CN104071866A - Porous membrane cathode for photoelectric-Fenton treating system, as well as preparation technology of porous member cathode - Google Patents
Porous membrane cathode for photoelectric-Fenton treating system, as well as preparation technology of porous member cathode Download PDFInfo
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- CN104071866A CN104071866A CN201410281461.0A CN201410281461A CN104071866A CN 104071866 A CN104071866 A CN 104071866A CN 201410281461 A CN201410281461 A CN 201410281461A CN 104071866 A CN104071866 A CN 104071866A
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Abstract
The invention discloses a porous membrane cathode for a photoelectric-Fenton treating system, as well as a preparation technology of the porous member cathode. The preparation technology comprises the following steps: pretreating graphite powder to obtain a substance B, and treating the substance B through a KNO3 water solution, a nonylphenol polyoxyethylene ether water solution, ethanol, tertbutyl alcohol and polytetrafluoroethylene emulsion to obtain cream A; smearing the cream A on one side of a treated nickel screen, and extruding to obtain a substance E; preparing a solution C; preparing a cream B from the substance B, a KNO3 water solution, a nonylphenol polyoxyethylene ether water solution, ethyl ether, methanol, 2-ethylanthraquinone, the solution C and the polytetrafluoroethylene emulsion; and smearing the cream B on the other side of the substance E, and extruding, forging and cooling to obtain the porous membrane cathode for the photoelectric-Fenton treating system.
Description
Technical field
The invention belongs to the chemically modified electrode technical field of electrocatalytic oxidation reduction, particularly a kind of porous-film negative electrode and preparation technology thereof for photoelectricity-Fenton treatment system.
Background technology
In recent years, utilize electrochemical method to process organic wastewater with difficult degradation thereby and be valued by the people gradually, wherein hydrogen peroxide is because it is nontoxic, the feature of noresidue receives much attention.Hydrogen peroxide can be further and Fe
2+there is Fenton (Fenton) reaction, be converted into strong oxidizer hydroxyl radical free radical (OH), can greatly improve the clearance of pollutent.Outside the hydrogen peroxide adopting in water technology at present, add mode has not only increased the transportation cost of wastewater treatment, and because hydrogen peroxide easily decomposes, makes its activity decreased, and therefore how in situ preparation hydrogen peroxide becomes the focus of research.Domestic and international many scholars to how utilizing electrochemical method to produce hydrogen peroxide are studied, the research of this respect at present mainly concentrates on the exploration of novel cathode material, there is a lot of research to concentrate on and modify cathode material to improve its hydrogen reduction catalytic performance, to produce more hydrogen peroxide.Obtain the productive rate of higher hydrogen peroxide, need to select suitable electrode, increase oxygen to electrode surface mass transfer, simultaneously electrode will have good catalytic activity to oxygen reduction reaction, and can well suppress 4 electron reductions of oxygen and promote 2 electron reductions of Hydrogen Peroxide.These factors depend primarily on the performance of electrode materials and the structure of negative electrode composition, and therefore developing suitable cathode material is the key that improves hydrogen peroxide yield.Because porous-film negative electrode has that reaction table area is large, absorption and the advantage such as mass transfer condition is good, therefore it can utilize large electrode activity internal surface to reach higher apparent current density under relatively low polarization of electrode, thereby obtains high hydrogen peroxide yield.Also lack at present the research of the aspects such as porous-film negative electrode and preparation method thereof.
Summary of the invention
Object of the present invention provides a kind of porous-film negative electrode and preparation technology thereof for photoelectricity-Fenton treatment system.Its concrete steps are as follows:
(1) get 6.5g Graphite Powder 99 and add in 500mL beaker, add 100mL deionized water and boil 2h, remove upper strata impurity vacuum filtration, the Graphite Powder 99 after suction filtration is put into the dry 12h of 95 DEG C of baking ovens, obtain substance A;
(2) substance A being put into 500mL beaker, is the HCl of 0.45mol/L to adding 100mL concentration in beaker, puts into the dry 24h of 95 DEG C of baking ovens after stirring 6h, obtains substance B;
(3) be 16cm by area
2square nickel screen is put into 500mL beaker, add 100mL deionized water and boil 1h, take out nickel screen 250mL washed with de-ionized water, nickel screen after cleaning is put into 500mL beaker, adding 100mL concentration is the hydrochloric acid soln immersion 0.5h of 0.1mol/L, then take out nickel screen 250mL deionized water rinsing, after drying, obtain substance C;
(4) 4.5g substance B is put into 500mL beaker, then adding 10mL concentration is the KCl aqueous solution of 4.5mol/L, the polyoxyethylene nonylphenol ether aqueous solution, 40mL ethanol, the 35mL trimethyl carbinol that 8.5mL mass percent concentration is 30%, under 100r/min condition, stir 10min, then adding 7.5mL mass percent concentration is 70% ptfe emulsion, under 100r/min condition, stir 10min, obtain solution A, solution A is put into 95 DEG C of thermostat water baths, be paste to solution, obtain paste A;
(5) side that paste A is spread upon to substance C obtains material D, material D is put on tabletting machine, and be pressurize 1min under 2t condition at pressure, obtain material E;
(6) by 5.30g FeCl
3be dissolved in 35mL ethylene glycol, under 1000r/min agitation condition, add 5.28g NaAc and stir 30min, obtain mixing solutions B;
(7) mixing solutions B is transferred in the high-pressure digestion tank that volume is 55mL, be heated to 200 DEG C and insulation reaction 10h, obtain solid product M;
(8) be under 6000r/min condition, to carry out centrifugation by solid product M at rotating speed, then use 15mL deionized water wash, the washing with alcohol that repeated washing twice is 95% with 20mL massfraction one time, is placed in dry 4h under 60 DEG C of conditions, obtains particle N;
(9) 20mg particle N is added in 250mL Erlenmeyer flask, then add 1.16g polyvinylpyrrolidone and 100mL deionized water, ultrasonic concussion 10min, adding 1.00mL mass concentration is the HAuCl of 0.02g/mL
4solution, continues ultrasonic concussion 5min;
(10) be 1% sodium citrate solution to adding 2.00mL weight percent in step (9) Erlenmeyer flask after treatment, concussion reaction 30min under 40 DEG C of conditions, centrifugal 15min under 6000r/min condition, remove supernatant liquor, then use 15mL deionized water wash, repeated washing twice obtains solid product P after dry 24h under 20 DEG C of conditions;
(11) 5.00g solid product P, 2.00g Sodium dodecylbenzene sulfonate, 50mL deionized water are added in 150mL Erlenmeyer flask, under 1000r/min condition, stir 10min, obtain solution C;
(12) 1.2g substance B is put into 500mL beaker, then adding 5.5mL concentration is the KNO of 4.5mol/L
3the polyoxyethylene nonylphenol ether aqueous solution, 45mL ether, 35mL methyl alcohol, 3.0g diethyl anthraquinone, 5mL solution C that the aqueous solution, 4.5mL mass percent concentration are 35%, under 100r/min condition, stir 10min, then adding 2.5mL mass percent concentration is 75% ptfe emulsion, under 100r/min condition, stir 10min, obtain solution D, solution D is put into 80 DEG C of thermostat water baths, be paste to solution, obtain paste B;
(13) opposite side that paste B is spread upon to material E obtains material F, material F is put on tabletting machine, and be pressurize 1min under 2t condition at pressure, obtain material G;
(14) material G being put into 300 DEG C of retort furnaces and calcine 1h, be then placed in thermocompressor, is 350 DEG C in temperature, and pressurize 1min under the condition that pressure is 10t can obtain the porous-film negative electrode for photoelectricity-Fenton treatment system after cooling.
The invention has the beneficial effects as follows, the porous-film cathodic oxygen reduction catalytic performance for photoelectricity-Fenton treatment system making is high, and electrode life is long.
Embodiment
The invention provides a kind of porous-film negative electrode and preparation technology thereof for photoelectricity-Fenton treatment system, below by an example, the process of in fact executing is described.
Embodiment 1.
Get 6.5g Graphite Powder 99 and add in 500mL beaker, add 100mL deionized water and boil 2h, remove upper strata impurity vacuum filtration, the Graphite Powder 99 after suction filtration is put into the dry 12h of 95 DEG C of baking ovens, obtain substance A; Substance A is put into 500mL beaker, is the HCl of 0.45mol/L to adding 100mL concentration in beaker, puts into the dry 24h of 95 DEG C of baking ovens after stirring 6h, obtains substance B;
Be 16cm by area
2square nickel screen is put into 500mL beaker, add 100mL deionized water and boil 1h, take out nickel screen 250mL washed with de-ionized water, nickel screen after cleaning is put into 500mL beaker, adding 100mL concentration is the hydrochloric acid soln immersion 0.5h of 0.1mol/L, then take out nickel screen 250mL deionized water rinsing, after drying, obtain substance C;
4.5g substance B is put into 500mL beaker, then adding 10mL concentration is the KCl aqueous solution of 4.5mol/L, the polyoxyethylene nonylphenol ether aqueous solution, 40mL ethanol, the 35mL trimethyl carbinol that 8.5mL mass percent concentration is 30%, under 100r/min condition, stir 10min, then adding 7.5mL mass percent concentration is 70% ptfe emulsion, under 100r/min condition, stir 10min, obtain solution A, solution A is put into 95 DEG C of thermostat water baths, be paste to solution, obtain paste A;
A side that paste A is spread upon to substance C obtains material D, material D is put on tabletting machine, and be pressurize 1min under 2t condition at pressure, obtain material E;
By 5.30g FeCl
3be dissolved in 35mL ethylene glycol, under 1000r/min agitation condition, add 5.28g NaAc and stir 30min, obtain mixing solutions B;
Mixing solutions B is transferred in the high-pressure digestion tank that volume is 55mL, be heated to 200 DEG C and insulation reaction 10h, obtain solid product M;
Be under 6000r/min condition, to carry out centrifugation by solid product M at rotating speed, then use 15mL deionized water wash, the washing with alcohol that repeated washing twice is 95% with 20mL massfraction one time, is placed in dry 4h under 60 DEG C of conditions, obtains particle N;
20mg particle N is added in 250mL Erlenmeyer flask, then add 1.16g polyvinylpyrrolidone and 100mL deionized water, ultrasonic concussion 10min, adding 1.00mL mass concentration is the HAuCl of 0.02g/mL
4solution, continues ultrasonic concussion 5min; Be 1% sodium citrate solution to adding 2.00mL weight percent in Erlenmeyer flask, concussion reaction 30min under 40 DEG C of conditions, centrifugal 15min under 6000r/min condition, remove supernatant liquor, then use 15mL deionized water wash, repeated washing twice obtains solid product P after dry 24h under 20 DEG C of conditions;
5.00g solid product P, 2.00g Sodium dodecylbenzene sulfonate, 50mL deionized water are added in 150mL Erlenmeyer flask, under 1000r/min condition, stir 10min, obtain solution C;
1.2g substance B is put into 500mL beaker, and then adding 5.5mL concentration is the KNO of 4.5mol/L
3the polyoxyethylene nonylphenol ether aqueous solution, 45mL ether, 35mL methyl alcohol, 3.0g diethyl anthraquinone, 5mL solution C that the aqueous solution, 4.5mL mass percent concentration are 35%, under 100r/min condition, stir 10min, then adding 2.5mL mass percent concentration is 75% ptfe emulsion, under 100r/min condition, stir 10min, obtain solution D, solution D is put into 80 DEG C of thermostat water baths, be paste to solution, obtain paste B;
The opposite side that paste B is spread upon to material E obtains material F, material F is put on tabletting machine, and be pressurize 1min under 2t condition at pressure, obtain material G;
Material G being put into 300 DEG C of retort furnaces and calcine 1h, be then placed in thermocompressor, is 350 DEG C in temperature, and pressurize 1min under the condition that pressure is 10t can obtain the porous-film negative electrode for photoelectricity-Fenton treatment system after cooling.
Be that the porous-film negative electrode for photoelectricity-Fenton treatment system that uses the inventive method to make is processed experiment to trichloroisocyanuric acid waste water below, further illustrate the present invention.
The porous-film negative electrode that uses the inventive method to make is processed experiment to trichloroisocyanuric acid waste water, result shows that this electrode can efficiently remove the COD in trichloroisocyanuric acid waste water: in the time that in water inlet, COD is 1243mg/L, taking porous-film negative electrode as negative electrode, pH is 3.5, voltage is 15V, treatment time is 180min, under UV-irradiation condition, adds Fe
2+as catalyzer, after processing, COD is 53mg/L, and processing efficiency reaches 95.74%.
Claims (1)
1. for porous-film negative electrode and the preparation technology thereof of photoelectricity-Fenton treatment system, it is characterized in that, the concrete steps of this technique are as follows:
(1) get 6.5g Graphite Powder 99 and add in 500mL beaker, add 100mL deionized water and boil 2h, remove upper strata impurity vacuum filtration, the Graphite Powder 99 after suction filtration is put into the dry 12h of 95 DEG C of baking ovens, obtain substance A;
(2) substance A being put into 500mL beaker, is the HCl of 0.45mol/L to adding 100mL concentration in beaker, puts into the dry 24h of 95 DEG C of baking ovens after stirring 6h, obtains substance B;
(3) be 16cm by area
2square nickel screen is put into 500mL beaker, add 100mL deionized water and boil 1h, take out nickel screen 250mL washed with de-ionized water, nickel screen after cleaning is put into 500mL beaker, adding 100mL concentration is the hydrochloric acid soln immersion 0.5h of 0.1mol/L, then take out nickel screen 250mL deionized water rinsing, after drying, obtain substance C;
(4) 4.5g substance B is put into 500mL beaker, then adding 10mL concentration is the KCl aqueous solution of 4.5mol/L, the polyoxyethylene nonylphenol ether aqueous solution, 40mL ethanol, the 35mL trimethyl carbinol that 8.5mL mass percent concentration is 30%, under 100r/min condition, stir 10min, then adding 7.5mL mass percent concentration is 70% ptfe emulsion, under 100r/min condition, stir 10min, obtain solution A, solution A is put into 95 DEG C of thermostat water baths, be paste to solution, obtain paste A;
(5) side that paste A is spread upon to substance C obtains material D, material D is put on tabletting machine, and be pressurize 1min under 2t condition at pressure, obtain material E;
(6) by 5.30g FeCl
3be dissolved in 35mL ethylene glycol, under 1000r/min agitation condition, add 5.28g NaAc and stir 30min, obtain mixing solutions B;
(7) mixing solutions B is transferred in the high-pressure digestion tank that volume is 55mL, be heated to 200 DEG C and insulation reaction 10h, obtain solid product M;
(8) be under 6000r/min condition, to carry out centrifugation by solid product M at rotating speed, then use 15mL deionized water wash, the washing with alcohol that repeated washing twice is 95% with 20mL massfraction one time, is placed in dry 4h under 60 DEG C of conditions, obtains particle N;
(9) 20mg particle N is added in 250mL Erlenmeyer flask, then add 1.16g polyvinylpyrrolidone and 100mL deionized water, ultrasonic concussion 10min, adding 1.00mL mass concentration is the HAuCl of 0.02g/mL
4solution, continues ultrasonic concussion 5min;
(10) be 1% sodium citrate solution to adding 2.00mL weight percent in step (9) Erlenmeyer flask after treatment, concussion reaction 30min under 40 DEG C of conditions, centrifugal 15min under 6000r/min condition, remove supernatant liquor, then use 15mL deionized water wash, repeated washing twice obtains solid product P after dry 24h under 20 DEG C of conditions;
(11) 5.00g solid product P, 2.00g Sodium dodecylbenzene sulfonate, 50mL deionized water are added in 150mL Erlenmeyer flask, under 1000r/min condition, stir 10min, obtain solution C;
(12) 1.2g substance B is put into 500mL beaker, then adding 5.5mL concentration is the KNO of 4.5mol/L
3the polyoxyethylene nonylphenol ether aqueous solution, 45mL ether, 35mL methyl alcohol, 3.0g diethyl anthraquinone, 5mL solution C that the aqueous solution, 4.5mL mass percent concentration are 35%, under 100r/min condition, stir 10min, then adding 2.5mL mass percent concentration is 75% ptfe emulsion, under 100r/min condition, stir 10min, obtain solution D, solution D is put into 80 DEG C of thermostat water baths, be paste to solution, obtain paste B;
(13) opposite side that paste B is spread upon to material E obtains material F, material F is put on tabletting machine, and be pressurize 1min under 2t condition at pressure, obtain material G;
(14) material G being put into 300 DEG C of retort furnaces and calcine 1h, be then placed in thermocompressor, is 350 DEG C in temperature, and pressurize 1min under the condition that pressure is 10t can obtain the porous-film negative electrode for photoelectricity-Fenton treatment system after cooling.
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| CN104787949A (en) * | 2015-05-11 | 2015-07-22 | 北京化工大学 | Method and device for treating refuse leachate through photoelectric Fenton oxidation reaction based on modified gas diffusion electrode |
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| CN105836855B (en) * | 2016-06-13 | 2019-02-15 | 西安工业大学 | A kind of preparation method and application of graphene gas-diffusion electrode |
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| WO2007132077A1 (en) * | 2006-05-16 | 2007-11-22 | Arkema France | Catalytic composition comprising catalytic activated carbon and carbon nanotubes, manufacturing process, electrode and super capacitator comprising the catalytic compound |
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| CN104787949A (en) * | 2015-05-11 | 2015-07-22 | 北京化工大学 | Method and device for treating refuse leachate through photoelectric Fenton oxidation reaction based on modified gas diffusion electrode |
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