CN110407300A - A kind of porous carbon mixed carbon black roll-in electrode material and its preparation method and application - Google Patents

A kind of porous carbon mixed carbon black roll-in electrode material and its preparation method and application Download PDF

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CN110407300A
CN110407300A CN201910683551.5A CN201910683551A CN110407300A CN 110407300 A CN110407300 A CN 110407300A CN 201910683551 A CN201910683551 A CN 201910683551A CN 110407300 A CN110407300 A CN 110407300A
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electrode material
roll
porous carbon
carbon black
mixed
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余方可
马宏瑞
曹天轶
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/467Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
    • C02F1/4672Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • C02F2001/46133Electrodes characterised by the material
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds

Abstract

A kind of porous carbon mixed carbon black roll-in electrode material and its preparation method and application, the method includes the steps 1, porous carbon, carbon black, polytetrafluoroethylene (PTFE) and EtOH Sonicate are uniformly dispersed, and stirring is to thick;Carbon black, polytetrafluoroethylene (PTFE) and EtOH Sonicate are uniformly dispersed, stirred to thick;Step 2, above-mentioned material is distinguished to the upper and lower surfaces of roll-in to metallic mesh;Step 3, it by the processing of obtained anneal of material, is cooled to room temperature to obtain porous carbon mixed carbon black roll-in electrode material;The electrode material can promote H2O2Yield, cathode access times and organic wastewater with difficult degradation thereby is effectively treated, it compares pure carbon black and pure porous carbon is conducive to improve stability, the sluicing intensity of electrode, service life of the GDE electrode in electric Fenton-like system can be extended, had great importance to the use of GDE electrode, the popularization for optimizing its application effect and electric Fenton technology in treatment of Organic Wastewater in electric Fenton-like system.

Description

A kind of porous carbon mixed carbon black roll-in electrode material and its preparation method and application
Technical field
The invention belongs to the technical field of electro catalytic electrode material, specially a kind of porous carbon mixed carbon black roll-in electrode material Material and its preparation method and application.
Background technique
Electric Fenton technology is that one of high-level oxidation technology of industrial organic waste water is effectively treated, and high-level oxidation technology can be write a Chinese character in simplified form For AOPs, it utilizes oxygen (O2) on cathode material surface it is reduced to hydrogen peroxide (H2O2), H2O2Pass through catalyst ferrous ion Fe2+Catalytic decomposition forms the hydroxyl radical free radical OH with strong oxidizing property, to realize the degradation to organic pollutant, therefore electricity Fenton technology is a kind of Modern New, efficient and clean Technologies for Organic Wastewater Treatment.
Air diffusion cathode (is abbreviated as GDE), due to good electric conductivity and convenient and fast aeration approach and as electricity High yield H in Fenton technical system2O2One of best cathodes type, but its H2O2Yield be subject to the group of GDE simultaneously and become a useful person Material.Cathode composition material is considered as improving H in electric Fenton technology2O2Yield and increase cathode are in degradation of contaminant process The biggest factor of performance.
With the cathode sheet that the carbon black of commercialization makes, H2O2Yield is higher, has some superiority in processing organic wastewater, But since carbon black materials electro catalytic activity itself is limited, the performance of this cathode sheet still has the space that can be promoted.As The porous carbon materials of one of cathode common used material in electric Fenton technology, although electric conductivity is not dominant compared with carbon black, its Large specific surface area possesses micropore and meso-hole structure abundant, can provide more electro-catalysis than pure carbon black during electro-catalysis Active site, more convenient and fast substance diffusion path, can promote the absorption of oxygen molecule, be very beneficial for high yield H2O2Oxygen also Original reaction.Therefore, develop a kind of electrode material that porous carbon is mixed with carbon black has to improve electric Fenton cathode electrocatalyst activity Important meaning, but the electrode material mixed at present about porous carbon with carbon black has not been reported.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provide a kind of porous carbon mixed carbon black roll-in electrode material and its Preparation method and application, easy to operate, applicability is wide, has industrial application value, easy to promote and utilize.
The present invention is to be achieved through the following technical solutions:
A kind of preparation method of porous carbon mixed carbon black roll-in electrode material, includes the following steps,
Step 1, mixed system ultrasonic disperse porous carbon, carbon black, polytetrafluoroethylene (PTFE) and ethyl alcohol formed is uniform, is mixed Zoarium system A, wherein the ratio between volume of the quality of porous carbon, the quality of carbon black and ethyl alcohol is (4~12) mg:(10~30) mg:(1 ~3) ml stirs mixed system A to roll-in electrode material Catalytic Layer that is thick, being tentatively modified;
The mixed system ultrasonic disperse that carbon black, polytetrafluoroethylene (PTFE) and ethyl alcohol are formed is uniform, obtains mixed system B, will mix Zoarium system B is stirred to roll-in electrode material diffusion layer that is thick, being tentatively modified;
Step 2, tentatively modified roll-in electrode material Catalytic Layer, tentatively modified roll-in electrode material diffusion layer are distinguished Upper and lower surfaces of the roll-in to metallic mesh, the roll-in electrode material being tentatively modified;
Step 3, tentatively modified roll-in electrode material is made annealing treatment, is cooled to room temperature to obtain porous carbon later mixed Close carbon black roll-in electrode material.
Preferably, roll-in electrode material tentatively modified in step 3 makes annealing treatment 1~2h at 327~450 DEG C.
Preferably, polytetrafluoroethylene (PTFE) described in step 1 uses polytetrafluoroethylene (PTFE) emulsion, polytetrafluoroethylene (PTFE) emulsion Solid content is 50%~60%, in mixed system B the volume of the quality of carbon black, the volume of polytetrafluoroethylene (PTFE) emulsion and ethyl alcohol it Than for (0.4~0.5) mg:(0.4~0.6) ml:(1~3) ml.
Preferably, the ultrasonic time for the mixed system that porous carbon, carbon black, polytetrafluoroethylene (PTFE) and ethyl alcohol form in step 1 is 5 ~30min, the ultrasonic time of the mixed system of carbon black, polytetrafluoroethylene (PTFE) and ethyl alcohol composition are 5~30min.
Preferably, mixed system A, mixed system B are stirred to viscous respectively under 65~80 DEG C of heating water bath in step 1 Thick shape, the roll-in electrode material Catalytic Layer being tentatively modified and tentatively modified roll-in electrode material diffusion layer.
Preferably, porous carbon described in step 1 obtains as follows,
Zn (NO is added in step 1a in ultrapure water or deionized water3)2·6H2After O and 2-methylimidazole react, centrifugation is washed It washs reaction product and obtains the presoma of porous carbon, wherein Zn (NO3)2·6H2The ratio between concentration of O and 2-methylimidazole is 74.4g/ L:(114.03~159.64) g/L;
The presoma of porous carbon is dried in vacuo by step 1b, later 908~1100 under the protection of inert gas 5~7h of calcining carbonization, obtains porous carbon at DEG C.
Further, the presoma of porous carbon is dried in vacuo 5~12h at 45~65 DEG C in step 1b.
A kind of preparation method of the porous carbon mixed carbon black roll-in electrode material as described in above-mentioned any one obtains more Hole carbon mixed carbon black roll-in electrode material.
A kind of application of porous carbon mixed carbon black roll-in electrode material, the porous carbon mixed carbon black roll-in electrode material As cathode, apply in electric Fenton-like system after 2h, H2O2Yield can reach 545mg/L.
A kind of application of porous carbon mixed carbon black roll-in electrode material, the porous carbon mixed carbon black roll-in electrode material Material, is applied when going in removal organic polluter, the percent of decolourization of rhodamine B reaches 100% after 15min.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention is equal by the mixed system ultrasonic disperse for forming porous carbon, carbon black, polytetrafluoroethylene (PTFE) and ethyl alcohol first Tentatively modified roll-in electrode material Catalytic Layer can be obtained to thick in stirring after even, by carbon black, polytetrafluoroethylene (PTFE) and ethyl alcohol Mixed system ultrasonic disperse, which is uniformly stirred afterwards to thick, can be obtained tentatively modified roll-in electrode material diffusion layer, then by gained Catalytic Layer and diffusion layer distinguish the upper and lower surfaces of roll-in to metallic mesh, are cooled to room temperature after finally making annealing treatment To required porous carbon mixed carbon black roll-in electrode material;Make full use of the high electrocatalytic active of porous carbon, i.e. electro-catalysis high yield H2O2And the electric conductivity and economy of hydrocarbon black powder, adhesiveness of the polytetrafluoroethylene (PTFE), that is, PTFE as binder, then gold conjugate Belong to hardness, aeration, electric conductivity and the support force of mesh, so that Catalytic Layer is anti-in the generation hydrogen reduction of solid, liquid, gas three phase boundary It answers and (is abbreviated as ORR), diffusion layer is ventilated for water proof, can promote H2O2Yield, cathode access times and be effectively treated difficult to degrade Organic wastewater, the preparation method of this GDE electrode to the use of GDE electrode in electric Fenton-like system, optimize it at organic wastewater The popularization of application effect and electric Fenton technology in reason has great importance.
Further, pass through Zn (NO3)2·6H2The combination reaction of O and 2-methylimidazole prepares the presoma of porous carbon, warp Cross vacuum drying and the obtained porous carbon of calcining carbonization, can improve the specific surface area of porous carbon, enrich its microcellular structure with it is mesoporous Structure has better electro catalytic activity.
Porous carbon mixed carbon black roll-in electrode material of the invention, improves H2O2Yield, and then increase organic matter degradation Effect, compares pure carbon black and pure porous carbon is conducive to improve stability, the sluicing intensity of electrode, can extend GDE electrode and exist Service life in electric Fenton-like system.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph for the tentatively modified roll-in electrode material diffusion layer that the embodiment of the present invention 1 obtains.
Fig. 2 is the scanning electron microscope (SEM) photograph for the tentatively modified roll-in electrode material Catalytic Layer that the embodiment of the present invention 1 obtains.
Fig. 3 is the roll-in electrode material and pure carbon black materials H in electric Fenton-like system that the embodiment of the present invention 1 obtains2O2Yield Comparison diagram.
Fig. 4 is that the roll-in electrode material that the embodiment of the present invention 1 obtains and pure carbon black materials handle sieve in electric Fenton-like system The effect contrast figure of red bright B.
Fig. 5 is that the roll-in electrode material that the embodiment of the present invention 1 obtains is applied to ten repetitions that electro-catalysis produces hydrogen peroxide Property use test chart.
Fig. 6 is that the roll-in electrode material that the embodiment of the present invention 1 obtains is applied to ten repetitions that electro-catalysis produces hydrogen peroxide Property use power consumption test chart.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and It is not to limit.
A kind of system for the porous carbon mixed carbon black roll-in electrode material being efficiently applied in electric Fenton technical system of the present invention Preparation Method includes the following steps,
Step 1, using 100~150ml ultrapure water or deionized water as solvent, by Zn (NO3)2·6H2O and 2-methylimidazole It is added thereto, at this time Zn (NO3)2·6H2The ratio between concentration of O and 2-methylimidazole is 74.4g/L:(114.03~159.64) g/ L, by after 200~500rpm magnetic agitation 12~combination reaction is complete for 24 hours, using supercentrifuge in 8000~10000rpm Lower to make cleaning agent using methanol, so that 2-methylimidazole residue removal is complete, 8~20min of centrifugation obtains the forerunner of porous carbon Body;
Step 2, the presoma of porous carbon is dried to 5~12h at 45~65 DEG C in a vacuum drying oven;After drying Presoma is put into quartz boat, and inert gas, such as N are passed through in high temperature process furnances2Under be carbonized 5~7h in 908~1100 DEG C of calcinings Afterwards, obtain black powder porous carbon, the porous carbon with high-specific surface area, microcellular structure abundant and meso-hole structure, have electricity Catalytic activity;
Step 3, the mixed system that porous carbon, commercial blacks powder, polytetrafluoroethylene (PTFE) emulsion and ethyl alcohol form is surpassed Sound disperses 5~30min, and at this time mixed system is in uniform state, obtains mixed system A, wherein the quality of porous carbon, carbon black The ratio between volume of quality, the volume of polytetrafluoroethylene (PTFE) emulsion and ethyl alcohol is (4~12) mg:(10~30) mg:(0.1~0.4) Ml:(1~3) ml, mixed system A is stirred under 65~80 DEG C of heating water bath to the thick roll-in electricity being tentatively modified Pole material Catalytic Layer;
Mixed system 5~30min of ultrasonic disperse that carbon black, polytetrafluoroethylene (PTFE) emulsion and ethyl alcohol are formed, mixes at this time System is in uniform state, obtains mixed system B, wherein the quality of carbon black, the volume of polytetrafluoroethylene (PTFE) emulsion and ethyl alcohol The ratio between volume is (0.4~0.5) mg:(0.4~0.6) ml:(1~3) ml, the heating water bath by mixed system B at 65~80 DEG C It is lower to stir to the thick roll-in electrode material diffusion layer being tentatively modified;
The solid content of above-mentioned polytetrafluoroethylene (PTFE) emulsion is 50%~60%, i.e. polytetrafluoroethylene (PTFE) dries under certain condition It is 50%~60% that polytetrafluoroethylene (PTFE), which accounts for the mass percent of polytetrafluoroethylene (PTFE) emulsion, after dry;
Step 4, tentatively modified roll-in electrode material Catalytic Layer, tentatively modified roll-in electrode material diffusion layer are distinguished Roll-in is to the upper and lower surfaces of metallic mesh, i.e., on obverse and reverse, the roll-in electrode material being tentatively modified, this The embodiment of invention only lists steel wire, and the metallic mesh of other pure metal materials, those skilled in the art It can be easy to do this popularization, therefore not enumerate other metallic mesh;
Step 5, tentatively modified roll-in electrode material is placed in Muffle furnace, make annealing treatment 1 at 327~450 DEG C~ 2h is cooled to room temperature to obtain porous carbon mixed carbon black roll-in electrode material later.
Embodiment 1
A kind of preparation side applied to the porous carbon mixed carbon black roll-in electrode material in electric Fenton technical system of the present invention Method includes the following steps,
Step 1, using 100ml ultrapure water as solvent, by Zn (NO3)2·6H2O is added thereto with 2-methylimidazole, at this time Zn (NO3)2·6H2The ratio between concentration of O and 2-methylimidazole is 74.4g/L:114.03g/L, passes through 200rpm magnetic agitation 12hization After closing fully reacting, make cleaning agent using methanol at 8000rpm using supercentrifuge, to go 2-methylimidazole residual Except complete, the presoma of centrifugation 8min acquisition porous carbon;
Step 2, the presoma of porous carbon is dried to 5h at 45 DEG C in a vacuum drying oven;Presoma after drying is put Enter quartz boat, inert gas, such as N are passed through in high temperature process furnances2Under after 908 DEG C of calcinings are carbonized 5h, it is more to obtain black powder Hole carbon, the porous carbon with high-specific surface area, micropore abundant and meso-hole structure, have electro catalytic activity;
Step 3, it is by the commercial blacks powder of 10mg, the ethyl alcohol of 1ml, the porous carbon dust of 4mg and 0.1ml solid content 60% polytetrafluoroethylene (PTFE) emulsion mixing, at this point, the mass ratio that porous carbon dust accounts for hydrocarbon black powder is 40%, ultrasonic disperse 5min, mixed system is in uniform state at this time, 65 DEG C of heating stirrings to it is thick it is spare be Catalytic Layer;
0.5mg commercial blacks powder, the ethyl alcohol of 1ml, the polytetrafluoroethylene (PTFE) emulsion that 0.4ml solid content is 60% are mixed It closes, ultrasonic disperse 10min, mixed system be in uniform state at this time, in 65 DEG C of heating stirrings to thick spare for diffusion layer;
Step 4, divide two sides using twin rollers roll-in two sides to 5cm Catalytic Layer and dispersion layer2Steel wire front and On reverse side, 327 DEG C of annealing 1h in Muffle furnace are placed in, are cooled to room temperature i.e. acquisition cathode material.
The roll-in electrode material diffusion layer scanning electron microscope that the example obtains is as shown in Figure 1, as control, roll-in electrode material Catalytic Layer is as shown in Fig. 2, it is apparent that porous carbon particle and the roll-in of hydrocarbon black powder close adhesion are in steel wire netlist in Fig. 1 Face, which increase the specific surface areas of cathode material, to increase the materials'use service life.
In the electric Fenton technical system of the embodiment, production roll-in electrode is anode as cathode, Pt electrode, is tested Cheng Caiyong 0.05M Na2SO4Solution is as electrolyte, pH value of solution 7, current density 20mA/cm2, aeration quantity 0.6L/min, such as Shown in Fig. 3, wherein NPC is porous carbon, and CB is carbon black, the H for the electrode that porous carbon and carbon black obtain after implementation 2h2O2Yield is reachable To 545mg/L, and pure carbon black materials H after embodiment 2h2O2Yield reaches 379mg/L.
It is evaluated with the removal of roll-in cathode electricity consumption Fenton made by example pollutant ability, test process addition is fragrant Pause reagent Fe2+Concentration 0.5mM, simulative organic wastewater rhodamine B solution 50mg/L, as shown in figure 4, degradation effect is reached in 15min To percent of decolourization 100%, and pure carbon black materials reach percent of decolourization 98% in 25min.Therefore can obviously judge, which combines more Hole carbon and the steel wire mesh frame carbonaceous cathodes of hydrocarbon black powder production have good electro catalytic activity, illustrate that this method is conducive to the electricity The ability of removal organic polluter is gone in pole in electric Fenton technical system.
Shown in Fig. 5,0.05M Na is used when test2SO4Solution is as electrolyte, pH value of solution 7, current density 28mA/ cm2, aeration quantity 0.6L/min, example electro-catalysis produce hydrogen peroxide test in ten yields of hydrogen peroxide are recycled 667 Between~726mg/L, illustrates that the electrode of this method production has certain stability in electro-catalysis test, use can be extended Service life.
The test condition of Fig. 6 is as above, and example produces in hydrogen peroxide test in electro-catalysis and ten power consumptions are recycled (Electric energy consumption, be abbreviated as EEC) illustrates that this method makes between 53.1~56.7kWh/kg Electrode power consumption tend to a certain range, have opposite stability.
Embodiment 2
A kind of preparation side applied to the porous carbon mixed carbon black roll-in electrode material in electric Fenton technical system of the present invention Method includes the following steps,
Step 1, using 125ml deionized water as solvent, by Zn (NO3)2·6H2O is added thereto with 2-methylimidazole, at this time Zn(NO3)2·6H2The ratio between concentration of O and 2-methylimidazole is 74.4g/L:136.62g/L, for 24 hours by 300rpm magnetic agitation After combination reaction is complete, make cleaning agent using methanol at 9000rpm using supercentrifuge, to remain 2-methylimidazole Completely, centrifugation 20min obtains the presoma of porous carbon for removal;
Step 2, the presoma of porous carbon is dried to 12h at 50 DEG C in a vacuum drying oven;By the presoma after drying It is put into quartz boat, inert gas, such as N are passed through in high temperature process furnances2Under after 1100 DEG C of calcinings are carbonized 6h, obtain black powder Porous carbon, the porous carbon with high-specific surface area, micropore abundant and meso-hole structure, have electro catalytic activity;
Step 3, it is by the commercial blacks powder of 20mg, the ethyl alcohol of 3ml, the porous carbon dust of 8mg and 0.4ml solid content 50% polytetrafluoroethylene (PTFE) emulsion mixing, ultrasonic disperse 30min, mixed system is in uniform state at this time, heats at 80 DEG C It stirs to thick spare for Catalytic Layer;
0.4g commercial blacks powder, the ethyl alcohol of 3ml, the polytetrafluoroethylene (PTFE) emulsion that 0.6ml solid content is 50% are mixed It closes, ultrasonic disperse 5min, mixed system be in uniform state at this time, in 70 DEG C of heating stirrings to thick spare for diffusion layer;
Step 4, divide two sides using twin rollers roll-in two sides to 5cm Catalytic Layer and dispersion layer2Steel wire front and On reverse side, 450 DEG C of annealing 1.5h in Muffle furnace are placed in, are cooled to room temperature i.e. acquisition cathode material.
Embodiment 3
A kind of preparation side applied to the porous carbon mixed carbon black roll-in electrode material in electric Fenton technical system of the present invention Method includes the following steps,
Step 1, using 150ml deionized water as solvent, by Zn (NO3)2·6H2O is added thereto with 2-methylimidazole, at this time Zn(NO3)2·6H2The ratio between concentration of O and 2-methylimidazole is 74.4g/L:159.64g/L, passes through 500rpm magnetic agitation 18h After combination reaction is complete, make cleaning agent using methanol at 10000rpm using supercentrifuge, so that 2-methylimidazole is residual Stay removal completely, centrifugation 12min obtains the presoma of porous carbon;
Step 2, the presoma of porous carbon is dried to 8h at 65 DEG C in a vacuum drying oven;Presoma after drying is put Enter quartz boat, inert gas, such as N are passed through in high temperature process furnances2Under after 1000 DEG C of calcinings are carbonized 7h, it is more to obtain black powder Hole carbon, the porous carbon with high-specific surface area, micropore abundant and meso-hole structure, have electro catalytic activity;
Step 3, by the commercial blacks powder of 30mg, the ethyl alcohol of 2ml, 12mg porous carbon dust and 0.3ml solid content It is mixed for 55% polytetrafluoroethylene (PTFE) emulsion, ultrasonic disperse 20min, mixed system is in uniform state at this time, adds at 70 DEG C Thermal agitation to it is thick it is spare be Catalytic Layer;
0.4g commercial blacks powder, the ethyl alcohol of 2ml, the polytetrafluoroethylene (PTFE) emulsion that 0.5ml solid content is 55% are mixed It closes, ultrasonic disperse 30min, mixed system be in uniform state at this time, in 80 DEG C of heating stirrings to thick spare for diffusion layer;
Step 4, divide two sides using twin rollers roll-in two sides to 5cm Catalytic Layer and dispersion layer2Steel wire front and On reverse side, 400 DEG C of annealing 2h in Muffle furnace are placed in, are cooled to room temperature i.e. acquisition cathode material.

Claims (10)

1. a kind of preparation method of porous carbon mixed carbon black roll-in electrode material, which is characterized in that include the following steps,
Step 1, mixed system ultrasonic disperse porous carbon, carbon black, polytetrafluoroethylene (PTFE) and ethyl alcohol formed is uniform, obtains mixture It is A, wherein the ratio between volume of the quality of porous carbon, the quality of carbon black and ethyl alcohol is (4~12) mg:(10~30) mg:(1~3) Ml stirs mixed system A to roll-in electrode material Catalytic Layer that is thick, being tentatively modified;
The mixed system ultrasonic disperse that carbon black, polytetrafluoroethylene (PTFE) and ethyl alcohol are formed is uniform, mixed system B is obtained, by mixture It is that B is stirred to roll-in electrode material diffusion layer that is thick, being tentatively modified;
Step 2, tentatively modified roll-in electrode material Catalytic Layer, tentatively modified roll-in electrode material diffusion layer are distinguished into roll-in To the upper and lower surfaces of metallic mesh, the roll-in electrode material being tentatively modified;
Step 3, tentatively modified roll-in electrode material is made annealing treatment, is cooled to room temperature to obtain porous carbon mixing charcoal later Inker presses electrode material.
2. a kind of preparation method of porous carbon mixed carbon black roll-in electrode material according to claim 1, which is characterized in that Roll-in electrode material tentatively modified makes annealing treatment 1~2h at 327~450 DEG C in step 3.
3. a kind of preparation method of porous carbon mixed carbon black roll-in electrode material according to claim 1, which is characterized in that Polytetrafluoroethylene (PTFE) described in step 1 uses polytetrafluoroethylene (PTFE) emulsion, and the solid content of polytetrafluoroethylene (PTFE) emulsion is 50%~ The ratio between volume of the quality of carbon black, the volume of polytetrafluoroethylene (PTFE) emulsion and ethyl alcohol is (0.4~0.5) in 60%, mixed system B Mg:(0.4~0.6) ml:(1~3) ml.
4. a kind of preparation method of porous carbon mixed carbon black roll-in electrode material according to claim 1, which is characterized in that The ultrasonic time for the mixed system that porous carbon, carbon black, polytetrafluoroethylene (PTFE) and ethyl alcohol form in step 1 is 5~30min, and carbon black gathers The ultrasonic time of the mixed system of tetrafluoroethene and ethyl alcohol composition is 5~30min.
5. a kind of preparation method of porous carbon mixed carbon black roll-in electrode material according to claim 1, which is characterized in that Mixed system A, mixed system B are stirred to thick respectively under 65~80 DEG C of heating water bath in step 1, tentatively changed Property roll-in electrode material Catalytic Layer and tentatively modified roll-in electrode material diffusion layer.
6. a kind of preparation method of porous carbon mixed carbon black roll-in electrode material according to claim 1, which is characterized in that Porous carbon described in step 1 obtains as follows,
Zn (NO is added in step 1a in ultrapure water or deionized water3)2·6H2After O and 2-methylimidazole react, centrifuge washing is anti- Product is answered to obtain the presoma of porous carbon, wherein Zn (NO3)2·6H2The ratio between concentration of O and 2-methylimidazole is 74.4g/L: (114.03~159.64) g/L;
The presoma of porous carbon is dried in vacuo by step 1b, later under the protection of inert gas at 908~1100 DEG C Calcining 5~7h of carbonization, obtains porous carbon.
7. a kind of preparation method of porous carbon mixed carbon black roll-in electrode material according to claim 6, which is characterized in that The presoma of porous carbon is dried in vacuo 5~12h at 45~65 DEG C in step 1b.
8. a kind of preparation method of the porous carbon mixed carbon black roll-in electrode material as described in claim 1~7 any one obtains The porous carbon mixed carbon black roll-in electrode material arrived.
9. a kind of application of porous carbon mixed carbon black roll-in electrode material as claimed in claim 8, which is characterized in that described Porous carbon mixed carbon black roll-in electrode material is applied in electric Fenton-like system after 2h, H as cathode2O2Yield can reach 545mg/ L。
10. a kind of application of porous carbon mixed carbon black roll-in electrode material as claimed in claim 8, which is characterized in that described Porous carbon mixed carbon black roll-in electrode material, apply when going in removal organic polluter, the percent of decolourization of rhodamine B after 15min Reach 100%.
CN201910683551.5A 2019-07-26 2019-07-26 A kind of porous carbon mixed carbon black roll-in electrode material and its preparation method and application Pending CN110407300A (en)

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CN111186942A (en) * 2020-01-09 2020-05-22 陕西科技大学 Biochar air diffusion electrode and preparation method and application thereof
CN111206259A (en) * 2020-01-14 2020-05-29 武汉科技大学 Preparation method of novel carbon black air diffusion cathode sheet capable of efficiently and stably producing hydrogen peroxide
CN111204851A (en) * 2020-01-17 2020-05-29 陕西科技大学 Graphite felt/porous carbon rolled electrode material, preparation method thereof and application thereof in jet reactor
WO2022056983A1 (en) 2020-09-15 2022-03-24 惠州亿纬锂能股份有限公司 Extrusion head for molding pole piece and molding device comprising same, and molding method and preparation method therefor

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111186942A (en) * 2020-01-09 2020-05-22 陕西科技大学 Biochar air diffusion electrode and preparation method and application thereof
CN111206259A (en) * 2020-01-14 2020-05-29 武汉科技大学 Preparation method of novel carbon black air diffusion cathode sheet capable of efficiently and stably producing hydrogen peroxide
CN111206259B (en) * 2020-01-14 2021-03-19 武汉科技大学 Preparation method of novel carbon black air diffusion cathode sheet capable of efficiently and stably producing hydrogen peroxide
CN111204851A (en) * 2020-01-17 2020-05-29 陕西科技大学 Graphite felt/porous carbon rolled electrode material, preparation method thereof and application thereof in jet reactor
WO2022056983A1 (en) 2020-09-15 2022-03-24 惠州亿纬锂能股份有限公司 Extrusion head for molding pole piece and molding device comprising same, and molding method and preparation method therefor

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Application publication date: 20191105