CN103046072B - 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 preparation method of a Mn/Nano-G|foam-Ni/Pd combination electrode, 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 global industry, water pollution problems is also more and more serious, particularly as waste water such as chemical industry, dyestuff, pharmacy due to high density, high toxicity, the reasons such as difficult degradation, administer and expend that fund is many, difficulty is large.In recent years, the organic pollutant in Electrochemical Technologies for Degradating waste water is adopted to receive much attention.Electrocatalysis high-grade oxidized technology (AEOP) can be at normal temperatures and pressures, directly or indirectly hydroxyl radical free radical is produced by there being the electrode reaction of catalytic activity, thus the organic pollutant of the effectively difficult biochemical treatment of degraded, overcome in high-level oxidation technology the defect needing to add oxidising agent.Because oxygen directly can not produce OH and so on active substance in cathodic reduction, therefore utilize oxygen to produce hydrogen peroxide in cathodic reduction and carry out the focus that degradable organic pollutant becomes research.H
2o
2a kind of strong oxidizer, can organic pollutant in oxidized waste water, its reaction product is water and oxygen, can not produce secondary pollution.In addition, the hydroxyl radical free radical generated by hydroperoxidation has extremely strong oxidisability, to organism non-selectivity, organic pollutant in 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 the most promising method of process organic waste water.
At present, the cathode material that hydrogen peroxide generating process uses is mostly graphite, mesh structural porous carbon dioxide process carbon electrode, carbon-tetrafluoroethylene oxygenated cathode and mercury electrode etc.After repeated, phenol degrading rate significantly reduces carbon material/tetrafluoroethylene single-layer electrodes electrode, and stability is bad, and reusing is low, and repeatedly uses and just there will be the phenomenon such as blow-up, foaming.
Summary of the invention
The present invention is that will to solve current carbon material/tetrafluoroethylene single-layer electrodes electrode stability poor, repeatedly uses the problem that there will be the phenomenon such as blow-up, foaming, provides Mn/Nano-G|foam-Ni/Pd combined electrode and preparation method thereof
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 up of manganese, natural flake graphite and tetrafluoroethylene, wherein the quality of manganese is the 3%-10% of natural flake graphite quality, the mass ratio 2-5:1 of natural flake graphite and tetrafluoroethylene; Described nickel foam absorption conductive layer is made up of 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, carries out according to the following steps:
One, natural flake graphite is made nano-graphite;
Two, manganese is loaded in nano-graphite: get 1-2g nano-graphite and join in 20-30mL deionized water, at room temperature stir, then add 0.48-0.5g manganese acetate, stir, obtain suspension liquid, in suspension liquid, then dropwise add the KMnO of 12-15mL0.1mol/L
4solution, continues stirring until suspension liquid variable color, then suspension liquid is heated to 80-90 DEG C, insulation 30min, filters to be placed in 80 DEG C of baking ovens and dries, through retort furnace 350-400 DEG C of roasting 2-3h, namely obtain the nano-graphite of Supported Manganese;
Three, the nano-graphite of Supported Manganese is mixed with tetrafluoroethylene, the mass ratio 2-5:1 of nano-graphite and tetrafluoroethylene, under being placed in the water bath with thermostatic control condition of 60-70 DEG C, drip 0.5-3mL dehydrated alcohol, be stirred to evenly, obtain lotion, adopt tabletting machine by lotion roll-in repeatedly again, the nano-graphite compound film sheet that thickness is 0.8-1mm is made in roll compacting, at 80 DEG C of dry 2-3h, as nano-graphite catalysis conductive layer;
Four, supported palladium in nickel foam, obtains and carries palladium nickel foam;
Five, by 0.5-2mL mass concentration be 2% the chitosan aqueous solution be evenly coated in and carry in palladium nickel foam, in 60-70 DEG C of dry 30-40min, then a year palladium nickel foam being immersed mass concentration is completely 3-5min in the glutaraldehyde water solution of 1%, take out in 60-70 DEG C of oven dry, obtain foam-Ni/Pd thin slice, as nickel foam absorption conductive layer;
Six, mass concentration is adopted to be that the 2% chitosan aqueous solution is as binding agent, nano-graphite compound film sheet step one prepared is fixed on foam-Ni/Pd thin slice prepared by step 2, two-layer diaphragm 2-3h is pressed at 60-70 DEG C, dry, namely obtain Mn/Nano-G|foam-Ni/Pd combined electrode.
Beneficial effect of the present invention:
The present invention uses nano-graphite for raw material, nano-graphite is as a kind of nano level new carbon, there is abundant laminated structure, except well having continued the good absorption property of graphite type material and conductivity, nano-graphite particle is little simultaneously, reference area is large, it can be used as the additive of electrode materials or electrode materials, the property that common carbon material electrode does not have can be obtained.But the degradation effect of single nano-graphite material is limited, therefore there is at coarse nano-graphite area load manganese etc. the metal oxide of catalytic performance, while the catalytic performance improving nano-graphite conductive network, also greatly can improve the growing amount of hydroxyl radical free radical in the degradation effect of phenol in cathode compartment and cathode compartment.
In diaphragm electrolysis system, the Mn/Nano-G|foam-Ni/Pd combined electrode prepared with the present invention is negative electrode, and under lasting aeration condition, current density is 39mA/cm
2, electrolyte concentration is 0.10mol/L, and initial phenol concentration is 100mg/L, electrolysis 120min, and the degradation rate of phenol can reach 96%-100%.
Mn/Nano-G|foam-Ni/Pd combined electrode prepared by the present invention still can ensure higher phenol degrading rate after a number of uses, good stability.And there is not the phenomenons such as breakage, blow-up, foaming in electrode after a number of uses.
Accompanying drawing explanation
Fig. 1 is the SEM photo of the nano-graphite of the Supported Manganese that embodiment nine step 2 obtains; Fig. 2 is the SEM photo on nano-graphite compound film sheet surface prepared by embodiment nine step 3; Fig. 3 is the SEM photo that year palladium nickel foam of embodiment nine step 4 acquisition amplifies 400 times; Fig. 4 is the SEM photo that year palladium nickel foam of embodiment nine step 4 acquisition amplifies 5000 times; Fig. 5 is Mn/Nano-G|foam-Ni/Pd combined electrode phenol degrading rate time history plot prepared by embodiment nine; Fig. 6 is that Mn/Nano-G|foam-Ni/Pd combined electrode prepared by embodiment nine recycles, the result that 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 up of manganese, natural flake graphite and tetrafluoroethylene, wherein the quality of manganese is the 3%-10% of natural flake graphite quality, the mass ratio 2-5:1 of natural flake graphite and tetrafluoroethylene; Described nickel foam absorption conductive layer is made up of palladium and nickel foam, and wherein the mol ratio of palladium and nickel foam is 1:150-300.
Embodiment two: present embodiment and embodiment one unlike: the quality of manganese is the 5%-6% of natural flake graphite quality.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one are unlike the mass ratio 4:1 of natural flake graphite and tetrafluoroethylene.Other is identical with embodiment one.
Embodiment four: present embodiment and embodiment one unlike: 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 nano-graphite: get 1-2g nano-graphite and join in 20-30mL deionized water, at room temperature stir, then add 0.48-0.5g manganese acetate, stir, obtain suspension liquid, in suspension liquid, then dropwise add the KMnO of 12-15mL0.1mol/L
4solution, continues stirring until suspension liquid variable color, then suspension liquid is heated to 80-90 DEG C, insulation 30min, filters to be placed in 80 DEG C of baking ovens and dries, through retort furnace 350-400 DEG C of roasting 2-3h, namely obtain the nano-graphite of Supported Manganese;
Three, the nano-graphite of Supported Manganese is mixed with tetrafluoroethylene, the mass ratio 2-5:1 of nano-graphite and tetrafluoroethylene, under being placed in the water bath with thermostatic control condition of 60-70 DEG C, drip 0.5-3mL dehydrated alcohol, be stirred to evenly, obtain lotion, adopt tabletting machine by lotion roll-in repeatedly again, the nano-graphite compound film sheet that thickness is 0.8-1mm is made in roll compacting, at 80 DEG C of dry 2-3h, as nano-graphite catalysis conductive layer;
Four, supported palladium in nickel foam, obtains and carries palladium nickel foam;
Five, by 0.5-2mL mass concentration be 2% the chitosan aqueous solution be evenly coated in and carry in palladium nickel foam, in 60-70 DEG C of dry 30-40min, then a year palladium nickel foam being immersed mass concentration is completely 3-5min in the glutaraldehyde water solution of 1%, take out in 60-70 DEG C of oven dry, obtain foam-Ni/Pd thin slice, as nickel foam absorption conductive layer;
Six, mass concentration is adopted to be that the 2% chitosan aqueous solution is as binding agent, nano-graphite compound film sheet step one prepared is fixed on foam-Ni/Pd thin slice prepared by step 2, two-layer diaphragm 2-3h is pressed at 60-70 DEG C, dry, namely obtain Mn/Nano-G|foam-Ni/Pd combined electrode.
Embodiment six: present embodiment and embodiment five unlike: the concrete grammar in step one, natural flake graphite being made nano-graphite is: the ratio of natural flake graphite and potassium permanganate 10:1 in mass ratio mixed, put into the container filling perchloric acid solution, Keep agitation, 40min is reacted under 35 DEG C of water bath with thermostatic control conditions, obtain resultant, resultant is carried out washing and suction filtration to washing lotion in neutral, then resultant is placed in 80 DEG C of drying in oven, obtain expansible black lead, expansible black lead is put into crucible, be put in microwave bulking 20s in microwave oven and obtain sulphur-free expanded graphite, again the ratio of sulphur-free expanded graphite and dehydrated alcohol 1:1000 is in mass ratio mixed, put into the Ultrasonic Cleaners ultrasonication 12-14h of 45W power, in 80 DEG C of oven dry, namely nano-graphite is received.Other is identical with embodiment five.
Embodiment seven: present embodiment and embodiment five or six are unlike the mass ratio 3:1 of nano-graphite and tetrafluoroethylene in step 3.Other is identical with embodiment five or six.
Embodiment eight: one of present embodiment and embodiment five to seven unlike: in step 4, in nickel foam, the concrete grammar of supported palladium is: using 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, the Palladous chloride deposit fluid that concentration is 1mmol/L is added in galvanic deposition cell, Palladous chloride deposit fluid is made not have negative electrode and anode, under the condition of 10mA continuous current, 40 DEG C of constant temperature, galvanic deposit 120min becomes colorless to deposit fluid, Keep agitation Palladous chloride deposit fluid in 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: the ratio of natural flake graphite and potassium permanganate 10:1 in mass ratio mixed, put into the container filling perchloric acid solution, Keep agitation, 40min is reacted under 35 DEG C of water bath with thermostatic control conditions, obtain resultant, resultant is carried out washing and suction filtration to washing lotion in neutral, then resultant is placed in 80 DEG C of drying in oven, obtain expansible black lead, expansible black lead is put into crucible, be put in microwave bulking 20s in microwave oven and obtain sulphur-free expanded graphite, again the ratio of sulphur-free expanded graphite and dehydrated alcohol 1:1000 is in mass ratio mixed, put into the Ultrasonic Cleaners ultrasonication 12h of 45W power, in 80 DEG C of oven dry, namely nano-graphite is received,
Two, manganese is loaded in nano-graphite: get 1.5g nano-graphite and join in 20mL deionized water, at room temperature stir, then add 0.49g manganese acetate, stir, obtain suspension liquid, in suspension liquid, then dropwise add the KMnO of 13mL0.1mol/L
4solution, continues stirring until suspension liquid variable color, then suspension liquid is heated to 80 DEG C, insulation 30min, filters to be placed in 80 DEG C of baking ovens and dries, through retort furnace 350 DEG C of roasting 2h, namely obtain the nano-graphite of Supported Manganese;
Three, the nano-graphite of Supported Manganese is mixed with tetrafluoroethylene, the mass ratio 3:1 of nano-graphite and tetrafluoroethylene, under being placed in the water bath with thermostatic control condition of 60 DEG C, drip 2mL dehydrated alcohol, be stirred to evenly, obtain lotion, adopt tabletting machine by lotion roll-in repeatedly again, the nano-graphite compound film sheet that thickness is 1mm is made in roll compacting, at 80 DEG C of dry 2h, as nano-graphite catalysis conductive layer;
Four, supported palladium in nickel foam, obtains and carries palladium nickel foam;
Five, by 1mL mass concentration be 2% the chitosan aqueous solution be evenly coated in and carry in palladium nickel foam, in 60 DEG C of dry 30min, then a year palladium nickel foam being immersed mass concentration is completely 5min in the glutaraldehyde water solution of 1%, take out in 60 DEG C of oven dry, obtain foam-Ni/Pd thin slice, as nickel foam absorption conductive layer;
Six, mass concentration is adopted to be that the 2% chitosan aqueous solution is as binding agent, nano-graphite compound film sheet step one prepared is fixed on foam-Ni/Pd thin slice prepared by step 2, two-layer diaphragm 2h is pressed at 60 DEG C, dry, namely obtain Mn/Nano-G|foam-Ni/Pd combined electrode.
In present embodiment step 4, in nickel foam, the concrete grammar of supported palladium is: using 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, the Palladous chloride deposit fluid that concentration is 1mmol/L is added in galvanic deposition cell, Palladous chloride deposit fluid is made not have negative electrode and anode, under the condition of 10mA continuous current, 40 DEG C of constant temperature, galvanic deposit 120min becomes colorless to deposit fluid, Keep agitation Palladous chloride deposit fluid in electrodeposition process.
As shown in Figure 1, can find out that Mn oxide is nano level bar-shaped existence, its length is about about 150nm to the SEM photo of the nano-graphite of the Supported Manganese that present embodiment step 2 obtains, and is evenly distributed on nano-graphite lamella surface.
The SEM photo on nano-graphite compound film sheet surface prepared by present embodiment step 3 as shown in Figure 2, under the condition of high-amplification-factor, the internal structure in visible groove and gap, abundant pore passage structure is had in uncompacted gap, adding electrode specific surface area, define well while conductive network, also make the oxygen in liquid phase can enter inside, duct, facilitate the generation of hydrogen reduction Hydrogen Peroxide and cathode compartment phase reaction.In addition, visible Mn oxide is that granular particles is inlayed at the electrode surface uniformly, and this inserted distribution effectively adds the surface-area of catalyzer, and Mn oxide can be made to give full play to its catalytic performance.
Year palladium nickel foam that present embodiment step 4 obtains amplifies the SEM photo of 400 times as shown in Figure 3, clearly can see that palladium metal is deposited on nickel foam substrate surface uniformly.Compared with nickel foam substrate, the avtive spot of its specific surface area and catalyzed reaction increases all greatly, is conducive to the transfer of electronics and the generation of Cathodic oxygen reduction.Year palladium nickel foam that step 4 obtains amplifies the SEM photo of 5000 times as shown in Figure 4, under higher magnification, palladium metal particle has covered whole nickel foam substrate surface completely, and presents closely uniform dendritic structure, there is good spatial extension, to be evenly distributed and in picturesque disorder.Acicular structure has darker groove structure, and which increase the specific surface area of palladium load foam nickel material and the avtive spot of reaction, this is conducive to making full use of of catalyzer.
In diaphragm electrolysis system, the Mn/Nano-G|foam-Ni/Pd combined electrode prepared with present embodiment is negative electrode, and under lasting aeration condition, current density is 39mA/cm
2, electrolyte concentration is 0.10mol/L, and initial phenol concentration is 100mg/L, electrolysis 120min, and 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.
Recycle Mn/Nano-G|foam-Ni/Pd combined electrode prepared by present embodiment, the result that phenol degrading rate changes with access times as shown in Figure 6.After Mn/Nano-G|foam-Ni/Pd combined electrode recycles nine times, its degradation rate does not significantly reduce.This shows, this two-layer composite cathode, has satisfactory stability and reusability, can save material simultaneously, reduces degraded cost.Through reusing repeatedly having good stability of electrode, the phenomenon such as do not occur bubbling, the breakage of traditional stainless (steel) wire carrier combined electrode, come off.As can be seen here, Mn/Nano-G|foam-Ni/Pd combined electrode can reusing and stability make it obtain larger application prospect in the treatment of waste water.
Claims (4)
- The preparation method of 1.Mn/Nano-G|foam-Ni/Pd combined electrode, is characterized in that the method is carried out according to the following steps:One, natural flake graphite is made nano-graphite;Two, manganese is loaded in nano-graphite: get 1-2g nano-graphite and join in 20-30mL deionized water, at room temperature stir, then add 0.48-0.5g manganese acetate, stir, obtain suspension liquid, in suspension liquid, then dropwise add the KMnO of 12-15mL0.1mol/L 4solution, continues stirring until suspension liquid variable color, then suspension liquid is heated to 80-90 DEG C, insulation 30min, filters to be placed in 80 DEG C of baking ovens and dries, through retort furnace 350-400 DEG C of roasting 2-3h, namely obtain the nano-graphite of Supported Manganese;Three, the nano-graphite of Supported Manganese is mixed with tetrafluoroethylene, the mass ratio 2-5:1 of nano-graphite and tetrafluoroethylene, under being placed in the water bath with thermostatic control condition of 60-70 DEG C, drip 0.5-3mL dehydrated alcohol, be stirred to evenly, obtain lotion, adopt tabletting machine by lotion roll-in repeatedly again, the nano-graphite compound film sheet that thickness is 0.8-1mm is made in roll compacting, at 80 DEG C of dry 2-3h, as nano-graphite catalysis conductive layer;Four, supported palladium in nickel foam, obtains and carries palladium nickel foam;Five, by 0.5-2mL mass concentration be 2% the chitosan aqueous solution be evenly coated in and carry in palladium nickel foam, in 60-70 DEG C of dry 30-40min, then a year palladium nickel foam being immersed mass concentration is completely 3-5min in the glutaraldehyde water solution of 1%, take out in 60-70 DEG C of oven dry, obtain foam-Ni/Pd thin slice, as nickel foam absorption conductive layer;Six, mass concentration is adopted to be that the 2% chitosan aqueous solution is as binding agent, nano-graphite compound film sheet step 3 prepared is fixed on foam-Ni/Pd thin slice prepared by step 5, two-layer diaphragm 2-3h is pressed at 60-70 DEG C, dry, namely obtain Mn/Nano-G|foam-Ni/Pd combined electrode.
- 2. the preparation method of Mn/Nano-G|foam-Ni/Pd combined electrode according to claim 1, it is characterized in that the concrete grammar in step one, natural flake graphite being made nano-graphite is: the ratio of natural flake graphite and potassium permanganate 10:1 in mass ratio mixed, put into the container filling perchloric acid solution, Keep agitation, 40min is reacted under 35 DEG C of water bath with thermostatic control conditions, obtain resultant, resultant is carried out washing and suction filtration to washing lotion in neutral, then resultant is placed in 80 DEG C of drying in oven, obtain expansible black lead, expansible black lead is put into crucible, be put in microwave bulking 20s in microwave oven and obtain sulphur-free expanded graphite, again the ratio of sulphur-free expanded graphite and dehydrated alcohol 1:1000 is in mass ratio mixed, put into the Ultrasonic Cleaners ultrasonication 12-14h of 45W power, in 80 DEG C of oven dry, namely nano-graphite is received.
- 3. the preparation method of Mn/Nano-G|foam-Ni/Pd combined electrode according to claim 1 and 2, is characterized in that the mass ratio 3:1 of nano-graphite and tetrafluoroethylene in step 3.
- 4. the preparation method of Mn/Nano-G|foam-Ni/Pd combined electrode according to claim 3, is characterized in that the concrete grammar of supported palladium in nickel foam in step 4 is: using 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, the Palladous chloride deposit fluid that concentration is 1mmol/L is added in galvanic deposition cell, Palladous chloride deposit fluid is made not have negative electrode and anode, under the condition of 10mA continuous current, 40 DEG C of constant temperature, galvanic deposit 120min becomes colorless to deposit fluid, Keep agitation Palladous chloride deposit fluid in electrodeposition process.
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