CN103114301A - Preparation process of nanometer Fe3O4-V2O5-Au-doped polythiophene-membrane-modified active carbon fiber electrode - Google Patents
Preparation process of nanometer Fe3O4-V2O5-Au-doped polythiophene-membrane-modified active carbon fiber electrode Download PDFInfo
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Abstract
The invention discloses a preparation process of a nanometer Fe3O4-V2O5-Au-doped polythiophene-membrane-modified active carbon fiber electrode. The preparation process comprises the following steps of: dissolving FeCl3 and NaAc into ethylene glycol, and drying to obtain particles A; mixing cetyl trimethyl ammonium bromide, normal octane and normal butanol, dividing into two parts, adding ammonium metavanadate and de-ionized water into one part, and stirring to obtain microemulsion A; adding diluted sulfuric acid into the other part and stirring to obtain microemulsion B; mixing the microemulsion A and the microemulsion B, centrifuging, washing and roasting to obtain particles B; mixing the particles A and the particles B, adding polyvinyl pyrrolidone, HAuCl4 solution and the de-ionized water into the mixed particles, vibrating, centrifuging, washing, drying and dissolving into anhydrous ethanol, vibrating and dropping 10mu L of the solution onto a pre-treated active carbon fiber electrode, standing to obtain a modified electrode A; and adding 1mL of thiophene into concentrated sulfuric acid, and carrying out electric polymerization by using the modified electrode as a working electrode to obtain the nanometer Fe3O4-V2O5-Au-doped polythiophene-membrane-modified active carbon fiber electrode.
Description
Technical field
The invention belongs to the chemically modified electrode technical field of electrocatalytic oxidation reduction, particularly a kind of nanometer Fe
3O
4-V
2O
5The preparation technology of the film modified Activated Carbon Fiber Electrodes of-Au doping Polythiophene.
Background technology
In recent years, along with the widespread use of electrochemical techniques at environmental area, the particularly pollution problem such as Fenton method Treatment of Wastewater in Coking, the hydrogen reduction catalytic performance that how to improve negative electrode becomes the focus of research, has a lot of researchs to concentrate on and modifies cathode material to improve its hydrogen reduction catalytic performance.
The material of modifying at present negative electrode in the research both at home and abroad mainly contains conductive polymers and inorganic magnetic mixture.Conductive polymers has large π key conjugated structure usually, and stiff chain is general insoluble not molten, chemical stability and good mechanical stability, but monomer whose through electroactive polymerization Direct precipitation at electrode surface, then firmly, be difficult for occuring the loss of active body, so its favorable reproducibility, electrode life is long; And conductive polymers is nontoxic, the preparation is easy, has higher conductivity and environmental stability, and what at present conductive polymers research was more is polypyrrole, polyaniline, polyphenylene etc.The inorganic magnetic mixture is cheap, aboundresources, be widely used in the aspects such as ultracapacitor, battery, fuel cell as a kind of important electrode materials, its nano material has the electro catalytic activity of uniqueness because of its small-size effect and surface effects, be used as the oxygen reduction catalyzer and studied, that at present nano inorganic magnetic composite research is more is Fe
3O
4And various ferrites, salt and other transition metal oxides etc.Based on above advantage, with common modified electrode after conductive polymers and the complexing of inorganic magnetic mixture, thereby can overcome the purpose that separately defective realizes improving the hydrogen reduction catalytic performance of negative electrode.But in the present research, only relate to one or both inorganic magnetic mixtures and a kind of conductive polymers complexing, and conductive polymers mostly is polyaniline and homologue thereof, the electrode of modifying mostly is graphite and gac, the preparation technology of the Activated Carbon Fiber Electrodes that therefore multiple mixture is modified also lacks the research of this aspect at present.
Summary of the invention
Purpose of the present invention provides a kind of nanometer Fe
3O
4-V
2O
5The preparation technology of the film modified Activated Carbon Fiber Electrodes of-Au doping Polythiophene.Its concrete steps are as follows:
(1) with 5.30g FeCl
3Be dissolved in the 35mL ethylene glycol, under the 1000r/min agitation condition, add 5.28g NaAc and stir 30min, obtain mixed solution A;
(2) mixed solution A that step (1) is obtained is transferred in the high-pressure digestion tank that volume is 55mL, is heated to 200 ℃ and insulation reaction 10h, obtains solid product B;
(3) the solid product B that step (2) is obtained is to carry out centrifugation under the 6000r/min condition at rotating speed, then use the 15mL deionized water wash, repeated washing twice is 95% washing with alcohol one time with the 20mL massfraction, place dry 4h under 60 ℃ of conditions, obtain particle A;
(4) 3.00g cetyl trimethylammonium bromide, 17.00mL octane, 5.00mL propyl carbinol are added in the 250mL Erlenmeyer flask successively, add again 2.00g ammonium meta-vanadate and 100mL deionized water, place 70 ℃ of water-baths under the 5000r/min condition, to stir 15min, obtain microemulsion A;
(5) 3.00g cetyl trimethylammonium bromide, 17.00mL octane, 5.00mL propyl carbinol are added in the 250mL Erlenmeyer flask successively, add again the dilute sulphuric acid that the 100mL volumetric molar concentration is 0.80mol/L, under the 1000r/min condition, stir 15min, obtain microemulsion B;
(6) the microemulsion A that step (4) is obtained mixes with the microemulsion B that step (5) obtains, then under the 1000r/min condition, stir 10min, leave standstill 10h, centrifugal 20min under the 6000r/min condition again, remove supernatant liquor, be 95% washing with alcohol with the 15mL massfraction, repeated washing 5 times obtains solid product C;
(7) the solid product C that step (6) is obtained dry 24h under 100 ℃ of conditions places retort furnace roasting 2h under 500 ℃ of conditions again, obtains particle B;
(8) the particle B that the particle A that 20mg step (3) is obtained and 20mg step (7) obtain adds in the 250mL Erlenmeyer flask, add again 1.16g polyvinylpyrrolidone and 100mL deionized water, ultrasonic concussion 10min, adding the 1.00mL mass concentration is the HAuCl of 0.02g/mL
4Solution continues ultrasonic concussion 5min;
(9) adding the 2.00mL weight percent in the Erlenmeyer flask of step (8) is 1% sodium citrate solution, concussion reaction 30min under 40 ℃ of conditions, centrifugal 15min under the 6000r/min condition, remove supernatant liquor, then use the 15mL deionized water wash, repeated washing twice obtains solid product D behind dry 24h under 20 ℃ of conditions;
(10) be that the activated carbon fiber of 1mm is cut into 5cm * l0cm size with thickness, place deionized water to boil 1h, take out and in the 50mL deionized water, soak 24h, then in baking oven, dry 24h, obtain pretreated Activated Carbon Fiber Electrodes;
(11) the solid product D that 0.1g step (9) is obtained, place the 10mL dehydrated alcohol, then ultrasonic concussion 10min takes out 10 μ L and drops on the pretreated Activated Carbon Fiber Electrodes of step (10), under 20 ℃ of conditions, leave standstill 30min, obtain modified electrode A;
(12) the 1mL thiophene being added the 10mL volumetric molar concentration is the H of 10.0mol/L
3PO
4In the solution, as the ionic liquid of electropolymerization, the modified electrode A that obtains take step (11) is as working electrode, take the Pt electrode as to electrode, and take the Ag electrode as reference electrode, 0～2V cyclic voltammetry polymerization, 10 circles, sweep velocity is 45mV/s, obtains nanometer Fe
3O
4-V
2O
5The film modified Activated Carbon Fiber Electrodes of-Au doping Polythiophene.
The invention has the beneficial effects as follows the nanometer Fe that makes
3O
4-V
2O
5The film modified Activated Carbon Fiber Electrodes hydrogen reduction of-Au doping Polythiophene catalytic performance is high, and electrode life is long.
Embodiment
The invention provides a kind of nanometer Fe
3O
4-V
2O
5The preparation technology of the film modified Activated Carbon Fiber Electrodes of-Au doping Polythiophene illustrates the process of in fact executing below by an example.
Embodiment 1.
With 5.30gFeCl
3Be dissolved in the 35mL ethylene glycol, add 5.28g NaAc and under the 1000r/min condition and stir 30min, obtain mixed solution A and it is transferred in the high-pressure digestion tank that volume is 55mL, be heated to 200 ℃ and insulation reaction 10h, get solid product B; Then be to carry out centrifugation under the 6000r/min condition with solid product B at rotating speed, then use the 15mL deionized water wash, repeated washing twice is 95% washing with alcohol one time with the 20mL massfraction, places dry 4h under 60 ℃ of conditions, obtains particle A.
3.00g cetyl trimethylammonium bromide, 17.00mL octane, 5.00mL propyl carbinol are added in the 250mL Erlenmeyer flask successively, add again 2.00g ammonium meta-vanadate and 100mL deionized water, place 70 ℃ of water-baths under the 5000r/min condition, to stir 15min, get microemulsion A; Then 3.00g cetyl trimethylammonium bromide, 17.00mL octane, 5.00mL propyl carbinol are added in the 250mL Erlenmeyer flask successively, add again the dilute sulphuric acid that the 100mL volumetric molar concentration is 0.80mol/L, under the 1000r/min condition, stir 15min, obtain microemulsion B; Microemulsion A is mixed with microemulsion B, then under the 1000r/min condition, stir 10min, leave standstill 10h, centrifugal 20min under the 6000r/min condition removes supernatant liquor again, is 95% washing with alcohol with the 15mL massfraction, repeated washing 5 times, obtain solid product C and with its dry 24h under 100 ℃ of conditions, place again retort furnace roasting 2h under 500 ℃ of conditions, obtain particle B.
20mg particle A and 20mg particle B are added in the 250mL Erlenmeyer flask, add again 1.16g polyvinylpyrrolidone and 100mL deionized water, ultrasonic concussion 10min, adding the 1.00mL mass concentration is the HAuCl of 0.02g/mL
4Solution continues ultrasonic concussion 5min; And then adding 2.00mL weight percent is 1% sodium citrate solution, concussion reaction 30min under 40 ℃ of conditions, centrifugal 15min under the 6000r/min condition, remove supernatant liquor, then use the 15mL deionized water wash, repeated washing twice obtains solid product D behind dry 24h under 20 ℃ of conditions.
Be that the activated carbon fiber of 1mm is cut into 5cm * 10cm size with thickness, place deionized water to boil 1h, take out and in the 50mL deionized water, soak 24h, then in baking oven, dry 24h, obtain pretreated Activated Carbon Fiber Electrodes; With 0.1g solid product D, place the 10mL dehydrated alcohol, then ultrasonic concussion 10min takes out 10 μ L and drops on the pretreated Activated Carbon Fiber Electrodes, leaves standstill 30min under 20 ℃ of conditions, obtains modified electrode A; Then the 1mL thiophene being added the 10mL volumetric molar concentration is the H of 10mol/L
3PO
4In the solution, as the ionic liquid of electropolymerization, take the modified electrode A that obtains as working electrode, take the Pt electrode as to electrode, take the Ag electrode as reference electrode, 0-2V cyclic voltammetry polymerization 10 circles, sweep velocity is 45mV/s, obtains nanometer Fe
3O
4-V
2O
5The film modified Activated Carbon Fiber Electrodes of-Au doping Polythiophene.
The below is the nanometer Fe of using the inventive method to make
3O
4-V
2O
5The film modified Activated Carbon Fiber Electrodes of-Au doping Polythiophene is processed experiment to coking chemical waste water, further specifies the present invention.
The nanometer Fe of using the inventive method to make
3O
4-V
2O
5The film modified Activated Carbon Fiber Electrodes of-Au doping Polythiophene is processed experiment to coking chemical waste water, and the result shows the efficiently volatile phenol in the Treatment of Wastewater in Coking of this electrode: when the volatile phenol concentration in the waste water is 284mg/L, with nanometer Fe
3O
4-V
2O
5The film modified Activated Carbon Fiber Electrodes of-Au doping Polythiophene is negative electrode, and pH is 3.5, and voltage is 13V, and the treatment time is 30min, and volatile phenol concentration is 15.37mg/L after processing, and processing efficiency reaches 94.59%.
Claims (1)
1. nanometer Fe
3O
4-V
2O
5The preparation technology of the film modified Activated Carbon Fiber Electrodes of-Au doping Polythiophene is characterized in that, the concrete steps of this technique are as follows:
(1) with 5.30g FeCl
3Be dissolved in the 35mL ethylene glycol, under the 1000r/min agitation condition, add 5.28g NaAc and stir 30min, obtain mixed solution A;
(2) mixed solution A that step (1) is obtained is transferred in the high-pressure digestion tank that volume is 55mL, is heated to 200 ℃ and insulation reaction 10h, obtains solid product B;
(3) the solid product B that step (2) is obtained is to carry out centrifugation under the 6000r/min condition at rotating speed, then use the 15mL deionized water wash, repeated washing twice is 95% washing with alcohol one time with the 20mL massfraction, place dry 4h under 60 ℃ of conditions, obtain particle A;
(4) 3.00g cetyl trimethylammonium bromide, 17.00mL octane, 5.00mL propyl carbinol are added in the 250mL Erlenmeyer flask successively, add again 2.00g ammonium meta-vanadate and 100mL deionized water, place 70 ℃ of water-baths under the 5000r/min condition, to stir 15min, obtain microemulsion A;
(5) 3.00g cetyl trimethylammonium bromide, 17.00mL octane, 5.00mL propyl carbinol are added in the 250mL Erlenmeyer flask successively, add again the dilute sulphuric acid that the 100mL volumetric molar concentration is 0.80mol/L, under the 1000r/min condition, stir 15min, obtain microemulsion B;
(6) the microemulsion A that step (4) is obtained mixes with the microemulsion B that step (5) obtains, then under the 1000r/min condition, stir 10min, leave standstill 10h, centrifugal 20min under the 6000r/min condition again, remove supernatant liquor, be 95% washing with alcohol with the 15mL massfraction, repeated washing 5 times obtains solid product C;
(7) the solid product C that step (6) is obtained dry 24h under 100 ℃ of conditions places retort furnace roasting 2h under 500 ℃ of conditions again, obtains particle B;
(8) the particle B that the particle A that 20mg step (3) is obtained and 20mg step (7) obtain adds in the 250mL Erlenmeyer flask, add again 1.16g polyvinylpyrrolidone and 100mL deionized water, ultrasonic concussion 10min, adding the 1.00mL mass concentration is the HAuCl of 0.02g/mL
4Solution continues ultrasonic concussion 5min;
(9) adding the 2.00mL weight percent in the Erlenmeyer flask of step (8) is 1% sodium citrate solution, concussion reaction 30min under 40 ℃ of conditions, centrifugal 15min under the 6000r/min condition, remove supernatant liquor, then use the 15mL deionized water wash, repeated washing twice obtains solid product D behind dry 24h under 20 ℃ of conditions;
(10) be that the activated carbon fiber of 1mm is cut into 5cm * 10cm size with thickness, place the 100mL deionized water to boil 1h, take out and in the 50mL deionized water, soak 24h, then in baking oven, dry 24h, obtain pretreated Activated Carbon Fiber Electrodes;
(11) the solid product D that 0.1g step (9) is obtained, place the 10mL dehydrated alcohol, then ultrasonic concussion 10min takes out 10 μ L and drops on the pretreated Activated Carbon Fiber Electrodes of step (10), under 20 ℃ of conditions, leave standstill 30min, obtain modified electrode A;
(12) the 1mL thiophene being added the 10mL volumetric molar concentration is the H of 10.0mol/L
3PO
4In the solution, as the ionic liquid of electropolymerization, the modified electrode A that obtains take step (11) is as working electrode, take the Pt electrode as to electrode, and take the Ag electrode as reference electrode, 0～2V cyclic voltammetry polymerization, 10 circles, sweep velocity is 45mV/s, obtains nanometer Fe
3O
4-V
2O
5The film modified Activated Carbon Fiber Electrodes of-Au doping Polythiophene.
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| CN105600866A (en) * | 2016-02-27 | 2016-05-25 | 太原理工大学 | Preparing method of electro-assisted photocatalysis cathode used for removing inorganic halite in water |
| CN106517437A (en) * | 2016-11-21 | 2017-03-22 | 北京益清源环保科技有限公司 | Modified carbon fiber particle electrode with electrocatalytic thiophene removal function and preparation method thereof |
| CN106601501A (en) * | 2017-03-07 | 2017-04-26 | 扬州大学 | Preparation method of three-dimensional band-shaped structure AlV3O9 electrode material for supercapacitor |
| CN108083393A (en) * | 2017-12-28 | 2018-05-29 | 光合强化（北京）生物科技有限公司 | The graphite electrode modified based on PbO-NiO-MgO and thiophene |
| CN108163931A (en) * | 2017-12-28 | 2018-06-15 | 光合强化（北京）生物科技有限公司 | The graphite electrode modified based on CeO-ZrO-NiO and pyrazine |
| CN108178248A (en) * | 2017-12-28 | 2018-06-19 | 光合强化（北京）生物科技有限公司 | The graphite electrode modified based on CuO-CoO-ZnO and pyridine |
| CN108178247A (en) * | 2017-12-28 | 2018-06-19 | 光合强化（北京）生物科技有限公司 | The graphite electrode modified based on CrO-FeO-PbO and quinoline |
| JP2021127518A (en) * | 2020-02-14 | 2021-09-02 | トヨタ自動車株式会社 | Polythiophene-based compound/carbon fiber cloth electrode for water-splitting oxygen generation and manufacturing method thereof |
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|---|---|---|---|---|
| CN105600866A (en) * | 2016-02-27 | 2016-05-25 | 太原理工大学 | Preparing method of electro-assisted photocatalysis cathode used for removing inorganic halite in water |
| CN106517437A (en) * | 2016-11-21 | 2017-03-22 | 北京益清源环保科技有限公司 | Modified carbon fiber particle electrode with electrocatalytic thiophene removal function and preparation method thereof |
| CN106601501A (en) * | 2017-03-07 | 2017-04-26 | 扬州大学 | Preparation method of three-dimensional band-shaped structure AlV3O9 electrode material for supercapacitor |
| CN108083393A (en) * | 2017-12-28 | 2018-05-29 | 光合强化（北京）生物科技有限公司 | The graphite electrode modified based on PbO-NiO-MgO and thiophene |
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| JP2021127518A (en) * | 2020-02-14 | 2021-09-02 | トヨタ自動車株式会社 | Polythiophene-based compound/carbon fiber cloth electrode for water-splitting oxygen generation and manufacturing method thereof |
| JP7133661B2 (en) | 2020-02-14 | 2022-09-08 | トヨタ自動車株式会社 | Polythiophene-based compound/carbon fiber cloth electrode for generating water-splitting oxygen and method for producing the same |
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