CN101250714A - Composite electrode for preparing high-purity polyaniline nanowires and preparation method - Google Patents
Composite electrode for preparing high-purity polyaniline nanowires and preparation method Download PDFInfo
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- 229920000767 polyaniline Polymers 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002070 nanowire Substances 0.000 title abstract description 65
- 229920002492 poly(sulfone) Polymers 0.000 claims abstract description 74
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 65
- 239000010935 stainless steel Substances 0.000 claims abstract description 65
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 18
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004695 Polyether sulfone Substances 0.000 claims abstract description 11
- 229920006393 polyether sulfone Polymers 0.000 claims abstract description 11
- 239000004697 Polyetherimide Substances 0.000 claims abstract description 10
- 239000004642 Polyimide Substances 0.000 claims abstract description 10
- 229920001601 polyetherimide Polymers 0.000 claims abstract description 10
- 229920001721 polyimide Polymers 0.000 claims abstract description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010941 cobalt Substances 0.000 claims abstract description 9
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052802 copper Inorganic materials 0.000 claims abstract description 9
- 239000010949 copper Substances 0.000 claims abstract description 9
- 229910021397 glassy carbon Inorganic materials 0.000 claims abstract description 9
- 239000010439 graphite Substances 0.000 claims abstract description 9
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 9
- 229910052742 iron Inorganic materials 0.000 claims abstract description 9
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- 239000010936 titanium Substances 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005266 casting Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 10
- 239000004411 aluminium Substances 0.000 claims 2
- 239000011159 matrix material Substances 0.000 claims 2
- 229940100630 metacresol Drugs 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 abstract description 37
- 238000005345 coagulation Methods 0.000 abstract description 20
- 230000015271 coagulation Effects 0.000 abstract description 20
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 230000009466 transformation Effects 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 abstract 1
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 42
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 36
- 238000006116 polymerization reaction Methods 0.000 description 25
- 239000003792 electrolyte Substances 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012695 Interfacial polymerization Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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Abstract
本发明公开了一种制备高纯度聚苯胺纳米线的复合电极及制备方法，属于制备聚苯胺纳米线材料的技术。所述的复合电极其基体为不锈钢、钛、镍、钴、铝、铁、铜、石墨或玻璃碳，基体上复合聚砜、聚醚砜、聚酰亚胺或聚醚酰亚胺的薄膜。所述的制备方法将聚砜、聚醚砜、聚酰亚胺或聚醚酰亚胺溶于N，N－二甲基乙酰胺、N，N－二甲基甲酰胺、N－甲基吡咯烷酮、二甲基亚砜或间甲酚中，配制成均匀透明铸膜液，涂敷在基体电极表面，之后迅速浸入到凝固浴中完成相转化，得到复合电极。本发明的优点在于使用该复合电极为工作电极制备聚苯胺纳米线，解决了在聚苯胺纳米线中存在聚苯胺颗粒的问题，提高了聚苯胺纳米线的纯度。
The invention discloses a composite electrode and a preparation method for preparing high-purity polyaniline nanowires, belonging to the technology for preparing polyaniline nanowire materials. The substrate of the composite electrode is stainless steel, titanium, nickel, cobalt, aluminum, iron, copper, graphite or glassy carbon, on which a thin film of polysulfone, polyethersulfone, polyimide or polyetherimide is compounded. The preparation method dissolves polysulfone, polyethersulfone, polyimide or polyetherimide in N,N-dimethylacetamide, N,N-dimethylformamide, N-methylpyrrolidone , dimethyl sulfoxide or m-cresol to prepare a uniform transparent casting solution, apply it on the surface of the substrate electrode, and then quickly immerse it in a coagulation bath to complete the phase transformation to obtain a composite electrode. The invention has the advantages of using the composite electrode as a working electrode to prepare polyaniline nanowires, solving the problem of polyaniline particles in the polyaniline nanowires, and improving the purity of the polyaniline nanowires.
Description
技术领域 technical field
本发明涉及一种制备高纯度聚苯胺纳米线的复合电极及制备方法，属于制备聚苯胺纳米线材料的技术。The invention relates to a composite electrode for preparing high-purity polyaniline nanowires and a preparation method, belonging to the technology for preparing polyaniline nanowire materials.
背景技术 Background technique
聚苯胺具有原料易得、合成方法简单、独特的质子酸掺杂行为、优良的电化学与光学性能、结构多样性及良好的环境稳定性等优点。这些优异的特性使得聚苯胺在传感器、传动器、电磁屏蔽、防静电涂层、金属防腐、气体分离膜、超大容量电容器及光电子器件等领域的应用受到广泛的关注，被认为是最有希望在实际中得到应用的导电聚合物之一。近年来，聚苯胺纳米线由于具有大的比表面积和优异的物理化学性质而引起研究者的极大关注。苯胺在聚合初期易于形成纳米线，随着聚合的进行往往得到颗粒状的产物。因此，为得到聚苯胺纳米线就必须控制苯胺聚合的进程或控制苯胺聚合的空间。目前，常用的制备聚苯胺纳米线的技术包括化学聚合法(模板法和非模板法)和电化学聚合法。模板聚合法的优点是当使用的模板合适时产品的产率较高，缺点是产品纯度低、得到纯纳米线的步骤繁杂。当使用非模板法(界面聚合法和快速混合法)时，得到的聚苯胺纳米线的纯度高，纳米线的直径和长度可控，但产率低。电化学聚合法产率高，环境友好，但在聚合过程中容易在电极表面首先形成一层聚苯胺颗粒，使得到的聚苯胺纳米线的纯度不高。因此开发一种电化学制备高纯度聚苯胺纳米线的新技术是十分必要的。Polyaniline has the advantages of readily available raw materials, simple synthesis methods, unique protonic acid doping behavior, excellent electrochemical and optical properties, structural diversity, and good environmental stability. These excellent characteristics make the application of polyaniline in the fields of sensors, actuators, electromagnetic shielding, antistatic coatings, metal anticorrosion, gas separation membranes, super large capacity capacitors and optoelectronic devices have attracted extensive attention. One of the conductive polymers used in practice. In recent years, polyaniline nanowires have attracted great attention of researchers due to their large specific surface area and excellent physical and chemical properties. Aniline is easy to form nanowires at the initial stage of polymerization, and granular products are often obtained as the polymerization progresses. Therefore, in order to obtain polyaniline nanowires, it is necessary to control the process of aniline polymerization or control the space of aniline polymerization. Currently, the commonly used techniques for preparing polyaniline nanowires include chemical polymerization (template and non-template) and electrochemical polymerization. The advantage of the template polymerization method is that the yield of the product is high when the template used is suitable, but the disadvantage is that the product has low purity and the steps to obtain pure nanowires are complicated. When using non-template methods (interfacial polymerization method and rapid mixing method), the obtained polyaniline nanowires have high purity and controllable diameter and length of nanowires, but the yield is low. The electrochemical polymerization method has high yield and is environmentally friendly, but it is easy to form a layer of polyaniline particles on the surface of the electrode during the polymerization process, so that the purity of the obtained polyaniline nanowires is not high. Therefore, it is necessary to develop a new technology for the electrochemical preparation of high-purity polyaniline nanowires.
发明内容 Contents of the invention
本发明的目的在于提供一种制备高纯度聚苯胺纳米线的复合电极及制备方法，所述的复合电极用于制备聚苯胺纳米线，纳米线纯度高，所述的复合电极制备过程简单。The object of the present invention is to provide a composite electrode for preparing high-purity polyaniline nanowires and a preparation method thereof. The composite electrode is used for preparing polyaniline nanowires, the nanowires have high purity, and the preparation process of the composite electrode is simple.
本发明是通过下述技术方案加以实现的：一种制备高纯度聚苯胺纳米线的复合电极，该复合电极以不锈钢、钛、镍、钴、铝、铁、铜、石墨或玻璃碳为基体，其特征在于在基体的表面上复合厚度为5～150μm的聚砜、聚醚砜、聚酰亚胺或聚醚酰亚胺的薄膜。The present invention is achieved through the following technical scheme: a composite electrode for preparing high-purity polyaniline nanowires, the composite electrode is based on stainless steel, titanium, nickel, cobalt, aluminum, iron, copper, graphite or glassy carbon, It is characterized in that polysulfone, polyethersulfone, polyimide or polyetherimide films with a thickness of 5-150 μm are compounded on the surface of the substrate.
上述的复合电极的制备方法，其特征在于包括以下过程：The preparation method of above-mentioned composite electrode is characterized in that comprising following process:
按照质量百分含量3～30％将聚砜、聚醚砜、聚酰亚胺或聚醚酰亚胺溶于N，N-二甲基乙酰胺、N，N-二甲基甲酰胺、N-甲基吡咯烷酮、二甲基亚砜或间甲酚中，配制成均匀透明铸膜液。铸膜液经静置脱泡后，均匀涂敷在不锈钢、钛、镍、钴、铝、铁、铜、石墨或玻璃碳表面，之后将其迅速浸入到凝固浴中完成相转化，得到复合电极。Dissolve polysulfone, polyethersulfone, polyimide or polyetherimide in N, N-dimethylacetamide, N, N-dimethylformamide, N - Methylpyrrolidone, dimethyl sulfoxide or m-cresol, prepared into a uniform transparent casting solution. After static defoaming, the casting solution is evenly coated on the surface of stainless steel, titanium, nickel, cobalt, aluminum, iron, copper, graphite or glassy carbon, and then quickly immersed in the coagulation bath to complete the phase transformation to obtain a composite electrode .
本发明的优点在于所制备的复合电极用于制备聚苯胺纳米线，纳米线纯度高，直径为30～300nm，长度为500nm～5μm，该复合电极制备方法过程简单。The invention has the advantage that the prepared composite electrode is used to prepare polyaniline nanowires, the nanowires have high purity, the diameter is 30-300nm, and the length is 500nm-5μm, and the preparation method of the composite electrode is simple.
附图说明 Description of drawings
图1为以本发明实施例2制得的复合电极所制备的聚苯胺纳米线的扫描电镜照片。FIG. 1 is a scanning electron micrograph of polyaniline nanowires prepared with the composite electrode prepared in Example 2 of the present invention.
图2为以本发明实施例18制得的复合电极所制备的聚苯胺纳米线的扫描电镜照片。Fig. 2 is a scanning electron micrograph of polyaniline nanowires prepared with the composite electrode prepared in Example 18 of the present invention.
图3为以不锈钢电极制备聚苯胺纳米线时得到的产物的扫描电境照片。Fig. 3 is a scanning electron field photograph of the product obtained when polyaniline nanowires are prepared with stainless steel electrodes.
由图1和图2所见，采用本发明的复合电极制备聚苯胺纳米线，不存在聚苯胺颗粒，聚苯胺纳米线纯度高。而由图3可见，采用不锈钢电极制备的聚苯胺纳米线中存在聚苯胺颗粒。As can be seen from Figures 1 and 2, the composite electrode of the present invention is used to prepare polyaniline nanowires without polyaniline particles, and the purity of polyaniline nanowires is high. However, it can be seen from FIG. 3 that there are polyaniline particles in the polyaniline nanowires prepared by using stainless steel electrodes.
具体实施方式 Detailed ways
实施例1.Example 1.
将0.629g的聚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚砜的N，N-二甲基乙酰胺溶液。然后在不锈钢电极表面涂膜，控制液膜厚度为5μm。之后迅速将涂有聚砜的N，N-二甲基乙酰胺溶液的不锈钢电极浸入到凝固浴(水)中完成相转化，得到聚砜/不锈钢复合电极。以聚砜/不锈钢复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polysulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 10% polysulfone. Then coat a film on the surface of the stainless steel electrode to control the thickness of the liquid film to 5 μm. Afterwards, the stainless steel electrode coated with polysulfone N, N-dimethylacetamide solution was quickly immersed in a coagulation bath (water) to complete phase inversion, and a polysulfone/stainless steel composite electrode was obtained. A polysulfone/stainless steel composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例2.Example 2.
将1.415g的聚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含20％聚砜的N，N-二甲基乙酰胺溶液。然后在不锈钢电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的N，N-二甲基乙酰胺溶液的不锈钢电极浸入到凝固浴(水)中完成相转化，得到聚砜/不锈钢复合电极。以聚砜/不锈钢复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。1.415 g of polysulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 20% polysulfone. Then coat a film on the surface of the stainless steel electrode to control the thickness of the liquid film to 100 μm. Afterwards, the stainless steel electrode coated with polysulfone N, N-dimethylacetamide solution was quickly immersed in a coagulation bath (water) to complete phase inversion, and a polysulfone/stainless steel composite electrode was obtained. A polysulfone/stainless steel composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例3.Example 3.
将2.425g的聚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含30％聚砜的N，N-二甲基乙酰胺溶液。然后在不锈钢电极表面涂膜，控制液膜厚度为150μm。之后迅速将涂有聚砜的N，N-二甲基乙酰胺溶液的不锈钢电极浸入到凝固浴(水)中完成相转化，得到聚砜/不锈钢复合电极。以聚砜/不锈钢复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。2.425 g of polysulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 30% polysulfone. Then coat a film on the surface of the stainless steel electrode to control the thickness of the liquid film to 150 μm. Afterwards, the stainless steel electrode coated with polysulfone N, N-dimethylacetamide solution was quickly immersed in a coagulation bath (water) to complete phase inversion, and a polysulfone/stainless steel composite electrode was obtained. A polysulfone/stainless steel composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例4.Example 4.
将0.192g的聚砜溶解于6mL的间甲酚中，得到含3％聚砜的间甲酚溶液。然后在不锈钢电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的间甲酚溶液的不锈钢电极浸入到凝固浴(水)中完成相转化，得到聚砜/不锈钢复合电极。以聚砜/不锈钢复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.192 g of polysulfone was dissolved in 6 mL of m-cresol to obtain a m-cresol solution containing 3% polysulfone. Then coat a film on the surface of the stainless steel electrode to control the thickness of the liquid film to 100 μm. Afterwards, the stainless steel electrode coated with the polysulfone-m-cresol solution was quickly immersed in a coagulation bath (water) to complete phase inversion, and a polysulfone/stainless steel composite electrode was obtained. A polysulfone/stainless steel composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例5.Example 5.
将0.300g的聚砜溶解于6mL的N，N-二甲基甲酰胺中，得到含5％聚砜的N，N-二甲基甲酰胺溶液。然后在不锈钢电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的N，N-二甲基甲酰胺溶液的不锈钢电极浸入到凝固浴(水)中完成相转化，得到聚砜/不锈钢复合电极。以聚砜/不锈钢复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.300 g of polysulfone was dissolved in 6 mL of N,N-dimethylformamide to obtain a solution containing 5% polysulfone in N,N-dimethylformamide. Then coat a film on the surface of the stainless steel electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the stainless steel electrode coated with polysulfone N, N-dimethylformamide solution into a coagulation bath (water) to complete the phase inversion to obtain a polysulfone/stainless steel composite electrode. A polysulfone/stainless steel composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例6.Example 6.
将0.731g的聚砜溶解于6mL的二甲基亚砜中，得到含10％聚砜的二甲基亚砜溶液。然后在不锈钢电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的二甲基亚砜溶液的不锈钢电极浸入到凝固浴(水)中完成相转化，得到聚砜/不锈钢复合电极。以聚砜/不锈钢复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.731 g of polysulfone was dissolved in 6 mL of dimethyl sulfoxide to obtain a dimethyl sulfoxide solution containing 10% polysulfone. Then coat a film on the surface of the stainless steel electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the stainless steel electrode coated with polysulfone-dimethylsulfoxide solution into a coagulation bath (water) to complete the phase inversion to obtain a polysulfone/stainless steel composite electrode. The polysulfone/stainless steel composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例7.Example 7.
将1.086g的聚砜溶解于6mL的N-甲基吡咯烷酮中，得到含15％聚砜的N-甲基吡咯烷酮溶液。然后在不锈钢电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的N-甲基吡咯烷酮溶液的不锈钢电极浸入到凝固浴(水)中完成相转化，得到聚砜/不锈钢复合电极。以聚砜/不锈钢复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。1.086 g of polysulfone was dissolved in 6 mL of N-methylpyrrolidone to obtain a 15% polysulfone-containing N-methylpyrrolidone solution. Then coat a film on the surface of the stainless steel electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the stainless steel electrode coated with polysulfone N-methylpyrrolidone solution into a coagulation bath (water) to complete the phase inversion to obtain a polysulfone/stainless steel composite electrode. The polysulfone/stainless steel composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例8.Example 8.
将0.629g的聚醚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚醚砜的N，N-二甲基乙酰胺溶液。然后在不锈钢电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚醚砜的N，N-二甲基乙酰胺溶液的不锈钢电极浸入到凝固浴(水)中完成相转化，得到聚醚砜/不锈钢复合电极。以聚醚砜/不锈钢复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polyethersulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a 10% polyethersulfone-containing N,N-dimethylacetamide solution. Then coat a film on the surface of the stainless steel electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the stainless steel electrode coated with polyethersulfone N,N-dimethylacetamide solution into a coagulation bath (water) to complete phase inversion to obtain a polyethersulfone/stainless steel composite electrode. A polyethersulfone/stainless steel composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte. 1.80V cell voltage electrolytic polymerization for 40min to obtain the product polyaniline nanowires, the purity of polyaniline nanowires is 100%.
实施例9.Example 9.
将0.629g的聚酰亚胺溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚酰亚胺的N，N-二甲基乙酰胺溶液。然后在不锈钢电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚酰亚胺的N，N-二甲基乙酰胺溶液的不锈钢电极浸入到凝固浴(水)中完成相转化，得到聚酰亚胺/不锈钢复合电极。以聚酰亚胺/不锈钢复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polyimide was dissolved in 6 mL of N,N-dimethylacetamide to obtain a 10% polyimide-containing N,N-dimethylacetamide solution. Then coat a film on the surface of the stainless steel electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the stainless steel electrode coated with polyimide-N,N-dimethylacetamide solution into a coagulation bath (water) to complete the phase inversion to obtain a polyimide/stainless steel composite electrode. A polyimide/stainless steel composite electrode was used as the working electrode, another piece of stainless steel was used as the counter electrode, and 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte at a distance of 1.5 cm. A 1.80V cell voltage was used to electrolytically polymerize for 40 minutes to obtain the product polyaniline nanowires, and the purity of the polyaniline nanowires was 100%.
实施例10.Example 10.
将0.629g的聚醚酰亚胺溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚醚酰亚胺的N，N-二甲基乙酰胺溶液。然后在不锈钢电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚醚酰亚胺的N，N-二甲基乙酰胺溶液的不锈钢电极浸入到凝固浴(水)中完成相转化，得到聚醚酰亚胺/不锈钢复合电极。以聚醚酰亚胺/不锈钢复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polyetherimide was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 10% polyetherimide. Then coat a film on the surface of the stainless steel electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the stainless steel electrode coated with polyetherimide-N,N-dimethylacetamide solution into a coagulation bath (water) to complete the phase inversion to obtain a polyetherimide/stainless steel composite electrode. A polyetherimide/stainless steel composite electrode was used as the working electrode, another piece of stainless steel was used as the counter electrode, and 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte at a distance of 1.5 cm. , using a cell voltage of 1.80V to electrolytically polymerize for 40 minutes to obtain a polyaniline nanowire product, and the purity of the polyaniline nanowire is 100%.
实施例11.Example 11.
将0.629g的聚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚砜的N，N-二甲基乙酰胺溶液。然后在钛电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的N，N-二甲基乙酰胺溶液的钛电极浸入到凝固浴(水)中完成相转化，得到聚砜/钛复合电极。以聚砜/钛复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polysulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 10% polysulfone. Then coat a film on the surface of the titanium electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the titanium electrode coated with polysulfone N,N-dimethylacetamide solution into a coagulation bath (water) to complete the phase inversion to obtain a polysulfone/titanium composite electrode. The polysulfone/titanium composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例12.Example 12.
将0.629g的聚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚砜的N，N-二甲基乙酰胺溶液。然后在镍电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的N，N-二甲基乙酰胺溶液的镍电极浸入到凝固浴(水)中完成相转化，得到聚砜/镍复合电极。以聚砜/镍复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polysulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 10% polysulfone. Then coat a film on the surface of the nickel electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the nickel electrode coated with polysulfone-N,N-dimethylacetamide solution into a coagulation bath (water) to complete the phase inversion to obtain a polysulfone/nickel composite electrode. The polysulfone/nickel composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例13.Example 13.
将0.629g的聚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚砜的N，N-二甲基乙酰胺溶液。然后在钴电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的N，N-二甲基乙酰胺溶液的钴电极浸入到凝固浴(水)中完成相转化，得到聚砜/钴复合电极。以聚砜/钴复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polysulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 10% polysulfone. Then coat a film on the surface of the cobalt electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the cobalt electrode coated with polysulfone-N,N-dimethylacetamide solution into a coagulation bath (water) to complete the phase inversion to obtain a polysulfone/cobalt composite electrode. The polysulfone/cobalt composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例14.Example 14.
将0.629g的聚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚砜的N，N-二甲基乙酰胺溶液。然后在铝电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的N，N-二甲基乙酰胺溶液的铝电极浸入到凝固浴(水)中完成相转化，得到聚砜/铝复合电极。以聚砜/铝复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polysulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 10% polysulfone. Then coat a film on the surface of the aluminum electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the aluminum electrode coated with polysulfone N, N-dimethylacetamide solution into a coagulation bath (water) to complete phase inversion to obtain a polysulfone/aluminum composite electrode. The polysulfone/aluminum composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例15.Example 15.
将0.629g的聚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚砜的N，N-二甲基乙酰胺溶液。然后在铁电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的N，N-二甲基乙酰胺溶液的铁电极浸入到凝固浴(水)中完成相转化，得到聚砜/铁复合电极。以聚砜/铁复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polysulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 10% polysulfone. Then coat a film on the surface of the iron electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the iron electrode coated with polysulfone-N,N-dimethylacetamide solution into a coagulation bath (water) to complete phase inversion to obtain a polysulfone/iron composite electrode. The polysulfone/iron composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例16.Example 16.
将0.629g的聚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚砜的N，N-二甲基乙酰胺溶液。然后在铜电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的N，N-二甲基乙酰胺溶液的铜电极浸入到凝固浴(水)中完成相转化，得到聚砜/铜复合电极。以聚砜/铜复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polysulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 10% polysulfone. Then coat a film on the surface of the copper electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the copper electrode coated with polysulfone-N,N-dimethylacetamide solution into a coagulation bath (water) to complete phase inversion to obtain a polysulfone/copper composite electrode. The polysulfone/copper composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例17.Example 17.
将0.629g的聚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚砜的N，N-二甲基乙酰胺溶液。然后在石墨电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的N，N-二甲基乙酰胺溶液的石墨电极浸入到凝固浴(水)中完成相转化，得到聚砜/石墨复合电极。以聚砜/石墨复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polysulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 10% polysulfone. Then, film is coated on the surface of the graphite electrode, and the thickness of the liquid film is controlled to be 100 μm. Then quickly immerse the graphite electrode coated with polysulfone-N,N-dimethylacetamide solution into a coagulation bath (water) to complete phase inversion to obtain a polysulfone/graphite composite electrode. The polysulfone/graphite composite electrode was used as the working electrode, and another piece of stainless steel was used as the counter electrode. Under the condition of a distance of 1.5 cm, 0.25 mol L -1 aniline and 1.00 mol L -1 sulfuric acid were used as the electrolyte, and 1.80 The polyaniline nanowires were obtained by V-cell voltage electrolytic polymerization for 40 minutes, and the purity of the polyaniline nanowires was 100%.
实施例18.Example 18.
将0.629g的聚砜溶解于6mL的N，N-二甲基乙酰胺中，得到含10％聚砜的N，N-二甲基乙酰胺溶液。然后在玻璃碳电极表面涂膜，控制液膜厚度为100μm。之后迅速将涂有聚砜的N，N-二甲基乙酰胺溶液的玻璃碳电极浸入到凝固浴(水)中完成相转化，得到聚砜/玻璃碳复合电极。以聚砜/玻璃碳复合电极为工作电极，以另一片不锈钢为对电极，在间距为1.5cm的条件下，以0.25mol·L-1苯胺和1.00mol·L-1硫酸为电解液，使用1.80V槽电压电解聚合40min得到产物聚苯胺纳米线，聚苯胺纳米线纯度为100％。0.629 g of polysulfone was dissolved in 6 mL of N,N-dimethylacetamide to obtain a N,N-dimethylacetamide solution containing 10% polysulfone. Then coat a film on the surface of the glassy carbon electrode to control the thickness of the liquid film to 100 μm. Then quickly immerse the glassy carbon electrode coated with polysulfone N,N-dimethylacetamide solution into a coagulation bath (water) to complete the phase inversion to obtain a polysulfone/glassy carbon composite electrode. A polysulfone/glassy carbon composite electrode was used as the working electrode, another piece of stainless steel was used as the counter electrode, and 0.25mol·L -1 aniline and 1.00mol·L -1 sulfuric acid were used as the electrolyte at a distance of 1.5cm. 1.80V cell voltage electrolytic polymerization for 40 minutes to obtain the product polyaniline nanowires, the purity of polyaniline nanowires is 100%.
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