CN103741164A - Preparation method of gas diffusion electrode for producing formic acid by electrochemical reduction of CO2 - Google Patents
Preparation method of gas diffusion electrode for producing formic acid by electrochemical reduction of CO2 Download PDFInfo
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- CN103741164A CN103741164A CN201410003643.1A CN201410003643A CN103741164A CN 103741164 A CN103741164 A CN 103741164A CN 201410003643 A CN201410003643 A CN 201410003643A CN 103741164 A CN103741164 A CN 103741164A
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Abstract
The invention relates to a preparation method of a gas diffusion electrode for producing formic acid by electrochemical reduction of CO2. The preparation method comprises the following steps: 1) adding anhydrous ethanol into powdery conductive carbon black till the powdery conductive carbon black is completely immersed, adding a polytetrafluoroethylene emulsion, performing reaction in a water bath, stirring till the formation of a lump, and then pressing by a roller to form a film, namely a diffusion layer film; 2) deoiling, acid-washing, tinning and drying a copper net to obtain a tinned copper net current collector; and 3) covering the diffusion layer film on the tinned copper net current collector, pressing by the roller, then cutting for formation, placing into a muffle furnace and calcining at the temperature of 3400 DEG C for 20-30min to prepare a target object. The preparation method provided by the invention has the advantages that according to the preparation method of the gas diffusion electrode, CO2 diffusion and mass transfer are strengthened by changing a CO2 transmission path and way of electrochemical reduction reaction of the CO2; and the preparation method has the advantages of simple process and low cost of raw materials, the prepared gas diffusion electrode has high mechanical strength, the electrochemical reduction efficiency of the CO2 is high, and the preparation method is suitable for engineering applications of electrochemical reduction of the CO2.
Description
Technical field
The present invention relates to applied chemistry-energy-conserving and emission-cutting technology field, particularly a kind of electrochemical reduction CO
2the preparation method of the gas diffusion electrode of formic acid processed.
Background technology
Present stage, CO in atmosphere
2caused Greenhouse effect have become one of environmental issue of being concerned about most in the whole world.In order to reduce CO
2content, by multiple technologies means by CO
2recycling is effective means the most.In various treatment processs, electrochemical reducing is because consume energy still less, can under suitable temperature and atmospheric pressure, react, in reaction process, can realize and having broad application prospects to the selectivity of product is synthetic by control electrode and reaction conditions.
CO
2electrochemical reduction has multi-products, and as carbon monoxide, formic acid, formaldehyde, methyl alcohol, methane etc., reaction equation is suc as formula (1)-(5):
CO
2+ 2H
++2e→CO + H
2O
E = 0.52 V (1)
CO
2 +2H
++2e→HCOOH
E = 0.61 V (2)
CO
2 +4H
++4e→HCHO+H
2O
E = 0.48V (3)
CO
2+6H
++6e→CH
3OH+H
2O
E = 0.38 V (4)
CO
2 + 8H
++8e→CH
4 +2H
2O
E = 0.24 V (5)。
Wherein formic acid is a kind of basic chemical raw materials, can resolve into CO
2and water, not producing pollution, the application market in the industries such as process hides, medicine and printing and dyeing has a extensive future, and consumption rises just year by year.
Water, as natural " proton source " and good electroconductibility, is electrochemical reduction CO
2emphasis medium.CO in the aqueous solution
2the interference that subject matter is proton that electrochemical reduction runs into, makes evolving hydrogen reaction and CO
2reduce and deposit generation, both ratios are directly determining the formation of product.In order to suppress the generation of evolving hydrogen reaction, electrode need be selected the metal with high overpotential of hydrogen evolution, and as Pb, Hg, Sn, In etc., wherein Sn toxicity for other metal is low and cost is low, is just being subject to more and more researchists' attention.And research show, in the aqueous solution of 101.325kPa, CO
2under the katalysis of Sn, can preferentially be reduced into formic acid.Yet, CO
2solubleness in water-soluble electrolyte very low (0.33mol/L, mark state), limited rate of mass transfer and concentration polarization phenomenon severe inhibition the efficiency of electrochemical reduction, fettered electrochemical reduction CO
2produce further developing and applying of formic acid.
Summary of the invention
The present invention, mainly for above-mentioned existing problems, provides a kind of electrochemical reduction CO
2the preparation method of the gas diffusion electrode of formic acid processed, this preparation method's technique is simple, raw materials cost is low, and the gas diffusion electrode physical strength making is high, CO
2electroreduction efficiency high, be suitable for CO
2the through engineering approaches application of electrochemical reduction.
Technical scheme of the present invention:
A kind of electrochemical reduction CO
2the preparation method of the gas diffusion electrode of formic acid processed, step is as follows:
1) Powdered graphitized carbon black added to dehydrated alcohol to complete submergence and be uniformly dispersed, at room temperature after ultrasonic agitation 20min, dropwise adding polytetrafluoroethylene (PTFE) emulsion, continuing ultrasonic agitation 20min, by the mixed solution obtaining through 80
oc water-bath and be stirred to into dough after by its roll-in film forming, be diffusion tunic;
2) by 60-80 object copper mesh through oil removing, pickling, zinc-plated, dry after, obtain zinc-plated copper mesh collector;
3) diffusion tunic is covered on zinc-plated copper mesh collector, after roll-forming, cut into the circle of diameter 4cm, put into retort furnace 340
0c calcines 20-30min, can make CO
2electrochemical reduction gas diffusion electrode.
The mass percent concentration of described PTFE emulsion is that the mass ratio of 60%, PTFE emulsion and graphitized carbon black is 3-4:1-2.
The degreaser of described copper mesh oil removing is acetone, and pickle solution is that mass percent concentration is 10% dilute hydrochloric acid.
Described tin plating method adopts electroless plating or plating, adopt the technique of electroless plating to be: chemical tin plating liquor is the mixed solution of stannous sulfate, sulfuric acid and thiocarbamide, stannous sulfate, sulfuric acid and the thiocarbamide concentration in mixed solution is respectively 0.2 mol/L, 0.22 mol/L and 0.6 mol/L, and plating temperature is 40-50
oc, plating time is 3min; Employing electroplating technique is: under constant potential, adopt three-electrode system to electroplate, take the zinc-plated current potential of Ag/AgCl during as reference electrode as-0.85V, plating tin liquor is the mixed solution of tin protochloride, Trisodium Citrate and hydrochloric acid, tin protochloride, Trisodium Citrate and the hydrochloric acid concentration in mixed solution is respectively 0.036 mol/L, 0.05 mol/L and 10-15mL/L, and electroplating time is 5min.
Advantage of the present invention and beneficial effect:
The preparation method of this gas diffusion electrode, by changing CO
2electrochemical reducting reaction CO
2transmission route and mode, strengthening CO
2diffusion mass transfer, CO
2the faradic efficiency of electrochemical reduction has improved approximately 30% without diffusion layer electrode; This preparation method's technique is simple, raw materials cost is low, and the gas diffusion electrode physical strength making is high, CO
2electroreduction efficiency high, be suitable for CO
2the through engineering approaches application of electrochemical reduction.
Accompanying drawing explanation
Fig. 1 is the Sn/Cu-GDL electrode prepared of electroless plating method and the electrochemical reduction CO of Sn/Cu electrode
2the faradic efficiency comparison diagram of preparing formic acid, in figure: ordinate zou FE%, represents CO
2electrochemical reduction generates the faradic efficiency % of formic acid; X-coordinate represents CO
2the electrode that electrochemical reducting reaction is used, wherein Sn/Cu-GDL is the electrode of patented invention, Sn/Cu is the electrode without diffusion layer GDL.
Fig. 2 is the Sn/Cu-GDL electrode prepared of electrochemical plating and the electrochemical reduction CO of Sn/Cu electrode
2the faradic efficiency comparison diagram of preparing formic acid, in figure, explanation is identical with Fig. 1.
Fig. 3 is the CO of Sn/Cu-GDL electrode
2electrochemical reduction is prepared the principle schematic of formic acid.
Embodiment
Embodiment 1:
A kind of electrochemical reduction CO
2the preparation method of the gas diffusion electrode of formic acid processed, step is as follows:
1) the Powdered graphitized carbon black of 0.9g added to 80mL dehydrated alcohol to complete submergence and be uniformly dispersed, at room temperature after ultrasonic agitation 20min, dropwise add 2.1g, 60wt% polytetrafluoroethylene (PTFE) emulsion, continue ultrasonic agitation 20min, by the mixed solution obtaining through 80
oc water-bath and be stirred to into dough after by its roll-in film forming, obtain spreading tunic;
2) by 60-80 object copper mesh after the dilute hydrochloric acid pickling of oil removing, washing, 10wt%, washing pre-treatment, put into chemical tin plating liquor, chemical tin plating liquor is the mixed solution of stannous sulfate, sulfuric acid and thiocarbamide, stannous sulfate, sulfuric acid and the thiocarbamide concentration in mixed solution is respectively 0.2mol/L, 0.22 mol/L and 0.6 mol/L, in 40-50
oat C temperature, after reaction 3min, make zinc-plated copper mesh collector;
3) diffusion tunic is covered on zinc-plated copper mesh collector, after roll-forming, cut into the circle of diameter 4cm, put into retort furnace 340
oc calcines 20-30min, obtains electrochemical reduction CO
2the gas diffusion electrode of formic acid processed, is designated as Sn/Cu-GDL.
Fig. 3 is the CO of Sn/Cu-GDL electrode
2electrochemical reduction is prepared the principle schematic of formic acid.On the basis that Sn/Cu-GDL electrode is Sn/Cu electrode at zinc-plated copper mesh collector, increased diffusion layer GDL, CO
2by gas diffusion layers GDL, be transferred on zinc-plated copper mesh collector electrochemical reducting reaction occurs.Owing to having increased diffusion layer GDL, changed CO
2path and the mode of transmission, strengthened CO
2gas diffusion, can effectively solve CO
2solubleness in water-soluble electrolyte is low, and limited rate of mass transfer and concentration polarization phenomenon suppress CO
2the problem of electrochemical reduction efficiency.
Adopt three-electrode system to carry out CO to the gas diffusion electrode of preparation
2electrochemical reducting reaction is wherein Pt electrode (1cm to electrode
2), reference electrode is Ag/AgCl, working electrode is Sn/Cu-GDL(7cm
2), electrolytic solution is 0.5 mol/L KHCO
3solution, electrolytic potential is-1.8V that temperature of reaction is 25
oc, CO
2flow is 30mL/min, reaction times 30min.Controlled trial working electrode is the zinc-plated copper mesh without diffusion layer, is designated as Sn/Cu(7cm
2), other experiment condition is identical.
Fig. 1 is the Sn/Cu-GDL electrode prepared of electroless plating method and the electrochemical reduction CO of Sn/Cu electrode
2the faradic efficiency comparison diagram of preparing formic acid.As shown in Figure 1, use the CO of Sn/Cu-GDL electrode
2electroreduction faradic efficiency (78.5%) is used Sn/Cu electrode (63.2%) to improve 24.2%.Owing to having increased diffusion layer GDL in Sn/Cu-GDL electrode, changed CO
2transmission route and mode, strengthened CO
2gas, to the diffusion transmission in solution, has suppressed the generation of hydrogen, shows significant advantage.
Embodiment 2:
A kind of electrochemical reduction CO
2the preparation method of the gas diffusion electrode of formic acid processed, step is as follows:
1) the Powdered graphitized carbon black of 0.9g added to 80mL dehydrated alcohol to complete submergence and be uniformly dispersed, at room temperature after ultrasonic agitation 20min, dropwise add 2.1g, 60wt% polytetrafluoroethylene (PTFE) emulsion, continue ultrasonic agitation 20min, by the mixed solution obtaining through 80
oc water-bath and be stirred to into dough after by its roll-in film forming, obtain spreading tunic;
2) by 60-80 object copper mesh after the dilute hydrochloric acid pickling of oil removing, washing, 10wt%, washing pre-treatment, put into and electroplate tin liquor, plating tin liquor is the mixed solution of tin protochloride, Trisodium Citrate and hydrochloric acid, tin protochloride, Trisodium Citrate and the hydrochloric acid concentration in mixed solution is respectively 0.036 mol/L, 0.05 mol/L and 10mL/L, under constant potential, adopt three-electrode system to electroplate, take the zinc-plated current potential of Ag/AgCl during as reference electrode as-0.85V, electroplating time is 5min, makes zinc-plated copper mesh collector;
3) diffusion tunic is covered on zinc-plated copper mesh collector, after roll-forming, cut into the circle of diameter 4cm, put into retort furnace 340
oc calcines 20-30min, obtains electrochemical reduction CO
2the gas diffusion electrode of formic acid processed, is designated as Sn/Cu-GDL.
Adopt three-electrode system to carry out CO to the gas diffusion electrode of preparation
2electrochemical reduction is wherein Pt electrode (1cm to electrode
2), reference electrode is Ag/AgCl, working electrode is Sn/Cu-GDL, (7cm
2); Electrolytic solution: 0.5 mol/L KHCO
3solution; Electrolytic potential :-1.8V; Temperature of reaction: 25
oc; CO
2flow: 30mL/min, reaction times 30min.Controlled trial working electrode is the zinc-plated copper mesh without diffusion layer, is designated as Sn/Cu(7cm
2), other experiment condition is identical.
Fig. 2 is the Sn/Cu-GDL electrode prepared of electrochemical plating and the electrochemical reduction CO of Sn/Cu electrode
2the faradic efficiency comparison diagram of preparing formic acid.As shown in Figure 2, use the CO of Sn/Cu-GDL electrode
2electroreduction faradic efficiency (82.95%) is used Sn/Cu electrode (63.72%) to improve 30.2%.Owing to having increased diffusion layer GDL in Sn/Cu-GDL electrode, changed CO
2transmission route and mode, strengthened CO
2gas, to the diffusion transmission in solution, has suppressed the generation of hydrogen, shows significant advantage.
Claims (4)
1. an electrochemical reduction CO
2the preparation method of the gas diffusion electrode of formic acid processed, is characterized in that step is as follows:
1) Powdered graphitized carbon black added to dehydrated alcohol to complete submergence and be uniformly dispersed, at room temperature after ultrasonic agitation 20min, dropwise adding polytetrafluoroethylene (PTFE) emulsion, continuing ultrasonic agitation 20min, by the mixed solution obtaining through 80
oc water-bath and be stirred to into dough after by its roll-in film forming, be diffusion tunic;
2) by 60-80 object copper mesh through oil removing, pickling, zinc-plated, dry after, obtain zinc-plated copper mesh collector;
3) diffusion tunic is covered on zinc-plated copper mesh collector, after roll-forming, cut into the circle of diameter 4cm, put into retort furnace 340
0c calcines 20-30min, can make CO
2electrochemical reduction gas diffusion electrode.
2. electrochemical reduction CO according to claim 1
2the preparation method of the gas diffusion electrode of formic acid processed, is characterized in that: the mass percent concentration of described PTFE emulsion is that the mass ratio of 60%, PTFE emulsion and graphitized carbon black is 3-4:1-2.
3. electrochemical reduction CO according to claim 1
2the preparation method of the gas diffusion electrode of formic acid processed, is characterized in that: the degreaser of described copper mesh oil removing is acetone, and pickle solution is that mass percent concentration is 10% dilute hydrochloric acid.
4. electrochemical reduction CO according to claim 1
2the preparation method of the gas diffusion electrode of formic acid processed, it is characterized in that: described tin plating method adopts electroless plating or plating, adopt the technique of electroless plating to be: chemical tin plating liquor is the mixed solution of stannous sulfate, sulfuric acid and thiocarbamide, stannous sulfate, sulfuric acid and the thiocarbamide concentration in mixed solution is respectively 0.2mol/L, 0.22 mol/L and 0.6 mol/L, and plating temperature is 40-50
oc, plating time is 3min; Employing electroplating technique is: under constant potential, adopt three-electrode system to electroplate, take the zinc-plated current potential of Ag/AgCl during as reference electrode as-0.85V, plating tin liquor is the mixed solution of tin protochloride, Trisodium Citrate and hydrochloric acid, tin protochloride, Trisodium Citrate and the hydrochloric acid concentration in mixed solution is respectively 0.036 mol/L, 0.05 mol/L and 10-15mL/L, and electroplating time is 5min.
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| CN104328046A (en) * | 2014-09-28 | 2015-02-04 | 南京工业大学 | Apparatus and method for producing acetic acid by reducing carbon dioxide through microbial-electrochemical system |
| CN104600328A (en) * | 2015-01-20 | 2015-05-06 | 南开大学 | Method for preparing gas diffusion electrode for promoting proton conduction and gas transmission and producing formic acid through electrochemical reduction of CO2 |
| CN104846397A (en) * | 2015-04-21 | 2015-08-19 | 盐城工学院 | Electrode for electrochemical reduction of CO2 and preparation of formic acid and preparation method and application thereof |
| CN105304910A (en) * | 2014-07-01 | 2016-02-03 | 中国科学院大连化学物理研究所 | Electrode of hydrocarbon produced by carbon dioxide through electrochemical reduction and preparation and application of electrode |
| CN105322185A (en) * | 2014-07-29 | 2016-02-10 | 中国科学院大连化学物理研究所 | Gas diffusion electrode for carbon dioxide electrochemical reduction reaction and preparation method for gas diffusion electrode |
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| CN104846397B (en) * | 2015-04-21 | 2018-08-31 | 盐城工学院 | One kind being used for electrochemical reduction CO2The electrode and its preparation method and application of formic acid processed |
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