CN103046072A - Mn/Nano-G|foam-Ni/Pd combination electrode and preparation method thereof - Google Patents
Mn/Nano-G|foam-Ni/Pd combination electrode and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a Mn/Nano-G|foam-Ni/Pd combination electrode and a preparation method thereof, and solves the problems of expansion, foaming and other phenomena due to repeated usage of the conventional carbon/polytetrafluoroethylene monolayer electrode with poor electrode stability. The combination electrode comprises a nano-graphite catalysis conductive layer and a foam nickel adsorption conductive layer; and the preparation method comprises the steps as follows: 1, preparing natural flake graphite into nano-graphite; 2, loading manganese into the nano-graphite; 3, preparing the nano-graphite catalysis conductive layer; 4, loading palladium onto foam nickel to obtain palladium-loaded foam nickel; 5, preparing the foam nickel adsorption conductive layer; 6, fixing a nano-graphite composite membrane to a foam-Ni/Pd sheet, pressing the membrane and the sheet, and drying to obtain the Mn/Nano-G|foam-Ni/Pd combination electrode. The Mn/Nano-G|foam-Ni/Pd combination electrode is applied to the field of organic pollutants in wastewater degraded by an electrochemical process.
Description
Technical field
The present invention relates to a kind of combined electrode and preparation method thereof.
Background technology
Along with the fast development of whole world industry, water pollution problems is also more and more serious, particularly as waste water such as chemical industry, dyestuff, pharmacy because high density, high toxicity, the reasons such as difficult degradation are administered and are expended that fund is many, difficulty is large.In recent years, adopt the organic pollutant in the Electrochemical Technologies for Degradating waste water to receive much attention.Electrocatalysis high-grade oxidized technology (AEOP) can be at normal temperatures and pressures, directly or indirectly produce hydroxyl radical free radical by the electrode reaction that catalytic activity is arranged, thereby the organic pollutant of the difficult biochemical treatment of effectively degrading has overcome the defective that needs to add oxidising agent in the high-level oxidation technology.Because oxygen can not directly produce OH and so on active substance in cathodic reduction, therefore utilize oxygen to produce hydrogen peroxide in cathodic reduction and come degradable organic pollutant to become the focus of research.H
2O
2A kind of strong oxidizer, the organic pollutant in can oxidized waste water, its reaction product is water and oxygen, can not produce secondary pollution.In addition, the hydroxyl radical free radical that is generated by hydroperoxidation has extremely strong oxidisability, to the organism non-selectivity, organic pollutant in the water can be direct oxidation into carbonic acid gas and water or be oxidized to nontoxic small molecules, oxidation is thorough fast, non-secondary pollution, and processing efficiency is high, easy and simple to handle, therefore this method is to process the most promising method of organic waste water.
At present, the employed cathode material of hydrogen peroxide generating process mostly is greatly graphite, mesh structural porous carbon dioxide process carbon electrode, carbon-tetrafluoroethylene oxygenated cathode and mercury electrode etc.Carbon material/tetrafluoroethylene single-layer electrodes electrode is after reusing, and the phenol degrading rate significantly reduces, and stability is bad, and reusing is low, and repeatedly the phenomenons such as blow-up, foaming will appear in use.
Summary of the invention
The present invention is that will to solve carbon current material/tetrafluoroethylene single-layer electrodes electrode stability poor, and repeatedly the problem of the phenomenons such as blow-up, foaming can appear in use, and Mn/Nano-G|foam-Ni/Pd combined electrode and preparation method thereof is provided
Mn/Nano-G|foam-Ni/Pd combined electrode of the present invention comprises nano-graphite catalysis conductive layer and nickel foam absorption conductive layer, described nano-graphite catalysis conductive layer is made by manganese, natural flake graphite and tetrafluoroethylene, wherein the quality of manganese is the 3%-10% of natural flake graphite quality, the mass ratio 2-5 of natural flake graphite and tetrafluoroethylene: 1; Described nickel foam absorption conductive layer is made by palladium and nickel foam, and wherein the mol ratio of palladium and nickel foam is 1: 150-300.
The preparation method of above-mentioned Mn/Nano-G|foam-Ni/Pd combined electrode, carry out according to the following steps:
One, natural flake graphite is made nano-graphite;
Two, manganese is loaded in the nano-graphite: get the 1-2g nano-graphite and join in the 20-30mL deionized water, at room temperature stir, then add the 0.48-0.5g manganese acetate, stir, suspension liquid, then dropwise add the KMnO of 12-15mL 0.1mol/L in the suspension liquid
4Solution continues stirring until the suspension liquid variable color, then suspension liquid is heated to 80-90 ℃, and insulation 30min filters to be placed in 80 ℃ of baking ovens and dries, and through retort furnace 350-400 ℃ of roasting 2-3h, namely obtains the nano-graphite of Supported Manganese;
Three, the nano-graphite with Supported Manganese mixes with tetrafluoroethylene, the mass ratio 2-5 of nano-graphite and tetrafluoroethylene: 1, place under 60-70 ℃ the water bath with thermostatic control condition, drip the 0.5-3mL dehydrated alcohol, be stirred to evenly, get lotion, adopt again tabletting machine with repeatedly roll-in of lotion, the nano-graphite compound film sheet that thickness is 0.8-1mm is made in roll compacting, at 80 ℃ of dry 2-3h, as nano-graphite catalysis conductive layer;
Four, supported palladium on nickel foam obtains to carry the palladium nickel foam;
Five, be that 2% the chitosan aqueous solution evenly is coated in and carries on the palladium nickel foam with the 0.5-2mL mass concentration, in 60-70 ℃ of dry 30-40min, then will carrying the palladium nickel foam, to immerse mass concentration fully be 3-5min in 1% the glutaraldehyde water solution, take out in 60-70 ℃ of oven dry, obtain the foam-Ni/Pd thin slice, as nickel foam absorption conductive layer;
Six, adopting mass concentration is that the 2% chitosan aqueous solution is as binding agent, the nano-graphite compound film sheet of step 1 preparation is fixed on the foam-Ni/Pd thin slice of step 2 preparation, press two-layer diaphragm 2-3h under 60-70 ℃, drying namely obtains the Mn/Nano-G|foam-Ni/Pd combined electrode.
Beneficial effect of the present invention:
The present invention uses nano-graphite to be raw material, nano-graphite is as a kind of nano level new carbon, has abundant laminated structure, continued the graphite type material good absorption property and conductivity except good, the nano-graphite particle is little simultaneously, reference area is large, with its additive as electrode materials or electrode materials, can obtain the property that common carbon material electrode is not had.But the degradation effect of single nano-graphite material is limited, therefore the metal oxide that has catalytic performance at coarse nano-graphite area load manganese etc., in the catalytic performance that improves the nano-graphite conductive network, also can greatly improve the growing amount of hydroxyl radical free radical in the degradation effect of phenol in the cathode compartment and the cathode compartment.
In the diaphragm electrolysis system, take the Mn/Nano-G|foam-Ni/Pd combined electrode of the present invention preparation as negative electrode, continuing under the aeration condition, current density is 39mA/cm
2, electrolyte concentration is 0.10mol/L, initial phenol concentration is 100mg/L, and electrolysis 120min, the degradation rate of phenol can reach 96%-100%.
The Mn/Nano-G|foam-Ni/Pd combined electrode of the present invention's preparation still can guarantee higher phenol degrading rate, good stability after repeatedly using.And repeatedly using rear electrode that the phenomenons such as breakage, blow-up, foaming do not occur.
Description of drawings
Fig. 1 is the SEM photo of the nano-graphite of the Supported Manganese that obtains of embodiment nine step 2; Fig. 2 is the SEM photo on the nano-graphite compound film sheet surface of embodiment nine step 3 preparation; Fig. 3 is that the palladium nickel foam of carrying that embodiment nine step 4 obtain is amplified 400 times SEM photo; Fig. 4 is that the palladium nickel foam of carrying that embodiment nine step 4 obtain is amplified 5000 times SEM photo; Fig. 5 is the Mn/Nano-G|foam-Ni/Pd combined electrode phenol degrading rate time history plot of embodiment nine preparations; Fig. 6 is that the Mn/Nano-G|foam-Ni/Pd combined electrode of embodiment nine preparations recycles the result that the phenol degrading rate changes with access times.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment Mn/Nano-G|foam-Ni/Pd combined electrode comprises nano-graphite catalysis conductive layer and nickel foam absorption conductive layer, described nano-graphite catalysis conductive layer is made by manganese, natural flake graphite and tetrafluoroethylene, wherein the quality of manganese is the 3%-10% of natural flake graphite quality, the mass ratio 2-5 of natural flake graphite and tetrafluoroethylene: 1; Described nickel foam absorption conductive layer is made by palladium and nickel foam, and wherein the mol ratio of palladium and nickel foam is 1: 150-300.
Embodiment two: what present embodiment and embodiment one were different is: the quality of manganese is the 5%-6% of natural flake graphite quality.Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is: the mass ratio of natural flake graphite and tetrafluoroethylene 4: 1.Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is: the mol ratio of palladium and nickel foam is 1: 200.Other is identical with embodiment one.
Embodiment five: the preparation method of present embodiment Mn/Nano-G|foam-Ni/Pd combined electrode, carry out according to the following steps:
One, natural flake graphite is made nano-graphite;
Two, manganese is loaded in the nano-graphite: get the 1-2g nano-graphite and join in the 20-30mL deionized water, at room temperature stir, then add the 0.48-0.5g manganese acetate, stir, suspension liquid, then dropwise add the KMnO of 12-15mL 0.1mol/L in the suspension liquid
4Solution continues stirring until the suspension liquid variable color, then suspension liquid is heated to 80-90 ℃, and insulation 30min filters to be placed in 80 ℃ of baking ovens and dries, and through retort furnace 350-400 ℃ of roasting 2-3h, namely obtains the nano-graphite of Supported Manganese;
Three, the nano-graphite with Supported Manganese mixes with tetrafluoroethylene, the mass ratio 2-5 of nano-graphite and tetrafluoroethylene: 1, place under 60-70 ℃ the water bath with thermostatic control condition, drip the 0.5-3mL dehydrated alcohol, be stirred to evenly, get lotion, adopt again tabletting machine with repeatedly roll-in of lotion, the nano-graphite compound film sheet that thickness is 0.8-1mm is made in roll compacting, at 80 ℃ of dry 2-3h, as nano-graphite catalysis conductive layer;
Four, supported palladium on nickel foam obtains to carry the palladium nickel foam;
Five, be that 2% the chitosan aqueous solution evenly is coated in and carries on the palladium nickel foam with the 0.5-2mL mass concentration, in 60-70 ℃ of dry 30-40min, then will carrying the palladium nickel foam, to immerse mass concentration fully be 3-5min in 1% the glutaraldehyde water solution, take out in 60-70 ℃ of oven dry, obtain the foam-Ni/Pd thin slice, as nickel foam absorption conductive layer;
Six, adopting mass concentration is that the 2% chitosan aqueous solution is as binding agent, the nano-graphite compound film sheet of step 1 preparation is fixed on the foam-Ni/Pd thin slice of step 2 preparation, press two-layer diaphragm 2-3h under 60-70 ℃, drying namely obtains the Mn/Nano-G|foam-Ni/Pd combined electrode.
Embodiment six: what present embodiment and embodiment five were different is: the concrete grammar of in the step 1 natural flake graphite being made nano-graphite is: with natural flake graphite and potassium permanganate in mass ratio 10: 1 ratio mix, put into the container that fills perchloric acid solution, continue to stir, under 35 ℃ of water bath with thermostatic control conditions, react 40min, get resultant, resultant washed with suction filtration to washing lotion be neutral, then resultant is placed 80 ℃ of drying in oven, obtain expansible black lead, expansible black lead is put into crucible, be put in that microwave bulking 20s obtains sulphur-free expanded graphite in the microwave oven, again with sulphur-free expanded graphite and dehydrated alcohol in mass ratio 1: 1000 ratio mix, put into the Ultrasonic Cleaners ultrasonication 12-14h of 45W power, in 80 ℃ of oven dry, namely receive nano-graphite.Other is identical with embodiment five.
Embodiment seven: what present embodiment was different from embodiment five or six is: the mass ratio 3: 1 of nano-graphite and tetrafluoroethylene in the step 3.Other is identical with embodiment five or six.
Embodiment eight: what present embodiment was different from one of embodiment five to seven is: in the step 4 on nickel foam the concrete grammar of supported palladium be: with the synthetic glass reactor as galvanic deposition cell, with Ti/IrO
2/ RuO
2Electrode is as anode, nickel foam is as negative electrode, adopt D.C. regulated power supply, adding concentration in the galvanic deposition cell is the Palladous chloride deposit fluid of 1mmol/L, make the Palladous chloride deposit fluid not have negative electrode and anode, under the condition of 10mA continuous current, 40 ℃ of constant temperature, galvanic deposit 120min becomes colorless to deposit fluid, the lasting Palladous chloride deposit fluid that stirs in the electrodeposition process.Other is identical with one of embodiment five to seven.
Embodiment nine: the preparation method of present embodiment Mn/Nano-G|foam-Ni/Pd combined electrode, carry out according to the following steps:
One, natural flake graphite is made nano-graphite: with natural flake graphite and potassium permanganate in mass ratio 10: 1 ratio mix, put into the container that fills perchloric acid solution, continue to stir, under 35 ℃ of water bath with thermostatic control conditions, react 40min, get resultant, resultant washed with suction filtration to washing lotion be neutral, then resultant is placed 80 ℃ of drying in oven, obtain expansible black lead, expansible black lead is put into crucible, be put in that microwave bulking 20s obtains sulphur-free expanded graphite in the microwave oven, again with sulphur-free expanded graphite and dehydrated alcohol in mass ratio 1: 1000 ratio mix, put into the Ultrasonic Cleaners ultrasonication 12h of 45W power, in 80 ℃ of oven dry, namely receive nano-graphite;
Two, manganese is loaded in the nano-graphite: get the 1.5g nano-graphite and join in the 20mL deionized water, at room temperature stir, then add the 0.49g manganese acetate, stir, get suspension liquid, then dropwise add the KMnO of 13mL 0.1mol/L in the suspension liquid
4Solution continues stirring until the suspension liquid variable color, then suspension liquid is heated to 80 ℃, and insulation 30min filters to be placed in 80 ℃ of baking ovens and dries, and through 350 ℃ of roasting 2h of retort furnace, namely obtains the nano-graphite of Supported Manganese;
Three, the nano-graphite with Supported Manganese mixes with tetrafluoroethylene, the mass ratio of nano-graphite and tetrafluoroethylene 3: 1, place under 60 ℃ the water bath with thermostatic control condition, drip the 2mL dehydrated alcohol, be stirred to evenly, get lotion, adopt again tabletting machine with repeatedly roll-in of lotion, the nano-graphite compound film sheet that thickness is 1mm is made in roll compacting, at 80 ℃ of dry 2h, as nano-graphite catalysis conductive layer;
Four, supported palladium on nickel foam obtains to carry the palladium nickel foam;
Five, be that 2% the chitosan aqueous solution evenly is coated in and carries on the palladium nickel foam with the 1mL mass concentration, in 60 ℃ of dry 30min, then will carrying the palladium nickel foam, to immerse mass concentration fully be 5min in 1% the glutaraldehyde water solution, take out in 60 ℃ of oven dry, obtain the foam-Ni/Pd thin slice, as nickel foam absorption conductive layer;
Six, adopting mass concentration is that the 2% chitosan aqueous solution is as binding agent, the nano-graphite compound film sheet of step 1 preparation is fixed on the foam-Ni/Pd thin slice of step 2 preparation, press two-layer diaphragm 2h under 60 ℃, drying namely obtains the Mn/Nano-G|foam-Ni/Pd combined electrode.
In the present embodiment step 4 on nickel foam the concrete grammar of supported palladium be: with the synthetic glass reactor as galvanic deposition cell, with Ti/IrO
2/ RuO
2Electrode is as anode, nickel foam is as negative electrode, adopt D.C. regulated power supply, adding concentration in the galvanic deposition cell is the Palladous chloride deposit fluid of 1mmol/L, make the Palladous chloride deposit fluid not have negative electrode and anode, under the condition of 10mA continuous current, 40 ℃ of constant temperature, galvanic deposit 120min becomes colorless to deposit fluid, the lasting Palladous chloride deposit fluid that stirs in the electrodeposition process.
The SEM photo of the nano-graphite of the Supported Manganese that the present embodiment step 2 obtains can find out that Mn oxide is nano level bar-shaped existence as shown in Figure 1, and its length is about about 150nm, is evenly distributed on nano-graphite lamella surface.
The SEM photo on the nano-graphite compound film sheet surface of present embodiment step 3 preparation as shown in Figure 2, under the condition of high-amplification-factor, as seen the internal structure in groove and slit, abundant pore passage structure is arranged in the uncompacted slit, increasing electrode specific surface area, when having formed well conductive network, also make the oxygen in the liquid phase can enter inside, duct, promoted the generation of hydrogen reduction Hydrogen Peroxide and cathode compartment phase reaction.In addition, visible Mn oxide is granular particles and is embedded in uniformly on the electrode surface, and this inserted distribution has effectively increased the surface-area of catalyzer, can make Mn oxide give full play to its catalytic performance.
The SEM photo that carries 400 times of palladium nickel foam amplifications that the present embodiment step 4 obtains can see clearly that palladium metal has been deposited on the nickel foam substrate surface uniformly as shown in Figure 3.Compare with nickel foam substrate, the avtive spot of its specific surface area and catalyzed reaction all increases greatly, is conducive to the transfer of electronics and the generation of Cathodic oxygen reduction.The SEM photo that carries 5000 times of palladium nickel foam amplifications that step 4 obtains as shown in Figure 4, under higher magnification, the palladium metal particle has covered whole nickel foam substrate surface fully, and has presented closely uniform dendritic structure, good space ductility is arranged, be evenly distributed and in picturesque disorder.Acicular structure has darker groove structure, has increased like this specific surface area of palladium load foam nickel material and the avtive spot of reaction, and this is conducive to taking full advantage of of catalyzer.
In the diaphragm electrolysis system, take the Mn/Nano-G|foam-Ni/Pd combined electrode of present embodiment preparation as negative electrode, continuing under the aeration condition, current density is 39mA/cm
2, electrolyte concentration is 0.10mol/L, initial phenol concentration is 100mg/L, and electrolysis 120min, the degradation rate of phenol can reach 98.7%.Mn/Nano-G|foam-Ni/Pd combined electrode phenol degrading rate time history plot as shown in Figure 5.
Mn/Nano-G|foam-Ni/Pd combined electrode to present embodiment preparation recycles, and the result that the phenol degrading rate changes with access times as shown in Figure 6.After the Mn/Nano-G|foam-Ni/Pd combined electrode recycled nine times, its degradation rate did not significantly reduce.This shows, this two-layer composite cathode has satisfactory stability and reusability, can save material simultaneously, reduces the degraded cost.Through reusing repeatedly having good stability of electrode, do not occur traditional stainless (steel) wire carrier combined electrode bubbling, breakage, the phenomenon such as come off.This shows, but the reusing of Mn/Nano-G|foam-Ni/Pd combined electrode and stability make it obtain larger application prospect in wastewater treatment.
Claims (8)
1.Mn/Nano-G|foam-Ni/Pd combined electrode, it is characterized in that this combined electrode comprises nano-graphite catalysis conductive layer and nickel foam absorption conductive layer, described nano-graphite catalysis conductive layer is made by manganese, natural flake graphite and tetrafluoroethylene, wherein the quality of manganese is the 3%-10% of natural flake graphite quality, the mass ratio 2-5 of natural flake graphite and tetrafluoroethylene: 1; Described nickel foam absorption conductive layer is made by palladium and nickel foam, and wherein the mol ratio of palladium and nickel foam is 1: 150-300.
2. Mn/Nano-G|foam-Ni/Pd combined electrode according to claim 1, the quality that it is characterized in that manganese is the 5%-6% of natural flake graphite quality.
3. Mn/Nano-G|foam-Ni/Pd combined electrode according to claim 1 is characterized in that the mass ratio 4: 1 of natural flake graphite and tetrafluoroethylene.
4. Mn/Nano-G|foam-Ni/Pd combined electrode according to claim 1, the mol ratio that it is characterized in that palladium and nickel foam is 1: 200.
5. the preparation method of Mn/Nano-G|foam-Ni/Pd combined electrode as claimed in claim 1 is characterized in that the method carries out according to the following steps:
One, natural flake graphite is made nano-graphite;
Two, manganese is loaded in the nano-graphite: get the 1-2g nano-graphite and join in the 20-30mL deionized water, at room temperature stir, then add the 0.48-0.5g manganese acetate, stir, suspension liquid, then dropwise add the KMnO of 12-15mL0.1mol/L in the suspension liquid
4Solution continues stirring until the suspension liquid variable color, then suspension liquid is heated to 80-90 ℃, and insulation 30min filters to be placed in 80 ℃ of baking ovens and dries, and through retort furnace 350-400 ℃ of roasting 2-3h, namely obtains the nano-graphite of Supported Manganese;
Three, the nano-graphite with Supported Manganese mixes with tetrafluoroethylene, the mass ratio 2-5 of nano-graphite and tetrafluoroethylene: 1, place under 60-70 ℃ the water bath with thermostatic control condition, drip the 0.5-3mL dehydrated alcohol, be stirred to evenly, get lotion, adopt again tabletting machine with repeatedly roll-in of lotion, the nano-graphite compound film sheet that thickness is 0.8-1mm is made in roll compacting, at 80 ℃ of dry 2-3h, as nano-graphite catalysis conductive layer;
Four, supported palladium on nickel foam obtains to carry the palladium nickel foam;
Five, be that 2% the chitosan aqueous solution evenly is coated in and carries on the palladium nickel foam with the 0.5-2mL mass concentration, in 60-70 ℃ of dry 30-40min, then will carrying the palladium nickel foam, to immerse mass concentration fully be 3-5min in 1% the glutaraldehyde water solution, take out in 60-70 ℃ of oven dry, obtain the foam-Ni/Pd thin slice, as nickel foam absorption conductive layer;
Six, adopting mass concentration is that the 2% chitosan aqueous solution is as binding agent, the nano-graphite compound film sheet of step 1 preparation is fixed on the foam-Ni/Pd thin slice of step 2 preparation, press two-layer diaphragm 2-3h under 60-70 ℃, drying namely obtains the Mn/Nano-G|foam-Ni/Pd combined electrode.
6. the preparation method of Mn/Nano-G|foam-Ni/Pd combined electrode according to claim 5, it is characterized in that the concrete grammar of in the step 1 natural flake graphite being made nano-graphite is: with natural flake graphite and potassium permanganate in mass ratio 10: 1 ratio mix, put into the container that fills perchloric acid solution, continue to stir, under 35 ℃ of water bath with thermostatic control conditions, react 40min, get resultant, resultant washed with suction filtration to washing lotion be neutral, then resultant is placed 80 ℃ of drying in oven, obtain expansible black lead, expansible black lead is put into crucible, be put in that microwave bulking 20s obtains sulphur-free expanded graphite in the microwave oven, again with sulphur-free expanded graphite and dehydrated alcohol in mass ratio 1: 1000 ratio mix, put into the Ultrasonic Cleaners ultrasonication 12-14h of 45W power, in 80 ℃ of oven dry, namely receive nano-graphite.
7. the mass ratio 3: 1 that it is characterized in that according to claim 5 or the preparation method of 6 described Mn/Nano-G|foam-Ni/Pd combined electrodes, nano-graphite and tetrafluoroethylene in the step 3.
8. the preparation method of Mn/Nano-G|foam-Ni/Pd combined electrode according to claim 7 is characterized in that in the step 4 that the concrete grammar of supported palladium is on nickel foam: with the synthetic glass reactor as galvanic deposition cell, with Ti/IrO
2/ RuO
2Electrode is as anode, nickel foam is as negative electrode, adopt D.C. regulated power supply, adding concentration in the galvanic deposition cell is the Palladous chloride deposit fluid of 1mmol/L, make the Palladous chloride deposit fluid not have negative electrode and anode, under the condition of 10mA continuous current, 40 ℃ of constant temperature, galvanic deposit 120min becomes colorless to deposit fluid, the lasting Palladous chloride deposit fluid that stirs in the electrodeposition process.
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