铵;苯胺与间氨基苯磺酸的质量比为4:1-6:1;
(4)常温搅拌下进行反应,反应结束并冷却至室温;
(5)离心分离得到沉淀物,用乙醇洗涤所述沉淀物,得到氧化石墨烯-聚苯胺-聚氨基苯磺酸三元纳米复合材料。
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CN110041739B (zh) * | 2019-04-02 | 2021-11-26 | 砥创(苏州)新材料科技有限公司 | 一种高效防腐用超大尺寸石墨烯水性浆料及其制备方法 |
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