CN103694473B - 水相法制备聚邻苯二胺纳米带的方法 - Google Patents
水相法制备聚邻苯二胺纳米带的方法 Download PDFInfo
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- CN103694473B CN103694473B CN201310725015.XA CN201310725015A CN103694473B CN 103694473 B CN103694473 B CN 103694473B CN 201310725015 A CN201310725015 A CN 201310725015A CN 103694473 B CN103694473 B CN 103694473B
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- phenylenediamine
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- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000002127 nanobelt Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000008346 aqueous phase Substances 0.000 title claims abstract description 8
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229960003280 cupric chloride Drugs 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 235000011194 food seasoning agent Nutrition 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 229920001940 conductive polymer Polymers 0.000 abstract description 3
- 238000000605 extraction Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 3
- 244000144992 flock Species 0.000 description 3
- 229920000767 polyaniline Polymers 0.000 description 3
- 239000000178 monomer Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
水相法制备聚邻苯二胺纳米带的方法,涉及一种聚邻苯二胺纳米带的制备方法。所述方法如下:将0.5mL0.001~0.15mol/L的邻苯二胺溶液加入到1mL去离子水中,加入0.8~1.2mLl饱和的NaCl溶液或KCl溶液,搅拌均匀,加入0.5mL?0.25~1.0mol/L氯化铜溶液,反应进行0.5~3小时后将溶液离心分离,沉淀物水洗后室温条件下自然干燥,即得聚邻苯二胺纳米带。本发明提供的合成方法操作简单,设备简易,容易控制,反应时间短,重复性好,可进行大量生产。通过本发明所制备的聚邻苯二胺纳米带可作为导电聚合物应用于光电技术领域或者作为吸附载体应用于重金属离子提取。
Description
技术领域
本发明涉及一种聚邻苯二胺纳米带的制备方法,具体涉及一种在水相环境中制备聚邻苯二胺纳米带的方法。
背景技术
聚苯胺导电聚合物是新型电极材料,它们具有电催化、电变色等特性,而聚苯胺衍生物比聚苯胺能提供更多的再修饰官能团,因此对开发新的聚合物材料有特殊意义。聚邻苯二胺是一种重要的导电聚合物,在光电晶体管等领域都有巨大的应用潜力。聚邻苯二胺纳米带具有较大的长径比,且形貌可控,在光电器件组装等方面具有独特的优势,因此关于聚邻苯二胺纳米带的研究具有重要的意义。聚邻苯二胺纳米带的合成路线对聚邻苯二胺纳米带的光电性能有着重要的影响,因此,发明一种操作简单、普适性好且产率高的聚邻苯二胺纳米带的方案具有重要的现实意义。
发明内容
本发明的目的是提供一种在水相环境中制备聚邻苯二胺纳米带的方法,该方法可以在室温条件下得到高产率的、形貌均一的聚邻苯二胺纳米带。
本发明的目的是通过以下技术方案实现的:
将0.5mL0.001~0.15mol/L的邻苯二胺溶液加入到1mL去离子水中,加入0.8~1.2mL饱和的NaCl溶液或KCl溶液,搅拌均匀,加入0.5mL氯化铜溶液(0.25~1.0mol/L),静置,溶液中出现大量肉眼可见的絮状沉淀,反应进行0.5~3小时后将溶液离心分离,沉淀物水洗后室温条件下自然干燥,即得聚邻苯二胺纳米带。
本发明在水溶液中,以邻苯二胺单体为原料,以氯化铜为氧化剂,在高浓度氯化钠或氯化钾存在的条件下,氧化剂和邻苯二胺单体发生氧化还原反应,生成聚邻苯二胺低聚体,低聚体在氯化钠和π-π作用的驱动下,发生一维的自组装过程,通过对反应物的浓度和配比以及反应时间进行控制,生成聚邻苯二胺纳米带。
相比于现有技术,本方法具有以下优点:
1、采用水相环境,避免了有机相的高毒性和高成本问题;
2、以氯化铜为氧化剂合成聚邻苯二胺纳米带;
3、实验中采用高浓度的氯化钠或氯化钾溶液作为反应的离子环境;
4、通过该工艺合成的纳米带形貌均一,缺陷少,可重复性好,产物的提取方便;
5、所有步骤均在室温条件下进行,无需加热;
6、操作简单,设备简易,容易控制,反应时间短,重复性好,可进行大量生产;
7、通过本发明所制备的聚邻苯二胺纳米带可作为导电聚合物应用于光电技术领域或者作为吸附载体应用于重金属离子提取。
附图说明
图1为本发明实施例1所制备聚邻苯二胺纳米带光学显微镜形貌图。
图2为本发明实施例2所制备聚邻苯二胺纳米带光学显微镜形貌图。
具体实施方式
下面结合实施例对本发明的技术方案作进一步的说明,但并不局限于此,凡是对本发明技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,均应涵盖在本发明的保护范围中。
实施例1:
将0.5mL现配的0.1mol/L的邻苯二胺溶液加入到1mL去离子水中,加入1mL饱和的NaCl溶液,搅拌均匀,加入0.5mL1.0mol/L的氯化铜溶液,静置,溶液中出现大量肉眼可见的絮状沉淀,反应进行1小时后将溶液离心并用去离子水洗三次,室温条件下自然干燥,即得聚邻苯二胺纳米带(图1)。
实施例2:
将0.5mL现配的0.01mol/L的邻苯二胺溶液加入到1mL去离子水中,加入1mL饱和的KCl溶液,搅拌均匀,加入0.5mL0.5mol/L的氯化铜,静置,溶液中出现大量肉眼可见的絮状沉淀,反应进行1小时后将溶液离心并用去离子水洗三次,室温条件下自然干燥,即得聚邻苯二胺纳米带(图2)。
Claims (5)
1.水相法制备聚邻苯二胺纳米带的方法,其特征在于所述方法步骤如下:
将0.5mL0.001~0.15mol/L的邻苯二胺溶液加入到1mL去离子水中,添加0.8~1.2mL饱和的NaCl溶液或KCl溶液提供离子环境,搅拌均匀,加入0.5mL0.25~1.0mol/L氯化铜溶液,反应进行0.5~3小时后将溶液离心分离,沉淀物水洗后室温条件下自然干燥,即得聚邻苯二胺纳米带。
2.根据权利要求1所述的水相法制备聚邻苯二胺纳米带的方法,其特征在于所述邻苯二胺溶液的浓度为0.1mol/L。
3.根据权利要求1所述的水相法制备聚邻苯二胺纳米带的方法,其特征在于所述邻苯二胺溶液的浓度为0.01mol/L。
4.根据权利要求1所述的水相法制备聚邻苯二胺纳米带的方法,其特征在于所述氯化铜溶液的浓度为0.5mol/L。
5.根据权利要求1所述的水相法制备聚邻苯二胺纳米带的方法,其特征在于所述氯化铜溶液的浓度为1.0mol/L。
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CN104119528B (zh) * | 2014-07-18 | 2016-04-27 | 哈尔滨工业大学 | 一种聚邻苯二胺/钯金属有机复合管的制备方法 |
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Citations (3)
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CN1621432A (zh) * | 2004-10-26 | 2005-06-01 | 中国科学院长春应用化学研究所 | 聚邻苯胺纳米带的制备方法 |
CN101020749A (zh) * | 2007-02-13 | 2007-08-22 | 同济大学 | 聚邻苯二胺的高温回流氧化制备方法 |
CN101020783A (zh) * | 2007-02-13 | 2007-08-22 | 同济大学 | 聚邻苯二胺与银的纳米复合粒子及其制备方法 |
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US7101961B2 (en) * | 2004-06-15 | 2006-09-05 | Changchun Institute Of Applied Chemistry Chinese Academy Of Sciences | Method for preparation of poly(o-phenylenediamine) Nano-belt |
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CN1621432A (zh) * | 2004-10-26 | 2005-06-01 | 中国科学院长春应用化学研究所 | 聚邻苯胺纳米带的制备方法 |
CN101020749A (zh) * | 2007-02-13 | 2007-08-22 | 同济大学 | 聚邻苯二胺的高温回流氧化制备方法 |
CN101020783A (zh) * | 2007-02-13 | 2007-08-22 | 同济大学 | 聚邻苯二胺与银的纳米复合粒子及其制备方法 |
Non-Patent Citations (3)
Title |
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Facile synthesis of poly(o-phenylenediamine) microfibrils using cupric sulfate as the oxidant;Liang Wang, et al;《Materials Letters》;20080307;第62卷(第17-18期);第3240-3242页 * |
Formation of o-phenylenediamine oligomers and their self-assembly into one-dimensional structures in aqueous medium;Xuping Sun, et al;《Macromolecular Rapid Communications》;20050923;第26卷(第18期);第1504-1508页 * |
水热法合成聚邻苯二胺微米带和光谱表征;周铁莉 等;《光谱学与光谱分析》;20101130;第30卷(第11期);第13-14页 * |
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