CN114059089B - Difunctional electrolytic reaction device - Google Patents
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- CN114059089B CN114059089B CN202111631462.XA CN202111631462A CN114059089B CN 114059089 B CN114059089 B CN 114059089B CN 202111631462 A CN202111631462 A CN 202111631462A CN 114059089 B CN114059089 B CN 114059089B
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Abstract
The invention discloses a difunctional electrolytic reaction device, which belongs to the technical field of electrocatalysis, and comprises an anode tank, an anode electrode plate, a cathode tank, a cathode catalyst electrode group, a ceramic diaphragm and an air chamber, wherein the anode electrode plate is arranged at the bottom of the anode tank and is provided with an external power supply contact point, the cathode catalyst electrode group is arranged at the bottom of the cathode tank and is also provided with an external power supply contact point, and the cathode catalyst electrode group comprises: a conductive layer, a catalyst layer, an isolation layer, and a support layer. The anode of the equipment can produce oxygen to achieve the purpose of purifying air, the cathode can be used for preparing hydrogen peroxide, the principle is that the oxygen is electrochemically reduced to generate the hydrogen peroxide, the equipment is simple to operate and low in cost, and the prepared hydrogen peroxide can meet the sterilization requirement of the market and has great application potential.
Description
Technical Field
The invention belongs to the technical field of electrocatalysis, and particularly relates to a bifunctional electrolytic reaction device.
Background
With the development of society, people put higher and higher requirements on the standard of life and health. Particularly, in recent years, the spread of epidemic situations causes great obstruction to the development of society, people's life is greatly influenced, and daily disinfection and sterilization are extremely important. The common disinfectants in the market at present comprise sodium hypochlorite, alcohol, ultraviolet, hydrogen peroxide and the like, but have certain disadvantages, for example, the sodium hypochlorite is used as a chlorine-containing reagent, and chlorine is discharged in the degradation process, so that the environment is influenced, and the human health is influenced; alcohol is a flammable substance and is prone to danger; how to control better sterilization by uv is also a great challenge; the hydrogen peroxide has strong oxidizability, and the decomposition products are water and oxygen, so that the requirement of environmental protection can be met, and the hydrogen peroxide is a clean and pollution-free green disinfectant.
The existing preparation of hydrogen peroxide mainly depends on the traditional anthraquinone method, the preparation process is complex, the pollution is serious, the cost is high, the long-term development is not facilitated, and meanwhile, the hydrogen peroxide sold on the market is subjected to dilution treatment, long-distance transportation and great risk of transportation. Therefore, on one hand, a more green hydrogen peroxide production mode is developed, and on the other hand, the solution of some safety problems in the use process is particularly important.
In recent years, the electrochemical method is developed rapidly due to the reasons of strong process controllability, green preparation process, easy product control and the like, so that the problem can be solved well by preparing hydrogen peroxide by the electrochemical method. Currently, the reaction faces two major problems, one is the catalyst aspect and one is the equipment aspect; the poor activity and stability of the electrocatalytic oxygen reduction catalyst are important reasons for hindering the application of the electrocatalytic oxygen reduction catalyst, and the development of equipment also determines the concentration of hydrogen peroxide to a great extent. In recent years, a lot of researches are carried out on the preparation of catalysts, for example, C-based catalysts, pd monatomic catalysts and the like are used for preparing hydrogen peroxide by electrocatalytic oxygen reduction, and the catalysts show good activity and stability, but reports on electrodes and equipment are few, and how to make up for the development defects in the field is very important.
Disclosure of Invention
In view of the problems of the prior art, the present invention aims to provide a dual-function electrolytic reaction device, wherein the cathode further changes the amount of oxygen participating in the reaction by controlling the contact manner of reactant oxygen and a catalyst electrode, so as to improve the reaction progress of oxygen reduction and enhance the diffusion of products, and the anode reaction obtains oxygen.
The invention discloses a difunctional electrolytic reaction device, which comprises a reaction device body, wherein a ceramic diaphragm arranged in the middle of the reaction device body divides the reaction device body into an anode tank and a cathode tank, an anode exhaust port is arranged at the top of the anode tank, a cathode exhaust port is arranged at the top of the cathode tank, the difunctional electrolytic reaction device is characterized in that an anode electrode plate is arranged at the bottom of the anode tank and is sealed by silicon rubber, a power supply contact is arranged on the anode electrode plate, a cathode catalyst electrode group and a cathode air chamber are arranged at the bottom of the cathode tank, an air inlet is arranged on the cathode air chamber, the cathode catalyst electrode group is of a four-in-one composite structure, and the anode is oxidized to generate oxygen under the power-on state; air in the cathode air chamber enters the cathode catalyst electrode group, and the cathode is subjected to reduction reaction under the action of the catalyst to generate a corresponding product.
The invention further defines that the cathode catalyst electrode group comprises a sealing gasket, a catalyst bed layer, an isolation layer and a supporting layer, wherein the catalyst bed layer is arranged on the conducting layer in a compounding mode through a catalyst, the catalyst layer is formed on the conducting layer and used for carrying out electrocatalytic reaction, the sealing gasket is arranged among the catalyst bed layer, the isolation layer and the supporting layer, the catalyst bed layer is located on one side of the cathode groove, the supporting layer is located on one side of the cathode air chamber, and the sealing gasket is arranged at the connecting position of the sealing gasket and the cathode air chamber respectively.
Furthermore, the invention also limits the compounding mode of the catalyst and the conducting layer to be transfer printing, ultrasonic spraying or magnetron sputtering, and the ultrasonic spraying is preferred.
Further, the invention also defines that the conducting layer is made of porous material, preferably carbon cloth, nickel foam or copper foam, and optimally the carbon cloth.
Furthermore, the invention also limits the isolating layer to be a gas-permeable and water-proof material, preferably a carbon material, an organic polymer film material or a ceramic material, and most preferably a carbon material.
Further, the invention also defines the sealing gasket as being made of rubber material, preferably styrene butadiene rubber or butadiene rubber, and optimally silicon rubber.
Furthermore, the invention also defines that the support layer is made of a porous hard material, preferably reticular nickel or reticular stainless steel, and most preferably reticular stainless steel.
Furthermore, the base adopts an air chamber, and the structure of the air chamber is completely the same as that of the cathode air chamber and is used as a spare cathode air chamber.
Furthermore, the invention also limits the anode electrode sheet to be a platinum-containing metal or iridium-tantalum metal, preferably an iridium-tantalum coating titanium anode.
Except the cathode catalyst electrode group, the joints of other parts are provided with sealing gaskets, and rubber materials such as silicon rubber, styrene butadiene rubber, butadiene rubber and the like can be selected, and the silicon rubber is preferred.
Compared with the prior art, the invention has the following beneficial effects:
1) According to the invention, a specific cathode catalyst electrode group structure is adopted, and the catalyst, the conductive layer, the isolation layer and the support structure are combined to form a 'four-in-one' structure, so that in performance, as the catalyst electrode has a larger area, gas can be gathered in a cathode air chamber, the 'four-in-one' structure plays a role in 'collecting flow', so that the gas can uniformly reach the surface of the catalyst electrode, one part of the gas is adsorbed by the catalyst for reaction, and the other part of the gas carries reaction products away from the catalyst electrode, so that the reaction products are separated, the reaction efficiency is improved, and in structure, the structure increases the mechanical stability of the electrode and prolongs the service life of equipment;
2) According to the invention, the anode electrode plate is embedded in the bottom of the anode tank, so that insufficient anode reaction caused by uneven contact between the electrode and the electrolyte can be effectively avoided, and the generated gas can be discharged, and the adopted iridium tantalum coating titanium anode and other anode electrode plate materials have good oxygen evolution performance and can generate high-purity oxygen as the anode of the device;
3) According to the bifunctional electrolytic reaction device, the cathode further changes the amount of oxygen participating in reaction by controlling the contact mode of reactant oxygen and the catalyst electrode, so that the reaction process of oxygen reduction is improved, the diffusion of products is enhanced, and the anode reaction obtains oxygen.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
fig. 2 is a schematic view of the cathode catalyst electrode assembly according to the present invention.
In fig. 1: 1. an anode tank; 2. an anode electrode sheet; 3. a cathode channel; 4. a cathode catalyst electrode assembly; 5. a ceramic diaphragm; 6. an air inlet; 7. a cathode air chamber; 8. an anode air chamber; 9. an anode exhaust port; 10. a cathode exhaust port;
in fig. 2: 41. a gasket; 42. a catalyst layer; 43. a conductive layer; 44. an isolation layer; 45. and (4) a support layer.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, but the scope of the invention is not limited to the scope described, and encompasses all peroxide disinfectants which use hydrogen peroxide as a reactant. The terms "upper" and "lower" in the present invention only represent relative positions in the drawings, and do not represent absolute positions of products.
As shown in fig. 1 and fig. 2, the bifunctional electrolytic reaction device of the present invention comprises a reaction device body, wherein a ceramic diaphragm 5 is arranged in the middle of the reaction device body, and is divided into an anode tank 1 and a cathode tank 3 by taking the ceramic diaphragm 5 as a center line, the connecting portion of the anode tank 1, the cathode tank 3 and the ceramic diaphragm 5 is provided with a sealing gasket, the bottom of the anode tank 1 is provided with an anode electrode sheet 2, the anode electrode sheet 2 is provided with a power supply contact, the bottom of the cathode tank 3 is connected with a cathode catalyst electrode group 4, the cathode catalyst electrode group 4 is directly connected with a cathode air chamber 7, the cathode air chamber 7 is provided with an air inlet 6, the connecting portion of the two components is provided with a sealing gasket, the cathode air chamber 7 plays a ventilation role, so that gas is fully filled, the gas further uniformly passes through the cathode catalyst electrode group 4, and when a reaction is performed, a reaction product is taken away from a catalyst electrode, which is beneficial for the reaction, and the reaction efficiency is improved; meanwhile, the upper end of the anode tank 1 is provided with an anode exhaust port 9, and the upper end of the cathode tank 3 is provided with a cathode exhaust port 10 for feeding, discharging and exhausting.
As shown in fig. 2, the cathode catalyst electrode assembly 4 adopting the "four-in-one" of the present invention includes a sealing pad 41, a catalyst bed layer, an isolation layer 44 and a supporting layer 45, wherein the catalyst bed layer is formed by compositely disposing a catalyst on a conductive layer 43 by means of transfer printing, ultrasonic spraying or magnetron sputtering, a catalyst layer 42 is formed on the conductive layer 43, and the catalyst layer 42 is used for performing an electrocatalytic reaction, in the embodiment of the present invention, the catalyst adopts a modified MXene supported Ni catalyst, referred to as Ni catalyst for short, which is disclosed in the patent application No. 202110564191.4, and the catalyst is coated on the conductive layer 43 by means of ultrasonic spraying; a separation sealing gasket 41 is arranged among the catalyst bed layer, the isolation layer 44 and the supporting layer 45, the sealing gasket 41 for separation is of a hollow structure, the area of the hollow part is smaller than that of the catalyst bed layer, the isolation layer 44 and the supporting layer 45, the catalyst bed layer, the isolation layer 44 and the supporting layer 45 are separated from the periphery by the sealing gasket 41, and a gap is reserved in the middle; the catalyst bed is located cathode trough 3 one side, and supporting layer 45 is located cathode air chamber 7 one side and the junction is equipped with sealed pad 41 respectively, through compound catalyst layer 42 and conducting layer 43 of mode ultrasonic spraying, and isolation layer 44 is favorable to the gas to penetrate from cathode air chamber 7 and react with the catalyst, and the one deck of lower extreme is porous supporting layer 45, prevents because of the destruction of the big cathode electrode group that leads to of electrolyte pressure, provides mechanical support.
For further explanation, the conductive layer 43 of the present invention is made of a porous material such as carbon cloth, nickel foam, or copper foam, and in the embodiment, carbon cloth is used; the isolation layer 44 is made of a gas-permeable and water-proof material, such as a carbon material, an organic polymer film material, a ceramic material, or the like, and in the embodiment, a carbon material is used; the sealing pad 41 is made of rubber material, such as silicon rubber, styrene butadiene rubber, etc., in the embodiment, silicon rubber is used; the supporting layer 45 is made of porous hard material, such as mesh nickel, mesh stainless steel, etc., in the embodiment, mesh stainless steel is adopted; the anode electrode sheet 2 of the invention is made of platinum-containing metal or iridium-tantalum metal, and the anode electrode sheet 2 adopted in the embodiment is an iridium-tantalum coating titanium anode.
In order to facilitate the installation of the device, the bottom of the anode electrode plate 2 is provided with a base, the base and the bottom surface of the cathode air chamber 7 are on the same horizontal plane, and the base can adopt an air chamber which is completely the same as the cathode air chamber 7 as a spare cathode air chamber.
Example 1: device for preparing oxygen and hydrogen peroxide in dual functions
And placing an iridium tantalum coating titanium anode (2cm x 4cm) between an anode tank and an anode air chamber, and sealing by using a sealing gasket (silicon rubber) to prevent the leakage of the electrolyte. The upper end of the anode tank is provided with an exhaust port for oxygen supply to be discharged for use, a ceramic diaphragm is arranged between the cathode tank and the anode tank, ions in the reaction process are selectively permeated, and the effect of separating the products of the cathode tank and the anode tank is achieved. The 'four-in-one' cathode catalyst electrode group 4 is arranged between the cathode tank 3 and the cathode air chamber 7, and is provided with a sealing gasket 41 (silicon rubber), and the main process is as follows: the method comprises the following steps of carrying out ultrasonic spraying on a catalyst (2cm x 4cm, ni-based catalyst) on a conductive layer (carbon cloth), specifically, arranging the carbon cloth on a heating table, preparing a catalyst solution (dispersing 100mg of the catalyst into 9ml of ethanol, and simultaneously adding 1ml of nafion solution), adding a mixed solution into a spray pen with an ultrasonic function, carrying out uniform spraying on the carbon cloth to form a uniform catalyst layer, separating the catalyst layer 42 from an isolation layer 44 by using silicon rubber for preparing a catalytic core of hydrogen peroxide to play roles of sealing and avoiding influencing the performance of the catalyst, wherein the isolation layer (carbon material) mainly plays a role in guiding gas and isolating liquid, so that reactants (oxygen) and the catalyst are fully mixed, the reaction efficiency is improved, and the lower end of the isolation layer is a supporting layer (reticular stainless steel) to play a role in protecting the isolation layer and avoid the isolation layer from being damaged due to the pressure of electrolyte. And a reactant air inlet is arranged in the cathode air chamber, oxygen is blown in for reaction, and the product is hydrogen peroxide. The specific reaction conditions are that the current of the reaction is controlled to be 300 mA, 400 mA and 500mA, the electrolyte is PBS buffer solution, and the actual catalytic area is 18 cm 2 The flow rate of oxygen was 5mL/min.
The reaction conditions were varied and the results were shown in Table 1.
TABLE 1 oxygen/Hydrogen peroxide yields at different currents
The results in table 1 show that the invention has excellent oxygen preparation performance and hydrogen peroxide production capacity, the hydrogen peroxide concentration can completely meet daily disinfection and sterilization, and the invention has good application potential.
Example 2: device for preparing oxygen and sodium percarbonate disinfectant by double functions
And placing an iridium tantalum coating titanium anode (2cm x 4cm) between an anode tank and an anode air chamber, and sealing by using a sealing gasket (silicon rubber) to prevent the leakage of the electrolyte. The upper end of the anode tank is provided with an exhaust port for oxygen supply to be discharged for use, a ceramic diaphragm is arranged between the cathode tank and the anode tank, ions in the reaction process are selectively permeated, and the effect of separating the products of the cathode tank and the anode tank is achieved. The four-in-one cathode catalyst electrode group 4 is arranged between the cathode tank 3 and the cathode air chamber 7, is provided with a sealing gasket 41 (silicon rubber), and mainly comprises the following steps: the method comprises the steps of ultrasonically spraying a catalyst (2cm x 4cm, ni-based catalyst) on a conductive layer (carbon cloth), specifically, placing the carbon cloth on a heating table, preparing a catalyst solution (dispersing 100mg of the catalyst into 9ml of ethanol, and simultaneously adding 1ml of nafion solution), adding a mixed solution into a spray pen with an ultrasonic function, uniformly spraying the mixed solution on the carbon cloth to form a uniform catalyst layer, separating the catalyst layer 42 and a separation layer 44 by using silicon rubber to play a role in sealing and avoiding influencing the performance of the catalyst in order to prepare a catalytic core of hydrogen peroxide, wherein the separation layer (carbon material) mainly plays a role in guiding gas and separating liquid, so that reactants (oxygen) and the catalyst are fully mixed, the reaction efficiency is improved, and the lower end of the separation layer is provided with a support layer (mesh stainless steel) to play a role in protecting the separation layer and avoid the damage of the separation layer caused by the pressure of electrolyte. The cathode air chamber is provided with a reactant inlet, oxygen is blown in for reaction, the product is sodium percarbonate disinfection solution, the reaction conditions are that the current of the reaction is controlled to be 30, 60 and 80mA, the electrolyte is edible soda or edible sodium bicarbonate solution, and the actual catalytic area is 18 cm 2 The flow rate of oxygen was 5mL/min.
The reaction conditions were varied and the results were as shown in Table 2.
TABLE 2 oxygen/sodium percarbonate production at different currents
The results in table 2 show that the invention has excellent oxygen preparation performance and sodium percarbonate production capacity, the sodium percarbonate concentration can meet the daily disinfection and sterilization requirements, and the invention can also be used for oxygen supply and sterilization of fish ponds and has good application potential.
Example 3: device of difunctional preparation oxygen and peracetic acid disinfectant
And placing an iridium tantalum coating titanium anode (2cm x 4cm) between an anode tank and an anode air chamber, and sealing by using a sealing gasket (silicon rubber) to prevent the leakage of the electrolyte. The upper end of the anode tank is provided with an exhaust port, oxygen supply gas is discharged for use, a ceramic diaphragm is arranged between the cathode tank and the anode tank, ions in the reaction process selectively permeate through the ceramic diaphragm, and the ceramic diaphragm has the function of separating products in the cathode tank and the anode tank. The 'four-in-one' cathode catalyst electrode group 4 is arranged between the cathode tank 3 and the cathode air chamber 7, and is provided with a sealing gasket 41 (silicon rubber), and the main process is as follows: the method comprises the following steps of carrying out ultrasonic spraying on a catalyst (2cm x 4cm, ni-based catalyst) on a conductive layer (carbon cloth), specifically, arranging the carbon cloth on a heating table, preparing a catalyst solution (dispersing 100mg of the catalyst into 9ml of ethanol, and simultaneously adding 1ml of nafion solution), adding a mixed solution into a spray pen with an ultrasonic function, carrying out uniform spraying on the carbon cloth to form a uniform catalyst layer, separating the catalyst layer 42 from an isolation layer 44 by using silicon rubber for preparing a catalytic core of hydrogen peroxide to play roles of sealing and avoiding influencing the performance of the catalyst, wherein the isolation layer (carbon material) mainly plays a role in guiding gas and isolating liquid, so that reactants (oxygen) and the catalyst are fully mixed, the reaction efficiency is improved, and the lower end of the isolation layer is a supporting layer (reticular stainless steel) to play a role in protecting the isolation layer and avoid the isolation layer from being damaged due to the pressure of electrolyte. The cathode air chamber is provided with a reactant inlet, oxygen is blown in to react, and the product is peroxyacetic acid disinfectant which is the reverse of the peroxyacetic acid disinfectantThe specific conditions are that the current of the reaction is controlled to be 300, 400 and 500mA, the electrolyte is edible vinegar, and the actual catalytic area is 18 cm 2 The flow rate of oxygen was 5mL/min.
The reaction conditions were varied and the test results are shown in Table 3.
TABLE 3 oxygen/Peroxyacetic acid production at different currents
The results in table 3 show that the invention has excellent oxygen preparation performance and production capacity of peracetic acid, the concentration of the peracetic acid can meet the daily requirements of infectious disease disinfection, drinking water disinfection, fabric disinfection and food industry, and the invention has good application prospect.
Claims (19)
1. A difunctional electrolytic reaction device comprises a reaction device body, wherein a ceramic diaphragm (5) arranged in the middle of the reaction device body divides the reaction device body into an anode tank (1) and a cathode tank (3), an anode exhaust port (9) is formed in the top of the anode tank (1), a cathode exhaust port (10) is formed in the top of the cathode tank, the difunctional electrolytic reaction device is characterized in that an anode electrode plate (2) is arranged at the bottom of the anode tank (1), a power supply contact is arranged on the anode electrode plate (2), a cathode catalyst electrode group (4) and a cathode air chamber (7) are arranged at the bottom of the cathode tank (3), an air inlet (6) is formed in the cathode air chamber (7), the cathode catalyst electrode group (4) is of a four-in-one composite structure, and under the power-on state, an anode is subjected to oxidation reaction to generate a product oxygen; air in the cathode air chamber (7) enters the cathode catalyst electrode group (4), and the cathode is subjected to reduction reaction under the action of a catalyst to generate a corresponding product;
the cathode catalyst electrode group (4) comprises a sealing gasket (41), a catalyst bed layer, an isolation layer (44) and a supporting layer (45), wherein the catalyst bed layer is arranged on a conductive layer (43) by compounding a catalyst, a catalyst layer (42) is formed on the conductive layer (43) and used for carrying out electrocatalytic reaction, the sealing gasket (41) is arranged between the catalyst bed layer, the isolation layer (44) and the supporting layer (45), the catalyst bed layer is positioned on one side of a cathode slot (3), the supporting layer (45) is positioned on one side of a cathode air chamber (7), and the connecting parts are respectively provided with the sealing gasket (41).
2. The apparatus of claim 1, wherein the catalyst and the conductive layer are combined by transfer printing, ultrasonic spraying or magnetron sputtering.
3. A dual function electrolytic reaction device as recited in claim 1 wherein the conductive layer (43) is made of a porous material.
4. A dual function electrolytic reaction device as recited in claim 1 wherein the separation layer (44) is a gas permeable and water impermeable material.
5. A dual function electrolytic reaction device in accordance with claim 1, wherein the sealing gasket (41) is a rubber material.
6. A dual function electrolytic reaction device as recited in claim 1, wherein the support layer (45) is a porous hard material.
7. The apparatus of claim 1, wherein the catalyst and the conductive layer are combined by ultrasonic spraying.
8. A dual function electrolytic reaction device as recited in claim 3, wherein the conductive layer (43) is a carbon cloth, nickel foam or copper foam.
9. A dual function electrolytic reaction device as recited in claim 3 wherein the conductive layer (43) is a carbon cloth.
10. A bifunctional electrolytic reaction device as claimed in claim 4 wherein the separation layer (44) is a carbon material, an organic polymer membrane material or a ceramic material.
11. A dual function electrolytic reaction device as claimed in claim 4, wherein the separation layer (44) is a carbon material.
12. A bifunctional electrolytic reaction device according to claim 1, wherein the sealing gasket (41) is made of silicone rubber, styrene-butadiene rubber or butadiene rubber.
13. A bifunctional electrolytic reaction device according to claim 1, characterized in that the sealing gasket (41) is silicone rubber.
14. A dual function electrolytic reaction device as recited in claim 1 wherein the support layer (45) is reticulated nickel or reticulated stainless steel.
15. A dual function electrolytic reaction device as recited in claim 1 wherein the support layer (45) is stainless steel mesh.
16. A bifunctional electrolytic reaction device as claimed in any one of claims 1-15 characterized in that the anode electrode sheet (2) has a base at the bottom, and the base is at the same level with the bottom of the cathode air chamber (7).
17. A dual function electrolytic reaction device in accordance with any one of claims 1-15, characterized in that the base employs an anode air chamber (8) having a configuration identical to that of the cathode air chamber (7) as a backup cathode air chamber.
18. A bifunctional electrolytic reaction device as claimed in any one of claims 1 to 15 wherein the anode electrode sheet (2) is platinum-containing metal or iridium-tantalum metal.
19. A bifunctional electrolytic reaction device as claimed in any one of claims 1-15 characterised in that the anode electrode sheet (2) is iridium tantalum metal.
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