CN114198850B - Gas-solid phase electrocatalytic electrode and preparation method and application thereof - Google Patents
Gas-solid phase electrocatalytic electrode and preparation method and application thereof Download PDFInfo
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24F—AIR-CONDITIONING; AIR-HUMIDIFICATION; VENTILATION; USE OF AIR CURRENTS FOR SCREENING
- F24F8/00—Treatment, e.g. purification, of air supplied to human living or working spaces otherwise than by heating, cooling, humidifying or drying
- F24F8/10—Treatment, e.g. purification, of air supplied to human living or working spaces otherwise than by heating, cooling, humidifying or drying by separation, e.g. by filtering
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- F24F8/167—Treatment, e.g. purification, of air supplied to human living or working spaces otherwise than by heating, cooling, humidifying or drying by separation, e.g. by filtering by chemical means using catalytic reactions
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- F24F8/00—Treatment, e.g. purification, of air supplied to human living or working spaces otherwise than by heating, cooling, humidifying or drying
- F24F8/10—Treatment, e.g. purification, of air supplied to human living or working spaces otherwise than by heating, cooling, humidifying or drying by separation, e.g. by filtering
- F24F8/192—Treatment, e.g. purification, of air supplied to human living or working spaces otherwise than by heating, cooling, humidifying or drying by separation, e.g. by filtering by electrical means, e.g. by applying electrostatic fields or high voltages
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Abstract
The invention provides a gas-solid phase electrocatalytic electrode, a preparation method and application thereof. The gas-solid phase electrocatalytic electrode comprises a conductive substrate, an anodic oxidation active layer and a hydrophilic solid electrolyte layer which are sequentially stacked. The gas-solid phase electrocatalytic electrode provided by the invention is modified by the hydrophilic solid electrolyte, so that the electron transfer rate in the gas-solid phase reaction is accelerated, the water activation capability is obviously improved, good catalytic oxidation capability is shown for indoor pollutants, and the preparation method is simple, and the operation is simple and easy to realize automation.
Description
Technical Field
The invention belongs to the technical field of electrocatalysis, and relates to a gas-solid phase electrocatalysis electrode, a preparation method and application thereof.
Background
The life of people spends 80% of their lives indoors, and as the process of urban treatment increases, the indoor air quality requirements of people increase continuously, and new requirements are put forward for indoor air purification technology. Indoor pollutants such as formaldehyde, VOCs and the like have strong irritation and toxicity, have three effects and have great harm to human health. The supported noble metal catalyst can effectively degrade formaldehyde at room temperature, but has high price and large actual large-scale application difficulty. Benzene series and the like cannot be degraded at room temperature because of stable structure. There is a need to develop catalysts that can degrade indoor contaminants at room temperature with a broad spectrum. The electrocatalytic oxidation method is a very promising technology because of the characteristics of high treatment efficiency, simple and convenient operation, easy automation realization and the like.
CN100450610C discloses a supported manganese cerium oxide catalyst, whose active components are silver, gold or platinum; the molar ratio of Mn/Ce in the manganese-cerium composite oxide is 1.0, and the loading amount of the active components is 0.1-5% of the weight of the manganese-cerium oxide. The preparation method mainly comprises the following steps: suspending manganese-cerium composite oxide powder in an aqueous solution, adding a solution of soluble silver, gold or platinum under stirring, and preparing manganese-cerium oxide powder suspension of silver, gold or platinum; adding KOH or K to the floating liquid in the step d respectively 2 CO 3 Solution, the pH value is equal to 9-10, and the solution is precipitated and filtered; and d, drying the precipitate obtained in the step e at 80-120 ℃ and roasting for 2-10 hours at 300-500 ℃ to obtain the target product.
CN101380574a discloses a high selectivity catalyst for catalyzing the complete oxidation of low concentration formaldehyde at room temperature. The catalyst can completely catalyze and convert formaldehyde into carbon dioxide and water under the room temperature condition, and the formaldehyde conversion rate is kept at 100% in a quite long time range, and complicated auxiliary equipment such as a light source, a heating furnace and the like and external conditions are not needed. The catalyst consists of porous inorganic oxide carrier, noble metal component and assistant component. The porous inorganic oxide carrier is one or more of cerium oxide, zirconium dioxide, titanium dioxide, aluminum oxide, tin dioxide, silicon dioxide, lanthanum oxide, magnesium oxide and zinc oxide or a compound oxide thereof, zeolite, sepiolite and porous carbon material; the noble metal component of the catalyst is at least one of platinum, rhodium, palladium, gold and silver, and the auxiliary component is at least one of alkali metal lithium, sodium, potassium, rubidium and cesium.
Both of these documents, although they can completely oxidize formaldehyde to CO at room temperature 2 And H 2 O, but the higher efficiency is concentrated on the noble metal platinum catalyst, and the atmosphere of high humidity in the room is not considered, and the noble metal catalyst is loaded with high price and difficult to be applied in a practical large scale.
Therefore, how to provide a catalyst capable of effectively removing indoor pollutants at room temperature is a technical problem to be solved.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a gas-solid phase electrocatalytic electrode, and a preparation method and application thereof. The gas-solid phase electrocatalytic electrode provided by the invention is modified by the hydrophilic solid electrolyte, so that the electron transfer rate in the gas-solid phase reaction is accelerated, the water activation capability is obviously improved, good catalytic oxidation capability is shown for indoor pollutants, and the preparation method is simple, and the operation is simple and easy to realize automation.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a gas-solid electrocatalytic electrode comprising a conductive substrate, an anodic oxidation active layer and a hydrophilic solid electrolyte layer, laminated in this order.
The gas-solid phase electrocatalytic electrode provided by the invention is modified by the hydrophilic solid electrolyte, so that the electron transfer rate in the gas-solid phase reaction is accelerated, the water activation capability is obviously improved, and good catalytic oxidation capability is shown for indoor pollutants.
The hydrophilic solid electrolyte in the invention is a solid electrolyte containing hydrophilic groups.
The gas-solid phase electrocatalytic electrode provided by the invention is suitable for gas-solid phase reaction of double electrodes.
The gas-solid phase electrocatalytic electrode provided by the invention cannot fully activate active sites and cannot form a conductive network if a solid electrolyte layer containing no hydrophilic group is used.
Preferably, the anodic oxidation active layer comprises an oxidation active oxide.
Preferably, the oxidation-active oxide comprises SnO 2 And/or PbO 2 。
Preferably, the loading amount of the oxidation active oxide is 10-100 mg/cm 2 For example 10mg/cm 2 、20mg/cm 2 、30mg/cm 2 、40mg/cm 2 、50mg/cm 2 、60mg/cm 2 、70mg/cm 2 、80mg/cm 2 、90mg/cm 2 Or 100mg/cm 2 Etc.
The loading provided by the invention is the mass distribution of the substances in the active layer on the conductive substrate.
Preferably, the conductive substrate comprises any one or a combination of at least two of metal foam, metal mesh or carbon paper.
Preferably, the hydrophilic group solid electrolyte layer has a thickness of 2 to 500 μm, for example, 2 μm, 10 μm, 20 μm, 50 μm, 100 μm, 130 μm, 150 μm, 180 μm, 200 μm, 230 μm, 250 μm, 280 μm, 300 μm, 330 μm, 350 μm, 380 μm, 400 μm, 430 μm, 450 μm, 480 μm, 500 μm, or the like.
In the invention, the thickness of the hydrophilic solid electrolyte layer is too small, which is unfavorable for the formation of a conductive network and the full activation of active sites, and the thickness is too large, which increases the conductive resistance of the system too much.
In a second aspect, the present invention provides a method for preparing a gas-solid phase electrocatalytic electrode according to the first aspect, comprising the steps of:
preparing a catalyst precursor with an anodic oxidation active layer arranged on the surface of a conductive substrate, and then coating hydrophilic group solid electrolyte solution on the surface of the anodic oxidation active layer to obtain the catalyst.
The preparation method provided by the invention is simple to operate, and the gas-solid phase catalyst electrode with higher catalytic oxidation activity can be obtained by simple coating without adopting a complex technical scheme.
Preferably, the concentration of the hydrophilic solid electrolyte solution is 1 to 50%, for example, 1%, 5%, 8%, 10%, 13%, 15%, 18%, 20%, 23%, 25%, 28%, 30%, 33%, 35%, 40%, 45% or 50%, etc., preferably 5 to 35%.
In the invention, the concentration of the hydrophilic solid electrolyte solution is less than 1%, which is unfavorable for the enrichment of the solid electrolyte on the surface of the active material, and if the concentration is more than 50%, the conductive resistance is increased; when the concentration is further adjusted to be within the range of 5 to 35 percent, the hydrophilic solid electrolyte has the advantage of ensuring proper enrichment of proper amount of hydrophilic solid electrolyte on the active surface.
Preferably, the hydrophilic solid electrolyte solution is used in an amount of 0.1 to 1mL/cm 2 For example 0.1mL/cm 2 、0.2mL/cm 2 、0.3mL/cm 2 、0.4mL/cm 2 、0.5mL/cm 2 、0.6mL/cm 2 、0.7mL/cm 2 、0.8mL/cm 2 、0.9mL/cm 2 Or 1mL/cm 2 Etc.
Preferably, the hydrophilic solid electrolyte comprises any one or a combination of at least two of polystyrene solid electrolyte, perfluorosulfonic acid solid electrolyte, polyacrylamide hydrochloride, polyacrylamide or polyamide epichlorohydrin, preferably perfluorosulfonic acid solid electrolyte and/or polystyrene sulfonic acid
Preferably, the preparation method of the catalyst precursor for arranging the anodic oxidation active layer on the surface of the conductive substrate comprises the following steps:
the oxidation active oxide is arranged on the surface of the conductive substrate by adopting a coating or electrodeposition method.
As a preferred technical scheme, the preparation method comprises the following steps:
setting oxidation active oxide on the surface of conductive substrate by coating or electrodeposition method, drying to obtain catalyst precursor with anode oxidation active layer on the surface of conductive substrate, and mixing hydrophilic group solid electrolyte solution with mass concentration of 5-35% with concentration of 0.1-1 mL/cm 2 The catalyst is obtained by coating the surface of the anodic oxidation active layer and drying.
In a third aspect, the present invention also provides the use of a gas-solid phase electrocatalytic electrode according to the first aspect for electrochemical catalytic oxidation of indoor pollutants.
The common gas-solid phase electrocatalytic electrode has poor electrocatalytic performance, and can generate 15 percent CO when being applied to electrocatalytic degradation of benzene series 2 The gas-solid phase electrocatalytic electrode provided by the invention can not degrade indoor pollutants such as formaldehyde. The activity is obviously increased, and the catalyst can degrade various indoor pollutants such as toluene, formaldehyde and the like, and has broad spectrum
Preferably, the indoor pollutants comprise formaldehyde, benzene series and other various indoor pollutants
Compared with the prior art, the invention has the following beneficial effects:
the gas-solid phase electrocatalytic electrode provided by the invention is modified by the hydrophilic solid electrolyte, the electron transfer rate in the gas-solid phase reaction is accelerated, the activation capability of water is obviously improved, good catalytic oxidation capability is shown for indoor pollutants, the preparation method is simple, the operation is simple and easy to realize automation, the mass concentration of the hydrophilic solid electrolyte is in the range of 5-35%, when the gas-solid phase electrocatalytic electrode provided by the invention is used for catalyzing and oxidizing toluene, the toluene removal rate is over 70% and the CO is realized after degradation for 1h 2 The conversion rate is more than 90 percent; when the catalyst is used for catalyzing formaldehyde, the catalyst is degraded for 1h, so that the formaldehyde removal rate is over 85 percent, and CO is realized 2 The conversion rate is more than 95%.
Detailed Description
The technical scheme of the invention is further described by the following specific examples. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a gas-solid phase electrocatalytic electrode, which comprises a conductive substrate, an anodic oxidation active layer and a hydrophilic solid electrolyte layer which are sequentially stacked;
the conductive substrate is foam Ti, and the anodic oxidation active layer is SnO 2 Layer of SnO 2 SnO in layer 2 Is 45mg/cm 2 The hydrophilic solid electrolyte layer was perfluorosulfonic acid solid electrolyte (Nafion), and the thickness of the hydrophilic solid electrolyte layer was 40 μm.
The preparation method of the gas-solid phase electrocatalytic electrode comprises the following steps:
SnO is prepared 2 Coating the slurry on the surface of a conductive substrate, drying to obtain a catalyst precursor with an anodic oxidation active layer on the surface of the conductive substrate, and then adding a hydrophilic group solid electrolyte solution with the mass concentration of 10% to 0.5mL/cm 2 The catalyst is obtained by coating the surface of the anodic oxidation active layer and drying.
Example 2
The embodiment provides a gas-solid phase electrocatalytic electrode, which comprises a conductive substrate, an anodic oxidation active layer and a hydrophilic solid electrolyte layer which are sequentially stacked;
the conductive substrate is foamed Ni, and the anodic oxidation active layer is PbO 2 Layer, pbO 2 PbO in layer 2 Is 10mg/cm 2 The hydrophilic solid electrolyte layer was Nafion, and the thickness of the hydrophilic solid electrolyte layer was 150 μm.
The preparation method of the gas-solid phase electrocatalytic electrode comprises the following steps:
PbO is prepared 2 The catalyst precursor with the anode oxidation active layer arranged on the surface of the conductive substrate is obtained after drying in an electrodeposition mode, and then hydrophilic group solid electrolyte solution with the mass concentration of 5% is added in a concentration of 0.1mL/cm 2 The catalyst is obtained by coating the surface of the anodic oxidation active layer and drying.
Example 3
The embodiment provides a gas-solid phase electrocatalytic electrode, which comprises a conductive substrate, an anodic oxidation active layer and a hydrophilic solid electrolyte layer which are sequentially stacked;
the conductive substrate is carbon paper, and the anodic oxidation active layer is SnO 2 Layer of SnO 2 SnO in layer 2 Is 100mg/cm 2 The hydrophilic solid electrolyte layer is sodium polystyrene sulfonate, and the thickness of the hydrophilic solid electrolyte layer is 50 mu m.
The preparation method of the gas-solid phase electrocatalytic electrode comprises the following steps:
SnO is prepared 2 Coating the slurry on the surface of a conductive substrate, drying to obtain a catalyst precursor with an anodic oxidation active layer on the surface of the conductive substrate, and then adding 1mL/cm hydrophilic group solid electrolyte solution with the mass concentration of 35% 2 The catalyst is obtained by coating the surface of the anodic oxidation active layer and drying.
Example 4
The difference between this example and example 1 is that the mass concentration of the hydrophilic group solid electrolyte solution in this example is 1%.
The remaining preparation methods and parameters were consistent with example 1.
Example 5
The difference between this example and example 1 is that the mass concentration of the hydrophilic group solid electrolyte solution in this example is 50%.
The remaining preparation methods and parameters were consistent with example 1.
Comparative example 1
The difference between this comparative example and example 1 is that the gas-solid phase electrocatalytic electrode provided in this comparative example does not contain a hydrophilic group solid electrolyte layer.
In the preparation method, the catalyst precursor is obtained, namely the gas-solid phase electrocatalytic electrode is obtained.
The remaining preparation methods and parameters were consistent with example 1.
Comparative example 2
The difference between this comparative example and example 1 is that in this comparative example, the solid electrolyte is polyethylene glycol.
The remaining preparation methods and parameters were consistent with example 1.
The gas-solid phase electrocatalytic electrodes provided in examples 1-5 and comparative examples 1-2 were tested for the catalytic oxidation of toluene at room temperature (25 ℃) as follows:
the reaction is carried out in a gas-solid phase electrochemical reaction tank, and the reaction atmosphere circularly flows through the catalyst. The initial atmosphere composition was (40 ppm toluene, 20% O) 2 Relative humidity 100%, total volume of about 1.4L, N 2 To balance the gas, the circulation flow rate was 100 mL/min). The anode was the electrode mentioned in the present invention, the cathode was a commercial Pt/C electrode, and the cell voltage was 3V, and the results are shown in Table 1.
TABLE 1
The reaction is carried out in a gas-solid phase electrochemical reaction tank, and the reaction atmosphere circularly flows through the catalyst. The initial atmosphere composition was (80 ppm formaldehyde, 20% O 2 Relative humidity 100%, total volume of about 1.4L, N 2 To balance the gas, the circulation flow rate was 100 mL/min). The anode was the electrode mentioned in the present invention, the cathode was a commercial Pt/C electrode, and the cell voltage was 3V, and the results are shown in Table 2.
TABLE 2
| Degradation time | Formaldehyde removal Rate (%) | CO 2 Conversion (%) | |
| Example 1 | 1h | 95 | 99 |
| Example 2 | 1h | 85 | 98 |
| Example 3 | 1h | 90 | 95 |
| Example 4 | 1h | 60 | 90 |
| Example 5 | 1h | 80 | 99 |
| Comparative example 1 | 1h | 48 | 80 |
| Comparative example 2 | 1h | 0 | 0 |
The data in tables 1 and 2 are combined to show that:
as is clear from the data of examples 1 and 4 and 5, the mass concentration of the hydrophilic solid electrolyte solution is too small to facilitate activation of the active site, while the mass concentration is too large to cause an increase in resistance and deterioration of activity.
From the data of example 1 and comparative example 1, it is understood that rapid and thorough electrocatalytic oxidation cannot be achieved without modification of the hydrophilic solid electrolyte.
From the data of example 1 and comparative example 2, it is understood that the reaction cannot proceed without the conductive ability in the solid electrolyte.
In conclusion, the gas-solid phase electrocatalytic electrode provided by the invention has the advantages that through modification by the hydrophilic solid electrolyte, the electron transfer rate in the gas-solid phase reaction is accelerated, the water activation capability is obviously improved, good catalytic oxidation capability is shown for indoor pollutants, the preparation method is simple, the operation is simple and easy to realize automation, the mass concentration of the hydrophilic solid electrolyte is in the range of 5-35%, when the gas-solid phase electrocatalytic electrode provided by the invention is used for catalyzing and oxidizing toluene, the toluene removal rate can be above 70% by degrading for 1h, and the CO 2 The conversion rate is more than 90 percent; when the catalyst is used for catalyzing formaldehyde, the catalyst is degraded for 1h, so that the formaldehyde removal rate is over 85 percent, and CO is realized 2 The conversion rate is more than 95%.
The applicant states that the detailed method of the present invention is illustrated by the above examples, but the present invention is not limited to the detailed method described above, i.e. it does not mean that the present invention must be practiced in dependence upon the detailed method described above. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (11)
1. The gas-solid phase electrocatalytic electrode is characterized by comprising a conductive substrate, an anodic oxidation active layer and a hydrophilic solid electrolyte layer which are sequentially stacked; the anodic oxidation active layer comprises an oxidation active oxide; the thickness of the hydrophilic group solid electrolyte layer is 2-500 mu m; the gas-solid phase electrocatalytic electrode is suitable for gas-solid phase reaction of double electrodes;
the gas-solid phase electrocatalytic electrode is prepared by a preparation method comprising the following steps of:
preparing a catalyst precursor of which the surface is provided with an anodic oxidation active layer, and then coating hydrophilic group solid electrolyte solution on the surface of the anodic oxidation active layer to obtain the catalyst; the concentration of the hydrophilic group solid electrolyte solution is 1-50%.
2. The gas-solid electrocatalytic electrode of claim 1, wherein the oxidatively active oxide comprises SnO 2 And/or PbO 2 。
3. The gas-solid phase electrocatalytic electrode of claim 1, wherein the loading of the oxidatively active oxide is 10-100 mg/cm 2 。
4. The gas-solid electrocatalytic electrode of claim 1, wherein the conductive substrate comprises any one or a combination of at least two of metal foam, metal mesh or carbon paper.
5. A method for producing a gas-solid phase electrocatalytic electrode according to any one of claims 1-4, wherein said method comprises the steps of:
preparing a catalyst precursor of which the surface is provided with an anodic oxidation active layer, and then coating hydrophilic group solid electrolyte solution on the surface of the anodic oxidation active layer to obtain the catalyst; the concentration of the hydrophilic group solid electrolyte solution is 1-50%.
6. The method for preparing a gas-solid electrocatalytic electrode according to claim 5, wherein the concentration of the hydrophilic solid electrolyte solution is 5-35%.
7. The method for preparing a gas-solid electrocatalytic electrode according to claim 5, wherein the hydrophilic group solid electrolyte solution is used in an amount of 0.1-1 mL/cm 2 。
8. The method for preparing a gas-solid electrocatalytic electrode according to claim 5, wherein the method for preparing a catalyst precursor with an anodic oxidation active layer on the surface of the conductive substrate comprises:
the oxidation active oxide is arranged on the surface of the conductive substrate by adopting a coating or electrodeposition method.
9. The method for producing a gas-solid phase electrocatalytic electrode according to claim 5, wherein the method comprises:
setting oxidation active oxide on the surface of a conductive substrate by adopting a coating or electrodeposition method to obtain a catalyst precursor with an anodic oxidation active layer on the surface of the conductive substrate, and then mixing hydrophilic group solid electrolyte solution with mass concentration of 5-35% with the concentration of 0.1-1 mL/cm 2 The catalyst is obtained by coating the surface of the anodic oxidation active layer and drying.
10. Use of a gas-solid phase electrocatalytic electrode according to any one of claims 1-4 for electrochemical catalytic oxidation of indoor pollutants.
11. Use of a gas-solid electrocatalytic electrode according to claim 10, wherein the indoor contaminants comprise formaldehyde and/or benzene series.
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