CN105749717B - A kind of electrochemical treatments SO2Gas-diffusion electrode preparation method - Google Patents
A kind of electrochemical treatments SO2Gas-diffusion electrode preparation method Download PDFInfo
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- CN105749717B CN105749717B CN201610153587.9A CN201610153587A CN105749717B CN 105749717 B CN105749717 B CN 105749717B CN 201610153587 A CN201610153587 A CN 201610153587A CN 105749717 B CN105749717 B CN 105749717B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/50—Sulfur oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/12—Methods and means for introducing reactants
Abstract
A kind of electrochemical treatments SO2Gas-diffusion electrode preparation method, step is as follows：1) powdered conductive carbon black is added in into absolute ethyl alcohol to being totally submerged, adds in ptfe emulsion, water-bath is simultaneously stirred to must spread tunic into being rolled into film after dough；2) gained diffusion tunic is covered on stainless (steel) wire collector, roll-forming takes out for use after being calcined in Muffle furnace；3) tunic must be catalyzed by powdered carbon black and a small amount of carbon nanotubes forming a film according to the method roll-in of step 1)；4) gained catalysis tunic is covered on the another side of stainless (steel) wire collector again, object is made in roll-forming.It is an advantage of the invention that：SO is strengthened by the gas transport duct for increasing electrode2Diffusion mass transfer；It is simple for process, cost of material is low, gas-diffusion electrode high mechanical strength obtained, reusability is good, SO2Transformation efficiency it is high, suitable for SO2The engineering application of electrochemical treatments.
Description
Technical field
The present invention relates to applied chemistry-energy-conserving and emission-cutting technology fields, particularly a kind of electrochemical treatments SO2Gas diffusion
The preparation method of electrode.
Technical background
Quite a few city of winter spring recent years China frequently occurs haze weather, SO2It is the master to form haze
Want one of substance.China is to SO2The norm controlling of discharge is increasingly stringent, and the flue gas desulfurization technique of commercial Application (do by such as wet method
Method semidry method etc.), concentration variation pollution sources greatly small to the discharge exhaust gas volumn such as small-sized thermal power plant and chemical plant, existing should
With of high cost, the problems such as fluctuation of service.The method of electrochemical control gas pollutant is in recent years since its is many good
Performance and be concerned by people, wherein electrochemical method processing SO2It is by SO using electronics as clean inorganic agent2It is converted into
The products such as sulfuric acid, niter cake.
Existing electrochemical treatments technology is mainly by SO2It is first passed through in electrolyte, then applies external electrical field and be oxidized.
This belongs to vapor-liquid two phases interfacial reaction in principle, and limited mass transfer rate and higher energy consumption seriously inhibit electrochemistry oxygen
The efficiency of change；This method is to SO2Concentration also there are certain requirements, the various low concentration sulfur-bearing of industrial complicated component can not be met
The processing requirement of flue gas has fettered electrochemical treatments SO2Further development and commercial Application.
The content of the invention
Present invention is generally directed to above-mentioned there are problem, a kind of electrochemical treatments SO is provided2Gas-diffusion electrode preparation
Method strengthens SO by the gas transport duct for increasing electrode2And O2Diffusion mass transfer.O2By gas diffusion under the action of electricity
Electrode catalyst is reduced to H2O2, the H of generation2O2With can be by SO2It is oxidized to H2SO4, this method is simple for process, cost of material is low,
Gas-diffusion electrode high mechanical strength obtained, reusability is good, SO2Transformation efficiency it is high, suitable for SO2At electrochemistry
The engineering application of reason.
Technical scheme：
A kind of electrochemical treatments SO2Gas-diffusion electrode preparation method, step is as follows：
1) powdered conductive carbon black is added in into absolute ethyl alcohol to being totally submerged and being uniformly dispersed, be stirred by ultrasonic at room temperature
Polytetrafluoroethylene (PTFE) (PTFE) lotion is added dropwise after 20min, continues that 20min is stirred by ultrasonic, by obtained mixed liquor through 80 DEG C of water
It bathes and stirs into its roll-in forming a film after dough, as spread tunic；
2) diffusion tunic obtained by step 1) is covered on stainless (steel) wire collector, diameter 6cm is cut into after roll-forming
Circle, be put into Muffle furnace at 340 DEG C and calcine 20-30min, take out for use.
3) powdered carbon black and a small amount of multi-walled carbon nanotube are added in into absolute ethyl alcohol to being totally submerged and being uniformly dispersed, in room
Polytetrafluoroethylene (PTFE) (PTFE) lotion is added dropwise after the lower ultrasonic agitation 20min of temperature, continues that 20min is stirred by ultrasonic, it is mixed by what is obtained
Liquid is closed through 80 DEG C of water-baths and is stirred into its roll-in forming a film after dough, is as catalyzed tunic；
4) catalysis tunic obtained by step 3) is covered in obtained by step 2) on the another side of stainless (steel) wire collector again, roll-in
Shaping subtracts the circular gas diffusion electrode that corner excess stock can be prepared by diameter 6cm.
The stainless (steel) wire collector be 60 mesh, thickness 0.5mm.
The diffusion layer film thickness is 0.5mm-1mm；The catalysis layer film thickness is 0.5mm-1mm.
The thickness of gained circular gas diffusion electrode is 0.8mm-1mm after roll-forming in the step 4).
The mass percent concentration of the PTFE emulsion is 60%；The mass ratio of PTFE emulsion and conductive black in step 1)
For 5:2, the mass ratio of PTFE emulsion, carbon black and carbon nanotubes is 5 in step 3)：19：1.
Advantages of the present invention and advantageous effect：
The preparation method of the gas-diffusion electrode, by changing SO2Transmission path and mode in electrochemical reaction increase
Strong SO2Diffusion mass transfer, SO2Transformation efficiency handles 1kgSO close to 100%2Only consume energy 1.70kWh；Preparation method technique letter
List, cost of material are low；Gas-diffusion electrode high mechanical strength obtained, reusability are good；SO2Transformation efficiency it is high,
It consumes energy low, non-secondary pollution, suitable for SO2The engineering application of electrochemical treatments.
Description of the drawings
Fig. 1 is gas-diffusion electrode (CB-CNT-GDE) processing SO prepared by the present invention2Principle schematic.
Fig. 2 is gas-diffusion electrode (CB-CNT-GDE) and the electrochemical treatments of common graphite electrode prepared by the present invention
SO2Efficiency and energy consumption comparison figure.
Fig. 3 is gas-diffusion electrode (CB-CNT-GDE) prepared by the present invention and is added without the gas diffusion electricity of carbon nanotubes
Pole (CB-GDE), the electrochemical treatments SO of the additional gas-diffusion electrode (CB-CNT-AC-GDE) for adding in activated carbon2Efficiency and
Energy consumption comparison figure.
Specific embodiment
Embodiment 1：
A kind of electrochemical treatments SO2Gas-diffusion electrode preparation method, step is as follows：
1) 2.0g powdered conductives carbon black is added in into 60mL absolute ethyl alcohols to being totally submerged and being uniformly dispersed, surpassed at room temperature
The ptfe emulsion (density about 1.45g/mL) that 5g mass fractions are 60% is added dropwise after sound stirring 20min, continues to surpass
Sound stirs 20min, and obtained mixed liquor through 80 DEG C of water-baths and is stirred into its roll-in forming a film after dough, obtains diffusion layer
Film；
2) diffusion tunic obtained by step 1) is covered on the stainless (steel) wire collector of 60 mesh, is cut into after roll-forming straight
The circle of footpath 6cm is put into 340 DEG C of calcining 20min in Muffle furnace, takes out for use.
3) the powdered carbon blacks of 1.9g and 0.1g multi-walled carbon nanotubes are added in into 60mL absolute ethyl alcohols to being totally submerged and disperse
Uniformly, polytetrafluoroethylene (PTFE) (PTFE) lotion that 0.5g mass fractions are 60% is added dropwise after 20min is stirred by ultrasonic at room temperature,
Continue that 20min is stirred by ultrasonic, obtained mixed liquor through 80 DEG C of water-baths and is stirred into its roll-in forming a film after dough, is
It is catalyzed tunic；
4) catalysis tunic obtained by step 3) is covered in obtained by step 2) on the another side of stainless (steel) wire collector again, roll-in
Shaping subtracts the circular gas diffusion electrode that corner excess stock can be prepared by diameter 6cm.
To SO2Electrochemical treatments are carried out, as shown in Figure 1, wherein cathode expands principle for the gas of the preparation of the present invention
Electrode is dissipated, anode is platinum electrode (diameter 1mm)；Electrolyte：50mM Na2SO4；Faradaic current：0.1A is constant；Reaction temperature：
25℃；SO2Flow：10mL/min,O2Flow：90mL/min；Reaction time 180min.Fig. 2 gives gas prepared by the present invention
The electrochemical treatments SO of body diffusion electrode (CB-CNT-GDE) and common graphite electrode2Efficiency and energy consumption comparison figure, can by Fig. 2
Know, use the SO of CB-CNT-GDE electrodes2Transformation efficiency (98%) and the SO that common graphite electrode is used in documents and materials2Highest
Transformation efficiency (96.6%) quite, but handles 1kg SO2The energy (1.70kWh) of consumption is than using common graphite electrode
(2.56kWh) has dropped 33.6%.This is because the use of gas-diffusion electrode changes SO2And O2Transmission path and side
Formula enhances SO2Diffusion of the gas into solution is transferred.
Embodiment 2：
A kind of electrochemical treatments SO2Gas-diffusion electrode preparation method, step is as follows：
1) 2.0g powdered conductives carbon black is added in into 60mL absolute ethyl alcohols to being totally submerged and being uniformly dispersed, surpassed at room temperature
The ptfe emulsion (density about 1.45g/mL) that 5g mass fractions are 60% is added dropwise after sound stirring 20min, continues to surpass
Sound stirs 20min, and obtained mixed liquor through 80 DEG C of water-baths and is stirred into its roll-in forming a film after dough, obtains diffusion layer
Film；
2) diffusion tunic obtained by step 1) is covered on the stainless (steel) wire collector of 60 mesh, is cut into after roll-forming straight
The circle of footpath 6cm is put into 340 DEG C of calcining 20min in Muffle furnace, takes out for use.
3) the powdered carbon blacks of 1.9g and 0.1g multi-walled carbon nanotubes are added in into 60mL absolute ethyl alcohols to being totally submerged and disperse
Uniformly, polytetrafluoroethylene (PTFE) (PTFE) lotion that 0.5g mass fractions are 60% is added dropwise after 20min is stirred by ultrasonic at room temperature,
Continue that 20min is stirred by ultrasonic, obtained mixed liquor through 80 DEG C of water-baths and is stirred into its roll-in forming a film after dough, is
It is catalyzed tunic CB-CNT；Catalytic membrane CB is made in the powdered carbon blacks of 2.0g with same method again, by the powdered carbon blacks of 1.61g,
Catalytic membrane CB-CNT-AC is made in 0.1g multi-walled carbon nanotubes and 0.29g powdered active carbons.
4) three kinds of catalysis tunics obtained by step 3) are respectively overlay in the another of stainless (steel) wire collector obtained by three steps 2)
On on one side, roll-forming subtracts the circular gas diffusion electrode (CB-CNT- that corner excess stock can be prepared by three diameter 6cm
GDE, CB-GDE and CB-CNT-AC-GDE).
To SO2Carry out electrochemical treatments, principle as shown in Figure 1, wherein cathode be three kinds of gas-diffusion electrodes, anode
For platinum electrode (diameter 1mm)；Electrolyte：50mM Na2SO4；Faradaic current：0.1A is constant；Reaction temperature：25℃；SO2Stream
Amount：10mL/min,O2Flow：90mL/min；Reaction time 180min.Fig. 3 gives gas-diffusion electrode prepared by the present invention
(CB-CNT-GDE) with being added without the gas-diffusion electrode (CB-GDE) of carbon nanotubes, additionally adding in the gas diffusion electricity of activated carbon
The electrochemical treatments SO of pole (CB-CNT-AC-GDE)2Efficiency and energy consumption comparison figure, from the figure 3, it may be seen that use CB-CNT-GDE electricity
The SO of pole2Transformation efficiency (98%) is higher than CB-GDE electrodes (89.11%) and CB-CNT-GDE electrodes (77.18%), processing
1kg SO2The energy (1.70kWh) of consumption is than using CB-GDE electrodes (1.96kWh) and CB-CNT-GDE electrodes
(2.33kWh) has dropped 13.3% and 27.0% respectively.This is because the addition of carbon nanotubes enhances gas-diffusion electrode
Chemical property and porous structure, and the addition of activated carbon inhibits this change.
In various embodiments above, gained diffusion layer film thickness is 0.5mm-1mm；Gained catalysis layer film thickness is 0.5mm-
1mm；Stainless (steel) wire afflux body thickness is 0.5mm.Due to being needed when tunic will be spread and Catalytic Layer deflector roll is pressed onto on stainless (steel) wire
Certain pressure is wanted, the diffusion tunic and catalysis layer film thickness for being finally compressed on stainless (steel) wire collector both ends are compressed so that
Gained circular gas diffusion electrode integral thickness is 0.8mm-1mm after roll-forming in step 4).
It should be noted that the above-mentioned description to embodiment is understood that for ease of those skilled in the art
With with the application of the invention, therefore, the invention is not restricted to embodiment here, those skilled in the art's announcement according to the present invention is right
It all should be within protection scope of the present invention in the improvement and modification that the present invention makes.
Claims (5)
1. a kind of electrochemical treatments SO2Gas-diffusion electrode preparation method, it is characterised in that step is as follows：
1) powdered conductive carbon black is added in into absolute ethyl alcohol to being totally submerged and being uniformly dispersed, 20min is stirred by ultrasonic at room temperature
After polytetrafluoroethylene (PTFE) (PTFE) lotion is added dropwise, continue be stirred by ultrasonic 20min, obtained mixed liquor through 80 DEG C of water-baths and is stirred
It mixes into its roll-in forming a film after dough, as spreads tunic；
2) diffusion tunic obtained by step 1) is covered on stainless (steel) wire collector, the circle of diameter 6cm is cut into after roll-forming,
It is put into Muffle furnace at 340 DEG C and calcines 20-30min, take out for use.
3) powdered carbon black and a small amount of multi-walled carbon nanotube are added in into absolute ethyl alcohol to being totally submerged and being uniformly dispersed, at room temperature
Polytetrafluoroethylene (PTFE) (PTFE) lotion is added dropwise after ultrasonic agitation 20min, continues that 20min, the mixed liquor that will be obtained is stirred by ultrasonic
It through 80 DEG C of water-baths and stirs into its roll-in forming a film after dough, is as catalyzed tunic；
4) catalysis tunic obtained by step 3) is covered in obtained by step 2) on the another side of stainless (steel) wire collector again, roll-forming
Subtract the circular gas diffusion electrode that corner excess stock can be prepared by diameter 6cm.
2. electrochemical treatments SO according to claim 12Gas-diffusion electrode preparation method, it is characterised in that：It is described not
Steel mesh collector become rusty for 60 mesh, thickness 0.5mm.
3. electrochemical treatments SO according to claim 12Gas-diffusion electrode preparation method, it is characterised in that：The expansion
It is 0.5mm-1mm to dissipate layer film thickness；The catalysis layer film thickness is 0.5mm-1mm.
4. electrochemical treatments SO according to claim 12Gas-diffusion electrode preparation method, it is characterised in that：The step
It is rapid 4) in after roll-forming the thickness of gained circular gas diffusion electrode be 0.8mm-1mm.
5. electrochemical treatments SO according to claim 12Gas-diffusion electrode preparation method, it is characterised in that：It is described
The mass percent concentration of PTFE emulsion is 60%；The mass ratio of PTFE emulsion and conductive black is 5 in step 1):2, step 3)
The mass ratio of middle PTFE emulsion, carbon black and carbon nanotubes is 5:19:1.
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| CN108325350A (en) * | 2018-01-24 | 2018-07-27 | 河海大学 | A kind of flow reactor and its device and method of electrochemical degradation volatile organic contaminant |
| CN108842162A (en) * | 2018-06-15 | 2018-11-20 | 重庆大学 | For electrochemical reduction CO2SnO2Nanometer sheet gas-diffusion electrode and method |
| CN108866569B (en) * | 2018-07-03 | 2020-07-03 | 青岛理工大学 | Preparation method of novel polytetrafluoroethylene thermal modification gas diffusion electrode |
| 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 |
| CN112599790A (en) * | 2020-12-14 | 2021-04-02 | 天津大学仁爱学院 | Cold pressing preparation method of air electrode |
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| CN102655235A (en) * | 2012-03-09 | 2012-09-05 | 南开大学 | Microbial fuel cell air cathode and preparation method thereof |
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