CN111905820A - Preparation method of oxygen evolution electrocatalyst containing transition metal organic polymer - Google Patents
Preparation method of oxygen evolution electrocatalyst containing transition metal organic polymer Download PDFInfo
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- CN111905820A CN111905820A CN202010721989.0A CN202010721989A CN111905820A CN 111905820 A CN111905820 A CN 111905820A CN 202010721989 A CN202010721989 A CN 202010721989A CN 111905820 A CN111905820 A CN 111905820A
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- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 36
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 34
- 239000001301 oxygen Substances 0.000 title claims abstract description 34
- 150000003624 transition metals Chemical class 0.000 title claims abstract description 21
- 229920000620 organic polymer Polymers 0.000 title claims abstract description 20
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title description 4
- -1 transition metal salt Chemical class 0.000 claims abstract description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- XJHABGPPCLHLLV-UHFFFAOYSA-N benzo[de]isoquinoline-1,3-dione Chemical compound C1=CC(C(=O)NC2=O)=C3C2=CC=CC3=C1 XJHABGPPCLHLLV-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 239000011572 manganese Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000000446 fuel Substances 0.000 claims description 5
- 125000006384 methylpyridyl group Chemical group 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229910021381 transition metal chloride Inorganic materials 0.000 claims description 3
- 229910002001 transition metal nitrate Inorganic materials 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- 150000003841 chloride salts Chemical class 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003860 storage Methods 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 3
- 238000003763 carbonization Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 5
- 229910001868 water Inorganic materials 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229920000557 Nafion® Polymers 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910021397 glassy carbon Inorganic materials 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- JXRWDHUZHAWOLC-UHFFFAOYSA-N naphthalene-1,2-dicarboxamide Chemical compound C1=CC=CC2=C(C(N)=O)C(C(=O)N)=CC=C21 JXRWDHUZHAWOLC-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
- B01J31/223—At least two oxygen atoms present in one at least bidentate or bridging ligand
- B01J31/2239—Bridging ligands, e.g. OAc in Cr2(OAc)4, Pt4(OAc)8 or dicarboxylate ligands
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- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
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- H01M4/90—Selection of catalytic material
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- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/70—Complexes comprising metals of Group VII (VIIB) as the central metal
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- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/845—Cobalt
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Abstract
The invention relates to an oxygen evolution electrocatalyst containing a transition metal organic polymer, which is prepared by mixing transition metal salt, chain naphthalimide, phthalic acid and NaOH, and putting into deionized water for uniform mixing; the obtained mixture is put into an autoclave with a polytetrafluoroethylene lining for reaction for 2 to 5 days at the temperature of 100-150 ℃, and the transition metal organic polymer which can be used for electrocatalytic oxygen precipitation reaction is obtained after the mixture is slowly cooled to room temperature and is filtered, washed and dried. The advantages are that: the method for preparing the catalyst has the advantages of easily available and cheap raw materials, simple synthesis process, high yield, easy operation, no need of strong heat carbonization, great energy saving, large-scale production and great significance for realizing commercialization of various energy conversion and storage systems finally.
Description
Technical Field
The invention belongs to the field of oxygen evolution electrocatalytic materials, and particularly relates to a preparation method of an oxygen evolution electrocatalyst containing a transition metal organic polymer, which can be used for electrocatalytic oxygen evolution reaction.
Background
With the continuous decrease of traditional fossil energy and the increasing environmental problems, the development of green and sustainable energy has come into the field of people. Hydrogen energy is an important energy source in the future, the share of energy consumption is rapidly increased, and hydrogen production is the basis of hydrogen energy.
Among various hydrogen production methods, (photo) hydro-hydrolysis hydrogen production is always the key development direction in the future, but still faces great challenges in practical application. In the water decomposition reaction, the oxygen evolution reaction of the anode is four orders of magnitude slower than the hydrogen evolution reaction of the cathode, which seriously restricts the hydrogen production efficiency, therefore, the acceleration of the oxygen evolution reaction rate is the key for improving the whole hydrolysis efficiency. On the other hand, the catalysts available for the highly efficient electrocatalytic oxygen evolution reaction are oxides of the noble metals ruthenium and iridium, but their high price and scarcity of resources limit their commercial large-scale use. Meanwhile, the oxygen evolution reaction is also an important reaction in many renewable energy conversion and storage systems (such as a renewable fuel cell, a metal air cell, a hydrolysis hydrogen production system and the like), such as a renewable fuel cell, a chargeable and dischargeable metal air cell and the like, so that the cost of various energy conversion and storage systems can be greatly reduced by developing a high-efficiency non-noble metal catalyst for the electrocatalytic oxygen evolution reaction, and necessary conditions are provided for commercialization of the energy conversion and storage systems.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a high-performance oxygen evolution electrocatalyst containing a transition metal organic polymer, which is simple, efficient and easy to operate, and has good electrocatalytic hydrolysis oxygen evolution reaction performance.
In order to achieve the purpose, the invention is realized by the following technical scheme:
an oxygen evolution electrocatalyst for transition metal containing organic polymers comprising the steps of:
1) mixing transition metal salt, chain naphthalimide, phthalic acid and NaOH, and putting into deionized water for uniform mixing; the amount of the transition metal salt is 0.5 to 6 times of the amount of the chain naphthalimide, the amount of the phthalic acid is 0.5 to 6 times of the amount of the chain naphthalimide, the amount of the NaOH is 1 to 10 times of the amount of the chain naphthalimide, and the molar concentration of the chain naphthalimide is controlled to be 0.001 to 0.02 mol/L;
2) putting the mixture obtained in the step 1) into an autoclave with a polytetrafluoroethylene lining, reacting for 2-5 days at the temperature of 100-150 ℃, slowly cooling to room temperature, filtering, washing and drying to obtain the transition metal organic polymer for the electrocatalytic oxygen evolution reaction.
The metal element in the transition metal salt is more than one of cobalt, nickel and manganese.
The transition metal salt is more than one of transition metal chloride salt, transition metal acetate and transition metal nitrate.
The chain naphthalimide is more than one of N, N-bis (methyl-pyrrolyl) -naphthalimide, N-bis (methyl-pyridyl) -naphthalimide, N-bis (methyl-piperidyl) -naphthalimide, N-bis (amino-pyrrolyl) -naphthalimide, N-bis (amino-pyridyl) -naphthalimide and N, N-bis (amino-piperidyl) -naphthalimide.
The methyl in the chain naphthalimide is dimethyl or tetramethyl.
The transition metal organic polymer obtained in the step 2) is applied to oxygen evolution reactions of fuel cells, metal air cells and electro-hydrolysis hydrogen evolution.
Compared with the prior art, the invention has the beneficial effects that:
1) the method for preparing the catalyst has the advantages of easily available and cheap raw materials, simple synthesis process, high yield, easy operation, no need of strong heat carbonization, great energy saving, large-scale production and great significance for realizing commercialization of various energy conversion and storage systems finally.
2) The transition metal polymer produced by the invention shows excellent high-current electrocatalytic hydrolysis oxygen evolution performance and can be used for large-scale hydrolysis hydrogen production reaction.
Drawings
FIG. 1 shows [ Ni (L) (1,2-BDC) (H)2O)2]·3H2Crystal structure diagram of O;
FIG. 2 shows [ Ni (L) (1,2-BDC) (H)2O)2]·3H2O is loaded on the oxygen precipitation linear scanning curve of the rotating disk electrode;
FIG. 3 is [ Co (L) (1,3-BDC) (H)2O)2]·3H2Crystal structure diagram of O;
FIG. 4 is [ Co (L) (1,3-BDC) (H)2O)2]·3H2O is loaded on the oxygen precipitation linear scanning curve of the rotating disk electrode;
FIG. 5 shows [ Mn (L) (2,5-BDC) (H)2O)2]·3H2Crystal structure diagram of O;
FIG. 6 shows [ Mn (L) (2,5-BDC) (H)2O)2]·3H2O oxygen evolution on a rotating disk electrode linear scan curve.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings, but it should be noted that the present invention is not limited to the following embodiments.
An oxygen evolution electrocatalyst for transition metal containing organic polymers comprising the steps of:
1) mixing transition metal salt, chain naphthalene dicarboxamide (hereinafter referred to as L), phthalic acid (hereinafter referred to as BDC) and NaOH, and putting into deionized water for uniform mixing; the amount of the transition metal salt is 0.5-6 times of the amount of the L substance, the amount of the BDC substance is 0.5-6 times of the amount of the L substance, the amount of the NaOH substance is 1-10 times of the amount of the L substance, and the molar concentration of the L is controlled to be 0.001-0.02 mol/L;
2) putting the mixture obtained in the step 1) into an autoclave with a polytetrafluoroethylene lining and a volume of 250-500 ml, reacting for 2-5 days at the temperature of 100-150 ℃, slowly cooling to room temperature, filtering, washing and drying to obtain the transition metal organic polymer for the electrocatalytic oxygen evolution reaction. The transition metal organic polymer is applied to oxygen evolution reactions of fuel cells, metal air cells and electro-hydrolysis hydrogen evolution.
Wherein the transition metal salt is one or more of transition metal chloride, transition metal acetate and transition metal nitrate. The chain naphthalimide is more than one of N, N-bis (methyl-pyrrolyl) -naphthalimide, N-bis (methyl-pyridyl) -naphthalimide, N-bis (methyl-piperidyl) -naphthalimide, N-bis (amino-pyrrolyl) -naphthalimide, N-bis (amino-pyridyl) -naphthalimide and N, N-bis (amino-piperidyl) -naphthalimide.
Example 1
N, N-bis (methyl-pyrrolyl) -naphthalimide, N-bis (methyl-pyridyl) -naphthalimide, N-bis (methyl-piperidyl) -naphthalimide, N-bis (amino-pyrrolyl) -naphthalimide, N-bis (amino-pyridyl) -naphthalimide, N-bis (amino-piperidyl) -naphthalimide
[Co(L)(1,2-BDC)(H2O)2]·3H2And (3) synthesis of O: based on L (N, N-bis (methyl-pyridyl) -naphthalamide) (amount of substance 0.002mol), CoCl was added2·6H2O、L、1,2-H2BDC and NaOH are 3: 1: 3: 6 was mixed with deionized water and the mixture was placed in a 250mL teflon-lined autoclave and stored at 120 c for 4 days. Slowly cooled to room temperature, filtered, washed and dried to obtain [ Co (L) (1,2-BDC) (H)2O)2]·3H2The crystal structure of O is shown in FIG. 1.
5mg of [ Co (L) (1,2-BDC) (H) are weighed out2O)2]·3H2O into a centrifuge tube, 0.49mL of deionized water, 0.49mL of absolute ethanol and 0.02mL of Nafion (5% by mass) solution are added, ultrasonic treatment is carried out for 30 minutes, 8.3. mu.L of the solution is sucked by a pipette and dropped on a glassy carbon rotating disk electrode (the diameter is 5 mm), and after drying at room temperature, linear scanning is carried out in an oxygen-saturated 1M KOH solutionThe curves are shown in fig. 2.
Example 2
[Ni(L)(1,3-BDC)(H2O)2]·3H2And (3) synthesis of O: based on L (N, N-bis (methyl-pyridyl) -naphthalamide) (amount of substance 0.001mol), Ni2(CH3COO)2、L、1,2-H2BDC and NaOH are respectively 2: 1: 2: 4 was mixed with deionized water and the mixture was placed in a 150mL teflon-lined autoclave and stored at 120 c for 4 days. Slowly cooled to room temperature, filtered, washed and dried to obtain [ Ni (L) (1,3-BDC) (H)2O)2]·3H2The crystal structure of O is shown in FIG. 3.
Weighing 5mg of [ Ni (L) (1,3-BDC) (H)2O)2]·3H2O samples were loaded into a centrifuge tube, 0.49mL deionized water, 0.49mL absolute ethanol and 0.02mL Nafion (5% by mass) solution were added, sonicated for 30 minutes, 8.3. mu.L of the solution was pipetted onto a glassy carbon rotating disk electrode (5 mm diameter), dried at room temperature and tested for linear scan curves in oxygen saturated 1M KOH solution as shown in FIG. 4.
Example 3
[Mn(L)(2,5-BDC)(H2O)2]·3H2And (3) synthesis of O: based on L (N, N-bis (methyl-pyridyl) -naphthalamide) (amount of substance 0.001mol), MnCl2、L、1,2-H2BDC and NaOH are respectively 1: 1: 1: 3 with an appropriate amount of deionized water, the mixture was placed in a 200mL teflon-lined autoclave and stored at 120 c for 4 days. Slowly cooled to room temperature, filtered, washed and dried to obtain [ Mn (L) (2,5-BDC) (H)2O)2]·3H2The crystal structure of O is shown in FIG. 5.
A5 mg sample was weighed into a centrifuge tube, 0.49mL deionized water, 0.49mL absolute ethanol and 0.02mL Nafion (5% by mass) solution were added, sonicated for 30 minutes, 8.3. mu.L of the solution was pipetted onto a glassy carbon rotating disk electrode (5 mm diameter), and the linear scan curve for testing in oxygen saturated 1M KOH solution after drying at room temperature is shown in FIG. 6.
Claims (6)
1. An oxygen evolution electrocatalyst for transition metal containing organic polymers, comprising the steps of:
1) mixing transition metal salt, chain naphthalimide, phthalic acid and NaOH, and putting into deionized water for uniform mixing; the amount of the transition metal salt is 0.5 to 6 times of the amount of the chain naphthalimide, the amount of the phthalic acid is 0.5 to 6 times of the amount of the chain naphthalimide, the amount of the NaOH is 1 to 10 times of the amount of the chain naphthalimide, and the molar concentration of the chain naphthalimide is controlled to be 0.001 to 0.02 mol/L;
2) putting the mixture obtained in the step 1) into an autoclave with a polytetrafluoroethylene lining, reacting for 2-5 days at the temperature of 100-150 ℃, slowly cooling to room temperature, filtering, washing and drying to obtain the transition metal organic polymer for the electrocatalytic oxygen evolution reaction.
2. The transition metal-containing organic polymer oxygen evolution electrocatalyst according to claim 1, characterized in that the metal element in the transition metal salt is one or more of cobalt, nickel, manganese.
3. The transition metal-containing organic polymer oxygen evolution electrocatalyst according to claim 1, characterized in that the transition metal salt is one or more of transition metal chloride salt, transition metal acetate, transition metal nitrate.
4. The transition metal-containing organic polymer oxygen evolution electrocatalyst according to claim 1, wherein the chain naphthalimide is one or more of N, N-bis (methyl-pyrrolyl) -naphthalimide, N-bis (methyl-pyridyl) -naphthalimide, N-bis (methyl-piperidyl) -naphthalimide, N-bis (amino-pyrrolyl) -naphthalimide, N-bis (amino-pyridyl) -naphthalimide, N-bis (amino-piperidyl) -naphthalimide.
5. The transition metal-containing organic polymer oxygen evolution electrocatalyst according to claim 4, characterized in that the methyl group in the chain naphthalimide is dimethyl or tetramethyl.
6. The oxygen evolution electrocatalyst for transition metal-containing organic polymers according to claim 1, wherein the transition metal organic polymers obtained in step 2) are used in oxygen evolution reactions in fuel cells, metal air cells, electro-hydrolysis hydrogen evolution.
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