CN103484920A - Preparation method of graphene/polyaniline composite anode - Google Patents
Preparation method of graphene/polyaniline composite anode Download PDFInfo
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- CN103484920A CN103484920A CN201310400293.8A CN201310400293A CN103484920A CN 103484920 A CN103484920 A CN 103484920A CN 201310400293 A CN201310400293 A CN 201310400293A CN 103484920 A CN103484920 A CN 103484920A
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Abstract
The invention relates to a preparation method of a graphene/polyaniline composite anode. The preparation method comprises the following steps: uniformly mixing 1-20g of graphene, 50-150g of aniline and 500-1000ml of 2mol/L hydrochloric acid, then adding 1-10g of ammonium persulfate, stirring and reacting for 1-3h at the temperature of 0-4 DEG C, respectively filtering and washing the reaction product with 3% by weight of hydrochloric acid and distilled water for three times respectively, drying at the temperature of 80 DEG C, grinding into scales, mixing the ground product with an adhesive and an organic solvent at a ratio of 70: 20: 10-80, then performing ultrasonic vibration treatment for 30min, stirring till the mixture is sticky, thus obtaining an electrode coating; and pulling many times by adopting a pulling method, coating an electrode coating layer on the surface of a titanium plate, drying for 3-7h at the temperature of 120-150 DEG C, and preparing the composite anode. The preparation method disclosed by the invention has simple process, and the prepared electrode has the advantages of stable performances, low cost and good conductive performance.
Description
Technical field
The invention belongs to electrochemistry and new energy materials field, relate to a kind of preparation method of graphene/polyaniline composite anode.
Background technology
Galvanic anode can be divided into soluble anode and insoluble anode by its solubility property.The effect of insoluble anode is conduction and controls the distribution of electric current at cathode surface, do not participate in the dissolving of metal, thereby be conducive to improve coating homogeneity, reduce energy consumption and need not often change the continuity that can guarantee operating rate and production etc., by modern electroplating industry, extensively adopted.But traditional coated electrode is that mostly metal oxide is precious metal at metal titanium surface metallization oxide compound, and production cost is very high, so develop the insoluble anode of with low cost and stable performance, to replace expensive coated electrode, Research Significance is arranged.
Polyaniline is a kind of important conducting polymer materials, there is the characteristics such as specific conductivity is high, with low cost, fine corrosion resistance, be widely used in anti-corrosion of metal, electromagnetic shielding, the field such as antistatic, be considered to the conduction high polymer of tool potentiality in actual applications.Graphene is one of dark concerned materials recent years, and the structure of himself monoatomic layer has been given the physicochemical property of its more uniqueness, and for example surface-area is large, and electronic mobility is high, and mass density is little, and thermostability is high, and chemical stability is good etc.Therefore utilize above bi-material processability stable, cost is low, and the composite anode conducted electricity very well is a direction of research.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of graphene/polyaniline composite anode.Adopt situ aggregation method to prepare the polyaniline of doped hydrochloride on graphene sheet layer, and utilize crystal pulling method to apply certain thickness graphene/polyaniline electrode materials at matrix surface, provide a kind of technique composite anode preparation method simple, with low cost.
The technical scheme adopted is:
A kind of method prepared by graphene/polyaniline composite anode, be to use situ aggregation method to make the polyaniline of doped hydrochloride on graphite linings, specifically comprises the steps:
The 2mol/L mixed in hydrochloric acid of getting 1-20g Graphene, 50-150g aniline and 500-1000ml adds the 1-10g ammonium persulphate after evenly, under 0-4 ℃, stirring reaction 1-3 hour by 3% hydrochloric acid and distilled water diafiltration by percentage to the quality each 3 times for product, is ground to flakey after 80 ℃ of oven dry.After product after grinding and cakingagent and organic solvent mix in the ratio of 70:20:10-80, ultrasonic concussion is processed 30 minutes, is stirred to thickly, makes electrode compound.Adopt crystal pulling method, through repeatedly lifting, at titanium plate surface-coated electrode compound layer, dry 3-7 hour at 120-150 ℃ of temperature, be prepared into composite anode.Carry out eleetrotinplate with the composite anode made, make the composite anode performance more stable.
Above-mentioned tackiness agent is epoxy resin or polyvinylidene difluoride (PVDF) (PVDF) etc.Organic solvent is organic easy volatile solvent such as N-Methyl pyrrolidone (NMP), chloroform, ethyl formate.
Under repeatedly lift and lift for 5-15 time.
Technique of the present invention is simple, and the electrode performance of preparing is stable, and cost is low, conducts electricity very well.
Embodiment
Embodiment 1
A kind of method prepared by graphene/polyaniline composite anode, it is characterized in that: by the 1g Graphene, 10g aniline, add the 1g ammonium persulphate after the 2mol/L mixed in hydrochloric acid of 70mL is even, under 0 ℃, stirring reaction 3 hours by 3% hydrochloric acid and distilled water diafiltration each 3 times for product, is ground to flakey after 80 ℃ of oven dry.After grinding after product and binding agent PVDF and NMP mixing in the 70:20:10 ratio, ultra-sonic oscillation are processed 30 minutes, be stirred to thick, adopt crystal pulling method to dry 5 hours at titanium plate surface-coated electrode coating material and under 130 ℃ of conditions, lift oven dry through 10 times and be prepared into composite anode.The anode that utilization makes carries out eleetrotinplate, the composite anode stable performance.
Embodiment 2
A kind of method prepared by graphene/polyaniline composite anode, it is characterized in that: by Graphene 0.5g, aniline 8g, after mixing, 2mol/L hydrochloric acid 40mL adds the 0.5g ammonium persulphate, 3 ℃ of lower stirring reactions 2 hours, by 3% hydrochloric acid and distilled water diafiltration each 3 times for product, after 80 ℃ of oven dry, be ground to flakey.After grinding after product and epoxy resin of binder and solvent ethyl formate mixing in the 70:20:10 ratio, ultra-sonic oscillation are processed 30 minutes, be stirred to thick, after adopting crystal pulling method to dry 4 hours at titanium plate surface-coated electrode coating material and under 150 ℃ of conditions, lift to dry through 15 times and prepare electrode, the anode that utilization makes carries out electro-galvanizing, the composite anode stable performance.
Embodiment 3
A kind of method prepared by graphene/polyaniline composite anode, it is characterized in that: by Graphene 0.5g, aniline 8g, after mixing, 2mol/L hydrochloric acid 40mL adds the 0.5g ammonium persulphate, 4 ℃ of lower stirring reactions 1 hour, by 3% hydrochloric acid and distilled water diafiltration each 3 times for product, after 80 ℃ of oven dry, be ground to flakey.The proportioning of active material, sizing agent and organic solvent is 80:15:5, after mixing, ultra-sonic oscillation are processed 30 minutes, be stirred to thickly, after adopting crystal pulling method to dry 6 hours at titanium plate surface-coated electrode coating material and under 120 ℃ of conditions, lift to dry through 5 times and prepare electrode.The anode that utilization makes carries out electrodeposited chromium, the composite anode stable performance.
Claims (2)
1. a method prepared by the graphene/polyaniline composite anode, be to use situ aggregation method to make the polyaniline of doped hydrochloride on graphite linings, it is characterized in that comprising the steps:
The 2mol/L mixed in hydrochloric acid of getting 1-20g Graphene, 50-150g aniline and 500-1000ml adds the 1-10g ammonium persulphate after evenly, under 0-4 ℃, stirring reaction 1-3 hour, by 3% hydrochloric acid and distilled water diafiltration by percentage to the quality each 3 times for product, be ground to flakey after 80 ℃ of oven dry, after product after grinding and cakingagent and organic solvent mix in the ratio of 70:20:10-80, ultrasonic concussion is processed 30 minutes, is stirred to thickly, makes electrode compound; Adopt crystal pulling method, through repeatedly lifting, at titanium plate surface-coated electrode compound layer, dry 3-7 hour at 120-150 ℃ of temperature, be prepared into composite anode.
2. the method that prepared by a kind of graphene/polyaniline composite anode according to claim 1, is characterized in that tackiness agent is epoxy resin or polyvinylidene difluoride (PVDF), and organic solvent is N-Methyl pyrrolidone, chloroform or ethyl formate;
Described repeatedly lifting lifts for 5-15 time.
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| CN201310400293.8A CN103484920A (en) | 2013-09-06 | 2013-09-06 | Preparation method of graphene/polyaniline composite anode |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104479190A (en) * | 2014-10-29 | 2015-04-01 | 上海大学 | Preparation method of medium-density polyethylene/graphene/polyaniline ternary composite conductive functional material |
| KR101584890B1 (en) * | 2014-04-03 | 2016-01-14 | 경북대학교 산학협력단 | Manufacturing method of polyaniline-graphene nonocompisites and Polyaniline-graphene nonocompisites film |
| WO2016026190A1 (en) * | 2014-08-21 | 2016-02-25 | 深圳市华星光电技术有限公司 | Method for preparing graphene conductive polymer conductive adhesive and graphene conductive polymer conductive adhesive |
| CN105885411A (en) * | 2016-06-21 | 2016-08-24 | 苏州法斯特信息科技有限公司 | Preparation method of high-conductivity polyaniline-graphene composite |
| CN109136992A (en) * | 2018-09-06 | 2019-01-04 | 索通发展股份有限公司 | The preparation method of pre-baked carbon anode graphene composite protection layer |
| CN114725404A (en) * | 2022-04-22 | 2022-07-08 | 福州大学 | Biocompatible microbial fuel cell composite anode material and preparation method thereof |
| CN115491708A (en) * | 2022-09-28 | 2022-12-20 | 西南石油大学 | Electrode for electrolytic hydrogen production of salt-containing wastewater and preparation method and application thereof |
| CN115557633A (en) * | 2022-09-28 | 2023-01-03 | 西南石油大学 | Integrated system for wastewater treatment and electrolytic hydrogen production and operation method |
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| US20090092747A1 (en) * | 2007-10-04 | 2009-04-09 | Aruna Zhamu | Process for producing nano-scaled graphene platelet nanocomposite electrodes for supercapacitors |
| CN101798462A (en) * | 2010-03-26 | 2010-08-11 | 武汉工程大学 | Graphene/conductive polymer composite film and preparation method thereof |
| CN102788822A (en) * | 2012-07-19 | 2012-11-21 | 西南交通大学 | Preparation method of nanometer composite film ammonia gas sensor |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101584890B1 (en) * | 2014-04-03 | 2016-01-14 | 경북대학교 산학협력단 | Manufacturing method of polyaniline-graphene nonocompisites and Polyaniline-graphene nonocompisites film |
| WO2016026190A1 (en) * | 2014-08-21 | 2016-02-25 | 深圳市华星光电技术有限公司 | Method for preparing graphene conductive polymer conductive adhesive and graphene conductive polymer conductive adhesive |
| CN104479190A (en) * | 2014-10-29 | 2015-04-01 | 上海大学 | Preparation method of medium-density polyethylene/graphene/polyaniline ternary composite conductive functional material |
| CN105885411A (en) * | 2016-06-21 | 2016-08-24 | 苏州法斯特信息科技有限公司 | Preparation method of high-conductivity polyaniline-graphene composite |
| CN109136992A (en) * | 2018-09-06 | 2019-01-04 | 索通发展股份有限公司 | The preparation method of pre-baked carbon anode graphene composite protection layer |
| CN114725404A (en) * | 2022-04-22 | 2022-07-08 | 福州大学 | Biocompatible microbial fuel cell composite anode material and preparation method thereof |
| CN114725404B (en) * | 2022-04-22 | 2023-09-01 | 福州大学 | Biocompatible microbial fuel cell composite anode material and preparation method thereof |
| CN115491708A (en) * | 2022-09-28 | 2022-12-20 | 西南石油大学 | Electrode for electrolytic hydrogen production of salt-containing wastewater and preparation method and application thereof |
| CN115557633A (en) * | 2022-09-28 | 2023-01-03 | 西南石油大学 | Integrated system for wastewater treatment and electrolytic hydrogen production and operation method |
| CN115491708B (en) * | 2022-09-28 | 2023-04-28 | 西南石油大学 | Electrode for electrolytic hydrogen production of salt-containing wastewater and preparation method and application thereof |
| CN115557633B (en) * | 2022-09-28 | 2023-05-05 | 西南石油大学 | Integrated system for wastewater treatment and electrolytic hydrogen production and operation method |
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Application publication date: 20140101 |