CN104016448B - Be applicable to three-dimensional porous negative electrode and the preparation technology thereof of electricity-Fenton system - Google Patents
Be applicable to three-dimensional porous negative electrode and the preparation technology thereof of electricity-Fenton system Download PDFInfo
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- CN104016448B CN104016448B CN201410281312.4A CN201410281312A CN104016448B CN 104016448 B CN104016448 B CN 104016448B CN 201410281312 A CN201410281312 A CN 201410281312A CN 104016448 B CN104016448 B CN 104016448B
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Abstract
The invention discloses a kind of three-dimensional porous negative electrode and the preparation technology thereof that are applicable to electricity-Fenton system.Graphite Powder 99 pre-treatment is obtained rear substance B, and substance B obtains paste A again after KCl, polyoxyethylene octylphenol ether, ethanol, the trimethyl carbinol and ptfe emulsion process; The titanium net side of being smeared by paste A after treatment obtains material E through extrusion process; By Pt (NO
3)
2solution B is prepared into, by Sr (NO with Virahol
3)
2, CoCl
2and NiCl
2be prepared into solution C; Substance B, the KCl aqueous solution, polyoxyethylene octylphenol ether, ethanol, the trimethyl carbinol, solution B, solution C and ptfe emulsion are prepared into paste B; Opposite side paste B being spread upon material E can obtain being applicable to the three-dimensional porous negative electrode of electricity-Fenton system again after extruding, calcining, cooling.
Description
Technical field
The invention belongs to the chemically modified electrode technical field of electrocatalytic oxidation reduction, particularly a kind of three-dimensional porous negative electrode and preparation technology thereof being applicable to electricity-Fenton system.
Background technology
In recent years, utilize electrochemical method process organic wastewater with difficult degradation thereby to be valued by the people gradually, wherein hydrogen peroxide because it is nontoxic, the feature of noresidue and receiving much attention.Hydrogen peroxide can further with Fe
2+there is Fenton (Fenton) reaction, be converted into strong oxidizer hydroxyl radical free radical (OH), greatly can improve the clearance of pollutent.The outer add mode of the hydrogen peroxide adopted in water technology at present not only increases the transportation cost of wastewater treatment, and easily decomposes due to hydrogen peroxide, makes it actively reduce, 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 current this respect 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 well can 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 composition of negative electrode, and therefore developing suitable cathode material is the key improving hydrogen peroxide yield.Due to three-dimensional porous negative electrode have 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, thus obtains high hydrogen peroxide yield.Also lack the research of the aspects such as three-dimensional porous negative electrode and preparation method thereof at present.
Summary of the invention
Object of the present invention provides a kind of three-dimensional porous negative electrode and the preparation technology thereof that are applicable to electricity-Fenton system.Its concrete steps are as follows:
(1) get 6.5g Graphite Powder 99 to add in 500mL beaker, add 100mL deionized water and boil 2h, remove upper strata impurity and vacuum filtration, the Graphite Powder 99 after suction filtration is put into 95 DEG C of dry 12h of baking oven, obtain substance A;
(2) substance A is put into 500mL beaker, in beaker, add the HCl that 100mL concentration is 0.45mol/L, put into 95 DEG C of dry 24h of baking oven after stirring 6h, obtain substance B;
(3) be 16cm by area
2500mL beaker put into by square titanium net, add 100mL deionized water and boil 1h, take out titanium net 250mL washed with de-ionized water, titanium net after cleaning is put into 500mL beaker, add the hydrochloric acid soln immersion 0.5h that 100mL concentration is 0.1mol/L, then take out titanium net 250mL deionized water rinsing, after drying, obtain substance C;
(4) 4.5g substance B is put into 500mL beaker, then add the KCl aqueous solution that 10mL concentration is 4.5mol/L, 8.5mL mass percent concentration be 30% the polyoxyethylene octylphenol ether aqueous solution, 40mL ethanol, the 35mL trimethyl carbinol, 10min is stirred under 100r/min condition, then the ptfe emulsion that 7.5mL mass percent concentration is 70% is added, 10min is stirred under 100r/min condition, obtain solution A, solution A is put into 95 DEG C of thermostat water baths, be paste to solution, obtain paste A;
(5) side paste A being spread upon substance C obtains material D, is put on tabletting machine by material D, and pressurize 1min under pressure is 2t condition, obtains material E;
(6) by 50ml concentration be the Pt (NO of 0.5mol/L
3)
2add in 150ml Virahol, obtain solution B;
(7) by 10ml concentration be the Sr (NO of 0.5mol/L
3)
2solution and 100ml concentration are the CoCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the NiCl that 10ml concentration is 0.5mol/L
2solution, shakes up and obtains solution C;
(8) 0.8g substance B is put into 500mL beaker, then add the KCl aqueous solution that 5.5mL concentration is 4.5mol/L, 4.5mL mass percent concentration be 30% the polyoxyethylene octylphenol ether aqueous solution, 40mL ethanol, the 35mL trimethyl carbinol, 5mL solution B, 7mL solution C, 10min is stirred under 100r/min condition, then the ptfe emulsion that 2.5mL mass percent concentration is 70% is added, 10min is stirred under 100r/min condition, obtain solution D, solution D is put into 80 DEG C of thermostat water baths, be paste to solution, obtain paste B;
(9) opposite side paste B being spread upon material E obtains material F, is put on tabletting machine by material F, and pressurize 1min under pressure is 2t condition, obtains material G;
(10) material G is put into 300 DEG C of retort furnaces and calcine 1h, being then placed in thermocompressor, is 350 DEG C in temperature, and pressure is pressurize 1min under the condition of 10t, can obtain the three-dimensional porous negative electrode being applicable to electricity-Fenton system after cooling.
The invention has the beneficial effects as follows, the three-dimensional porous cathodic oxygen reduction catalytic performance of the obtained electricity-Fenton system that is applicable to is high, and electrode life is long.
Embodiment
The invention provides a kind of three-dimensional porous negative electrode and the preparation technology thereof that are applicable to electricity-Fenton system, illustrate below by an example and in fact execute process.
Embodiment 1.
Get 6.5g Graphite Powder 99 to add in 500mL beaker, add 100mL deionized water and boil 2h, remove upper strata impurity and vacuum filtration, the Graphite Powder 99 after suction filtration is put into 95 DEG C of dry 12h of baking oven, obtain substance A; Substance A is put into 500mL beaker, in beaker, add the HCl that 100mL concentration is 0.45mol/L, put into 95 DEG C of dry 24h of baking oven after stirring 6h, obtain substance B;
Be 16cm by area
2500mL beaker put into by square titanium net, add 100mL deionized water and boil 1h, take out titanium net 250mL washed with de-ionized water, titanium net after cleaning is put into 500mL beaker, add the hydrochloric acid soln immersion 0.5h that 100mL concentration is 0.1mol/L, then take out titanium net 250mL deionized water rinsing, after drying, obtain substance C;
4.5g substance B is put into 500mL beaker, then add the KCl aqueous solution that 10mL concentration is 4.5mol/L, 8.5mL mass percent concentration be 30% the polyoxyethylene octylphenol ether aqueous solution, 40mL ethanol, the 35mL trimethyl carbinol, 10min is stirred under 100r/min condition, then the ptfe emulsion that 7.5mL mass percent concentration is 70% is added, 10min is stirred under 100r/min condition, obtain solution A, solution A is put into 95 DEG C of thermostat water baths, be paste to solution, obtain paste A;
Side paste A being spread upon substance C obtains material D, is put on tabletting machine by material D, and pressurize 1min under pressure is 2t condition, obtains material E;
Be the Pt (NO of 0.5mol/L by 50ml concentration
3)
2add in 150ml Virahol, obtain solution B;
Be the Sr (NO of 0.5mol/L by 10ml concentration
3)
2solution and 100ml concentration are the CoCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the NiCl that 10ml concentration is 0.5mol/L
2solution, shakes up and obtains solution C;
0.8g substance B is put into 500mL beaker, then add the KCl aqueous solution that 5.5mL concentration is 4.5mol/L, 4.5mL mass percent concentration be 30% the polyoxyethylene octylphenol ether aqueous solution, 40mL ethanol, the 35mL trimethyl carbinol, 5mL solution B, 7mL solution C, 10min is stirred under 100r/min condition, then the ptfe emulsion that 2.5mL mass percent concentration is 70% is added, 10min is stirred under 100r/min condition, obtain solution D, solution D is put into 80 DEG C of thermostat water baths, be paste to solution, obtain paste B;
Opposite side paste B being spread upon material E obtains material F, is put on tabletting machine by material F, and pressurize 1min under pressure is 2t condition, obtains 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 pressure is pressurize 1min under the condition of 10t, can obtain the three-dimensional porous negative electrode being applicable to electricity-Fenton system after cooling.
Here is that the three-dimensional porous negative electrode being applicable to electricity-Fenton system using the inventive method to obtain carries out process experiment to trichloroisocyanuric acid waste water, further illustrates the present invention.
The obtained three-dimensional porous negative electrode of the inventive method is used to carry out process experiment to trichloroisocyanuric acid waste water, result shows that this electrode efficiently can remove the COD in trichloroisocyanuric acid waste water: when in intaking, COD is 1243mg/L, with three-dimensional porous negative electrode for negative electrode, pH is 3.5, voltage is 15V, treatment time is 180min, adds Fe
2+as catalyzer, after process, COD is 86mg/L, and processing efficiency reaches 93.08%.
Claims (1)
1. be applicable to a three-dimensional porous negative electrode for electricity-Fenton system, it is characterized in that, the concrete steps of the preparation technology of this three-dimensional porous negative electrode are as follows:
(1) get 6.5g Graphite Powder 99 to add in 500mL beaker, add 100mL deionized water and boil 2h, remove upper strata impurity and vacuum filtration, the Graphite Powder 99 after suction filtration is put into 95 DEG C of dry 12h of baking oven, obtain substance A;
(2) substance A is put into 500mL beaker, in beaker, add the HCl that 100mL concentration is 0.45mol/L, put into 95 DEG C of dry 24h of baking oven after stirring 6h, obtain substance B;
(3) be 16cm by area
2500mL beaker put into by square titanium net, add 100mL deionized water and boil 1h, take out titanium net 250mL washed with de-ionized water, titanium net after cleaning is put into 500mL beaker, add the hydrochloric acid soln immersion 0.5h that 100mL concentration is 0.1mol/L, then take out titanium net 250mL deionized water rinsing, after drying, obtain substance C;
(4) 4.5g substance B is put into 500mL beaker, then add the KCl aqueous solution that 10mL concentration is 4.5mol/L, 8.5mL mass percent concentration be 30% the polyoxyethylene octylphenol ether aqueous solution, 40mL ethanol, the 35mL trimethyl carbinol, 10min is stirred under 100r/min condition, then the ptfe emulsion that 7.5mL mass percent concentration is 70% is added, 10min is stirred under 100r/min condition, obtain solution A, solution A is put into 95 DEG C of thermostat water baths, be paste to solution, obtain paste A;
(5) side paste A being spread upon substance C obtains material D, is put on tabletting machine by material D, and pressurize 1min under pressure is 2t condition, obtains material E;
(6) by 50ml concentration be the Pt (NO of 0.5mol/L
3)
2add in 150ml Virahol, obtain solution B;
(7) by 10ml concentration be the Sr (NO of 0.5mol/L
3)
2solution and 100ml concentration are the CoCl of 0.5mol/L
2solution joins in 120ml Virahol and 5ml concentrated hydrochloric acid, and then adds the NiCl that 10ml concentration is 0.5mol/L
2solution, shakes up and obtains solution C;
(8) 0.8g substance B is put into 500mL beaker, then add the KCl aqueous solution that 5.5mL concentration is 4.5mol/L, 4.5mL mass percent concentration be 30% the polyoxyethylene octylphenol ether aqueous solution, 40mL ethanol, the 35mL trimethyl carbinol, 5mL solution B, 7mL solution C, 10min is stirred under 100r/min condition, then the ptfe emulsion that 2.5mL mass percent concentration is 70% is added, 10min is stirred under 100r/min condition, obtain solution D, solution D is put into 80 DEG C of thermostat water baths, be paste to solution, obtain paste B;
(9) opposite side paste B being spread upon material E obtains material F, is put on tabletting machine by material F, and pressurize 1min under pressure is 2t condition, obtains material G;
(10) material G is put into 300 DEG C of retort furnaces and calcine 1h, being then placed in thermocompressor, is 350 DEG C in temperature, and pressure is pressurize 1min under the condition of 10t, can obtain the three-dimensional porous negative electrode being applicable to electricity-Fenton system after cooling.
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| CN102659221A (en) * | 2012-05-10 | 2012-09-12 | 刘娟 | Electro-catalytic oxidation material for wastewater treatment, preparation method and application |
| CN103539231A (en) * | 2013-10-30 | 2014-01-29 | 北京师范大学 | Two-dimensional electrode reactor used for treating nitrogen, sulfur and oxygen containing heterocyclic compound wastewater |
| CN103556176A (en) * | 2013-10-30 | 2014-02-05 | 北京师范大学 | Electrocatalytic anode plate with high activity to nitrogen, sulfur and oxygen heterocyclic compounds and preparation process thereof |
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| CN102659221A (en) * | 2012-05-10 | 2012-09-12 | 刘娟 | Electro-catalytic oxidation material for wastewater treatment, preparation method and application |
| CN103539231A (en) * | 2013-10-30 | 2014-01-29 | 北京师范大学 | Two-dimensional electrode reactor used for treating nitrogen, sulfur and oxygen containing heterocyclic compound wastewater |
| CN103556176A (en) * | 2013-10-30 | 2014-02-05 | 北京师范大学 | Electrocatalytic anode plate with high activity to nitrogen, sulfur and oxygen heterocyclic compounds and preparation process thereof |
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