CN114314765A - Method and device for producing hydrogen by combining electrochemical resource desulfurization wastewater and application - Google Patents
Method and device for producing hydrogen by combining electrochemical resource desulfurization wastewater and application Download PDFInfo
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Abstract
The invention belongs to the technical field of wastewater treatment and electrolytic hydrogen production, and discloses a method, a device and application for producing hydrogen by combining electrochemical resource desulfurization wastewater, wherein desulfurization wastewater and sulfuric acid solution are respectively introduced into an anode chamber and a cathode chamber of an electrolyzer; switching on the power supply of the electrolyzer, and collecting the generated hydrogen on the cathode side of the electrolyzer; and when the concentration of the sulfite in the desulfurization wastewater is reduced to the target concentration or the target product is accumulated to the specified concentration, switching off the power supply, discharging the anolyte and recovering sulfate or persulfate or other resource products from the anolyte of the electrolyzer. The method utilizes the electro-oxidation reaction of sulfite in the desulfurization wastewater to replace the traditional water electrolysis anode oxygen evolution reaction, obviously reduces the operating hydrogen evolution potential of the electrolyzer, obviously reduces the power consumption and the cost of hydrogen production by water electrolysis, is favorable for application and popularization of hydrogen energy, and is used for realizing the target assistance of carbon neutralization and carbon peak reaching.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment and electrolytic hydrogen production, and particularly relates to a method and a device for producing hydrogen by combining electrochemical resource desulfurization wastewater and application of the method and the device.
Background
At present, under the large policy background of carbon neutralization and carbon peak reaching, hydrogen energy technology is coming to a new round of chance and development. The search and development of green and economic hydrogen production technology are always the central importance of hydrogen energy development. The hydrogen production by water electrolysis can utilize the electric energy of abandoned wind and abandoned light and the electric energy of peak clipping and valley filling of the power grid to prepare hydrogen, and is considered to be a green hydrogen production technology with great prospect. However, the anode oxygen evolution reaction potential is high, and the requirement on the anode material is high, which is a main limiting factor causing high cost and difficult large-scale application of the hydrogen production by water electrolysis. Therefore, the selection of a proper low-potential reaction to replace an oxygen evolution reaction as an anode reaction is very important for reducing the running cost and the device cost of the hydrogen production by electrolyzing water.
Through the above analysis, the problems and defects of the prior art are as follows: the existing method for producing hydrogen by electrolyzing water has higher cost and is difficult to be applied on a large scale.
The difficulty in solving the above problems and defects is: rare and noble metals such as iridium and ruthenium are required to be used as anode materials, so that the resource is limited and the price is high; the anode oxygen evolution potential +1.23V restricts the power consumption of the water electrolysis hydrogen production to be further reduced.
The significance of solving the problems and the defects is as follows: the anode reaction with lower reaction potential is used for replacing oxygen evolution reaction, and the reaction voltage of water electrolysis hydrogen evolution is theoretically broken through 1.23V, so that the energy consumption of water electrolysis hydrogen production is further reduced; the use of metals such as lead and the like as the catalyst can obviously reduce the cost of the electrolyzer device, break through the resource limitation of rare and precious metals and is beneficial to the large-scale popularization and application of the technology.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method and a device for producing hydrogen by combining electrochemical resource desulfurization waste water and application.
The invention is realized in such a way that a method for producing hydrogen by combining electrochemical resource desulfurization waste water comprises the following steps: and (3) using the desulfurization wastewater as an anolyte and a sulfuric acid solution as a catholyte, and oxidizing sulfite and producing hydrogen by using an electrolyzer.
Further, the method for producing hydrogen by the cooperation of electrochemical resource desulfurization wastewater comprises the following steps:
step one, introducing desulfurization wastewater and sulfuric acid solution into an anode chamber and a cathode chamber of an electrolyzer respectively; switching on the power supply of the electrolyzer, and collecting the generated hydrogen on the cathode side of the electrolyzer;
and step two, after the concentration of the sulfite in the desulfurization wastewater is reduced to the target concentration or the target product is accumulated to the specified concentration, switching off the power supply, discharging the desulfurization wastewater, and recovering sulfate or persulfate or other resource products from the anode side of the electrolyzer.
Further, the electrolyzer is a membrane electrolyzer.
Further, a catalyst is added to the electrolyzer.
Further, the catalyst is a platinum group metal catalyst, gold, silver catalyst or lead catalyst.
Further, the electrolyzer can be used in a reversed polarity.
Further, the working temperature of the electrolyzer is 40-90 ℃.
Further, the mass fraction of the sulfuric acid solution is 0-20%.
Further, the collecting the produced hydrogen gas at the cathode side of the electrolyzer comprises: collecting hydrogen at the cathode liquid storage tank of the electrolyzer by a gas-liquid separation method.
The invention also aims to provide an electrochemical resource desulfurization waste water collaborative hydrogen production device for implementing the electrochemical resource desulfurization waste water collaborative hydrogen production method.
The invention also aims to provide the application of the method for producing hydrogen by the cooperation of electrochemical resource desulfurization wastewater and hydrogen production in desulfurization wastewater treatment.
By combining all the technical schemes, the invention has the advantages and positive effects that:
according to the method for producing hydrogen by using the electrochemical method resource desulfurization wastewater, the conventional electrolysis water anode oxygen evolution reaction is replaced by the sulfite electrooxidation reaction in the desulfurization wastewater, so that the operation potential of an electrolyzer is obviously reduced, and the power consumption and the cost of hydrogen production by electrolysis water are obviously reduced; lead and other metals can be selected as sulfite catalytic materials correspondingly, so that the cost of the electrolyzer is reduced, the application and the popularization of hydrogen energy are facilitated, and the aim of carbon neutralization and carbon peak reaching is achieved.
The invention converts sulfur dioxide pollutants captured from the flue gas into resource products such as sulfate fertilizer or persulfate with high added value, changes waste into valuable, realizes the large circulation of sulfur element, and provides an economic and feasible treatment scheme for high-salinity wastewater which is difficult to biochemically treat.
The same multifunctional catalyst can be selected for the cathode and the anode, the electrolyzer can be used in a reversed mode, the problem of electrode fouling frequently caused by wastewater treatment by an electrochemical method can be effectively solved, the electrolytic performance of the electrolyzer can be guaranteed, and the durability can be improved.
The invention converts sulfur dioxide pollutants captured from the flue gas into sulfate fertilizer or persulfate with high added value, thereby changing waste into valuable. The cathode and the anode of the electrolyzer have high production value and good economical efficiency and application prospect.
Drawings
FIG. 1 is a schematic diagram of a method for producing hydrogen by using electrochemical resource desulfurization wastewater in cooperation.
FIG. 2 is a flow chart of a method for producing hydrogen by using electrochemical resource desulfurization wastewater in cooperation.
Figure 3 is a graph of potentiodynamic sweep of an electrolyzer provided by an embodiment of the present invention.
FIG. 4 is a performance diagram of the resource-oriented desulfurized wastewater provided by the embodiment of the invention.
Figure 5 is a potentiodynamic sweep plot of an electrolyzer at different temperatures provided by an embodiment of the present invention.
FIG. 6 is a graph of the step voltage test performance of an electrolyzer provided by an embodiment of the invention.
FIG. 7 is a graph showing the performance of resource-desulfurization waste water in example 4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a method for producing hydrogen by combining electrochemical resource desulfurization wastewater and hydrogen production, and the invention is described in detail by combining the attached drawings.
As shown in fig. 1, the method for producing hydrogen by using electrochemical resource desulfurization wastewater in synergy provided by the embodiment of the present invention includes:
and (3) taking the desulfurization wastewater as an anolyte and a sulfuric acid solution as a catholyte, and desulfurizing and producing hydrogen by using an electrolyzer.
As shown in fig. 2, the method for producing hydrogen by using electrochemical resource desulfurization wastewater in coordination includes the following steps:
s101, introducing desulfurization wastewater and a sulfuric acid solution with the mass fraction of 0-20% into an anode chamber and a cathode chamber of a diaphragm electrolyzer respectively; connecting the power supply of the electrolyzer, and collecting hydrogen at a catholyte storage tank of the electrolyzer by a gas-liquid separation method;
s102, after the concentration of the sulfite in the desulfurization wastewater is reduced to the target concentration or the target product is accumulated to the designated concentration, the power supply is cut off, the desulfurization wastewater is discharged, and sulfate or persulfate or other resource products are recovered from the anode side of the electrolyzer.
The electrolyzer provided by the embodiment of the invention is added with a catalyst.
The catalyst provided by the embodiment of the invention is a platinum group metal catalyst, a gold catalyst, a silver catalyst or a lead catalyst.
The electrolyzer provided by the embodiment of the invention can be used in a reversed mode.
The working temperature of the electrolyzer provided by the embodiment of the invention is 40-90 ℃.
The technical solution of the present invention is further described with reference to the following specific embodiments.
As can be seen from the above reaction equation, the potential of the sulfite or bisulfite electrooxidation reaction is much lower than the oxygen evolution potential (1.23V), and is an excellent alternative reaction. In the flue gas desulfurization process, sulfur dioxide in the flue gas is absorbed by alkali liquor to obtain desulfurization wastewater containing a large amount of sulfite or bisulfite. The direct discharge of the desulfurization waste water can pollute water body, and the desulfurization waste water needs to be treated first. Therefore, the desulfurization waste water is selected as the anolyte, and the electrolysis of sulfite coupled cathode hydrogen production has high economic benefit and environmental benefit.
A method for producing hydrogen by using electrochemical method resource desulfurization waste water in synergy comprises the following steps:
s1, introducing desulfurization wastewater and sulfuric acid solution into the anode chamber and the cathode chamber of the electrolyzer respectively;
s2, electrifying to enable the electrolyzer to work, and collecting the generated hydrogen on the cathode side;
s3, stopping electrifying, and discharging the desulfurization wastewater;
s4, recovering valuable products from the treated desulfurization waste water.
The method for producing hydrogen by the cooperation of the electrochemical method resource desulfurization wastewater, which is disclosed by the application, is characterized in that the sulfur wastewater is produced by flue gas desulfurization, and a large amount of sulfite or bisulfite exists in the desulfurization wastewater; pumping the desulfurization wastewater into an anode chamber of an electrolyzer, and converting sulfite or bisulfite into high value-added products such as sulfate or persulfate by electrocatalysis; the operation potential of the electrolyzer is reduced, the cathode simultaneously evolves hydrogen, the power consumption and the cost of hydrogen production by water electrolysis are obviously reduced, and the method has good economical efficiency and application prospect.
In some embodiments, the catholyte sulfuric acid solution has a concentration of 0 to 20%.
In some embodiments, the catalyst used by the electrolyzer is a platinum group metal catalyst or a gold, silver catalyst.
In some embodiments, the electrolyzer has an operating temperature of 40-90 ℃.
In some embodiments, the valuable product is a sulfate or persulfate salt.
The method for producing hydrogen by recycling desulfurization waste water through an electrochemical method is further described below by using specific examples.
Example 1
A method for producing hydrogen by using electrochemical method resource desulfurization waste water in synergy comprises the following steps:
s1, circularly introducing the ammonium desulfurization wastewater into the anode chamber of the electrolyzer, wherein the concentration of sulfite in the wastewater is 4.84 mol per liter; introducing pure water into the cathode chamber; the temperature of the solution is 55 ℃;
s2, electrifying to enable the electrolyzer to work, and collecting the generated hydrogen on the cathode side; the used electrolyzer is a membrane electrode electrolyzer, the cathode and anode catalysts are carbon-supported platinum-palladium catalysts, and the catalysts are directly loaded on a proton exchange membrane (DuPont, Nafion N212) to prepare a membrane electrode assembly;
s3, stopping electrifying, and discharging the desulfurization wastewater;
s4, evaporating and crystallizing the treated desulfurization wastewater to recover ammonium sulfate fertilizer.
Example 2
A method for producing hydrogen by using electrochemical method resource desulfurization waste water in synergy comprises the following steps:
s1, circularly introducing the ammonium desulfurization wastewater into the anode chamber of the electrolyzer, wherein the concentration of sulfite in the wastewater is 4.84 mol per liter; introducing a sulfuric acid solution with the mass fraction of 15% into the cathode chamber; the temperature of the solution is 40-90 ℃;
s2, electrifying to enable the electrolyzer to work, and collecting the generated hydrogen on the cathode side; the used electrolyzer is a membrane electrode electrolyzer, the cathode and anode catalysts are carbon-supported gold silver catalysts, and the catalysts are directly loaded on a proton exchange membrane (DuPont, Nafion N212) to prepare a membrane electrode assembly;
s3, stopping electrifying, and discharging the desulfurization wastewater;
s4, evaporating and crystallizing the treated desulfurization wastewater to recover ammonium sulfate fertilizer.
Example 3
A method for producing hydrogen by using electrochemical method resource desulfurization waste water in synergy comprises the following steps:
s1, circularly introducing the ammonium desulfurization wastewater into the anode chamber of the electrolyzer, wherein the concentration of sulfite in the wastewater is 4.84 mol per liter; introducing a sulfuric acid solution with the mass fraction of 20% into the cathode chamber; the temperature of the solution is 55 ℃;
s2, electrifying to enable the electrolyzer to work, and collecting the generated hydrogen on the cathode side; the used electrolyzer is a diaphragm electrolyzer, and the cathode and the anode both adopt platinum coating titanium anodes;
s3, stopping electrifying, and discharging the desulfurization wastewater;
s4, evaporating and crystallizing the treated desulfurization wastewater to recover ammonium persulfate.
Example 4
A method for producing hydrogen by using electrochemical method resource desulfurization waste water in synergy comprises the following steps:
s1, circularly introducing the ammonium desulfurization wastewater into the anode chamber of the electrolyzer, wherein the concentration of sulfite in the wastewater is 4.84 mol per liter; introducing a sulfuric acid solution with the mass fraction of 15% into the cathode chamber; the temperature of the solution is 55 ℃;
s2, electrifying to enable the electrolyzer to work, and collecting the generated hydrogen on the cathode side; the electrolyzer is a membrane electrode electrolyzer, the anode catalysts are lead dioxide nano catalysts, the cathode catalysts are carbon-supported platinum catalysts, and the catalysts are directly loaded on a proton exchange membrane (DuPont, Nafion N212) to prepare a membrane electrode assembly;
s3, stopping electrifying, and discharging the desulfurization wastewater;
s4, evaporating and crystallizing the treated desulfurization wastewater to recover ammonium sulfate fertilizer.
Performance testing
FIG. 3 is the present inventionPotentiodynamic sweep curve for the electrolyzer of clear example 1; as can be seen from FIG. 3, the electrolyzer has obvious electrolysis current when the electrolysis voltage is higher than 0.6V, and 284.48mA cm can be realized at 1.5V-2。
FIG. 4 is a graph showing the behavior of desulfurized wastewater for reclamation in example 1 of the present invention; constant electrolytic current of 200mA cm-2The working area of the electrode is 1cm2The wastewater treatment capacity is 50 mL; the electrolytic voltage is controlled within 2V, and 94 percent of ammonium sulfite can be electro-oxidized into ammonium sulfate within 20 h.
FIG. 5 is a potentiodynamic sweep curve of an electrolyzer at different temperatures for example 2 of the present invention; from FIG. 5, the electrolyzer shows good performance in the range of 30-90 ℃.
FIG. 6 is a graph of the electrolyzer step voltage test performance of example 3 of the invention; as can be seen in FIG. 6, the electrolyzer can achieve 10mA cm at 0.8V-2The current can be realized at 300mA cm under 1.6V-2The current is applied.
FIG. 7 is a graph showing the behavior of the desulfurized wastewater as a resource in example 4 of the present invention; constant electrolytic current of 100mA cm-2The working area of the electrode is 25cm2The wastewater treatment capacity is 150 mL; the electrolytic voltage is controlled within 3V, and 100 percent of ammonium sulfite can be electrically oxidized into ammonium sulfate within 7 h.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. The method for producing hydrogen by combining electrochemical resource desulfurization wastewater is characterized by comprising the following steps of:
and (3) using the desulfurization wastewater as an anolyte and a sulfuric acid solution as a catholyte, and oxidizing sulfite and producing hydrogen by using an electrolyzer.
2. The method for producing hydrogen by combining electrochemical resource desulfurization waste water and the electrochemical resource desulfurization waste water as claimed in claim 1, wherein the method for producing hydrogen by combining electrochemical resource desulfurization waste water and the electrochemical resource desulfurization waste water comprises the following steps:
step one, introducing desulfurization wastewater and sulfuric acid solution into an anode chamber and a cathode chamber of an electrolyzer respectively; switching on the power supply of the electrolyzer, and collecting the generated hydrogen on the cathode side of the electrolyzer;
and step two, after the concentration of the sulfite in the desulfurization wastewater is reduced to the target concentration or the target product is accumulated to the specified concentration, switching off the power supply, discharging the desulfurization wastewater, and recovering sulfate or persulfate or other resource products from the anode side of the electrolyzer.
3. The method for producing hydrogen by combining electrochemical resource desulfurization waste water with the cooperation of the claim 2, characterized in that the electrolyzer is a diaphragm electrolyzer.
4. The method for producing hydrogen by the cooperation of the electrochemical resource desulfurization waste water as claimed in claim 4, wherein the catalyst is a platinum group metal catalyst, a gold catalyst, a silver catalyst or a lead catalyst.
5. The method for producing hydrogen by combining electrochemical resource desulfurization waste water with the synergy of the electrochemical resource desulfurization waste water as claimed in claim 2, characterized in that the electrolyzer can be used in a reversed mode.
6. The method for producing hydrogen by combining electrochemical resource desulfurization wastewater and hydrogen as claimed in claim 2, wherein the working temperature of the electrolyzer is 40-90 ℃.
7. The method for producing hydrogen by combining electrochemical resource desulfurization wastewater and hydrogen production as claimed in claim 2, wherein the mass fraction of the sulfuric acid solution is 0-20%;
the collecting of the produced hydrogen at the cathode side of the electrolyzer comprises: collecting hydrogen at the cathode liquid storage tank of the electrolyzer by a gas-liquid separation method.
8. An electrochemical resource desulfurization waste water collaborative hydrogen production device for implementing the method for producing hydrogen by combining electrochemical resource desulfurization waste water according to any one of claims 1 to 7.
9. The application of the method for producing hydrogen by the cooperation of electrochemical resource desulfurization waste water as claimed in any one of claims 1 to 7 in desulfurization waste water treatment.
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