CN107321686B - Cleaning method and cleaning solution for aluminum-air battery catalyst - Google Patents
Cleaning method and cleaning solution for aluminum-air battery catalyst Download PDFInfo
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- CN107321686B CN107321686B CN201710415444.5A CN201710415444A CN107321686B CN 107321686 B CN107321686 B CN 107321686B CN 201710415444 A CN201710415444 A CN 201710415444A CN 107321686 B CN107321686 B CN 107321686B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
Abstract
The invention discloses a cleaning method and a cleaning solution for an aluminum-air battery catalyst, which comprises the following steps: mixing and stirring a catalyst and a first cleaning solution for a first specified time at a first temperature, and filtering to obtain first filter residue; mixing and stirring the first filter residue and a second cleaning solution for a second designated time at a second temperature, and filtering to obtain a second filter residue; mixing and stirring the second filter residue and a third cleaning solution for a third designated time at a third temperature, and filtering to obtain a third filter residue; and at a fourth temperature, washing and filtering the third filter residue by using purified water until the pH value of the filtrate reaches 6-8, thereby obtaining the washed catalyst. The catalyst is cleaned by a first cleaning solution and a second cleaning solution which are weak in acidity so as to achieve the purpose of adjusting the pH value; the third cleaning solution with strong acidity corrodes the surface of the catalyst, so that the surface roughness of the catalyst is increased, the contact area of the catalyst is increased, and the catalytic performance is improved.
Description
Technical Field
The invention relates to the field of new energy, in particular to a method for cleaning an aluminum-air battery catalyst and a cleaning solution thereof.
Background
The metal-air battery is a new generation of green storage battery, and has the advantages of low manufacturing cost, high specific energy, recyclable raw materials and excellent performance. At present, zinc-air batteries, aluminum-air batteries, lithium-air batteries and the like are the most studied metal-air batteries. In a potential sequence, aluminum is more active than zinc, and higher battery voltage can be obtained; one aluminum atom can release three electrons, and the aluminum can improve the energy of the battery; in addition, the aluminum reserves are abundant and the price is low, so the research progress of the aluminum air battery is very rapid, and the aluminum air battery is an air battery with development prospect.
An aluminum-air battery is a novel battery which takes aluminum and air as battery materials. Aluminum has its unique advantages as an anode material for air cells: the electrochemical equivalent is high, the electrochemical equivalent of the aluminum is 2980 A.h/kg, and the aluminum is the highest metal except lithium; the electrode potential is more negative, the standard electrode potential is-2.35V (vs. SHE) in alkaline solution, and for the anode material, the more negative the potential, the better the potential, and the battery can provide larger electromotive force; the aluminum has rich resources and low price. At present, the first problems of the aluminum anode material for the air battery are as follows: the self-corrosion of aluminum in alkaline solution is serious, which causes the utilization rate of the anode to be greatly reduced, and the commercial application of the aluminum-air battery is hindered. Researchers develop a novel aluminum anode material through microalloying, and a corresponding electrolyte corrosion inhibitor is added, so that the self-corrosion rate of aluminum can be reduced. The common alloying elements of the anode material of the aluminum-air battery mainly comprise zinc, magnesium, gallium, indium, tin, lead, mercury, bismuth and the like. These elements are added to aluminum to form ternary, quaternary, etc. multi-element alloys.
The aluminum-air battery consists of an aluminum anode, an air cathode and electrolyte; during the discharging process, oxygen in the air enters the electrolyte through the air cathode to reach the reaction interface to generate reduction reaction, and electric energy is released. The catalytic layer is a key part of the air electrode and plays a decisive role in the electrochemical performance, and the performance of the aluminum air cell depends to a large extent on the cathode catalyst selected. The performance of the air electrode can directly influence the reaction balance of the electrode, so that the performance of the air electrode is improved, the utilization rate of the cathode of the aluminum air battery can be improved to a certain extent, the self-corrosion of the cathode aluminum is inhibited, and the commonly used aluminum air battery catalyst generally comprises the following types:
noble metal catalyst: platinum and silver are commonly used, and the catalytic activity is high, the performance is stable, but the availability is not high due to the high price and the shortage of resources.
Metallomacrocycle catalysts: organometallic macrocycles have good catalytic activity for oxygen reduction, especially when they are adsorbed on large surface area carbon. And their activity and stability can be significantly improved by heat treatment. Therefore, the catalyst is expected to replace a noble metal oxygen reduction catalyst. Common methods for synthesizing metal macrocyclic compounds include thermal decomposition and precursor preparation. However, the thermal treatment process of the thermal decomposition method causes a reaction between the metal macrocyclic compound and the carbon substrate, and the catalyst prepared by the precursor method has poor activity, so that the application has certain problems.
Perovskite-type oxide catalyst: the perovskite type oxide has high catalytic activity on reduction and precipitation of oxygen and low price, so the perovskite type oxide has wide application prospect in aluminum air batteries and fuel cells. Current research on perovskite oxygen electrode catalysts has focused primarily on improving the preparation process and on finding new replacement elements to improve catalytic performance. The amorphous precursor method, especially the malic acid precursor method, can prepare perovskite oxides with fine crystal grains and large specific surface area, thereby greatly improving the catalytic activity of the perovskite oxides, and is a better method for preparing the perovskite oxides at present.
Cheap catalyst: the most important representative is manganese dioxide catalyst, which has the greatest advantages of abundant raw materials and low cost and can be widely applied to batteries of aqueous or non-aqueous electrolyte, but the electrocatalytic activity of single manganese dioxide has a certain limit, so that the research of people in this field has never been stopped.
AB2O4 spinel type oxide catalyst: the crystal lattice of spinel is face-centered cubic. There are 32 close-packed 02-ions in the unit cell, 64 tetrahedral voids and 32 octahedral voids occupied by metal ions. The dehydration activity of spinel is related to the fraction of B ions in tetrahedral voids, the larger the fraction is, the surface acidity of the catalyst is increased, and the dehydration activity is increased, and the catalyst is not adopted by the aluminum-air battery generally.
Other metal and alloy catalysts: nickel is relatively inexpensive and has high corrosion resistance under anodic polarization conditions in alkaline electrolytes, while the oxygen evolution efficiency of nickel is the highest among the metallic elements, so nickel has been conventionally used as an alkaline water electrolysis anode material. Nickel-iron, nickel-cobalt, and other alloy catalysts, which have good catalytic activity and corrosion resistance, are also frequently used, and are considered catalyst orientations for aluminum-air batteries.
Composite catalyst: two or more catalysts are compounded together to better improve the catalytic activity of the air electrode of the aluminum-air battery.
Most of the catalysts manufactured in the prior art are alkaline after production, and the catalysts have good catalytic performance and neutral pH value, so that how to adjust the pH value of the catalysts is a problem which needs to be solved urgently nowadays.
Disclosure of Invention
The invention mainly aims to provide an aluminum-air battery electrolyte, and provides a cleaning method capable of adjusting the pH value of a catalyst so as to improve the catalytic performance of the catalyst.
The invention provides a liquid and a third cleaning liquid, wherein the pH value of the first cleaning liquid is 4.5-5; the pH value of the second cleaning solution is between 3.5 and 4.5; the pH value of the third cleaning solution is between 2 and 3, and the method further comprises the following steps:
mixing and stirring the catalyst and the first cleaning solution for a first specified time at a first temperature, and filtering to obtain first filter residue;
mixing and stirring the first filter residue and the second cleaning liquid for a second designated time at a second temperature, and filtering to obtain a second filter residue;
mixing and stirring the second filter residue and the third cleaning solution for a third designated time at a third temperature, and filtering to obtain a third filter residue;
and at a fourth temperature, washing and filtering the third filter residue by using purified water until the pH value of the filtrate reaches 6-8, thereby obtaining the washed catalyst.
Further, in the method for cleaning the aluminum-air battery catalyst, the filtering is reduced pressure filtering, vacuum filtering or suction filtering.
Further, the method for cleaning the aluminum-air battery catalyst further includes, after the step of cleaning and filtering the third filter residue with purified water at the fourth temperature until the PH of the filtrate reaches 6 to 8 to obtain a cleaned catalyst:
and drying the cleaned catalyst.
Further, in the method for cleaning the aluminum-air battery catalyst, the surface temperature of the cleaned catalyst in the drying process is less than 150 ℃.
Further, in the method for cleaning the aluminum-air battery catalyst, the first specified temperature, the second specified temperature and the third specified temperature are all between 70 ℃ and 90 ℃.
Further, in the method for cleaning the aluminum-air battery catalyst, the fourth designated temperature is between 40 ℃ and 85 ℃.
Further, in the method for cleaning the aluminum-air battery catalyst, the first designated time is 15 to 35 minutes.
Further, in the method for cleaning the aluminum-air battery catalyst, the second designated time is between 5 and 30 minutes.
Further, in the method for cleaning the aluminum-air battery catalyst, the third designated time is 5 to 30 seconds.
A cleaning solution for an aluminum-air battery catalyst comprises a first cleaning solution, a second cleaning solution and a third cleaning solution, wherein solutes of the first cleaning solution, the second cleaning solution and the third cleaning solution respectively comprise one or more of sulfuric acid, hydrochloric acid, nitric acid, oxalic acid and acetic acid.
According to the cleaning method and the cleaning solution for the aluminum-air battery catalyst, the catalyst is cleaned by the first cleaning solution and the second cleaning solution which are weak in acidity, so that the purpose of adjusting the pH value is achieved; the third cleaning solution with strong acidity corrodes the surface of the catalyst, so that the surface roughness of the catalyst is increased, the contact area of the catalyst is increased, and the catalytic performance is improved.
Drawings
FIG. 1 is a schematic flow chart of a method for cleaning an aluminum-air battery catalyst according to an embodiment of the present invention;
fig. 2 is a schematic flow chart of a method for cleaning an aluminum-air battery catalyst according to an embodiment of the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Referring to fig. 1, in an embodiment of the present invention, the present invention provides a method for cleaning an aluminum-air battery catalyst, including a first cleaning solution, a second cleaning solution, and a third cleaning solution, where a PH of the first cleaning solution is between 4.5 and 5; the pH value of the second cleaning solution is between 3.5 and 4.5; the pH value of the third cleaning solution is between 2 and 3, and the method further comprises the following steps: s1, mixing and stirring the catalyst and the first cleaning liquid for a first designated time at a first temperature, and filtering to obtain a first filter residue; s2, mixing and stirring the first filter residue and the second cleaning liquid for a second designated time at a second temperature, and filtering to obtain a second filter residue; s3, mixing and stirring the second filter residue and the third cleaning solution for a third designated time at a third temperature, and filtering to obtain a third filter residue; and S4, washing the third filter residue with purified water at a fourth temperature, and filtering until the pH value of the filtrate reaches 6-8 to obtain the washed catalyst.
Mixing the catalyst and the first cleaning solution at a first temperature, stirring for a first designated time, and filtering to clean alkaline residues on the surface of the catalyst to obtain a first filter residue, wherein the catalyst generally comprises a new catalyst obtained by production and an old catalyst obtained by recycling waste batteries; the first designated time is generally 15-35 minutes, and in the embodiment of the present invention, preferably 20-30 minutes, because the first cleaning agent is an acidic cleaning agent with a relatively high PH value, a relatively long time is required for the first cleaning agent to effectively clean the residues on the catalyst to ensure the completeness of cleaning; wherein, the first temperature is generally between 60 ℃ and 95 ℃, in the embodiment of the invention, the preferred temperature is between 65 ℃ and 95 ℃, at which the cleaning agent can clean the catalyst efficiently and the catalyst can not be deactivated due to overhigh temperature, the first cleaning solution is slowly added into the catalyst during the mixing process, the stirring is continuously carried out during the mixing process, and the filtering is carried out after the stirring time reaches a specified time, wherein, the filtering in the step S1 is preferably reduced pressure filtering, vacuum filtering and suction filtering;
mixing the first filter residue obtained in the step S1 with the second cleaning solution at a second temperature, stirring for a second designated time, preferably 5-30 minutes, in the embodiment of the present invention, and filtering to clean the alkaline residue and the remaining stains on the surface of the catalyst, wherein the second designated time is also 5-15 minutes, and the second cleaning solution is also an acidic cleaning solution with a relatively high PH value, so that a relatively long time is required for the reaction to effectively clean the residue on the catalyst; wherein, the second temperature is generally between 60 ℃ and 95 ℃, in the embodiment of the invention, the preferred temperature is between 65 ℃ and 95 ℃, at which the cleaning agent can clean the catalyst efficiently and the catalyst can not be deactivated due to overhigh temperature, the second cleaning solution is slowly added into the catalyst during the mixing process, the stirring is continuously carried out during the mixing process, and the filtering is carried out after the stirring time reaches the specified time, wherein, the filtering in the step S2 is preferably reduced pressure filtering, vacuum filtering and suction filtering;
mixing the second filter residue obtained in the step S3 and the third cleaning solution at a third temperature, stirring for a third specified time and filtering, so as to corrode the surface of the cleaned catalyst to make the surface of the catalyst rougher, thereby increasing the surface area of the catalyst and improving the catalytic efficiency, wherein the third specified time is generally 5 to 30 seconds, preferably 10 to 20 seconds in the embodiment of the present invention, and the third cleaning solution is an acidic cleaning agent with a relatively low PH value, so that a relatively short time of reaction is required, and the excessive corrosion degree is prevented from affecting the catalytic effect of the catalyst after the third specified time is too long; wherein, the third temperature is generally between 60 ℃ and 95 ℃, in the embodiment of the present invention, the preferred temperature is between 65 ℃ and 95 ℃, at which temperature, the cleaning agent is ensured to corrode the surface of the catalyst at an ideal rate, the catalyst is easily corroded too much by too high temperature to affect the quality of the catalyst, the best effect is not achieved by too low corrosion, and the catalyst is also ensured not to be deactivated by too high temperature, the third cleaning solution is slowly added into the catalyst during the mixing process, stirring is continuously carried out during the mixing process, and after the stirring time reaches a specified time, filtering is carried out, wherein, the filtering in the step S3 is preferably reduced pressure filtering;
and (4) cleaning and filtering the filter residue obtained in the step S3 by using purified water until the pH value of the filtrate reaches 6-8, wherein the filtrate is generally the cleaning residual acid liquor in the step S4.
In this embodiment, in the method for cleaning an aluminum-air battery catalyst, the filtering is reduced-pressure filtering, because the cleaning method uses an acidic liquid as a cleaning solution, it is important to ensure the contact time between the cleaning solution and the catalyst, if the cleaning is not complete due to too short contact time with the cleaning solution, the catalyst is destroyed and deactivated due to too long contact time, and in step S1-3, the catalyst is contacted with the cleaning solution, so that in order to ensure that the contact time between the catalyst and the cleaning solution does not exceed a preset time period, the solution in step S1-3 is filtered by a rapid filtering method such as reduced-pressure filtering, vacuum filtering or suction filtering to reduce the time error caused by the filtering time, thereby affecting the cleaning effect.
Referring to fig. 2, in this embodiment, the method for cleaning an aluminum-air battery catalyst, at the fourth temperature, cleaning and filtering the third filter residue with purified water until the PH of the filtrate reaches 6 to 8, and obtaining a cleaned catalyst, further includes: and S5, drying the cleaned catalyst.
And (3) drying the third filter residue obtained in the step S4 in the step S5, wherein the drying temperature is not higher than 150 ℃, preferably 105 ℃ to 125 ℃ in the embodiment of the invention, so as to prevent the catalyst from being damaged due to too high temperature.
In this embodiment, in the method for cleaning the aluminum-air battery catalyst, the surface temperature of the filter residue in the drying process is not higher than 150 ℃, and in this embodiment of the present invention, the temperature is preferably between 105 ℃ and 125 ℃, so as to prevent the catalyst from being damaged due to an excessively high temperature.
In this embodiment, in the method for cleaning the aluminum-air battery catalyst, the first specified temperature, the second specified temperature and the third specified temperature are all between 60 ℃ and 95 ℃, and in the embodiment of the present invention, the preferred temperature is between 65 ℃ and 95 ℃.
In this embodiment, in the method for cleaning the aluminum-air battery catalyst, the fourth specified temperature is between 40 ℃ and 85 ℃, in an embodiment of the present invention, the temperature is preferably between 45 ℃ and 75 ℃, and the fourth temperature is generally lower than the third temperature, so as to slow down the corrosion effect of the third cleaning agent and prevent the cleaning agent attached to the surface of the catalyst from corroding the catalyst again due to the excessively high temperature of the purified water during cleaning.
In this embodiment, in the method for cleaning the aluminum-air battery catalyst, the first designated time is 15-35 minutes, and in this embodiment of the present invention, preferably 20-30 minutes, since the first cleaning agent is an acidic cleaning agent with a relatively high PH, a relatively long reaction time is required to effectively clean the residues on the catalyst to ensure the completeness of cleaning.
In this embodiment, the second designated time is between 5 minutes and 30 minutes, preferably between 5 minutes and 15 minutes in the embodiment of the present invention, and the second cleaning agent is also an acidic cleaning agent with a relatively high PH, so that a relatively long reaction time is required to effectively clean the residues on the catalyst.
In this embodiment, in the method for cleaning the aluminum-air battery catalyst, the third designated time is between 5 seconds and 30 seconds, and in this embodiment of the present invention, preferably between 10 seconds and 20 seconds, since the third cleaning agent is an acidic cleaning agent with a relatively low PH, a relatively short time is required for the reaction, and the catalytic effect of the catalyst is prevented from being affected by excessively long time and excessively high corrosion degree.
A cleaning solution for an aluminum-air battery catalyst comprises a first cleaning solution, a second cleaning solution and a third cleaning solution, wherein solutes of the first cleaning solution, the second cleaning solution and the third cleaning solution respectively comprise one or more of sulfuric acid, hydrochloric acid, nitric acid, oxalic acid and acetic acid; the pH value of the first cleaning solution is between 4.5 and 5; the pH value of the second cleaning solution is between 3.5 and 4.5; the pH of the third wash liquid is comprised between 2 and 3.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. The method for cleaning the aluminum-air battery catalyst is characterized by comprising a first cleaning solution, a second cleaning solution and a third cleaning solution, wherein the pH value of the first cleaning solution is 4.5-5; the pH value of the second cleaning solution is between 3.5 and 4.5; the pH value of the third cleaning solution is between 2 and 3, and the method further comprises the following steps:
mixing and stirring the catalyst and the first cleaning solution for a first specified time at a first temperature, and filtering to obtain first filter residue;
mixing and stirring the first filter residue and the second cleaning liquid for a second designated time at a second temperature, and filtering to obtain a second filter residue;
mixing and stirring the second filter residue and the third cleaning solution for a third designated time at a third temperature, and filtering to obtain a third filter residue;
at a fourth temperature, cleaning and filtering the third filter residue by using purified water until the pH value of the filtrate reaches 6-8 to obtain a cleaned catalyst; the fourth temperature is lower than the third temperature.
2. The method for cleaning the aluminum-air battery catalyst according to claim 1, wherein the filtration is reduced pressure filtration, vacuum filtration or suction filtration.
3. The method for cleaning the catalyst of the aluminum-air battery according to claim 1, wherein the step of cleaning and filtering the third filter residue with purified water at the fourth temperature until the pH value of the filtrate reaches 6-8 to obtain the cleaned catalyst further comprises:
and drying the cleaned catalyst.
4. The method of claim 3, wherein the surface temperature of the cleaned catalyst during the drying process is less than 150 degrees Celsius.
5. The method of cleaning an aluminum-air cell catalyst as recited in claim 1 wherein the first temperature, the second temperature and the third temperature are each between 60 ℃ and 95 ℃.
6. The method of cleaning an aluminum-air cell catalyst as set forth in claim 1, wherein the fourth temperature is between 40 ℃ and 85 ℃.
7. The method of cleaning an aluminum-air cell catalyst according to any one of claims 1 to 6, wherein the first prescribed time is between 15 and 35 minutes.
8. The method of cleaning an aluminum-air cell catalyst according to any one of claims 1 to 6, wherein the second designated time is between 5 and 30 minutes.
9. The method of cleaning an aluminum-air cell catalyst according to any one of claims 1 to 6, wherein the third specified time is between 5 and 30 seconds.
10. An aluminum-air battery catalyst cleaning solution, which is used for cleaning an aluminum-air battery catalyst by the aluminum-air battery catalyst cleaning method according to any one of claims 1 to 9, and is characterized by comprising a first cleaning solution, a second cleaning solution and a third cleaning solution, wherein solutes of the first cleaning solution, the second cleaning solution and the third cleaning solution respectively comprise one or more of sulfuric acid, hydrochloric acid, nitric acid, oxalic acid and acetic acid, and the pH value of the first cleaning solution is between 4.5 and 5; the pH value of the second cleaning solution is between 3.5 and 4.5; the pH value of the third cleaning solution is between 2 and 3.
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